CN114789915A - Continuous automatic production method of phosphorus pentafluoride - Google Patents
Continuous automatic production method of phosphorus pentafluoride Download PDFInfo
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- CN114789915A CN114789915A CN202210373323.XA CN202210373323A CN114789915A CN 114789915 A CN114789915 A CN 114789915A CN 202210373323 A CN202210373323 A CN 202210373323A CN 114789915 A CN114789915 A CN 114789915A
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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 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000005303 weighing Methods 0.000 claims abstract description 55
- 239000011261 inert gas Substances 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000007789 gas Substances 0.000 claims abstract description 31
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 8
- 239000002912 waste gas Substances 0.000 claims description 5
- 230000006872 improvement Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 239000010808 liquid waste Substances 0.000 description 6
- RLOWWWKZYUNIDI-UHFFFAOYSA-N phosphinic chloride Chemical compound ClP=O RLOWWWKZYUNIDI-UHFFFAOYSA-N 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 230000000007 visual effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- -1 lithium hexafluorophosphate Chemical compound 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65G—TRANSPORT OR STORAGE DEVICES, e.g. CONVEYORS FOR LOADING OR TIPPING, SHOP CONVEYOR SYSTEMS OR PNEUMATIC TUBE CONVEYORS
- B65G65/00—Loading or unloading
- B65G65/30—Methods or devices for filling or emptying bunkers, hoppers, tanks, or like containers, of interest apart from their use in particular chemical or physical processes or their application in particular machines, e.g. not covered by a single other subclass
- B65G65/34—Emptying devices
- B65G65/40—Devices for emptying otherwise than from the top
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D88/00—Large containers
- B65D88/54—Large containers characterised by means facilitating filling or emptying
- B65D88/64—Large containers characterised by means facilitating filling or emptying preventing bridge formation
- B65D88/70—Large containers characterised by means facilitating filling or emptying preventing bridge formation using fluid jets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65G—TRANSPORT OR STORAGE DEVICES, e.g. CONVEYORS FOR LOADING OR TIPPING, SHOP CONVEYOR SYSTEMS OR PNEUMATIC TUBE CONVEYORS
- B65G15/00—Conveyors having endless load-conveying surfaces, i.e. belts and like continuous members, to which tractive effort is transmitted by means other than endless driving elements of similar configuration
- B65G15/30—Belts or like endless load-carriers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65G—TRANSPORT OR STORAGE DEVICES, e.g. CONVEYORS FOR LOADING OR TIPPING, SHOP CONVEYOR SYSTEMS OR PNEUMATIC TUBE CONVEYORS
- B65G43/00—Control devices, e.g. for safety, warning or fault-correcting
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
Abstract
The invention provides a continuous automatic production method of phosphorus pentafluoride, which comprises the following steps: opening a second pipeline to fill inert gas into a part of the weighing and conveying bins, opening corresponding exhaust ports to remove residual air and moisture in the part of the weighing and conveying bins, and closing the second pipeline and the exhaust ports; opening feeding valves and weighing and conveying units corresponding to part of weighing and conveying bins to weigh and feed the phosphorus pentachloride, and simultaneously opening a hydrogen fluoride supply tank to feed anhydrous HF to the corresponding part of reactors and perform reaction; before the reaction of part of reactors is finished, simultaneously opening a second pipeline to fill inert gas into the rest of the weighing and conveying bins, opening corresponding exhaust ports to remove residual air and water gas in the rest of the weighing and conveying bins for standby, and closing the second pipeline and the exhaust ports; and opening the feeding valves corresponding to the rest weighing and conveying bins and the weighing and conveying units to weigh and feed the phosphorus pentachloride, and simultaneously opening the hydrogen fluoride supply tank to feed anhydrous HF to the rest reactor and perform reaction.
Description
Technical Field
The invention relates to a continuous and automatic production method of phosphorus pentafluoride.
