Method for separating sugar alcohol dehydration reaction product by adding hydrophobic ionic liquid under reduced pressure distillation

A technology of ionic liquid and dehydration reaction, applied in the direction of organic chemistry, etc., can solve the problems of low volatility, reduced yield of isosorbide, intensified carbonization, etc., and achieve the goal of reducing carbonization, improving distillation yield and purity, and reducing loss Effect

Active Publication Date: 2020-06-02
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Recently, Jie Deng et al. (Catal.Sci. Technol, 2017, 7, 2065) disclosed a process for preparing isosorbide by dehydration of sorbitol using acidic ionic liquid as a catalyst. The low volatility of ionic liquid can be used for neutralization without alkali Catalyst directly distills the reaction solution to purify the reaction product, but in the distillation process, the high temperature and low pressure make the carbonization of the reactant and the reaction product intensified, reducing the yield of isosorbide

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  • Method for separating sugar alcohol dehydration reaction product by adding hydrophobic ionic liquid under reduced pressure distillation

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Experimental program
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Effect test

Embodiment 1

[0022] figure 1 The schematic flow chart of the embodiment of the present invention, the flow process is as follows:

[0023] 1) Sorbitol and catalyst reaction:

[0024] Add 36.4 g of sorbitol into a 100 mL three-neck flask with a magnetic sub, and heat to 130 oC After melting the sorbitol, add 0.364 g of 1-sulfopropyl-3-methylimidazolium tetrafluoroborate ionic liquid, and react under a pressure of 4 kPa for 4 h to obtain a reaction product;

[0025] 2) Add hydrophobic ionic liquid to the reaction product

[0026] After the reaction was completed, 36.4 g of 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid was added, and after mixing evenly, the temperature of the system was gradually raised to 160 o C, the pressure drops to 20 Pa, collect 120 o Fraction C, when the temperature of the fraction increases, the reaction is stopped, and the quality of isosorbide collected by weighing is 25.1 g, the purification yield is 86%, and the component content analyzed by high...

Embodiment 2

[0029] Add 36.4 g of sorbitol into a 100 mL three-neck flask with a magnetic sub, and heat to 130 oC After the sorbitol was melted, 0.3640 g of 1-sulfopropyl-3-methylimidazolium bisulfate ionic liquid was added and reacted for 4 h under a pressure of 4 kPa; after the reaction was completed, 36.4 g of 1-butyl-3-methylimidazolium bis Trifluoromethanesulfonimide salt ionic liquid, after mixing evenly, the system temperature is gradually raised to 160 o C, the pressure drops to 20 Pa, collect 120 o Fraction C, when the fraction temperature rises, the reaction is stopped, and the quality of isosorbide collected by weighing is 24.2 g, the purification yield is 83%, and the component content analyzed by high performance liquid chromatography is 99.98%.

[0030] After the distillation is completed, cool the system to room temperature, add 50 mL of dichloromethane, mix evenly, add 30 mL of deionized water to shake and extract, and then let it stand still. After the phase separation is...

Embodiment 3

[0032] Add 36.4 g of sorbitol into a 100 mL three-neck flask with a magnetic sub, and heat to 130 oC After the sorbitol was melted, 0.364 g of 1-sulfopropyl-3-methylimidazolium bisulfate ionic liquid was added and reacted for 4 h under a pressure of 4 kPa; Fluoromethanesulfonylimide salt ionic liquid, after mixing evenly, the temperature of the system is gradually raised to 170 o C, the pressure drops to 40 Pa, collect 120 o C fraction, when the temperature of the fraction increases, the reaction is stopped, the quality of isosorbide collected by weighing is 23.6 g, the purification yield is 81%, and the component content analyzed by high performance liquid chromatography is 99.98%.

[0033] After the distillation is completed, cool the system to room temperature, add 50 mL of dichloromethane, mix evenly, add 30 mL of deionized water to shake and extract, and then let it stand still. After the phase separation is clear, remove the water phase, add deionized water again, and r...

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Abstract

The invention relates to a method for adding hydrophobic ionic liquid to separate a sugar alcohol dehydration reaction product by reduced pressure distillation. The sugar alcohol dehydration product is separated from the top of a distillation column, heavy components are extracted by a column and contain hydrophobic ionic liquid and sugar alcohol carbide, and the hydrophobic ionic liquid can be extracted, regenerated and reused through water / organic solvent. In the separation method, the hydrophobic ionic liquid is taken as a diluent in a product rectification process after sugar alcohol reaction, the viscosity of the reaction mixture is lowered, the carbonization function of a catalyst for a reactant and the reaction product in a rectification process can be diluted, the rectification yield and purity of the sugar alcohol dehydration product can be improved, and a whole distillation and extraction combination technology has the advantages of simpleness in operation and high resource use ratio.

Description

technical field [0001] The invention relates to a separation process of a sugar alcohol dehydration product, in particular to a process method for separating a sugar alcohol dehydration reaction product by adding a hydrophobic ionic liquid to vacuum distillation. Background technique [0002] The dehydration products of polysaccharide alcohols are widely used in medicine, food, cosmetics, polymers and other fields due to their special chiral structure; especially the application of isosorbide, the dehydration product of sorbitol, in the polymer industry makes the isosorbide Preparation and purification have become the focus of attention in this field. Isosorbide is a new type of plant-based functional diol with a chiral structure. At present, it is mainly prepared by two-step dehydration of sorbitol under the action of acid catalysis. [0003] Sorbitol dehydration catalysts include liquid mineral acids and solid acids. Among them, the use of solid acid catalyst has the adv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 何丹农邓洁童琴代卫国赵昆峰金彩虹
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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