Safe separation and purification method of nitrate ester

A purification method and technology for nitrates, applied in the preparation of nitrates, nitrites, organic chemistry, etc., can solve the problems of easy explosion and unstable heating of pure nitrate products, and achieve the avoidance of danger, long-term storage, solvent The effect of high recovery rate

Active Publication Date: 2010-03-10
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems existing in the prior art, the present invention provides a method for the safe separation and purification of nitrates, which solves the problems in the prior art that the pure nitrates are prone to explosion and other dangerous problems due to thermal instability

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Propylene oxide and dinitrogen pentoxide are carried out nitration reaction in dichloromethane solution, obtain dihydric alcohol nitrate such as 1,2-propanediol dinitrate (PGDN)) / dichloromethane solution 40mL (total weight 57g, wherein PGDN mass content 7%) joins in the 1000mL still kettle, adds 400mL distilled water. Carry out heating distillation at 0.1MPa, collect fractions at 38°C~40°C, and the fractions are automatically divided into two layers in the collection bottle after being cooled. When the distillate temperature rises suddenly, stop heating and let it stand still, the obtained kettle liquid is in a liquid-liquid two-phase state, the lower layer is the PGDN product, and the upper layer is undistilled water. Product and distillate are cooled to room temperature, and the weight of nitrate ester and water is 398.5g in the distillation kettle, and the purity of chromatographic analysis nitrate ester is 99.9%; Distillation fraction gross weight is 56.5g, separate...

Embodiment 2

[0022] Carry out nitration reaction of propylene oxide and dinitrogen pentoxide in chloroform solution to obtain 40mL of 1,2-propanediol dinitrate (PGDN) / chloroform solution (63.2g in total weight, wherein PGDN mass content is 6.3%) Add to a 500mL still, add 200mL distilled water. Carry out heating distillation at 0.1MPa, collect fractions at 55°C~61°C, and the fractions are automatically divided into two layers in the collection bottle after being cooled. When the distillate temperature rises suddenly, stop heating and let it stand still, the obtained kettle liquid is in a liquid-liquid two-phase state, the lower layer is PGDN product, and the upper layer is undistilled water. Product and distillate are cooled to room temperature, and the weight of nitrate ester and water is 202g in the still kettle, and the purity of chromatographic analysis nitrate ester is 99.8%; The distillate cut is divided into two layers automatically, and gross weight is 59.5g, separates The weight o...

Embodiment 3

[0024] Carry out nitration reaction of propylene oxide and dinitrogen pentoxide in tetrachloromethane solution to obtain 40 mL of 1,2-propanediol dinitrate (PGDN) / tetrachloromethane solution (67.6 g in total weight, wherein PGDN mass content is 5.9%) Add to a 100mL distillation pot, add 40mL distilled water. Carry out heating distillation at 0.1MPa, collect fractions at 65°C~68°C, and the fractions are automatically divided into two layers in the collection bottle after being cooled. When the distillate temperature rises suddenly, stop heating and let it stand still, the obtained kettle liquid is in a liquid-liquid two-phase state, the lower layer is PGDN product, and the upper layer is undistilled water. Product and distillate are cooled to room temperature, and the weight of nitrate ester and water is 41.3g in the weighing still kettle, and the purity of chromatographic analysis nitrate ester is 99.8%; Distillation cut is divided into two layers automatically, and total weig...

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Abstract

The invention discloses a safe separation and purification method of nitrate ester, comprising the steps: organic solvent is distilled from the organic solution of nitrate ester by distillation; in distillation, distilled water is added into the organic solution of nitrate ester; and the organic solvent and water can form azeotropy, azeotrope formed by the distilled water and the organic solvent is distilled out, distillate is collected, the organic solvent is completely distilled out, then residue is obtained and divided into liquid-liquid two phases after standing, and the nitrate ester product phase at a lower layer is covered by the water phase. Compared with the method for removing the organic solvent from the nitrate ester by direct atmospheric and vacuum distillation, the safe separation and purification method of nitrate ester is simple in operation, safe and clean in process and high in product purity and yield, and leads the obtained nitrate ester to be safely protected by water, avoid dangers, and be stored for a long time.

Description

technical field [0001] The invention relates to an efficient and safe separation and purification method for nitrate compounds, which belongs to the separation and purification technology of nitrate esters. Background technique [0002] Nitrate is an important organic compound, which has a very wide range of uses in medicine, pesticides, civilian explosives and military fields. In the synthesis of nitrate esters, the traditional methods mostly use polyols as starting materials, and use nitric-sulfur mixed acid, nitric acid, etc. as nitrating agents for preparation. At present, the new nitration technology of nitrating epoxy compounds with dinitrogen pentoxide as nitrating agent has become a research hotspot in the synthesis of nitrate compounds. However, the nitrate ester product obtained through the above preparation method usually exists in the form of an organic solution of nitrate ester. In order to obtain a pure nitrate ester product, it is necessary to separate and pu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/02C07C201/04C07C203/04C07C203/06
Inventor 王庆法王莅张香文刘国柱邹吉军米镇涛
Owner TIANJIN UNIV
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