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Synthesis method of propylene glycol ether

A synthetic method and technology of propylene glycol ether, which is applied in the fields of ether preparation, alkylene oxide preparation ether, organic chemistry, etc., can solve the problems of low proportion of primary ether, poor selectivity, poor activity and stability, etc., and achieve high catalytic activity and selectivity high effect

Inactive Publication Date: 2009-03-11
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the homogeneous catalyst is characterized by uniform acid-base strength and high catalytic efficiency, but there are many disadvantages in the homogeneous catalytic reaction, such as separation of product and catalyst, waste liquid treatment and equipment corrosion.
The solid acid catalyst has higher activity and stability, but the ratio of primary ether in the product is low and the selectivity is poor.
The solid basic catalysts currently reported mainly include alkaline hydrotalcite, anion hydroxide clay, anion exchange resin, magnesium aluminum composite hydroxide and alkali metal exchange molecular sieve, which have the characteristics of high selectivity and easy separation of primary ethers, but Activity and stability are relatively poor

Method used

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  • Synthesis method of propylene glycol ether
  • Synthesis method of propylene glycol ether

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Preparation of zinc-magnesium-aluminum hydrotalcite (ZnMgAl-HTlc) products

[0014] Add 150 g of H to a 1 L three-necked flask 2 O, 24.8g NaOH and 3.0g Na 2 CO 3 , after stirring evenly at 70°C, dropwise add 150g of H 2 O, 2.38g Zn(NO 3 ) 2 6H 2 O, 61.6gMg(NO 3 ) 2 ·6H 2 O, 18.0g Al(NO 3 ) 3 9H 2 The mixed solution of O, the dropping time is 0.5h, the pH value of the solution is controlled at 8, after the dropping, continue to stir for 15h to nucleate and crystallize, then cool, filter, wash to neutral, vacuum dry at 70°C for 7h, 450 ℃ roasting for 4h to obtain the product A1.

Embodiment 2

[0016] Preparation of FeMgAl-HTlc Products

[0017] Add 150 g of H to a 1 L three-necked flask 2 O, 24.8g NaOH and 3.0g Na 2 CO 3 , after stirring evenly at 70°C, dropwise add 150g of H 2 O, 3.5g Fe(NO 3 ) 3 9H 2 O, 61.6gMg(NO 3 ) 2 ·6H 2 O, 18.0g Al(NO 3 ) 3 ·6H 2 The mixed solution of O, the dropwise addition time is 0.5h, the pH value of the solution is controlled at 8, after the dropwise addition, continue to stir for 15h to nucleate and crystallize, then cool, filter, wash to neutral, vacuum dry at 90°C for 6h, 450 ℃ roasting for 4h to obtain the product A2.

Embodiment 3

[0019] Add methanol and propylene oxide at a molar ratio of 5:1, and catalyst A1 with an amount of 1.35% into the autoclave, purged with nitrogen for 10 minutes, and heated to 120° C. under stirring conditions, and the pressure was 1 MPa, and reacted for 3 hours. Propylene Glycol Ether.

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Abstract

This invention relates to a propylene glycol ether preparation method. Add Methanol and propylene oxide in the molar ratio of 1 ~ 6:1, and the amount of 1 ~ 2.5% (w) of ternary hydrotalcite products into high-pressure reactor; the nitrogen blow for 10 ~ 15 min; under mixing conditions, warming up to 100~ 140 deg C, pressure 1-2MPa, and taking reaction for 4h, to obtain propylene glycol ethers. Feature of this invention: solid base catalyst has high catalytic activity and higher selectivity of ether.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a synthesis method of propylene glycol ether. Background technique [0002] Alcohol ether compounds are one of the important industrial derivatives of epoxy compounds and a class of fine chemical products with a wide range of uses, known as "universal solvents". Alcohol ether products are divided into two series, propylene glycol ether (P-series) and ethylene glycol ether (E-series), and E-series alcohol ether products have always been dominant. However, since the European Center for Chemical Industry and Toxicology (E-CETOC) published a report on the toxicity of ethylene glycol ethers in 1982, propylene glycol ethers are gradually replacing ethylene glycol ethers because of their low toxicity and similar physical and chemical properties to ethylene glycol ethers. alcohol ether. [0003] There are many synthetic routes of propylene glycol ether, among which, the simp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/03C07C43/10
Inventor 杨建国程文萍于心玉刘玲梁学正刘彩华王雯娟何鸣元
Owner EAST CHINA NORMAL UNIV