CN118236965A - Industrial continuous production device and method for phosphorus pentafluoride - Google Patents
Industrial continuous production device and method for phosphorus pentafluoride Download PDFInfo
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- CN118236965A CN118236965A CN202410328211.1A CN202410328211A CN118236965A CN 118236965 A CN118236965 A CN 118236965A CN 202410328211 A CN202410328211 A CN 202410328211A CN 118236965 A CN118236965 A CN 118236965A
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- phosphorus pentafluoride
- phosphorus
- hydrogen fluoride
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- OBCUTHMOOONNBS-UHFFFAOYSA-N phosphorus pentafluoride Chemical compound FP(F)(F)(F)F OBCUTHMOOONNBS-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 238000010924 continuous production Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 85
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000007788 liquid Substances 0.000 claims abstract description 77
- 238000006243 chemical reaction Methods 0.000 claims abstract description 63
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 59
- 239000000428 dust Substances 0.000 claims abstract description 44
- 239000007787 solid Substances 0.000 claims abstract description 38
- 238000003860 storage Methods 0.000 claims abstract description 35
- 238000000926 separation method Methods 0.000 claims abstract description 33
- 238000004062 sedimentation Methods 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 17
- 238000011084 recovery Methods 0.000 claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 8
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000020335 dealkylation Effects 0.000 description 1
- 238000006900 dealkylation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Abstract
The invention relates to the technical field of phosphorus pentafluoride production devices, in particular to an industrial continuous production device and method of phosphorus pentafluoride; the device comprises a phosphorus pentafluoride generating device, a liquid film dust removing device and a hydrogen fluoride recovery device, wherein the phosphorus pentafluoride generating device, the liquid film dust removing device and the hydrogen fluoride recovery device are connected in sequence; the phosphorus pentafluoride generating device comprises a phosphorus pentafluoride generator, a phosphorus pentachloride bin and a hydrogen fluoride storage tank; the phosphorus pentafluoride generator is sequentially provided with a feeding section, a suspension reaction section and a gas-solid separation sedimentation section from bottom to top. According to the invention, the phosphorus pentafluoride generator is adopted to enable phosphorus pentachloride and hydrogen fluoride gas to undergo a gas-solid reaction, and excessive hydrogen fluoride is recovered to obtain phosphorus pentafluoride, so that the continuous production of the phosphorus pentafluoride is realized; the hydrogen chloride is absorbed to obtain hydrochloric acid for self-use or sale, and the gas is recycled, and the production device and the method enable the atomic utilization rate to reach 100%, so that the production process flow is greatly simplified, the production efficiency is improved, and the method is suitable for industrial continuous production.
Description
Technical Field
The invention relates to the technical field of phosphorus pentafluoride production devices, in particular to an industrial continuous production device and method of phosphorus pentafluoride.
Background
Phosphorus pentafluoride (PF 5), a very active phosphorus-halogen compound, is severely hydrolyzed in humid air to produce toxic and corrosive hydrogen fluoride white fumes. In the field of electronic industry, phosphorus pentafluoride is an N-type doping source in the processes of silicon epitaxy, diffusion and ion implantation, so that the performance of a semiconductor can be effectively improved; in the field of polymer materials, phosphorus pentafluoride is a raw material for synthesizing polymer materials such as fluorinated organic dithiophosphate, terephthalate and the like; in the field of catalysis, phosphorus pentafluoride is a catalyst for polymerization, hydrocarbylation, dealkylation and hydrocarbon cracking reactions, and the selectivity of the reaction can be improved by using metal oxides such as titanium, nickel, beryllium and the like treated by phosphorus pentafluoride as the catalyst.
The synthesis method of phosphorus pentafluoride is mainly divided into a direct method and an indirect method, wherein phosphorus pentafluoride products with extremely high purity and selectivity can be obtained by directly reacting elemental phosphorus with fluorine gas in the direct method, but the fluorine gas serving as a raw material is expensive, the reaction is severe, and the requirement on equipment materials is high. The method widely used in industry at present is to react phosphorus pentachloride or phosphorus pentoxide with liquid hydrogen fluoride, and the method has the advantages of easily available raw materials, simple process and easy control; but the reaction period is long, the reaction is usually low-temperature reaction, the product index is unstable, the utilization rate of raw materials is low, and the continuous production is difficult to realize industrially.
