CN108975294B - Production device and method of electronic grade phosphorus pentoxide - Google Patents
Production device and method of electronic grade phosphorus pentoxide Download PDFInfo
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Abstract
A production device and a method of electronic grade phosphorus pentoxide are disclosed, the device consists of a primary reactor, a temperature controller, a heater, a secondary reactor, a large-flow fan, a condenser, a material collector and a dryer; the method comprises the following steps: (1) removing air in the equipment by using nitrogen, placing high-purity yellow phosphorus in a first-stage reactor, covering the reactor with ultrahigh-purity water, and heating the reactor until water is completely evaporated; (2) introducing high-purity oxygen into a primary reactor to enable the high-purity oxygen to react with yellow phosphorus in a combustion mode; (3) and introducing high-purity oxygen into the secondary reactor, continuing to perform full oxidation reaction, and collecting to obtain a high-purity phosphorus pentoxide product. The invention adopts the production process of firstly generating the phosphorus trioxide and then converting the phosphorus trioxide into the phosphorus pentoxide, the combustion reaction is mild, and the process is easy to control; the sealing production device made of the high-purity quartz material is not influenced by the environment, the product purity can stably reach 6N grade, and the product purity is high and the quality stability is good. Is suitable for preparing electronic grade phosphorus pentoxide by using high-purity yellow phosphorus.
Description
Technical Field
The invention relates to phosphorus oxide, in particular to phosphorus pentoxide, and specifically relates to a production device and a process method of electronic grade phosphorus pentoxide.
Background
The high-purity electronic grade phosphorus pentoxide is widely applied to the semiconductor industry and the photoelectron industry, is used as a doping source of a semiconductor phosphorus source, or is used for producing optical or heat-resisting glass, or is used as a manufacturing raw material of a high-purity phosphide product.
At present, the domestic method for producing high-purity phosphorus pentoxide is mainly prepared by directly burning yellow phosphorus in sufficient oxygen or air, and in the domestic production technology, patent CN 101979310B discloses a production method of 99.9999% phosphorus pentoxide, which is to prepare the phosphorus pentoxide by controlling excessive oxygen with flow of 8-12L/min, air with flow rate of 45-65L/min and liquid yellow phosphorus with flow rate of about 300-500 g/h to burn in a tray type phosphorus burning area in a burning tower. The patent CN 103553010B discloses a production process of high-purity phosphorus pentoxide, which comprises the steps of heating and melting industrial yellow phosphorus, sequentially carrying out alkali washing, water washing and microfiltration, carrying out high-strength phosphorus spraying combustion on the obtained refined liquid yellow phosphorus in a combustion furnace to obtain a phosphorus pentoxide gasification product, and carrying out forced cold precipitation on the phosphorus pentoxide gasification product to obtain a high-purity phosphorus pentoxide product. Patent CN 104528674A discloses a method for producing high-purity phosphorus pentoxide in large scale, which comprises the steps of feeding liquid yellow phosphorus into a phosphorus combustion furnace for combustion, adopting a molecular sieve for temperature swing adsorption and drying air, cooling gaseous phosphorus pentoxide to obtain a solid phosphorus pentoxide product, remarkably improving the drying effect, avoiding the influence of moisture and sulfate radicals on the product quality, and improving the product purity. In the production of the methods of the patents, yellow phosphorus reacts violently in excessive oxygen and can only be carried out in a combustion tower, so that the requirements on equipment are high, the influence of the equipment is great, and the influence on the quality of products is great.
Disclosure of Invention
The invention aims to provide a production device of electronic grade phosphorus pentoxide, which can produce 6N (99.9999%) grade phosphorus pentoxide in batches and can effectively stabilize the product quality.
The invention also aims to provide a production method of the electronic grade phosphorus pentoxide, which has mild production conditions and easier process control and can overcome the defects of the prior art.
