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Modified butanediol ester poly succinic acid and synthetic method

A technology of polybutylene succinate and butanediol, which is applied in the field of maleopimaric anhydride copolymerized modified polybutylene succinate and its synthesis, can solve the impact of biodegradation performance and the toxic and side effects of degradation products To achieve the effect of improving crystallization behavior, avoiding toxic and side effects, and reducing crystallization temperature

Inactive Publication Date: 2006-07-05
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Darwin P.R.Kint [Polymer 44 (2003) 1321-1330] and Wilt, U [Macromol. The introduction of terephthalic acid structure) can improve the relative mechanical properties of aliphatic polyesters to a certain extent, but its biodegradation properties will be greatly affected, and the degradation products are suspected to have toxic side effects on the environment

Method used

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  • Modified butanediol ester poly succinic acid and synthetic method
  • Modified butanediol ester poly succinic acid and synthetic method
  • Modified butanediol ester poly succinic acid and synthetic method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 0.1mol of maleopimaric anhydride (RMA), 0.1mol of glycine, and 150ml of N,N-dimethylformamide (DMF) into a four-neck flask equipped with a thermometer, stirring, and nitrogen protection device, and stir at room temperature for 8 hours , heated to 130°C and stirred for 4 hours, cooled to room temperature, and turned into a yellow-brown solid, added 200ml of water, stirred, and a yellow precipitate formed. Filtration, washing, vacuum drying for 3 hours, repeated recrystallization with DMF and water, the final product became a white powdery solid, placed in a vacuum oven at 90° C. for 10 hours of vacuum drying to obtain maleopimaric acid imide dicarboxylic acid ( RMID), spare, 56% yield.

[0041]Take 0.05 mol of maleopimaric acid imide dicarboxylic acid prepared in the previous step and add excess 1,4-butanediol into a four-neck flask equipped with stirring, heating, and nitrogen protection device, at 230-300°C The mixture of zinc acetate and antimony trioxide is used...

Embodiment 2

[0044] Add 0.1 mol of maleopimaric anhydride (RMA), 0.1 mol of 6-aminocaproic acid, and 150 ml of N, N-dimethylformamide (DMF) into a four-neck flask equipped with a thermometer, stirring, and nitrogen protection device, and stir at room temperature After 18 hours, the temperature was raised to 140° C. and stirred for 4 hours, cooled to room temperature, and a yellow-brown solid was formed. Added 200 ml of water, stirred, and a yellow precipitate formed. Filtration, washing, vacuum drying for 5 hours, repeated recrystallization with DMF and water, the final product was a white powdery solid, placed in a vacuum drying oven at 90°C for 10 hours in vacuum to obtain maleopimaric acid imide dicarboxylic acid, Standby, yield 70%.

[0045] Take 0.05 mol of maleopimaric acid imide dicarboxylic acid prepared in the previous step and add excess 1,4-butanediol into a four-neck flask equipped with stirring, heating, and nitrogen protection device, at 230-300°C Using antimony trioxide as ...

Embodiment 3

[0048] Add 0.1mol of maleopimaric anhydride (RMA), 0.1mol of p-aminobenzoic acid, and 150ml of N,N-dimethylformamide (DMF) into a four-neck flask equipped with a thermometer, stirring, and nitrogen protection device, and stir at room temperature for 3 After 1 hour, the temperature was raised to 150° C. and stirred for 2 hours, cooled to room temperature, and a yellow-brown solid was formed. Added 200 ml of water, stirred, and a yellow precipitate formed. Filter and wash, vacuum dry for 3 hours, DMF and water recrystallize repeatedly, the final product becomes a white powdery solid, put it in a vacuum drying oven at 90°C and vacuum dry for 10 hours to obtain maleopimaric acid imide dicarboxylic acid (RMID) , standby, yield 86%. See Figure 1~4 .

[0049] Take 0.05 mol of maleopimaric acid imide dicarboxylic acid prepared in the previous step and add excess 1,4-butanediol into a four-neck flask equipped with stirring, heating, and nitrogen protection device, at 230-300°C A mi...

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Abstract

This invention relates to a cyclic compound, especially poly (butylenes succinate) modified by copolymerization with maleopimaric anhydride and its synthesis method. Succinic acid, 1,4-butanediol are mixed at a mole ratio of 1:1~4, and 4~20g maleopimaric imine dicarboxylic ester oligomers are added per 163g succinic acid / 1,4-butanediol mixture. The system is stirred at a temperature of 160~200 deg.C in the presence of inert gas, and cadmium acetate, zincum acetate, stibium oxide, butyl titanate or their optional combinations are added as catalysts at a mass fraction of 0.1~3% for a polymerization at a temperature of 230~280 deg.C and a pressure of 5~10Pa to produce modified poly(butylenes succinate) with a following structure. Such an environmentally friendly polymer performs a good elongation rate at break, impact-resistance strength and bending strength.

Description

technical field [0001] The patent relates to a cyclic compound, in particular to maleopimaric anhydride copolymerized modified polybutylene succinate and a synthesis method thereof. Background technique [0002] In recent years, due to the development of the plastics industry and people's increasing attention to environmental issues, the problem of "white pollution" caused by plastics has attracted more and more attention. How to find a degradable, environmentally friendly and meet people's different needs Plastics have become a common problem faced by the majority of scientific workers. As a recognized biodegradable plastic, aliphatic polyester is gaining more and more popularity. [0003] Polybutylene succinate (PBS) is an aliphatic polyester with relatively high melting point and strength, and it is most likely to replace other current non-biodegradable plastics and become a new general-purpose material. As early as a few years ago, the Japanese Showa Polymer Company an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/91
Inventor 刘小青李春成张栋萧耀南
Owner INST OF CHEM CHINESE ACAD OF SCI
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