CN101709110A - Novel polymerizing catalysis stable method of polyester - Google Patents
Novel polymerizing catalysis stable method of polyester Download PDFInfo
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- CN101709110A CN101709110A CN200910144637A CN200910144637A CN101709110A CN 101709110 A CN101709110 A CN 101709110A CN 200910144637 A CN200910144637 A CN 200910144637A CN 200910144637 A CN200910144637 A CN 200910144637A CN 101709110 A CN101709110 A CN 101709110A
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Abstract
The invention relates to a polymerizing catalysis stable method of polyester, which is characterized by comprising the following steps: in the production process of fiber-grade polyester, preparing slurry by dibasic acid and dibastic alcohol serving as polycondensation raw materials and bi-catalyst titanium isopropoxide and paratoluenesulfonic acid in a slurry pot firstly; conveying the slurry to an esterification reaction kettle to perform an esterification reaction and then to perform a pre-polycondensation reaction; and adding phosphoric acid serving as a stabilizer into the esterification reaction kettle in a final polycondensation phase. The polymerizing catalysis stable method can reduce catalyst dosage, shorten synthesis time, improve the stability of the polyester and reduce synthesis cost.
Description
Technical field
The present invention relates to a kind of polymerizing catalysis stable method of polyester, belong to the Application Areas of the synthetic middle auxiliary agent of polyester.
Background technology
In the synthesis technique of polyester, the use of titanium catalyst in recent years studies show that titanium catalyst has very high catalytic activity, but the use of titanium catalyst can be deepened the color of polyester; The many reaction kettle of the esterification that when beginning, add of stablizer, participate in polyester each stage of synthetic, but stablizer can make catalyst deactivation in the interpolation in esterification stage, reduce catalytic activity, cause the polyester generated time long, catalyst levels is big, and catalyst content is higher in the pet copolyester that finally obtains, the production cost height.
Summary of the invention
The objective of the invention is to solve the color that the use of titanium catalyst in the synthesis technique can be deepened polyester, stablizer makes the problem of catalyst deactivation in the interpolation in esterification stage, provides a kind of low cost, short period of time, polymerizing catalysis stable method of polyester efficiently.
The present invention relates to a kind of polymerizing catalysis stable method of polyester, it is characterized in that: in the production technique of fiber-grade polyester, polycondensation raw material diprotic acid and dibasic alcohol at first are configured to slurry with dual catalyst titanium isopropoxide and tosic acid in slurry tank, after be transported to and carry out esterification in the reaction kettle of the esterification, carry out prepolymerization reaction then, add stablizer phosphoric acid in the poly-stage of final minification.This polymerizing catalysis stable method can reduce the catalyst levels of polyester, shortens generated time, improves the stability of polyester, reduces synthetic cost.
Polyester uses dual catalyst in polymerization, wherein Primary Catalysts titanium isopropoxide addition is 1/600 of a diprotic acid molar weight, mainly play katalysis in polycondensation phase, the addition of tosic acid is that 1/800 of diprotic acid molar weight mainly works in Esterification Stage.
Dual catalyst titanium isopropoxide and tosic acid and raw material terephthalic acid, ethylene glycol enters reaction kettle of the esterification together, and stablizer added in the poly-stage of final minification, and the stablizer that uses is phosphoric acid, and addition is 1/1000 of a diprotic acid molar weight.
Progressive meaning of the present invention is:
1. the use of tosic acid can effectively reduce the yellow degree of polyester, reduces the existence of small molecular weight in the polyester.
2. be chosen in the poly-stage interpolation of final minification stablizer, addition manner is more reasonable, can effectively avoid the passivation of stablizer to catalyzer, reduces catalyst consumption.
3. pass through the change of the using method of dual catalyst, stablizer, improved the quality of polyester, because the reduction of additive amount is improved the spinning property of follow-up trevira, service life of equipment prolongs, and has also reduced the content of the metal ion in the melt simultaneously.
Embodiment
The present invention is applied in the continuous condensed production equipment of polyester, in the production technique of fiber-grade polyester, the polycondensation raw material at first is configured to slurry with dual catalyst titanium isopropoxide and tosic acid to diprotic acid and dibasic alcohol in slurry tank, after be transported to and carry out esterification in the reaction kettle of the esterification, carry out prepolymerization reaction then, add stablizer phosphoric acid in the poly-stage of final minification.