The production device of the electronic grade phosphorus pentoxide that the inventor provided comprises primary reactor, thermostat, heater, secondary reactor, large-traffic fan, condenser, material collector and desicator, wherein: the primary reactor is fixed in the heater, one end of the primary reactor is connected with a purified oxygen inlet pipe with a valve and flow control, and the other end of the primary reactor is connected with the one-way valve and then connected with the secondary reactor; the secondary reactor is provided with two air inlets and an air outlet, the two air inlets are respectively connected with an inert gas inlet pipe and a primary reactor air outlet pipe with a one-way valve, the air outlet end is connected with a high-flow fan, and the air outlet end of the high-flow fan is connected with a condenser; the tail end of the condenser is connected with a material collector, a material collecting bag in the material collector is fixed at the tail end of the air outlet pipeline, and the air outlet end of the material collector is connected with the dryer; the dryer is a cylindrical container filled with liquid desiccant; the heater is a jacketed container with a groove in the center, a heating part and a heating medium are arranged in the container, a thermocouple is inserted in the medium for heating, and a thermocouple guide pipe is connected with a temperature controller; the temperature controller is internally provided with a chip and an electronic integrated circuit, and the heating temperature of the heater is controlled to rise and fall according to a set program.
The first-stage reactor and the second-stage reactor are cylindrical containers and are made of high-purity quartz materials.
The heater is cylindrical as a whole, the central groove is cylindrical, the diameter of the central groove is larger than that of the first-stage reactor, and the central groove is used for fixing a heating part of the first-stage reactor.
The large-flow fan is an adjustable fan.
The single-tube straight condenser of the condenser is not easy to cause the blockage of solid particles, and warm water is used as cooling liquid.
The material collector adopts a clean transparent nonmetal container, and the material collecting bag is a clean composite bag.
The inert gas is purified nitrogen or argon.
The liquid drying agent in the dryer is concentrated sulfuric acid.
The production method of the electronic grade phosphorus pentoxide provided by the inventor adopts the device to prepare the high-purity phosphorus pentoxide, and comprises the following steps:
(1) placing high-purity yellow phosphorus with the purity of 6N in a primary reactor, covering the yellow phosphorus with ultrahigh-purity water, controlling a heater by a temperature controller to heat the primary reactor at 105-110 ℃ until trace moisture in the pure water and the yellow phosphorus is completely evaporated, and then closing the heater; the tail gas is discharged through a one-way valve by a large-flow fan;
(2) opening the inlet valve, outlet valve and receiving valve of the secondary reactor, closing the exhaust valve and pipeline valve in the device(ii) a Opening a gas pressure regulating valve on a gas inlet pipe, introducing high-purity oxygen subjected to oil removal, water removal and 0.1 mu m micropore filtration treatment into a primary reactor to enable the high-purity oxygen to react with yellow phosphorus in a combustion manner, wherein insufficient oxygen in the primary reactor reacts with the yellow phosphorus in the combustion manner to generate smoke-shaped gaseous P2O3And P2O5Pumping into a secondary reactor by a high-flow fan;
(3) introducing high-purity oxygen into the secondary reactor, and introducing incompletely oxidized P2O3Reacting with sufficient oxygen in the reactor to form P2O5Pumping the powder into a condenser through a large-flow fan, cooling the powder into powdery phosphorus pentoxide, and collecting the powdery phosphorus pentoxide in a material receiving bag; and finally obtaining the phosphorus pentoxide product after full reaction.
The invention adopts the production process of firstly generating the phosphorus trioxide and then converting the phosphorus trioxide into the phosphorus pentoxide, the combustion reaction is mild, and the process is easy to control; the sealing production device made of the high-purity quartz material is not influenced by the environment, the product purity can stably reach 6N grade, and the product purity is high and the quality stability is good. Is suitable for preparing electronic grade phosphorus pentoxide by using high-purity yellow phosphorus.
Drawings
FIG. 1 is a diagram of a production apparatus of the present invention.
The labels in the figure are: the system comprises a heater 1, a first-stage reactor 2, a temperature controller 3, an air pressure regulating valve A4, a flowmeter A5, an air pressure regulating valve B6, a flowmeter B7, a one-way control valve 8, a secondary reactor inlet valve 9, a secondary reactor 10, a pipeline valve 11, a secondary reactor outlet valve 12, a large-flow fan 13, an exhaust valve 14, a material receiving valve 15, a condenser 16, a material receiving bag 17, a material receiver 18, a one-way valve 19 and a dryer 20.