Background
Phosphorus pentafluoride (chemical formula: PF) 5 ) Is an important inorganic compound and can be used for electronic industry, high molecular materials and organic synthesis catalysts. In the new century, high-performance lithium ion batteries increasingly become an important field for development of new energy industry, lithium hexafluorophosphate serving as a key raw material for producing lithium ion batteries has higher and higher quality requirements, and how to produce high-quality phosphorus pentafluoride with high efficiency has very important significance for synthesis of lithium hexafluorophosphate. At present, one of the methods for industrially producing phosphorus pentafluoride is to generate phosphorus pentafluoride by reacting phosphorus pentachloride with hydrogen fluoride gas. Phosphorus pentachloride is light yellow crystalline powder at normal temperature and normal pressure, has a melting point of 179-181 ℃, has pungent smell, is easy to sublimate, has strong irritation to skin, eyes and mucous membranes, is a compound with great activity, and can react violently with moisture in the air to generate toxic and corrosive hydrogen chloride smoke.
PCl 5 +H 2 O→POCl 3 +2HCl PCl 5 +4H 2 O→H 3 PO 4 +5HCl
The phosphorus pentachloride in the traditional phosphorus pentafluoride preparation process is manually fed, the labor intensity is high, the total consumption of the phosphorus pentachloride in the total flow is large, the consumption of single reaction equipment is low, multiple times of feeding and reaction are required by a plurality of generating devices, the efficiency is influenced, and more importantly, toxic and corrosive gases are generated in the feeding process, so that the problems of health of production personnel, the service life of production equipment and environmental pollution are directly influenced.
Disclosure of Invention
The invention provides a continuous automatic production method of phosphorus pentafluoride, which can effectively solve the problems.
The invention is realized by the following steps:
the invention provides a continuous automatic production method of phosphorus pentafluoride, which comprises the following steps:
s12, opening the second pipeline to fill inert gas into a part of the weighing and conveying bins, opening corresponding exhaust ports to remove residual air and moisture in the part of the weighing and conveying bins, and closing the second pipeline and the exhaust ports;
s13, opening the feed valves corresponding to part of the weighing and conveying bins and the weighing and conveying units to weigh and feed the phosphorus pentachloride, and simultaneously opening the hydrogen fluoride supply tank to feed anhydrous HF to the corresponding part of the reactors for reaction; before the reaction of the partial reactor is finished, simultaneously opening the second pipeline to fill inert gas into the rest of the weighing and conveying bins, opening corresponding exhaust ports to remove residual air and moisture in the rest of the weighing and conveying bins for standby, and closing the second pipeline and the exhaust ports;
s14, opening the feed valves corresponding to the rest of the weighing and conveying bins and the weighing and conveying units to weigh and feed the phosphorus pentachloride, and simultaneously opening the hydrogen fluoride supply tank to feed anhydrous HF into the rest of the reactor and perform reaction; and in the reaction process of the rest reactors, opening the second pipeline to fill inert gas into the partial reactors and opening a waste gas discharge port so as to remove residual gas in the partial reactors for later use, and repeating the above steps to continuously and automatically produce the phosphorus pentafluoride.
The beneficial effects of the invention are: the continuous and automatic production method of phosphorus pentafluoride provided by the invention comprises the step of filling inert gas into the charging barrel and each weighing and conveying bin through the second pipeline respectively, so that residual air and moisture in the charging barrel and each weighing and conveying bin are removed, and further, the phosphorus pentafluoride can be continuously and automatically producedPrevention can significantly reduce POCl in the product 3 、H 3 PO 4 And the content of water vapor. POCl in the product 3 、H 3 PO 4 And the content of the water vapor is reduced to be below 0.01 vt% from the original 1-3 vt%, and the purity of the product is improved. In addition, the continuous and automatic production method of the phosphorus pentafluoride can be used for automatically feeding a plurality of reactors at the same time, and a plurality of generating devices can be used for feeding and reacting for a plurality of times, so that the efficiency is obviously improved, and the influence on human bodies is reduced. In addition, through the accurate control to pay-off each time to weighing that can be accurate improves reaction efficiency.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic structural diagram of a continuous automatic production apparatus for phosphorus pentafluoride provided by an embodiment of the present invention.
