Sodium azide synthesis process

A sodium azide and synthesis process technology, applied in the direction of azide acid/azide/halogen azide, etc., can solve the problems of safety hazards, large liquid holding capacity, environmental pollution, etc., and achieve low risk and side effects The effect of low product and reduced production cost

Active Publication Date: 2019-11-19
CHEM TECH ACAD OF SHANDONG PROVINCE
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this Kebad reaction is relatively mature, due to the natural defects of the Kebad reaction, there are serious problems of large liquid holding capacity, running, popping, dripping, and leaking in the production process, causing huge environmental pollution; nitrite, sodium azide All belong to explosive and highly toxic dangerous goods, and there are huge potential safety hazards

Method used

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  • Sodium azide synthesis process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Connect the G1 microchannel reactor module (a complete set of 10 modules, with a total liquid holding capacity of 90ml), rinse the pipeline with methanol, and use a high-pressure liquid phase pump to prepare a molar ratio of n (水合肼) :n (氢氧化钠) :n (水) = 1:1:2 water phase mixture and molar ratio is n (亚硝酸甲酯) :n (甲醇) = 1:1 oil phase mixture, put into 10 G1 reactor modules, the design flux is 30ml / min, combined with the measured water phase density and oil phase density, calculate the mass flow rate of the two phases as m (水相) =17.3g / min, m (油相) =12.86g / min, respectively use a stopwatch and an electronic scale to calibrate the two-phase mass flow. After the normal feed rate is calibrated, adjust the back pressure to 2bar, raise the temperature to 50°C, and react for 15 minutes to sample, quench and separate. The aqueous phase is the sodium azide aqueous solution. Take out the sample and use potentiometric titration to determine the aqueous phase According to the content...

Embodiment 2

[0032] Connect the G1 microchannel reactor module (a complete set of 10 modules, with a total liquid holding capacity of about 90ml), rinse the pipeline with ethanol, and use a high-pressure liquid phase pump to prepare a molar ratio of n (水合肼) :n (氢氧化钠) :n (水溶液) = 1:1:2 water phase mixture and molar ratio is n (亚硝酸乙酯) :n (乙醇) = 1:1 oil phase mixture, put into 10 G1 reactor modules, the design flux is 30ml / min, combined with the measured water phase density and oil phase density, calculate the mass flow rate of the two phases as m (水相) =18.5g / min, m (油相) =11.9g / min, respectively use a stopwatch and an electronic scale to calibrate the two-phase mass flow. After the normal feed rate is calibrated, adjust the back pressure to 2bar, raise the temperature to 50°C, and react for 15 minutes to sample, quench and separate. The aqueous phase is the sodium azide aqueous solution. Take out the sample and use potentiometric titration to determine the aqueous phase According to the c...

Embodiment 3

[0034] Connect the G1 microchannel reactor module (a complete set of 10 modules, with a total liquid holding capacity of about 90ml), rinse the pipeline with isopropanol, and use a high-pressure liquid phase pump to prepare a molar ratio of n (水合肼) :n (氢氧化钠) :n (水溶液) = 1:1.3:2 water phase mixture and molar ratio is n (亚硝酸异丙酯) :n (异丙醇) = 1:1 oil phase mixture, put into 10 G1 reactor modules, the design flux is 50ml / min, combined with the measured water phase density and oil phase density, calculate the mass flow rate of the two phases as m (水相) =28.6g / min, m (油相) =21.43g / min, respectively use a stopwatch and an electronic scale to calibrate the two-phase mass flow. After the normal feed rate is calibrated, adjust the back pressure to 2bar, raise the temperature to 50°C, and react for 9 minutes to sample, quench and separate. The aqueous phase is the sodium azide aqueous solution. Take out the sample and use potentiometric titration to determine the aqueous phase. According...

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Abstract

The invention belongs to the field of organic chemical industry, and particularly relates to a sodium azide synthesis process, wherein sodium azide is prepared by using a micro-channel reactor systemand / or a tubular reactor system as a reaction device, using nitrite, hydrazine hydrate and sodium hydroxide as main raw materials and using an alcohol as a solvent through a continuous production process. Compared with the traditional kettle type reaction, the synthesis process of the present invention has advantages of low danger during the production, high safety factor, high product conversionrate, high product purity, low by-products and no waste salt generation. According to the present invention, corresponding alcohols, water, centrifugation mother liquors and the like generated by thereaction can be recovered and applied so as to reduce the production cost and reduce the environmental pressure, such that the economic benefits and the environmental benefits are improved.

Description

technical field [0001] The invention belongs to the field of organic chemical industry, and specifically relates to a synthesis process of sodium azide, in particular to a new continuous and aqueous phase synthesis process of sodium azide. Background technique [0002] Sodium azide is a fine chemical product, which is widely used in automobiles, military, medicine, pesticides, biology and other fields. At the same time, sodium azide, as an important pharmaceutical intermediate, can be used to synthesize cephalosporin antibiotics and sartan antihypertensive drugs, etc. With the rapid development of the automobile manufacturing industry, the amount of sodium azide used as an inflator for automobile airbags is increasing year by year. [0003] At present, the industrial production of sodium azide mainly uses sulfuric acid, sodium nitrite, alcohol, nitrite, hydrazine hydrate, liquid caustic soda, etc. as the main raw materials. A small number of manufacturers such as Qingdao S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/08
CPCC01B21/08C01P2006/80
Inventor 岳涛高维丹刘启奎程远志陈贵军冯维春
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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