CN101831058A - 1,2-propylene glycol modified PTTPET (Polytrimethylene Terephthalate Polyethylene Terephthalate) copolymer fiber - Google Patents
1,2-propylene glycol modified PTTPET (Polytrimethylene Terephthalate Polyethylene Terephthalate) copolymer fiber Download PDFInfo
- Publication number
- CN101831058A CN101831058A CN 200910102103 CN200910102103A CN101831058A CN 101831058 A CN101831058 A CN 101831058A CN 200910102103 CN200910102103 CN 200910102103 CN 200910102103 A CN200910102103 A CN 200910102103A CN 101831058 A CN101831058 A CN 101831058A
- Authority
- CN
- China
- Prior art keywords
- propylene glycol
- fiber
- acid
- terephthalic acid
- ammediol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention relates to a 1,2-propylene glycol modified PTTPET (polytrimethylene terephthalate polyethylene terephthalate) copolymer fiber which is characterized in that the synthesis raw materials of the fiber comprise terephthalic acid, ethylene glycol, 1,3-propylene glycol and 1,2-propylene glycol; the composition of two substances of sulfamic acid and isopropoxy titanium is used as a catalyst; and in the preparation of the fiber, the first step is to carry out an esterification reaction on the terephthalic acid and dihydric alcohols to form a prepolymer, and the second step is to carry out a condensation polymerization reaction on the prepolymer in the presence of high temperature and high vacuum. Through the introduction of methyl on the upside of the main chain of the PTT/PET copolymer fiber, the crystallinity of the PTT/PET copolymer fiber and the symmetry of the molecular main chain are reduced, and the dying capacity and the properties of the polyester fiber are improved.
Description
Technical field
The present invention relates to a kind of modified copolymer fiber preparation method, particularly 1, the preparation method of the propylene glycol modified PET/PTT copolymer fibre of 2-belongs to the synthetic field of fiber.
Background technology
Polybutylene terephthalate in man-made fiber (PET) and propylene glycol ester terephthalate (PTT) structural similitude obtain through terephthalic acid and the polymerization of straight chain binary aliphatic alcohol.Polyester is regular owing to macromolecular chain structure, the molecular chain rigid structure, and easily crystallization lacks hydrophilic radical and easily causes dyeing behavior poor.Though make moderate progress on the PET/PTT copolymer fibre structure, in whole high polymer main chain, present linear chain structure, the improved performance of copolymer fibre is less.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, the 2-propylene glycol carries out modification to the PET/PTT copolymer fibre, by the introducing of pending methyl group on PET/PTT copolymer fibre main chain, reduce the crystallinity of PET/PTT copolymer fibre, the symmetry of molecular backbone chain, the colouring power of raising polyester improves the trevira performance.
The present invention relates to a kind of 1, the preparation method of the propylene glycol modified PET/PTT copolymer fibre of 2-is characterized in that: the fiber synthesis material is terephthalic acid, ethylene glycol, 1, ammediol and 1, the 2-propylene glycol, the combination of using thionamic acid and two kinds of materials of titanium isopropoxide 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, ethylene glycol, 1, ammediol and 1, and the 2-propylene glycol, 1,2-propylene glycol addition is an alcohol amount 5～10%, and the ethylene glycol consumption is an alcohol amount 20～30%, 1, and the ammediol consumption is an alcohol amount 75～60%.The material ratio of dibasic alcohol and terephthalic acid is 1.10～1.15.
Use thionamic acid and two kinds of combinations of substances of titanium isopropoxide as catalyzer, the titanium isopropoxide consumption is 350 * 10 of an acid amount
-6, measuring with amino of sulfonic acid is 150 * 10 of acid amount
-6
Fiber will add multiple auxiliary agent in synthetic, comprise stablizer, matting agent, fire retardant, etherificate inhibitor.
Stablizer phosphoric acid 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 production technique 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/℃ | ??200～210 | ??200～210 | ??230～240 | ??240～250 |
| Reaction pressure/Pa | ??(1.2～1.3)×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. thionamic acid and two kinds of materials of titanium isopropoxide use that combines during the copolymer fibre polymerization improves catalytic effect, reduces catalyst levels.
