Preparation Process of Polylactic Acid

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Preparation process of polylactic acid-base thermoplastic wood-plastic

composite material

Abstract

The present invention relates to preparation process of polylactic acid-base thermoplastic wood-plastic
composite material, which is prepared with polylactic acid and wood powder as main materials, and
through reacting and mixing with compatibilizing agent, brightening agent, plasticizer, nucleater,
dispersant, stabilizer and other assistant in a high speed stirrer; extrusion pelletizing the mixture in a
double screw extruder; cooling and cutting; and drying in a vacuum drier to obtain the polylactic acid-base
thermoplastic wood-plastic composite material. The composite material of the presentinvention has
excellent comprehensive performance, is degradable, and may be used as packing material, environment
protecting material and decoration material.

  Patents

Preparation process of polylactic acid-base thermoplastic wood-plastic


composite material

Abstract

The present invention relates to preparation process of polylactic acid-base thermoplastic wood-plastic
composite material, which is prepared with polylactic acid and wood powder as main materials, and
through reacting and mixing with compatibilizing agent, brightening agent, plasticizer, nucleater,
dispersant, stabilizer and other assistant in a high speed stirrer; extrusion pelletizing the mixture in a
double screw extruder; cooling and cutting; and drying in a vacuum drier to obtain the polylactic acid-base
thermoplastic wood-plastic composite material. The composite material of the presentinvention has
excellent comprehensive performance, is degradable, and may be used as packing material, environment
protecting material and decoration material.

Classifications

 B29C48/40 Means for plasticising or homogenising the moulding material or forcing it through the nozzle
or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more
parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders

 B29C48/04 Particle-shaped

Hide more classifications


CN101020780B

Description

Preparation of polylactic acid-based thermoplastic WPC

FIELD

[0001] relates to a method for producing a polylactic acid-based thermoplastic WPC, the resulting
composite material according to the present invention

Used as packaging materials, environmentally friendly materials and decoration materials. The present
invention belongs to the field of polymer processing techniques. Background technique

[0002] synthetic polymer materials to bring convenience to people's lives at the same time, because most
of the materials derived from petroleum caused energy shortages, the other because most do not have
the biodegradable synthetic polymer properties, abandoned after causing serious Environmental
Pollution. The application of biodegradable polymer materials can fundamentally solve the problem of
environmental pollution, and therefore biodegradable polymer materials research in this area has become
active again. Wherein polylactic acid (PLA) having excellent biocompatibility and is completely
biodegradable aliphatic polyester-based polymer material, it is completely decomposed under the action
of microbial nature, water, acid, alkali etc. . The final product was 1120 and C02, environmental pollution,
can be used as environmentally friendly materials instead of conventional polymer materials. Not only
biodegradable polylactic acid, and the preparation of its starting material also be derived from renewable
resources environment, it may be made of corn starch to lactic acid fermentation to obtain a
polymerization, it is now possible mass production, but there are also expensive, more brittle material
shortcomings, thus limit its widespread use.

[0003] refers to wood waste wood flour, straw powder, shell powder, bamboo powder, flour or bran shell
powder, peanut shell nature of the crop, low prices, from nature, and then use attributable to
natural. Thermoplastic WPC using wood flour as the main material and thermoplastics, a new composite
material is prepared by mixing and processing. The development of the material and energy resources to
alleviate the shortage of oil resources and the growing demand for timber and forest products brought
about, it is an effective means to protect the environment and reduce energy consumption, and
thermoplastic plastic composite materials as well as durable, than wood good dimensional stability,
moldability, low water absorption, corrosion resistance, and recyclable characteristics, has become a hot
research field material. WPC currently used in the preparation of a thermoplastic mainly polyvinyl chloride
(PVC) (. CN200610034685 7), polyethylene (the PE) (Fang Zhengping et al., China Plastics, 1999, 13
(11), 44; GRAPHIC COMMUNICATION Wu Jun , Beijing Institute of Graphic Communication, 2006, 15
(5), 9;. CN99111051.X), polypropylene (PP) (CN02104432 5) and other types, wood flour and plastic
compatibility is only for these types of materials , usually applied fence, outdoor board, brackets, etc.,
although there are some applications, but limited variety, fewer species, limiting the development of
wood-plastic materials, it can not be widely used. If the use of composite wood meal and polylactic acid,
can not only reduce the cost of polylactic acid, polylactic acid can also improve the workability and
toughness, while having biodegradable properties can be obtained cheap green composite. There are not
yet publicly reported in this area of technology.

