Preparation method of sodium azide

A technology of sodium azide and sodium hydroxide, applied in the direction of azide acid/azide/halide azide, etc., can solve the problems of complex process flow, low product yield, poor industrial practicability, etc., and achieve the production process The process is simple, the product qualification rate is good, and the effect of improving product yield

Active Publication Date: 2012-10-10
济南尚博生物科技有限公司
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

The process is complicated, the operation steps are cumbersome, the product yield is low, the process weight yield (in terms of hydrazine hydrate) is 65%-70%, the product content is about 99%, CO 3 2- The content is about 0.3%
It

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] C 2 h 5 OH+NaNO 2 +H 2 SO 4 →NO-OC 2 h 5 +Na 2 SO 4 +H 2 O (1)

[0021] NH 2 ·NH 2 ·H 2 O+NO-OC 2 h 5 +NaOH-→NaN 3 +C 2 h 5 OH+3H 2 o

[0022] (2)

[0023] Add 100g ethanol (2.17mol) and 140.7g sodium nitrite (2.04mol) into a 1L three-necked flask, control the reaction temperature between 0-5°C, add dropwise 327.1g of sulfuric acid solution with a mass ratio of 30%, for 30min After the time has been added dropwise, ethyl nitrite gas is generated during the dropwise addition, and the reaction formula is as formula (1). Washing with water is to remove the entrained inorganic acid in the gas, and the ethyl nitrite gas generated is 152.93g (2mol).

[0024] Pass ethyl nitrite gas into a three-necked flask filled with 102g of hydrazine hydrate, 64.4g of NaOH, 240g of ethanol, and 7.4g of catalyst tributylamine, and control the reaction temperature at 20°C. After the gas introduction is complete, react for another ...

Embodiment 2

[0026] Add 115g of ethanol and 172.5g of sodium nitrite (2.04mol) into a 1L three-necked flask, control the reaction temperature between 0-5°C, add dropwise 327.1g of sulfuric acid solution with a mass ratio of 30%, and complete the dropwise addition in 25 minutes , generate ethyl nitrite gas in the dropwise addition process, reaction formula is as formula (1), wash with water to remove the inorganic acid of entrainment, the ethyl nitrite gas of generation is 170.3g.

[0027] Pass ethyl nitrite gas into a three-necked flask filled with 115g of hydrazine hydrate, 90.8g of NaOH, 208g of ethanol, and 9.2g of catalyst tributylamine, and control the reaction temperature at 20°C. After the gas introduction is complete, react for another 2h. The reaction formula is as follows Formula (2), then the reaction solution decompression distillation reclaims ethanol, suction filtration, gets NaN 3 The wet product was dried under reduced pressure to obtain 133.8g of the product, and the yield...

Embodiment 3

[0029] Add 92g of ethanol and 138g of sodium nitrite into a 1L three-necked flask, control the reaction temperature between 0-5°C, add dropwise 327.1g of sulfuric acid solution with a mass ratio of 30%, and complete the dropwise addition in 20 minutes. Generate ethyl nitrite gas, the reaction formula is as formula (1), wash with water to remove entrained inorganic acid, the generated ethyl nitrite gas is 150g.

[0030] Pass ethyl nitrite gas into a three-necked flask filled with 120g of hydrazine hydrate, 80g of NaOH, 276g of ethanol, and 5.6g of catalyst benzyltriethylammonium chloride, and control the reaction temperature at 20°C. After the gas introduction is complete, react for another 2 hours , the reaction formula is as formula (2), and then the reaction solution is distilled under reduced pressure to recover ethanol, and suction filtered to obtain NaN 3 The wet product was dried under reduced pressure to obtain 140.1g of the product, and the calculation yield of this em...

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PUM

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Abstract

The invention provides a preparation method of sodium azide. The preparation method comprises the steps of adding sulfuric acid to a solution consisting of an ethanol, a sodium nitrite, introducing the produced ethyl nitrite gas into a mixture consisting of a hydrazine hydrate, a sodium hydroxide, a catalyst, and an ethanol, and after the gas is introduced, carrying out a reaction for 1.5 to 2.5h at a temperature of 18 to 25 DEG C. The preparation method provided by the invention which adopts one step to prepare the sodium azide has the advantages of simple production process and easy operation. Since just one step is adopted, the intermediate product is not wasted, the product yield is greatly improved, the yield is more than 90%, the product qualification rate is great, and the purity is more than 99%.

Description

technical field [0001] The invention belongs to the field of azide, in particular to a preparation method of sodium azide. Background technique [0002] Sodium azide, the molecular formula is NaN 3 , Colorless hexagonal crystalline powder. Mainly used in the manufacture of explosives, airbags, analytical reagents, pharmaceutical intermediates, etc. This product is similar to cyanide, has inhibitory effect on cytochrome oxidase and other enzymes, and can block the formation of oxyhemoglobin in the body, and has a significant antihypertensive effect. [0003] Sodium azide can use SN 2 Preparation by reaction method. At present, there are a small number of sodium azide manufacturers who use the nitrite method. The process flow is to use multi-step reactions to obtain crude products, and then to obtain qualified products after refining. The specific process flow is: the lower alcohol , Ammonium nitrite is put into the ammonium nitrite synthesis kettle in a certain proportion...

Claims

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Application Information

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IPC IPC(8): C01B21/08
Inventor 江成真刘顶张文岺
Owner 济南尚博生物科技有限公司
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