Method for preparing poly(butylene succinate) through transesterification method

A technology of polybutylene succinate and dimethyl succinate, which is applied in the field of polymer material synthesis, can solve the problems of many by-product small molecules, low yield and high corrosion, and achieve good catalytic effect, High catalytic activity and high activity effect

Active Publication Date: 2017-05-31
NINGBO ZHETIE JIANGNING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of the present invention can overcome the problem of high corrosiveness of polymerized monomers in the prior art on the one hand, and can overcome the problems of many by-product small molecules and low yield in the prior art on the other hand, thereby effectively reducing polysuccinic acid Butanediol ester production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a dry nitrogen atmosphere, 47.4 g (0.25 mol) of TiCl 4 Slowly add to 58.28 g (0.65 mol) of anhydrous BDO that is vigorously stirred, a large amount of white smoke is produced in the container, the solution is light yellow, keep stirring, and continue to drop a certain amount of triethylamine to neutralize the hydrogen chloride produced by the reaction , control the pH value to be neutral, after standing for 30min, filter, and carry out vacuum distillation to the obtained filtrate, until the filtrate is only about 100mL, wash with acetone, a white suspension appears, carry out suction filtration and drying to obtain 1,4- Butanedioxide titanium solid catalyst 46.2 grams, yield 82.8%.

Embodiment 2

[0033] In a dry nitrogen atmosphere, 47.4 g (0.25 mol) of TiCl 4 Slowly add to 40.3 g (0.65 mol) of anhydrous ethylene glycol that is vigorously stirred, a large amount of white smoke is produced in the container, the solution is light yellow, keep stirring, and continue to drop a certain amount of dimethylamine to neutralize the reaction hydrogen chloride, control the pH value to be neutral, let it stand for 30 minutes, filter, and carry out vacuum distillation on the obtained filtrate, until the filtrate is only about 100mL, wash with acetone, a white suspension appears, carry out suction filtration and drying to obtain B 23.5 grams of titanium glycolate solid catalysts, yield 89.6%.

Embodiment 3

[0035] In a dry nitrogen atmosphere, 47.4 g (0.25 mol) of TiCl 4 Slowly add to 40.3 g (0.65 mol) of anhydrous ethylene glycol that is vigorously stirred, a large amount of white smoke is produced in the container, the solution is light yellow, keep stirring, and continue to drop a certain amount of ammonia gas to neutralize the reaction. Hydrogen chloride, control the pH value to be neutral, let it stand for 20 minutes, filter, and carry out vacuum distillation on the obtained filtrate, until the filtrate is only about 100mL, wash with acetone, a white suspension appears, carry out suction filtration and drying to obtain ethylene dichloride Titanium alkoxide solid catalyst 25 grams, yield 93.6%.

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Abstract

The invention relates to the field of high polymer material synthesis and discloses a method for preparing poly(butylene succinate) through a transesterification method. The method comprises the following steps: carrying out esterification reaction on dimethyl succinate, a dihydric alcohol monomer containing 1,4-butanediol and a composite catalyst in a nitrogen atmosphere, wherein the reaction temperature is 110-150 DEG C and the reaction time is 2-3 hours; carrying out condensation polymerization in a vacuum condition, wherein the vacuum degree is 10-300Pa of absolute pressure, the reaction temperature is 150-240 DEG C and the reaction time is 2-3 hours, thereby preparing the poly(butylene succinate). According to the method, on one hand, the problem of high corrosivity of a polymeric monomer in the prior art can be solved, and on the other hand, the problems of multiple byproduct micromolecules and relatively low yield in the prior art can be solved, so that the production cost of the poly(butylene succinate) can be effectively reduced.

Description

technical field [0001] The invention relates to the field of polymer material synthesis, in particular to a method for preparing polybutylene succinate by transesterification. Background technique [0002] Polybutylene succinate (PBS) is an important polymer material, especially as a biodegradable material, which is easily decomposed and metabolized by various microorganisms in nature or enzymes in animals and plants, and has good mechanical properties And heat performance, is one of the effective ways to fundamentally solve the problem of white pollution, and has a very wide range of applications in the fields of packaging, tableware, medical supplies, agricultural films, slow-release materials and biomedical materials. [0003] The synthesis of PBS has come a long way since Lathers first synthesized polybutylene succinate 70 years ago. The melt polycondensation method is commonly used in the synthesis of PBS, which is a two-step synthesis method. Firstly, succinic acid a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/85C08G63/87
CPCC08G63/16C08G63/85C08G63/87C08G2230/00
Inventor 窦和瑞徐晓航黄军吕文钧吕荣闫静
Owner NINGBO ZHETIE JIANGNING CHEM
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