2. by on PET/PTT copolymer fibre main chain, introducing a shape 1,2-propylene glycol, fusing point, degree of crystallinity, the end carboxyl number of reduction fiber.Viscosity, elongation at break, the dye uptake of fiber have been improved.
Embodiment
A kind of 1, the preparation method of the propylene glycol modified PET/PTT copolymer fibre of 2-, the fiber synthesis material is terephthalic acid, ethylene glycol, 1, ammediol and 1,2-propylene glycol, the combination of using thionamic acid and two kinds of materials of titanium isopropoxide are as catalyzer, and the first step terephthalic acid and dibasic alcohol carry out esterification and form performed polymer, second the step be performed polymer under the condition of high temperature high vacuum, carry out polycondensation.
Embodiment
The catalyst solution configuration, catalyzer thionamic acid and titanium isopropoxide add the catalyzer batch tank, inject a spot of 1, ammediol stirs, heating, make catalyzer 80 ℃ 1, dissolve in the ammediol, after the dissolving 1, the ammediol catalyst solution enters thinning tank, injects remaining 1, ammediol, 1,2-propylene glycol and ethylene glycol stir the content that catalyzer is measured in the back, finish the configuration of catalyst solution.
The 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 | Esterification I | Esterification II | Precondensation | Final minification is poly- |
| Temperature of reaction/℃ | ??200～210 | ??200～210 | ??230～240 | ??240～250 |
| Reaction pressure/Pa | ??(1.2～1.3)×10 5 | ??60000～70000 | ??2500～3000 | ??50～100 |
| The residence time/min | ??90～100 | ??90～120 | ??50～70 | ??120～150 |
The copolymerization result:
1. 1,2-propylene glycol addition is an alcohol amount 5%, and the ethylene glycol consumption be an alcohol amount 20%, 1, and the ammediol consumption be purely to measure 75%.
2. 1,2-propylene glycol addition is an alcohol amount 8%, and the ethylene glycol consumption be an alcohol amount 25%, 1, and the ammediol consumption be purely to measure 67%.
3. 1,2-propylene glycol addition is an alcohol amount 10%, and the ethylene glycol consumption be an alcohol amount 30%, 1, and the ammediol consumption be purely to measure 60%.
4. the ethylene glycol consumption is an alcohol amount 25%, 1, and the ammediol consumption is an alcohol amount 75%.
Claims (4)
1.2-the preparation method of propylene glycol modified PTTPET (Polytrimethylene Terephthalate Polyethylene Terephthalate) copolymer fiber, it is characterized in that: the fiber synthesis material is a terephthalic acid, ethylene glycol, 1, ammediol and 1, the 2-propylene glycol, the combination of using thionamic acid and two kinds of materials of titanium isopropoxide 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, carrying out polycondensation, to prepare raw material be terephthalic acid, ethylene glycol, 1, ammediol and 1, the 2-propylene glycol, 1,2-propylene glycol addition is an alcohol amount 5～10%, and the ethylene glycol consumption is an alcohol amount 20～30%, 1, the ammediol 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 thionamic acid and two kinds of materials of titanium isopropoxide is as catalyzer, and the titanium isopropoxide consumption is 350 * 10 of an acid amount
-6, measuring with amino of sulfonic acid is 150 * 10 of 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.
