CN116873885A - Method for deep dearsenification of high-purity yellow phosphorus through reactive distillation - Google Patents
Method for deep dearsenification of high-purity yellow phosphorus through reactive distillation Download PDFInfo
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- CN116873885A CN116873885A CN202310853635.5A CN202310853635A CN116873885A CN 116873885 A CN116873885 A CN 116873885A CN 202310853635 A CN202310853635 A CN 202310853635A CN 116873885 A CN116873885 A CN 116873885A
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- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000000066 reactive distillation Methods 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 25
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011552 falling film Substances 0.000 claims abstract description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 238000010926 purge Methods 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 4
- 239000002151 riboflavin Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 2
- 230000008676 import Effects 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 20
- 239000011574 phosphorus Substances 0.000 description 20
- 229910052751 metal Inorganic materials 0.000 description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 239000013206 MIL-53 Substances 0.000 description 9
- 239000007800 oxidant agent Substances 0.000 description 9
- 239000002184 metal Substances 0.000 description 8
- 230000001590 oxidative effect Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 239000013291 MIL-100 Substances 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001577 simple distillation Methods 0.000 description 2
- 239000013179 MIL-101(Fe) Substances 0.000 description 1
- 239000013216 MIL-68 Substances 0.000 description 1
- 239000013215 MIL-88B Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/04—Purification of phosphorus
- C01B25/047—Purification of phosphorus of yellow phosphorus
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention provides a method for deeply removing arsenic by reactive distillation of high-purity yellow phosphorus. The method mainly comprises the key equipment such as a reaction rectifying tower T101, a falling film evaporator E101, a circulating pump P101 and the like. The method can realize the dearsenification of the yellow phosphorus without introducing other impurities, and the preparation of the electronic grade high-purity yellow phosphorus lays a solid foundation for further preparation of the electronic grade phosphoric acid. The method can be widely applied to the fields of medicine, food, automobile manufacturing, aviation, military industry and the like, and can reduce the dependence of the high-purity yellow phosphorus on foreign import.
Description
Technical Field
The invention relates to a method for deeply removing arsenic in the yellow phosphorus rectification reaction process.
Background
Yellow phosphorus is an important chemical basic raw material, china is one of the world phosphorite resource major countries, the yellow phosphorus yield is about 80% of the world, the domestic industrial yellow phosphorus is usually produced by adopting an electric furnace method, and the product purity is generally 99.8%. The impurities are mainly metal elements, semi-metal elements and organic impurities, wherein the most main impurities are semi-metal elements arsenic and organic matters.
The yellow phosphorus molecule (P4) is in the form of phosphorus disposed at each vertex of the regular tetrahedron, and it is presumed that arsenic as an impurity contained in yellow phosphorus may be present in a state of being substituted with one of the phosphorus in the regular tetrahedron. Therefore, it is difficult to separate arsenic from yellow phosphorus by simple distillation, rectification, or the like. At present, main processes for removing arsenic from yellow phosphorus include a distillation method, a melt crystallization method, an alloy reduced pressure distillation method and the like. U.S. Pat. No. 4,182,62 discloses a distillation process for purifying yellow phosphorus by simple distillation, wherein the arsenic content in the yellow phosphorus which is separated by refining is 1ppm, and the arsenic content is higher. The alloy reduced pressure distillation method uses a metal having a low melting point such as Al, pb, in, tl, which is easily alloyed with arsenic in phosphorus, and heats the metal at a temperature equal to or higher than the melting point of the metal to alloy impurities with the metal, and then the metal is distilled under reduced pressure to recover phosphorus. When the method is used for carrying out heat treatment on phosphorus and metals, the phosphorus and the metals need to be heated to be higher than the melting point of each metal, the metal alloy method needs high reaction temperature, equipment needs high heat resistance requirement, operation is difficult, and production energy consumption is high. AZschalich et al used concentrated sulfuric acid as the oxidizing agent to reduce the sulfur content in phosphorus, mixed the phosphorus and concentrated sulfuric acid intensively to form an emulsion, broken the emulsion by contact with water or dilute sulfuric acid, and then separated the phosphorus and dilute sulfuric acid immediately. The separated phosphorus was then stored in water until further treatment was required, reducing the sulfur mass concentration therein to about 50mg/L. The method can only reduce the content of sulfur impurities in the waste sulfuric acid liquid, and the generated waste sulfuric acid liquid is difficult to treat. Nitric acid can be used as an oxidizing agent for arsenic removal, zhou Junhong and the like, and yellow phosphorus is removed by a nitric acid oxidation method, and the results show that the arsenic removal effect is poor with the decrease of the arsenic content in yellow phosphorus. Liu Jun and the like adopt ferric sulfate composite oxidant to remove arsenic from yellow phosphorus, and have good arsenic removal effect, but the arsenic content is still higher.