Detailed Description
The invention is further described below with reference to the accompanying drawings and examples.
EXAMPLE 1 production apparatus for electronic grade phosphorus pentoxide
The production device of electronic grade phosphorus pentoxide shown in fig. 1 is composed of a primary reactor 2, a temperature controller 3, a heater 1, a secondary reactor 10, a large flow fan 13, a condenser 16, a material collector 18 and a dryer 20, wherein: the primary reactor 2 is arranged in the heater 1, one end of the primary reactor 2 is connected with purified oxygen inlet pipes with air pressure regulating valves 4 and 6 and flow control, and the other end of the primary reactor 2 is connected with a one-way control valve 8 and then connected with the secondary reactor 10; the secondary reactor 10 is provided with two air inlets and an air outlet, the two air inlets are respectively connected with an inert gas inlet pipe and an air outlet pipe of the primary reactor 2 with a one-way control valve 8, the air outlet end is connected with a large-flow fan 13, and the air outlet end of the large-flow fan 13 is connected with a condenser 16; the tail end of the condenser 16 is connected with a material collector 18, a material collecting bag 17 in the material collector 18 is fixed at the tail end of the air outlet pipeline, and the air outlet end of the material collector 18 is connected with a dryer 20; the drier 20 is a cylindrical container filled with a liquid desiccant concentrated sulfuric acid; the heater 1 is a jacketed container with a groove in the center, a heating part and a heating medium are arranged in the container, a thermocouple is inserted in the medium heating, and a thermocouple guide pipe is connected with the temperature controller 3; the temperature controller 3 is internally provided with a chip and an electronic integrated circuit, and the heating temperature of the heater 1 is controlled to rise and fall according to a set program. The primary reactor 2 and the secondary reactor 10 are both cylindrical containers and are made of high-purity quartz materials.
The heater 1 is cylindrical as a whole, the central groove is cylindrical, the diameter of the central groove is larger than that of the first-stage reactor 2, and the central groove is used for fixing a heating part of the first-stage reactor.
The large flow fan 13 is an adjustable fan. The condenser 16 is a single-tube straight type condenser, and warm water is used as a cooling liquid. The material collector 18 adopts a clean transparent nonmetal container, and the material collecting bag 17 is a clean composite bag.
Example 2 electronic grade phosphorus pentoxide was prepared using the apparatus of example 1, with the equipment purged of air with purified nitrogen, according to the following procedure:
(1) 1.5kg of liquid high-purity yellow phosphorus with the purity of 6N is transferred into a primary reactor 2 through siphoning, covered by ultra-high-purity water, a pipeline valve 11 and an exhaust valve 14 in the device are opened, a large-flow fan 13 is operated, and meanwhile, a temperature controller 3 is adjusted to control a heater 1 to heat the primary reactor at 105 ℃ until trace moisture in the pure water and the yellow phosphorus is completely evaporated;
(2) opening a secondary reactor inlet valve 9, a secondary reactor outlet valve 12 and a receiving valve 15, and closing an exhaust valve 14 and a pipeline valve 11 in the device; opening the air pressure regulating valve A4 and the air pressure regulating valve B6 on the air inlet pipe, introducing high-purity oxygen subjected to oil removal, water removal and 0.1 mu m micropore filtration into the primary reactor 2 at the flow rate of 2.5L/min to react with yellow phosphorus in a combustion manner, wherein insufficient oxygen in the primary reactor 2 reacts with yellow phosphorus in a combustion manner to generate smoke-like gaseous P2O3And P2O5Is pumped into the secondary reactor 10 by a large flow fan 13;
(3) high purity oxygen was fed into the secondary reactor 10 at a flow rate of 10L/min, incompletely oxidized P2O3Reacts with sufficient oxygen in reactor 10 to form P2O5Then the mixture is pumped into a condenser 16 by a large flow fan 13 and cooled into powdery phosphorus pentoxide which is collected in a material collecting bag 17; after 8 hours of full reaction, 3.25kg of phosphorus pentoxide product is finally obtained.
