Patent CN103113564A - Color-fixing polyester and preparation method th... https://www.google.com/patents/CN103113564A?cl=en&dq=CN103113...

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Color-fixing polyester and preparation method

thereof
CN 103113564 A

ABSTRACT

The invention relates to color-fixing polyester which is prepared through the

copolymerization of pure terephthalic acid and ethylene glycol used as basic
materials. The color-fixing polyester also contains polyethyleneglycol which
accounts for 0.5-0.8wt% of the color-fixing polyester and has an average
molecular weight of 4000-8000. The preparation method comprises the following
steps: mixing the pure terephthalic acid and the ethylene glycol according to a
mol ratio of (1.2-1.5):1, pulping, adding a catalyst and assistants, and evenly
mixing; then feeding into an esterification kettle, and performing esterification reaction; and feeding the esterification product into a polycondensation kettle, adding
the polyethyleneglycol which has a molecular weight of 4000-8000, and performing polymerization reaction, wherein the amount of the polyethyleneglycol accounts
for 0.5-0.8wt% of the color-fixing polyester. When a color-fixing polyester/coloring master batch blended molten mass and an alkali-soluble polyester molten mass
are subjected to island-in-sea composite spinning, dye in island components can not migrate to sea components, and the color is stable; and figured island-in-sea
composite ultrafine short fibers can not be subjected to alkali weight reduction in the subsequent product processing course.

DESCRIPTION translated from Chinese CLAIMS (4) translated from Chinese

Fixing polyester and preparation method A method of fixing polyester, characterized in that the purified terephthalic acid
and ethylene glycol as raw materials copolymerization fixing further contains
Technology
0.5-0.8% by weight of polyester, with an average molecular weight of 4000 PEG

[0001] The present invention relates to a polyester-fixing and a preparation -8000.

method of the masterbatch blend of polyester and molten alkali-soluble polyester

melt and the melt colored molten sea-island type composite spinning islands ,
keep the color and color stability does not migrate, are polyester chemical
technology.
BACKGROUND
[0002] In the microfiber fabric and leather production process, often need to use
colored fibers to make specific parts of the product or products show a certain
color, which play the role of aesthetics or logo. PET with ordinary colored
masterbatch production plus a fixed-island microfiber composite island, color
instability, mainly due to the alkali-soluble polyester colored sea component is
strong, the bicomponent spinning process, the island component within the
colored dye migration occurs lead.
SUMMARY OF THE INVENTION
[0003] The object of the present invention is to solve the prior art and to provide
a polyester-fixing, to melt and melt blending the masterbatch with an alkali
soluble polyester melts molten composite spinning islands When the dye within
the island components not migrate to the sea component, while the fixed-island
microfiber short fiber composite island in the subsequent processing of products base reduction does not occur.
The process of claim 1, wherein the fixing method for preparing
polyester, characterized by comprising the steps of: (1) the purified
terephthalic acid and ethylene glycol at a molar ratio (1.2-1.5): 1
mixture of beating , catalyst is added to the slurry and additives, mix
into the esterification reactor for esterification; (2) the esterification
product into the polycondensation reactor, adding polyethylene glycol of
molecular weight of 4000-8000 polymerization reaction , polyethylene
glycol polyester plus fixing accounts for 0.5-0.8% by weight.
3 as claimed in claim 2, wherein the fixing method for preparing
polyester, characterized in that step (I) in the esterification reaction at a
temperature of 250-255 ° C, time is 190-220min.
4 as claimed in claim 2 or 3, wherein the fixing method for the
preparation of polyester, characterized in that step (2), the polyethylene
glycol with a 180 ° C saturated steam melt into the melt, and then
added to the polycondensation kettle.

[0004] The present invention is a solid color polyester from purified terephthalic acid and ethylene glycol as raw materials
copolymerization fixing further contains 0.5-0.8% by weight of polyester, with an average molecular weight of 4000-8000
polyethylene glycols.

[0005] fixing the above-described method for preparing polyester comprising the steps of:

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Patent CN103113564A - Color-fixing polyester and preparation method th... https://www.google.com/patents/CN103113564A?cl=en&dq=CN103113...

[0006] (I) the purified terephthalic acid and ethylene glycol at a molar ratio (1.2-1.5): 1 mixture of beating, the slurry was
added to the catalyst and additives, mix into the esterification reactor for esterification reaction; said catalyst is antimony
trioxide, adding an amount of fixing 0.022-0.025% by weight of polyester, said additive is trimethyl phosphate and cobalt
acetate were added in an amount representing the weight polyester fixing 0.016-0.018% and 0.0015-0.002%.