SUMMARY

[0004] The object of the present invention is less than for the prior art process for preparing lactic acid-
based thermoplastic WPC provides a polyethylene, simple process, excellent overall performance of the
resulting composites, green biodegradable material to expand range of applications.
[0005] To achieve this object, the technical solution of the present invention, a twin screw extruder a
polylactic acid (PLA),

Wood flour, compatibility agents, brighteners, plasticizers, nucleating agents, dispersing agents and
stabilizers for reactive blending, to obtain a comprehensive performance

Polylactic acid-based semi-rigid plastic composite material excellent in surface finish and other
advantages of the environmentally degradable.

[0006] The method of the present invention is specifically: by weight, component material: polylactic acid
(PLA) 30_90 parts, wood 5_65

3 parts of the compatibilizing agent 0. 5 to 30 parts, 0. 1-5 parts brightener, a plasticizer, 0.5 to 10 parts,
0. 5-5 parts of a nucleating agent, 0.5 to 10 parts Dispersant 0.2 to 5 parts and stabilizer, the sum of the
raw material composition of 100 parts. First, polylactic acid (PLA), wood flour, compatibility agents,
brighteners, plasticizers, nucleating agents, dispersing agents and stabilizers mixed in a high speed
stirrer, the stirrer rotating at high speed 3000-9000 rpm / min, the mixed materials extruded into pellets in
a twin-screw extruder, screw temperature to 70-24 (TC, speed of 90-600 rev / min, the material in the
screw 5_15 residence time of 0.5 minutes, extrusion after the material is cooled, pelletized by a pelletizer
to obtain pellets, 60-12 (TC dried in a vacuum oven for 5-48 hours, to obtain a polylactic acid based
thermoplastic WPC.

The polylactic acid according to the invention [0007] The present lactic acid or lactide polycondensate.

[0008] The present invention is a wood powder, wood flour, peanut hull flour, nut shell flour, bran shell
flour, straw powder or a bamboo powder, or mixtures thereof.

[0009] The compatibilizing agent of the present invention is a class of the polylactic acid and wood
materials have good affinity for the 4, 4'-isopropylidene bis (phenol salicylate), octadecane amine
bromide, stearyl ammonium chloride, boric acid ester coupling agent, silane coupling agent, a titanate
coupling agent, diisocyanate (TDI), p-hydroxybenzoic acid esters, cetyl chloride amines, 2,2 '- (l, 3-
phenylene) - bis-oxazoline, 2-mercaptobenzoxazole, l, 4 phenylene bis 2-oxazoline two, cetyl ammonium
bromide , o-hydroxybenzoic acid phenyl ester, epoxy resin, chlorinated polyethylene, epoxidized styrene
copolymer, polyester urethane, ethylene - vinyl acetate copolymer (EVA), polyethylene glycol (PEG), poly
ethylene - vinyl alcohol copolymer (EVOH), ethylene - acrylate copolymers (EAA), styrene - maleic
anhydride copolymer (SMAH epoxidized copolymer, styrene - methacrylic ester copolymer, acrylamide
branched polyethylene, acrylamide grafted ethylene-vinyl acetate copolymer _, _ an ethylene methyl
acrylate copolymer (EMA), maleic anhydride grafted polyethylene copolymer (PE-g-MAH), maleic
anhydride, then Polypropylene copolymer (PP-g-MAH), polyvinyl acrylic graft copolymer (PE-g-AA), _
glycidyl methacrylate graft copolymer of polypropylene (PP-g-GMA), acrylic polypropylene graft
copolymer (PP-g-AA), alkyd resins, maleic anhydride-grafted styrene - butadiene - styrene copolymer
(SBS-g-MAH), ethylene - butyl acrylate copolymer (EBA), maleic anhydride grafted acrylonitrile -
butadiene-styrene copolymer _ (ABS-g-MAH), ionomers acrylate, butyl maleic acid grafted ethylene -
octene copolymer (POE-g -DBM), maleic anhydride grafted ethylene - octene copolymer (POE-g-MAH),
maleic anhydride grafted ethylene - vinyl acetate copolymer (EVA-g-MAH), glycidyl methacrylate contact
branch ethylene - vinyl acetate copolymer (EVA-g-GMA), glycidyl methacrylate - polyethylene graft
copolymer (PE-g-GMA) or phenolic resins, or mixtures composed of these.