The arsenic content in the industrial yellow phosphorus can reach 70-l 00ppm, and the arsenic content in the electronic grade low-arsenic yellow phosphorus is required to be less than 5ppb. The invention mainly provides a method for deep dearsenification by reactive distillation, which has the arsenic content lower than 5ppb and provides a raw material for preparing electronic grade phosphoric acid.
Disclosure of Invention
According to the defects of the prior art, the invention provides a method for deep dearsenification of high-purity yellow phosphorus by reactive distillation. The method mainly comprises the key equipment such as a reaction rectifying tower T101, a falling film evaporator E101, a circulating pump P101 and the like. The method can realize the dearsenification of the yellow phosphorus without introducing other impurities, and the preparation of the electronic grade high-purity yellow phosphorus lays a solid foundation for further preparation of the electronic grade phosphoric acid. The method can be widely applied to the fields of medicine, food, automobile manufacturing, aviation, military industry and the like, and can reduce the dependence of the high-purity yellow phosphorus on foreign import.
A method for deep dearsenification of high-purity yellow phosphorus by reactive distillation comprises the following steps:
i, after nitrogen purges the rectifying tower, yellow phosphorus is added into the rectifying tower, hydrogen peroxide is slowly pumped in, and then a catalyst is added;
II, after vacuumizing, starting heating and starting a circulating pump, conveying tower kettle materials from the circulating pump to a falling film evaporator, enabling liquid phase unreacted materials coming out of the lower part of the falling film evaporator and raw materials in the step (1) to further react in a reaction kettle, enabling gas phase to enter the bottom of a rectifying tower, enabling liquid at the bottom of the reaction kettle to be continuously conveyed to the falling film evaporator by the circulating pump, starting tower top condensate water circulation and tower kettle heating, starting reflux operation after the temperature of the tower kettle is raised to be stable, enabling yellow phosphorus liquid flowing back from the tower top and yellow phosphorus steam rising from the tower bottom to fully contact in the tower, performing gas-liquid exchange, and extracting high-purity yellow phosphorus.
The catalyst is selected from any one of MIL-100 (Fe), MIL-125 (Ti), MIL-101 (Fe), MIL-88B (Fe), MIL-53 (Al), MIL-53 (Fe), MIL-47 (V) and MIL-68 (Fe).
The added volume of the hydrogen peroxide is 5-40% of that of the yellow phosphorus, and the mass of the catalyst is 0.01-3% of that of the yellow phosphorus.
The added volume of the hydrogen peroxide is 10% -30% of that of the yellow phosphorus, and the mass of the catalyst is 0.1% -0.5% of that of the yellow phosphorus.
In the rectification process, the temperature of the top of the rectification tower is 100-130 ℃; the temperature of the tower bottom of the rectifying tower is 150-175 ℃; the pressure in the rectifying tower is 12-25kPa, and the reflux ratio of the top of the rectifying tower is 3-6:1.
In the preferred scheme, the top temperature of the rectifying tower is 120 ℃; the temperature of the tower bottom of the rectifying tower is 165 ℃; the pressure in the rectifying tower is 20kPa, and the reflux ratio of the top of the rectifying tower is 6:1.
