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Method for catalytically synthesizing propylene glycol monomethyl ether by using solid base catalyst [Smim]X/SBA-15

A solid base catalyst, propylene glycol methyl ether technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of reducing reaction temperature, propylene oxide conversion rate High, poor repetition effect and other problems, to achieve the effect of less dosage, high catalytic activity, good repeated use effect

Inactive Publication Date: 2016-09-28
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Jing Xiaoxiao (Fine Chemical Industry 2013, 30(3): 304-307) used titanate nanofibers as a carrier, and used an impregnation method to support alkali metal halides as a solid base catalyst, and catalyzed propylene oxide and methanol to prepare propylene glycol methyl ether. The reaction temperature is reduced, the reaction time is shortened, and it shows good base catalytic activity, but the catalyst is easy to lose, and the repetition effect is not good
Patent CN103012077A discloses a method of catalyzing the alcoholysis of propylene oxide to prepare propylene glycol methyl ether. Propylene oxide, methanol, solvent and catalyst are mixed and contacted, and the catalyst is characterized in that the catalyst contains polymetallic oxoacid or polymetallic oxoacid And titanium silicon molecular sieve, this method has a high conversion rate of propylene oxide and good selectivity of propylene glycol methyl ether, but it needs to add acetonitrile, acetone and other organic solvents, which have a certain impact on the separation of products
Patent CN103008007A discloses a resin-type solid base catalyst for the synthesis of propylene glycol methyl ether, which is an ion-exchange resin of styrene-divinylbenzene copolymer of a nitrogen-containing heterocyclic quaternary ammonium base, but the preparation method is complicated and the reaction takes a long time

Method used

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  • Method for catalytically synthesizing propylene glycol monomethyl ether by using solid base catalyst [Smim]X/SBA-15
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  • Method for catalytically synthesizing propylene glycol monomethyl ether by using solid base catalyst [Smim]X/SBA-15

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Experimental program
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Effect test

Embodiment 1

[0033] (1) In inert gas N 2 protection, at 25°C, add 10g of SBA-15 mesoporous material and 200ml of toluene into the reactor in turn, stir and mix for 2h, then add 6g of coupling agent 3-chloropropyltriethoxysilane, stir and reflux at 110°C After 24 hours, cool to 25° C., filter, wash with dichloromethane, and dry the filter cake in a vacuum oven at 70° C. for 24 hours to obtain SBA-15 mesoporous material loaded with chlorosilane. In inert gas N 2 Protection, at 30°C, add 10g of the above-prepared SBA-15 mesoporous material loaded with chlorosilane, 6.7g of 1-methylimidazole and 200ml of toluene into the reactor, stir and mix for 2h, then stir and reflux at 110°C for 24h , cooled to 25°C, filtered, washed with dichloromethane, and dried in a vacuum oven at 70°C for 24 hours to obtain 1-propyl (triethoxysilyl)-3 methylimidazolium chloride SBA-15 mesoporous material [Smim]Cl / SBA-15.

[0034] (2) At 25°C, 10 g of the above prepared SBA-15 mesoporous material [Smim]Cl / SBA-15 lo...

Embodiment 2

[0037] Embodiment 2 The operating steps are the same as in Example 1, and the difference is that the alkaline substance added in the preparation catalyst step (2) is KOAc, and the prepared solid base catalyst is [Smim]OAc / SBA-15 to obtain synthetic propylene glycol methyl ether The mass yield of the product is 79.24%, and the mass percentage content of the isomer 1-methoxy-2-propanol (primary ether) is 86.47%.

Embodiment 3

[0038] Example 3 The operation steps are the same as in Example 1, the difference is that the basic substance added in the preparation of the catalyst step (2) is CH 3 ONa, the solvent are methanol, and the prepared solid base catalyst is [Smim]OCH 3 / SBA-15, the mass yield of the synthetic propylene glycol methyl ether product is 90.25%, wherein the mass percentage of isomer 1-methoxy-2-propanol (primary ether) is 94.46%.

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PUM

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Abstract

The invention discloses a method for catalytically synthesizing propylene glycol monomethyl ether by using a solid base catalyst [Smim]X / SBA-15. The catalyst is prepared by supporting and modification by the following steps: bonding a coupling agent 3-propyltriethoxysilane to an SBA-15 mesoporous material through silicon-oxygen bonds to obtain a supported chlorosilane-containing SBA-15 mesoporous material, carrying out N-alkylation reaction on 1-methylimidazole and the prepared supported chlorosilane-containing SBA-15 mesoporous material, impregnating in an alkaline matter solution for modification, and drying. The supported alkaline matter can do small damage to the SBA-15 mesoporous material structure and enhances the alkali strength of the catalyst, so that the catalyst has the advantages of high catalytic activity and low consumption and can be easily separated from the reaction system. The catalyst can be reused after being dried and recovered, and has higher yield for catalyzing synthesis of propylene glycol monomethyl ether from epoxypropane and methanol and higher content of isomer 1-methoxy-2-propanol(primary ether).

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and relates to a method for synthesizing propylene glycol methyl ether from propylene oxide and methanol with a solid base catalyst [Smim]X / SBA-15. Background technique [0002] Propylene glycol methyl ether is an excellent solvent with low volatility, high flash point and strong solvency. The molecular structure and physical and chemical properties of propylene glycol methyl ether are similar to those of ethylene glycol ether, and it is considered as a substitute for ethylene glycol ether. Industrially use propylene oxide and methanol as raw materials to synthesize propylene glycol methyl ether. Due to the different ring-opening orientations of propylene oxide, there are two isomers of propylene glycol methyl ether in the synthetic product, namely 1-methoxy-2-propanol (primary ether) and 2-methoxy-1-propanol (secondary ether), the former is less toxic than the latter. Therefore, how to sy...

Claims

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Application Information

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IPC IPC(8): C07C41/03C07C43/13B01J31/02
CPCB01J31/0275B01J2231/34C07C41/03C07C43/13
Inventor 刘跃进李蒙刘宁李姗姗吴志民骆战涛徐文质周健李勇飞潘浪胜
Owner XIANGTAN UNIV