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Method for preparing isosorbide from sorbitol

A technology for isosorbide and sorbitol, which is applied in the field of chemical preparation, can solve the problems of easy coking in a fixed bed and many by-products, and achieves the effects of avoiding condensation coking, reducing by-products, and improving reaction effect.

Pending Publication Date: 2022-05-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process needs to be operated under reduced pressure, and the liquid phase sorbitol is easy to coke when it enters the fixed bed, and there are many by-products in the obtained crude product

Method used

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  • Method for preparing isosorbide from sorbitol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 8g of sorbitol, 5mL of water, and 60mL of toluene into the autoclave, add 0.8g of H-β molecular sieves, and blow with nitrogen. The reaction temperature was raised to 130° C., the rotation speed was 300 rpm, and the reaction was carried out for 1.5 hours, and then the reaction temperature was raised to 180° C., and the reaction was carried out for 1.5 hours. After cooling down, the solid acid catalyst was separated by filtration, the filtrate was allowed to stand for stratification, and the clarified liquid in the lower layer was dehydrated and evaporated to dryness, and the crude isosorbide was melted and crystallized at 110°C to obtain high-purity isosorbide.

Embodiment 2

[0031] Take 8g of sorbitol, 2.4mL of water, and 28mL of toluene into the autoclave, add 0.4g of H-β molecular sieve, and blow nitrogen for 3 times. The reaction temperature was raised to 130° C., the rotation speed was 300 rpm, and the reaction was carried out for 1.5 hours, and then the reaction temperature was raised to 180° C., and the reaction was carried out for 1.5 hours. After cooling down, the solid acid catalyst was separated by filtration, the filtrate was allowed to stand for stratification, and the clarified liquid in the lower layer was dehydrated and evaporated to dryness, and the crude isosorbide was melted and crystallized at 110°C to obtain high-purity isosorbide.

Embodiment 3

[0033] Take 8g of sorbitol, 12mL of water, and 80mL of toluene into the autoclave, add 2.4g of H-β molecular sieve, and blow nitrogen for 3 times. The reaction temperature was increased to 130° C., the rotation speed was 300 rpm, and the reaction was performed for 1.5 hours. The reaction temperature was increased to 180° C., and the reaction was performed for 1.5 hours. After cooling down, the solid acid catalyst was separated by filtration, the filtrate was allowed to stand for stratification, and the clarified liquid in the lower layer was dehydrated and evaporated to dryness, and the crude isosorbide was melted and crystallized at 110°C to obtain high-purity isosorbide.

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Abstract

The invention relates to a method for preparing isosorbide from sorbitol, which comprises the following steps: by taking sorbitol as a raw material, adding a solid acid catalyst and an organic solvent for full contact, adding a small amount of water, reacting at a certain temperature, filtering and recovering the solid acid catalyst after the reaction is finished, standing and layering filtrate, taking lower-layer clear liquid, and dehydrating to obtain a crude product of isosorbide; and carrying out melt crystallization to obtain an isosorbide product. According to the reaction characteristics of preparation of isosorbide from sorbitol, a specific solid acid catalyst and a solvent system are selected, a high-quality isosorbide product is obtained by combining melt crystallization, and the method has the advantages of high yield, low chromaticity, low energy consumption and the like.

Description

technical field [0001] The invention belongs to the field of chemical preparation, and in particular relates to a method for preparing isosorbide from sorbitol. Background technique [0002] As an important material and chemical intermediate for future bioenergy, isosorbide has been widely used in the pharmaceutical, food and chemical material industries. Due to the rigid structure and chiral structure characteristics of its molecules, the prepared polymer materials such as isosorbide carbonate have excellent mechanical properties, and have become a research hotspot at home and abroad. Isosorbide is mainly prepared from sorbitol through acid-catalyzed dehydration twice. At present, sulfuric acid is used as a catalyst in industry, and isosorbide is prepared by "one-pot" dehydration reaction. The liquid acid has great damage to the equipment, and there are many by-products, and the post-treatment process is many and complicated, which makes the production cost of isosorbide h...

Claims

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Application Information

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IPC IPC(8): C07D493/04B01J29/70B01J37/10B01J37/08B01J29/18B01J29/08
CPCC07D493/04B01J29/7007B01J37/10B01J37/08B01J29/18B01J29/084
Inventor 白毓黎张通白富栋李澜鹏彭绍忠
Owner CHINA PETROLEUM & CHEM CORP