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Synthesis of degradable poly-beta-oxybate

A technology of hydroxybutyrate and ethyl hydroxybutyrate, which is applied in the field of fully degradable plastics, can solve the problems of complex reaction process and low degree of polymer polymerization, and achieve the effect of abundant sources, low cost and high quality

Inactive Publication Date: 2005-08-24
BIOLOGY INST OF SHANDONG ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complex reaction process, the degree of polymerization of the product polymer is relatively low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Preparation of β-hydroxybutyraldehyde

[0021] Reactant acetaldehyde 88g, solvent benzene 88g, catalyst NaOH aqueous solution 26.7g, reaction temperature 4-5°C, reaction time 1.0 hour, use acetic acid to neutralize the catalyst, the product contains acetaldehyde 19.36g, enaldehyde 0.89g, β -Hydroxybutyraldehyde is 61.68g, the reaction yield is: 70.1%, and the conversion rate of acetaldehyde is: 78.0%.

[0022] (2) Preparation of β-hydroxybutyric acid

[0023] Reactant β-hydroxybutyraldehyde 161g, solvent ethyl acetate 144.7ml, catalyst cobalt acetate 1.5852g, reaction time 5 hours, reaction temperature 90°C, reaction pressure 10MPa, β-hydroxybutyric acid in the product was 165.57g, butene The aldehyde is 14.75g, the reaction yield is: 88.9%, and the conversion rate is: 90.9%.

[0024] (3) Preparation of ethyl β-hydroxybutyrate

[0025] The reactants β-hydroxybutyric acid 10.41g, ethanol 3.84g, catalyst p-toluenesulfonic acid 1g, the reaction time is 3 hours, the ...

Embodiment 2

[0029] (1) Preparation of β-hydroxybutyraldehyde

[0030] Reactant acetaldehyde 90g, solvent benzene 54g, catalyst NaOH 50.7g, reaction temperature 4-5°C, reaction 1.0-1.5 hours, use acetic acid to neutralize the catalyst, the product contains acetaldehyde 25.19g, enaldehyde 2.73g, β -Hydroxybutyraldehyde is 48.24g, the reaction yield is: 53.60%, and the conversion rate of acetaldehyde is: 72.01%.

[0031] (2) Preparation of β-hydroxybutyric acid

[0032] Reactant β-hydroxybutyraldehyde 176.8g, solvent ethyl acetate 117.9ml, catalyst cobalt acetate 1.2434, reaction time 3 hours, reaction temperature 60°C, reaction pressure 10MPa, β-hydroxybutyric acid in the product was 43.12g, butene Acid 7.20g, reaction yield: 47.83%, conversion rate: 50.32%.

[0033] (3) Preparation of ethyl β-hydroxybutyrate

[0034] Reactant β-hydroxybutyric acid 12.19g, ethanol 4.51g, catalyst p-toluenesulfonic acid 1.5g, reaction time is 5 hours, reaction temperature is 80 ℃, β-hydroxybutyric acid et...

Embodiment 3

[0038] (1) Preparation of β-hydroxybutyraldehyde

[0039] Reactant acetaldehyde 75g, solvent benzene 60g, catalyst NaOH aqueous solution 22.8g, reaction temperature 7-8°C, in the product, acetaldehyde was 10.45g, enaldehyde was 3.19g, β-hydroxybutyraldehyde was 35.16g, and the reaction yield For: 46.88%, acetaldehyde conversion rate: 86.06%.

[0040] (2) Preparation of β-hydroxybutyric acid

[0041] Reactant β-hydroxybutyraldehyde 168g, solvent ethyl acetate 150ml, catalyst cobalt acetate 1.1760g, reaction time 1 hour, reaction temperature 50°C, reaction pressure 10MPa, β-hydroxybutyric acid in the product was 26.77g, crotonaldehyde It is 8.16g, the reaction yield is: 28.42%, and the conversion rate is: 33.47%.

[0042](3) Preparation of ethyl β-hydroxybutyrate

[0043] Reactant β-hydroxybutyric acid 8.15g, ethanol 1.05g, catalyst p-toluenesulfonic acid 0.73g, reaction time is 1 hour, reaction temperature is 80 ℃, β-hydroxybutyric acid ethyl ester in the product is 5.45g, y...

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Abstract

The method for synthesizing completely-degradable plastics poly beta-hydroxybutyrate includes the folloiwng steps: adopting acetaldehyde as raw material to prepare beta-hydroxybutanal; oxidizing it to prepare beta-hydroxybutyric acid; esterifying it to prepare ethyl beta-hydroxybutyrate and polymerizing it to prepare poly beta-hydroxybutyrate. It is characterized by that preparation of beta-hydroxybutanal adopts benzene as solvent, sodium hydroxide as catalyst, its reaction temp. is 1-15 deg.C and the organic acid is used as neutralizing reagent, the preparation of beta-hydroxybutyric acid adopts ethyl acetate as solvent, cobalt acetate as catalyst, its reaction temp. is 40-100 deg.c and reaction pressure is 0.3-1.5 MPa, the preparation of ethyl ebeta-hydroxybutyrate adopts cresulsulfonic acid as catalyst and ethyl alcohol as solvent and polymerization preparation of beta-hydroxybutyrate uses isopropyl titanate as catalyst.

Description

technical field [0001] The invention belongs to a technology of completely degradable plastics synthesized by chemical method, more precisely, it belongs to a technology of preparing polyβ-hydroxybutyrate completely plastics by using acetaldehyde. Background technique [0002] Poly-β-hydroxybutyrate (PHB) is a widely used aliphatic cluster polyester biodegradable polymer, which can be degraded by microorganisms under both aerobic and anaerobic conditions. Under oxygen-enriched conditions, the degradation of PHB produces a very small amount of β-hydroxybutyric acid, most of which are oxidized to carbon dioxide and water; under anaerobic conditions, the decomposition products are acetoacetate and β-hydroxybutyric acid. It can be seen that PHB degradation products can directly enter the ecological cycle system, fundamentally solving the problem of environmental pollution [1，2] . [0003] At present, the main method of producing PHB at home and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/06
Inventor 王加宁马沛生杨合同聂玉敏王彦飞姚碗生
Owner BIOLOGY INST OF SHANDONG ACAD OF SCI
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