Stablizer phosphoric acid 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 ‰
4. according to claim 1, it is characterized in that: the synthetic employing continous way production technique 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 |
|---|---|---|---|
| CN 200910102103 CN101831058A (en) | 2009-08-12 | 2009-08-12 | 1,2-propylene glycol modified PTTPET (Polytrimethylene Terephthalate Polyethylene Terephthalate) copolymer fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910102103 CN101831058A (en) | 2009-08-12 | 2009-08-12 | 1,2-propylene glycol modified PTTPET (Polytrimethylene Terephthalate Polyethylene Terephthalate) copolymer fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101831058A true CN101831058A (en) | 2010-09-15 |
Family
ID=42715292
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910102103 Pending CN101831058A (en) | 2009-08-12 | 2009-08-12 | 1,2-propylene glycol modified PTTPET (Polytrimethylene Terephthalate Polyethylene Terephthalate) copolymer fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101831058A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102330170A (en) * | 2011-05-20 | 2012-01-25 | 江苏鹰翔化纤股份有限公司 | 1,2-propylene glycol-modified terylene pre-oriented yarn |
| CN102329420A (en) * | 2011-06-20 | 2012-01-25 | 江苏鹰翔化纤股份有限公司 | Preparation method of 1,2-propanediol modified polyester chips |
| CN106120022A (en) * | 2016-07-19 | 2016-11-16 | 林启东 | A kind of high-elastic flame-resistant terylene |
| CN107746457A (en) * | 2017-10-19 | 2018-03-02 | 浙江恒逸高新材料有限公司 | A kind of preparation method of PET copolyesters |
-
2009
- 2009-08-12 CN CN 200910102103 patent/CN101831058A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102330170A (en) * | 2011-05-20 | 2012-01-25 | 江苏鹰翔化纤股份有限公司 | 1,2-propylene glycol-modified terylene pre-oriented yarn |
| CN102329420A (en) * | 2011-06-20 | 2012-01-25 | 江苏鹰翔化纤股份有限公司 | Preparation method of 1,2-propanediol modified polyester chips |
| CN106120022A (en) * | 2016-07-19 | 2016-11-16 | 林启东 | A kind of high-elastic flame-resistant terylene |
| CN107746457A (en) * | 2017-10-19 | 2018-03-02 | 浙江恒逸高新材料有限公司 | A kind of preparation method of PET copolyesters |
| CN107746457B (en) * | 2017-10-19 | 2020-10-27 | 浙江恒逸高新材料有限公司 | Preparation method of PET copolyester |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104258795B (en) | Exchange reaction system, the modified poly ester production system comprising it and modified poly ester production method | |
| CN107936237B (en) | Bio-based degradable polyester fiber and preparation method thereof | |
| CN101831058A (en) | 1,2-propylene glycol modified PTTPET (Polytrimethylene Terephthalate Polyethylene Terephthalate) copolymer fiber | |
| CN101824140A (en) | Preparation method of 1,3-butanediol modified PBTPET (Polybutylece Terephthalate Polyethylene Terephthalate) copolymer fiber | |
| CN102086261B (en) | Preparation method of polyol copolyester | |
| CN108003332B (en) | Easily hydrolyzed polyester and synthesis method thereof | |
| CN107118339A (en) | A kind of continuous method for preparing modified poly ester | |
| CN110938197A (en) | Preparation method of copolyester containing sodium sulfonate group | |
| CN103665350B (en) | The preparation technology of a kind of modified copolyester section and fiber | |
| CN101671432A (en) | 1, 2-propylene glycol modified polyethylene glycol terephthalate | |
| CN103628173A (en) | Preparation method of high-hydrophilicity flame-retardant polyester fiber | |
| CN115806661B (en) | Method for preparing high molecular weight acidic dyeable block copolyesters by liquid phase polycondensation | |
| CN111101226A (en) | Bio-based degradable polyester fiber and preparation method thereof | |
| CN101831057A (en) | 1,3-butanediol modified PBTPTT (polybutylece terephthalate polytrimethylene terephthalate) copolymer fiber | |
| CN101928383A (en) | 1,2-propylene glycol modified PBT PTT (Poly Butylenes Terephthalate Polytrimethylene Terephthalate) copolymer fiber | |
| CN103910981B (en) | A kind of branched chain type degradable hydrophilic polyester master particle and preparation method thereof | |
| US10961641B2 (en) | Feather-like polyester fiber and preparing method thereof | |
| CN101928384A (en) | 1,2-propylene glycol modified PBTPET (Poly Butylenes Terephthalate Polyethylene Terephthalate) copolymer fiber | |
| KR101792080B1 (en) | Manufacturing method of elution type knitted fabric | |
| CN101660214A (en) | Preparation method of 1, 5-pentanediol modified PET/PTT (polyethylene terephthalate/polytrimethylene terephthalate) copolymer fiber | |
| CN103102647B (en) | Preparation method of polyester film with high heat shrinkage | |
| CN102977347B (en) | Continuous polymerization method of polytrimethylene terephthalate copolymer | |
| CN101693761A (en) | Method for preparing 1,2-propylene glycol modified polybutylene terephthalate | |
| KR20120078211A (en) | Water soluble polyester composite and preparing thereof | |
| CN101643946B (en) | Polyethylene 1, 2-propylene glycol fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20100915 |