The method mainly comprises the key equipment such as a reaction rectifying tower T101, a falling film evaporator E101, a circulating pump P101 and the like.
According to the invention, the organic frame material is used as a catalyst, hydrogen peroxide is used as an oxidant for high-purity yellow phosphorus oxidation, the purity of the high-purity yellow phosphorus can be improved under the condition that other impurities are not introduced, the yellow phosphorus is dearsenified by using a rectifying tower through a reaction rectification method, the process is reliable, the discharge of three wastes is low, the safe operation is convenient, the dearsenification effect is obvious, the arsenic content in the product is low, the index requirement of electronic-grade low-arsenic yellow phosphorus can be met, the method has important significance for the subsequent preparation of electronic-grade phosphoric acid, and the method is a green and efficient high-purity yellow phosphorus dearsenification method.
Drawings
FIG. 1 is a process flow diagram of deep dearsenification of high purity yellow phosphorus by reactive distillation.
E101: falling film evaporator, T101: reactive rectifying tower, P101: and a circulation pump.
Detailed Description
Comparative example 1
As shown in figure 1, the low-arsenic yellow phosphorus is obtained by a rectification technology by taking high-purity yellow phosphorus as a raw material without using any oxidant such as hydrogen peroxide, and without using any catalyst. Firstly, nitrogen purging and water adding are carried out, a nitrogen main pipe is opened to be connected with a valve of the reaction tank, a vacuum pump is started to exchange air, the vacuum degree is l0kPa, and full nitrogen purging is carried out. The temperature of the top of the rectifying tower is 120 ℃; the temperature of the tower bottom of the rectifying tower is 165 ℃; the pressure in the rectifying tower is 20kPa, and the reflux ratio of the top of the rectifying tower is 6:1. A certain amount of yellow phosphorus was added and weighed in the reaction kettle. The yellow phosphorus vapor is cold suspected through a tower top condenser and flows back into the tower, the yellow phosphorus liquid flowing back from the tower top and the yellow phosphorus vapor rising from the tower bottom are fully contacted in the tower to carry out gas-liquid exchange, and the yellow phosphorus with the arsenic content of 78ppb is extracted from the tower top.
Comparative example 2
As shown in figure 1, the high-purity yellow phosphorus is used as a raw material, hydrogen peroxide is used as an oxidant, and the low-arsenic yellow phosphorus is obtained by a reaction rectification technology under the condition of not using any catalyst. Firstly, nitrogen purging and water adding are carried out, a nitrogen main pipe is opened to be connected with a valve of the reaction tank, a vacuum pump is started to exchange air, the vacuum degree is l0kPa, and full nitrogen purging is carried out. The temperature of the top of the rectifying tower is 120 ℃; the temperature of the tower bottom of the rectifying tower is 165 ℃; the pressure in the rectifying tower is 20kPa, and the reflux ratio of the top of the rectifying tower is 6:1. Adding a certain amount of yellow phosphorus, weighing in a reaction kettle, and slowly pumping hydrogen peroxide, wherein the added volume of the hydrogen peroxide is 20% of that of the yellow phosphorus. The yellow phosphorus vapor is cold suspected through a tower top condenser and flows back into the tower, the yellow phosphorus liquid flowing back from the tower top and the yellow phosphorus vapor rising from the tower bottom are fully contacted in the tower to carry out gas-liquid exchange, and the yellow phosphorus with the arsenic content of 36ppb is extracted from the tower top.
