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~ " ' MM II II II II MM Mill MM II I II

J European Patent Office


© Publication number: 0 2#>«
9 4>i f0t1l i0n nB 1i
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Office europeen J
des brevets

© EUROPEAN PATENT SPECIFICATION

© Date of publication of patent specification: 06.05.92 © Int. CI.5: C1 1 D 17/00, C11D 1 3 / 0 0

© Application number: 88300763.5

@ Date of filing: 29.01.88

Process and apparatus for the continuous production of transparent soap.

© Priority: 30.04.87 US 44221 © Proprietor: NEUTROGENA CORPORATION


5755 West 96th Street
@ Date of publication of application: Los Angeles California 90045(US)
07.12.88 Bulletin 88/49
@ Inventor: Jungermann, Eric
© Publication of the grant of the patent: 2323 N Central Avenue
06.05.92 Bulletin 92/19 Phoenix Arizona 85004(US)
Inventor: Hassapls, Thomas
© Designated Contracting States: 8472 Ivy Circle
AT BE CH DE ES FR GB GR IT LI LU NL SE Huntington Beach California 92646(US)
Inventor: Scott, Richard A.
© References cited: 2036 Valley Street
DE-A- 1 082 690 Burbank California 91505(US)
FR-A- 1 062 600 Inventor: Wortzman, Mitchell S.
US-A-2 578 366 5818 W 75th Street
US-A- 3 926 828 Los Angeles California 90045(US)

© Representative: Coxon, Philip et al


Eric Potter & Clarkson St. Mary's Court St.
Mary's Gate
Nottingham NG1 1LE(GB)

00

CM
Note: Within nine months from the publication of the mention of the grant of the European patent, any person
may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition
shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee
has been paid (Art. 99(1) European patent convention).
Rank Xerox (UK) Business Services
(3.08/2. 19/2.0)
EP 0 294 010 B1

Description

The present invention relates to soap and more particularly to new and improved compositions and
processes for the continuous production of transparent soap bars.
5 The basic reactions in soapmaking are quite simple. They either consist of reacting fat with an alkali to
produce soap and glycerine, or to neutralize fatty acids with an alkali. On the other hand, the technology of
soapmaking is quite involved, and practical soapmaking borders at times on an art because of the complex
physical nature of soap and its aqueous systems. Saponification of fats is in itself an exacting operation and
is illustrated by Equation 1, below:
70

H2C"°"(f0"Rl H
H 2C?- 'O0 H
H
HC-0-CO-R2 + 3 NaOH- - 3 R-COONa + HC-OH
I
75 H C-O-io-R" H C-OH
1 3 72

wherein Ri represents saturated, unsaturated, polyunsaturated, or branched aliphatic chains having C = 7-


19;
20 R2 represents saturated, unsaturated, polyunsaturated, or branched aliphatic chains having C = 7-19;
R3 represents saturated, unsaturated, polyunsaturated, or branched aliphatic chains having C = 7-19; and
R represents a mixture of R1 , R2 and R3.

Equation 1.
25
In this process, the soap, after saponification, is usually carried through a series of phase changes for
the removal of impurities, the recovery of glycerine, and reduction of the moisture content to a relatively low
level. The complex series of operations in the production of an ordinary full-boiled or settled soap is as
follows: (a) reaction of the fat with alkali until it is largely saponified, (b) graining out of the soap from
30 solution with salt in two or more stages for recovery of the glycerol produced by the reaction; (c) boiling of
the material with an excess of alkali to complete saponification, followed by graining out with alkali; and (d)
separation of the batch into immiscible phases of neat soap and niger, the so-called "fitting" operation. The
final result is "neat" soap with a composition ranging from 60-65% soap and about 35-40% water, plus
small amounts of salt and glycerine.
35 When fatty acids are used as the starting material, reaction with alkali is a conventional neutralization as
shown in equation 2.

R- COOH + NaOH - R-COONa + H20

40 Equation 2.

The fatty acids are usually obtained by splitting fats into fatty acids and glycerol using high pressure
steam with and without the use of a catalyst. (Bailey's Industrial Oil and Fat Products, 4th Edition, Volume 1,
Chapter 8, pp 99-103, John Wiley and Sons Inc., 1979.) This is followed by distillation of the crude fatty
45 acids and neutralization of the distilled fatty acids. Selection of the proper concentration of alkali will result
in the production of neat soap described above. For the production of non transparent and certain
translucent soaps, the neat soap is then dried to a moisture content of 12-15%.
A breakthrough from the traditional soap-boiling processes was the advent of various continuous
saponification processes which emerged after World War II. These processes fell into two main categories:
50 those based on the continuous saponification of fats, i.e., the DeLaval, the Sharpies, Mechaniche Moderne,
and the Mazzoni SCN-LR processes; and those based on the continuous splitting of fats into fatty acids
followed by distillation and neutralization. Typical examples are the Mazzoni SC and the Armour-Dial
processes. A more complete description of these processes appears in Bailey's (Ibid, pp. 535-549), and will
not be repeated here.
55 In spite of the development of continuous soapmaking processes, industry has heretofore been unable
to adapt any of these processes to the efficient and economical production of high quality transparent
soaps. Transparent soaps are traditionally prepared by the semi-boiled or by the "cold process", utilizing

