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Method for synthesizing 3-hydracrylic acid ester

A technology of hydroxypropionate and cobalt carbonyl, which is applied in the field of synthesizing 3-hydroxypropionate, can solve the problems such as difficult separation of catalysts, and achieve the effect of mild catalytic reaction conditions, high activity and difficult separation

Active Publication Date: 2017-02-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] What the present invention aims to solve is the problem that the homogeneous system catalyst in the prior art is difficult to separate, and provides a new synthetic method of 3-hydroxypropionate, which has the advantage that the catalyst system is easily separated from the reaction system

Method used

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  • Method for synthesizing 3-hydracrylic acid ester
  • Method for synthesizing 3-hydracrylic acid ester
  • Method for synthesizing 3-hydracrylic acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1. Catalyst preparation

[0040] 1.0 mmol of Co 2 (CO) 8 Dissolve in 740mmol of methanol, add poly(4-vinylpyridine) powder with a number average molecular weight of 100,000, make the molar ratio of nitrogen to cobalt carbonyl 2:1, stir at room temperature for 2 hours to obtain a catalyst mixture.

[0041] 2. Synthesis of methyl 3-hydroxypropionate

[0042] The obtained catalyst mixture was transferred to a 100 mL reactor; the reactor was purged three times with nitrogen, and carbon monoxide and 50 mmol ethylene oxide were added to make the system pressure 5 MPa; reacted at 60° C. for 6 hours. After the reaction was completed, the reactor body was cooled to 0° C., the pressure was slowly released to normal pressure, and the reactor was purged three times with nitrogen. Sampling analysis showed that the conversion rate of ethylene oxide was 31%, and the selectivity of methyl 3-hydroxypropionate was 79%.

[0043] For the convenience of comparison, the results of the sy...

Embodiment 2

[0045] 1. Catalyst preparation

[0046] 1.0 mmol of Co 2 (CO) 8 Dissolve in 740mmol of methanol, add poly(4-vinylpyridine-co-styrene) powder with a number average molecular weight of 100,000 (wherein the molar ratio of 4-vinylpyridine monomer units to styrene monomer units is 1:1), The molar ratio of nitrogen to cobalt carbonyl was 2:1, and stirred at room temperature for 2 hours to obtain a catalyst mixture.

[0047] 2. Synthesis of methyl 3-hydroxypropionate

[0048]The obtained catalyst mixture was transferred to a 100 mL reactor; the reactor was purged three times with nitrogen, and carbon monoxide and 50 mmol ethylene oxide were added to make the system pressure 5 MPa; reacted at 60° C. for 6 hours. After the reaction was completed, the reactor body was cooled to 0° C., the pressure was slowly released to normal pressure, and the reactor was purged three times with nitrogen. Sampling analysis showed that the conversion rate of ethylene oxide was 34%, and the selectivi...

Embodiment 3

[0051] 1. Catalyst preparation

[0052] 1.0 mmol of Co 2 (CO) 8 Dissolve in 740mmol of methanol, add poly(4-vinylpyridine-co-ethylvinylbenzene) powder with a number average molecular weight of 100,000 (wherein the molar ratio of 4-vinylpyridine monomer unit to ethylvinylbenzene monomer unit 1:1), the molar ratio of nitrogen to cobalt carbonyl was 2:1, and stirred at room temperature for 2 hours to obtain a catalyst mixture.

[0053] 2. Synthesis of methyl 3-hydroxypropionate

[0054] The obtained catalyst mixture was transferred to a 100 mL reactor; the reactor was purged three times with nitrogen, and carbon monoxide and 50 mmol ethylene oxide were added to make the system pressure 5 MPa; reacted at 60° C. for 6 hours. After the reaction was completed, the reactor body was cooled to 0° C., the pressure was slowly released to normal pressure, and the reactor was purged three times with nitrogen. Sampling analysis showed that the conversion rate of oxirane was 40%, and the ...

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Abstract

The invention relates to a method for synthesizing 3-hydracrylic acid ester. The method mainly solves the problem that in the prior art, catalysts in a homogeneous system are difficult to separate. The method for synthesizing 3-hydracrylic acid ester includes the following steps that firstly, a ligand and cobalt carbonyl are subjected to a coordination reaction in an alcohol solvent to obtain turbid liquid of a catalyst; secondly, ethylene oxide and carbon monoxide are added, and a reaction is conducted to obtain 3-hydracrylic acid ester. According to the technical scheme, the ligand is selected from 4-vinylpyddine homopolymers or copolymers containing 4-vinylpyddine monomeric units, the technical problem is well solved, and the method can be used in industrial production of 3-hydracrylic acid ester.

Description

technical field [0001] The present invention relates to a method for synthesizing 3-hydroxypropionate. Background technique [0002] 1,3-Propanediol is an important organic fine chemical, which can be used as a raw material for the production of antifreeze, plasticizer, preservative and emulsifier, and is also widely used in industries such as food, cosmetics and pharmaceuticals. Its most important The application is to synthesize polytrimethylene terephthalate (PTT) polyester fiber as a monomer. Compared with the commonly used polyethylene terephthalate (PET) fiber, PTT fiber has light resistance, less water absorption, and stable It has excellent properties such as good resistance, and at the same time has the advantages of good resilience, easy biodegradation and little environmental pollution. It has a wide range of application prospects and is the focus of current research and development. At present, there are three main processes for 1,3-propanediol: the ethylene oxi...

Claims

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Application Information

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IPC IPC(8): C07C69/675C07C67/37B01J31/22
CPCB01J31/22B01J2531/845C07C67/37C07C69/675
Inventor 刘波金照生吕建刚李晓明
Owner CHINA PETROLEUM & CHEM CORP
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