Chinese patent CN114789915A discloses a continuous automatic production process for producing phosphorus pentafluoride from hydrogen fluoride gas and phosphorus pentachloride, which employs hydrogen fluoride gas to react from bottom to top through a phosphorus pentachloride powder reaction bed. The method can obviously improve the contact area and contact time of the gas phase and the solid phase, but the reaction can only be carried out after the surface reaction of the solid phosphorus pentachloride powder is finished, so that the method has longer reaction period and lower efficiency.
Disclosure of Invention
Aiming at the problems, the invention provides an industrial continuous production device and method of phosphorus pentafluoride; the production device has short reaction period and high production efficiency, and can continuously and stably produce phosphorus pentafluoride gas.
In order to solve the problems, the invention adopts the following technical scheme:
The invention provides an industrial continuous production device of phosphorus pentafluoride, which comprises a phosphorus pentafluoride generating device, a liquid film dust removing device and a hydrogen fluoride recovery device, wherein the phosphorus pentafluoride generating device, the liquid film dust removing device and the hydrogen fluoride recovery device are sequentially connected;
The phosphorus pentafluoride generating device comprises a phosphorus pentafluoride generator, a phosphorus pentachloride storage bin and a hydrogen fluoride storage tank; the phosphorus pentafluoride generator is sequentially provided with a feeding section, a suspension reaction section and a gas-solid separation sedimentation section from bottom to top, the bottom of the feeding section is provided with a hydrogen fluoride inlet, and the side surface of the feeding section is provided with a phosphorus pentachloride inlet; the bottom of the phosphorus pentachloride bin is connected to the phosphorus pentachloride inlet, and the hydrogen fluoride storage tank is connected with the hydrogen fluoride inlet;
and air valves are arranged on the pipelines of the phosphorus pentachloride bin and the phosphorus pentafluoride generator, and a gas storage tank is also connected on the pipelines of the phosphorus pentachloride bin and the phosphorus pentafluoride generator.
Further, the liquid film dust removing device comprises a liquid film dust remover, a circulating pump and a circulating liquid heat exchanger; the liquid film dust remover is connected with the top of the phosphorus pentafluoride generator, the bottom of the liquid film dust remover is sequentially connected with a circulating pump and a circulating liquid heat exchanger, and the other end of the circulating liquid heat exchanger is connected with the top of the liquid film dust remover.
Further, the hydrogen fluoride recovery device comprises a condenser and a gas-liquid separation tank; the condenser is connected with the top of the liquid film dust remover, the other end of the condenser is connected with the gas-liquid separation tank, the bottom of the gas-liquid separation tank is connected with the bottom of the liquid film dust remover, and the other end of the gas separation tank is connected with the gas compressor.
Further, the feed section, the suspension reaction section and the gas-solid separation sedimentation section have a cylinder diameter ratio of 1:3 to 6: 7-12, the height ratio is 1:3 to 15:3 to 15.
Further, the liquid film dust remover is of a cylindrical structure or a tube array structure or a tower structure.
Further, the phosphorus pentafluoride generator is also connected with a tail gas absorption tower.
The second aspect of the invention provides a method for continuously producing phosphorus pentafluoride by adopting the industrial continuous production device, which comprises the following specific steps:
Introducing hydrogen fluoride gas from the bottom of the phosphorus pentafluoride generator, starting to introduce the gas into the phosphorus pentafluoride generator, opening a wind shutoff valve at the lower part of a phosphorus pentachloride storage bin after the flow rate is stable, and taking the gas as carrier gas to carry phosphorus pentachloride into the phosphorus pentafluoride generator for reaction; and introducing the reaction product into a liquid film dust remover for dust removal, condensing by a condenser, conveying the condensed product to a gas-liquid separation tank, and conveying the separated phosphorus pentachloride gas into a gas compressor to obtain phosphorus pentafluoride.
The reaction equation is as follows:
PC15+5HF→PF5+5HCI
further, the temperature of the gas-solid reaction of phosphorus pentachloride and hydrogen fluoride is-50-300 ℃; further, the temperature is 30 to 150 ℃.
