Pharmaceutical grade glycerin purification method

A purification method and a pharmaceutical-grade technology are applied in the field of purification of pharmaceutical-grade glycerol to achieve the effects of less adsorbed glycerol, abundant raw material sources, and favorable for smooth passage.

Inactive Publication Date: 2017-08-18
天长市康宁甘油科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Glycerol, 1,2,3-propanetriol, exists in a compounded state in vegetable and animal oils and fats as glycerol compounded with fatty acids such as stearic acid, oleic acid, palmitic acid, and lauric acid Existing in the form of triesters, the industrial process for obtaining glycerol from vegetable and animal oils and fats involves saponification, high-pressure hydrolysis and transesterification with alcohols such as ethanol or methanol. Crude glycerol includes various impurities , involving numerous and complex processing steps, glycerol is extremely versatile, especially the natural high-purity and high-quality biomedical grade. With the continuous development and emergence of its new application fields, the market will definitely be in short supply. It has been hundreds of years to extract glycerol as a raw material, but most of them use traditional and backward technology and processes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of purification method of pharmaceutical grade glycerol proposed by the present invention comprises the following steps:

[0019] S1. Grind the muscovite, add barium nitrate aqueous solution to mix and stir, adjust the pH of the system to 5.5-6.5 with hydrochloric acid, add cetyltrimethylammonium chloride to raise the temperature and stir, filter, and wash to obtain pretreated muscovite;

[0020] S2. Heat up the sepiolite powder, keep it warm, cool to room temperature, add hydrochloric acid, heat up and stir, filter, wash until it is neutral, dry, add furfural and mix evenly, heat up, keep warm, heat up under nitrogen protection, keep warm, cool, Wash until neutral, add pretreated muscovite, stir, dry, and pulverize to obtain sepiolite muscovite compound;

[0021] S3. Add water to crude glycerin, add sepiolite muscovite compound and stir, let stand; filter under reduced pressure, the filtrate passes through a 001×7 type cation exchange resin column rinsed with wa...

Embodiment 2

[0023] A kind of purification method of pharmaceutical grade glycerol proposed by the present invention comprises the following steps:

[0024] S1. Grind 30 parts of muscovite in parts by weight to pass through a 200-mesh sieve, add 140 parts of barium nitrate aqueous solution with a concentration of 0.4 mol / L and mix and stir for 60 minutes. Use hydrochloric acid to adjust the pH value of the system to 5.5-6.5, and add 2 parts of sixteen Alkyltrimethylammonium chloride was heated to 70°C and stirred for 2h, filtered and washed to obtain pretreated muscovite;

[0025] S2. Heat up 16 parts of sepiolite powder to 650°C in parts by weight, keep it warm for 60min, cool to room temperature, add 50 parts of hydrochloric acid with a concentration of 2.5mol / L, heat up to 60°C and stir for 70min, filter, and wash until medium properties, dry, add 10 parts of furfural and mix evenly, heat up to 240°C, keep warm for 15h, heat up to 820°C under nitrogen protection, keep warm for 3h, cool,...

Embodiment 3

[0028] A kind of purification method of pharmaceutical grade glycerol proposed by the present invention comprises the following steps:

[0029] S1. Grind 50 parts of muscovite in parts by weight to pass through a 200-mesh sieve, add 100 parts of barium nitrate aqueous solution with a concentration of 0.8 mol / L and mix and stir for 40 minutes. Use hydrochloric acid to adjust the pH value of the system to 5.5-6.5, and add 4 parts of hexadecane Alkyltrimethylammonium chloride was heated to 60°C and stirred for 4h, filtered and washed to obtain pretreated muscovite;

[0030] S2. Heat up 8-16 parts of sepiolite powder to 650°C in parts by weight, keep it warm for 60min, cool to room temperature, add 50 parts of hydrochloric acid with a concentration of 2.5mol / L, heat up to 60°C and stir for 70min, filter and wash until Neutral, dry, add 10 parts of furfural and mix evenly, heat up to 240°C, keep warm for 15h, heat up to 820°C under nitrogen protection, keep warm for 3h, cool, wash ...

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PUM

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Abstract

The invention discloses a pharmaceutical grade glycerin purification method, which comprises: grinding muscovite, adding a barium nitrate aqueous solution, carrying out mixing stirring, adjusting the pH value of the system to 5.5-6.5 with hydrochloric acid, adding hexadecyltrimethylammonium chloride, carrying out heating stirring, filtering, and washing to obtain pre-treated muscovite; heating sepiolite powder, carrying out thermal insulation, cooling to a room temperature, adding hydrochloric acid, carrying out heating stirring, filtering, washing to achieve a neutral state, drying, adding furfural, uniformly mixing, heating, carrying out thermal insulation, adding the pre-treated muscovite, stirring, drying, and crushing to obtain a sepiolite-muscovite compound; adding water to crude glycerin, adding the sepiolite-muscovite compound, stirring, and standing; carrying out pressure reducing filtration, loading the filtrate onto a cation exchange resin column, loading onto an anion exchange resin column, carrying out rotary evaporation, carrying out heating evaporation until no distillate is distilled out, and continuously sucking the gas; and conveying into a distillation tower, collecting the distillated, carrying out deordorization heat exchange, and carrying out decolorization treatment to obtain the pharmaceutical grade glycerol.

Description

technical field [0001] The invention relates to the technical field of glycerin, in particular to a method for purifying medical grade glycerin. Background technique [0002] Glycerol, 1,2,3-propanetriol, exists in a compounded state in vegetable and animal oils and fats as glycerol compounded with fatty acids such as stearic acid, oleic acid, palmitic acid, and lauric acid Existing in the form of triesters, the industrial process for obtaining glycerol from vegetable and animal oils and fats involves saponification, high-pressure hydrolysis and transesterification with alcohols such as ethanol or methanol. Crude glycerol includes various impurities , involving numerous and complex processing steps, glycerol is extremely versatile, especially the natural high-purity and high-quality biomedical grade. With the continuous development and emergence of its new application fields, the market will definitely be in short supply. The extraction of glycerol as a raw material has a h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/76C07C31/22B01J20/10B01J20/30
CPCB01J20/10C07C29/76C07C31/225
Inventor 祁建兵
Owner 天长市康宁甘油科技有限公司
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