[0010] The present invention is a brightener of methyl methacrylate and butyl acrylate copolymer, N, N-
acetyl ethylene bis stearic acid amide, polyether-modified silicone, acrylate copolymer or polar group-
modified ethylene bis-fatty acid amide, or a mixture composed thereof.

[0011] The plasticizer of the present invention may be a barium stearate, dibutyl phthalate (DBP), diethyl
phthalate (DOP), acetyl tributyl citrate (the ATBC), chlorinated paraffins, dibutyl maleate, stearic acid, zinc
stearate, calcium stearate, dioctyl adipate (the DOA), a polyester type plasticizer or plasticizers
polyurethane, or a mixture composed thereof. [0012] The nucleating agent according to the present
invention is calcium carbonate, talc, wollastonite, sorbitol, clay, mica, feldspar, silica, glass beads,
graphite, carbon black, sodium citrate, titanium dioxide , magnesium hydroxide, aluminum hydroxide,
magnesium hydroxide, potassium sorbate, aluminum oxide, zinc oxide, kaolin, or whiskers, or a mixture
composed thereof.

[0013] The dispersant of the present invention may be silicon esters, oleic acid amide, low molecular
weight polylactic acid, silicone, organosilane, high Organosilane molecules, liquid paraffin, erucamide, a
silicone oil or white wax, or mixtures composed of these.

[0014] The stabilizing agent according to the present invention is 4,4 '- (P, 13' _ dihydroxy-dipropyl
oxyphenyl) 2,2-propane (bisphenol A), tribasic lead sulfate, dibasic lead stearate, tris (2,4-di-tert-
butylphenyl) phosphite (antioxidant 168), N, N'- bis [3- (3,5-di-t-butyl-4-hydroxy phenyl) propionyl]
hydrazine (antioxidant 1098), tetrakis [P- (3 ', 5'- di-t-butyl-4'-hydroxyphenyl) propionate] (antioxidant
1010), di salt lead phthalate, dioctyl tin maleic acid, tert-butyl-4-methylphenol (antioxidant 264), dilauryl
thiodipropionate (antioxidant DLTP), pentaerythritol diphosphite bis (2,4-di-tert-butylphenyl) phosphite
(antioxidant 626), methyl tin, 4,4'-methylene-bis (2,3-di-t-butylphenol 6_) (anti 4426 oxygen agent) or
butylated hydroxytoluene (antioxidant T501), wherein two or more take a complex thereof.

[0015] Preparation of polylactic acid-based thermoplastic WPC present invention, the use of renewable
environment polylactic acid (PLA) and wood flour as the main raw material, with compatible agents,
brighteners, plasticizers, nucleating agents, dispersing agents and stabilizers for reactive blending various
adjuvants, simple process, the resulting composite having excellent performance and environmental
degradation, etc., can be used as packaging materials, decorative materials and environmentally friendly
materials, On the one hand reduces the cost of polylactic acid, expanded its scope of application, it also
added a new variety of thermoplastic WPC, has broad application and industrialization prospect.