Further, the gas flow rate of the feeding section is 0.8-2 m/s, the gas flow rate of the suspension reaction section is 0.3-0.5 m/s, the reaction residence time is 15-25 s, the gas flow rate of the gas-solid separation sedimentation section is 0.05-0.1 m/s, and the reaction residence time is 90-150 s.
Further, the gas is carbon dioxide or nitrogen or argon or helium or neon.
Compared with the prior art, the invention has the following beneficial effects:
The invention adopts the phosphorus pentafluoride generator to lead phosphorus pentachloride and hydrogen fluoride gas to generate gas-solid reaction, leads the phosphorus pentachloride to completely react, recovers excessive hydrogen fluoride to obtain phosphorus pentafluoride, and realizes the continuous production of the phosphorus pentafluoride; the hydrogen chloride is absorbed to obtain hydrochloric acid for self-use or sale, and the gas is recycled, and the production device and the method enable the atomic utilization rate to reach 100%, so that the production process flow is greatly simplified, the production efficiency is improved, and the method is suitable for industrial continuous production.
Drawings
FIG. 1 shows an industrial continuous production device of phosphorus pentafluoride of the invention;
Reference numerals illustrate:
1. Phosphorus pentachloride stock bin; 2. a phosphorus pentafluoride generator; 21. a feed section; 22. a suspension reaction section; 23. a gas-solid separation sedimentation section; 3. a hydrogen fluoride storage tank; 4. a gas storage tank; 5. an air valve; 6. a liquid film dust remover; 7. a circulation pump; 8. a circulating liquid heat exchanger; 9. a condenser; 10. a gas-liquid separation tank; 11. a gas compressor; 12. and a tail gas absorption tower.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clear and clear, the present invention will be described in further detail below with reference to the accompanying drawings and examples.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "upper", "lower", "inner", "outer", "front end", "rear end", "both ends", "one end", "the other end", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or element to be referred to must have a specific direction, be configured and operated in the specific direction, and thus should not be construed as limiting the present invention. In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "provided," "connected," and the like are to be construed broadly, and may be fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
Example 1
Referring to fig. 1, an industrial continuous production device of phosphorus pentafluoride comprises a phosphorus pentafluoride generating device, a liquid film dust removing device and a hydrogen fluoride recovery device, wherein the phosphorus pentafluoride generating device, the liquid film dust removing device and the hydrogen fluoride recovery device are sequentially connected;
The phosphorus pentafluoride generating device comprises a phosphorus pentafluoride generator 2, a phosphorus pentachloride storage bin 1 and a hydrogen fluoride storage tank 3; the phosphorus pentafluoride generator 2 is sequentially provided with a feeding section 21, a suspension reaction section 22 and a gas-solid separation sedimentation section 23 from bottom to top, wherein the bottom of the feeding section 21 is provided with a hydrogen fluoride inlet, and the side surface of the feeding section is provided with a phosphorus pentachloride inlet; the bottom of the phosphorus pentachloride bin 1 is connected to the phosphorus pentachloride inlet, and the hydrogen fluoride storage tank 3 is connected with the hydrogen fluoride inlet; the hydrogen fluoride inlet is arranged below the phosphorus pentafluoride inlet, so that phosphorus pentachloride solid can be prevented from falling to the bottom of the generator 2, and smooth reaction is ensured.
The pipeline of the phosphorus pentachloride bin 1 and the phosphorus pentafluoride generator 2 is provided with an air valve 5, and the pipeline of the phosphorus pentachloride bin 1 and the phosphorus pentafluoride generator 2 is also connected with a gas storage tank 4. A phosphorus pentachloride feed inlet is arranged above the phosphorus pentachloride feed bin 1. The gas carries the feed to fluidize the phosphorus pentachloride, which is convenient for better contact and reaction with the hydrogen fluoride, and if the phosphorus pentachloride solid is not fluidized, the phosphorus pentachloride solid is easily deposited at the bottom of the reactor, so that the reaction cannot be carried out.
The phosphorus pentachloride bin 1 is of a closed structure, so that phosphorus pentachloride is prevented from being exposed to the air to be wetted, gas is replaced when necessary, a weighing module (comprising a weighing sensor) can be arranged in the phosphorus pentachloride bin 1, the phosphorus pentachloride enters a phosphorus pentachloride feeding pipeline quantitatively through a wind shut-off valve 5, the gas conveys phosphorus pentachloride to a phosphorus pentafluoride generator 2 at a certain flow rate, a fluidization state is formed, the phosphorus pentachloride reacts with hydrogen fluoride gas entering from the bottom, and reaction heat is taken away through a large amount of hydrogen fluoride gas.
