Preparation method of 1, 3-propanediol

A technology of propylene glycol and propylene, which is applied in the field of preparation of 1,3-propylene glycol, can solve the problems of high cost, high energy consumption, unfavorable large-scale production, etc., and achieves the effect of low cost and high benefit

Inactive Publication Date: 2014-04-09
DALIAN LONGTAI TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis method and product separation method of the products in the above processes are either too complicated, or the reagents used are toxic, costly, or have problems such as large energy consumption and serious environmental pollution, which are not conducive to large-scale production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] ①Synthesis of 1-bromo-3-chloropropane: Weigh 38.3 grams (0.5 moles) of 3-chloro-1-propene, 0.2 grams (0.01 moles) of benzoyl peroxide and 160 grams (1 mol), respectively added to the dropping funnel; three dropping funnels were placed on the top of the packed tower, and the bottom of the packed tower was connected to a four-necked reaction flask. Under normal pressure, dry hydrogen bromide was introduced from the bottom of the tower at a flow rate of 2 liters / hour until the hydrogen bromide gas in the packed tower was 11.5 liters, and then the material in the dropping funnel was added dropwise to the packed tower.

[0041]Control the reaction temperature at 10-20°C, return the unqualified part to the upper part and add it again, and analyze it by gas chromatography normalization method until the content of 3-chloro-1-propene at the bottom of the packed tower is lower than 0.1% according to gas chromatography analysis.

[0042] ②Synthesis of 1,3-propanediol: Prepare sodi...

Embodiment 2

[0046] ①Synthesis of 1-bromo-3-chloropropane: Weigh 77 grams (1 mole) of 3-chloro-1-propene, 0.2 grams (0.01 moles) of benzoyl peroxide and 240 grams (1.5 moles) of 1-bromo-3-chloropropane mol), respectively added to the dropping funnel; three dropping funnels were placed on the top of the packed tower, and the bottom of the packed tower was connected to a four-necked reaction flask. Under normal pressure, dry hydrogen bromide is introduced from the bottom of the tower at a flow rate of 2 liters / hour until the hydrogen bromide gas in the packed tower is 23 liters, and then the material in the dropping funnel is added dropwise to the packed tower. Control the reaction temperature at 10-20°C, return the unqualified part to the upper part and add it again, and analyze it by gas chromatography normalization method until the content of 3-chloro-1-propene at the bottom of the packed tower is lower than 0.1% according to gas chromatography analysis.

[0047] ② Synthesis of 1,3-propan...

Embodiment 3

[0050] ①Synthesis of 1-bromo-3-chloropropane: Weigh 41 grams (0.6 moles) of 3-chloro-1-propene, 0.2 grams (0.01 moles) of benzoyl peroxide and 160 grams (1 mol), respectively added to the dropping funnel; three dropping funnels were placed on the top of the packed tower, and the bottom of the packed tower was connected to a four-necked reaction flask. Under normal pressure, dry hydrogen bromide is passed from the bottom of the tower at a flow rate of 2 liters / hour until the hydrogen bromide gas in the packed tower is 14 liters, and then the material in the dropping funnel is added dropwise to the packed tower. Control the reaction temperature at 10-20°C, return the unqualified part to the upper part and add it again, and analyze it by gas chromatography normalization method until the content of 3-chloro-1-propene at the bottom of the packed tower is lower than 0.1% according to gas chromatography analysis.

[0051] ② Synthesis of 1,3-propanediol: prepare aqueous sodium hydroxi...

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PUM

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Abstract

The invention relates to a preparation method of 1, 3-propanediol, belonging to the field of synthesis of chemical products. The preparation method of 1, 3-propanediol comprises the following steps: (1) synthesizing 1-bromo-3-chloropropane: enabling 3-chloro-1-propene, hydrogen bromide and benzoyl peroxide to react according to the molar ratio of 1: 1: (0.001-0.03) to obtain 1-bromo-3-chloropropane; (2) synthesizing 1, 3-propanediol: enabling 1-bromo-3-chloropropane, sodium hydroxide and water to react according to the molar ratio of 1: (1.9-2.5): (4-15) under the conditions that the reaction pressure is not more than 0.5MPa and the reaction temperature is 120-140 DEG C. According to the preparation method provided by the invention, although bromine is taken as a reaction raw material, bromine can be recycled, the production of three wastes is low, and the obtained product has the advantages of low cost and high benefits and can completely realize large-tonnage production.

Description

technical field [0001] The invention relates to a preparation method of 1,3-propanediol, which belongs to the field of chemical product synthesis. Background technique [0002] 1,3-Propanediol is an important chemical raw material widely used in cosmetics, liquid detergents, antifreeze, clothing, interior decoration materials, engineering polymers and many other fields. As a diol containing two functional groups, 1,3-propanediol can be used in a variety of organic synthesis reactions, especially as a monomer for the synthesis of polyesters, polyethers and polyurethanes. One of its most important uses Polytrimethylene terephthalate is formed with terephthalic acid. This polyester has excellent performance and broad application prospects. [0003] Currently, there are three types of preparation methods for 1,3-propanediol. One is International Shell Research Co., Ltd. Patent No. CN1216034, ethylene oxide, carbon monoxide and hydrogen can effectively generate the intermediate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/09C01D3/04
CPCC07C29/09C07C17/087
Inventor 王刃郑学胜宋立刚毕书有孙业飞袁麟
Owner DALIAN LONGTAI TECH DEV
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