After the product is sampled and treated, the product is detected on an ICP-MS machine, and the detection and analysis results of the impurity content are shown in Table 1:
TABLE 1P of example 12O5Results of measurement and analysis of impurity content (unit ppb, N.D means no detection)
| Detecting items | Al | As | Ba | Ca | Cr | Cu | Fe | Pb | Mg |
| Test results | 20.43 | 20.21 | 1.84 | 38.44 | 4.81 | 7.95 | 57.49 | 4.91 | 19.33 |
| Detecting items | Mn | Ni | K | Na | Sr | Zn | Cd | Co | Li |
| Test results | 4.54 | 5.18 | 66.98 | 33.55 | N.D | 23.44 | N.D | N.D | N.D |
The quality of the obtained product completely meets the quality requirements of phosphorus pentoxide in the semiconductor industry and the photoelectron industry.
Example 3 using the manufacturing apparatus of example 1, electronic grade phosphorus pentoxide was prepared by first purging the equipment of air with purified argon gas according to the following procedure:
(1) transferring 2kg of liquid high-purity yellow phosphorus with the purity of 6N into a primary reactor 2 through siphoning, covering with ultra-high-purity water, starting a pipeline valve 11 and an exhaust valve 14 in the device, operating a large-flow fan 13, adjusting a temperature controller 3 to control a heater 1 to heat the primary reactor at 110 ℃, and stopping heating until trace moisture in pure water and yellow phosphorus is completely evaporated;
(2) opening a secondary reactor inlet valve 9, a secondary reactor outlet valve 12 and a receiving valve 15, and closing an exhaust valve 14 and a pipeline valve 11 in the device; opening the air pressure regulating valve A4 and the air pressure regulating valve B6 on the air inlet pipe, introducing high-purity oxygen subjected to oil removal, water removal and 0.1 mu m micropore filtration into the primary reactor 2 at the flow rate of 3L/min to react with yellow phosphorus in a combustion manner, wherein insufficient oxygen in the primary reactor 2 reacts with yellow phosphorus in a combustion manner to generate smoke-like gaseous P2O3And P2O5Is pumped into the secondary reactor 10 by a large flow fan 13;
(3) high purity oxygen was fed into the secondary reactor 10 at a flow rate of 10L/min, incompletely oxidized P2O3Reacts with sufficient oxygen in reactor 10 to form P2O5Then the mixture is pumped into a condenser 16 by a large flow fan 13 and cooled into powdery phosphorus pentoxide which is collected in a material collecting bag 17; after 10 hours of full reaction, 4.29kg of phosphorus pentoxide product is finally obtained.
After the product is sampled and treated, the product is detected on an ICP-MS machine, and the detection and analysis results of the impurity content are shown in Table 2:
table 2 example 2P2O5Results of measurement and analysis of impurity content (unit ppb, N.D means no detection)
| Detecting items | Al | As | Ba | Ca | Cr | Cu | Fe | Pb | Mg |
| Test results | 21.13 | 22.24 | 2.04 | 45.44 | 3.34 | 7.58 | 56.35 | 3.78 | 21.78 |
| Detecting items | Mn | Ni | K | Na | Sr | Zn | Cd | Co | Li |
| Test results | 3.99 | 4.33 | 54.76 | 36.78 | N.D | 19.56 | N.D | N.D | N.D |
The quality of the obtained product completely meets the quality requirements of phosphorus pentoxide in the semiconductor industry and the photoelectron industry.
