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Preparation method of methyl-3-hydroxypropanoate

A technology of methyl hydroxypropionate and methanol, which is applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, organic compound/hydride/coordination complex catalyst, etc., can solve the problem of complex catalyst preparation and high energy consumption , the problem of high reaction temperature, to achieve the effect of low price, improved conversion rate and high activity

Inactive Publication Date: 2017-12-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is that the preparation of the catalyst in the prior art is complicated, the reaction temperature is relatively high, and the problem of high energy consumption; a new method for preparing 3-hydroxypropionate methyl ester is provided, which has a catalyst The advantages of simple preparation, stable properties, low cost and mild reaction

Method used

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  • Preparation method of methyl-3-hydroxypropanoate
  • Preparation method of methyl-3-hydroxypropanoate
  • Preparation method of methyl-3-hydroxypropanoate

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Add 5 mmol of ionic liquid A, 5 mmol of ferric chloride, and 40 mL of acetone into a 100 mL reaction tube, and react at room temperature for 12 hours. After the reaction was completed, the solvent acetone was removed under reduced pressure, and catalyst A was obtained after vacuum drying.

[0034]

[0035] Add 1 mmol of Catalyst A to a 100 mL reactor, purged the reactor three times with nitrogen, added 10 mmol of ethylene oxide and 30 mL of methanol, introduced carbon monoxide to make the system pressure 5.0 MPa, and reacted at 60°C for 3 hours. After the reaction was completed, the reactor body was fully cooled to 0°C, and the pressure was slowly released to normal pressure. The reactor was purged three times with nitrogen, and samples were taken for analysis. The experimental results are shown in Table 1.

Embodiment 2

[0037] Add 5 mmol of ionic liquid B, 5 mmol of ferric chloride, and 40 mL of tetrahydrofuran into a 100 mL reaction tube, and react at room temperature for 12 hours. After the reaction was completed, the solvent tetrahydrofuran was removed under reduced pressure, and catalyst B was obtained after vacuum drying.

[0038]

[0039] Add 1mmol of Catalyst B to a 100mL reactor, purge the reactor with nitrogen three times, add 20mmol of ethylene oxide and 30mL of methanol, and introduce carbon monoxide to make the system pressure 8.0MPa, and react at 45°C for 8 hours. After the reaction was completed, the reactor body was fully cooled to 0°C, and the pressure was slowly released to normal pressure. The reactor was purged three times with nitrogen, and samples were taken for analysis. The experimental results are shown in Table 1.

Embodiment 3

[0041] Add 5 mmol of ionic liquid C, 5 mmol of ferric chloride, and 40 mL of acetone into a 100 mL reaction tube, and react at room temperature for 12 hours. After the reaction was completed, the solvent acetone was removed under reduced pressure, and catalyst C was obtained after vacuum drying.

[0042]

[0043] Add 1mmol of Catalyst C to a 100mL reactor, purge the reactor with nitrogen three times, add 30mmol of ethylene oxide and 30mL of methanol, feed in carbon monoxide, make the system pressure 3.0MPa, and react at 100°C for 6 hours. After the reaction was completed, the reactor body was fully cooled to 0°C, and the pressure was slowly released to normal pressure. The reactor was purged three times with nitrogen, and samples were taken for analysis. The experimental results are shown in Table 1.

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Abstract

The invention relates to a preparation method of methyl-3-hydroxypropanoate and mainly aims at solving the problems of complex catalyst preparation, relatively high reaction temperature and high energy consumption in the prior art. The technical problems are better solved by adopting the technical scheme that the preparation method of methyl-3-hydroxypropanoate comprises the following steps: a) reacting an ionic liquid and iron chloride in a solvent to obtain a catalyst; and b) reacting ethylene oxide, carbon monoxide and methanol in the existence of the catalyst to obtain methyl-3-hydroxypropanoate, wherein the ionic liquid has the following structure shown as the specification, X is selected from halogens, and R1 and R2 are independently selected from alkyl, alkenyl, cyclo, aryl or substituted aryl; and the preparation method can be used for industrial production of methyl-3-hydroxypropanoate.

Description

technical field [0001] The invention relates to a method for preparing methyl 3-hydroxypropionate, in particular to a method for preparing methyl 3-hydroxypropionate with ethylene oxide and synthesis gas as raw materials. 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...

Claims

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Application Information

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IPC IPC(8): C07C67/37C07C69/675B01J31/30B01J31/02
CPCB01J31/0284B01J31/30C07C67/37C07C69/675Y02P20/54
Inventor 刘波李晓明吕建刚金照生黄祖娟赵帅
Owner CHINA PETROLEUM & CHEM CORP
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