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A kind of synthetic method of polybutylene succinate

A technology of polybutylene succinate and a synthesis method is applied in the synthesis field of polybutylene succinate and polybutylene succinate, and can solve the problem of increasing equipment investment and chain extender. Increase the synthesis steps, increase the residue and other problems, to achieve the effect of short reaction time, obvious reduction in energy efficiency, and increase in vapor pressure

Active Publication Date: 2015-09-09
HENAN COAL CHEM IND GROUP INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of chain extenders increases the synthesis steps, increases the investment in equipment in industrial production, and also increases the residual monomers in the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 1,4-butanediol and succinic anhydride according to the molar ratio of 1.15:1, place them in a stainless steel reactor, add stannous chloride and p-toluenesulfonic acid to compound Catalyst, then seal the reaction kettle, and then replace the air in the kettle with inert gas to protect the raw materials and catalyst from being oxidized during the heating process. Heat until the center temperature of the kettle is 100°C, start stirring at a stirring rate of 40r / min, keep the temperature at about 100°C for about half an hour, then raise the center temperature to 165°C, and react for 2 hours. The whole process is at normal pressure, and the flow of inert gas is always maintained. Then slowly raise the temperature to about 180°C, then evacuate to 500Pa and keep it for 1h. Then increase the degree of vacuum, reduce the pressure to about 20Pa, and increase the temperature to 205°C at the same time, react for 3 hours, and the reaction ends. Close the vacuum system, heat...

Embodiment 2

[0025] Weigh 1,4-butanediol and succinic anhydride according to the molar ratio of 1.05:1, place them in a stainless steel reactor, add stannous octoate and benzenesulfonic acid composite catalyst according to 2‰ and 5‰ of the molar weight of succinic anhydride, Afterwards, the reaction kettle is sealed, and the air in the kettle is replaced with an inert gas to protect the raw materials and catalysts from being oxidized during the heating process. Heat until the center temperature of the kettle is 100°C, start stirring at a stirring rate of 40r / min, keep the temperature at about 100°C for about half an hour, then raise the center temperature to 170°C, and react for 2 hours. The whole process is at normal pressure, and the flow of inert gas is always maintained. Then slowly raise the temperature to about 180°C, then vacuumize to 1500Pa and keep it for 3h. Then increase the degree of vacuum, reduce the pressure to about 50Pa, and increase the temperature to 230°C at the same t...

Embodiment 3

[0027]Weigh 1,4-butanediol and succinic anhydride according to the molar ratio of 1.2:1, place them in a stainless steel reactor, add stannous oxalate and 4-methylbenzenesulfonate according to 3‰ and 1‰ of the molar weight of succinic anhydride Acid anhydride composite catalyst, then seal the reaction kettle, and then replace the air in the kettle with inert gas to protect the raw materials and catalysts from being oxidized during the heating process. Heat until the center temperature of the kettle is 100°C, start stirring at a stirring rate of 40r / min, keep the temperature at about 100°C for about half an hour, then raise the center temperature to 150°C, and react for 3 hours. The whole process is at normal pressure, and the flow of inert gas is always maintained. Then slowly raise the temperature to about 200°C, then vacuumize to 700Pa and keep it for 2h. Then increase the degree of vacuum, reduce the pressure to about 30Pa, and increase the temperature to 220°C at the same...

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Abstract

The invention discloses a synthesis method of poly(butylene succinate), belonging to the technical field of high polymer material synthesis. The method comprises the following steps: (1) adding raw materials butanedioic anhydride and 1,4-butanediol and a catalyst into a polymerization plant, and reacting at 150-170 DEG C in an inert gas protective atmosphere for 1-3 hours; (2) carrying out prepolycondensation reaction at 170-200 DEG C under the pressure of 300-1500Pa for 1-5 hours; and (3) finally, heating to 200-230 DEG C, lowering the pressure to 10-100Pa, and polycondensing under such conditions for 1-5 hours to obtain the product poly(butylene succinate). The molecular weight of the product is 80-150 thousand. By adopting the composite catalytic system, the consumption of the butanediol is lower than the prior art, no antioxidant or chain extender is needed, the molecular weight of the product is high, and the reaction temperature is lowered. The butanedioic anhydride used as the reaction raw material has the advantages of high reaction activity, low dehydration and low requirements for corrosion resistance of equipment.

Description

Technical field [0001] The present invention involves a synthesis method of a polytexyl diite dilate, which is a high -molecular material synthesis technology field.In particular, it involves a method of combining dinicine anhydride as the raw material and using a composite catalyst to synthesize polynonol dilate. Background technique [0002] The advantages of plastic are increasingly widely used in industry and life with the advantages of good performance, low density, and good processing performance."At present, the total amount of abandoned plastic products in the world exceeds 60 million tons, and China has more than 3 million tons of abandonment each year. Traditional burial and incineration treatment will bring pollution.Development can be degradable materials is an effective way for the greening of polymer materials today. At the same time, the supply of global oil resources is becoming increasingly tense, and the development of the low -carbon economy has also brought ne...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/16C08G63/85
Inventor 赵清香李宁刘民英付瑶付鹏徐柳崔喆李壮张建平曹国喜刘焦萍
Owner HENAN COAL CHEM IND GROUP INST
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