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Isopropyl nitrite preparation method

A technology of isopropyl nitrite and sodium nitrite, which is applied in the field of preparation of isopropyl nitrite, can solve the problems of low added value of by-product sodium sulfate, high operating condition requirements, high production cost, etc. The conditions are difficult to control, the process is clean and environmentally friendly, and the additional effect is high

Inactive Publication Date: 2018-11-27
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation method of traditional isopropyl nitrite has 3 kinds, and a kind of is by isopropanol-nitrosation method, uses isopropanol, sodium nitrite, sulfuric acid as raw material, reacts under methylene chloride solvent and makes, and Sulfuric acid is raw material, and the added value of by-product sodium sulfate is lower, and sulfuric acid concentration is within 40%, and water consumption is bigger, and reaction yield is lower (84%); Silver nitrate is prepared as a raw material; not only the reaction yield is low (52%), but also the requirements for operating conditions are high, the amount of waste water is large, and the production cost is expensive; there is also a method to prepare by reacting benzophenone and isopropanol , but the by-product dimethyl ketone will be generated, and the reaction is not easy to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Stir 105ml (0.5mol) of 30% nitric acid solution into a mixed system consisting of 69g (1.0mol) of sodium nitrite and 80.4ml (1.05mol) of isopropanol, keep it warm at 25°C, and keep it warm after 1.5h of dropwise addition React at 40°C for 0.5h, collect liquid isopropyl nitrite from the dropwise addition of nitric acid until no more is received, and obtain 82.0 g of isopropyl nitrite, the reaction yield is 92.0%.

Embodiment 2

[0024] Stir 105ml (0.5mol) of 30% nitric acid solution into a mixed system consisting of 69g (1.0mol) of sodium nitrite and 80.4ml (1.05mol) of isopropanol, keep warm at 40°C, and keep warm after 2.0h of dropwise addition React at 50° C. for 2.0 h, collect liquid isopropyl nitrite from the dropwise addition of nitric acid, and obtain 85.6 g of isopropyl nitrite until the liquid isopropyl nitrite is no longer received. The reaction yield is 96.0%.

Embodiment 3

[0026] 64.9ml (0.7mol) of 68% nitric acid solution was stirred and added to the mixed system consisting of 69g (1.0mol) of sodium nitrite and 80.4ml (1.05mol) of isopropanol. Insulate at 40°C and react for 2.0 hours. Liquid isopropyl nitrite was collected from the dropwise addition of nitric acid until no more was received, and 77.5 g of isopropyl nitrite was obtained. The reaction yield was 87.0%.

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PUM

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Abstract

The invention discloses an isopropyl nitrite preparation method. The method particularly comprises the following steps that isopropanol is added in a reaction vessel, sodium nitrite is added while stirring is conducted, the reaction temperature is controlled to range from 20 DEG C to 50 DEG C, a dilute sulfuric acid solution is dropwise added slowly, after dropwise adding is completed, a thermal reaction is conducted, separation is conducted, and isopropyl nitrite is obtained. The preparation method is simple in technology, the condition is easy to control, the production cost is low, the safety coefficient is high, convenience is brought to aftertreatment, and the method has very high operability and repeatability; according to the synthetic method, the product yield can reach 95% or above, industrial production is facilitated, and the problems that a traditional technology has difficulty in controlling the reaction condition and is high in production cost, low in yield and the like are solved.

Description

technical field [0001] The present invention relates to a kind of synthetic method, be specifically related to a kind of preparation method of isopropyl nitrite. It belongs to the technical field of organic synthesis. Background technique [0002] Isopropyl nitrite is a kind of nitrite, which has low stability, is easy to explode, and is difficult to store. It plays an important role in dilating blood vessels, lowering blood pressure and tachycardia. It is widely used in the fields of military, engineering technology and medicine. At the same time, isopropyl nitrite is a better diazotization reagent. [0003] The preparation method of traditional isopropyl nitrite has 3 kinds, and a kind of is by isopropanol-nitrosation method, uses isopropanol, sodium nitrite, sulfuric acid as raw material, reacts under methylene chloride solvent and makes, and Sulfuric acid is raw material, and the added value of by-product sodium sulfate is lower, and sulfuric acid concentration is with...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/04C07C203/00
CPCC07C201/04C07C203/00
Inventor 邢文国岳涛冯维春杨旭魏凤邢伶
Owner QINGDAO UNIV OF SCI & TECH
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