CN101824140A - Preparation method of 1,3-butanediol modified PBTPET (Polybutylece Terephthalate Polyethylene Terephthalate) copolymer fiber - Google Patents
Preparation method of 1,3-butanediol modified PBTPET (Polybutylece Terephthalate Polyethylene Terephthalate) copolymer fiber Download PDFInfo
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- CN101824140A CN101824140A CN200910102102A CN200910102102A CN101824140A CN 101824140 A CN101824140 A CN 101824140A CN 200910102102 A CN200910102102 A CN 200910102102A CN 200910102102 A CN200910102102 A CN 200910102102A CN 101824140 A CN101824140 A CN 101824140A
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Abstract
The invention relates to a preparation method of a 1,3-butanediol modified PBTPET (Polybutylece Terephthalate Polyethylene Terephthalate) copolymer fiber. The preparation method is characterized in that raw materials for fiber synthesis comprise terephthalic acid, butanediol, ethylene glycol and 1,3-butanediol; and the combination of p-toluenesulfonic acid and stannous chloride is used as a catalyst. The preparation method comprises the following steps of: (1) carrying out an esterification reaction on the terephthalic acid and dihydric alcohol to form a prepolymer; and (2) carrying out a condensation polymerization reaction on the prepolymer in the presence of high temperature and high vacuum. Compared with a PBT/PET copolymer fiber, the prepared 1,3-butanediol modified copolymer fiber has higher inherent viscosity and lower terminal carboxyl group number, and the dye-uptake of the modified fiber is also obviously improved.
Description
Technical field
The present invention relates to a kind of modified copolymer fiber preparation method, particularly the preparation method of 1,3 butylene glycol modified PBT PET copolymer fibre belongs to the synthetic field of fibre modification.
Background technology
Polyethylene terephthalate in man-made fiber (PET), polybutylene terephthalate (PBT) and propylene glycol ester terephthalate (PTT) structural similitude obtain through terephthalic acid and the polymerization of straight chain binary aliphatic alcohol.Three kinds of polyester are regular owing to macromolecular chain structure, the molecular chain rigid structure, and easily crystallization lacks hydrophilic radical and easily causes dyeing behavior poor.People can add other comonomer and additive, to improve the trevira performance in order to satisfy the needs of different purposes in polymerization process.
Summary of the invention
The objective of the invention is to utilize 1,3 butylene glycol that the PBT/PET copolymer fibre is carried out modification,, reduce the crystallinity of PET by the introducing of pending methyl group on the main chain, the symmetry of molecular backbone chain, the colouring power of raising polyester improves the trevira performance.
A kind of 1, the preparation method of 3-butyleneglycol modified PBT/PET copolymer fibre, it is characterized in that: the fiber synthesis material is terephthalic acid, butyleneglycol, ethylene glycol and 1, the 3-butyleneglycol, the combination of using tosic acid and two kinds of materials of tin protochloride is as catalyzer, the first step terephthalic acid and dibasic alcohol carry out esterification and form performed polymer, second step be performed polymer under the condition of high temperature high vacuum, carry out polycondensation.
The preparation raw material is terephthalic acid, butyleneglycol, ethylene glycol and 1,3 butylene glycol, and the 1,3 butylene glycol addition is an alcohol amount 5～10%, and the butyleneglycol consumption is an alcohol amount 20～30%, and the ethylene glycol consumption is an alcohol amount 75～60%.The material ratio of dibasic alcohol and terephthalic acid is 1.10～1.15.
Use tosic acid and two kinds of combinations of substances of tin protochloride as catalyzer, the tin protochloride consumption is 300 * 10 of an acid amount
-6, the consumption of tosic acid is 100 * 10 of an acid amount
-6
Fiber will add multiple auxiliary agent in synthetic, comprise stablizer, matting agent, fire retardant, etherificate inhibitor.
