CN1290762C - Production of phosphorus oxychloride with purity of 99.99999% - Google Patents
Production of phosphorus oxychloride with purity of 99.99999% Download PDFInfo
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- CN1290762C CN1290762C CN 200410081252 CN200410081252A CN1290762C CN 1290762 C CN1290762 C CN 1290762C CN 200410081252 CN200410081252 CN 200410081252 CN 200410081252 A CN200410081252 A CN 200410081252A CN 1290762 C CN1290762 C CN 1290762C
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- phosphorus
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- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000012535 impurity Substances 0.000 claims abstract description 19
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010992 reflux Methods 0.000 claims abstract description 9
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 7
- 239000011574 phosphorus Substances 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims description 45
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 24
- 239000000460 chlorine Substances 0.000 claims description 24
- 229910052801 chlorine Inorganic materials 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 15
- 229910019213 POCl3 Inorganic materials 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- 229910052804 chromium Inorganic materials 0.000 claims description 9
- 229910052785 arsenic Inorganic materials 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 229910052748 manganese Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 claims description 2
- RLOWWWKZYUNIDI-UHFFFAOYSA-N phosphinic chloride Chemical compound ClP=O RLOWWWKZYUNIDI-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005660 chlorination reaction Methods 0.000 abstract description 3
- 238000005194 fractionation Methods 0.000 abstract 1
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000007788 liquid Substances 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 239000013307 optical fiber Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
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Abstract
The present invention relates to the technology for producing phosphorus oxychloride with the purity of 99.99999%. The present invention adopts high-purity phosphorus to react with high-purity chlorine gas in order to produce phosphorus trichloride. The obtained phosphorus trichloride is made into pure phosphorus trichloride products by distillation. The pure phosphorus trichloride products are made into phosphorus oxychloride products by drip chlorination, refluxing, distillation and fractionation. The maximum content of a single impurity is not greater than 9 ppb.
Description
The technical field is as follows: the invention relates to a production process of phosphorus oxychloride with the purity of 99.99999 percent. The process adopts high-purity yellow phosphorus or red phosphorus(99.9999%), high-purity chlorine (metal impurities are not more than 50ppb) and pure water to prepare electronic-grade ultrapure phosphorus oxychloride, the highest content of single impurities is not more than 9ppb, and the metal impurities are not more than 5ppb, so that the production requirements of ultra-large-scale integrated circuits and optical fibers are met.
Technical background: high-purity phosphorus oxychloride (99.9999 percent and 99.99999 percent) is a doping agent for producing integrated circuits and solar cells, is one of raw materials for manufacturing optical fiber preforms, and the phosphorus oxychloride of the high-purity phosphorus oxychloride requires that the purity reaches 99.9999 to 99 percent99999 percent, the highest content of impurities is not more than 10ppb (Zn is less than or equal to 10ppb, Al is less than or equal to 10ppb, Hg is less than or equal to 8ppb, As is less than or equal to 7ppb, Ca is less than or equal to 6ppb, Li is less than or equal to 6ppb), especially Fe must be less than or equal to 5ppb to 8ppb, Mn is less than or equal to 1ppb to 5ppb, and Cr, Ag, Ni and Te are less than or equal to 1 ppb. At present, the production and production process of 99.99999 percent phosphorus oxychloride is not reported, and the reported chemical purity research comprises the following steps: ion exchange method-emission spectrometry for BBr as high-purity chemical reagent3、POCl3The separation and measurement of eight impurities such as Mn in the matrix (chemical reagents, 1989, 11, (3), 132-); there are two kinds of chlorination hydrolysis method and trichlorination method which are commonly used in industry, and the literature reports that: oxygen catalytic oxidation and a combined method (phosphorus oxychloride and oxygen oxidation method in the chlorination industry, a gas phase oxidation method and a method for co-producing phosphorus oxychloride bythionyl chloride). But the production process and the product with the grade of the top grade purity of more than 9.99 percent are only rarely reported.
The invention content is as follows: the invention aims to: provides a production process and a product of electronic grade ultrapure (99.99999%) phosphorus oxychloride. It is used for synthesizing, distilling and rectifying under the conditions of normal temperature and normal pressure to produce POCl3The product produced by the process can meet the production requirements of the ultra-large scale integrated circuit, the solar cell and the optical fiber perform.
