Method for catalytic synthesis of 1,3-dibasic alcohol or cyclic acetal of 1,3-dibasic alcohol by using ionic liquid

A technology of cyclic acetals and acidic ionic liquids, applied in chemical instruments and methods, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve the problems of many side reactions, complex processes, strong corrosiveness of catalysts, etc., and achieve easy operation , simple process, low catalyst corrosion effect

Inactive Publication Date: 2010-03-10
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the defects of strong catalyst corrosion, many side reactions and complicated process in the prior art, and provide an ionic liquid to catalyze the condensation reaction of formaldehyde and olefin to synthesize 1,3-di Alcohol or its cyclic acetal (1,3-dioxane derivatives) method

Method used

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  • Method for catalytic synthesis of 1,3-dibasic alcohol or cyclic acetal of 1,3-dibasic alcohol by using ionic liquid
  • Method for catalytic synthesis of 1,3-dibasic alcohol or cyclic acetal of 1,3-dibasic alcohol by using ionic liquid

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Experimental program
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Effect test

Embodiment 1

[0030] Add 0.42g ionic liquid [MBsIm][CF in the high-pressure reactor of 30mL 3 SO 3 ] and 15.4g 37% formaldehyde solution, airtight reactor, with the air in the nitrogen replacement reaction system of 2.0MPa, charge into 5.6g ethylene, be filled with nitrogen to 3.0MPa. Stir, heat up to 80°C within 30 minutes, and react for 8 hours under the condition of 8.0MPa. After the reaction, cool to room temperature and release the pressure. GC analysis, quantification by internal standard method. The conversion rate of formaldehyde is 99.2%, the selectivity of 1,3-dioxane is 83.9%, the selectivity of 1,3-propanediol is 12.3%, target product 1,3-dioxane and 1,3- The overall selectivity to propylene glycol was 96.2%.

Embodiment 2

[0032] With embodiment 1. React at 100°C, the conversion rate of formaldehyde is 78.4%, the selectivity of 1,3-dioxane is 31.5%, the selectivity of 1,3-propanediol is 67.5%, and the target product 1,3-dioxane The overall selectivity to cyclic and 1,3-propanediol was 99.0%.

Embodiment 3

[0034] With embodiment 1. With ionic liquid [MBsIm][HSO 4 ] as a catalyst, reacted at 100°C, the conversion rate of formaldehyde was 82.5%, the selectivity of 1,3-dioxane was 11.9%, the selectivity of 1,3-propanediol was 86.1%, and the target product 1,3 - The overall selectivity to dioxane and 1,3-propanediol is 98.0%.

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Abstract

The invention discloses a method for synthesizing 1,3-dibasic alcohol or cyclic acetal of 1,3-dibasic alcohol(1,3-dioxane derivative)by using a functional acid ionic liquid serving as a catalyst to catalyze the condensation reaction of formaldehyde and alkene. In the method, the aqueous solution of formaldehyde and the alkene are used as reactants to the 1,3-dibasic alcohol or cyclic acetal of 1,3-dibasic alcohol(1,3-dioxane derivative) under a mild reaction condition in the presence of the functional acid ionic liquid serving as the catalyst. The method has the advantages of readily availablereaction materials, low-corrosivity high-catalytic activity reusable catalyst, high product selectivity, simple reaction process, easy operation and strong controllability.

Description

technical field [0001] The invention relates to a method for synthesizing 1,3-dibasic alcohol or its cyclic acetal (1,3-dioxane derivative) by catalyzing the condensation reaction of formaldehyde and olefin by using functionalized acidic ionic liquid as a catalyst. Background technique [0002] 1,3-diol has the characteristics of odorless, low toxicity, and good water solubility. It is mainly used as a monomer for polyester and polyurethane, as well as a solvent, antifreeze or protective agent, and can also be directly used as a wetting agent and softening agent. agent. It is widely used in fine chemical industry, medicine, dyestuff and other fields. Especially 1,3-propanediol, as the main raw material for the production of polytrimethylene terephthalate (PTT), is currently a hot spot in the development of synthetic fibers in the world. PTT is a new type of polyester material with excellent resilience, dyeability, and stain resistance. It has broad application prospects in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/38C07D319/06B01J31/04
CPCY02P20/584
Inventor 陈静宋河远夏春谷唐中华
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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