CN109957099A - A kind of production method of low melting point anionic copolymerization type modified poly ester - Google Patents
A kind of production method of low melting point anionic copolymerization type modified poly ester Download PDFInfo
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- CN109957099A CN109957099A CN201910152753.7A CN201910152753A CN109957099A CN 109957099 A CN109957099 A CN 109957099A CN 201910152753 A CN201910152753 A CN 201910152753A CN 109957099 A CN109957099 A CN 109957099A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- Health & Medical Sciences (AREA)
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- Polymers & Plastics (AREA)
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- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention provides a kind of production methods of low melting point anionic copolymerization type modified poly ester, take anion powder, ethylene glycol, titanate coupling agent, dispersing agent JFC by mass fraction；Grinding slurry is mixed and be ground into, grinding slurry is pumped into centrifugation in centrifuge and is obtained as anion slurry a；Take M-phthalic acid, p-phthalic acid, PEG, ethylene glycol, Sb2O3Slurry b is made in reaction, and slurry b is imported reaction in reaction kettle of the esterification and obtains carboxylate；Carboxylate is imported and carries out the final finished product of polycondensation reaction in batch condensation polymerization reactor.Low melting point anion modified poly ester obtained by the present invention has stronger functionality, the slurry of releasable negative oxygen ion can not only be made, and PEG and catalyst since proper ratio is added, greatly strengthen the degree of polymerization of low-melting point polyester, when carrying out composite spinning using product of the present invention and chemical fibre etc., the intensity of blended ratio or fabric can be enhanced.
Description
Technical field
The present invention relates to technical field of function materials more particularly to a kind of lifes of low melting point anionic copolymerization type modified poly ester
Production method.
Background technique
Low-melting point polyester in the prior art does not have the master batch function of can be made into releasing negative oxygen ion function, and often exists
With in the fusion process of chemical fibre and blend fibre, since adhesiveness not enough causes obtained fabric lining intensity lower.
Summary of the invention
Goal of the invention: in view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of low melting point anionic copolymerization
The production method of type modified poly ester.
The innovation of the invention consists in that low melting point anion modified poly ester obtained by the present invention has stronger functionality,
The slurry of releasable negative oxygen ion, and PEG and catalyst since proper ratio is added can not only be made, greatly strengthen eutectic
The degree of polymerization of point polyester can enhance the strong of blended ratio or fabric when using the progress composite spinning such as product of the present invention and chemical fibre
Degree.
Technical solution: in order to achieve the above object of the invention, the present invention is specifically achieved like this: a kind of low melting point bear from
The production method of sub- copoly type modified poly ester, comprising the following steps:
(1) by mass fraction take 20 parts of anion powders, 80 parts of ethylene glycol, 0.02 ~ 0.05 part of titanate coupling agent, 0.01 ~
0.05 part of dispersing agent JFC；Mix each component simultaneously grind 2 ~ 8 hours formation grinding slurries, by grinding slurry be pumped into centrifuge from
Gains in depth of comprehension are to centrifugate, and the centrifugate is anion slurry a, and the partial size of anion slurry a is 20 ~ 800nm；
(2) 10 ~ 30 parts of M-phthalic acids, 42 ~ 58 parts of p-phthalic acids, 2 ~ 20 parts of PEG, 12 ~ 26 parts of second are taken by mass fraction
Glycol, 0.004 ~ 0.008 part of Sb2O3Mashing reaction kettle reaction is added, reaction temperature control at 80 ~ 120 DEG C, uniform stirring 30 ~
Slurry b is made after 60min；
(3) slurry b is imported in reaction kettle of the esterification, is warming up to 220 ~ 260 DEG C of one stage esterifications of progress, single order under normal pressure
Section reaction time of esterification is 120 ~ 180min；Anion slurry a, trimethyl phosphate are added after one stage esterification, bear from
The quality of sub- slurry a be slurry b mass 4 ~ 25%, trimethyl phosphate quality be slurry a mass 0.001 ~ 0.01%, continue into
Row two-stage esterification, two-stage reaction time of esterification are 30 ~ 60min, obtain carboxylate after two-stage reaction；
(4) carboxylate obtained by step (3) is imported in batch condensation polymerization reactor, is warming up to 260 ~ 270 under the pressure of 1400 ~ 2000Pa
DEG C, stage polycondensation reaction is carried out, a stage polycondensation reaction time is 60 ~ 90min；Pressure will be adjusted after the polycondensation reaction of one stage
To 20 ~ 100Pa, temperature is adjusted to 270 ~ 285 DEG C, continues two-stage polycondensation reaction, and two-stage polycondensation reaction time is 60 ~
120min, final finished product.