The liquid film dust removing device comprises a liquid film dust remover 6, a circulating pump 7 and a circulating liquid heat exchanger 8; the liquid film dust remover 6 is connected with the top of the phosphorus pentafluoride generator 2, the bottom of the liquid film dust remover 6 is sequentially connected with a circulating pump 7 and a circulating liquid heat exchanger 8, and the other end of the circulating liquid heat exchanger 8 is connected with the top of the liquid film dust remover 6; when a very small amount of phosphorus pentachloride particles with very small particle size are taken out of the phosphorus pentachloride generator 2 by a gas clamp, the phosphorus pentachloride generator 2 needs to be purified and dedusted, the liquid film deduster 6 enables liquid hydrogen fluoride to be fully contacted with phosphorus pentachloride, and the very small amount of phosphorus pentachloride with small particle size is captured, so that the phosphorus pentachloride gas is ensured not to contain phosphorus pentachloride; the circulating pump 7 and the circulating liquid heat exchanger 8 provide liquid hydrogen fluoride for the liquid film dust remover 6.
The hydrogen fluoride recovery device comprises a condenser 9 and a gas-liquid separation tank 10; the condenser 9 is connected with the top of the liquid film dust remover 6, the other end of the condenser 9 is connected with the gas-liquid separation tank 10, the bottom of the gas-liquid separation tank 10 is connected with the bottom of the liquid film dust remover 6, and the other end of the gas separation tank is connected with the gas compressor 11. The boiling point of the hydrogen fluoride is 19.5 ℃, the hydrogen fluoride can be cooled into liquid hydrogen fluoride through the condenser 9 which is filled with a refrigerant, and when one condenser 9 is insufficient to fully condense the hydrogen fluoride gas, a plurality of serial connection forms can be adopted; the gas-liquid separation tank 10 separates liquid hydrogen fluoride, the liquid hydrogen fluoride is pumped into the circulating liquid heat exchanger 8 through the circulating pump 7 to be cooled and then enters the top of the liquid film dust remover 6 to be sprayed, the sprayed hydrogen fluoride is partially vaporized, the unvaporized part flows into the bottom of the liquid film dust remover 6, and the unvaporized part is pumped into the circulating liquid heat exchanger 8 through the circulating pump 7 to be cooled and then enters the top of the liquid film dust remover 6 to be sprayed, so that circulation is formed. The liquid hydrogen fluoride can be conveyed to the liquid film dust remover 6 for recycling, and can also be conveyed to a liquid hydrogen fluoride storage tank (not shown) for standby.
Further, the ratio of the cylinder diameters of the feeding section 21, the suspension reaction section 22 and the gas-solid separation sedimentation section 23 is 1:3 to 6: 7-12, the height ratio is 1:3 to 15:3 to 15. The smaller cylinder diameter of the feeding section 21 is because the gas speed of the section needs to be ensured when the solid is fed, so that the solid is fluidized, and sedimentation is avoided; the cylinder diameter of the suspension reaction section 22 is increased by expanding the diameter and reducing the gas speed, so that the residence time of reactants is increased, and gas-solid two phases are fully contacted and reacted; the cylinder diameter of the gas-solid separation sedimentation section 23 is enlarged again, so that the gas speed is further reduced, a small number of unreacted solid phosphorus pentachloride is settled down until the suspension reaction section 22 is further reacted with hydrogen fluoride, and the reaction of the solid phosphorus pentachloride is ensured to be complete.
The liquid film dust remover 6 is of a cylindrical structure, a tubular structure or a tower structure.
The phosphorus pentafluoride generator 2 is also connected with a tail gas absorption tower 12; the exhaust gas enters the exhaust gas absorption tower 12 for innocent treatment.
The gas is carbon dioxide or nitrogen or argon or helium or neon, and the gas is not reacted with the materials used in the invention, and is not repeated herein.