Example 1
As shown in figure 1, the low-arsenic yellow phosphorus is obtained by using high-purity yellow phosphorus as a raw material, MIL-100 (Fe) as a catalyst and hydrogen peroxide as an oxidant through a reaction rectification technology. Firstly, nitrogen purging and water adding are carried out, a nitrogen main pipe is opened to be connected with a valve of the reaction tank, a vacuum pump is started to exchange air, the vacuum degree is l0kPa, and full nitrogen purging is carried out. The temperature of the top of the rectifying tower is 120 ℃; the temperature of the tower bottom of the rectifying tower is 165 ℃; the pressure in the rectifying tower is 20kPa, and the reflux ratio of the top of the rectifying tower is 6:1. Adding a certain amount of yellow phosphorus, weighing in a reaction kettle, slowly pumping hydrogen peroxide, adding MIL-100 (Fe) as a catalyst, wherein the added volume of the hydrogen peroxide is 20% of that of the yellow phosphorus, and the added mass of the MIL-100 (Fe) is 0.3% of that of the high-purity yellow phosphorus. The yellow phosphorus vapor is cold suspected through a tower top condenser and flows back into the tower, the yellow phosphorus liquid flowing back from the tower top and the yellow phosphorus vapor rising from the tower bottom are fully contacted in the tower to carry out gas-liquid exchange, and the electronic grade low-arsenic yellow phosphorus with the arsenic content of 2ppb is extracted from the tower top.
Example 2
As shown in figure 1, the low-arsenic yellow phosphorus is obtained by using high-purity yellow phosphorus as a raw material, MIL-53 (Al) as a catalyst and hydrogen peroxide as an oxidant through a reaction rectification technology. Firstly, nitrogen purging and water adding are carried out, a nitrogen main pipe is opened to be connected with a valve of the reaction tank, a vacuum pump is started to exchange air, the vacuum degree is l0kPa, and full nitrogen purging is carried out. The temperature of the top of the rectifying tower is 130 ℃; the temperature of the tower bottom of the rectifying tower is 170 ℃; the pressure in the rectifying tower is 40kPa, and the reflux ratio of the top of the rectifying tower is 4:1. Adding a certain amount of yellow phosphorus, weighing in a reaction kettle, slowly pumping hydrogen peroxide, and adding MIL-53 (Al), wherein the added volume of the hydrogen peroxide is 25% of that of the yellow phosphorus, and the added mass of the MIL-53 (Al) is 0.2% of that of the high-purity yellow phosphorus. The yellow phosphorus vapor is cold suspected through a tower top condenser and flows back into the tower, the yellow phosphorus liquid flowing back from the tower top and the yellow phosphorus vapor rising from the tower bottom are fully contacted in the tower to carry out gas-liquid exchange, and the electronic grade low-arsenic yellow phosphorus with the arsenic content of 3ppb is extracted from the tower top.
Example 3
As shown in FIG. 1, the low-arsenic yellow phosphorus is obtained by using high-purity yellow phosphorus as a raw material, MIL-47 (V) as a catalyst and hydrogen peroxide as an oxidant through a reaction rectification technology. Firstly, nitrogen purging and water adding are carried out, a nitrogen main pipe is opened to be connected with a valve of the reaction tank, a vacuum pump is started to exchange air, the vacuum degree is l0kPa, and full nitrogen purging is carried out. The temperature of the top of the rectifying tower is 110 ℃; the temperature of the tower bottom of the rectifying tower is 150 ℃; the pressure in the rectifying tower is 30kPa, and the reflux ratio of the top of the rectifying tower is 8:1. Adding a certain amount of yellow phosphorus, weighing in a reaction kettle, slowly pumping hydrogen peroxide, adding MIL-47 (V) catalyst, wherein the added volume of hydrogen peroxide is 10% of that of yellow phosphorus, and the added mass of MIL-47 (V) is 0.1% of that of high-purity yellow phosphorus. The yellow phosphorus vapor is cold suspected through a tower top condenser and flows back into the tower, the yellow phosphorus liquid flowing back from the tower top and the yellow phosphorus vapor rising from the tower bottom are fully contacted in the tower to carry out gas-liquid exchange, and the electronic grade low-arsenic yellow phosphorus with the arsenic content of 5ppb is extracted from the tower top.