FIG. 2 is a schematic structural diagram of an automatic phosphorus pentachloride weighing and feeding device provided in an embodiment of the present invention.
FIG. 3 is a flow chart of a continuous automatic production method of phosphorus pentafluoride according to an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to imply that the number of technical features indicated is significant. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1 to 2, an embodiment of the present invention provides a continuous and automatic phosphorus pentafluoride production apparatus, including:
phosphorus pentachloride automatic weighing feeding equipment comprises:
the phosphorus pentachloride bunker 10 comprises a charging barrel 101, a feeding hole 102 and a first air outlet 103 which are arranged at the top of the charging barrel 101, a multi-grid conveying pipe 104 arranged at the bottom of the charging barrel 101, a feeding valve 105 arranged at each conveying port of the multi-grid conveying pipe 104, and a first air inlet 106;
a plurality of weighing and conveying units 11, wherein each weighing and conveying unit 11 comprises a weighing and conveying bin 111 correspondingly arranged at the bottom of each feed valve 105 and communicated with the grid conveying pipe 104, a weighing unit 113 arranged in the weighing and conveying bin 111, a conveying unit 112 arranged on the weighing unit 113, a transfer pot 115 arranged at the conveying terminal of the conveying unit 112, and a second air inlet 117;
a high pressure inert gas unit 12 including an inert gas tank 121, a first pipe 123 disposed between the inert gas tank 121 and the first gas inlet 106, and a second pipe 125 disposed between the inert gas tank 121 and the second gas inlet 117;
a hydrogen fluoride supply tank 14;
a plurality of reactors 13, each disposed at the bottom of each of the transfer tanks 115, and communicating with the hydrogen fluoride supply tank 14 through a pipe.
The phosphorus pentachloride silo 10 is used for storing a phosphorus pentachloride raw material. The interior of the phosphorus pentachloride bin 10 can be passivated so as to prevent the phosphorus pentachloride from reacting with the phosphorus pentachloride raw material. In one embodiment, the phosphorus pentachloride silo 10 is a stainless steel silo that has been passivated with fluorine gas. The introduction of the inert gas through the first gas inlet 106 may be used to drive off air, moisture, etc. remaining in the cartridge 101. Further, the first air inlet 106 may be disposed at the grid feed delivery conduit 104. When the grid feed pipe 104 is clogged, the introduction of high-pressure inert gas through the first gas inlet 106 can be used to unblock the clogging of the grid feed pipe 104. The total phosphorus pentachloride consumption in the total process of the phosphorus pentafluoride preparation process is large, and the consumption of single reaction equipment is low, so that a plurality of reactors are required for carrying out multiple feeding and reaction. Thus, a plurality of reactors 13 can be fed simultaneously through the multi-grid feed conveyor 104. The multi-grid conveying pipe 104 is provided with a plurality of grid-shaped conveying pipes, and a conveying opening of each grid-shaped conveying pipe is correspondingly provided with a feeding valve 105, so that conveying control is performed on each conveying pipe. The number of the multi-grid conveying pipes 104 is not limited, and can be 2-20. In one embodiment, the multi-grid conveyor 104 has 6 conveyors, corresponding to 6 weigh conveyor units 11 and 6 reactors 13, respectively.
In other embodiments, the bottom of the cartridge 101 is further provided with an observation window 107 for determining the remaining material condition of the cartridge 101. As a further improvement, in other embodiments, a visual sensor may be further disposed outside the viewing window 107 for detecting the height of the material in the cartridge 101, so as to further realize full-automatic control. The visual sensor is mainly used for judging whether the material in the charging barrel 101 is lower than a set value or not so as to remind of further charging and the like.
