CN101659742A - Polymerization stabilizing method in polyethylene glycol terephthalate synthesis process - Google Patents
Polymerization stabilizing method in polyethylene glycol terephthalate synthesis process Download PDFInfo
- Publication number
- CN101659742A CN101659742A CN200910144622A CN200910144622A CN101659742A CN 101659742 A CN101659742 A CN 101659742A CN 200910144622 A CN200910144622 A CN 200910144622A CN 200910144622 A CN200910144622 A CN 200910144622A CN 101659742 A CN101659742 A CN 101659742A
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- CN
- China
- Prior art keywords
- terephthalic acid
- polymerization
- polyethylene terephthalate
- stablizer
- addition
- 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
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 13
- 230000000087 stabilizing effect Effects 0.000 title claims abstract description 7
- 239000002202 Polyethylene glycol Substances 0.000 title abstract 3
- 229920001223 polyethylene glycol Polymers 0.000 title abstract 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 title abstract 3
- 230000015572 biosynthetic process Effects 0.000 title description 5
- 238000003786 synthesis reaction Methods 0.000 title description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 30
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 238000005886 esterification reaction Methods 0.000 claims abstract description 11
- 230000032050 esterification Effects 0.000 claims abstract description 10
- 230000009977 dual effect Effects 0.000 claims abstract description 9
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims abstract description 9
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- -1 polyethylene terephthalate Polymers 0.000 claims description 14
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 14
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 8
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 claims description 6
- 229920000728 polyester Polymers 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 230000000593 degrading effect Effects 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
Landscapes
- Polyesters Or Polycarbonates (AREA)
Abstract
A method for stabilizing the polymerization of polyethylene glycol terephthalate is disclosed, which is applied to the polymerization process of fiber-grade polyethylene glycol terephthalate.A slurry is prepared from terephthalic acid and glycol as polycondensation raw materials, tetrabutyl titanate as dual catalyst and p-toluenesulfonic acid, and then the slurry is sent to an esterification reactor for esterification reaction and then pre-polycondensation reaction.
Description
Technical field
The present invention relates to the polymerization stabilizing method in a kind of polyethylene terephthalate synthesis technique, belong to the synthetic middle auxiliary agent Application Areas of polyester.
Background technology
In the synthesis technique of polyethylene terephthalate, stablizer and single catalyzer are added into reaction kettle of the esterification, interpolation at esterification stage stablizer can make catalyst deactivation, reduce catalytic activity, cause the polyethylene terephthalate generated time to be extended virtually, the addition that reaches certain synthetic effect catalyzer increases, and the polyethylene terephthalate polyester catalyst content that finally obtains is higher, and production cost is increased.
Summary of the invention
The objective of the invention is to solve the problem in the above polyethylene terephthalate synthesis technique, a kind of low cost is provided, short period of time, polyethylene terephthalate polymerization stabilizing method efficiently.
The present invention relates to a kind of polyethylene terephthalate polymerization stabilizing method, be applied in the polymerization technique of fibre-grade polyethylene terephthalate, polycondensation raw material terephthalic acid and ethylene glycol at first are configured to slurry with dual catalyst tetrabutyl titanate and tosic acid, be transported to and carry out esterification in the reaction kettle of the esterification, carry out prepolymerization reaction then, add the stablizer trimethyl phosphite 99 in the poly-stage of final minification, play the effect of stablizing the polycondensation result, prevent that polyester from degrading under hot conditions.
Polyethylene terephthalate uses dual catalyst in polymerization, wherein the tetrabutyl titanate 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.
Stablizer added in the poly-stage of final minification, and the stablizer that uses is trimethyl phosphite 99, and addition is 1/1000 of a terephthalic acid molar weight.
Progressive meaning of the present invention is:
1. use dual catalyst tetrabutyl titanate and tosic acid in the polymerization, improved catalytic effect, reduce generated time.
2. be chosen in the poly-stage interpolation of final minification stablizer, addition manner is reasonable, reduces catalyst consumption.
Embodiment
The present invention is applied in the continuous condensed production equipment of polyethylene terephthalate, polycondensation raw material terephthalic acid and ethylene glycol at first are configured to slurry with dual catalyst tetrabutyl titanate and tosic acid, be transported to and carry out esterification in the reaction kettle of the esterification, carry out prepolymerization reaction then, add the stablizer trimethyl phosphite 99 in the poly-stage of final minification, play the effect of stablizing the polycondensation result, prevent that polyester from degrading under hot conditions.
