Preparation method of polyadipic acid-butylene terephthalate with high molecular weight

A technology of butylene phthalate and terephthalic acid is applied in the field of preparation of high molecular weight polyadipate-butylene terephthalate, and can solve the problems of high temperature instability of melt, low catalytic efficiency, The problem of high cost is to achieve the effect of narrow molecular weight distribution, high catalytic efficiency and improved heat resistance.

Active Publication Date: 2013-06-05
山东悦泰生物新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of high molecular weight polybutylene adipate-terephthalate, which overcomes the shortco

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0018] Example 1

[0019] Put 136g of butanediol, 80g of adipic acid and 75g of terephthalic acid into the reactor, stir evenly, add composite catalyst 0.058g MgO and 0.29g bistriethanolamine diisopropyl titanate, at a temperature of 180℃ The esterification was carried out under normal pressure and the constant temperature reaction was 2.3 hours. Then, the temperature was raised to 220°C, 0.087g of stabilizer polycarbodiimide was added, and the pressure was reduced to 30 Pa for polycondensation reaction, and the reaction was carried out for 3 hours. The molecular weight of the obtained polybutylene adipate-terephthalate was 9.4× 10 4 , The molecular weight distribution is 1.62, the tensile strength is 18.21MPa, the elongation at break is 743%, the L value is 82, and the acid value is 18.6mol / t.

Example Embodiment

[0020] Example 2

[0021] Put 180g butanediol, 102g adipic acid and 50g terephthalic acid into the reactor, stir evenly, add 0.166g Al of composite catalyst 2 O 3 And 2.65 g of bis(ethyl acetoacetate) diisopropyl titanate, esterification under normal pressure at a temperature of 230°C, and constant temperature reaction for 1.5 hours. Then, the temperature was raised to 250°C, 0.332g of stabilizer dicyclohexylcarbodiimide was added, and the pressure was reduced to 50 Pa for polycondensation reaction, and the reaction was carried out for 3.5 hours. The molecular weight of the obtained polybutylene adipate-terephthalate was 15.2×10 4 , The molecular weight distribution is 1.87, the tensile strength is 17.42MPa, the elongation at break is 795%, the L value is 81, and the acid value is 20.2mol / t.

Example Embodiment

[0022] Example 3

[0023] Put 92g butanediol, 88g adipic acid and 66g terephthalic acid into the reactor, stir evenly, add 0.025g Li of composite catalyst 2 O and 1.23 g of tetraethyl titanate were esterified under normal pressure at a temperature of 215°C and reacted at a constant temperature for 2 hours. Then, the temperature was raised to 230°C, 0.123g of stabilizer polycarbodiimide was added, and the pressure was reduced to 80 Pa for polycondensation reaction. The reaction was carried out for 2.5 hours. The molecular weight of the obtained polybutylene adipate-terephthalate was 11.9× 10 4 , The molecular weight distribution is 1.57, the tensile strength is 20.91MPa, the elongation at break is 602%, the L value is 85, and the acid value is 16.7 mol / t.

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Abstract

The invention belongs to the technology in the preparation field of completely biodegradable fat-aromatic copolyester and in particular relates to a preparation method of polyadipic acid-butylene terephthalate with high molecular weight. The preparation method comprises the following steps of: adding butanediol, adipic acid and terephthalic acid into a reactor; adding a composite catalyst to the reactor for carrying out esterification reaction; and carrying out polycondensation to obtain a product, wherein the composite catalyst is a mixture of metal oxide and titanium organic esters, and the metal oxide is at least one of oxides of Li, Na, K, Mg, Al, Ca, Mn and Co. The composite catalyst is adopted, so that the catalytic efficiency is high, the polymerization reaction velocity is greatly increased and the cost of the product is technically reduced. A stabilizer is added during the polycondensation stage, so that the high-temperature degradation side reaction is reduced, the molecular weight of the polymer is improved, the product color phase is improved, the terminal carboxyl content of the polymer is effectively reduced, the post-processing heat resistant performance of the product is improved, and the using value is greater.

Description

technical field [0001] The invention belongs to the technical field of preparation of completely biodegradable aliphatic-aromatic copolyesters, and in particular relates to a preparation method of high-molecular-weight polybutylene adipate-terephthalate. Background technique [0002] With the development of the plastics industry, synthetic polymer materials play an extremely important role in various fields of industrial and agricultural production and daily life, but because they are not degradable after being discarded, they have brought serious pollution to social life. The search for an environmentally friendly plastic that can meet various needs has attracted the attention of many scientists. In recent years, degradable polyester has become a research hotspot at home and abroad because of its degradation characteristics and economical efficiency. [0003] Polybutylene adipate-terephthalate is one of the completely biodegradable polyester materials, which is easily decom...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/85C08G63/83
Inventor 杨苹苹卢伟高丽霞孙莹莹杨军
Owner 山东悦泰生物新材料有限公司
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