The specific working process (phosphorus pentachloride continuous production method) of the phosphorus pentachloride continuous production device is as follows:
Firstly, introducing hydrogen fluoride gas from the bottom of a phosphorus pentafluoride generator 2, starting to introduce the gas into the phosphorus pentafluoride generator 2, opening a wind shutoff valve 5 at the lower part of a phosphorus pentachloride storage bin 1 after the flow rate is stable, and taking the gas as carrier gas to carry phosphorus pentachloride into the phosphorus pentafluoride generator 2 for reaction; the reaction product is introduced into a liquid film dust remover 6 for dust removal, condensed by a condenser 9 and then conveyed to a gas-liquid separation tank 10, and the separated phosphorus pentafluoride is conveyed into a gas compressor 11 to obtain phosphorus pentafluoride; wherein the hydrochloric acid is obtained by absorption treatment and is used for self-use or sale, and the gas is recycled.
The phosphorus pentachloride can be first grade phosphorus pentachloride which is sold in the market and meets the rule, and the particle size is smaller than 250um.
The temperature of the gas-solid reaction of phosphorus pentachloride and hydrogen fluoride is-50-300 ℃; further, the temperature is 30 to 150 ℃.
The gas flow rate of the feeding section 21 is 0.8-2 m/s, the gas flow rate of the suspension reaction section 22 is 0.3-0.5 m/s, the reaction residence time is 15-25 s, the gas flow rate of the gas-solid separation sedimentation section 23 is 0.05-0.1 m/s, and the reaction residence time is 90-150 s.
Example 2
Firstly, phosphorus pentachloride solid with the quality requirement reaching the quality index of first class product of phosphorus pentachloride for HG/T4108-2009 industry is hermetically and continuously conveyed into a phosphorus pentachloride storage bin 1, the storage bin volume is 0.5m 3, and when the conveyed solid reaches 200kg, the conveying speed is adjusted to be 18kg/h;
Then, introducing hydrogen fluoride gas from the bottom of the phosphorus pentafluoride generator 2, wherein the air inlet pressure is 0.2MPa, the volume flow is 30Nm 3/h, and the temperature is 40 ℃; simultaneously, the phosphorus pentafluoride generator 2 starts to be filled with nitrogen at normal temperature, the air inlet pressure is 1MPa, the volume flow is 80Nm 3/h, the flow speed is 5m/s, after the flow speed is stable, the air valve 5 at the lower part of the phosphorus pentachloride storage bin 1 is opened, the phosphorus pentafluoride conveying speed is controlled to be 18kg/h, the constant weight of the storage bin is ensured, and nitrogen is taken as carrier gas to carry phosphorus pentachloride to enter the phosphorus pentafluoride generator 2 for reaction; the flow rate of the gas in the feeding section 21 of the phosphorus pentafluoride generator 2 is controlled at 1.2m/s, the flow rate of the gas in the suspension reaction section 22 is controlled at 0.4m/s, the reaction residence time is 18s, the flow rate of the gas in the gas-solid separation sedimentation section 23 is 0.06m/s, the reaction residence time is 100s, and the reaction temperature is 130 ℃ to obtain 10.88kg/h of continuous and stable phosphorus pentafluoride gas.
Example 3
Firstly, phosphorus pentachloride solid with the quality requirement reaching the quality index of first class product of phosphorus pentachloride for HG/T4108-2009 industry is hermetically and continuously conveyed into a phosphorus pentachloride storage bin 1, the storage bin volume is 0.5m 3, and when the conveyed solid reaches 200kg, the conveying speed is adjusted to be 18kg/h;
Then, introducing hydrogen fluoride gas from the bottom of the phosphorus pentafluoride generator 2, wherein the air inlet pressure is 0.2MPa, the volume flow is 30Nm 3/h, and the temperature is 40 ℃; simultaneously, the phosphorus pentafluoride generator 2 starts to be filled with nitrogen at normal temperature, the air inlet pressure is 1MPa, the volume flow is 80Nm 3/h, the flow speed is 5m/s, after the flow speed is stable, the air valve 5 at the lower part of the phosphorus pentachloride storage bin 1 is opened, the phosphorus pentafluoride conveying speed is controlled to be 18kg/h, the constant weight of the storage bin is ensured, and nitrogen is taken as carrier gas to carry phosphorus pentachloride to enter the phosphorus pentafluoride generator 2 for reaction; the gas flow rate of the feeding section 21 of the phosphorus pentafluoride generator 2 is controlled at 1.6m/s, the gas flow rate of the suspension reaction section 22 is controlled at 0.3m/s, the reaction residence time is 25s, the gas flow rate of the gas-solid separation sedimentation section 23 is 0.08m/s, the reaction residence time is 120s, and the reaction temperature is 30 ℃ to obtain 11.42kg/h of continuous and stable phosphorus pentafluoride gas.