Embodiment
The material ratio of ethylene glycol and terephthalic acid is 1.10～1.15, and dual catalyst tetrabutyl titanate 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.Dual catalyst at first is dissolved in a small amount of 80 ℃ ethylene glycol and makes ethylene glycol solution, be mixed with slurry by a certain percentage with terephthalic acid then, 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 terephthalic acid molar weight.
Claims (3)
1. polyethylene terephthalate polymerization stabilizing method, be applied in the polymerization technique of fibre-grade polyethylene terephthalate, it is characterized in that: polycondensation raw material terephthalic acid and ethylene glycol at first are configured to slurry with dual catalyst tetrabutyl titanate and tosic acid, be transported to and carry out esterification in the reaction kettle of the esterification, carry out prepolymerization reaction then, add the stablizer trimethyl phosphite 99 in the poly-stage of final minification, play the effect of stablizing the polycondensation result, prevent that polyester from degrading under hot conditions.
2. according to claim 1, it is characterized in that: polyethylene terephthalate uses dual catalyst in polymerization, wherein the tetrabutyl titanate 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: stablizer added in the poly-stage of final minification, and the stablizer that uses is trimethyl phosphite 99, and addition is 1/1000 of a terephthalic acid molar weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910144622A CN101659742A (en) | 2009-08-24 | 2009-08-24 | Polymerization stabilizing method in polyethylene glycol terephthalate synthesis process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910144622A CN101659742A (en) | 2009-08-24 | 2009-08-24 | Polymerization stabilizing method in polyethylene glycol terephthalate synthesis process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101659742A true CN101659742A (en) | 2010-03-03 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910144622A Pending CN101659742A (en) | 2009-08-24 | 2009-08-24 | Polymerization stabilizing method in polyethylene glycol terephthalate synthesis process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101659742A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838447A (en) * | 2010-05-25 | 2010-09-22 | 南通华盛新材料股份有限公司 | Fully-degradable polyester/inorganic nanoparticle composite material and method for preparing same |
| CN102796247A (en) * | 2011-05-24 | 2012-11-28 | 江苏鹰翔化纤股份有限公司 | Method for preparing 2,6-naphthalene diacid modified polyester chips |
| CN102796354A (en) * | 2011-05-24 | 2012-11-28 | 江苏鹰翔化纤股份有限公司 | Method for preparing 2,3-butanediol modified polyester chips |
| CN102796353A (en) * | 2011-05-24 | 2012-11-28 | 江苏鹰翔化纤股份有限公司 | Method for preparing succinic acid modified polyester chips |
| CN102796248A (en) * | 2011-05-24 | 2012-11-28 | 江苏鹰翔化纤股份有限公司 | Method for preparing adipic acid modified polyester slice |
| CN107629200A (en) * | 2017-10-25 | 2018-01-26 | 宝鸡市永盛泰钛业有限公司 | A kind of method for manufacturing HMW polyethylene terephthalate |
-
2009
- 2009-08-24 CN CN200910144622A patent/CN101659742A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838447A (en) * | 2010-05-25 | 2010-09-22 | 南通华盛新材料股份有限公司 | Fully-degradable polyester/inorganic nanoparticle composite material and method for preparing same |
| CN102796247A (en) * | 2011-05-24 | 2012-11-28 | 江苏鹰翔化纤股份有限公司 | Method for preparing 2,6-naphthalene diacid modified polyester chips |
| CN102796354A (en) * | 2011-05-24 | 2012-11-28 | 江苏鹰翔化纤股份有限公司 | Method for preparing 2,3-butanediol modified polyester chips |
| CN102796353A (en) * | 2011-05-24 | 2012-11-28 | 江苏鹰翔化纤股份有限公司 | Method for preparing succinic acid modified polyester chips |
| CN102796248A (en) * | 2011-05-24 | 2012-11-28 | 江苏鹰翔化纤股份有限公司 | Method for preparing adipic acid modified polyester slice |
| CN107629200A (en) * | 2017-10-25 | 2018-01-26 | 宝鸡市永盛泰钛业有限公司 | A kind of method for manufacturing HMW polyethylene terephthalate |
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| 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: 20100303 |