The weighing conveyor units 11 may be arranged side by side or in a matrix, and will not be described again here. The weighing unit 113 is used for weighing the conveying unit 112 and the input materials. The conveying unit 112 may be a conveyor belt or the like. Inert materials such as Teflon are coated on the conveying belt, so that the conveying belt is prevented from being corroded by phosphorus pentachloride. The interior of the transfer pot 115 may also be passivated to prevent reaction with the phosphorus pentachloride feedstock. The top of the weigh bin 111 is further provided with an exhaust port 114 for exhausting residual air and moisture when the second pipe 125 is filled with inert gas. Further, the second air inlet 117 may be disposed on the bottom of the relay tank 115. In one embodiment, the second gas inlet 117 is arranged to communicate with the bottom of the transfer tank 115, so that when the bottom of the transfer tank 115 is blocked, the introduction of the high-pressure inert gas through the second gas inlet 117 can be used to unblock the bottom of the transfer tank 115.
In other embodiments, as a further improvement, the transfer tank 115 may further be provided with a viewing window 118 for judging the residual material condition of the transfer tank 115. As a further improvement, in other embodiments, a visual sensor may be further disposed outside the observation window 107 for detecting the material level of the transfer pot 115, so as to further realize fully automatic control. The vision sensor is primarily used to determine whether there is a reduction in material in the transfer pot 115, thereby determining whether there is a blockage.
The high pressure inert gas unit 12 may further include an inflation tube 127 and a valve 126 disposed on the inflation tube 127 for supplying inert gas when the high pressure inert gas unit 12 is exhausted. The high pressure inert gas unit 12 may further include a first valve 122 disposed on the first pipe 123 and a second valve 124 disposed on the second pipe 125. In one embodiment, the inert gas is selected from nitrogen. The pressure of the high-pressure inert gas unit 12 may be 0.2 to 2 MPa. Preferably, the pressure of the high pressure inert gas unit 12 may be 0.5 to 1 MPa. In one embodiment, the high pressure inert gas unit 12 has a pressure of about 0.6MPa, so as to dredge the blockage.
The hydrogen fluoride supply tank 14 is used to supply a high-purity hydrogen fluoride gas.
The reactor 13 is configured to react the hydrogen fluoride gas provided by the hydrogen fluoride supply tank 14 with the phosphorus pentachloride provided by the phosphorus pentachloride automatic weighing and feeding device to prepare a phosphorus pentafluoride gas, and store the phosphorus pentafluoride gas in the storage tank 15. The reactor 13 comprises a reaction chamber 131, a cooling jacket 134 arranged outside the reaction chamber 131, a stirring device 135 arranged in the middle of the reaction chamber 131, a tail gas discharge port 131 and a product discharge port 132 arranged at the top of the reaction chamber 131, and a hydrogen fluoride gas buffer chamber 136 arranged at the bottom of the reaction chamber 131; and a solid-liquid discharge port 137 provided at the bottom of the reaction chamber 131. The gas of the product discharge port 132 is filled in the holding tank 15. The hydrogen fluoride gas enters the hydrogen fluoride gas buffer chamber 136 from the bottom gas inlet, then enters the reaction chamber 131 through the meshes uniformly through the porous surface structure, and passes through the phosphorus pentachloride powder reaction bed from bottom to top, so that the contact area and the contact time of a gas-solid phase are remarkably improved, the reaction is more complete, and the conversion rate of anhydrous hydrogen fluoride is obviously improved. In addition, the hydrogen fluoride is introduced into the reaction chamber 131 from the bottom of the reaction chamber 131 and fully contacts with the phosphorus pentachloride, so that the problem of low utilization rate of the hydrogen fluoride caused by the fact that anhydrous hydrogen fluoride in the prior art is easy to gasify and the generated phosphorus pentafluoride and hydrogen chloride gas are easy to discharge out of the reactor is solved. The specific structure of said reactor 13 can be found in the patent of the invention in the chinese application No. 201922288722.2, entitled "a reactor for phosphorus pentafluoride", and will not be described again here.
