CN101979310B - Production method of 99.9999 percent phosphorus pentoxide - Google Patents
Production method of 99.9999 percent phosphorus pentoxide Download PDFInfo
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- CN101979310B CN101979310B CN201010550797A CN201010550797A CN101979310B CN 101979310 B CN101979310 B CN 101979310B CN 201010550797 A CN201010550797 A CN 201010550797A CN 201010550797 A CN201010550797 A CN 201010550797A CN 101979310 B CN101979310 B CN 101979310B
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Abstract
The invention discloses a production method of 99.9999 percent phosphorus pentoxide. The method comprises the following steps of: feeding 2,000 to 5,000 grams of 99.9999 percent high-purity yellow phosphorus into a tray phosphorus burning region in a combustion tower at the flow speed of between 300 and 350 grams/hour; introducing air or oxygen of which the pressure is between 0.2 and 0.5kgf/cm<2> and the metal impurity content is not more than 50ppb, wherein the excess coefficient molar ratio of effective oxygen is between 1.8 and 2.6, the oxygen flow is controlled to be between 8 to 12 liters/minute, and the air flow is controlled to be between 45 and 65 liters/minute; and reacting and combusting for 6 to 15 hours and collecting a phosphorus pentoxide product from a discharge hole at the bottom of the tower by using a clean composite bag. The maximum single metal impurity content of the product produced by the method does not surpass 100ppb, the total amount of 20 common metal impurities does not surpass 0.5ppm and the doping requirements of a semiconductor separating apparatus and an integrated circuit can be met.
Description
Technical field
The present invention relates to chemical technology field, relate in particular to a kind of working method of Vanadium Pentoxide in FLAKES.
Background technology
High-purity Vanadium Pentoxide in FLAKES mixes particularly at semiconducter device and has a wide range of applications aspect the high-power electric device, and extensively be useful for photoelectron, opticglass, laser crystals makes the field.
At present; Domesticly do not see the report that 99.9999% (6N) level Vanadium Pentoxide in FLAKES technology and product are arranged as yet, high-purity Vanadium Pentoxide in FLAKES that manufacturer can provide, its quality is below 99.995%; And quality stability is poor; Domestic less demanding part semiconductor device client uses reluctantly this product, but result of use is not good, has problems such as the relatively poor and instability of device withstand voltage ability more.6N level import product mainly is that Taiwan-owned enterprise and part are being used the strict enterprise of quality.Abroad, public information shows that extra best best is 99.9999% product of sigma-aldrich, and product price is very expensive.It is the gas mixture that in the combustion zone, feeds exsiccant air and pure oxygen that U.S. Pat 4777025 discloses " a kind of working method of Vanadium Pentoxide in FLAKES " on October 11st, 1988, and combustion liquid yellow phosphorus.Comprise Vanadium Pentoxide in FLAKES in the air-flow that generates.Let air communication overcooling district then, use fluid (should mainly refer to water) cooling draught.Air-flow temperature when flowing through the cooling zone is allowed to condition in the cooling zone and kept 2～5 seconds between 450～600 ℃.The control difficulty was bigger during its method was produced, and it is insufficient to be prone to burning, cools off situation such as incomplete.
Summary of the invention
The highest 100ppb of being no more than of a kind of product individual event metals content impurity that the objective of the invention is to overcome above-mentioned shortcoming and provide; Common 20 metallic impurity total amounts are no more than 0.5ppm, can reach the working method of 99.9999% Vanadium Pentoxide in FLAKES of semi-conductor discrete device and the adulterated requirement of unicircuit.
The working method of a kind of 99.9999% Vanadium Pentoxide in FLAKES of the present invention may further comprise the steps:
(1) is 99.9999% high-purity yellow phosphorus, 2000～5000 grams with purity, press the pellet type that the speed of about 300～350 Grams Per Hours of flow velocity gets in the combustion tower and fire the phosphorus district;
(2) feeding pressure is 0.2～0.5kgf/cm
2Metals content impurity be not more than the air or oxygen of 50ppb, the excess coefficient mol ratio of its available oxygen is 1.8～2.6, the oxygen flow span of control is 8～12 liters/minute, air draught amount span of control is 45～65 liters/minute;
(3) through 6～15 hours reactive combustion, collect the Vanadium Pentoxide in FLAKES product with clean laminated bag discharge port at the bottom of tower.
The working method of 99.9999% above-mentioned Vanadium Pentoxide in FLAKES; Wherein: metals content impurity is not more than the air or oxygen of 50ppb; Be that industrial oxygen or low-pressure compressed air filter through the 0.05um millipore filter; Carry out oil removal treatment through oil eliminator again, last again through being that the Pyatyi air-washer of dry washing composition obtains with 98% CP sulfuric acid.