Example 4
Firstly, phosphorus pentachloride solid with the quality requirement reaching the quality index of first class product of phosphorus pentachloride for HG/T4108-2009 industry is hermetically and continuously conveyed into a phosphorus pentachloride storage bin 1, the storage bin volume is 0.5m 3, and when the conveyed solid reaches 200kg, the conveying speed is adjusted to be 18kg/h;
Then, introducing hydrogen fluoride gas from the bottom of the phosphorus pentafluoride generator 2, wherein the air inlet pressure is 0.2MPa, the volume flow is 30Nm 3/h, and the temperature is 40 ℃; simultaneously, the phosphorus pentafluoride generator 2 starts to be filled with nitrogen at normal temperature, the air inlet pressure is 1MPa, the volume flow is 80Nm 3/h, the flow speed is 5m/s, after the flow speed is stable, the air valve 5 at the lower part of the phosphorus pentachloride storage bin 1 is opened, the phosphorus pentafluoride conveying speed is controlled to be 18kg/h, the constant weight of the storage bin is ensured, and helium is taken as carrier gas to carry phosphorus pentachloride to enter the phosphorus pentafluoride generator 2 for reaction; the flow rate of the gas in the feeding section 21 of the phosphorus pentafluoride generator 2 is controlled at 2m/s, the flow rate of the gas in the suspension reaction section 22 is controlled at 0.5m/s, the reaction residence time is 15s, the flow rate of the gas in the gas-solid separation sedimentation section 23 is 0.1m/s, the reaction residence time is 150s, the reaction temperature is-50 ℃, and 11.05kg/h of continuous and stable phosphorus pentafluoride gas is obtained.
Example 5
Firstly, phosphorus pentachloride solid with the quality requirement reaching the quality index of first class product of phosphorus pentachloride for HG/T4108-2009 industry is hermetically and continuously conveyed into a phosphorus pentachloride storage bin 1, the storage bin volume is 0.5m 3, and when the conveyed solid reaches 200kg, the conveying speed is adjusted to be 18kg/h;
Then, introducing hydrogen fluoride gas from the bottom of the phosphorus pentafluoride generator 2, wherein the air inlet pressure is 0.2MPa, the volume flow is 30Nm 3/h, and the temperature is 40 ℃; simultaneously, the phosphorus pentafluoride generator 2 starts to be filled with nitrogen at normal temperature, the air inlet pressure is 1MPa, the volume flow is 80Nm 3/h, the flow speed is 5m/s, after the flow speed is stable, the air valve 5 at the lower part of the phosphorus pentachloride storage bin 1 is opened, the phosphorus pentafluoride conveying speed is controlled to be 18kg/h, the constant weight of the storage bin is ensured, and carbon dioxide is taken as carrier gas to carry phosphorus pentachloride to enter the phosphorus pentafluoride generator 2 for reaction; the flow rate of the gas in the feeding section 21 of the phosphorus pentafluoride generator 2 is controlled at 0.8m/s, the flow rate of the gas in the suspension reaction section 22 is controlled at 0.5m/s, the reaction residence time is 22s, the flow rate of the gas in the gas-solid separation sedimentation section 23 is 0.05m/s, the reaction residence time is 90s, and the reaction temperature is 300 ℃ to obtain 10.96kg/h of continuous and stable phosphorus pentafluoride gas.
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.