Referring to fig. 3, an embodiment of the present invention further provides a continuous and automatic method for producing phosphorus pentafluoride, including the following steps:
s12, opening the second pipeline 125 to fill inert gas into a part of the weigh conveying bin 111, opening the corresponding exhaust port 114 to remove air and moisture remaining in the part of the weigh conveying bin 111, and closing the second pipeline 125 and the exhaust port 114;
s13, opening the feeding valve 105 corresponding to the partial weighing and conveying bin 111 and the weighing and conveying unit 11 to weigh and feed the phosphorus pentachloride, and simultaneously opening the hydrogen fluoride supply tank 14 to feed anhydrous HF to the corresponding partial reactor 13 for reaction; before the reaction of the partial reactor 13 is finished, simultaneously opening the second pipeline 125 to fill inert gas into the rest of the weighing and conveying bins 111, opening the corresponding exhaust port 114 to remove residual air and water vapor in the rest of the weighing and conveying bins 111 for standby, and closing the second pipeline 125 and the exhaust port 114;
s14, opening the feeding valves 105 corresponding to the rest of weighing and conveying bins 111 and the weighing and conveying units 11 to weigh and feed the phosphorus pentachloride, and simultaneously opening the hydrogen fluoride supply tank 14 to feed anhydrous HF to the rest of the reactors 13 for reaction; and in the reaction process of the rest of the reactors 13, opening the second pipeline 125 to fill inert gas into the partial reactors 13 and opening the waste gas discharge port 133 to remove residual gas in the partial reactors 13 for later use, and repeating the above circulation to continuously and automatically produce the phosphorus pentafluoride.
Before step S12, the method may further include:
s10, opening the first pipe 123 to fill the inert gas into the barrel 101, and opening the first air outlet 103 to remove air and moisture remaining in the barrel 101;
and S11, after the first pipeline 123 and the first air outlet 103 are closed, feeding materials through the feeding hole 102, and closing the feeding hole 102 after the feeding is finished.
In step S10, it is preferable that whether the air and moisture remaining in the barrel 101 are removed can be judged by detecting the content of the inert gas in the first air outlet 103. More preferably, when the content of the inert gas in the first air outlet 103 is higher than 99 vt%, it can be basically judged that the air and moisture remaining in the barrel 101 are removed.
In step S11, since the barrel 101 forms a closed cavity, the height of the fed material should not be too high, and preferably, the height of the fed material is 8 to 9 of the height of the barrel 101, so as to prevent a large negative pressure from being formed in the subsequent blanking process and affecting the blanking.
In step S12, the number of the partial weigh hoppers 111 is not limited, and may be half or more of the number of all the weigh hoppers 111. In one of the exemplary embodiments, half of the 6 weighing conveyor units 11, i.e. 3 weighing conveyor units 11, are opened.
As a further improvement, whether the air and moisture remaining in the weigh bin 111 are removed can be judged by detecting the content of the inert gas in the exhaust port 114. More preferably, when the content of the inert gas in the exhaust port 114 is higher than 99 vt%, it can be basically judged that the air and moisture remaining in the weigh bin 111 have been removed.
As a further modification, the second pipe 125 may be further opened to fill the inert gas into the reactor 13, and the offgas discharge port 131 may be opened to remove air and moisture remaining in the reactor 13. Of course, it is also possible to judge whether the air and moisture remaining in the reactor 13 are removed completely by detecting the content of the inert gas in the offgas discharge port 131.
In step S13, before the partial reactor 13 finishes the reaction, the second pipe 125 is opened to fill the remaining weigh transport bins 111 with inert gas, and the corresponding exhaust ports 114 are opened to remove the air and water remaining in the remaining weigh transport bins 111 for use. The time before the partial reactor 13 is finished can be controlled to be about 5 to 30 minutes, because the air in the weighing and conveying bin 111 and the reactor 13 can be removed by about 5 to 30 minutes for general industrial production. Preferably, the time can be controlled to be 15 to 20 minutes before the reaction is finished.