The working method of 99.9999% above-mentioned Vanadium Pentoxide in FLAKES; Wherein: combustion phosphorus pallet is set in the combustion tower as pellet type combustion phosphorus district; High-purity yellow phosphorus gets on the combustion phosphorus pallet through conduit; The air or oxygen that metals content impurity is not more than 50ppb gets into combustion phosphorus pallet top through conduit, guarantees the abundant burning of phosphorus.
The working method of 99.9999% above-mentioned Vanadium Pentoxide in FLAKES, wherein: combustion tower and combustion phosphorus pallet material are 316L stainless steel, 904 alloys or Hastelloy etc.This material has certain corrosion resistance, and the Vanadium Pentoxide in FLAKES that can guarantee to generate does not influence quality product because of its erosion resistance difference during attached to the tower wall.
The present invention compared with prior art; Have following tangible advantage and useful effect; Can know from above technical scheme: selecting high-purity yellow phosphorus (99.9999%), uncontaminated air or oxygen (metals content impurity is not more than 50ppb) for use is raw material, in the combustion tower internal combustion, generates Vanadium Pentoxide in FLAKES; And the combustion tower material is 316L, 904 or Hastelloy etc., and these materials have certain corrosion resistance, and the Vanadium Pentoxide in FLAKES that can guarantee to generate does not influence quality product because of its erosion resistance difference during attached to the tower wall; Combustion phosphorus pallet is set in the combustion tower, and high-purity yellow phosphorus gets into pallet through conduit, and the air or oxygen that metals content impurity is not more than 50ppb gets into combustion phosphorus pallet top through conduit, guarantees the abundant burning of phosphorus.Collect, be packaged to be product.The highest 100ppb that is no more than of product individual event metals content impurity; Common 20 metallic impurity total amounts are no more than 0.5ppm; Reach the adulterated requirement of semi-conductor discrete device and unicircuit; The particularly adulterated requirement of high-power electric device, and extensively be useful for photoelectron, opticglass, laser crystals manufacturing field.
Embodiment of the present invention further specifies beneficial effect of the present invention.
Embodiment
Embodiment 1:
A kind of working method of 99.9999% Vanadium Pentoxide in FLAKES may further comprise the steps:
(1) be 99.9999% high-purity yellow phosphorus, 2000 grams with purity, the speed of press about 300 Grams Per Hours of flow velocity is fired the phosphorus district through the pellet type that conduit gets on the combustion phosphorus pallet in the combustion tower;
(2) feeding pressure is 0.2kgf/cm
2Industrial oxygen filters through the 0.05um millipore filter, carries out oil removal treatment through oil eliminator again, and last oxygen flow is controlled at 8 liters/minute again through being the Pyatyi gas washing drying installation of dry washing composition with 98% CP sulfuric acid, gets into combustion phosphorus pallet top through conduit;
(3) through 7 hours reactive combustion, collect 4350 gram Vanadium Pentoxide in FLAKES products with clean laminated bag discharge port at the bottom of tower.
Wherein: combustion tower and combustion phosphorus pallet material are the 316L stainless steel.
Through the ICP-MS analyzing and testing, each item metals content impurity: Al=20.87ppb, As=21.35ppb, Ba=1.82ppb, Ca=58.06ppb; Cr=5.36ppb, Cu=8.59ppb, Fe=79.79ppb, Pb=5.36ppb; Mg=23.12ppb, Mn=4.46ppb, Ni=7.55ppb, K=77.11ppb; Na=30.01ppb, Sr=0.25ppb, Zn=30.30ppb, Cd, Co, Li do not detect (＜0.1ppb).Reach the specification of quality of semiconductor doping fully, and extensively be useful for photoelectron, opticglass, laser crystals manufacturing field with Vanadium Pentoxide in FLAKES.
Embodiment 2:
A kind of working method of 99.9999% Vanadium Pentoxide in FLAKES may further comprise the steps:
(1) be 99.9999% high-purity yellow phosphorus, 2000 grams with purity, the speed of press about 350 Grams Per Hours of flow velocity is fired the phosphorus district through the pellet type that conduit gets on the combustion phosphorus pallet in the combustion tower;
(2) feeding pressure is 0.3kgf/cm
2Industrial oxygen filters through the 0.05um millipore filter; Carry out oil removal treatment through oil eliminator again; Last the oxygen flow span of control is 12 liters/minute again through being the Pyatyi gas washing drying installation of dry washing composition with 98% CP sulfuric acid, gets into combustion phosphorus pallet top through conduit;
(3) through 6 hours reactive combustion, collect 4320 gram Vanadium Pentoxide in FLAKES products with clean laminated bag discharge port at the bottom of tower.
Wherein: combustion tower and combustion phosphorus pallet material are 904 alloys.