2
EP 0 294 010 B1

special fat blends. (Bailey's, Ibid, pg. 534.) They often contain additives such as sugar, glycerol, alcohol,
triethanolamine and rosins. They are poured into frames, held at room temperature for periods of time, and
thereafter cut into bars.
Processes for the manufacture of transparent soaps have been known for a long time, the oldest
5 recorded product being "Pears Transparent Soap" which was first offered for sale in England in 1789.
As a point of reference, "transparent soap", as that term is used herein encompasses soaps having a
wide degree of color and gloss but which are sufficiently transparent so that one with normal vision can
effectively see through a toilet sized bar. Specifically, if 14 point type can be seen through a 0.00635 m (1/4
inch) thick bar of soap, that bar of soap is defined as "transparent". (Wells, F.M., Soap and Cosmetic
w Specialties, 31 (6-7) June-July, 1955.)
Because regular and transparent soaps traditionally have a pH of 10 or higher, and many transparent
soaps often contained alcohol, they acquired a reputation of causing skin dryness. Fromont (U.S.
2,820,768) addressed this issue with a less alkaline transparent soap free of alcohol and based on a blend
of sodium and triethanolamine soaps from tallow, coconut oil and castor oil and "superfatted" with fatty
is acids such as stearic acid and oleic acid. Soap manufactured under this patent was marketed under the
trade name Neutrogena® and found to be exceptionally mild. The mildness of this formula has been
demonstrated using the Soap Chamber Test. (Frosch, P.J. and Kligman, A.M.: (The Soap ChamberTest, J.
American Academy Dermatology, 1:35, 1979 and Dyer, D. and Hassapis, T. Comparison of Detergent
Based Versus Soap Based Liquid Soap, Soap Cosmetic and Chemical Specialties, July, 1983). In this test,
20 an 8% soap solution is applied to the arms of volunteers using an occlusive patch/chamber. The soaps are
applied for 8 hours per day for 5 days, and the resultant damage to the skin is rated. In this testing the
Neutrogena® transparent bar formula has been shown to be milder than the other bar soaps tested. In
addition, this mildness has also been demonstrated in exaggerated use tests and antecubical wash test.
(Principle of Cosmetics for the Dermatologist, Frost, P. and Horwitz, S., Chapter 1, pp 5-12, C.V. Mosby
25 Company, T982T)
Pape (U.S. 2,005,160) described a method for making milled transparent soap from a blend containing
rosin but no alcohol or sugar. The process included "shock cooling", that is, reducing the temperature of
the soap mass from 100 ° C to 20 ° C in 2 seconds.
Later, Kelly (U.S. Patent 2,970,116; French Patent 1,291,638; and U.K. Pat. 1,033,422) developed a
30 process for making milled translucent soaps by mechanical working and milling at controlled temperatures
and vacuum plodding. Though having obvious advantages over the older processes, Kelly's processes
never achieved any wide scale use or success. The bars were translucent and did not achieve the
transparency defined previously.
Kamer et al (U.S. 3,562,167) taught a batch process for making a transparent soap formulation
35 containing specified nonionic surfactants. In addition, Lager was granted U.S. Patent No. 3,969,259 for
incorporating germicides such as 2,4,4' -trichloro-2'-hydroxydiphenyl ether (Irgasan DP 300) into transparent
soap bars.
At this point in time, the production of transparent soaps worldwide remains a batch process;
continuous production without serious aesthetic defects (i.e. loss of transparency) has not been obtained.
40 The economic desideratum still eludes the industry for, except as indicated, the production of
transparent soap remains a batch by batch process and continual production without serious aesthetic
defects has not been obtained.
The present invention is directed to a process for the continuous production of transparent soap while
improving the economy of production, enhancing the volume and rate of production without sacrificing any
45 of the clarity associated with batch produced bars. In addition, quality improvements, such a lighter color
and greater perfume stability is obtained by this continuous process.
An improved composition and process for manufacture of transparent soap is described which is more
efficient and economical than any heretofore obtainable. Specifically the present disclosure describes a
continuous process for the saponification of a mild transparent soap which is quicker, more easily
50 controlled, conserves energy and produces a more uniform product with lighter color and superior fragrance
stability than heretofore obtainable.
More particularly, the present invention involves the delivery of one or more streams of stoichiometrical-
ly balanced ingredients into a heated mixing apparatus, stirring the blended ingredients for a period of time,
and thereafter withdrawing the contents therefrom, placing the mixture into molds which are quickly chilled
55 to complete the bar which is ten available for packaging. In this manner, the present invention substantially
obviates all of the problems which haunted previous efforts to continuously produce transparent soap.

3
EP 0 294 010 B1

An embodiment of the present invention provides a process for continuously saponifying a transparent
soap mixture and continuously producing transparent soap bars therefrom comprising: (a) introducing a first
blend of soap-making reagents containing cocofatty acid, stearic acid, and cocoDEA but no NaOH 50% into
a first storage tank; (b) introducing a second blend of soap-making reagents containing NaOH 50% but not
5 cocofatty acid, stearic acid, or cocoDEA into a second storage tank; (c) independently pumping said first
blend from said first storage tank and said second blend from said second storage tank continuously into a
first heated mixing tank, each being pumped at a rate predetermined to create a stoichiometrically balanced
mixture between said first blend and said second blend in said first heated mixing tank to initiate the
saponification of said mixture therewithin; (d) continuously transferring said stoichiometrically balanced
io mixture from said first heated mixing tank into a second heated mixing tank while stirring at a rate to
complete the saponification thereof in said heated second mixing tank; (e) continuously pumping said
completely saponified mixture from said second heated mixing tank into bar molds to fill said molds; (f)
introducing said filled molds into a chilled environment to quickly cool and solidify said mixture into
solidified bars without impairing the transparency thereof; (g) removing the chilled molds containing the
is solidified bars from said chilled environment; (h) separating the solidified bars from the chilled molds; (i)
recycling said molds to a point downstream of said second mixing tank for refilling; and (j) packaging said
bars.
Another embodiment of the invention is as recited in claim 2.
In a further aspect the invention provides an apparatus for the continuous production of transparent
20 soap bars, comprising storage means for separately storing first and second blends of soap making
reagents, first feed means for independently feeding the first and second blends from said storage means
to a first heated mixing means and second feed means for feeding the mixture to a second heated mixing
means, stirring means for stirring the blends in the first and second mixing means characterised by
comprising withdrawal means for withdrawing the saponified mixture from the second mixing means and for
25 depositing the saponified mixture into bar molds, cooling means for rapidly cooling the saponified mixture to
produce solidified soap bars, and packaging means for packaging the soap bars.
Accordingly, it is a prime object of the present invention to provide new and useful processes which
enable transparent soap to be produced continuously.
A further object of the present invention is to provide a novel process for the continuous and
30 controllable production of transparent soap bars which equals or exceeds the quality of bars produced by
similar bath processes.
Still another object of the present invention is to provide a novel process for the continuous production
of transparent soap bars which provide substantial improvement in unit costs, enhances the volume of
production and sacrifices neither clarity nor purity in the resulting bar.
35 A still further object of the present invention is to provide a new and improved process for producing
transparent soap which provides a bar soap which fully equals the clarity, quality, mildness, purity and
beauty heretofore obtainable only by batch processing.
A further object of the present invention is to provide a new and improved process for producing
transparent soap bars which eliminates the need for cooling frames, extruders and cutters by utilizing direct
40 molding and rapid cooling (-20° C to 6° C) in its continuous production system.
These and still further objects as shall hereinafter appear are fulfilled by the process of the present
invention in a remarkably unexpected fashion as will be readily discerned from a careful consideration of
the following detailed description of exemplary embodiments thereof, especially when read in conjunction
with the accompanying drawing in which like parts bear like numerals throughout the several views.
45 In the drawing:
FIG 1 is a flow diagram of a soap process embodying the present invention.
In the practice of the present invention, the novel composition hereof contains triethanolamine (TEA),
sodium hydroxide, distilled water, oleic acid, stearic acid, glycerine, ricinoleic acid, coco fatty acids, tallow
fatty acids and other minor ingredients such as fragrance, antioxidants, chelating agents, foam stabilizers,
50 colors, germicides, etc.
More particularly, the composition hereof contains the following ingredients in the following ranges
(expressed in weight percent):