Further, the grinding in the step (2) can be used grinder grinding, and the partial size of the grinder zirconium pearl is 1 ~
100μm。
Beneficial effects of the present invention: compared with traditional technology, the present invention has the advantage that
Low melting point anion modified poly ester obtained by the present invention has stronger functionality, can not only be made releasable negative oxygen from
The slurry of son, and PEG and catalyst since proper ratio is added, greatly strengthen the degree of polymerization of low-melting point polyester, are utilizing
When product of the present invention and chemical fibre etc. carry out composite spinning, the intensity of blended ratio or fabric can be enhanced.
Specific embodiment
Embodiment 1: a kind of production method of low melting point anionic copolymerization type modified poly ester takes 20 parts to bear by mass fraction
Ion powder, 80 parts of ethylene glycol, 0.02 part of titanate coupling agent, 0.01 part of dispersing agent JFC；It mixes each component and uses zirconium bead
Diameter is that 1 μm of grinder grinds 2 hours formation grinding slurries, and it is undispersed that grinding slurry is pumped into centrifuge separation removal in centrifuge
Bulky grain obtains centrifugate, and centrifugate is anion slurry a, and the partial size of anion slurry a is 20 ~ 800nm, anion slurry a
Solid content be 20%；10 parts of M-phthalic acids are taken to take 10 ~ 30 parts of M-phthalic acids, 42 parts of essences by mass fraction by mass fraction again
Terephthalic acid (TPA), 2 parts of PEG, 12 parts of ethylene glycol, 0.004 part of catalyst Sb2O3Mashing reaction kettle reaction, reaction temperature control is added
Slurry b is made after 80 ~ 120 DEG C, uniform stirring 30min；Slurry b is imported in reaction kettle of the esterification, is warming up to 220 under normal pressure
~ 260 DEG C of one stage esterifications of progress, a stage reaction time of esterification are 120min；It is added after one stage esterification negative
Ion slurry a, stabilizer trimethyl phosphate, the quality of anion slurry a are the 4% of slurry b mass, and trimethyl phosphate quality is
The 0.001% of slurry a mass, continues two-stage esterification, and two-stage reaction time of esterification is 30min, two-stage reaction
After obtain carboxylate, by carboxylate import batch condensation polymerization reactor in, 260 ~ 270 DEG C are warming up under the pressure of 1400 ~ 2000Pa, into
Row one stage polycondensation reaction, a stage polycondensation reaction time are 60min；To be adjusted after the polycondensation reaction of one stage pressure to 20 ~
100Pa, temperature are adjusted to 270 ~ 285 DEG C, continue two-stage polycondensation reaction, and two-stage polycondensation reaction time is 60min, most
Whole finished product.
Embodiment 2: a kind of production method of low melting point anionic copolymerization type modified poly ester takes 20 parts to bear by mass fraction
Ion powder, 80 parts of ethylene glycol, 0.03 part of titanate coupling agent, 0.03 part of dispersing agent JFC；It mixes each component and uses zirconium bead
Diameter is that 50 μm of grinders grind 5 hours formation grinding slurries, and grinding slurry is pumped into centrifuge separation removal in centrifuge and is not dispersed
Bulky grain obtain centrifugate, centrifugate is anion slurry a, and the partial size of anion slurry a is 20 ~ 800nm, anion slurry
The solid content of a is 20%；20 parts of M-phthalic acids, 50 parts of p-phthalic acids, 10 parts of PEG, 20 parts of second two are taken by mass fraction again
Alcohol, 0.006 part of catalyst Sb2O3Mashing reaction kettle reaction is added, reaction temperature controls after 80 ~ 120 DEG C, uniform stirring 45min
Slurry b is made；Slurry b is imported in reaction kettle of the esterification, is warming up to 220 ~ 260 DEG C of one stage esterifications of progress under normal pressure,
One stage reaction time of esterification is 150min；Anion slurry a, stabilizer tripotassium phosphate are added after one stage esterification
Ester, the quality of anion slurry a are the 15% of slurry b mass, and trimethyl phosphate quality is the 0.005% of slurry a mass, continue into
Row two-stage esterification, two-stage reaction time of esterification are 45min, obtain carboxylate after two-stage reaction, carboxylate is led
Enter in batch condensation polymerization reactor, 260 ~ 270 DEG C are warming up under the pressure of 1400 ~ 2000Pa, carries out stage polycondensation reaction, a stage
Polycondensation reaction time is 75min；Pressure will be adjusted after the polycondensation reaction of one stage to 20 ~ 100Pa, temperature is adjusted to 270 ~ 285 DEG C,
Continue two-stage polycondensation reaction, two-stage polycondensation reaction time is 90min, final finished product.