Through the ICP-MS analyzing and testing, each item metals content impurity: Al=19.35ppb, As=20.85ppb, Ba=1.72ppb, Ca=53.06ppb; Cr=5.59ppb, Cu=10.49ppb, Fe=88.79ppb, Pb=6.36ppb; Mg=25.12ppb, Mn=4.6ppb, Ni=7.74ppb, K=78.13ppb; Na=31.55ppb, Sr=0.25ppb, Zn=32.42ppb, Cd, Co, Li do not detect (＜0.1ppb).
Embodiment 3:
A kind of working method of 99.9999% Vanadium Pentoxide in FLAKES may further comprise the steps:
(1) be 99.9999% high-purity yellow phosphorus, 5000 grams with purity, the speed of press about 350 Grams Per Hours of flow velocity is fired the phosphorus district through the pellet type that conduit gets on the combustion phosphorus pallet in the combustion tower;
(2) feed pressure 0.5kgf/cm
2Low-pressure compressed air needs to filter through the 0.05um millipore filter; Carry out oil removal treatment through oil eliminator again; Last again through being the dry air-washer of Pyatyi gas washing of dry washing composition with 98% CP sulfuric acid, air draught amount span of control is 45 liters/minute, gets into combustion phosphorus pallet top through conduit;
(3) through 15 hours reactive combustion, collect 10800 gram Vanadium Pentoxide in FLAKES products with clean laminated bag discharge port at the bottom of tower.
Wherein: combustion tower and combustion phosphorus pallet material are Hastelloy.
Through the ICP-MS analyzing and testing, each item metals content impurity: Al=25.86ppb, As=15.88ppb, Ba=4.70ppb, Cd=1.06ppb; Co=0.27ppb, Ca=64.26ppb, Cr=2.58ppb, Cu=9.18ppb, Fe=74.40ppb; Pb=8.50ppb, Li=4.04ppb, Mg=33.64ppb, Mn=3.96ppb, Ni=7.07ppb; K=87.31ppb, Na=18.66ppb, Sr＜0.1ppb, Zn=36.58ppb.Product reaches the specification of quality of semiconductor doping with Vanadium Pentoxide in FLAKES fully, and extensively is useful for photoelectron, opticglass, laser crystals manufacturing field.
Embodiment 4:
A kind of working method of 99.9999% Vanadium Pentoxide in FLAKES may further comprise the steps:
(1) be 99.9999% high-purity yellow phosphorus, 5000 grams with purity, the speed of press about 350 Grams Per Hours of flow velocity is fired the phosphorus district through the pellet type that conduit gets on the combustion phosphorus pallet in the combustion tower;
(2) feed pressure 0.5kgf/cm
2Low-pressure compressed air needs to filter through the 0.05um millipore filter; Carry out oil removal treatment through oil eliminator again; Last again through being the dry air-washer of Pyatyi gas washing of dry washing composition with 98% CP sulfuric acid, air draught amount span of control is 65 liters/minute, gets into combustion phosphorus pallet top through conduit;
(3) through 15 hours reactive combustion, collect 10600 gram Vanadium Pentoxide in FLAKES products with clean laminated bag discharge port at the bottom of tower.
Wherein: combustion tower and combustion phosphorus pallet material are the 316L stainless steel.
Through the ICP-MS analyzing and testing, each item metals content impurity: Al=27.95ppb, As=13.28ppb, Ba=3.56ppb, Cd=1.35ppb; Co=0.45ppb, Ca=64.98ppb, Cr=2.79ppb, Cu=5.17ppb, Fe=65.40ppb; Pb=8.30ppb, Li=3.54ppb, Mg=30.64ppb, Mn=5.96ppb, Ni=7.24ppb; K=80.31ppb, Na=15.36ppb, Sr＜0.14ppb, Zn=32.38ppb.Product reaches the specification of quality of semiconductor doping with Vanadium Pentoxide in FLAKES fully, and extensively is useful for photoelectron, opticglass, laser crystals manufacturing field.
Comparative Examples 1: by the description of implementing 1; Industrial oxygen filters and the oil eliminator oil removal treatment without the 0.05um millipore filter; Or its gas handles without the dry air-washer of the Pyatyi gas washing that with 98% analytical pure sulfuric acid is dry washing composition, and the finished product quality has great reduction
Through the ICP-MS analyzing and testing, following metals content impurity: Al=98.12ppb, Ba=35.56ppb, Ca=146.28ppb, Fe=205.26ppb, K=280.24ppb, Na=145.6ppb, Zn=131.05ppb.Partial impurities content increases obviously,
Comparative Examples 2: the description of pressing embodiment 3; Pressurized air is filtered and the oil eliminator oil removal treatment without the 0.05um millipore filter; Or its gas handles without the dry air-washer of the Pyatyi gas washing that with 98% analytical pure sulfuric acid is dry washing composition, and the finished product quality has great reduction
Through the ICP-MS analyzing and testing, following metals content impurity: Al=122.3ppb, Ba=38.45ppb, Ca=174.15ppb, Fe=204.35ppb, K=320.24ppb, Na=122.6ppb, Zn=141.2ppb.Partial impurities content increases obviously,
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any pro forma restriction; Anyly do not break away from technical scheme content of the present invention, to any simple modification, equivalent variations and modification that above embodiment did, all still belong in the scope of technical scheme of the present invention according to technical spirit of the present invention.