The principle of the invention is that high-purity dry chlorine and excess phosphorus are used for preparing primary phosphorus trichloride:
PCl3colorless liquid, distilling the primary phosphorus trichloride to obtain PCl3And (5) producing the product.
PCl3The product is jected to chlorine introduction and water dropping reaction, and distilled to obtain POCl after the reaction is finished3And (5) performing primary product.
POCl3Rectifying the primary product to obtain electronic grade ultrapure (99.99999%) phosphorus oxychlorideThe highest content of single impurities is not more than 9 PPb.
The invention is formed in such a way that high-purity phosphorus (yellow phosphorus or red phosphorus) and dried high-purity chlorine are synthesized into a phosphorus trichloride primary product, the phosphorustrichloride primary product is distilled to obtain a fraction with the temperature of 71-78 ℃ to obtain a phosphorus trichloride product, the phosphorus trichloride product is placed in a glass flask provided with a reflux device and is subjected to chlorine-introducing and water-dropping reaction, and the chlorine-introducing and water-dropping reaction is followed by reflux to obtain phosphorus oxychloride POCl3The initial product is distilled when the temperature reaches 99-103 ℃, and 100-107 ℃ fractions are taken to obtain POCl3Pure product, POCl3The pure product is rectified to obtain 99.99999 percent electronic grade ultrapure phosphorus oxychloride POCl3。
The purity of the high-purity phosphorus of the invention is required to be 99.9999 percent, the content of organic matters, As, S and single items in the impurity content is less than or equal to 100ppb, the content of metal impurities such As Al, Fe, Cu, Cr, Co, Mn and the like is less than or equal to 50ppb, the content of organic matters, As and S impurities in the high-purity chlorine is less than or equal to 20ppb, and the content of metal impurities such As Fe, Ni, Cu, Zn, Cr, Mn and the like is less than or equal to 50 ppb; the high-purity water used in the chlorine-introducing dripping water synthesis process reaches the secondary water specified in GB 6682-92.
Note: the PPb means a content of 1/109。
The reaction time of chlorine introduction and water dropping in the process of the invention is determined according to POCl3The amount of (A) is generally 18 to 28 hours, and the amount of chlorine introduced is the mass of phosphorus trichloride multiplied by 0.51. The amount of water dropped is PCl3(phosphorus trichloride) mass multiplied by 0.13. The ratio of chlorine to water was 3.9: 1. The rectification time is 2-6 hours.
The distillation equipment for distilling phosphorus trichloride and phosphorus oxychloride is hard corrosion-resistant glass equipment; the equipment for rectifying the phosphorus oxychloride is tower plate rectifying equipment of high-purity quartz glass.
The packaging of the terminal product of the invention has strict requirements on the packaging environment of the terminal product being a hundred-grade purification environment.
Example 1: (1) putting 1000 g of 99.9999 percent red phosphorus into a 3000ml glass bottle, putting the glass bottle on a temperature-controllable electric furnace, connecting the lower opening of the glass bottle with a condenser, connecting the outlet of the condenser with a product receiving bottle, and connecting the upper opening of the glass bottle with a chlorine pipe;(2) heating red phosphorus, introducing chlorine gas, and controlling to avoid generation of PCl5(ii) a (3) Stopping chlorine introduction and heating after the red phosphorus reaction is basically completed to obtain 4260g of primary phosphorus trichloride, distilling the primary phosphorus trichloride, and taking distillate at 71-78 ℃ to obtain 4190g of a phosphorus trichloride product; (4) putting 4190g of distilled phosphorus trichloride product into a 3000ml three-mouth glass bottle provided with reflux equipment, adding chlorine by dripping water, strictly controlling the proportion of chlorine to water to be 3.9: 1, adding 2160g of chlorine and 545.0g of water, reacting for 21h, refluxing to obtain a phosphorus oxychloride primary product, distilling, collecting 99-108 ℃ fractions to obtain 3512g of phosphorus oxychloride pure product, rectifying the obtained phosphorus oxychloride pure product by a quartz rectifier, and collecting 105-107 ℃ fractions to obtain 3110 g of 99.99999% electronic grade ultrapure product. The product is colorless transparent liquid, the purity of the phosphorus oxychloride is 99.99999 percent, the single impurities of Zn, Cr, As, Hg and the like are 9ppbMax, Cu, Ag, Hg and the like,3ppbMax of single impurities such as Au, Mn, Ni and the like.