Stablizer trimethyl phosphite 99 2.8～3.0 ‰
TITANIUM DIOXIDE DELUSTRANT 1.8～2.0 ‰
Fire retardant phosphorus flame retardant 2.2～2.5 ‰
Etherificate inhibitor sodium-acetate 1.3～1.5 ‰
The synthetic employing continous way polyester production process of copolymer fibre, the first step esterification is finished through two reaction kettle of the esterification, and polycondensation is finished through prepolymerization reaction still and the poly-reactor of final minification.
| Condition | Esterification I | Esterification II | Precondensation | Final minification is poly- |
| Temperature of reaction/℃ | ??240～250 | ??250～260 | ??260～270 | ??270～280 |
| Reaction pressure/Pa | ??(1.3～1.5)×10 5 | ??60000～70000 | ??2500～3000 | ??50～100 |
| The residence time/min | ??90～100 | ??90～120 | ??50～70 | ??120～150 |
The preparation result of modification by copolymerization fiber is:
Progressive meaning of the present invention is:
1. tosic acid and two kinds of materials of tin protochloride use that combines during the copolymer fibre polymerization improves catalytic efficiency, reduces catalyst levels.
2. by on PBT/PET copolymer fibre main chain, introducing a shape 1,3 butylene glycol, reduce fusing point, degree of crystallinity, the end carboxyl number of fiber, improved viscosity, elongation at break, the dye uptake of fiber.
Embodiment
A kind of 1, the preparation method of 3-butyleneglycol modified PBT/PET copolymer fibre, the fiber synthesis material is terephthalic acid, butyleneglycol, ethylene glycol and 1, the 3-butyleneglycol, the combination of using tosic acid and two kinds of materials of tin protochloride is as catalyzer, the first step terephthalic acid and dibasic alcohol carry out esterification and form performed polymer, second step be performed polymer under the condition of high temperature high vacuum, carry out polycondensation.
Embodiment
The catalyst solution configuration: catalyzer tosic acid and tin protochloride add the catalyzer batch tank, inject a spot of ethylene glycol, stir, heat, catalyzer is dissolved in 100 ℃ ethylene glycol, ethylene glycol catalyst solution after the dissolving enters thinning tank, inject remaining ethylene glycol, 1,3 butylene glycol and butyleneglycol.Stir the content that catalyzer is measured in the back, finish the configuration of catalyst solution.
Slurry configuration: terephthalic acid is joined in the slurry batch tank in 1.10～1.15 ratio according to the material ratio of dibasic alcohol and terephthalic acid, injecting catalyst solution, add stablizer, matting agent, fire retardant, etherificate inhibitor, through mixing form slurry, the slurry that configures is transported in the esterification device.
The synthetic employing continous way polyester production process of copolymer fibre, the first step esterification is finished through two reaction kettle of the esterification, and polycondensation is finished through prepolymerization reaction still and the poly-reactor of final minification.
| Condition | Reaction kettle of the esterification I | Reaction kettle of the esterification II | The prepolymerization reaction still | Final minification gathers reactor |
| Temperature of reaction/℃ | ??240～250 | ??250～260 | ??260～270 | ??270～280 |
| Reaction pressure/Pa | ??(1.3～1.5)×10 5 | ??60000～70000 | ??2500～3000 | ??50～100 |
| The residence time/min | ??90～100 | ??90～120 | ??50～70 | ??120～150 |
The copolymerization result:
1. the 1,3 butylene glycol addition is an alcohol amount 5%, and the butyleneglycol consumption is an alcohol amount 20%, and the ethylene glycol consumption is an alcohol amount 75%.
| Cationic dyestuff dye uptake (100 ℃) | ??69 |
| Polyester elongation at break/% | ??244 |
2. the 1,3 butylene glycol addition is an alcohol amount 8%, and the butyleneglycol consumption is an alcohol amount 25%, and the ethylene glycol consumption is an alcohol amount 67%.
3. the 1,3 butylene glycol addition is an alcohol amount 10%, and the butyleneglycol consumption is an alcohol amount 30%, and the ethylene glycol consumption is an alcohol amount 60%.
4. the butyleneglycol consumption is an alcohol amount 25%, and the ethylene glycol consumption is an alcohol amount 75%.
| Degree of crystallinity/% | ??23 |
| Cationic dyestuff dye uptake (100 ℃) | ??45 |
| Polyester elongation at break/% | ??138 |
Claims (4)
1.3-the preparation method of butyleneglycol modified PBT PET copolymer fibre, it is characterized in that: the fiber synthesis material is a terephthalic acid, butyleneglycol, ethylene glycol and 1, the 3-butyleneglycol, the combination of using tosic acid and two kinds of materials of tin protochloride is as catalyzer, the first step terephthalic acid and dibasic alcohol carry out esterification and form performed polymer, second step was that performed polymer is under the condition of high temperature high vacuum, carrying out polycondensation, to prepare raw material be terephthalic acid, butyleneglycol, ethylene glycol and 1, the 3-butyleneglycol, 1,3-butyleneglycol addition is an alcohol amount 5～10%, and the butyleneglycol consumption is an alcohol amount 20～30%, and the ethylene glycol consumption is an alcohol amount 75～60%.The material ratio of dibasic alcohol and terephthalic acid is 1.10～1.15.