In order to realize accurate feeding of the phosphorus pentachloride raw material, preferably, each time of feeding, the conveying unit 112 is controlled to run at a constant speed at a first speed for less than half a cycle to receive the material, that is, the running is less than half a cycle; after the material bearing is finished, the conveying unit 112 is controlled to run at a second speed at a constant speed less than half a cycle to dump the material. Preferably, each time the material is fed, the conveying unit 112 is controlled to run at a constant speed of 1/3 weeks to receive the material; after the material bearing is finished, the conveying unit 112 is controlled to run at a constant speed for 1/2 weeks to pour the materials, so that the materials can be guaranteed to be poured cleanly. As a further improvement, after 1/3 weeks of operation, the weighing unit 113 is used to weigh the materials in the conveying unit 112 to reach a set value, if yes, the feed valve 105 is controlled to close, and then the conveying unit 112 is controlled to operate at a constant speed for 1/2 weeks to pour the materials; otherwise, the feeding valve 105 is controlled to be continuously opened for feeding until the set value is reached, and then the conveying unit 112 is controlled to run at a constant speed for 1/2 weeks for pouring the materials.
The phosphorus pentachloride and the anhydrous HF are generally fed and mixed in a mass ratio of about 1:2. However, since anhydrous HF is volatilized to cause a certain loss, it is preferable that the phosphorus pentachloride and the anhydrous HF are fed and mixed in a mass ratio of about 1:2.1 to about 2.4. In one embodiment, the phosphorus pentachloride and the anhydrous HF are generally fed mixed in a molar ratio of about 1: 2.1.
As a further improvement, when the metering of the weighing unit 113 is not increased or is increased slowly during the uniform operation of the conveying unit 112 at the first speed, the feed valve 105 is blocked, and then, the method may further include:
s131, introducing high-pressure inert gas through the first gas inlet 106 to dredge the blockage of the discharge hole 104. In the dredging process, whether dredging is performed or not can be further judged through the metering change of the weighing unit 113, otherwise, high-pressure inert gas is continuously introduced or an alarm is given, and manual dredging is performed.
As a further improvement, when the feeding valve 105 is controlled to be continuously opened for feeding, and the metering of the weighing unit 113 is obviously not increased or slowly increased, the feeding valve 105 is indicated to be blocked, and then, the method may further comprise the following steps:
s132, introducing high-pressure inert gas through the first gas inlet 106 to dredge the blockage of the discharge hole 104. In the dredging process, whether dredging is carried out or not can be further judged through the metering change of the weighing unit 113, and otherwise, high-pressure inert gas is continuously introduced or an alarm is carried out to carry out manual dredging.
When the material pouring is finished, the residual material condition of the transfer tank 115 can be further judged through the observation window 118 on the transfer tank 115. When the excess material of the transfer pot 115 is not reduced or is reduced too slowly, it may be judged that the bottom of the transfer pot 115 is clogged. At this time, it may further include:
and S133, introducing high-pressure inert gas through the second gas inlet 117 to dredge the blockage at the bottom of the transit tank 115.
In step S14, the reaction process and the process of unblocking the clogging are the same as those in step S13, and a description thereof will not be repeated.
In the actual production process, the POCl in the product can be obviously reduced through automatic feed control 3 、H 3 PO 4 And the content of water vapor. POCl in the product 3 、H 3 PO 4 And the content of the water vapor is reduced to be below 0.01 vt% from the original 1-3 vt%, and the purity of the product is improved.
