Preparation method of glycerin trinitrate

A technology of nitroglycerin and fuming nitric acid, which is applied in the chemical industry, can solve the problems of accelerating the decomposition of nitroglycerin, failing to meet quality requirements, and exceeding the standard of nitroglycerin substances, and achieve the effects of reducing losses, avoiding dissolution and decomposition, and high yield

Active Publication Date: 2018-05-29
GUANGZHOU BAIYUNSHAN MINGXING PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The temperature in the above production process, the residual water and acid in the reaction solution will cause the decomposition of nitroglycerin, and the decomposition products include 1,2-dinitroglycerin and 1,3-dinitroglycerin. The content of relevant substances is limited. Further, the two impurities in nitroglycerin will accelerate the decomposition of nitroglycerin, which will eventually lead to the excess of relevant substances in the storage process of nitroglycerin and its preparations, which cannot meet the quality requirements.

Method used

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  • Preparation method of glycerin trinitrate
  • Preparation method of glycerin trinitrate
  • Preparation method of glycerin trinitrate

Examples

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Embodiment 1

[0026] An embodiment of the method for preparing nitroglycerin of the present invention comprises the following steps: (1) Nitration reaction: Weigh 3 parts of fuming nitric acid cooled to 10°C, add it to a reaction vessel placed in an ice bath, and slowly add it while stirring Mix 6 parts of concentrated sulfuric acid cooled to 10°C evenly to obtain a mixed acid; when the mixed acid cools down to 10°C, slowly add 1 part of glycerol dropwise while stirring, and control the temperature of the reaction solution at 12°C during the dropping process; After the dropwise addition, continue to stir at 12°C for 0.8h, and after standing to separate layers, discard the acid solution in the lower layer to obtain crude nitroglycerin;

[0027] (2) Refining: A, purified water washing: transfer the nitroglycerin crude product obtained in step (1) into a separatory container with an equal volume of purified water in advance, shake and wash fully, leave to stand for stratification, discard the u...

Embodiment 2

[0029] An embodiment of the method for preparing nitroglycerin of the present invention comprises the following steps: (1) Nitration reaction: Weigh 1 part of fuming nitric acid cooled to 6° C., add it to a reaction vessel placed in an ice bath, and slowly add it while stirring. Mix 2 parts of concentrated sulfuric acid cooled to 6°C evenly to obtain a mixed acid; when the mixed acid cools down to 15°C, slowly add 0.5 parts of glycerol dropwise while stirring, and control the temperature of the reaction solution at 18°C ​​during the dropping process; After the dropwise addition, continue to stir at 18°C ​​for 0.5h, and after standing to separate layers, discard the acid solution in the lower layer to obtain crude nitroglycerin;

[0030] (2) Refining: A, purified water washing: transfer the nitroglycerin crude product obtained in step (1) into a separatory container with an equal volume of purified water in advance, shake and wash fully, leave to stand for stratification, discar...

Embodiment 3

[0033] An embodiment of the method for preparing nitroglycerin of the present invention comprises the following steps: (1) Nitration reaction: Weigh 3.5 parts of fuming nitric acid cooled to 9° C., add it to a reaction vessel placed in an ice bath, and slowly add it while stirring. 5.5 parts of concentrated sulfuric acid cooled to 9°C, mixed evenly to obtain a mixed acid; when the temperature of the mixed acid was lowered to 15°C, slowly add 1 part of glycerol dropwise while stirring, and the temperature of the reaction solution was controlled at 12°C during the dropping process; After the dropwise addition, continue to stir at 12°C for 0.7h, and after standing to separate layers, discard the acid solution in the lower layer to obtain crude nitroglycerin;

[0034] (2) Refining: A, purified water washing: transfer the nitroglycerin crude product obtained in step (1) into a separatory container with an equal volume of purified water in advance, shake and wash fully, leave to stan...

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Abstract

The invention discloses a preparation method of glycerin trinitrate. The preparation method comprises the following steps: (1) nitration reaction; and (2) refining: A, purified water washing; B, waterremoval by using a drying agent; and C, activated carbon adsorption. The invention further provides glycerin trinitrate prepared by using the preparation method and an absolute ethyl alcohol solutionof glycerin trinitrate. The preparation method provided by the invention is high in yield, few in produced impurities and capable of effectively avoiding decomposition effects of reaction temperature, residual water and acids to glycerin trinitrate, reducing decomposition products of glycerin trinitrate and controlling the content of related substances in a storage process of glycerin trinitrateand the absolute ethyl alcohol solution thereof to make a glycerin trinitrate product more stable and ensure that the quality of the glycerin trinitrate product conforms to relevant regulations in a validity period.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of nitroglycerin. Background technique [0002] Nitroglycerin, the scientific name is glycerol trinitrate (glycerol trinitrate), and its molecular formula is C 3 h 5 (ONO 2 ) 3 , is the product of the esterification reaction of glycerol and nitric acid. In the field of medicine, nitroglycerin can relax blood vessels to facilitate blood circulation and significantly improve the cardiovascular system. [0003] Nitroglycerin, based on its own structure and characteristics, determines that it is a relatively sensitive drug, and impurities, water, acid, and temperature will all affect its decomposition. According to literature records, the melting point of nitroglycerin is 2.8°C, which is an unstable type, and it is a stable type at 13.5°C. It begins to decompose above 50°C, and when the temperature is lower than 13.2°C, it will crystall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/02C07C203/06A61K31/21A61K9/08A61P9/12
CPCA61K9/0019A61K9/08A61K31/21A61K47/02C07C201/02C07C203/06
Inventor 李同根李心花黄孟秋王家祺颜慷祺刘宏刘顺国陈文超潘碧妍
Owner GUANGZHOU BAIYUNSHAN MINGXING PHARM CO LTD
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