CN101012055A - Method of preparing sodium azide - Google Patents
Method of preparing sodium azide Download PDFInfo
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- CN101012055A CN101012055A CN 200610156064 CN200610156064A CN101012055A CN 101012055 A CN101012055 A CN 101012055A CN 200610156064 CN200610156064 CN 200610156064 CN 200610156064 A CN200610156064 A CN 200610156064A CN 101012055 A CN101012055 A CN 101012055A
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- sodiumazide
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- hydrazine hydrate
- ethanol
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Abstract
The invention discloses a making method of sodium azide, which comprises the following steps: dripping sulfuric acid in the solution with alcohol, sodium nitrite and water; aerating ethyl nitrite gas into solution with hydrazine hydrate, sodium hydroxide, tetrabutylammonium bromide and alcohol; generating sodium azide; evaporating solvent; crystallizing; separating solid from liquid to obtain the product.
Description
Technical field
The present invention relates to a kind of chemical products preparation method, especially the preparation method of sodiumazide.
Background technology
At present, domestic have only minority sodiumazide manufacturer to adopt the nitrous acid ester method, but, its technical process all is to adopt polystep reaction to obtain crude product, after refining, just can obtain up-to-standard product again, concrete technical process is: with lower alcohol, Sodium Nitrite drops into the nitrous acid ester synthesis reactor by a certain percentage, drips sulfuric acid, and the nitrous acid ester gas of generation feeds hydrazine hydrate, in the solution of sodium hydroxide, the sodiumazide of the low levels that generates, finish, centrifugal, obtain the crude product sodiumazide, again crude product and suitable quantity of water are dropped into the azoimide synthesis reactor, drip sulfuric acid, generate azoimide, the azoimide gas of generation feeds the liquid caustic soda still, generate the sodiumazide product, concentrate, centrifugal, obtain up-to-standard sodiumazide product.This technical process complexity, operation steps is lengthy and tedious, and product yield is low, and technology weight yield (in hydrazine hydrate) is 65%-70%, and product content is about 99%, CO
3 2-Content is about 0.3%.Be difficult to obtain highly purified product in production operation, and produce the azoimide gas of severe toxicity in process of production, relatively difficulty is leaked in control, and is therefore, extremely strict to operator's requirement.
Summary of the invention
Technical problem to be solved by this invention is: be intended to overcoming the deficiency of prior art, provide that a kind of technological process of production is simple, operation easier is little, product yield is high, the preparation method of the sodiumazide of good product quality.Its technical scheme is: a kind of preparation method of sodiumazide, it is characterized in that: sulphuric acid soln is splashed in the solution that constitutes by ethanol, Sodium Nitrite and water, ethyl nitrite gas with its generation feeds in the solution that is made of hydrazine hydrate, sodium hydroxide, Tetrabutyl amonium bromide and ethanol again, generate sodiumazide, boil off solvent, crystallization is after solid-liquid separation promptly gets the sodiumazide elaboration.
The concentration of above-mentioned sulphuric acid soln is 60%-80%.
The weight ratio of the above-mentioned sulphuric acid soln that splashes into and ethanol, Sodium Nitrite and water is 1: 0.8-1.1: 1.8-2.2: 2.8-3.2.
The ethyl nitrite gas of above-mentioned feeding and hydrazine hydrate, sodium hydroxide, Tetrabutyl amonium bromide and alcoholic acid weight ratio are 1: 0.5-0.7: 0.3-0.5: 0.004-0.006: 0.8-1.1.
Useful technique effect of the present invention is: compared with prior art, the present invention adopts single stage method to prepare sodiumazide, and its technological process of production is simple, easy handling, less demanding to operator; Technology weight yield (in hydrazine hydrate) is 85%, and product content is more than 99.5%, CO
3 2-Content is below 0.1%, product yield height, good product quality.
Embodiment
With concentration is that 70% sulphuric acid soln 200g splashes in the solution that is made of ethanol 200g, Sodium Nitrite 400g and water 600g; And the rate of addition of control sulphuric acid soln.Again with the stable 30M that is controlled at of the ethyl nitrite gas flow of its generation
3/ H feeds in the solution that is made of hydrazine hydrate 195g, sodium hydroxide 130g and catalyzer-Tetrabutyl amonium bromide 1.6g and ethanol 330g of 90 ℃ of 70 ℃ of ∽; Reaction times is about 8 hours, and the sodiumazide of generation boils off etoh solvent for 90 ℃ at 80 ℃ of ∽; Then, be cooled to below 50 ℃,, promptly get sodiumazide elaboration 165g through solid-liquid separation.Technology weight yield (in hydrazine hydrate) is 85%, and product content is more than 99.5%, CO
3 2-Content is below 0.1%.