55

4
EP 0 294 010 B1

RANGES
Minimum Optimum Maximum
W/W% W/W% W/W%
TEA 27.0 32.5 38.0
NaOH (50%) 7.0 8.2 9.4
Dl-Water 1.0 2.4 7.0
Oleic Acid 0.0 3.4 6.0
Stearic Acid 6.0 17.5 20.5
Cocodiethanolamide (CDEA) 0.0 1.5 4.0
Glycerine 0.0 11.0 25.0
Antioxidant 0.0 .1 .5
Fragrance 0.0 1.0 3.0
Ricinoleic Acid 1.0 4.8 6.0
Coco Fatty Acid 3.0 6.3 20.2
Tallow Fatty Acid 8.0 11.0 14.0
Laneth-10-Acetate 0.0 2.0 4.0
Nonoxylnol-14/PEG-4-Octanoate 0.0 1.0 2.0
Triethanolamine Lauryl Sulfate 0.0 8.0 10.0
Acetylated Lanolin Alcohol 0.0 2.0 4.0
Witch Hazel 0.0 1.0 3.0
Lauroyl Sarcosine 0.0 1.0 2.5
Citric Acid 0.0 1.0 2.0
Gluconic Acid 0.0 0.2 1.5
Sodium Metabisulfite 0.0 0.5 1.5
4-Chloro-2-(2,4 Dichloro-Phenoxy)phenol (lrgasan-300) 0.0 0.5 2.0

In addition to the above-listed ingredients, or as alternatives therefor depending on the availability of the
30 reagents and/or the secondary characteristics desired, the following ingredients represent materials which
may be incorporated into the blend without diminishing any of the primary characteristics required. Thus,
satisfactory results are obtained with the addition of an antioxidant such as tocopherol, tocopherol acetate,
BHA, BHT, citric acid, sodium meta-bisulfite, succinic acid and the like; a chelating agent such as EDTA,
DTPA and similar agents; commercial grades of triethanolamine (TEA), such as 85% TEA which can contain
35 both the corresponding secondary and primary amines as impurities; surfactants and/or foam boosters
selected from a wide group of anionic, amphoteric, nonionic, and certain cationic surfactants as exemplified
by (but not limited to) oleyl betaine, cocamidopropyl betaine, lauramide, C12-C18 olefin sulfonate, sodium
lauryl sulfate, sodium laureth sulfate, cetyltrimethyl ammonium chloride, sodium cocoyl isethionate, Tween
20-80, and the like; fatty acids such as hydrogenated tallow, isostearic acid, lauric acid, palmitic acid, neo-
40 decanoic acid, lanolin fatty acids, palm kernel fatty acids, palm oil fatty acids and the like; solvents such as
diethanolamine, propylene glycol, hexylene, quadrol and the like; and miscellaneous additives such as
polyethylene glycol, lanolin, PEG-20, hydrolyzed animal proteins, sorbitol and the like. It has also been
found, when the exigencies of production require, that potassium hydroxide can be used as a suitable
substitute for sodium hydroxide in the neutralization process.
45 The formulation as described above has the unexpected propensity, when introduced into and
processed through the equipment shown in the flow diagram of FIG 1, for substantially instant saponifica-
tion, as will hereinafter appear, and produces a light colored soap having superior fragrance stability to that
obtained by the batch process while achieving at least equivalent physical properties such as hardness,
foaming, solubility and clarity.
50 Referring to FIG 1, one practice of the present invention comprises dividing the aforesaid composition
into a first and second blend of ingredients, one disposed in each of a first and second discrete tank 11,12.
Each blend is thereafter pumped from tanks 11,12 by speed controlled pumps 13,14, respectively, into a
mixing tank 15 surrounded by water jacket 16. Thereafter, the mixture of the first and second blends, whose
relationship has been carefully controlled by individually regulating the speed of feed pumps 13,14 to create
55 a stoichiometric balance thereof in mixing tank 15, is pumped by a third speed controlled pump 18 into a
second mixing tank 19 which is also surrounded by water jacket 20. Additional specialized ingredients can

5
EP 0 294 010 B1

be added to the formulation at this point of the process. In tank 19, the mixture receives additional mixing
and is thereafter discharged through outlet 21 into suitable molds 22 for further handling as will be
hereinafter described in detail.
A suitable water heater 23 is disposed adjacent water jacket 16 and supplies jacket 16 with inlet water
5 heated to about 90 °C. This water from jacket 16 is fed to jacket 20 via suitable piping 24 and the water
from jacket 20 is withdrawn therefrom via suitable piping 25 through which it may be directed to a drain (not
shown) or returned to the reservoir 26 of heater 23, whatever the exigencies of a particular installation may
require.
Regardless of the blend, the soap bars produced hereby are formed by discharging the warmed (60 °C-
io 85° C) soap mixture into the bar molds which are thereafter processed in identical fashion which will now be
described.
The filled molds 22 are preferably disposed upon a suitable conveyor system 28 which transports the
molds 22 into a chiller 29 having a cooling medium of from about -30° to about 6°C provided by
refrigeration. The filled molds 22 are maintained in the cooling environment at this temperature for a period
is of from 5-45 minutes whereupon a transparent bar of acceptable hardness (circa 120 + 40), free of crystals
and without discoloration is produced. (See: Examples XII and XIII, infra.) The hardness, as reported herein,
is measured using a penetrometer (Penetrometer, Precision Scientific, Chicago, IL). It is measured as the
depth in millimeters a needle with a 50 gram weight will penetrate the bar in a given time. The greater the
penetration, the softer the soap bar. The finished bars are then removed from the molds and packaged in
20 the usual way and are ready for market.
To further aid in the understanding of the present invention, and not by way of limitation, the following
examples are presented.

EXAMPLE I
25
Transparent soap bars were prepared in accordance with the dual tank procedure of the present
invention. The first tank was filled with Blend A and the second tank was filled with Blend B, both shown
below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in stoichiometric
amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs during
30 agitation.

BLEND A
Triethanolamine (TEA) 4.2%
Ricinoleic Acid 4.8
Coco Fatty Acid 6.3
Tallow Fatty Acid 11.0
Oleic Acid 3.4
Stearic Acid 17.5
CDEA 1.8
dl-a-Tocopherol 0.10
Fragrance 1.0
Total 50.0
45

BLEND B
TEA 28.4
NaOH 50% 8.2
Dl-Water 2.4
Glycerine 11.0
Total 50.0
55
Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
in accordance with Example XII.