Embodiment 3: a kind of production method of low melting point anionic copolymerization type modified poly ester takes 20 parts to bear by mass fraction
Ion powder, 80 parts of ethylene glycol, 0.03 part of titanate coupling agent, 0.05 part of dispersing agent JFC；It mixes each component and uses zirconium bead
Diameter is that 100 μm of grinders grind 8 hours formation grinding slurries, and grinding slurry is pumped into centrifuge separation removal in centrifuge and is not dispersed
Bulky grain obtain centrifugate, centrifugate is anion slurry a, and the partial size of anion slurry a is 20 ~ 800nm, anion slurry
The solid content of a is 20%；30 parts of M-phthalic acids, 58 parts of p-phthalic acids, 20 parts of PEG, 26 parts of second two are taken by mass fraction again
Alcohol, 0.008 part of catalyst Sb2O3Mashing reaction kettle reaction is added, reaction temperature controls after 80 ~ 120 DEG C, uniform stirring 60min
Slurry b is made；Slurry b is imported in reaction kettle of the esterification, is warming up to 220 ~ 260 DEG C of one stage esterifications of progress under normal pressure,
One stage reaction time of esterification is 180min；Anion slurry a, stabilizer tripotassium phosphate are added after one stage esterification
Ester, the quality of anion slurry a are the 25% of slurry b mass, and trimethyl phosphate quality is the 0.01% of slurry a mass, continue into
Row two-stage esterification, two-stage reaction time of esterification are 60min, obtain carboxylate after two-stage reaction, carboxylate is led
Enter in batch condensation polymerization reactor, 260 ~ 270 DEG C are warming up under the pressure of 1400 ~ 2000Pa, carries out stage polycondensation reaction, a stage
Polycondensation reaction time is 90min；Pressure will be adjusted after the polycondensation reaction of one stage to 20 ~ 100Pa, temperature is adjusted to 270 ~ 285 DEG C,
Continue two-stage polycondensation reaction, two-stage polycondensation reaction time is 120min, final finished product.
Claims (2)
1. a kind of production method of low melting point anionic copolymerization type modified poly ester, which comprises the following steps:
(1) by mass fraction take 20 parts of anion powders, 80 parts of ethylene glycol, 0.02 ~ 0.05 part of titanate coupling agent, 0.01 ~
0.05 part of dispersing agent JFC；Mix each component simultaneously grind 2 ~ 8 hours formation grinding slurries, by grinding slurry be pumped into centrifuge from
Gains in depth of comprehension are to centrifugate, and the centrifugate is anion slurry a, and the partial size of anion slurry a is 20 ~ 800nm；
(2) 10 ~ 30 parts of M-phthalic acids, 42 ~ 58 parts of p-phthalic acids, 2 ~ 20 parts of PEG, 12 ~ 26 parts of second are taken by mass fraction
Glycol, 0.004 ~ 0.008 part of Sb2O3Mashing reaction kettle reaction is added, reaction temperature control at 80 ~ 120 DEG C, uniform stirring 30 ~
Slurry b is made after 60min；
(3) slurry b is imported in reaction kettle of the esterification, is warming up to 220 ~ 260 DEG C of one stage esterifications of progress, single order under normal pressure
Section reaction time of esterification is 120 ~ 180min；Anion slurry a, trimethyl phosphate are added after one stage esterification, bear from
The quality of sub- slurry a be slurry b mass 4 ~ 25%, trimethyl phosphate quality be slurry a mass 0.001 ~ 0.01%, continue into
Row two-stage esterification, two-stage reaction time of esterification are 30 ~ 60min, obtain carboxylate after two-stage reaction；
(4) carboxylate obtained by step (3) is imported in batch condensation polymerization reactor, is warming up to 260 ~ 270 under the pressure of 1400 ~ 2000Pa
DEG C, stage polycondensation reaction is carried out, a stage polycondensation reaction time is 60 ~ 90min；Pressure will be adjusted after the polycondensation reaction of one stage
To 20 ~ 100Pa, temperature is adjusted to 270 ~ 285 DEG C, continues two-stage polycondensation reaction, and two-stage polycondensation reaction time is 60 ~
120min, final finished product.