In other embodiments, as a further improvement, the step of opening the second pipe 125 to fill the inert gas into the partial reactor 13 and opening the waste gas discharge port 133 during the reaction process of the remaining reactor 13 to remove the residual gas in the partial reactor 13 for standby further comprises:
and simultaneously opens the solid-liquid discharge port 137 at the bottom of the partial reaction chamber 131 to discharge the solid-liquid waste remaining in the bottom of the partial reaction chamber 131. The solid-liquid waste is a side reaction product, such as PF, produced by the reaction of phosphorus pentachloride and anhydrous HF 3 Cl 2 Etc., which need to be periodically discharged to improve reaction efficiency; and reduces the risk of side reaction products remaining in the reaction chamber 131. Preferably, the solid-liquid waste is discharged every 3 to 5 cycles. As a further improvement, in other embodiments, a volatile solvent may be further introduced through the solid-liquid discharge port 137 for dissolving and removing the solid-liquid waste in the bottom of the partial reaction chamber 131. After the solid-liquid waste is removed by dissolution, inert gas may be further introduced into the partial reactor 13 through the second pipe 125 and the waste gas discharge port 133 may be opened to remove the organic solvent from the partial reactor 13. In actual productionIn the process, the concentration of other side reaction products can be reduced by more than an order of magnitude by periodically removing solid-liquid waste in the bottom of the partial reaction chamber 131.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A continuous and automatic production method of phosphorus pentafluoride comprises the following steps:
s12, opening the second pipeline to fill inert gas into a part of the weighing and conveying bins, opening corresponding exhaust ports to remove residual air and moisture in the part of the weighing and conveying bins, and closing the second pipeline and the exhaust ports;
s13, opening the feed valves corresponding to part of the weighing and conveying bins and the weighing and conveying units to weigh and feed the phosphorus pentachloride, and simultaneously opening the hydrogen fluoride supply tank to feed anhydrous HF to the corresponding part of the reactors for reaction; before the reaction of the partial reactors is finished, simultaneously opening the second pipeline to fill inert gas into the rest weighing and conveying bins, opening corresponding exhaust ports to remove residual air and water vapor in the rest weighing and conveying bins for standby, and closing the second pipeline and the exhaust ports;
s14, opening the feed valves corresponding to the rest of the weighing and conveying bins and the weighing and conveying units to weigh and feed the phosphorus pentachloride, and simultaneously opening the hydrogen fluoride supply tank to feed anhydrous HF into the rest of the reactor and perform reaction; and in the reaction process of the rest reactors, opening the second pipeline to fill inert gas into the partial reactors and opening a waste gas discharge port so as to remove residual gas in the partial reactors for later use, and repeating the above steps to continuously and automatically produce the phosphorus pentafluoride.
2. The continuous and automatic phosphorus pentafluoride production method according to claim 1, wherein in step S12, whether the air and moisture remaining in the weigh bin are removed is judged by detecting the content of the inert gas in the exhaust port.
3. The continuous and automatic process of phosphorus pentafluoride according to claim 1, wherein in step S13, the partial reactor is opened 5-30 minutes before the reaction is completed, and the second pipe is opened to fill the remaining weigh transport bins with inert gas and the corresponding exhaust ports are opened to remove the air and moisture remaining in the remaining weigh transport bins for use.
4. The continuous and automatic phosphorus pentafluoride production process of claim 1, wherein in step S13, the conveying unit is controlled to run at a constant speed at a first speed for less than half a cycle of receiving materials at each feeding; and after the material bearing is finished, controlling the conveying unit to run at a second speed at a constant speed less than half a week to dump the materials.
5. The continuous and automatic phosphorus pentafluoride production method according to claim 4, wherein the conveying unit is controlled to run at a constant speed for 1/3 weeks to receive materials; and after the material bearing is finished, controlling the conveying unit to operate at a constant speed for 1/2 weeks to pour the materials.
6. The continuous and automatic phosphorus pentafluoride production method according to claim 4, wherein when the conveying unit runs at a constant speed at the first speed and the metering amount of the weighing unit is obviously not increased or is slowly increased, the method further comprises the following steps:
s131, introducing high-pressure inert gas through the first gas inlet to dredge the blockage of the discharge hole.
7. The continuous and automatic phosphorus pentafluoride production method according to claim 4, wherein when the feeding valve is controlled to be continuously opened for feeding, and the metering of the weighing unit is obviously not increased or slowly increased, the method further comprises the following steps:
s132, introducing high-pressure inert gas through the first gas inlet to dredge the blockage of the discharge hole.
8. The continuous, automatic production process of phosphorus pentafluoride according to any one of claims 6 to 7, wherein the high-pressure inert gas unit 12 has a gas pressure of 0.5 to 1 MPa.
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