Modified polyester, preparation method thereof, and modified polyester film preparation method

A modified polyester and polyester technology, applied in the field of polyester, can solve the problems of weak hydroxyl activity, low reactivity, difficult polymerization of modified polyester, etc., and achieve fast polymerization speed, good esterification effect, and not easy to evaporate Effect

Inactive Publication Date: 2019-11-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these two monomers are secondary carbon-based alcohols, that is, secondary alcohols, which have large steric hindrance, and the activity of their hydroxyl groups is weaker than that of ethylene glycol. Therefore, during the polycondensation process, a considerable amount of monomers do not participate in polymerization and are extracted In the vacuum system, the utilization efficiency of the monomer is relatively low
At the same time, because these two monomers are secondary carbon alcohols, the reactivity is low, the polymerization of the modified polyester of these two monomers is relatively difficult, and the production is difficult.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: 350 grams of terephthalic acid, 130 grams of spiroglycol, 22 grams of NPG, 170 grams of ethylene glycol, 0.0175 grams of monobutyltin oxide were added to a 2L reactor, and the esterification temperature was 200°C to 260°C. Esterification under the esterification pressure (gauge pressure) of 2.5 MPa. When the water output reaches the theoretical value, the esterification is terminated, released to normal pressure, 0.0261 g of phosphoric acid is added, and stirring is continued for 10 minutes. After adding 0.13 g of ethylene glycol antimony, gradually Heating up and turning into low vacuum stage. After low vacuum time is about 45 minutes, it enters high vacuum polycondensation stage (vacuum <100Pa), polycondensation temperature is 270℃~290℃, and the material is discharged when the stirring power reaches the rated value. The synthesized modified polyester glass The transition temperature is 100.3°C, the intrinsic viscosity is 0.762dL / g, the carboxyl group is 38mo...

Embodiment 2

[0026] Example 2: 350 grams of terephthalic acid, 160 grams of spiroglycol, 19 grams of NPG, 160 grams of ethylene glycol, 0.070 grams of monobutyltin oxide were added to a 2L reactor, and the esterification temperature was 200°C to 260°C. Esterification under the esterification pressure (gauge pressure) of 2.5 MPa. When the water output reaches the theoretical value, the esterification is terminated, released to normal pressure, 0.0175 grams of phosphoric acid is added, and stirring is continued for 10 minutes. After adding 0.13 grams of ethylene glycol antimony, gradually Heating up and turning into low vacuum stage. After low vacuum time is about 45 minutes, it enters high vacuum polycondensation stage (vacuum <100Pa), polycondensation temperature is 270℃~290℃, and the material is discharged when the stirring power reaches the rated value. The synthesized modified polyester glass The transition temperature is 105.2°C, the intrinsic viscosity is 0.751dL / g, the carboxyl end gr...

Embodiment 3

[0028] Example 3: 350 grams of terephthalic acid, 200 grams of spiroglycol, 10 grams of NPG, 160 grams of ethylene glycol, 0.044 grams of monobutyltin oxide were added to a 2L reactor, and the esterification temperature was 200°C to 260°C. Esterification under esterification pressure (gauge pressure) 2.5MPa, when the water output reaches the theoretical value, end the esterification, release to normal pressure, add 0.035 grams of phosphoric acid, continue stirring for 10 minutes, add 0.15 grams of ethylene glycol antimony, gradually Heating up and turning into low vacuum stage. After low vacuum time is about 45 minutes, it enters high vacuum polycondensation stage (vacuum <100Pa), polycondensation temperature is 270℃~290℃, and the material is discharged when the stirring power reaches the rated value. The synthesized modified polyester glass The transition temperature is 110°C, the intrinsic viscosity is 0.699dL / g, the carboxyl end group is 41mol / t, and the color value (L / a / b) ...

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Abstract

The invention discloses a modified polyester, a preparation method thereof, and a modified polyester film preparation method, and belongs to the field of polyester. According to the preparation method, spiroglycol and 2, 2-dimethyl-1, 3 propylene glycol are taken as copolymerization modification monomers, direct esterification method is adopted to synthesize a copolyester with a glass-transition temperature higher than 100 DEG C; film prepared of the modified polyester is capable of satisfying battery label film requirements; a tin / phosphorus / antimony composite catalyst is adopted in preparation of the modified polyester; in the esterification period, a tin compound is added as an esterification catalyst; after esterification, a phosphorus compound is added for passivation of the tin catalyst; and a antimony series catalyst is added as a polycondensation catalyst. According to the above steps, the tin compound is capable of achieving catalyst effect on esterification reaction, and yellowing and thermal stability reduction caused by taking the tin compound as a polycondensation catalyst are avoided.

Description

technical field [0001] The invention belongs to the field of polyester, and in particular relates to a modified polyester and a preparation method thereof and a film preparation method thereof. Background technique [0002] Shrink film is mainly used for labels and packaging, etc. The materials used to produce shrink film mainly include polyvinyl chloride and polystyrene materials. PVC shrink film has good shrinkage performance, durability, tear resistance, softness, chemical corrosion resistance, transparency and other characteristics, and is widely used in the packaging of beverages and daily necessities. However, PVC materials are not conducive to environmental protection and have been restricted or banned. The polystyrene material is environmentally friendly, and the shrinkage rate can reach 80%. However, the polystyrene label will loosen and fall off when the polystyrene shrink film is bundled and packaged for the second time, which limits its application. PVC, PS mat...

Claims

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Application Information

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IPC IPC(8): C08G63/199C08G63/86C08J5/18C08L67/02
CPCC08G63/199C08G63/866C08J5/18C08J2367/02
Inventor 戴志彬夏峰伟周倩
Owner CHINA PETROLEUM & CHEM CORP
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