Claims (10)
1. The industrial continuous production device of phosphorus pentafluoride comprises a phosphorus pentafluoride generating device, a liquid film dust removing device and a hydrogen fluoride recovery device, and is characterized in that the phosphorus pentafluoride generating device, the liquid film dust removing device and the hydrogen fluoride recovery device are connected in sequence;
The phosphorus pentafluoride generating device comprises a phosphorus pentafluoride generator (2), a phosphorus pentachloride storage bin (1) and a hydrogen fluoride storage tank (3); the phosphorus pentafluoride generator (2) is sequentially provided with a feeding section (21), a suspension reaction section (22) and a gas-solid separation sedimentation section (23) from bottom to top, the bottom of the feeding section (21) is provided with a hydrogen fluoride inlet, and the side surface of the feeding section is provided with a phosphorus pentachloride inlet; the bottom of the phosphorus pentachloride bin (1) is connected to the phosphorus pentachloride inlet, and the hydrogen fluoride storage tank (3) is connected with the hydrogen fluoride inlet;
The pipeline of the phosphorus pentachloride bin (1) and the phosphorus pentafluoride generator (2) is provided with an air valve (5), and the pipeline of the phosphorus pentachloride bin (1) and the phosphorus pentafluoride generator (2) is also connected with a gas storage tank (4).
2. The industrial continuous production device of phosphorus pentafluoride according to claim 1, characterized in that the liquid film dust removing device comprises a liquid film dust remover (6), a circulating pump (7) and a circulating liquid heat exchanger (8); the liquid film dust remover (6) with phosphorus pentafluoride generator (2) top links to each other, circulating pump (7) and circulating liquid heat exchanger (8) have been connect gradually to liquid film dust remover (6) bottom, circulating liquid heat exchanger (8) other end with liquid film dust remover (6) top is connected.
3. The industrial continuous production device of phosphorus pentafluoride according to claim 1, characterized in that the hydrogen fluoride recovery device comprises a condenser (9), a gas-liquid separation tank (10); the condenser (9) is connected with the top of the liquid film dust remover (6), the other end of the condenser (9) is connected with the gas-liquid separation tank (10), the bottom of the gas-liquid separation tank (10) is connected with the bottom of the liquid film dust remover (6), and the other end of the gas separation tank (10) is connected with the gas compressor (11).
4. The industrial continuous production device of phosphorus pentafluoride according to claim 1, characterized in that the ratio of the cylinder diameters of the feeding section (21), the suspension reaction section (22) and the gas-solid separation sedimentation section (23) is 1:3 to 6: 7-12, the height ratio is 1:3 to 15:3 to 15.
5. The industrial continuous production device of phosphorus pentafluoride according to claim 1, characterized in that the liquid film dust remover (6) is of a cylindrical structure or a tubular structure or a tower structure.
6. The industrial continuous production device of phosphorus pentafluoride according to claim 1, characterized in that the phosphorus pentafluoride generator (2) is also connected with a tail gas absorption tower (12).
7. An industrial continuous production method of phosphorus pentafluoride, which is characterized by adopting the industrial continuous production device of phosphorus pentachloride according to any one of claims 1 to 6, and comprising the following specific steps:
introducing hydrogen fluoride gas from the bottom of the phosphorus pentafluoride generator (2), starting to introduce the gas into the phosphorus pentafluoride generator (2), opening an air valve (5) at the lower part of the phosphorus pentachloride storage bin (1) after the flow rate is stable, and carrying phosphorus pentachloride into the phosphorus pentafluoride generator (2) by taking the gas as carrier gas for reaction; the reaction product is introduced into a liquid film dust remover (6) for dust removal, condensed by a condenser (9) and then conveyed to a gas-liquid separation tank (10), and the separated phosphorus pentafluoride is conveyed to a gas compressor (11) to obtain the phosphorus pentafluoride.
8. The industrial continuous production method of phosphorus pentafluoride according to claim 7, wherein the temperature at which the phosphorus pentachloride and hydrogen fluoride undergo gas-solid reaction is-50-300 ℃.
9. The industrial continuous production method of phosphorus pentafluoride according to claim 7, characterized in that the gas flow rate of the feeding section (21) is 0.8-2 m/s, the gas flow rate of the suspension reaction section (22) is 0.3-0.5 m/s, the reaction residence time is 15-25 s, the gas flow rate of the gas-solid separation sedimentation section (23) is 0.05-0.1 m/s, and the reaction residence time is 90-150 s.
10. The industrial continuous production method of phosphorus pentafluoride according to claim 7, characterized in that the gas is carbon dioxide or nitrogen or argon or helium or neon.
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| Publication Number | Publication Date |
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| CN118236965A true CN118236965A (en) | 2024-06-25 |
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