Preparation technique of isosorbide

A technology of isosorbide and preparation process, which is applied in the field of pharmacy, can solve the problems of high cost, low conversion rate, carbonization of raw materials, etc., and achieve the effect of improving utilization rate, avoiding the disadvantage of high energy consumption, and excellent quality

Active Publication Date: 2012-10-31
SHANDONG FUTASTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To solve the problems of the prior art using concentrated sulfuric acid dehydration and high-temperature oil bath distillation to prepare isosorbide, resulting in severe carbonization of raw materials, low conversion rate, high cost, serious environmental pollution, and difficulty in large-scale industrial production and preparation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Dehydration reaction

[0025] Weigh 250kg of solid sorbitol, melt it in a pressure reactor at 120°C, add 30% by weight of the catalyst obtained by mixing perfluorosulfonic acid resin and carbon-based palladium (mixed 4:1 by weight), at 150°C The reaction was stirred for 4 hours, and a hydrogen pressure of 0.2 MPa was always maintained in the reactor during the reaction.

[0026] The light transmittance of the obtained reaction solution was 86%, and the purity was 75.3% as detected by HPLC.

[0027] (2) Neutralization and decolorization

[0028] Pure water was added to dilute the reaction solution to a Brix of 19%. Use calcium carbonate suspension to adjust the pH value to neutral; add 7.5% activated carbon based on dry matter and stir at 75°C for 30 minutes to decolorize, and the transmittance of the reaction solution obtained by filtration is 96%.

[0029] (3) Electrodialysis desalination

[0030] After the treatment in step (2), the conductivity was 17600 μs / c...

Embodiment 2

[0040] (1) Dehydration reaction

[0041] Weigh 250kg of solid sorbitol, melt it in a pressure reactor at 110°C, add 5% by weight of perfluorosulfonic acid resin and carbon-based palladium mixed catalyst (6:1 by weight), at 150°C The reaction was stirred for 7 hours, and a hydrogen pressure of 0.3 MPa was always maintained in the reactor during the reaction.

[0042] The light transmittance of the obtained reaction solution was 89%, and the purity was 72.8% as detected by HPLC.

[0043] (2) Neutralization and decolorization

[0044] Pure water was added to dilute the reaction solution until the Brix was 20%. Use calcium carbonate suspension to adjust the pH value to neutral; add 5% activated carbon based on dry matter and stir at 75°C for 40 minutes to decolorize, and the transmittance of the reaction solution obtained by filtration is 98%.

[0045] (3) Electrodialysis desalination

[0046] After the treatment in step (2), the conductivity was 15300 μs / cm, and after further...

Embodiment 3

[0056] (1) Dehydration reaction

[0057] Weigh 250kg of solid sorbitol, melt it in a pressure reactor at 130°C, add 15% by weight of a catalyst obtained by mixing perfluorosulfonic acid resin and carbon-based palladium (8:1 by weight), at 150°C The reaction was stirred for 2 hours, and a hydrogen pressure of 0.2 MPa was always maintained in the reactor during the reaction.

[0058] The light transmittance of the obtained reaction solution was 82%, and the purity was 75.6% as detected by HPLC.

[0059] (2) Neutralization and decolorization

[0060] Pure water was added to dilute the reaction solution to a Brix of 18%. Use calcium carbonate suspension to adjust the pH value to neutral; add 10% activated carbon based on dry matter and stir at 75°C for 20 minutes to decolorize, and the transmittance of the reaction solution obtained by filtration is 99%.

[0061] (3) Electrodialysis desalination

[0062] After the treatment in step (2), the conductivity was 20200 μs / cm, and afte...

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Abstract

The invention relates to a preparation technique of isosorbide, belonging to the technical field of pharmacy. In the preparation technique, solid sorbitol is used as the raw material, a mixture of perfluoro-sulfonic acid resin and palladium on carbon is used as the catalyst, and hydrogen is used as an anti-carbonation agent to prepare the non-carbonized light-colored isosorbide reaction liquid; and low-temperature concentration and solvent crystallization are utilized to substitute the original high-temperature distillation. The preparation technique comprises the following steps: dehydration reaction, neutralization decolorization, electrodialysis desalination, water removal by concentration, extraction crystallization, freeze-drying, and quality inspection and packaging (after the product is qualified in inspection, packaging, and warehousing as the finished product). The invention can prevent carbonization and prevent the reaction liquid from becoming dark, thereby enhancing the utilization ratio of the raw material; most calcium salts are precipitated due to low solubility, and the electric conductivity of the reaction liquid is low, thereby being beneficial to subsequent extraction; and the invention overcomes the defect of high energy consumption in the high-temperature distillation technique, and the quality of the prepared isosorbide is more excellent.

Description

technical field [0001] The invention belongs to the technical field of pharmacy. Background technique [0002] Isosorbide (English name isosorbitol, isosorbide), which itself is an effective osmotic oral dehydration diuretic. At present, isosorbide is mainly used as a raw material for the preparation of cardiovascular drug isosorbide mononitrate in my country. [0003] Because the pharmaceutical market is relatively small, it affects people's research in the field of isosorbide preparation to a certain extent. With the increasing depletion of the world's energy resources and the improvement of people's requirements for the quality of artificial polymers, people have discovered the unique role of isosorbide in improving the properties of polymers in extended research. [0004] In recent years, the research focus on isosorbide is to use it as a comonomer to synthesize modified commercial polymers, such as PET, polyether, polyester, polyurethane, polycarbonate, etc. Adding i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
Inventor 赵光辉邱学良李林于军伟秦海青张长伶
Owner SHANDONG FUTASTE
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