Claims (4)
1, a kind of preparation method of sodiumazide, it is characterized in that: sulphuric acid soln is splashed in the solution that constitutes by ethanol, Sodium Nitrite and water, ethyl nitrite gas with its generation feeds in the solution that is made of hydrazine hydrate, sodium hydroxide, Tetrabutyl amonium bromide and ethanol again, generate the sodiumazide crude product, boil off solvent, crystallization is after solid-liquid separation promptly gets the sodiumazide elaboration.
2, the preparation method of a kind of sodiumazide according to claim 1 is characterized in that: the concentration of described sulphuric acid soln is 60%-80%.
3, the preparation method of a kind of sodiumazide according to claim 1 is characterized in that: the weight ratio of the described sulphuric acid soln that splashes into and ethanol, Sodium Nitrite and water is 1: 0.8-1.1: 1.8-2.2: 2.8-3.2.
4, the preparation method of a kind of sodiumazide according to claim 1 is characterized in that: the ethyl nitrite gas of described feeding and hydrazine hydrate, sodium hydroxide, Tetrabutyl amonium bromide and alcoholic acid weight ratio are 1: 0.5-0.7: 0.3-0.5: 0.004-0.006: 0.8-1.1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610156064 CN101012055A (en) | 2006-12-31 | 2006-12-31 | Method of preparing sodium azide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610156064 CN101012055A (en) | 2006-12-31 | 2006-12-31 | Method of preparing sodium azide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101012055A true CN101012055A (en) | 2007-08-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610156064 Pending CN101012055A (en) | 2006-12-31 | 2006-12-31 | Method of preparing sodium azide |
Country Status (1)
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| CN (1) | CN101012055A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659088A (en) * | 2012-05-09 | 2012-09-12 | 山东艾孚特科技有限公司 | Water-phase synthesis method of sodium azide |
| CN102718197A (en) * | 2012-04-28 | 2012-10-10 | 济南圣泉唐和唐生物科技有限公司 | Preparation method of sodium azide |
| CN103523758A (en) * | 2013-09-28 | 2014-01-22 | 青岛雪洁助剂有限公司 | Method for continuously preparing sodium azide |
| CN104502337A (en) * | 2014-12-30 | 2015-04-08 | 山东艾孚特科技有限公司 | Method for quantitatively detecting various components in sodium azide aqueous-phase synthesis mother solution |
| CN110467161A (en) * | 2019-09-25 | 2019-11-19 | 山东省化工研究院 | A kind of synthesis technology of sodium azide |
-
2006
- 2006-12-31 CN CN 200610156064 patent/CN101012055A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718197A (en) * | 2012-04-28 | 2012-10-10 | 济南圣泉唐和唐生物科技有限公司 | Preparation method of sodium azide |
| CN102659088A (en) * | 2012-05-09 | 2012-09-12 | 山东艾孚特科技有限公司 | Water-phase synthesis method of sodium azide |
| CN103523758A (en) * | 2013-09-28 | 2014-01-22 | 青岛雪洁助剂有限公司 | Method for continuously preparing sodium azide |
| CN103523758B (en) * | 2013-09-28 | 2015-03-25 | 青岛雪洁助剂有限公司 | Method for continuously preparing sodium azide |
| CN104502337A (en) * | 2014-12-30 | 2015-04-08 | 山东艾孚特科技有限公司 | Method for quantitatively detecting various components in sodium azide aqueous-phase synthesis mother solution |
| CN104502337B (en) * | 2014-12-30 | 2017-02-22 | 山东艾孚特科技有限公司 | Method for quantitatively detecting various components in sodium azide aqueous-phase synthesis mother solution |
| CN110467161A (en) * | 2019-09-25 | 2019-11-19 | 山东省化工研究院 | A kind of synthesis technology of sodium azide |
| CN110467161B (en) * | 2019-09-25 | 2021-07-06 | 山东省化工研究院 | Synthesis process of sodium azide |
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