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Preparation method of polybutylene succinate

A technology for polybutylene succinate and succinic acid is applied in the field of ester preparation, which can solve the problems of complex preparation method, difficulty in popularization and application, and achieve the effects of low preparation cost and simple operation.

Inactive Publication Date: 2017-05-31
SHAANXI YIPINDA PETROCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are ubiquitous disadvantages that the preparation method is complicated and difficult to popularize and apply.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The preparation method of polybutylene succinate comprises the following steps:

[0018] (1) Esterification reaction: Add 0.1 mol of succinic acid, 0.11 mol of butanediol and 0.01 mol of butyl titanate into a 250 mL three-neck round bottom flask, heat in an oil bath, and control the temperature at 130°C under stirring. Water vacuum pump depressurizes to -0.1MPa, reacts for 2h;

[0019] (2) Polycondensation reaction: add nitrogen, stir, raise the temperature of the oil bath to 220°C, remove the nitrogen, use a circulating water vacuum pump to depressurize to -0.1MPa, and react at a constant temperature for 2 hours, stop heating and stirring, remove the oil bath, and cool naturally To room temperature, obtain thick polybutylene succinate;

[0020] (3) Purification of polybutylene succinate: dissolve the crude polybutylene succinate obtained in step (2) with 200 mL of chloroform to obtain trichloromethane of crude polybutylene succinate methane solution, then under the c...

Embodiment 2

[0022] The preparation method of polybutylene succinate comprises the following steps:

[0023] (1) Esterification reaction: Add 0.1 mol of succinic acid, 0.11 mol of butanediol and 0.01 mol of butyl titanate into a 250 mL three-neck round bottom flask, heat in an oil bath, and control the temperature at 150°C under stirring. Water vacuum pump depressurizes to -0.1MPa, reacts for 2h;

[0024] (2) Polycondensation reaction: Introduce nitrogen, stir, raise the temperature of the oil bath to 230°C, remove the nitrogen, use a circulating water vacuum pump to depressurize to -0.1MPa, react at constant temperature for 2 hours, stop heating and stirring, remove the oil bath, and cool naturally To room temperature, obtain thick polybutylene succinate;

[0025] (3) Purification of polybutylene succinate: dissolve the crude polybutylene succinate obtained in step (2) with 200 mL of chloroform to obtain trichloromethane of crude polybutylene succinate methane solution, then under the c...

Embodiment 3

[0027] The preparation method of polybutylene succinate comprises the following steps:

[0028] (1) Esterification reaction: Add 0.1 mol of succinic acid, 0.11 mol of butanediol and 0.01 mol of butyl titanate into a 250 mL three-neck round bottom flask, heat in an oil bath, and control the temperature at 140°C under stirring. Water vacuum pump depressurizes to -0.1MPa, reacts for 2h;

[0029] (2) Polycondensation reaction: add nitrogen, stir, raise the temperature of the oil bath to 225°C, remove the nitrogen, use a circulating water vacuum pump to depressurize to -0.1MPa, react at a constant temperature for 2 hours, stop heating and stirring, remove the oil bath, and cool naturally To room temperature, obtain thick polybutylene succinate;

[0030] (3) Purification of polybutylene succinate: dissolve the crude polybutylene succinate obtained in step (2) with 200 mL of chloroform to obtain trichloromethane of crude polybutylene succinate methane solution, then under the condi...

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Abstract

The invention provides a preparation method of polybutylene succinate. The preparation method comprises the following steps: (1) carrying out an esterification reaction, namely adding succinic acid, butylene glycol and tetrabutyl titanate into a flask; heating in an oil bath at 130 DEG C-150 DEG C; decompressing to -0.1MPa by utilizing a circulating water vacuum pump and reacting for 2h; (2) carrying out a condensation polymerization, namely introducing nitrogen gas and stirring; raising the temperature of the oil bath to 220 DEG C-230 DEG C; removing the nitrogen gas; decompressing to -0.1MPa by utilizing the circulating water vacuum pump and reacting for 2h; stopping heating and stirring; moving out the oil bath and naturally cooling to a room temperature to obtain crude polybutylene succinate; and (3) purifying the polybutylene succinate to obtain the polybutylene succinate. The preparation method of the polybutylene succinate, provided by the invention, is simple to operate and low in preparation cost; the intrinsic viscosity number of the prepared polybutylene succinate reaches 0.355.

Description

technical field [0001] The invention belongs to the field of ester preparation, in particular to a preparation method of polybutylene succinate. Background technique [0002] Polybutylene succinate (PBS), a biodegradable aliphatic polyester with good thermal, mechanical and processing properties, has been used in degradable plastics. However, PBS fibers have not been successfully developed. If PBS can be spun into fibers and blended with natural or recycled fibers, it will play a positive role in promoting the development and application of degradable and environmentally friendly fibers in the world. Therefore, optimize and improve the synthesis conditions and methods of PBS, improve the relative molecular weight and spinnability of PBS, and lay the foundation for the future PBS fiber spinning. [0003] At present, the research on PBS and its copolyester is the most extensive. Commonly used PBS synthesis methods include melt polycondensation, chain extension, solution poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/85C08G63/90
CPCC08G63/16C08G63/85C08G63/90
Inventor 李长英
Owner SHAANXI YIPINDA PETROCHEM CO LTD