The product uses a plasma mass spectrometer ICP-MS and a graphite furnace atomic absorption analyzer GAAS to detect the contents of Al, Ag, Au, As, Co, Cu, Cr, Fe, Mg, Mn, Ni, Sn, Zn and the like in the product, and CS-444 is used to detect the content of S in the product: the results are as follows; (single ppb) Al is less than or equal to 9ppb, As is less than or equal to 7ppb, Ag is less than or equal to 1ppb, Au is less than or equal to 1ppb, Ba is less than or equal to 1ppb, Bi is less than or equal to 1ppb, Ca is less than or equal to 1ppb, Co is less than or equal to 2ppb, Cu is less than or equal to 3ppb, Cr is less than or equal to 1ppb, Fe is less than or equal to 8ppb, Ga is less than or equal to 1ppb, Hg is less than or equal to 7ppb, K is less than or equal to 3ppb, Li is less than or equal to 6ppb, Mg is less than or equal to 5ppb, Mn is less than or equal to 1ppb, Na is.
Example 2: (1) putting 5000 g of 99.9999 percent yellow phosphorus into a 8000ml glass reactor, wherein the glass reactor is provided with a temperature-controllable device, one port of the reactor is connected with a condenser, the outlet of the condenser is connected with a product receiving bottle, and the other port of the reactor is connected with a chlorine pipe; (2) chlorine gas is turned on to control not to generate PCl5A solid; (3) stopping introducing chlorine after the yellow phosphorus reaction is basically completed to obtain 22100g of primary phosphorus trichloride, distilling the primary phosphorus trichloride, and taking a fraction at 71-78 ℃ to obtain 20950g of a phosphorus trichloride product; (4) 20950g of distilled phosphorus trichloride product is put into 16000ml of glass provided with a reflux deviceAnd (2) adding chlorine into the reactor by dripping water, strictly controlling the ratio of chlorine to water to be 3.9: 1, wherein the addition amount of chlorine is 12500g, the addition amount of water is 2720g, reacting for 23h, refluxing to obtain a phosphorus oxychloride initial product, distilling, collecting 99-108 ℃ fractions to obtain 22000g of a phosphorus oxychloride pure product, rectifying the phosphorus oxychloride pure product by using a quartz rectifier, and collecting 105-107 ℃ fractions to obtain 19860 g of a 99.99999% electronic grade ultrapure product. The product is colorless transparent liquid, the purity of phosphorus oxychloride is 99.99999%, the single impurities of Fe, Zn, Cr, As, Hg and the like are 9ppbMax, and the single impurities of Cu, Ag, Au, Mn, Ni and the like are 3 ppbMa.
The product is detected with plasma mass spectrometer ICP-MS and graphite furnace atomic absorption analyzer GAAS for Al, Ag, Au, As, Co, Cu, Cr, Fe, Mg, Mn, Ni, Sn, Zn, etc. and CS-444 for S content. The results are as follows: (single ppb) Al is less than or equal to 9ppb, As is less than or equal to 7ppb, Ag is less than or equal to 1ppb, Au is less than or equal to 1ppb, Ba is less than or equal to 1ppb, Bi is less than or equal to 1ppb, Ca is less than or equal to 1ppb, Co is less than or equal to 2ppb, Cu is less than or equal to 3ppb, Cr is less than or equal to 1ppb, Fe is less than or equal to 8ppb, Ga is less than or equal to 1ppb, Hg is less than or equal to 7ppb, K is less than or equal to 3ppb, Li is less than or equal to 6ppb, Mg is less than or equal to 5ppb, Mn is less than or equal to 1ppb, Na is.
Compared with the prior art: the invention has the advantages of simple and safe process, less equipment investment, high product purity, good product stability, easy realization of industrialization and the like. The production process provided by the invention ensures the high purity and quality of the product through the following conditions:
(1) strictly controlling the quality, namely the purity, of the raw material phosphorus; (2) the purity of chlorine is strictly controlled; (3) strictly controlling the purity of water; (4) the material of the equipment is required not to cause secondary pollution; (5) the rectification equipment is required to be quartz column plate rectification equipment; (6) the packaging environment of the end product must be class 100.
