CN1962420A - Process for refining high-purity yellow phosphorus - Google Patents
Process for refining high-purity yellow phosphorus Download PDFInfo
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- CN1962420A CN1962420A CN 200610051289 CN200610051289A CN1962420A CN 1962420 A CN1962420 A CN 1962420A CN 200610051289 CN200610051289 CN 200610051289 CN 200610051289 A CN200610051289 A CN 200610051289A CN 1962420 A CN1962420 A CN 1962420A
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Abstract
The invention discloses a manufacturing method of refined high-purity yellow phosphor, which comprises the following steps: adding 20-30% yellow phosphor into 70-80% water in the sandwich insulating furnace; heating to fuse into liquid pattern; doping 8-15% carbonate; heating to 70-75 Deg C; stirring; washing through 75-80 Deg C; stewing; sedimenting; making arsenic content less than 0.2PPM and each impurity content less than 300PPM; refining to obtain 5-6N high-purity yellow phosphor.
Description
Technical field
The invention belongs to chemical technology field, particularly a kind of production method of refining high-purity yellow phosphorus.
Background technology
High-purity yellow phosphorus is the doped source of preparation semi-conductor and semiconductor material, also is the raw material of producing the pure phosphorus oxychloride of electronics.According to the quality standard of high-purity yellow phosphorus, the content of arsenic should be less than 0.2PPM, and all the other every foreign matter contents should be less than below the 300PPM.At this point, for reaching this content standard, each state has all carried out the research of a large amount of different methods.
Japanese kokai publication hei 5-116916 discloses, and the yellow phosphorus that adopts concentrated nitric acid to handle 48～50 ℃ of scopes reaches 12 hours, and the arsenic content in the yellow phosphorus is reduced to below the 10PPM by 55PPM.Clear and the 54-93692 of Japan discloses, to adopt concentration be 6～18% nitric acid with concentration be 15～38% sulfuric acid be mixed with concentration be 3.5～6.5 moles mix acid-treated yellow phosphorus need 5～10 hours, arsenic content is reduced to below the 1PPM by 90PPM.Above-described method, acid consumption is big, and the rate of recovery of phosphorus only is 70%, and is difficult to make in the yellow phosphorus arsenic content less than below the 0.2PPM.
The high-purity yellow phosphorus that Japan's special permission described phosphuret-(t)ed hydrogen reduction method of communique 59-217609 and the described chromatography of Britain Brit942831 are produced, though the arsenic content in the yellow phosphorus is reduced to less than below the 0.2PPM, all the other every foreign matter contents are less than below the 300PPM.But their production link complexity, required condition harshness can set off an explosion poor stability slightly accidentally.
Summary of the invention
Purpose of the present invention is the problem that the production method in conjunction with above-mentioned high-purity yellow phosphorus exists, and provides a kind of under normal temperature, normal pressure, easy to operate, the treatment time is short, arsenic-removing rate and removal of impurity rate height, and Production Flow Chart is simple, the production method of the refining high-purity yellow phosphorus that security is good.
The production method of refining high-purity yellow phosphorus of the present invention is achieved in that
The industrial yellow phosphorus of weight 20～30% is put into the refining kettle of the strap clamp layer insulation that fills weight 70～80% water, and liquid phosphor is dissolved in heating.Mixing weight in liquid phosphor is the carbonate of industrial yellow phosphorus weight 8～15%, through being heated to 70～75 ℃, and stirring reaction 2 hours at least, use 75～80 ℃ water washing again after, quiescent settling is 1 hour at least.
Above-mentioned treated liquid phosphor is put into concentration 15～18%, weight is the salpeter solution and the concentration 6～10% of industrial yellow phosphorus weight 150～200%, weight is in the laminated heat-preserving enamel refining kettle of reductant solution of high-purity iodine preparation of industrial yellow phosphorus weight 10～40%, be heated to 70～75 ℃, stirring reaction through 1～3 hour, after 75～80 ℃ water washing, mixing weight is the Powdered Activated Carbon of industrial yellow phosphorus weight 0.2～0.5%, again through being heated to 70～75 ℃, at least stirred 1 hour, at least quiescent settling 1 hour again, after filtering at last, with 75～80 ℃ water washing.Thereby reach make arsenic content less than 0.2PPM, all the other every foreign matter contents are less than below the 300PPM, promptly are refined into 5～N level, content reaches 99.999% high-purity yellow phosphorus.
The production method of refining high-purity yellow phosphorus of the present invention, its flow process is simple, and is easy to operate, and the treatment time is short, operational safety, arsenic-removing rate and removal of impurity rate height, cost is low, and less investment is easy to promote.