[0007] (2) into the polycondensation product of the esterification reactor, by adding a molecular weight of 4000-8000
polymerization of polyethylene glycol, polyethylene glycol, polyester plus fixing accounts for 0.5-0.8% by weight.
Polymerization is carried out under negative pressure, low vacuum stage of polymerization (the degree of vacuum between
2-3Kpa absolute pressure), temperature controlled at 248-252 ° C, time is l_2h, the polymerization reaction under high
vacuum stage (abs. 50-150Pa), temperature controlled at 274-278 ° C, time is 24h. After completion of the reaction, the
resulting polymer extruded from the autoclave, granulation, ie.

[0008] Step (I) in the esterification reaction at a temperature of 250-255 ° C, the esterification reaction time is 190_220min.

[0009] Step (2), since the high degree of polymerization polyethylene glycol is solid state, added to the product in order to
ensure the uniform distribution of polyethylene glycol linked to the product, it is preferable to use polyethylene glycol 180 ° C
saturated steam melt into the melt, and then added to the polycondensation vessel.

[0010] The present invention is obtained by fixing polyester, m.p. 245-255 ° C, b value 5-7, diethylene glycol content of
1.2-1.8mol / t, intrinsic viscosity of 0.62-0.67dl / g, which and masterbatch melt blended with molten alkali-soluble polyester
composite melt spinning melt for the island, the island components within the composition of the dye does not migrate to the
sea and color stability, while the fixed-island sea composite ultra-fine fibers in the subsequent processing of products base
reduction does not occur. Specific embodiments

[0011] The following examples illustrate the present invention with further instructions.

[0012] Example 1

[0013] The purified terephthalic acid and ethylene glycol are mixed at a molar ratio of 1.2:1 beating, adding weight
accounted for fixing polyester

0.025% of antimony trioxide, 0.016% of potassium phosphate ester and 0.0015% of cobalt acetate, mix into the
esterification reactor for esterification; the esterification reaction product into the polycondensation reactor, and then adding
the solid 0.8% by weight of polyester color average molecular weight of polyethylene glycol 4000, after mixing the
polymerization. Low vacuum stage of the polymerization reaction, the temperature controlled at 248 ° C, time was 2h, high
vacuum stage of the polymerization reaction, the temperature controlled at 275 ° C, time of 3h. After completion of the
reaction, the resulting polymer extruded from the autoclave, granulation, ie.

[0014] This embodiment obtained polyester solid color, a melting point of 245 ° C, b value of 5.3, diethylene glycol content
of 1.3mol / t, an intrinsic viscosity of 0.63dl / g.

[0015] Example 2

[0016] The purified terephthalic acid and ethylene glycol are mixed at a molar ratio of 1.3:1 beating, adding weight
accounted for fixing polyester

0.023% of antimony trioxide, 0.0165% of tripotassium phosphate ester and 0.0017% cobalt acetate, mix into the
esterification reactor for esterification; the esterification reaction product into the polycondensation reactor, and then adding
the solid 0.7 percent by weight of polyester color average molecular weight of polyethylene glycol 5000, after mixing the
polymerization. Low vacuum stage of the polymerization reaction, the temperature controlled at 249 ° C, time of 1.5h,
polymerization high vacuum stage, the temperature controlled at 276 ° C, time is 3.75h. After completion of the reaction, the
resulting polymer extruded from the autoclave, granulation, ie.

[0017] This embodiment obtained polyester solid color, a melting point of 248 ° C, b value of 5.9, diethylene glycol content
of 1.5mol / t, an intrinsic viscosity of 0.64dl / g.

[0018] Example 3

[0019] The purified terephthalic acid and ethylene glycol are mixed at a molar ratio of 1.5:1 beating, adding weight
accounted for fixing polyester

0.025% of antimony trioxide, 0.0175% of tripotassium phosphate ester and 0.002% cobalt acetate, mix into the
esterification reactor for esterification; the esterification condensation reaction product into the autoclave, and then added
as a solid 0.5% by weight of polyester color average molecular weight of polyethylene glycol 7000, after mixing the
polymerization. Low vacuum stage of the polymerization reaction, the temperature controlled at 250 ° C, time of lh, the high
vacuum stage of the polymerization reaction, the temperature controlled at 278 ° C, time of 2h. After completion of the
reaction, the resulting polymer extruded from the autoclave, granulation, ie.

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[0020] This embodiment obtained polyester solid color, a melting point of 253 ° C, b value of 6.6, diethylene glycol content
of 1.7mol / t, an intrinsic viscosity of 0.66dl / g.