Claims (4)
1. A production process of 99.99999 percent phosphorus oxychloride is characterized in that: high-purity yellow phosphorus or red phosphorus with purity of 99.9999% and dryingGood high-purity chlorine synthesis phosphorus trichloride primary product, primary product phosphorus trichloride PCl3Distilling to obtain distillate at 71-78 deg.C to obtain phosphorus trichloride product, placing the phosphorus trichloride product in a glass flask equipped with reflux device, making chlorine-introducing dripping water reaction, making reflux to obtain POCl3Primary crystal, distilling when the temperature reaches 99-103 ℃, and obtaining POCl by taking 100-107 ℃ fraction3Pure product, POCl3The pure product is rectified and the 105-107 ℃ fraction is collected to obtain 99.99999 percent electronic grade ultrapure phosphorus oxychloride POCl3The content of organic matters, As, S and single items in the high-purity phosphorus impurity is less than or equal to 100ppb, the content of metal impurities such As Al, Fe, Cu, Cr, Co, Mn and the like is less than or equal to 50ppb, the content of organic matters, As and S impurities in the high-purity chlorine is less than or equal to 20ppb, and the content of metal impurities such As Fe, Ni, Cu, Zn, Cr, Mn and the like is less than or equal to 50 ppb; the high-purity water used in the chlorine-introducing dripping water synthesis process reaches the secondary water specified in GB 6682-92.
2. The process according to claim 1, wherein the reaction time of chlorine introduction and water dropping is determined according to POCl3The amount of chlorine introduced is the mass of phosphorus trichloride multiplied by 0.51. The dropping amount is the mass of the phosphorus trichloride multiplied by 0.13, and the ratio of the chlorine to the water is 3.9: 1.
3. The process according to claim 1, wherein the distillation apparatus for distilling phosphorus trichloride and phosphorus oxychloride is a hard corrosion-resistant glass apparatus; the equipment for rectifying the phosphorus oxychloride is tower plate rectifying equipment of high-purity quartz glass.
4. The process of claim 1, wherein the packaging environment of the end product is a hundred-class clean environment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410081252 CN1290762C (en) | 2004-11-10 | 2004-11-10 | Production of phosphorus oxychloride with purity of 99.99999% |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410081252 CN1290762C (en) | 2004-11-10 | 2004-11-10 | Production of phosphorus oxychloride with purity of 99.99999% |
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| Publication Number | Publication Date |
|---|---|
| CN1613752A CN1613752A (en) | 2005-05-11 |
| CN1290762C true CN1290762C (en) | 2006-12-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410081252 Active CN1290762C (en) | 2004-11-10 | 2004-11-10 | Production of phosphorus oxychloride with purity of 99.99999% |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559932B (en) * | 2009-05-26 | 2010-12-01 | 向东 | Method for producing phosphorus trichloride with purity of 99.9999 percent and device therefor |
| CN101774554B (en) * | 2009-12-30 | 2011-09-07 | 邹岳明 | System for producing phosphorus trichloride |
| CN102126711B (en) * | 2010-12-03 | 2013-05-01 | 贵州威顿晶磷电子材料有限公司 | Method for producing phosphorus oxychloride with purity of 99.99999 percent |
| CN102249201B (en) * | 2011-06-14 | 2013-04-24 | 吴跃友 | Method and device for producing electronic grade phosphorus oxychloride |
| CN103350989A (en) * | 2013-06-28 | 2013-10-16 | 徐州市建平化工有限公司 | One-step production method for phosphorus trichloride with purity of 99.95% |
| CN108821254B (en) * | 2018-09-11 | 2021-11-26 | 安徽东至广信农化有限公司 | Method for removing inorganic and organic impurities in phosphorus trichloride synthesis process |
| CN113264512A (en) * | 2021-07-03 | 2021-08-17 | 江苏万隆化学有限公司 | Environment-friendly phosphorus trichloride production process |
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- 2004-11-10 CN CN 200410081252 patent/CN1290762C/en active Active
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| CN1613752A (en) | 2005-05-11 |
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