Detailed ways

[0016] The following further description of the technical solution of the present invention through specific
embodiments. The following examples further illustrate the present invention and not to limit the scope of
the invention. [0017] Example l

[0018] The feed components by weight: 90 parts of a polylactic acid, nut shell powder, 5 parts of styrene-
maleic anhydride copolymer 1 _ parts, 0.3 parts of acrylic acid ester copolymer, 1 part of barium stearate,
oxide 1 part of zinc, 1.5 parts of a silicone oil, dibasic lead stearate 0.1 parts to 0.1 parts antioxidant 168.

[0019] The first polylactic acid, shell powder, styrene - maleic anhydride copolymers, acrylate copolymers,
barium stearate, zinc oxide, silicone oil, dibasic lead stearate, antioxidants in a high-speed 168 mixed on
the mixer, a high-speed stirrer speed of 3000 r / min, then the mixed material into a twin screw extruder,
extruded into pellets, screw temperature of 70/90/120/150/160 / 165t :, speed of 600 rev / min, the
material in the screw residence time of 0.5 minutes, after the extruded material is cooled, pelletized by a
pelletizer to obtain pellets in a vacuum oven 6 (TC dried for 48 hours to give excellent overall properties,
high surface finish and biodegradable polylactic acid-based thermoplastic plastic composite material.
[0020] Example 2

[0021] The feed components by weight: 30 parts of a polylactic acid, 65 parts of bamboo powder, 2 parts
of a titanate coupling agent, N, N- ethylene bis stearic acid amide 0.5 parts of stearic acid 0 5 parts, 0.5
parts of whiskers, silicone 0.5 parts, 0.3 parts antioxidant 1010,0 7 parts antioxidant

Agent 264.
[0022] The first polylactic acid, bamboo powder, a titanate coupling agent, N, N- ethylene bis stearic acid
amide, stearic, whiskers, silicone, antioxidant 1010, antioxidant 264 uniformly mixing the high-speed
mixer, a homomixer speed of 8000 rev / min, then the mixed material into a twin screw extruder, extruded
into pellets, screw temperature of 160/180/200/220/240/235 ° C, speed 90 rev / min, the material in the
screw residence time of 15 minutes, after the extruded material is cooled, pelletized by a pelletizer to
obtain pellets in a vacuum oven 8 (TC dried for 24 hours to give excellent overall properties, high surface
finish and biodegradable polylactic acid-based thermoplastic plastic composite material. [0023] Example 3

[0024] The raw material components of 50 parts by weight of frozen lactic acid, 30 parts of wood powder,
ethylene --10 parts butyl acrylate copolymer, polyether-modified silicone 3 parts, 2 parts of chlorinated
paraffin, wollastonite 1 part, 2 parts of oleic acid amide, 1 part of antioxidant 1098, 1 626 parts of an
antioxidant.

[0025] The first polylactic acid, wood flour, _ ethylene butyl acrylate copolymer, polyether-modified
silicones, chlorinated paraffin,

Wollastonite, oleic acid amide, antioxidant 1098, antioxidant 626 mixed in a homomixer, a high-speed
stirrer rotation

Speed of 6000 rev / min, then the mixed material into a twin screw extruder, extruded into pellets, the
temperature of the screw

160/180/200/200/200/205 ° C, 300 rpm / min, the material in the screw residence time of 2 min, extrusion

After the material is cooled, pelletized by a pelletizer to obtain pellets, 12 (TC dried in a vacuum oven for
5 hours to give overall performance

Excellent surface finish and a biodegradable polylactic acid-based thermoplastic plastic composite
material.

[0026] As can be seen from the results of Examples, the polylactic acid-based WPC obtained in the
present invention has excellent overall

Performance and environmental degradation, etc., can be used as packaging materials, decorative
materials and environmentally friendly materials and the like, and has a broad industrial application

Industry prospects.

