CN1156122A - Process for producing barium azide - Google Patents
Process for producing barium azide Download PDFInfo
- Publication number
- CN1156122A CN1156122A CN 96117183 CN96117183A CN1156122A CN 1156122 A CN1156122 A CN 1156122A CN 96117183 CN96117183 CN 96117183 CN 96117183 A CN96117183 A CN 96117183A CN 1156122 A CN1156122 A CN 1156122A
- Authority
- CN
- China
- Prior art keywords
- barium azide
- sodium hydroxide
- sodiumazide
- azide
- sulphuric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- UUXFWHMUNNXFHD-UHFFFAOYSA-N Barium azide Chemical compound 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[Ba+2].[N-]=[N+]=[N-].[N-]=[N+]=[N-] UUXFWHMUNNXFHD-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N sodium azide Chemical compound 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[Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound 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- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000001117 sulphuric acid Substances 0.000 claims description 12
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- 229910052782 aluminium Inorganic materials 0.000 claims description 2
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[Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910001864 baryta Inorganic materials 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N calcium Chemical compound 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[Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound 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[Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- -1 hydrogen potassium oxide Chemical class 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N magnesium Chemical compound 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[Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 2
- 238000001953 recrystallisation Methods 0.000 claims description 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound 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[OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 abstract 1
- 229910001863 barium hydroxide Inorganic materials 0.000 abstract 1
- XGZRAKBCYZIBKP-UHFFFAOYSA-L disodium;dihydroxide Chemical compound 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[OH-].[OH-].[Na+].[Na+] XGZRAKBCYZIBKP-UHFFFAOYSA-L 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 238000001291 vacuum drying Methods 0.000 abstract 1
- 239000003643 water by type Substances 0.000 description 2
- 230000002950 deficient Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Abstract
A process for producing barium azide with such raw materials as sodium azide, sodium hydroxide, sulfuric acid solution and barium hydroxide in ratio of 1:0.33:6:2.4 includes the steps of taking sodium azide and sodium hydroxide, installing dripping funnel and condenser connected to two-mouth flask, dripping 40% sulfuric acid solution, stopping distilling at 105 deg.C, stirring, filter, concentrating mother liquid and recrystallizing to obtain barium azide, low-temp. vacuum drying, sieving and packing. Its advantages are simple process and reliable performance of product.
Description
What the present invention relates to is a kind of production technique of barium azide.
Barium azide is as a kind of novel, and the lamp of superior performance is adopted and alternative traditional getter by increasing light source manufacturer with getter.More outstanding is, in recent years, by the automobile bubble production line that Taiwan, Korea S introduce, 110V starter production line, and partly red-letter day bubble, decorate bubble production line etc. and all will use barium azide as getter, and consumption grows with each passing day.The whole dependence on import of the barium azide of domestic use, and because it belongs to hazardous substance, be not to unify import by national foreign trade agency, so cause very big difficulty to applying unit.
The objective of the invention is to defective, develop a kind of production technique of barium azide voluntarily, to satisfy demestic user's needs at above-mentioned existence.
Technical solution of the present invention:
The weight proportion of its each composition is a sodiumazide: sodium hydroxide: sulphuric acid soln: hydrated barta=1: 1.33-0.133: 6: 2.4;
40% sulphuric acid soln has the hydrated barta of 8 crystal water;
The weight ratio of each composition can be a sodiumazide: sodium hydroxide: sulphuric acid soln: hydrated barta=1: 1.33-0.133: 6: 2.4 or=1: 0.33: 12-3: the optimum weight ratio of 2.4 each composition is sodiumazide: sodium hydroxide: sulphuric acid soln: hydrated barta=1: 0.33: 6: 2.4, the sodium hydroxide in above-mentioned is the available hydrogen potassium oxide also.
The production technique of barium azide, it is characterized in that branch (1) is by each composition part by weight, getting sodiumazide and sodium hydroxide packs into and uses water dissolution in three mouthfuls of distilling flasks, (2) install dropping funnel and condenser, one end of condenser is connected with two mouthfuls of flasks that the band that the baryta water that contains 8 crystal water is housed stirs with joint, (3) treat sodiumazide, the solution boiling of sodium hydroxide, the sulphuric acid soln of dropping 40%, continue distillation, when treating that three mouthfuls of solution temperatures in the distilling flask reach 105 ℃, stop to add thermal distillation, (4) solution in two mouthfuls of flasks is continued to stir 10 minutes, (5) filter, obtain anhydrous barium azide, (6) again with mother liquor with being with water-cooled rotatory evaporator to concentrate or using cryogenic freezing to carry out recrystallization, obtain a hydration barium azide, (7) are with above-mentioned (5), (6) barium azide that obtains carries out vacuum dehydrating at lower temperature respectively; (8) sieve with 100 mesh sieve, (9) dress up finished product with bottled or vacuum packet after doing the mensuration of content calcium, magnesium, iron, aluminium, copper.
Advantage of the present invention: technology is simply superior, and reliable product quality can satisfy user's service requirements and needs.