6
EP 0 294 010 B1

EXAMPLE II

Transparent soap bars were prepared in accordance with the dual tank procedure of the present
invention. The first tank was filled with Blend C and the second tank was filled with Blend D, both as
5 reported below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in
stoichiometric amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs
during agitation.

BLEND C
Ricinoleic Acid 4.7%
Coco Fatty Acid 6.3
Tallow Fatty Acid 11.0
Oleic Acid 3.4
Stearic Acid 17.5
CDEA 1.8
dl-a-Tocopherol 0.5
Total 45.2

BLEND D
TEA 32.5
NaOH 50% 8.2
Dl-Water 3.1
Glycerine 11.0
Total 54.8
30
Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
in accordance with Example XII.

EXAMPLE III
35
Transparent soap bars were prepared in accordance with the dual tank procedure of the present
invention. The first tank was filled with Blend E and the second tank was filled with Blend F, both as
reported below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in
stoichiometric amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs
40 during agitation.

BLEND E
Ricinoleic Acid 4.8%
Coco Fatty Acid 6.3
Tallow Fatty Acid 11.0
Oleic Acid 3.4
Stearic Acid 17.5
CDEA 1.8
Glycerine 11.0
dl-a-Tocopherol 0.05
Total 55.9

55

7
EP 0 294 010 B1

BLEND F
TEA 32.5
NaOH 50% 8.2
Dl-Water 3.4
Total 44.1

Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
io in accordance with Example XII.

EXAMPLE IV

Transparent soap bars were prepared in accordance with the dual tank procedure of the present
is invention. The first tank was filled with Blend G and the second tank was filled with Blend H, both as
reported below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in
stoichiometric amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs
during agitation.

20
BLEND G
Triethanolamine (TEA) 33.3%
Ricinoleic Acid 4.8
Coco Fatty Acid 6.3
25 Tallow Fatty Acid 11.0
Oleic Acid 3.4
Stearic Acid 17.5
dl-a-Tocopherol .1
Dl-Water 3.4
30 Glycerine 12.0
Total 91 .8

BLEND H
NaOH 50% 8.2

Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
in accordance with Example XII.

EXAMPLE V

Transparent soap bars were prepared in accordance with the dual tank procedure of the present
invention. The first tank was filled with Blend I and the second tank was filled with Blend J, both as reported
below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in stoichiometric
amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs during
agitation.

55

8
EP 0 294 010 B1

BLEND I
Triethanolamine (TEA) 32.5%
Ricinoleic Acid 4.8
Coco Fatty Acid 6.3
Tallow Fatty Acid 11.0
Oleic Acid 3.4
Stearic Acid 17.5
Laurie Diethanolamide 1.0
Glycerine 11.8
dl-a-Tocopherol 0.1
Total 88.4

BLEND J
NaOH 50% 8.2
Dl-Water 3.4
Total 11.6

Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
in accordance with Example XII.
25
EXAMPLE VI

Transparent soap bars were prepared in accordance with the dual tank procedure of the present
invention. The first tank was filled with Blend K and the second tank was filled with Blend L, both as
30 reported below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in
stoichiometric amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs
during agitation.

BLEND K
Triethanolamine (TEA) 34.3%
Ricinoleic Acid 4.8
Coco Fatty Acid 6.3
Tallow Fatty Acid 11.0
Oleic Acid 3.4
Stearic Acid 17.5
dl-a-Tocopherol .1
Total 77.4

BLEND L
NaOH 50% 8.2
Dl-Water 3.4
Glycerine 11.0
Total 22.6

55 Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
in accordance with Example XII.

9
EP 0 294 010 B1

EXAMPLE VII

Transparent soap bars were prepared in accordance with the dual tank procedure of the present
invention. The first tank was filled with Blend M and the second tank was filled with Blend N, both as
5 reported below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in
stoichiometric amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs
during agitation.

BLEND M
Ricinoleic Acid 4.8%
Coco Fatty Acid 6.3
Tallow Fatty Acid 11.0
Oleic Acid 3.4
Stearic Acid 17.5
CDEA 3.6
dl-a-Tocopherol .1
Total 46.7

BLEND N
TEA 31 .7
NaOH 50% 8.2
Dl-Water 3.4
Glycerine 10.0
Total 53.3
30
Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
in accordance with Example XII.

EXAMPLE VIII
35
Transparent soap bars were prepared in accordance with the dual tank procedure of the present
invention. The first tank was filled with Blend O and the second tank was filled with Blend P, both as
reported below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in
stoichiometric amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs
40 during agitation.

BLEND O
Triethanolamine (TEA) 4.1%
Ricinoleic Acid 4.8
Coco Fatty Acid 6.3
Tallow Fatty Acid 11.0
Oleic Acid 3.4
Stearic Acid 17.5
CDEA 1.8
dl-a-Tocopherol .1
Total 49.0

55

10
EP 0 294 010 B1

BLEND P
TEA 28.4%
NaOH 50% 8.2
Glycerine 11.0
Dl-Water 3.4
Total 51 .0

10 Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
in accordance with Example XII.

EXAMPLE IX

is Transparent soap bars were prepared in accordance with the dual tank procedure of the present
invention. The first tank was filled with Blend Q and the second tank was filled with Blend R, both as
reported below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in
stoichiometric amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs
during agitation.
20
BLEND Q
Ricinoleic Acid 4.8%
Coco Fatty Acid 6.3
Tallow Fatty Acid 11.0
Oleic Acid 3.4
Stearic Acid 17.5
CDEA 1.8
Glycerine 11.0
dl-a-Tocopherol .1
Total 55.9

BLEND R
TEA 32.5
NaOH 50% 8.2
Dl-Water 3.4
40
Total 44.1

Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
in accordance with Example XII.
45
EXAMPLE X

Transparent soap bars were prepared in accordance with the dual tank procedure of the present
invention. The first tank was filled with Blend S and the second tank was filled with Blend T, both as
50 reported below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in
stoichiometric amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs
during agitation.

55

11
EP 0 294 010 B1

BLEND S
Triethanolamine (TEA) 30.2%
Coco Fatty Acid 20.2
Stearic Acid 20.2
Glycerine 12.1
Dl-Water 7.0
Citric Acid 0.5
Gluconic Acid 0.2
Sodium Metabisulfite 0.5
Total 90.9

BLEND T
NaOH 50% 9.1%
Total 9.1

Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
in accordance with Example XII.

EXAMPLE XI

Transparent soap bars were prepared in accordance with the dual tank procedure of the present
invention. The first tank was filled with Blend U and the second tank was filled with Blend V, both as
reported below. Each tank was preheated to 70-80 ° C and the contents were pumped therefrom in
stoichiometric amounts into a mixing vessel surrounded by a hot water jacket wherein saponification occurs
during agitation.

