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Water-phase synthesis method of sodium azide

A technology of sodium azide and hydrazine hydrate, applied in the direction of azide acid/azide/halide azide, chemical recovery, etc., can solve the problems of low utilization rate of raw nitrite, long reaction period and high production cost , to achieve the effect of good product purity, low cost and little environmental pollution

Active Publication Date: 2012-09-12
山东艾孚特科技有限公司
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Problems solved by technology

These processes all have the problems of long reaction cycle, low utilization rate of raw material nitrite, high energy consumption, large amount of three wastes, and high production cost.

Method used

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  • Water-phase synthesis method of sodium azide
  • Water-phase synthesis method of sodium azide
  • Water-phase synthesis method of sodium azide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Mix 66.0g (0.66 moles) of 98% concentrated sulfuric acid and pure water to form a 50% sulfuric acid solution, and drop the obtained sulfuric acid solution into a mixed system consisting of 90.6g (1.3 moles) of sodium nitrite and 64.4g (1.33 moles) of ethanol while stirring During the process, control the reaction temperature at 25-40°C, start to condense and collect liquid ethyl nitrite, and drop sulfuric acid in about 2 hours. After adding the acid, keep the reaction at 30-40°C for 0.5h until liquid ethyl nitrite is no longer received, and a total of 90.6g of ethyl nitrite is obtained.

[0020] Mix 62.5g (1.0 mole) of hydrazine hydrate with 137.5g (1.1 mole) of 32% liquid caustic soda and cool down to 10-15°C, add 1.5g of 1wt% tetrabutylammonium bromide solution, and dissolve the liquid ethyl nitrite obtained above Add all to the system, seal the reaction, keep the reaction temperature at 15-20°C, react for 10 hours, and finally the system pressure reaches 0.32MPa. Op...

Embodiment 2

[0022] Other conditions are constant, only change the mol ratio of hydrazine hydrate, sodium hydroxide and ethyl nitrite, react according to the step of embodiment 1, reaction result is shown in Table 1:

[0023]

[0024] From the experimental results, the yield is better when the molar ratio of hydrazine hydrate: sodium hydroxide: liquid ethyl nitrite is 1:1.1-1.2: 1.2-1.3.

Embodiment 3

[0026] Other conditions are unchanged, only the type of phase transfer catalyst, the catalyst is all configured as a 1wt% solution, the addition is 1.5g, and the reaction is carried out according to the steps of Example 1. The reaction results are shown in Table 2:

[0027]

[0028] From the experimental results, the catalytic effects of several catalysts are not much different.

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Abstract

The invention discloses a water-phase synthesis method of sodium azide, which comprises the following steps: adding liquid ethyl nitrite into a reaction system composed of hydrazine hydrate, sodium hydroxide, phase-transfer catalyst and solvent water to react under closed conditions; and after the reaction finishes, recycling unreacted ethyl nitrite, byproduct ethanol and water, and filtering thereaction liquid to obtain the sodium azide. The method uses water as the reaction solvent, carries out the reaction under pressurized conditions, and has the advantages of low energy consumption, mild reactions, high product yield and high product purity; and besides, the reaction byproduct ethanol, the unreacted ethyl nitrite, the centrifugal mother solution and the like can be recycled, therebysaving the cost, relieving the environmental pressure and further enhancing the product yield. Thus, the invention is suitable for industrialized clean production.

Description

technical field [0001] The invention relates to an aqueous phase synthesis method of sodium azide, which belongs to the technical field of organic synthesis. Background technique [0002] Sodium azide, as a common chemical product, is widely used in industries such as automobile airbag gas generating agent, medicine, explosives, pesticide and chemical synthesis. [0003] There are two main methods for industrial production of sodium azide, one is the sodium metal method, which uses sodium metal and liquid ammonia as raw materials, and the other is the hydrazine-nitrite method. At present, the production process of sodium azide both at home and abroad adopts the hydrazine hydrate-nitrite-sodium hydroxide method, and the nitrite used includes methyl nitrite, ethyl nitrite, butyl nitrite, and isoamyl nitrite. wait. The preparation technology of methyl nitrite and ethyl nitrite is mostly a gas-liquid two-phase method in which nitrite gas is passed into an ethanol solution of h...

Claims

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Application Information

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IPC IPC(8): C01B21/08
CPCY02P20/584
Inventor 贾卫斌杨旭纪晓红常丽霞王灏柳泽岳迟金龙张新一
Owner 山东艾孚特科技有限公司
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