Claims (4)

Hide Dependent 

1. Preparing a poly WPC acid based thermoplastic, comprising: by weight of component material:
30-90 parts of polylactic acid, 5-65 parts wood flour, 0.5 to 30 parts of a compatibilizing agent,
0.1-5 parts brightener, from 0.5 to 10 parts of a plasticizer, 0.5-5 parts of a nucleating agent, a
dispersant 0.2 to 5 parts and stabilizer 0.5-10 parts, the sum of the raw material composition is
100 parts; at first the raw material uniformly mixing the high-speed mixer, a high-speed stirrer
speed of 3000-9000 rev / min, and then the mixed materials extruded into pellets in a twin-screw
extruder, screw temperature of 70-240 deg.] C, speed of 90-600 rpm / min, residence time in the
screw from 0.5 to 15 minutes, after the extruded material is cooled, pelletized by a pelletizer to
obtain pellets, and dried in a vacuum oven at 60-120 ℃ 5-48 hours, to obtain poly acid-based
thermoplastic plastic composite materials; wherein: the compatibilizing agent is a boric acid ester
coupling agent, a silane coupling agent, a titanate coupling agent, diisocyanate, epoxidized
styrene copolymer, ethylene - vinyl acetate copolymers, polyethylene glycol, polyethylene - vinyl
alcohol copolymers, ethylene - acrylate copolymers, styrene Alkenyl - maleic anhydride
copolymer, epoxidized ethylene copolymers, styrene - methacrylic acid ester copolymers,
acrylamide graft polyethylene, acrylamide grafted ethylene - vinyl acetate copolymer, maleic
anhydride-grafted polypropylene ethylene copolymers, copolymers of maleic anhydride grafted
polypropylene, acrylic acid graft polyethylene, glycidyl methacrylate - polypropylene graft
copolymers, acrylic acid graft polypropylene, alkyd resins, maleic anhydride, then branched
styrene - butadiene - styrene copolymer, maleic anhydride grafted acrylonitrile - butadiene -
styrene copolymer, maleic acid ester grafted ethylene - octene copolymer, maleic anhydride
grafted ethylene - octene copolymer, maleic anhydride grafted ethylene - vinyl acetate copolymer,
glycidyl methacrylate grafted ethylene - vinyl acetate copolymer, glycidyl methacrylate -
polyethylene graft copolymer or phenolic resins, or mixtures composed of these; the brightener is
N, N- ethylene bis stearic acid amide, polyether-modified silicone, acrylate copolymer or a polar
group-modified of ethylene bis-fatty acid amide, or a Their mixture thereof; said dispersant is
silicon esters, oleic acid amide, silicone, organosilane, liquid paraffin, erucamide, a silicone oil or
white wax, or a mixture composed thereof; said stabilizer is 4,4 '- (β, β'- dihydroxy dipropyl
oxyphenyl) 2,2-propane (bisphenol A), tribasic lead sulfate, dibasic lead stearate, 168
antioxidants, anti- 1098-oxidants, antioxidant 1010, dibasic lead phthalate, dioctyl tin maleate,
antioxidant 264, antioxidant DLTP, antioxidant 626, antioxidant 4426 T501 or antioxidants, taken
wherein the complex of two or more thereof.

2. A method according to claim WPC prepared polylactic acid based heat plasticity 1,
wherein said polylactic acid is lactic acid or lactide polycondensate.

3. The method for preparing a polylactic acid based heat plasticity WPC claim, wherein said
plasticizer is barium stearate, dibutyl phthalate, diethyl phthalate , acetyl tributyl citrate,
chlorinated paraffins, dibutyl maleate, stearic acid, zinc stearate, calcium stearate, dioctyl
adipate, or mixtures composed of these.

4. The method for preparing polylactic acid-based thermoplastic WPC claimed in claim l,
wherein said nucleating agent is calcium carbonate, talc, wollastonite, sorbitol, clay, mica,
feldspar, silica, glass beads, graphite, carbon black, sodium citrate, titanium oxide,
magnesium hydroxide, aluminum hydroxide, magnesium hydroxide, potassium sorbate,
aluminum oxide, zinc oxide, or kaolin, or mixtures composed of these.

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