Table 1
Comparison table of impurities of yellow phosphorus raw material before and after reaction rectification after adding catalyst
Claims (6)
1. The method for deeply removing arsenic by high-purity yellow phosphorus reaction rectification is characterized by comprising the following steps of:
i, after nitrogen purges the rectifying tower, yellow phosphorus is added into the rectifying tower, hydrogen peroxide is slowly pumped in, and then a catalyst is added;
II, after vacuumizing, starting heating and starting a circulating pump, conveying tower kettle materials from the circulating pump to a falling film evaporator, enabling liquid phase unreacted materials coming out of the lower part of the falling film evaporator and raw materials in the step (1) to further react in a reaction kettle, enabling gas phase to enter the bottom of a rectifying tower, enabling liquid at the bottom of the reaction kettle to be continuously conveyed to the falling film evaporator by the circulating pump, starting tower top condensate water circulation and tower kettle heating, starting reflux operation after the temperature of the tower kettle is raised to be stable, enabling yellow phosphorus liquid flowing back from the tower top and yellow phosphorus steam rising from the tower bottom to fully contact in the tower, performing gas-liquid exchange, and extracting high-purity yellow phosphorus.
2. The method for deep dearsenification of high purity yellow phosphorus according to claim 1, wherein the catalyst is selected from any one of MILs-100 (Fe), MILs-125 (Ti), MILs-101 (Fe), MILs-88B (Fe), MILs-53 (Al), MILs-53 (Fe), MILs-47 (V), MILs-68 (Fe).
3. The method for deep dearsenification of high purity yellow phosphorus by reactive distillation according to claim 1, wherein the added volume of hydrogen peroxide is 5% -40% of the mass of yellow phosphorus, and the mass of the catalyst is 0.01% -3% of the mass of yellow phosphorus.
4. The method for deep dearsenification of high purity yellow phosphorus by reactive distillation according to claim 3, wherein the added volume of hydrogen peroxide is 10% -30% of the mass of yellow phosphorus, and the mass of the catalyst is 0.1% -0.5% of the mass of yellow phosphorus.
5. The method for deep dearsenification of high purity yellow phosphorus by reactive distillation according to claim 1, wherein the temperature of the top of the distillation column is 100-130 ℃ in the distillation process; the temperature of the tower bottom of the rectifying tower is 150-175 ℃; the pressure in the rectifying tower is 12-25kPa, and the reflux ratio of the top of the rectifying tower is 3-6:1.
6. The method for deep dearsenification of high purity yellow phosphorus by reactive distillation according to claim 5, wherein the temperature of the top of the distillation column is 120 ℃; the temperature of the tower bottom of the rectifying tower is 165 ℃; the pressure in the rectifying tower is 20kPa, and the reflux ratio of the top of the rectifying tower is 6:1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07299301A (en) * | 1994-05-10 | 1995-11-14 | Tadashi Yazaki | Alcohol distillation method |
| CN103949225A (en) * | 2014-05-12 | 2014-07-30 | 南京大学 | Resin-based limited range self-assembly nano MOFs (Metal-Organic Frameworks) and preparation method thereof |
| CN114249307A (en) * | 2021-12-08 | 2022-03-29 | 湖北兴福电子材料有限公司 | Method for preparing electronic-grade low-arsenic yellow phosphorus by rectification |
| WO2022155762A1 (en) * | 2021-01-19 | 2022-07-28 | 万华化学(四川)有限公司 | Preparation method for lactide and reaction device |
-
2023
- 2023-07-12 CN CN202310853635.5A patent/CN116873885A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07299301A (en) * | 1994-05-10 | 1995-11-14 | Tadashi Yazaki | Alcohol distillation method |
| CN103949225A (en) * | 2014-05-12 | 2014-07-30 | 南京大学 | Resin-based limited range self-assembly nano MOFs (Metal-Organic Frameworks) and preparation method thereof |
| WO2022155762A1 (en) * | 2021-01-19 | 2022-07-28 | 万华化学(四川)有限公司 | Preparation method for lactide and reaction device |
| CN114249307A (en) * | 2021-12-08 | 2022-03-29 | 湖北兴福电子材料有限公司 | Method for preparing electronic-grade low-arsenic yellow phosphorus by rectification |
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