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Trihydroxymethyl hexane trinitrate and its making method

A technology of trimethylolhexane trinitrate and methylolhexane trinitrate, which is applied in the field of trimethylolhexane trinitrate and its preparation, and can solve the problems of undiscovered, poor insensitivity, etc. problems, to achieve the effect of expanding use, abundant raw materials, and low prices

Inactive Publication Date: 2006-05-31
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Trimethylolethane trinitrate is an energetic plasticizer. It has a similar structure to nitroglycerin and is much less toxic than nitroglycerin. Although its impact sensitivity is lower than that of nitroglycerin, its insensitivity performance is still obvious Poor, currently only small-scale domestic production
Through domestic and foreign online searches, no relevant reports have been found on the preparation of trimethylolhexane trinitrate from trimethylolhexane

Method used

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  • Trihydroxymethyl hexane trinitrate and its making method
  • Trihydroxymethyl hexane trinitrate and its making method
  • Trihydroxymethyl hexane trinitrate and its making method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add the nitrating agent of 98% nitric acid into the reaction kettle, and under the condition of good stirring, add the raw material trimethylol hexane into the reaction kettle in batches, the molar ratio of trimethylol hexane to nitric acid is 1:20. After the feeding is completed, the reaction is continued, and the temperature is controlled at 0° C. to 15° C. during the reaction, and the time is 0.5 to 3 hours. After the reaction, a large number of crystals appeared at the bottom of the reaction kettle. After filtering and washing with water until the washing liquid was neutral and dry, the product collected from the reaction mixture was white crystals. It was proved by infrared spectroscopy, nuclear magnetic resonance and elemental analysis The white crystal is the product trimethylolhexane trinitrate. The yield of the product trimethylolhexane trinitrate can reach 86.2%.

Embodiment 2

[0031] Add the nitrating agent and catalyst of 98% nitric acid into the reaction kettle in sequence, and under the condition of good stirring, add the raw material trimethylol hexane into the reaction kettle in batches, and the molar ratio of trimethylol hexane to nitric acid is 1 : 10, the catalyst is urea, and the amount added is 3% to 8% of trimethylolhexane in terms of mass percentage. After the feeding is completed, the reaction is continued, and the temperature is controlled at 5° C. to 25° C. during the reaction, and the time is 1 to 4 hours. After the reaction, a large number of crystals appeared at the bottom of the reaction kettle. After filtering and washing with water until the washing liquid was neutral and dry, the product collected from the reaction mixture was white crystals. It was proved by infrared spectroscopy, nuclear magnetic resonance and elemental analysis The white crystal is the product trimethylolhexane trinitrate. The yield of the product trimethyl...

Embodiment 3

[0033] Add the nitrating agent of anhydrous nitric acid into the reaction kettle, and under the condition of good stirring, add the raw material trimethylol hexane into the reaction kettle in batches, and the molar ratio of trimethylol hexane to nitric acid is 1:25. After the feeding is completed, the reaction is continued, and the temperature is controlled at 10° C. to 20° C. during the reaction, and the time is 2 to 5 hours. After the reaction, a large number of crystals appeared at the bottom of the reaction kettle. After filtering and washing with water until the washing liquid was neutral and dry, the product collected from the reaction mixture was white crystals. It was proved by infrared spectroscopy, nuclear magnetic resonance and elemental analysis The white crystal is the product trimethylolhexane trinitrate. The yield of the product trimethylolhexane trinitrate can reach 88.2%.

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Abstract

The invention relates to trimethylolhexane trinitrate and a preparation method thereof. Trimethylolhexane trinitrate can be used in pharmaceuticals and as a component of plasticizers and energetic materials, and is a widely used organic intermediate. The molecular formula of trimethylolhexane trinitrate is C 9 h 17 o 9 N 3 , The chemical structural formula is: ∴ Trimethylolhexane trinitrate is obtained by esterification of trimethylolhexane as raw material under the action of nitrating agent. The nitrating agent is 98% concentrated nitric acid, anhydrous nitric acid, nitric-sulfur mixed acid composed of concentrated nitric acid and concentrated sulfuric acid, and the range of the mass ratio of nitric acid, sulfuric acid to water is 5~25:90~60:5~15, or concentrated Nitrate-sulfur mixed acid composed of nitric acid and oleum is used as a nitrating agent, the mass ratio range of nitric acid and sulfuric acid is 30-40:70-60, the reaction temperature is -5-30°C, and the reaction time is 0.5-7 hours. The molar ratio of hydroxymethyl hexane to nitric acid is 1:4-30, the catalyst is urea, and the consumption of urea is 1%-10%.

Description

technical field [0001] The invention belongs to a method for preparing nitrate from polyhydric alcohol, in particular to trimethylolhexane trinitrate and a preparation method thereof. Background technique [0002] Nitroglycerin is a widely used good solvent for nitrocellulose, and is widely used in double-base propellants. However, the production of nitroglycerin is dangerous and highly volatile, and it tends to migrate from the inside of the double-base drug to the outside, making the drug body Reduced strength. Nitroglycerin double-base drugs are usually produced by solvent technology, and the product has a short shelf life. [0003] In order to find a substitute for nitroglycerin, a lot of research work has been done at home and abroad. In the late 1960s, a trimethylolethane trinitrate (TMETN) was developed and made into a propellant containing trimethylolethane trinitrate. Trimethylolethane trinitrate is an energetic plasticizer. It has a similar structure to nitrogly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C203/04C07C201/02
Inventor 崔建兰赵树森曹端林
Owner ZHONGBEI UNIV