Embodiment
The specific embodiment of the present invention takes following examples to realize:
Embodiment: the industrial yellow phosphorus of weight 20% is put into the refining kettle of the strap clamp layer insulation that fills weight 80% pure water, be heated to 50 ℃, dissolve into liquid phosphor.Mixing weight in liquid phosphor is the carbonate of industrial yellow phosphorus weight 12%, its desirable bicarbonate of ammonia or carbon ammonium are through being heated to 75 ℃, the agitator stirring reaction of 70～100 rev/mins of rotating speeds of employing 2 hours, after using 80 ℃ pure water washed twice again, quiescent settling 1 hour.
Above-mentioned treated liquid phosphor is put into concentration 17%, weight is the salpeter solution and the concentration 8% of industrial yellow phosphorus weight 180%, weight is in the laminated heat-preserving enamel refining kettle of reductant solution of high-purity iodine preparation of industrial yellow phosphorus weight 20%, be heated to 75 ℃, adopt the agitator of 70～100 rev/mins of rotating speeds, stirring reaction through 2 hours, after using 80 ℃ pure water washed twice again, mixing weight is the Powdered Activated Carbon of industrial yellow phosphorus weight 0.4%, again through being heated to 75 ℃, adopt the agitator of 70～100 rev/mins of rotating speeds to stir after 1 hour, quiescent settling is 1 hour again, after filtering with 2～5um strainer then, use 80 ℃ pure water washed twice again.Make arsenic content less than 0.2PPM thereby reach, all the other every foreign matter contents are less than below the 300PPM, promptly are refined into 5～6N level, content reaches 99.999% high-purity yellow phosphorus.
Claims (1)
1, a kind of production method of refining high-purity yellow phosphorus, it is characterized in that the industrial yellow phosphorus of weight 20～30% is put into the strap clamp layer heat-insulation purifying pot internal heating that fills weight 70～80% water dissolves into liquid phosphor, mixing weight is the carbonate of industrial yellow phosphorus weight 8～15%, through being heated to 70～75 ℃, and stirring reaction 2 hours at least, after using 75～80 ℃ water washing again, at least quiescent settling is 1 hour, again treated liquid phosphor is put into concentration 15～18%, weight is the salpeter solution and the concentration 6～10% of industrial yellow phosphorus weight 150～200%, weight is in the laminated heat-preserving enamel refining kettle of reductant solution of high-purity iodine preparation of industrial yellow phosphorus weight 10～40%, through being heated to 70～75 ℃, again through 1～3 hour stirring reaction, after 75～80 ℃ water washing, mixing weight is the Powdered Activated Carbon of industrial yellow phosphorus weight 0.2～0.5%, again through being heated to 70～75 ℃, and stirred at least 1 hour, at least quiescent settling 1 hour again, after filtering at last, with 75～80 ℃ water washing, promptly be refined into high-purity yellow phosphorus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100512895A CN100497167C (en) | 2006-11-19 | 2006-11-19 | Process for refining high-purity yellow phosphorus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100512895A CN100497167C (en) | 2006-11-19 | 2006-11-19 | Process for refining high-purity yellow phosphorus |
Publications (2)
| Publication Number | Publication Date |
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| CN1962420A true CN1962420A (en) | 2007-05-16 |
| CN100497167C CN100497167C (en) | 2009-06-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2006100512895A Expired - Fee Related CN100497167C (en) | 2006-11-19 | 2006-11-19 | Process for refining high-purity yellow phosphorus |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759164B (en) * | 2009-12-09 | 2011-08-10 | 湖北兴福电子材料有限公司 | Production method of high-purity yellow phosphorus |
| CN103723693A (en) * | 2013-12-20 | 2014-04-16 | 云南省化工研究院 | Arsenic removal method of yellow phosphorus |
| CN111533097A (en) * | 2019-10-30 | 2020-08-14 | 贵州新天鑫化工有限公司 | Yellow phosphorus oxidation dearsenification method |
-
2006
- 2006-11-19 CN CNB2006100512895A patent/CN100497167C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759164B (en) * | 2009-12-09 | 2011-08-10 | 湖北兴福电子材料有限公司 | Production method of high-purity yellow phosphorus |
| CN103723693A (en) * | 2013-12-20 | 2014-04-16 | 云南省化工研究院 | Arsenic removal method of yellow phosphorus |
| CN103723693B (en) * | 2013-12-20 | 2016-03-09 | 云南省化工研究院 | A kind of Yellow phosphorus arsenic removing method |
| CN111533097A (en) * | 2019-10-30 | 2020-08-14 | 贵州新天鑫化工有限公司 | Yellow phosphorus oxidation dearsenification method |
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| Publication number | Publication date |
|---|---|
| CN100497167C (en) | 2009-06-10 |
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Assignee: Xuzhou JianPing Chemical Co., Ltd. Assignor: Huang Pinhui|Yang Yi Contract record no.: 2011320000648 Denomination of invention: Process for refining high-purity yellow phosphorus Granted publication date: 20090610 License type: Exclusive License Open date: 20070516 Record date: 20110422 |
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Granted publication date: 20090610 Termination date: 20111119 |