Embodiment 1:
Getting 15 gram barium azide and 5 gram sodium hydroxide packs into and dissolves with 100 ml waters in 250 milliliters of three mouthfuls of distilling flasks, install dropping funnel and condenser, one end of condenser is connected with two mouthfuls of flasks of 500ml that band stirs with joint, the hydrated barta (8 crystal water) and 200 ml waters that contain 36 grams in this flask, to above-mentioned there-necked flask heating, make sodiumazide, the solution boiling of sodium hydroxide, drip 90 milliliters of 40% sulphuric acid solns with that, continue to add thermal distillation when treating that solution temperature reaches 105 ℃ in three mouthfuls of distilling flasks, stop to add thermal distillation, solution in two mouthfuls of flasks is continued to stir 10 minutes after-filtration can obtain anhydrous barium azide, mother liquor is with being with water-cooled rotatory evaporator to concentrate, can obtain a hydration barium azide, an above-mentioned anhydrous barium azide and a hydration barium azide are carried out vacuum dehydrating at lower temperature respectively; 100 orders sieve, and obtain total barium azide 25.4 grams.
Embodiment 2,3, the same embodiment 1, and only changing sodium hydroxide weight respectively is 20g, 2g.
Embodiment 4,5, and with embodiment 1, the weight that only changes 40% sulphuric acid soln is 180ml, 45ml.
Embodiment 1-5 result is similar.
Claims (5)
1, barium azide is characterized in that its each composition has sodiumazide, sodium hydroxide, sulphuric acid soln, hydrated barta.
2, barium azide according to claim 1 is characterized in that 40% sulphuric acid soln, and the hydrated barta of 8 crystal water is arranged.
3, according to claim 1,2 described barium azide, the weight ratio that it is characterized in that each composition can be a sodiumazide: sodium hydroxide: sulphuric acid soln: hydrated barta=1: 1.33-0.133: 6: 2.4 or=1: 0.33: 12-3: 2.4.
4, barium azide according to claim 1, the optimum weight ratio that it is characterized in that each composition is a sodiumazide: sodium hydroxide: sulphuric acid soln: hydrated barta=1: 0.33: 6: 2.4;
Sodium hydroxide in above-mentioned is the available hydrogen potassium oxide also.
5, the production technique of barium azide, it is characterized in that branch (1) is by each composition part by weight, getting sodiumazide and sodium hydroxide packs into and uses water dissolution in three mouthfuls of distilling flasks, (2) install dropping funnel and condenser, one end of condenser is connected with two mouthfuls of flasks that the band that the baryta water that contains 8 crystal water is housed stirs with joint, (3) treat sodiumazide, the solution boiling of sodium hydroxide, the sulphuric acid soln of dropping 40%, continue distillation, when treating that three mouthfuls of solution temperatures in the distilling flask reach 105 ℃, stop to add thermal distillation, (4) solution in two mouthfuls of flasks is continued to stir 10 minutes, (5) filter, obtain anhydrous barium azide, (6) again with mother liquor with being with water-cooled rotatory evaporator to concentrate or using cryogenic freezing to carry out recrystallization, obtain a hydration barium azide, (7) are with above-mentioned (5), (6) barium azide that obtains carries out vacuum dehydrating at lower temperature respectively; (8) sieve with 100 mesh sieve, (9) dress up finished product with bottled or vacuum packet after doing the mensuration of content calcium, magnesium, iron, aluminium, copper.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117183A CN1085616C (en) | 1996-11-25 | 1996-11-25 | Process for producing barium azide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96117183A CN1085616C (en) | 1996-11-25 | 1996-11-25 | Process for producing barium azide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1156122A true CN1156122A (en) | 1997-08-06 |
| CN1085616C CN1085616C (en) | 2002-05-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN96117183A Expired - Fee Related CN1085616C (en) | 1996-11-25 | 1996-11-25 | Process for producing barium azide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102099908B (en) * | 2008-03-24 | 2013-08-21 | 通用电气公司 | Getter precursors for hermetically sealed packaging |
| CN103864034A (en) * | 2014-03-17 | 2014-06-18 | 南京理工大学 | Method and device for synthesizing copper azide |
| CN110204340A (en) * | 2019-05-27 | 2019-09-06 | 北京智芯微电子科技有限公司 | Make the method for raw material synthesis I- type silicon substrate Runge-Kutta integration under high temperature and pressure with barium azide |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0222520B2 (en) * | 1980-04-21 | 1990-05-18 | Toshiba Electric Equip | |
| FR2573060B1 (en) * | 1984-11-13 | 1987-02-20 | Centre Nat Rech Scient | NITROGEN OR OXYAZOTE COMPOUNDS WITH PEROVSKITE STRUCTURE, THEIR PREPARATION AND THEIR APPLICATION TO THE MANUFACTURE OF DIELECTRIC COMPONENTS |
| KR890001418B1 (en) * | 1985-12-27 | 1989-05-03 | 김의동 | Preparation for making method of azid |
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1996
- 1996-11-25 CN CN96117183A patent/CN1085616C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102099908B (en) * | 2008-03-24 | 2013-08-21 | 通用电气公司 | Getter precursors for hermetically sealed packaging |
| CN103864034A (en) * | 2014-03-17 | 2014-06-18 | 南京理工大学 | Method and device for synthesizing copper azide |
| CN110204340A (en) * | 2019-05-27 | 2019-09-06 | 北京智芯微电子科技有限公司 | Make the method for raw material synthesis I- type silicon substrate Runge-Kutta integration under high temperature and pressure with barium azide |
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