BLEND U
Coco Fatty Acid 20.2%
Stearic Acid 20.2
Citric Acid .5
Gluconic Acid .2
Sodium Metabisulfite .5
Total 41 .6

BLEND V
NaOH 50% 9.1
Dl-Water 7.0%
Glycerine 12.1
Triethanolamine (TEA) 30.2
Total 58.4
50
Thereafter the final mixture is withdrawn from the mixing tank into appropriate molds which are chilled
in accordance with Example XII.

55

12
EP 0 294 010 B1

EXAMPLE XII

One hundred grams of the hot soap mixture prepared according to the procedure described in Example
I, was poured at 85 °C into plastic soap molds and subjected to rapid cooling in a variety of controllable
5 media. The internal temperature of the bars was monitored until it reached 25 ° C at which time the bar was
removed from the cooling medium and tested for color, clarity, stability and hardness.
The results are shown in Table A below. Surprisingly, there was no adverse effect on any of the
properties of the resultant bars with the exception of hardness at very low temperature <-50 ° C. Color,
clarity, stability and chemical properties all compared favorably with the conventionally prepared transparent
io soap bars.

TABLE A
Hardness
75 Cooling Medium T°C (min) (mm)

Dry ice/Alcohol -50 15 275


Freezer -20 27 194

Refrigerator 5 35 149
20
Ambient 25 120 132

Cooling Medium Color Clarity

Dry ice/Alcohol 43.4 OK


25 42.2 OK
Freezer
Refrigerator 41.6 OK
Ambient 40.4 OK
30
Color is recorded as the "L" lightness value, as measured by a Macbeth Colorimeter, Model 1500,
Macbeth, Inc., New York, NY.

EXAMPLE XIII

In further cooling experiments, a PVC soap mold (8.0cm x 5.0cm x 2.5 cm) containing 100g of molten
soap (80 °C) from Example I, was drawn through a cooling tunnel (2.5908 m (8.5 ft) in length and 0.1397 m
(5.5 inch) diameter) with an average temperature of 0 to 4° C. In these experiments, the molds were drawn
through the cooling tunnel at various rates, and the physical properties determined as in Example XII.

TABLE B-1

Time Bar Temp. (°C) Initial Hardness (mm) Final Hardness (mm)
5 min 53.3 -- 134
7 min 47.2 -- 154
9 min 42.6 -- 122
11 min 39.2 -- 126
13 min 36.1 820 138
15 min 33.1 420 142
17 min 30.4 338 130
19 min 28.4 272 132
12 Hrs. (Control) 22.4 126 130

13
EP 0 294 010 B1

TABLE B-2

Time Color Clarity Stability


5 min 44.2 OK OK
7 min 44.6 OK OK
9 min 44.5 OK OK
11 min 44.7 OK OK
13 min 43.9 OK OK
15 min 44.2 OK OK
17 min 44.2 OK OK
19 min 44.1 OK OK
12 Hrs. (Control) 43.8 OK OK

In this experiment, it was found that after 15 to 17 minutes of cooling, the resultant bar was sufficiently
solidified to allow handling and initial hardness measurements. In addition, the hardness of these bars was
again determined after 12 hours at room temperature (Final Hardness). No significant difference was found
between the final hardness of the rapidly cooled bars, and that of the control bars which were cooled at
room temperature in a metal frame for 12 hours (720 min). No significant changes in color, clarity, stability,
or texture were found in the rapidly cooled bars.

EXAMPLE XIV

In a further series of experiments, the basic formula shown in Example I was made 3 times
(Experiments 4, 5 and 6) using the continuous process, and compared to 3 batches (Experiments 1, 2 and
3) made using the same formula (Example I) but prepared using a batch process. In the batch process, the
triethanolamine (50% of the total TEA), ricinoleic acid, coco fatty acid, and tallow fatty acids are mixed with
the caustic soda and heated at 90-96 °C for 30 minutes. After the 30 minute heating, additional
triethanolamine is added and the batch cooled to 85 °C, followed by the addition of oleic acid, stearic acid,
30
cocodiethanolamine (CDEA) and glycerine. After the addition of these ingredients, other minor ingredients
such as antioxidants, fragrances etc, are added. The soap is then poured into frames or molds and allowed
to cool. The resultant soaps were compared for color, appearance, hardness, pH, foaming and stability.

TABLE C
35

Experiment Process Color Hardness(mm) pH Foam Stability


1 Batch 35.97 138 9.0 295 OK
2 Batch 36.55 148 9.0 300 OK
40
3 Batch 35.90 124 8.9 295 OK
4 Continuous 43.10 130 8.9 300 OK
5 Continuous 42.70 138 9.0 295 OK
6 Continuous 43.30 120 8.9 300 OK
45
Foam Test results are listed as ml of foam produced, by shaking 50 ml of a 1.0% soap solution with
199 ml of tap water (120 ppm of hardness) and 1.0 ml olive oil in a stoppered volumetric flask. The mixture
is inverted 10 times in 25 seconds, and the foam height produced, is measured.

50 EXAMPLES XV - XXIX

The two-phase procedure of Example I was repeated using the apparatus of FIG. 1 and the blends
reported in Table B below. In every case, transparent soap bars having the improved characteristics of the
present invention were produced.
55

14
EP 0 294 010 B1

TABLE B-l

EXAMPLES XV XVI XVII XVI I I

INGREDIENTS
PHASE I

Tr i e t h a n o l a m i n e 33.5 33.8 27 38
Caustic Soda 50% 8.4 8.5 8.4 8.4
Wa t e r 4.1 4.1 4.1 4.1

Glycerine 10.2 10.4 17 5

PHASE II
Ricinoleic Acid 4, 4.8 4.8 4,
Coco Fatty Acid 5. 6 5.9 5.
Ta 1 1 ow Fa 1 1 y Ac i d 11 , 11.3 11 11 ,
Oleic Acid 3. 0 3.5 3,
Stearic Acid 17, 18.1 17.1 17,
CDEA 0 1.9 1 0,
Ant i o x i d a n t 0 0.5 0.2 0

Fragrance 0.6

TOTAL 100 100 100 100

TABLE B-2
EXAMPLES XIX XX XXI XXII
INGREDIENTS
PHASE I
Triethanolamine 33.6 37 30.6 30
Caustic Soda 50% 8.2 9.4 7.4 8.2
Water 1 5 3 2

