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Preparation method of trimethylol ethane trinitrate

A technology of hydroxymethylethane trinitrate and trimethylolethane, which is applied in the field of nitration of saturated fatty alcohols, can solve the problems of high cost, high price, and high risk of extraction agents in the nitration system, and solve the problems of relatively low cost. High, reduce the preparation cost, improve the effect of stability

Active Publication Date: 2018-01-23
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the deficiencies and defects of the high cost of the nitrification system, the high risk of the extractant and the high price in the background technology, and provide a liquid-phase feed, low cost of the nitrification system, safe and cheap extractant TMETN synthesis method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Preparation of TMETN

[0016] Into a 100mL four-necked flask equipped with a thermometer, stirrer, condenser, etc., add 15.0g of concentrated sulfuric acid, stir, and start to add 18.0g of nitric acid and 10.0g of trimethylolethane aqueous solution successively. After the addition is complete, React at 12°C for 10 minutes. After the reaction, it was extracted with 21.0 g of dichloromethane, washed with water three times, 15 mL each time, and the dichloromethane was removed under reduced pressure to obtain 5.84 g of product TMETN with a yield of 91.6% and a purity of ≥99.3%.

[0017] Structural identification of TMETN:

[0018] Elemental analysis: C 5 H 9 N 3 O 9 , Calculated value C 23.53, H 3.529, N 16.47,

[0019] Measured value C 23.54, H 3.527, N 16.49.

[0020] IR(KBr),υ / cm -1 :2993,2905,1474,1379(-CH 2 ,-CH 3 ); 1641,1278,860(-ONO 2 ).

[0021] 1 H NMR(DMSO-d 6 ,δ,ppm):1.10(s,3H,-CH 3 ),4.58(s,6H,-CH 2 -).

[0022] Analysis and testing confirmed that the product obtained in...

Embodiment 2

[0024] Preparation of TMETN

[0025] Into a 100mL four-necked flask equipped with a thermometer, stirrer, condenser, etc., add 20.0g of concentrated sulfuric acid, stir, and start to add 15.0g of nitric acid and 10.0g of trimethylolethane aqueous solution successively. After the addition is complete, React at 15°C for 10 minutes. After the reaction, it was extracted with 28.0 g of dichloromethane, washed with water three times, 15 mL each time, and the dichloromethane was removed under reduced pressure to obtain 5.63 g of product TMETN with a yield of 82.5% and a purity of ≥99.1%.

Embodiment 3

[0027] Preparation of TMETN

[0028] Into a 100mL four-necked flask equipped with a thermometer, stirrer, condenser, etc., add 15.0g of concentrated sulfuric acid, stir, and start to add 15.0g of nitric acid and 10.0g of trimethylolethane aqueous solution dropwise. React at 10°C for 10 minutes. After the reaction, it was extracted with 21.0 g of dichloromethane, washed with water three times, 15 mL each time, and the dichloromethane was removed under reduced pressure to obtain 4.77 g of product TMETN with a yield of 74.8% and a purity of ≥98.5%.

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Abstract

The invention discloses a preparation method of trimethylol ethane trinitrate (TMETN). The preparation method takes trimethylol ethane as a raw material and comprises the following steps: firstly dissolving trimethylol ethane into water, so that trimethylol ethane aqueous solution with the mass fraction of 20-40% is obtained, then adding concentrated sulfuric acid into a reaction bottle, sequentially adding concentrated nitric acid and the trimethylol ethane aqueous solution, carrying out nitration reaction, after the reaction is completed, extracting with dichloromethane, washing with water for three times, and carrying out reduced pressure dichloromethane removal, so that the TMETN is obtained, wherein the mass ratio of the concentrated sulfuric acid to the concentrated nitric acid to the trimethylol ethane aqueous solution to the dichloromethane is (1.1-2.2):(1.3-2.6):1:(1.6-3.2), reaction temperature is 10-15 DEG C, and reaction time is 10 minutes. The invention aims at solving theproblems that reaction conditions of a preparation process of the TMETN are harsh, solvent dosage is high and cost is high, and the preparation method disclosed by the invention is mainly used for preparation of the TMETN.

Description

Technical field [0001] The invention relates to the nitration of saturated fatty alcohols, in particular to a preparation method of trimethylolethane trinitrate (TMETN), which belongs to organic synthesis. Background technique [0002] Trimethylolethane trinitrate (TMETN) is a new insensitive liquid energetic plasticizer for mixed explosives, solid propellants and propellants. Compared with the traditional liquid energetic plasticizer nitroglycerin, it can endow Propellant has better safety performance and process performance, and is a better candidate to replace nitroglycerin. TMETN is often used as an energy-containing plasticizer in the development of high-energy squeeze-cast explosives, high-energy low-sensitivity solid propellants and high-energy low-vulnerability propellants to reduce the flame temperature and danger of the formulation. [0003] The synthesis method of trimethylolethane trinitrate (TMETN) mostly uses trimethylolethane as raw material and is prepared by batch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C203/04C07C201/02
Inventor 陈斌汪伟汪营磊高福磊姬月萍丁峰刘卫孝刘亚静
Owner XIAN MODERN CHEM RES INST
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