Claims (6)
1. A method of producing electronic grade phosphorus pentoxide, comprising the steps of:
(1) building production equipment: the production equipment consists of a primary reactor, a temperature controller, a heater, a secondary reactor, a large-flow fan, a condenser, a material collector and a dryer, wherein: the primary reactor is fixed in the heater, one end of the primary reactor is connected with a purified oxygen inlet pipe with a valve and flow control, and the other end of the primary reactor is connected with the one-way valve and then connected with the secondary reactor; the secondary reactor is provided with two air inlets and an air outlet, the two air inlets are respectively connected with an inert gas inlet pipe and a primary reactor air outlet pipe with a one-way valve, the air outlet end is connected with a high-flow fan, and the air outlet end of the high-flow fan is connected with a condenser; the tail end of the condenser is connected with a material collector, a material collecting bag in the material collector is fixed at the tail end of the air outlet pipeline, and the air outlet end of the material collector is connected with the dryer; the dryer is a cylindrical container filled with liquid desiccant; the heater is a jacketed container with a groove in the center, a heating part and a heating medium are arranged in the container, a thermocouple is inserted in the medium for heating, and a thermocouple guide pipe is connected with a temperature controller; a chip and an electronic integrated circuit are arranged in the temperature controller, and the heating temperature of the heater is controlled to rise and fall according to a set program;
(2) firstly, removing air in equipment by using purified inert gas, placing high-purity yellow phosphorus with the purity of 6N in a primary reactor, covering the primary reactor by using ultra-high-purity water, controlling a heater by a temperature controller to heat the primary reactor at 105-110 ℃ until trace moisture in the pure water and the yellow phosphorus is completely evaporated, and then closing the heater; the tail gas is discharged through a one-way valve by a large-flow fan;
(3) opening an inlet valve, an outlet valve and a receiving valve of the secondary reactor, and closing an exhaust valve and a pipeline valve in the device; opening a gas pressure regulating valve on a gas inlet pipe, introducing high-purity oxygen subjected to oil removal, water removal and 0.1 mu m micropore filtration treatment into a primary reactor to enable the high-purity oxygen to react with yellow phosphorus in a combustion manner, wherein insufficient oxygen in the primary reactor reacts with the yellow phosphorus in the combustion manner to generate smoke-shaped gaseous P2O3And P2O5Pumping into a secondary reactor by a high-flow fan;
(4) introducing high-purity oxygen into the secondary reactor, and introducing incompletely oxidized P2O3Reacting with sufficient oxygen in the reactor to form P2O5After full reaction, the mixture is pumped into a condenser by a large flow fan and cooled into powdery phosphorus pentoxide which is collected in a material collecting bag; finally obtaining the phosphorus pentoxide product.
2. The method of producing electronic grade phosphorus pentoxide of claim 1, wherein: the primary reactor and the secondary reactor are both cylindrical containers and are made of high-purity quartz materials.
3. The method of producing electronic grade phosphorus pentoxide of claim 1, wherein: the heater is integrally cylindrical, the central groove is cylindrical, the diameter of the central groove is larger than that of the first-stage reactor, and the central groove is used for fixing a heating part of the first-stage reactor.
4. The method of producing electronic grade phosphorus pentoxide of claim 1, wherein: the large-flow fan is an adjustable fan.
5. The method of producing electronic grade phosphorus pentoxide of claim 1, wherein: the condenser is a single-tube straight condenser, and warm water is used as cooling liquid.
6. The method of producing electronic grade phosphorus pentoxide of claim 1, wherein: the material collector adopts a clean transparent nonmetal container, and the material collecting bag is a clean composite bag.
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| 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 |
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| CN202729802U (en) * | 2012-08-28 | 2013-02-13 | 向东 | Production device of electronic-grade phosphoric acid |
| CN203065162U (en) * | 2012-11-15 | 2013-07-17 | 防城港博森化工有限公司 | Horizontal yellow phosphorus combustion furnace |
| CN103288063A (en) * | 2013-06-07 | 2013-09-11 | 江苏天源化工有限公司 | New technology for producing phosphorus pentoxide |
| CN103771367A (en) * | 2013-12-30 | 2014-05-07 | 广西明利化工有限公司 | Method for producing electronic-grade phosphoric acid by stirring and crystallizing |
| CN104528674A (en) * | 2015-01-22 | 2015-04-22 | 中国化学工程第七建设有限公司 | Method for large-scale production of high-purity diphosphorus pentoxide |
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- 2018-10-17 CN CN201811205869.4A patent/CN108975294B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN101784475A (en) * | 2007-11-28 | 2010-07-21 | 斯特瑞马克控股公司 | Process for the manufacture of p4o6 |
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| CN104528674A (en) * | 2015-01-22 | 2015-04-22 | 中国化学工程第七建设有限公司 | Method for large-scale production of high-purity diphosphorus pentoxide |
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