Glycerine 15 0 11 25

15
EP 0 294 010 B1

PHASE II
Ricinoleic Acid 3.5 6 6 4
5 Coco Fatty Acid 3 8.6 7 4
Tallow Fatty Acid 11 9 8 14
Oleic Ac id 3.4 5 6 4
70 Stearic Acid 19 16. 7 20. 5 6
CDEA 1.8 1.8 0 2
Antioxidant 0.5 0.5 0.5 0
Fragrance
75

TOTAL 100 100 100 100

20
TABLE B-3

EXAMPLES XXIII XXIV XXV XXVI


INGREDIENTS
PHASE 1
Triethanolamine 32.5 30.2 30.2 30.5
Caustic Soda 50% 8.2 9.1 9.1 8.1
Water 2 6.8 7 3.5
Glycerine 11 12.1 12.1 9.4

TABLE B-3
35

EXAMPLES XXIII XXIV XXV XXVI


PHASE II
Ricinoleic Acid 4.7 0 0 4.6
Coco Fatty Acid 6.3 20.2 20.2 5.6
Tallow Fatty Acid 11 - - 10.5
Oleic Acid 3 - - 3.3
Stearic Acid 16.8 18.9 18.9 16.5
CDEA 4 - - 1.5
Citric Acid 1 1
Gluconic Acid 0.2 1
Sodium Metabisulfite 1.5 0.5
Laneth-10-Acetate 4
Nonoxynol-14/PEG-4-Octanoate 2
Antioxidant 0.5 0.5
Fragrance
TOTAL 100 100 100 100

16
EP 0 294 010 B1

TABLE B-4

EXAMPLES XXVII XXVIII XXIX


INGREDIENTS
PHASE I
Triethanolamine 28.5 30.5 32
Caustic Soda 50% 7.7 8.1 8.2
Water 3.1 3.5 3
Glycerine 8 9.5 10

TABLE B-4
75

EXAMPLES XXVII XXVIII XXIX


PHASE II
Ricinoleic Acid 4.4 4.6 4.6
Coco Fatty Acid 5.4 5.6 6.1
Tallow Fatty Acid 9.2 10.5 10.5
Oleic Acid 3 3.3 3.3
Stearic Acid 14.7 16.5 17.5
CDEA 1.5 1.5 1.5
Citric Acid
Gluconic Acid
Sodium Metabisulfite
Laneth-10-Acetate
Nonoxynol-1 4/PEG-4-Octanoate
TEA-Lauryl Sulfate 10
Acetylated Lanolin Alcohol 4
Witch Hazel 3
Lauroyl Sarcosine 2.5
Antioxidant 0.5 0.5 0.3
Fragrance 0.4 3
TOTAL 100 100 100

From the foregoing, it is apparent that there are several important features associated with the practice
of the present invention. Thus a process is herein described and illustrated which obtains the production of
transparent soap on a continuous basis which soap has improved color, improved fragrance, stability and
more uniform quality than was heretofor obtainable by existing batch procedures.
In addition to the foregoing, the process of the present invention provides significant economic
advantages in reduced processing time and lower labor costs while the composition/ process interaction
enables rapid cooling from 80 ° C to 30 ° C without affecting the basic characteristics of such soap, namely,
hardness, solubility, clarity and foaming.
All compositions are expressed in weight percent.

Claims
50
1. A process for continuously saponifying a transparent soap mixture and continuously producing
transparent soap bars therefrom comprising: (a) introducing a first blend of soap-making reagents
containing cocofatty acid, stearic acid, and cocoDEA (cocodiethanolamide) but no NaOH 50% into a
first storage tank; (b) introducing a second blend of soap-making reagents containing NaOH 50% but
no cocofatty acid, stearic acid, or cocoDEA into a second storage tank; (c) independently pumping said
first blend from said first storage tank and said second blend from said second storage tank
continuously into a first heated mixing tank, each being pumped at a rate predetermined to create a
stoichiometrically balanced mixture between said first blend and said second blend in said first heated

17
EP 0 294 010 B1

mixing tank to initiate the saponification of said mixture therewithin; (d) continuously transferring said
stoichiometrically balanced mixture from said first heated mixing tank into a second heated mixing tank
while stirring at a rate to complete the saponification thereof in said second heated mixing tank; (e)
continuously pumping said completely saponified mixture from said second heated mixing tank into bar
5 molds to fill said molds; (f) introducing said filled molds into a chilled environment to quickly cool and
solidify said mixture into solidified bars without impairing the transparency thereof; (g) removing the
chilled molds containing the solidified bars from said chilled environment; (h) separating the solidified
bars from the chilled molds; (i) recycling said molds to a point downstream of said second mixing tank
for refilling; and (j) packaging said bars.
10
2. A continuous process for producing a transparent soap containing (in weight percent): from 27.0 to
38.0, TEA (triethanolamine); from 7.0 to 9.4, NaOH; from 1.0 to 7.0, Dl-Water (eionized water); from 6.0
to 20.5, stearic acid; from 5.0 to 25.0, glycerine; and from 4.0 to 20.2, coco fatty acid, said process
comprising dividing said ingredients into at least two separate blends in which one contains the NaOH
is and another contains the stearic acid and the coco fatty acid and the remaining ingredients are
disposed in either blend; introducing a first blend into a first tank and a second blend into a second
tank; and then applying the sequence of steps (c) to (j) according to Claim 1.

3. A process for producing transparent soap bars on a continuous basis comprising intermixing two or
20 more streams of preselected stoichiometrically balanced ingredients for reaction in a heated mixing
apparatus, stirring the intermixed ingredients for a time sufficient to effect saponification therebetween
and create a homogeneous blend therefrom; withdrawing said homogeneous blend from the mixing
apparatus and depositing it into bar molds; quickly chilling the bar molds to solidify said homogeneous
blend into bars; removing the bars from the molds; and packaging the bars.
25
4. A continuous process according to Claim 3, characterised in that said balanced ingredients include
triethanolamine, sodium hydroxide, distilled water, oleic acid, stearic acid, glycerine, ricinoleic acid,
coco fatty acids, and tallow fatty acid.

30 5. A continuous process according to any one of the preceding claims, characterised in that either said
first blend or said second blend or said balanced ingredients contain additionally one or more
ingredients selected from the group consisting of: fragrances, antioxidants, chelating agents, foam
stabilizers, colors and germicides.

35 6. A continuous process according to any preceding claim, characterised in that said chilled environment
is controlled at a temperature from about -30 ° C up to about + 30 ° C.

7. A continuous process according to any preceding claim, characterised in that said mixture is cooled
from 85 ° C to 25 ° C in about twenty minutes.
40
8. A continuous process according to any of Claims 1 to 7, characterised in that the contents of the bar
molds are chilled to an internal bar temperature of 25° C in twenty minutes.

