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Poly(butylene succinate) and preparation method thereof

A technology of polybutylene succinate and butanediol, which is applied in the field of aliphatic copolyesters, can solve the problems of difficult reaction control and degradation of material performance, so as to prolong the maintenance/replacement cycle and reduce the degree of crystallization , the effect of high heat resistance

Active Publication Date: 2012-11-14
KINGFA SCI & TECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the diisocyanate reaction unit is easy to generate a gel point during the reaction, and the reaction control is difficult. The appearance of the gel will lead to a decrease in the performance of the material.

Method used

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  • Poly(butylene succinate) and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 23.0g of 1,4-butanediol, 5.0g of 1,4-cyclohexanedimethanol, and 25.0g of succinic acid were heated up to 210°C under the protection of nitrogen, and 30mg of titanium ethylene glycol was added to maintain the temperature in the reactor. At the same time, the water produced by the reaction is removed by split flow, and the degree of reaction is judged by weighing the water generated by the reaction. When the esterification rate reaches 95%, after the temperature reaches 230°C, add 3.6 mg of phosphorous acid and react for 30 minutes. , and then began to slowly heat up to 245 ° C, gradually increase the degree of vacuum, keep the temperature constant, keep the pressure in the kettle below 80 Pa, and react for 3.5 hours. The reactor was flushed with nitrogen to normal pressure, 0.05 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide compound was added, stirred for 5 minutes, and the obtained product was obtained.

[0049] The relevant indicators of the product were obtained:...

Embodiment 2

[0051]Put 38.0g of 1,4-butanediol, 5.0g of 2,2,4,4-tetramethyl-1,3-cyclobutanediol, 25.0g of succinic acid, under the protection of nitrogen, raise the temperature to 200°C, add Titanium glycolate 30mg, maintain the temperature in the reactor at 200°C, and remove the water produced by the reaction by splitting, and judge the degree of reaction by weighing the water generated by the reaction. When the esterification rate reaches 95%, lower the temperature to 230°C Finally, add 3.6mg of phosphorous acid, react for 30 minutes, then start to slowly raise the temperature to 245°C, gradually increase the degree of vacuum, keep the temperature constant, keep the pressure in the kettle below 80Pa, and react for 3.5 hours. The reactor was flushed with nitrogen to normal pressure, 0.05 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide was added, stirred for 5 minutes, and the obtained product was obtained.

[0052] The relevant indicators of the product were obtained: viscosity 1.33dL / ...

Embodiment 3

[0054] Put 33.0g of 1,4-butanediol, 5.0g of 2,2,4,4-tetramethyl-1,3-cyclobutanediol, 25.0g of succinic acid, under the protection of nitrogen, raise the temperature to 190°C, add Titanium glycolate 30mg, maintain the temperature in the reactor at 190°C, and remove the water produced by the reaction by splitting, and judge the degree of reaction by weighing the water generated by the reaction. When the esterification rate reaches 95%, lower the temperature to 230°C Finally, add 5.0 mg of phosphorous acid, react for 30 minutes, then start to slowly raise the temperature to 245°C, gradually increase the degree of vacuum, keep the temperature constant, keep the pressure in the kettle below 80Pa, and react for 3.5 hours. The reactor was flushed with nitrogen to normal pressure, 0.08 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide was added, stirred for 5 minutes, and the obtained product was obtained.

[0055] The relevant indicators of the product were obtained: viscosity 1.33d...

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Abstract

The invention discloses a poly(butylene succinate) which is prepared by copolymerizing succinic acid, butylene glycol and cyclic dibasic alcohol. The poly(butylene succinate) comprises succinic acid residue, butylene glycol residue and cyclic diol residue, wherein the butylene glycol residue accounts for 90-98% of the total dibasic alcohol, and the cyclic diol residue accounts for 2-10% of the total dibasic alcohol. The preparation method comprises the following steps: reacting succinic acid, butylene glycol and cyclic dibasic alcohol at 200-230 DEG C under the action of a catalyst to perform direct esterification, thereby obtaining an esterified substance; adding a stabilizer, and carrying out pre-polycondensation reaction at 220-250 DEG C to obtain a prepolymer; carrying out polycondensation reaction on the prepolymer at 235-250 DEG C while gradually reducing the vacuum degree of the reaction system to less than 150Pa; and after the polycondensation finishes, adding carbodiimide compounds into the reaction product, and mixing for 2-15 minutes, thereby obtaining the poly(butylene succinate). The polyester synthesized by the method disclosed by the invention has the advantages of high heat resistance, high melting point, controllable degradation rate, excellent mechanical properties and excellent processability.

Description

technical field [0001] The invention relates to an aliphatic copolyester, in particular to a polybutylene succinate and a preparation method thereof. Background technique [0002] With the further improvement of environmental awareness, people have realized that the pressure of non-degradable plastics on the environment is getting higher and higher, and finding new biodegradable alternative materials is one of the most interesting topics for people. Biodegradable polymers are a class of polymer materials that can decompose into carbon dioxide and water after a certain time span under suitable environmental conditions. This degradation process is usually divided into two processes. First, the molecular weight of macromolecules becomes smaller after hydrolysis and light / oxygen degradation, and then they are further consumed by microorganisms. Such microorganisms may be bacteria, fungi, yeast, algae, etc. [0003] Polybutylene succinate (PBS) has good biodegradability and cont...

Claims

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Application Information

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IPC IPC(8): C08G63/85C08G63/199
Inventor 苑仁旭徐依斌焦健赵巍蔡彤旻夏世勇曾祥斌
Owner KINGFA SCI & TECH CO LTD
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