2. according to claim 1, it is characterized in that: the combination of using tosic acid and two kinds of materials of tin protochloride is as catalyzer, and the tin protochloride consumption is 300 * 10 of an acid amount
-6, the consumption of tosic acid is 100 * 10 of an acid amount
-6
3. according to claim 1, it is characterized in that: fiber will add multiple auxiliary agent in synthetic, comprise stablizer, matting agent, fire retardant, etherificate inhibitor.
A) stablizer trimethyl phosphite 99 2.8～3.0 ‰
B) TITANIUM DIOXIDE DELUSTRANT 1.8～2.0 ‰
C) fire retardant phosphorus flame retardant 2.2～2.5 ‰
D) etherificate inhibitor sodium-acetate 1.3～1.5 ‰
4. according to claim 1, it is characterized in that: the synthetic employing continous way polyester production process of copolymer fibre, the first step esterification is finished through two reaction kettle of the esterification, and polycondensation is finished through prepolymerization reaction still and the poly-reactor of final minification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910102102A CN101824140A (en) | 2009-08-12 | 2009-08-12 | Preparation method of 1,3-butanediol modified PBTPET (Polybutylece Terephthalate Polyethylene Terephthalate) copolymer fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910102102A CN101824140A (en) | 2009-08-12 | 2009-08-12 | Preparation method of 1,3-butanediol modified PBTPET (Polybutylece Terephthalate Polyethylene Terephthalate) copolymer fiber |
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|---|---|
| CN101824140A true CN101824140A (en) | 2010-09-08 |
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| CN200910102102A Pending CN101824140A (en) | 2009-08-12 | 2009-08-12 | Preparation method of 1,3-butanediol modified PBTPET (Polybutylece Terephthalate Polyethylene Terephthalate) copolymer fiber |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329482A (en) * | 2011-06-20 | 2012-01-25 | 江苏鹰翔化纤股份有限公司 | Preparation method of 1, 3-butanediol modified terylene slice |
| CN104073908A (en) * | 2012-08-08 | 2014-10-01 | 江苏德赛化纤有限公司 | Preparation method of multifunctional super-imitated cotton biomass polyester staple fiber |
| CN107313128A (en) * | 2017-08-07 | 2017-11-03 | 太仓荣文合成纤维有限公司 | A kind of PBT fiber fabrication process |
| CN109422868A (en) * | 2017-08-30 | 2019-03-05 | 中国石化仪征化纤有限责任公司 | A kind of production method of high-viscosity polyester |
| CN110802856A (en) * | 2019-11-01 | 2020-02-18 | 兰利军 | Production process of PBT (polybutylene terephthalate) odor-breaking bag |
-
2009
- 2009-08-12 CN CN200910102102A patent/CN101824140A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329482A (en) * | 2011-06-20 | 2012-01-25 | 江苏鹰翔化纤股份有限公司 | Preparation method of 1, 3-butanediol modified terylene slice |
| CN104073908A (en) * | 2012-08-08 | 2014-10-01 | 江苏德赛化纤有限公司 | Preparation method of multifunctional super-imitated cotton biomass polyester staple fiber |
| CN104073908B (en) * | 2012-08-08 | 2016-04-13 | 江苏德赛化纤有限公司 | A kind of preparation method of multi-functional super imitative cotton biomass polyester short fiber dimension |
| CN107313128A (en) * | 2017-08-07 | 2017-11-03 | 太仓荣文合成纤维有限公司 | A kind of PBT fiber fabrication process |
| CN109422868A (en) * | 2017-08-30 | 2019-03-05 | 中国石化仪征化纤有限责任公司 | A kind of production method of high-viscosity polyester |
| CN110802856A (en) * | 2019-11-01 | 2020-02-18 | 兰利军 | Production process of PBT (polybutylene terephthalate) odor-breaking bag |
| CN110802856B (en) * | 2019-11-01 | 2022-09-23 | 兰利军 | Production process of PBT (polybutylene terephthalate) odor-blocking bag |
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