9. Apparatus for the continuous production of transparent soap bars, comprising storage means (11,12) for
45 separately storing first and second blends of soap making reagents, first feed means (13,14) for
independently feeding the first and second blends from said storage means (11,12) to a first heated
mixing means (15) and second feed means (18) for feeding the mixture to a second heated mixing
means (19), stirring means for stirring the blends in the first and second mixing means (15,19)
characterised by comprising withdrawal means (21) for withdrawing the saponified mixture from the
50 second mixing means (19) and for depositing the saponified mixture into bar molds (22), cooling means
(29) for rapidly cooling the saponified mixture to produce solidified soap bars, and packaging means for
packaging the soap bars.

Revendicatlons
55
1. Procede pour la saponification en continu d'un melange pour savons transparents et la production en
continu de pains de savons transparents qui en resultent, comprenant

18
EP 0 294 010 B1

a) I'introduction, dans un premier reservoir de stockage, d'un premier melange de reactifs de


saponification contenant de I'acide gras de coco, de I'acide stearique et du diethanolamide de coco
(DEA coco) a I'exclusion de NaOH (50 %) ;
b) I'introduction, dans un second reservoir de stockage, d'un second melange de reactifs de
5 saponification contenant de la NaOH (50 %) a I'exclusion d'acide gras de coco, d'acide stearique ou
de DEA coco ;
c) le pompage independant en continu dudit premier melange issu dudit premier reservoir de
stockage, et dudit second melange issu dudit second reservoir de stockage, dans une premiere
cuve melangeuse chauffee, chaque melange etant pompe a un debit predetermine pour constituer
io un melange equilibre stoechiometriquement entre ledit premier melange et ledit second melange,
dans ladite premiere cuve melangeuse chauffee, pour y initier entre eux la saponification dudit
melange ;
d) le transfert en continu dudit melange equilibre stoechiometriquement, de ladite premiere cuve
melangeuse chauffee vers une seconde cuve melangeuse chauffee tandis que Ton agite de fagon a
is terminer la saponification desdits reactifs dans ladite seconde cuve melangeuse chauffee ;
e) I'introduction desdits moules remplis dans une zone refroidie pour assurer un refroidissement et
une solidification rapide dudit melange, sous forme de pains solidifies sans alterer leur transparence

g) I'enlevement des moules refroidis contenant les pains solidifies de ladite zone de refroidissement
20 ;
h) la separation des pains solidifies des moules refroidis ;
i) le recyclage desdits moules en un point situe en aval de ladite seconde cuve melangeuse pour un
nouveau remplissage ; et
j) le conditionnement desdits pains.
25
2. Procede en continu pour la production de savon transparent contenant (en pourcentage ponderal) : de
27,0 a 38,0 de triethanolamine (TEA) ; de 7,0 a 9,4 de NaOH ; de 1,0 a 7,0 d'eau desionisee (eau Dl) ;
de 6,0 a 20,5 d'acide stearique ; de 5,0 a 25,0 de glycerine ; et de 4,0 a 20,2 d'acide gras de coco,
ledit procede comprenant la division desdits ingredients en au moins deux melanges separes dans
30 lesquels I'un contient la NaOH et un autre contient I'acide stearique et I'acide gras de coco, le reste
des ingredients etant contenu dans I'un ou I'autre des melanges ; I'introduction d'un premier melange
dans une premiere cuve melangeuse ; et la mise en oeuvre de la sequence de phases operatoires c) a
j) de la revendication 1.

35 3. Procede de production de pains de savons transparents sur une base continue, comprenant le melange
entre eux de deux flux ou plus d'ingredients equilibres stoechiometriquement pour la reaction dans un
appareillage melangeur chauffe, I'agitation desdits ingredients melanges entre eux pendant une duree
suffisante pour effectuer la saponification entre eux et creer un melange resultant homogene, I'extrac-
tion dudit melange homogene dudit appareillage melangeur et son depot dans des moules a pains ; le
40 refroidissement rapide des moules a pains pour solidifier ledit melange homogene sous forme de pains
; I'enlevement des pains des moules ; et le conditionnement des pains.

4. Procede en continu selon la revendication 3, caracterise en ce que lesdits ingredients equilibres


comprennent de la diethanolamine, de I'hydroxyde de sodium, de I'eau distillee, de I'acide olei'que, de
45 I'acide stearique, de la glycerine, de I'acide ricinolei'que, des acides gras de coco et de I'acide gras de
suif.

5. Procede en continu selon I'une quelconque des revendications precedentes, caracterise en ce que
dans I'un ou I'autre dudit premier melange et dudit second melange ou dans lesdits ingredients
50 equilibres contiennent de plus un ou plusieurs ingredients choisis dans le groupe consistant en :
parfums, antioxydants, agents de chelation, stabilisants de mousse, colorants et germicides.

6. Procede en continu selon I'une quelconque des revendications precedentes, caracterise en ce que
ladite zone refroidie est commandee a une temperature d'environ -30° C a environ +30°C.
55
7. Procede en continu selon I'une quelconque des revendications precedentes, caracterise en ce que ledit
melange est refroidi de 85° C a 25° C en environ vingt minutes.

19
EP 0 294 010 B1

8. Procede en continu selon I'une quelconque des revendications 1 a 7 caracterise en ce que les
contenus des moules a pains sont refroidis jusqu'a une temperature interne des pains de 25 °C en
vingt minutes.

5 9. Appareillage pour la production en continu de pains de savons transparents, comprenant des moyens
de stockage (11,12) pour stacker separement premier melange et second melange de reactifs de
saponification, des premiers moyens d'alimentation (13,14) pour alimenter independamment en premier
melange et en second melange issus desdits moyens de stockage (11,12) des premiers moyens
melangeurs chauffes (15) et des seconds moyens d'alimentation (18) pour alimenter en melange des
io seconds moyens melangeurs chauffes (19), des moyens d'agitation pour agiter les melanges dans
lesdits premiers moyens melangeurs et lesdits seconds moyens melangeurs (15,19), caracterise en ce
qu'il comprend des moyens (21) d'extraction pour extraire le melange saponifie des seconds moyens
melangeurs (19) et pour deposer le melange saponifie dans les moules a pains (22), des moyens de
refroidissement (29) pour refroidir rapidement le melange saponifie pour produire des pains de savons
is solidifies, et des moyens de conditionnement pour conditionner les pains de savons.