Claims (5)
1. the working method of a Vanadium Pentoxide in FLAKES may further comprise the steps:
(1) is 99.9999% high-purity yellow phosphorus, 2000～5000 grams with purity, press the pellet type that the speed of flow velocity 300～350 Grams Per Hours gets in the combustion tower and fire the phosphorus district;
(2) feeding pressure is 0.2～0.5kgf/cm
2Metals content impurity be not more than the air or oxygen of 50ppb, the excess coefficient mol ratio of its available oxygen is 1.8～2.6, the oxygen flow span of control is 8～12 liters/minute, air draught amount span of control is 45～65 liters/minute;
(3) through 6～15 hours reactive combustion, collect the Vanadium Pentoxide in FLAKES product with clean laminated bag discharge port at the bottom of tower.
2. the working method of 99.9999% Vanadium Pentoxide in FLAKES as claimed in claim 1; Wherein: metals content impurity is not more than the air or oxygen of 50ppb; Be that industrial oxygen or low-pressure compressed air filter through the 0.05um millipore filter; Carry out oil removal treatment through oil eliminator again, last again through being that the Pyatyi air-washer of dry washing composition obtains with 98% CP sulfuric acid.
3. according to claim 1 or claim 2 the working method of 99.9999% Vanadium Pentoxide in FLAKES, wherein: the combustion tower material is 316L stainless steel, 904 alloys or Hastelloy.
4. according to claim 1 or claim 2 the working method of 99.9999% Vanadium Pentoxide in FLAKES, wherein: high-purity yellow phosphorus gets on the combustion phosphorus pallet through conduit, and the air or oxygen that metals content impurity is not more than 50ppb gets into combustion phosphorus pallet top through conduit.
5. the working method of 99.9999% Vanadium Pentoxide in FLAKES as claimed in claim 4, wherein: combustion tower combustion phosphorus pallet material is 316L stainless steel, 904 alloys or Hastelloy.
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| CN201010550797A CN101979310B (en) | 2010-11-19 | 2010-11-19 | Production method of 99.9999 percent phosphorus pentoxide |
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| CN101979310B true CN101979310B (en) | 2012-10-10 |
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| RU2539057C1 (en) * | 2013-07-15 | 2015-01-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "ДАГЕСТАНСКИЙ ГОСУДАРСТВЕННЫЙ УНИВЕРСИТЕТ" | Method of obtaining phosphorus pentoxide |
| CN108975294B (en) * | 2018-10-17 | 2021-11-12 | 贵阳精一科技有限公司 | Production device and method of electronic grade phosphorus pentoxide |
| CN109607502B (en) * | 2019-01-16 | 2020-12-01 | 中州新材料(杭州)有限公司 | Energy-saving and environment-friendly phosphorus pentoxide production process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4525329A (en) * | 1983-04-29 | 1985-06-25 | Hoechst Aktiengesellschaft | Process and apparatus for making phosphorus pentoxide with utilization of reaction heat |
| US4603039A (en) * | 1983-05-13 | 1986-07-29 | Hoechst Aktiengesellschaft | Process for making phosphorus pentoxide and optionally phosphoric acid with utilization of the reaction heat |
| CN1033780A (en) * | 1987-07-27 | 1989-07-12 | 罗仑-波莱尼克有限公司施托福化学公司部 | P will ignite 4Material is converted into the method for Vanadium Pentoxide in FLAKES material |
| CN101214939A (en) * | 2008-01-14 | 2008-07-09 | 四川大学 | Method for preparing phosphorus pentoxide by combustion dynamic wave |
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2010
- 2010-11-19 CN CN201010550797A patent/CN101979310B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4525329A (en) * | 1983-04-29 | 1985-06-25 | Hoechst Aktiengesellschaft | Process and apparatus for making phosphorus pentoxide with utilization of reaction heat |
| US4603039A (en) * | 1983-05-13 | 1986-07-29 | Hoechst Aktiengesellschaft | Process for making phosphorus pentoxide and optionally phosphoric acid with utilization of the reaction heat |
| CN1033780A (en) * | 1987-07-27 | 1989-07-12 | 罗仑-波莱尼克有限公司施托福化学公司部 | P will ignite 4Material is converted into the method for Vanadium Pentoxide in FLAKES material |
| CN101214939A (en) * | 2008-01-14 | 2008-07-09 | 四川大学 | Method for preparing phosphorus pentoxide by combustion dynamic wave |
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