Aqueous-phase synthetic method of sodium azide with n-butyl alcohol circularly recycled
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A sodium azide water, recycling technology, applied in the direction of azide acid/azide/halogen azide, organic chemistry, nitrite preparation, etc., can solve the problems of gas leakage and achieve low cost and high yield high efficiency and reduce environmental pollution
Active Publication Date: 2015-07-08
ZHEJIANG HAILAN CHEM GRP
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Ethanol can be reused in this technical solution, but this method is a synthesis process involving gas-liquid two-phase, which needs to be operated under high pressure, there is a risk of gas leakage, and the condition control is relatively strict
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Embodiment 1
[0023] Embodiment 1 (sodium azide is synthesized):
[0024] In a 1000mL round bottom flask, add sodium hydroxide (40g, 1mol) and dissolve it in 80ml of water (4.44mol), add hydrazine hydrate (1mol), add methanol (3.2g, 0.1mol), add dropwise butyl nitrite Ester (113.4 g, 1.1 mol). Take it out after reacting at room temperature 25°C for 12 hours, recover n-butanol by distillation under reduced pressure, and filter to obtain a white solid. In the white solid, the free alkali content obtained by inspection is 0.85%, and sodium azide is 97.07%, that is, the white solid contains sodium azide The mass percent is 97.07%, that is, the purity is 97.07%, and the yield is 91%.
Embodiment 2
[0025] Embodiment 2 (sodium azide is synthesized):
[0026] Add sodium hydroxide (40g, 1mol) and dissolve in 80 ml of water (4.44mol) in a 1000mL round bottom flask, add hydrazine hydrate (1mol), add tetrabutylammonium chloride (0.06g, 0.0002mol), Butyl nitrite (113.4 g, 1.1 mol) was added dropwise. React at room temperature 25°C for 12 hours and take it out. Distill under reduced pressure to recover n-butanol, filter to obtain a white solid, check the free base content of 1.11%, sodium azide 97.35%, and the yield is 94%.
Embodiment 3
[0027] Embodiment 3 (sodium azide is synthesized):
[0028] Add sodium hydroxide (40g, 1mol) in 1000mL round bottom flask and dissolve in 80ml of water (4.44mol), add hydrazine hydrate (1mol), add tetrabutylammonium bromide (40g, 0.0002mol), drop Add butyl nitrite (113.4 g, 1.1 mol). React at room temperature 25°C for 12 hours and take it out. Recover n-butanol by distillation under reduced pressure, and filter to obtain a white solid. The free base content of the obtained product is 4.08%, sodium azide is 94.48%, and the yield is 90%.
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Abstract
The invention discloses an aqueous-phase synthetic method of sodium azide with n-butyl alcohol being circularly recycled, wherein the method includes following steps: (1) mixing butyl nitrite, sodium hydroxide, hydrazine hydrate, a catalyst and water to form a reaction system; (2) after the reaction finished, recycling the n-butyl alcohol and water; and (3) filtering a reaction solution to obtain a sodium azide (white solid) and circularly recycling the recycled n-butyl alcohol. In the method, by means of the butyl nitrite for synthesizing the sodium azide, so that compared with a synthesis route from ethyl nitrite, the synthetic method is free of high-pressure operations and the risk of leakage of gas. Meanwhile, the reaction can be carried out in the aqueous phase and just needs to added with the catalyst in a micro amount (especially, herein the catalyst may be composited of tributylamine and methanol), so that the synthetic method is environmental-protective. The method is high in yield of product, is low in the content of free alkali and is high in product purity. Meanwhile, the reaction achieves the recycle of a by-product n-butyl alcohol for synthesizing the butyl nitrite, by means of the technical scheme, the environmental pollution is reduced while the economic benefit is increased.
Description
technical field [0001] The invention relates to the field of preparation of sodium azide, in particular to a synthesis process of sodium azide aqueous phase in which n-butanol is recycled. Background technique [0002] Sodium azide (NaN 3 ), English name sodium azide, also known as sodium azide, is a colorless hexagonal crystal, which has only solid form, no liquid and gas form, dissolved in water and liquid ammonia, slightly soluble in ethanol, insoluble in ether. Sodium azide is often used as an important synthetic raw material, in addition to the synthesis of azide such as azide acid and lead azide, it is also used in the synthesis of organic intermediates with physiological activity and pharmaceutical activity. At present, sodium azide has been widely used in the fields of medicine, explosives, photographic agents, synthetic resins, pesticides, chemical synthesis, etc. Determination etc. In recent years, with the frequent occurrence of automobile accidents and the enh...
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