Embodiment
The material ratio of dibasic alcohol and diprotic acid is 1.10～1.15, and dual catalyst titanium isopropoxide addition is 1/600 of a terephthalic acid molar weight, and the addition of tosic acid is to 1/800 of diprotic acid molar weight.Dual catalyst at first is dissolved in a small amount of 80 ℃ dibasic alcohol and makes alcoholic solution, be mixed with slurry by a certain percentage then with to diprotic acid, enter reaction kettle of the esterification together, generate prepolymer through over-churning and precondensation, stablizer enters reactor in the poly-stage of final minification with prepolymer and finishes polyreaction, the stablizer that uses is trimethyl phosphite 99, and addition is 1/1000 of a diprotic acid molar weight.At the Esterification Stage titanium isopropoxide and to the acting in conjunction of toluene sulphur, can effectively reduce esterification time, improve esterification yield, enter precondensation stage, tosic acid can steam under high vacuum condition, thereby can not aggravate high molecular degraded.Stablizer mainly suppresses the thermal destruction of high molecular weight polyesters, mainly works in the poly-stage of final minification.
Claims (3)
1. polymerizing catalysis stable method of polyester, it is characterized in that: in the production technique of fiber-grade polyester, polycondensation raw material diprotic acid and dibasic alcohol at first are configured to slurry with dual catalyst titanium isopropoxide and tosic acid in slurry tank, after be transported to and carry out esterification in the reaction kettle of the esterification, carry out prepolymerization reaction then, add stablizer phosphoric acid in the poly-stage of final minification.
2. according to claim 1, it is characterized in that: polyester uses dual catalyst in polymerization, and wherein Primary Catalysts titanium isopropoxide addition is 1/600 of a terephthalic acid molar weight, and the addition of tosic acid is 1/800 of a terephthalic acid molar weight.
3. according to claim 1, it is characterized in that: the present invention selects stablizer to add in the poly-stage of final minification, and the stablizer that uses is phosphoric acid, and addition is 1/1000 of a terephthalic acid molar weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910144637A CN101709110A (en) | 2009-08-24 | 2009-08-24 | Novel polymerizing catalysis stable method of polyester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910144637A CN101709110A (en) | 2009-08-24 | 2009-08-24 | Novel polymerizing catalysis stable method of polyester |
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| Publication Number | Publication Date |
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| CN101709110A true CN101709110A (en) | 2010-05-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200910144637A Pending CN101709110A (en) | 2009-08-24 | 2009-08-24 | Novel polymerizing catalysis stable method of polyester |
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| CN (1) | CN101709110A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104341586A (en) * | 2013-08-06 | 2015-02-11 | 新光合成纤维股份有限公司 | Process for preparing copolyester |
| CN110092897A (en) * | 2019-03-28 | 2019-08-06 | 北京化工大学 | The method that binary composite catalyst catalyzes and synthesizes polyether ester |
| CN115677988A (en) * | 2022-11-23 | 2023-02-03 | 大连理工大学 | In-situ preparation method of polybutylene oxalate |
| CN115785424A (en) * | 2022-07-04 | 2023-03-14 | 新倍斯(杭州)材料科技有限公司 | Hydrolysis-resistant composite titanium catalyst, preparation method and preparation method of high-molecular-weight oxalic acid-based polyester |
-
2009
- 2009-08-24 CN CN200910144637A patent/CN101709110A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104341586A (en) * | 2013-08-06 | 2015-02-11 | 新光合成纤维股份有限公司 | Process for preparing copolyester |
| CN104341586B (en) * | 2013-08-06 | 2016-05-04 | 新光合成纤维股份有限公司 | Process for preparing copolyester |
| CN110092897A (en) * | 2019-03-28 | 2019-08-06 | 北京化工大学 | The method that binary composite catalyst catalyzes and synthesizes polyether ester |
| CN110092897B (en) * | 2019-03-28 | 2021-03-26 | 北京化工大学 | Method for synthesizing polyether ester by catalysis of binary composite catalyst |
| CN115785424A (en) * | 2022-07-04 | 2023-03-14 | 新倍斯(杭州)材料科技有限公司 | Hydrolysis-resistant composite titanium catalyst, preparation method and preparation method of high-molecular-weight oxalic acid-based polyester |
| CN115677988A (en) * | 2022-11-23 | 2023-02-03 | 大连理工大学 | In-situ preparation method of polybutylene oxalate |
| CN115677988B (en) * | 2022-11-23 | 2024-02-20 | 大连理工大学 | In-situ preparation method of polybutylene oxalate |
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Open date: 20100519 |