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Method for catalysis synthesis of glycerol formal by gemini dication acidic ion liquid

A technology of acidic ionic liquid and glycerin formal, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve uneven distribution of active centers and long reaction time and other problems, to achieve the effect of less catalyst consumption, simple post-treatment and high product selectivity

Inactive Publication Date: 2011-02-02
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

However, these catalytic systems have inherent disadvantages of heterogeneous catalysis: uneven distribution of active centers and long reaction time (Deutsch J, Martin A, Lieske H.J.Catal., 2007, 245:428)

Method used

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  • Method for catalysis synthesis of glycerol formal by gemini dication acidic ion liquid
  • Method for catalysis synthesis of glycerol formal by gemini dication acidic ion liquid
  • Method for catalysis synthesis of glycerol formal by gemini dication acidic ion liquid

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Experimental program
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Effect test

Embodiment 1

[0033] Add glycerin 18.4g (0.2mol) successively in the 100ml round bottom flask that has water trap, reflux condenser, 37% formaldehyde aqueous solution 19.4g (0.24mol), ionic liquid 1 (5 * 10 -4 mol), with water agent cyclohexane, reflux at 100°C for 4 hours. After the reaction solution was processed and added with an internal standard, the yield of the product by GC quantitative analysis was 85.1%, and the ratio of I and II in the product was 73:27.

Embodiment 2

[0035] Add glycerol 18.4g (0.2mol) successively in the 100ml round bottom flask that has water trap, reflux condenser, 37% formaldehyde aqueous solution 19.4g (0.24mol), ionic liquid 2 (2 * 10 -4 mol), with water agent cyclohexane, reflux at 100°C for 4 hours. After the end, the reaction solution was treated and added with an internal standard, and the yield of the product was 98.7% according to GC quantitative analysis, and the ratio of I and II in the product was 85:15.

Embodiment 3

[0037] Add glycerin 18.4g (0.2mol) successively in the 100ml round bottom flask that has water separator, reflux condenser, 37% formaldehyde aqueous solution 19.4g (0.24mol), ionic liquid 3 (2 * 10 -3 mol), with water agent cyclohexane, reflux at 100°C for 4 hours. After the reaction solution was processed and added with an internal standard, the yield of the product by GC quantitative analysis was 81.9%, and the ratio of I and II in the product was 59:41.

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Abstract

The invention discloses a method for catalysis synthesis of glycerol formal by gemini dication acidic ion liquid. In the method, gemini dication acidic ion liquid is used as catalyst, glycerol and formaldehyde solution are taken as reactant, cyclohexane is taken as water-carrying agent, and the raw material is subject to catalysis synthesis at the temperature of 40-120 DEG C to obtain glycerol formal. The method has moderate reaction condition, low catalyst corrosivity, high catalytic activity, high product selectivity, simple operation process and strong controllability and can be reused.

Description

technical field [0001] The invention relates to a method for synthesizing glycerol formal by catalyzing the reaction of glycerol and formaldehyde aqueous solution with geminal dianion acidic ionic liquid. Background technique [0002] Glycerol formal is a new type of pharmaceutical solvent, an important substitute for glycerin and propylene glycol, and can be used in the pharmaceutical manufacturing industry, animal non-aqueous injections (ivermycin, nimesulide), injection liquid solvents (long-acting oxytetracycline , sulfa), paint industry, cosmetics, printing ink manufacturing, foundry and insecticide manufacturing, etc. In particular, the raw material formaldehyde solution and glycerin for preparing the substance have a wide range of sources and are cheap. One of its isomers, the six-membered ring product I, can be hydrolyzed after catalytic hydrogenation and selective oxidation to obtain important chemical products 1,3-propanediol and 1,3-dihydroxyacetone. Glycerol fo...

Claims

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Application Information

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IPC IPC(8): C07D317/20B01J31/02C07D319/06
CPCY02P20/584
Inventor 陈静李臻夏春谷
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI