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Method for preparing 3-hydroxypropionate

A technology of hydroxypropionate and acrylonitrile, which is applied in the direction of chemical instruments and methods, carbon monoxide or formate reaction preparation, organic compound/hydride/coordination complex catalyst, etc., can solve the problems such as difficult separation of catalysts, and achieve The catalytic reaction conditions are mild, the activity is high, and the effect of solving separation difficulties

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 is to solve is the problem that the homogeneous system catalyst in the prior art is difficult to separate, and a new method for preparing 3-hydroxypropionate is provided, which has the advantage that the catalyst system is easily separated from the reaction system

Method used

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  • Method for preparing 3-hydroxypropionate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1. Synthetic catalyst

[0039] 1.0 mmol Co 2 (CO) 8 Dissolve in 740 mmol of methanol, add polyacrylonitrile powder with a degree of polymerization of 1000, make the molar ratio of nitrogen to cobalt carbonyl 2:1, and stir at room temperature for 2 hours to obtain a catalyst mixture.

[0040] 2. Preparation of methyl 3-hydroxypropionate

[0041] 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 39%, and the selectivity of methyl 3-hydroxypropionate was 77%.

[0042] For the convenience of comparison, the results of the synthesis reac...

Embodiment 2

[0044] 1. Synthetic catalyst

[0045] 1.0 mmol Co 2 (CO) 8 Be dissolved in the methyl alcohol of 740mmol, add the poly(acrylonitrile-co-vinylidene chloride) powder that the number of acrylonitrile monomer unit is 1000 (acrylonitrile monomer unit and vinylidene chloride monomer unit in the copolymer The molar ratio of nitrogen and carbonyl cobalt is 1:1), and the molar ratio of nitrogen and cobalt carbonyl is 2:1, and stirred at room temperature for 2 hours to obtain a catalyst mixture.

[0046] 2. Preparation of methyl 3-hydroxypropionate

[0047] 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 anal...

Embodiment 3

[0050] 1. Synthetic catalyst

[0051] 1.0 mmol Co2 (CO) 8 Be dissolved in the methyl alcohol of 740mmol, add the poly(acrylonitrile-co-butadiene) powder that the number of acrylonitrile monomer unit is 1000 (the mole of acrylonitrile monomer unit and butadiene monomer unit in the described copolymer The ratio is 1:1), the molar ratio of nitrogen and cobalt carbonyl is 2:1, and stirred at room temperature for 2 hours to obtain a catalyst mixture.

[0052] 2. Preparation of methyl 3-hydroxypropionate

[0053] 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 et...

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Abstract

The invention relates to a method for preparing 3-hydroxypropionate and mainly aims to solve the problem that in the prior art, a catalyst in a homogeneous system is hard to separate. The method for preparing 3-hydroxypropionate comprises the steps that first, a ligand and cobalt carbonyl are subjected to a coordination reaction in an alcoholic solvent to obtain turbid liquid of a catalyst; second, ethylene oxide and carbon monoxide are added, and a reaction is carried out to obtain 3-hydroxypropionate. According to the technical scheme that the ligand is an acrylonitrile homopolymer or a copolymer which contains acrylonitrile monomer units, the technical problem is well solved, and the method can be applied to industrial production of 3-hydroxypropionate.

Description

technical field [0001] The present invention relates to a process for the preparation of 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 ethyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/37C07C69/675B01J31/22
CPCB01J31/1625B01J2231/30C07C67/37C07C69/675
Inventor 吕建刚刘波金照生李晓明黄祖娟
Owner CHINA PETROLEUM & CHEM CORP
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