[0021] Example 4

[0022] The purified terephthalic acid and ethylene glycol are mixed at a molar ratio of 1.4:1 beating, adding weight
accounted for fixing polyester

0.024% of antimony trioxide, 0.017% of potassium phosphate ester and 0.0019% of cobalt acetate, mix into the
esterification reactor for esterification; the esterification reaction product into the polycondensation reactor, and then adding
the solid 0.6% by weight of polyester color average molecular weight of polyethylene glycol 6000, after mixing the
polymerization. Low vacuum stage of the polymerization reaction, the temperature controlled at 250 ° C, time of 1.25h, the
high vacuum stage of the polymerization reaction, the temperature controlled at 277 ° C, time of 3.5h. After completion of
the reaction, the resulting polymer extruded from the autoclave, granulation, ie.

[0023] This embodiment obtained polyester solid color, a melting point of 250 ° C, b value of 6.2, diethylene glycol content
of 1.6mol / t, an intrinsic viscosity of 0.65dl / g. [0024] Example 5 [0025] The average molecular weight of polyethylene
glycol 6000 accounted for fixing polyester plus 0.5% by weight, the rest were the same as in Example 4.

[0026] Example 6

[0027] The average molecular weight of polyethylene glycol 6000 accounted for fixing polyester plus 0.7 wt%, the rest were
the same as in Example 4.

[0028] Example 7

[0029] The average molecular weight of polyethylene glycol 6000 accounted for fixing polyester plus 0.8% by weight, the
rest were the same as in Example 4.

[0030] Comparative Example 1-5

[0031] The average molecular weight of 6000 plus the amount of polyethylene glycol polyester fixing accounted for 0.2% by
weight, 0.3%, 0.4%, 0.9%, 1.0%, the rest were the same as in Example 4.

[0032] Performance Testing:

[0033] 1, 4-7 and Comparative Examples 1-5 The polyester obtained alkali Reduction Test: Take Comparative Examples
and a polyester obtained 100g, with 95 ° C, 3% concentration of NaOH solution soak 30min, then washed with deionized
water clean, dried and weighed, such as saying that the weight data obtained close to 100g, it indicates that did not happen
base reduction. Test results are shown in Table I.

[0034] 2, 4-7 and Comparative Examples 1-5 obtained by spinning a polyester prepared by polymerization colored short
fixed-island sea composite fibers and then tested.

`[0035] Semi-island sea-island type composite short fiber preparation process: The Comparative Examples and the
obtained polyester masterbatch respectively at 92: 8 mixed in a weight ratio as the islands component, an alkali-soluble
polyester as a the sea component, the island component and the sea component is pre-crystallized, dried, respectively,
through a twin-screw extruder melt extrusion, into two housings, the sea component extruder four temperature control zone
and cabinet temperature was 2450C, 2700C, 275 ° C, 275 ° C, 270 ° C; island component of the screw extruder four
temperature control zone and cabinet temperature was 260 ° C, 270 ° C , 28 (TC, 275 ° C, 27 (rC. into two casing by a
melt metering pump and then were metered together into a spinning pack, the island component and the sea component
controlling the weight ratio of 70: 30, component spinning the melt-mixed in the discharge from the spinneret, quenching
after forming oiling side winding, the winding speed of 880m/min, and then the cluster, due to stretch into the oil bath, oil
bath temperature of 70 ° C, less stretch factor of 3, less stretch backward 100-120 ° C steam, then curl, drying
stereotypes, stereotypes drying temperature an area of 110 ° C, two zone is 120 ° C, three District 125 ° C, total
stereotypes drying time is 25min, and finally cut off the tow package, get colored fixed-island microfiber short fiber
composite island.

[0036] ① take fixed-island sea composite colored ultra-fine fibers 100g, with 95 ° C, 3% NaOH solution for 30min
concentration observed after alkaline color, as the island component and the sea component in a weight ratio of 70 : 30, as
the sea component is an alkali-soluble polyester alkali lye solution out, so if alkaline hydrolysis with NaOH solution after the
color of the dye, then the dye within the island components to sea component migration occurred, ① otherwise not be the
fiber after the alkali solution was washed with deionized water, clean, dried and weighed, as said weight data obtained
close to 70g, it indicates that the alkali reduction did not happen; ③ ① in the fiber after alkaline hydrolysis with the use of
conventional polyester obtained through the same process for comparing colors colored fibers, such as the same color, it
indicates that the dye is not within the island components components migrate to the sea and the color stability, if the color
is subdued, that the dye had migrated The test results are shown in Table I.

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[0037] Table I Performance Test Results

[0038]

[0039] From the above table of test results can be seen that the present invention is a solid color masterbatch blend of
polyester and molten alkali-soluble polyester melt and the melt when the melt-spun islands, island components the dye does
not migrate to the sea component and color stability.

CLASSIFICATIONS

International Classification C08G63/672, D01F8/14

LEGAL EVENTS

Date Code Event Description

Jun 19, 2013 C10 Request of examination as to substance
May 22, 2013 C06 Publication

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