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Preparation method of modified polyester for high-heat-resistant bottles

A technology of modified polyester and high heat resistance, applied in the field of polyester modification, can solve the problems of low polyester yield, low reactivity, difficult production, etc., achieves an increase in glass transition temperature, and has a wide range of applications , good effect of esterification

Inactive Publication Date: 2019-04-30
SINOPEC YIZHENG CHEM FIBER +1
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Problems solved by technology

However, these two modified monomers are all secondary carbon-based alcohols, that is, secondary alcohols, which have a large steric hindrance, and the activity of their hydroxyl groups is weaker than that of ethylene glycol. Therefore, a considerable amount of monomers do not participate in the polymerization during the polycondensation process. Being pumped into the vacuum system, the utilization efficiency of the monomer is relatively low
At the same time, since these two monomers are secondary carbon alcohols and have low reactivity, it is difficult to use these two monomers to carry out the polymerization process of modified polyester, and the production is difficult.
[0005] Chinese patent CN102264794A discloses the use of isobehenyl alcohol to prepare heat-resistant polyester. As mentioned above, the isobehenyl alcohol used is a secondary carbon-based alcohol, and the monomer utilization efficiency is low
Chinese patent CN101679619 discloses the use of 2,2,4,4-tetramethyl-1,3-cyclobutanediol and 1,4-cyclohexanedimethanol to prepare heat-resistant polyester. 2,2,4,4-Tetramethyl-1,3 cyclobutanediol is a secondary carbon alcohol with low reactivity
[0006] U.S. Patent US2945008 uses titanium catalysts and spiro diols to prepare heat-resistant polyesters. However, titanium-based catalysts are hydrolyzed and easily react with water generated in the reaction system to form hydrolyzate, which not only reduces the catalytic efficiency, but also easily deposits the hydrolyzate. Blockage of pipelines brings inconvenience to production
[0007] Chinese patent CN1424338 adopts PTA method, does not use esterification catalyst, prepares heat-resistant polyester with spirocyclic diol, because this method does not use esterification catalyst, so the reaction activity is low, and the output rate of polyester is low
Chinese patent CN102257031 uses a titanium catalyst as an esterification catalyst, or a tin compound as an esterification and polycondensation catalyst at the same time, and spirodiol is used to prepare heat-resistant polyester. As mentioned above, the titanium-based catalyst used in it has hydrolysis phenomenon, which is easy to mix with the reaction system. The water generated in the reaction produces hydrolysis products, which reduces the catalytic efficiency

Method used

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  • Preparation method of modified polyester for high-heat-resistant bottles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 350 grams of terephthalic acid, 65 grams of spiroglycol, 182 grams of ethylene glycol, and 0.0175 monobutyltin oxide into a 2L reactor. The esterification temperature is 200°C-260°C, and the esterification pressure (gauge pressure) is 2.5 Esterification at MPa, when the water output reaches the theoretical value, end the esterification, release to normal pressure, add 0.0261 grams of phosphoric acid, continue stirring for 10 minutes, add 0.13 grams of ethylene glycol antimony, gradually increase the temperature and transfer to the low vacuum stage, low After the vacuum time is about 45 minutes, it enters the high vacuum polycondensation stage (vacuum <100Pa), the polycondensation temperature is 270°C-290°C, and the material is discharged when the stirring power reaches the rated value. The glass transition temperature of the synthesized modified polyester is 100°C, and the intrinsic viscosity 0.851dL / g, terminal carboxyl group 22mol / t, color value (L / a / b) 87.3 / -1.1 / 4...

Embodiment 2

[0028] Add 350 grams of terephthalic acid, 90 grams of spiroglycol, 229 grams of ethylene glycol, 0.070 monobutyltin oxide into a 2L reaction kettle, the esterification temperature is 200°C-260°C, and the esterification pressure (gauge pressure) is 2.5 Esterification at MPa, when the water output reaches the theoretical value, end the esterification, release to normal pressure, add 0.0175 grams of phosphoric acid, continue to stir for 10 minutes, add 0.13 grams of ethylene glycol antimony, gradually increase the temperature and transfer to the low vacuum stage, After about 45 minutes of vacuum time, it enters the stage of high vacuum polycondensation (vacuum <100Pa), the polycondensation temperature is 270°C-290°C, and the material is discharged when the stirring power reaches the rated value. The glass transition temperature of the synthesized modified polyester is 108°C, and the intrinsic viscosity 0.821dL / g, terminal carboxyl group 26mol / t, color value (L / a / b) 88.3 / -1.2 / 5.2,...

Embodiment 3

[0030] Add 350 grams of terephthalic acid, 45 grams of spiroglycol, 212 grams of ethylene glycol, and 0.044 monobutyltin oxide into a 2L reaction kettle. Esterification at MPa, when the water output reaches the theoretical value, end the esterification, release to normal pressure, add 0.035 grams of phosphoric acid, continue to stir for 10 minutes, add 0.13 grams of ethylene glycol antimony, gradually increase the temperature and transfer to the low vacuum stage, low After a vacuum time of about 45 minutes, it enters the stage of high vacuum polycondensation (vacuum <100Pa), the polycondensation temperature is 270°C-290°C, and the material is discharged when the stirring power reaches the rated value. The glass transition temperature of the synthesized modified polyester is 95°C, and the intrinsic viscosity 0.881dL / g, carboxyl terminal 20mol / t, color value (L / a / b) 88.3 / -1.8 / 2.6, the bottle produced by the polyester prepared in this experiment will not deform when filled with ho...

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Abstract

The invention provides a preparation method of modified polyester for high-heat-resistant bottles. The preparation method comprises: using terephthalic acid and ethylene glycol as main reaction raw materials, adding modified monomers 1,4-cyclohexane dimethanol and spiro diol, and carrying out direct esterification by using a tin / phosphorus / antimony composite catalyst to prepare the modified polyester. According to the present invention, the tin compound is added as the esterification catalyst at the esterification stage, the phosphorus compound is added to passivate the tin catalyst after theesterification is completed, and the antimony-based catalyst is added as the condensation polymerization catalyst, such that the catalysis effect of the tin compound to the esterification reaction can be ensured, and the problems that the tin catalyst as the condensation polymerization catalyst can yellow the polyester to cause the poor thermal stability of the product can be avoided.

Description

technical field [0001] The invention relates to the modification of polyester, in particular to the modification of polyethylene terephthalate (PET), in particular to a method for preparing the modified polyester for high heat-resistant bottles. Background technique [0002] Polyester, a general term for polymers obtained by polycondensation of polyols and polybasic acids, mainly including polyethylene terephthalate (PET), polybutylene terephthalate (PBT) and polyarylate (PAR) . Because PET has the characteristics of electrical insulation, creep resistance, fatigue resistance, friction resistance, high dimensional stability, and good physical and mechanical properties, in addition to its industrial application in the fiber field, its application has now been extended to non-fiber fields. Bottles, films, engineering plastics, etc. [0003] The glass transition temperature of conventional PET is only 80°C, and its heat resistance is poor. For fields that require certain heat...

Claims

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Application Information

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IPC IPC(8): C08G63/672C08G63/85C08G63/86
CPCC08G63/672C08G63/85C08G63/866
Inventor 戴志彬夏峰伟周倩常玉王余伟
Owner SINOPEC YIZHENG CHEM FIBER
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