Patentanspruche

1. Verfahren zum kontinuierlichen Verseifen eines durchsichtigen Seifegemischs und zum kontinuierlichen
20 Herstellen durchsichtiger Seiferiegel aus diesem, durch:
(a) Einfullen einer ersten Mischung aus Reagentien zur Seifeherstellung, enthaltend Kokosnu/Sfett-
saure, Stearinsaure und Kokosnu/S-DEA (Kokosnu/Sdiethanolamid), jedoch keine 50%ige NaOH, in
einen ersten Lagertank;
(b) Einfullen einer zweiten Mischung aus Reagentien zur Seifeherstellung, enthaltend 50%ige NaOH,
25 jedoch keine Kokosnu/Sfettsaure, Stearinsaure oder Kokosnu/S-DEA, in einen zweiten Lagertank;
(c) kontinuierliches und voneinander unabhangig durchgefuhrtes Pumpen der ersten Mischung aus
dem ersten Lagertank und der zweiten Mischung aus dem zweiten Lagertank in einen ersten
beheizten Mischtank, wobei jeder Pumpvorgang mit einer gegebenen Geschwindigkeit durchgefuhrt
wird, urn ein stochiometrisch ausgeglichenes Gemisch zwischen erster Mischung und zweiter
30 Mischung in dem ersten beheizten Mischtank zur Einleitung der Verseifung des darin befindlichen
Gemischs bereitzustellen;
(d) kontinuierliches Weiterleiten des stochiometrisch ausgeglichenen Gemischs aus dem ersten
beheizten Mischtank in einen zweiten beheizten Mischtank unter Ruhren mit einer solchen Ge-
schwindigkeit, da/S ihre Verseifung in dem zweiten beheizten Mischtank vervollstandigt wird;
35 (e) kontinuierliches Weiterpumpen des vollstandig verseiften Gemischs aus dem zweiten beheizten
Mischtank in Riegelformen zum Fullen dieser Formen;
(f) Einbringen der gefullten Formen in eine gekuhlte Umgebung zur raschen Abkuhlung und
Verfestigung des Gemischs zu festen Riegeln ohne Beeintrachtigung ihrer Transparenz;
(g) Entfernen der gekuhlten Formen mit den (darin befindlichen) verfestigten Riegeln aus der
40 gekuhlten Umgebung;
(h) Entformen der verfestigten Riegel aus den gekuhlten Formen;
(i) Ruckfuhren der Formen an einen Punkt stromabwarts des zweiten Mischtanks zum Wiederfullen
und
(j) Verpacken der Riegel.
45
2. Kontinuierliches Verfahren zur Herstellen einer durchsichtigen Seife mit (in Gew.-%) 27,0 - 38,0 TEA
(Triethanolamin), 7,0 - 9,4 NaOH, 1,0 - 7,0 Dl-Wasser (entionisiertes Wasser), 6,0 - 20,5 Stearinsaure,
5,0 - 25,0 Glycerin und 4,0 - 20,2 Kokosnu/Sfettsaure, umfassend eine Aufteilung der Bestandteile in
mindestens zwei getrennte Mischungen, von denen eine die NaOH und die andere die Stearinsaure
50 und die Kokosnu/Sfettsaure enthalt, wobei die restlichen Bestandteile in einer der Mischungen unterge-
bracht werden, die Einfuhrung einer ersten Mischung in einen ersten Tank und einer zweiten Mischung
in einen zweiten Tank und die anschlie/Sende Durchfuhrung der Stufenfolge (c) bis (j) gema/S Anspruch
1.

55 3. Verfahren zur Herstellung durchsichtiger Seiferiegel auf kontinuierlicher Basis durch Vermischen von
zwei oder mehreren Stromen von zuvor ausgewahlten, stochiometrisch ausgeglichenen Bestandteilen
zur Umsetzung in einer beheizten Mischvorrichtung, ausreichend langes Verruhren der vermischten
Bestandteile zur Herbeifuhrung einer Verseifung und Ausbildung einer homogenen Mischung dersel-

20
EP 0 294 010 B1

ben, Abziehen der homogenen Mischung aus der Mischvorrichtung und Ablagern derselben in Riegel-
formen, rasches Abschrecken der Riegelformen zur Verfestigung der homogenen Mischung zu Riegeln,
Entformen der Riegel aus den Formen und Verpacken der Riegel.

Kontinuierliches Verfahren nach Anspruch 3, dadurch gekennzeichnet, da/S die ausbalancierten Be-
standteile Triethanolamin, Natriumhydroxid, destilliertes Wasser, Olsaure, Stearinsaure, Glycerin, Rici-
nolsaure, Kokosnu/Sfettsauren und Talgfettsauren umfassen.

Kontinuierliches Verfahren nach einem der vorhergehenden Anspruche, dadurch gekennzeichnet, da/S
entweder die erste Mischung oder die zweite Mischung oder die ausbalancierten Bestandteile zusatz-
lich einen oder mehrere Bestandteil(e) aus der Gruppe Duftstoffe, Antioxidantien, Chelatbildner,
Schaumstabilisatoren, Farbstoffe und keimtotende Mittel enthalten.

Kontinuierliches Verfahren nach einem der vorhergehenden Anspruche, dadurch gekennzeichnet, da/S
die gekuhlte Umgebung auf einer Temperatur von etwa -30° C bis zu etwa +30° C gehalten wird.

Kontinuierliches Verfahren nach einem der vorhergehenden Anspruche, dadurch gekennzeichnet, da/S
das Gemisch in etwa 20 min von 85° C auf 25° C gekuhlt wird.

Kontinuierliches Verfahren nach einem der Anspruche 1 bis 7, dadurch gekennzeichnet, da/S der Inhalt
der Riegelformen auf eine Riegelinnentemperatur von 25 °C in 20 min gekuhlt wird.

Vorrichtung zur kontinuierlichen Herstellung von durchsichtigen Seiferiegeln, umfassend Lagereinrich-


tungen (11, 12) zur getrennten Lagerung erster und zweiter Mischungen von Reagentien zur Seifeher-
stellung, erste Zufuhreinrichtungen (13, 14) zum unabhangigen Weiterleiten der ersten und zweiten
Mischungen aus den Lagereinrichtungen (11, 12) zu einer ersten beheizten Mischeinrichtung (15) und
eine zweite Zufuhreinrichtung (18) zur Weiterleitung des Gemischs zu einer zweiten beheizten Misch-
einrichtung (19), Ruhreinrichtungen zum Ruhren der Mischungen in den ersten und zweiten Mischein-
richtungen (15, 19), gekennzeichnet durch eine Abzieheinrichtung (21) zum Abziehen des verseiften
Gemischs aus der zweiten Mischeinrichtung (19) und zum Einbringen des verseiften Gemischs in
Riegelformen (22), eine Kuhleinrichtung (29) zum raschen Abkuhlen des verseiften Gemischs zur
Herstellung verfestigter Seiferiegel und eine Verpackungseinrichtung zum Verpacken der Seiferiegel.

21
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