2. the production method of low melting point anionic copolymerization type modified poly ester according to claim 1, which is characterized in that described
Grinder grinding can be used in grinding in step (2), and the partial size of the grinder zirconium pearl is 1 ~ 100 μm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910152753.7A CN109957099A (en) | 2019-02-28 | 2019-02-28 | A kind of production method of low melting point anionic copolymerization type modified poly ester |
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| CN201910152753.7A CN109957099A (en) | 2019-02-28 | 2019-02-28 | A kind of production method of low melting point anionic copolymerization type modified poly ester |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112553734A (en) * | 2020-11-30 | 2021-03-26 | 闽江学院 | Method for preparing non-ironing multifunctional blended yarn by utilizing electrostatic spinning nanotechnology |
| CN112575410A (en) * | 2020-12-10 | 2021-03-30 | 合肥学院 | Preparation method of negative ion textile fabric with air purification capacity |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1451673A (en) * | 2002-04-15 | 2003-10-29 | 上海金樱环保科技有限公司 | Chemical fibre grade polyester resin with health function and making method thereof |
| CN104558560A (en) * | 2013-10-11 | 2015-04-29 | 中国石油化工股份有限公司 | A preparing method of low-melting point polyester used for manufacturing terylene sewing threads |
| US20150291733A1 (en) * | 2012-10-29 | 2015-10-15 | Uhde Inventa-Fischer Gmbh | Method for the production of a high-molecular polyester or copolyester and also of a polymer blend comprising these |
| CN104988594A (en) * | 2015-01-16 | 2015-10-21 | 浙江真北纺织新材料研究院有限公司 | Preparation method of negative ion release, far-infrared and fire retardation composite function polyester fibers |
| CN105063797A (en) * | 2015-07-16 | 2015-11-18 | 中国纺织科学研究院 | Method for preparing low-melting-point polyester composite fiber by adopting continuous polymerization and melt direct-spinning |
-
2019
- 2019-02-28 CN CN201910152753.7A patent/CN109957099A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1451673A (en) * | 2002-04-15 | 2003-10-29 | 上海金樱环保科技有限公司 | Chemical fibre grade polyester resin with health function and making method thereof |
| US20150291733A1 (en) * | 2012-10-29 | 2015-10-15 | Uhde Inventa-Fischer Gmbh | Method for the production of a high-molecular polyester or copolyester and also of a polymer blend comprising these |
| CN104558560A (en) * | 2013-10-11 | 2015-04-29 | 中国石油化工股份有限公司 | A preparing method of low-melting point polyester used for manufacturing terylene sewing threads |
| CN104988594A (en) * | 2015-01-16 | 2015-10-21 | 浙江真北纺织新材料研究院有限公司 | Preparation method of negative ion release, far-infrared and fire retardation composite function polyester fibers |
| CN105063797A (en) * | 2015-07-16 | 2015-11-18 | 中国纺织科学研究院 | Method for preparing low-melting-point polyester composite fiber by adopting continuous polymerization and melt direct-spinning |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112553734A (en) * | 2020-11-30 | 2021-03-26 | 闽江学院 | Method for preparing non-ironing multifunctional blended yarn by utilizing electrostatic spinning nanotechnology |
| CN112575410A (en) * | 2020-12-10 | 2021-03-30 | 合肥学院 | Preparation method of negative ion textile fabric with air purification capacity |
| CN112575410B (en) * | 2020-12-10 | 2022-12-13 | 合肥学院 | Preparation method of negative ion textile fabric with air purification capacity |
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Application publication date: 20190702 |
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