Preparation method of 1, 1-dialkoxy alkane

A technology of alkyl and methyl, applied in the field of preparation of 1,1-dialkoxyalkane, can solve the problem of low yield of acetal

Active Publication Date: 2021-04-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above research shows that when molecular sieve is used as catalyst, the yield of acetal is low

Method used

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  • Preparation method of 1, 1-dialkoxy alkane
  • Preparation method of 1, 1-dialkoxy alkane
  • Preparation method of 1, 1-dialkoxy alkane

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preparation example Construction

[0015] According to the present invention, the preparation method of the 1,1-dialkoxyalkane comprises: in the presence of a catalyst, R 1 -OH Alcohol and R 2 For the contact reaction of aldehydes represented by CHO, the catalyst is a molecular sieve with a hydrogen type EWT structure.

[0016] According to the invention, in the presence of a catalyst, R 1 -OH Alcohol and R 2 The aldehyde represented by -CHO undergoes a condensation reaction to obtain R 2 -CH-(OR 1 ) 2 Acetals, that is, 1,1-dialkoxyalkanes.

[0017] According to the present invention, R 1 The alcohol shown in -OH can be a monohydric alcohol conventionally used in the art, for example, R 1 It may be a C1-C5 alkyl group, specifically, a methyl group, an ethyl group, a propyl group, a butyl group or a pentyl group. Alcohol R 1 Specific examples of -OH include, but are not limited to, methanol, ethanol, propanol, butanol, or pentanol.

[0018] According to the present invention, R 2 R in the aldehyde rep...

Embodiment approach

[0024] According to a specific embodiment of the present invention, the preparation method of the catalyst comprises: performing ammonium exchange on the raw EWT molecular sieve powder in an ammonium salt aqueous solution at 80-90°C, drying and calcining at 500-600°C for 1-5 hours ; Wherein, the ammonium salt is selected from one or more of ammonium nitrate, ammonium chloride and ammonium sulfate.

[0025]According to the present invention, the raw powder of molecular sieve with EWT structure can be obtained commercially, or can be prepared according to conventional methods in this field, such as the method disclosed in CN109422627A.

[0026] According to the present invention, the R 1 -OH Alcohol and R 2 The conditions of the aldehyde contact reaction shown in -CHO generally include reaction temperature and reaction pressure, wherein, the reaction temperature will ensure that R 1 -OH Alcohol and R 2 -CHO can undergo a condensation reaction under the catalysis of the cataly...

preparation example 1

[0044] Add 23.35g template agent R (1,5-bis(N-propylpyrrolidinium) pentane dihydroxide) aqueous solution (the content of R is 25% by mass) into a 45mL polytetrafluoroethylene container, add 1.25g sodium metaaluminate and 7.67g deionized water, stirred for 30 minutes until uniform, then added 9.64g solid silica gel (SiO 2 content is 93.37% by mass), stirred for 5 minutes and fully mixed, wherein the molar ratio of each component is: SiO 2 / Al 2 o 3 =90,H 2 O / SiO 2 =9.82, template R / SiO 2 = 0.15, OH - / SiO 2 = 0.08.

[0045] The above mixture was put into a 45mL polytetrafluoroethylene-lined steel autoclave, covered and sealed, and the autoclave was placed in a rotating convection oven with the rotation speed set at 20rpm, and reacted at 150°C for 5 days. Take out the autoclave and let it cool down to room temperature quickly, separate the mixture on a 5000rpm high-speed centrifuge, collect the solid, wash it thoroughly with deionized water, and dry it at 100°C for 5 hou...

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Abstract

The invention relates to the field of catalytic chemistry, and discloses a preparation method of 1, 1-dialkoxy alkane, the preparation method is as follows: in the presence of a catalyst, subjecting alcohol as shown in R1OH and aldehyde as shown in R2-CHO to a contact reaction, wherein the catalyst is a hydrogen type EWT structure molecular sieve, R1 is methyl, ethyl, propyl, butyl or pentyl, and R2 is hydrogen, methyl, ethyl, propyl or butyl. According to the method, a molecular sieve type catalyst with a hydrogen type EWT structure is adopted and has higher reaction activity and better acetal yield.

Description

technical field [0001] The present invention relates to the catalytic chemical technology, in particular to the preparation method of 1,1-dialkoxyalkane. Background technique [0002] EWT structural molecular sieve has a 3-dimensional 21-membered ring channel structure. It is the first synthesized silicon-alumina molecular sieve with an ultra-large pore structure. It has a stable structure and can be used in the industry to catalyze and separate macromolecular reactions. EWT structural molecular sieves were first synthesized by ExxonMobil in the United States. At present, there are few reports on the application of molecular sieves with EWT structure. CN109422627A discloses that a catalyst containing molecular sieve with EWT structure is applied to the catalytic reaction of glycerin etherification to prepare tert-butyl glycerol ether. Specifically, a method for preparing tert-butylglycerol ether by glycerin etherification is disclosed, the method comprises contacting glyce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/50C07C43/303B01J29/70B01J35/10
CPCC07C41/50B01J29/70B01J35/10C07C43/303
Inventor 谢明观王永睿慕旭宏
Owner CHINA PETROLEUM & CHEM CORP
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