CN116237006B - Energy-saving production device and production method for high-purity phosphorus pentachloride - Google Patents
Energy-saving production device and production method for high-purity phosphorus pentachloride Download PDFInfo
- Publication number
- CN116237006B CN116237006B CN202310324464.7A CN202310324464A CN116237006B CN 116237006 B CN116237006 B CN 116237006B CN 202310324464 A CN202310324464 A CN 202310324464A CN 116237006 B CN116237006 B CN 116237006B
- Authority
- CN
- China
- Prior art keywords
- chlorine
- reaction kettle
- kettle body
- phosphorus
- phosphorus pentachloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 178
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims abstract description 137
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 93
- 239000000460 chlorine Substances 0.000 claims abstract description 93
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 93
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- 230000001105 regulatory effect Effects 0.000 claims description 34
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 29
- 239000000498 cooling water Substances 0.000 claims description 23
- 238000002309 gasification Methods 0.000 claims description 19
- 238000001914 filtration Methods 0.000 claims description 15
- 238000009434 installation Methods 0.000 claims description 14
- 238000005086 pumping Methods 0.000 claims description 8
- 230000003139 buffering effect Effects 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 description 15
- 230000006872 improvement Effects 0.000 description 8
- 239000012320 chlorinating reagent Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- -1 aldehyde ketone Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000009396 hybridization Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006237 Beckmann rearrangement reaction Methods 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- UXJHQBVRZUANLK-UHFFFAOYSA-N azanylidyne(dichloro)-$l^{5}-phosphane Chemical compound ClP(Cl)#N UXJHQBVRZUANLK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000009191 jumping Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
-
- 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
- C01B25/10—Halides or oxyhalides of 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses an energy-saving production device and a production method of high-purity phosphorus pentachloride, wherein the energy-saving production device comprises a reaction kettle body, electromagnetic vibrating plates, a phosphorus trichloride conveying device and a chlorine conveying device, the reaction kettle body comprises a first shell and a second shell, the electromagnetic vibrating plates are arranged in the reaction kettle body and are arranged in a plurality, the electromagnetic vibrating plates are arranged in a crossed mode, a base is arranged at the lower end of each electromagnetic vibrating plate, a reaction plate is arranged at the upper end of each electromagnetic vibrating plate, and a heating disc is arranged in each reaction plate. According to the invention, the plurality of electromagnetic vibrating plates are arranged in the reaction kettle, each layer of vibrating plate vibrates phosphorus trichloride and generated phosphorus pentachloride, so that the vibrating plates are fully and uniformly contacted with chlorine, the chlorine and the phosphorus trichloride are ensured to react completely, the synthesized phosphorus pentachloride has higher purity, and finally the synthesized phosphorus pentachloride with high purity is gasified and then conveyed to a condensing device, so that the phosphorus pentachloride with higher purity is obtained, and the prepared phosphorus pentachloride meets the standard.
Description
Technical Field
The invention belongs to the technical field of phosphorus pentachloride production, and particularly relates to an energy-saving production device and method for high-purity phosphorus pentachloride.
Background
Phosphorus pentachloride is an inorganic compound, has a chemical formula of PCl5, is one of the most important phosphorus chlorides, is light yellow crystalline powder, has pungent odor, is easy to sublimate, and is mainly used as a chlorinating agent. The structural unit of phosphorus pentachloride in solid state can be written as PCl4+, PCl6-, cesium chloride crystal structure, two ions are tetrahedral and octahedral structure respectively, the phosphorus atom in cation is sp3 hybridization, and the phosphorus in anion is sp3d2 hybridization. The gaseous phosphorus pentachloride and the liquid phosphorus pentachloride have single molecular structures, and the molecules are triangular biconical, which is consistent with that predicted by VSEPR theory.
Phosphorus pentachloride is mainly used as chlorinating reagent of alcohol, carboxylic acid, amide, aldehyde ketone and enol and Beckmann rearrangement reagent, is used as chlorinating agent and catalyst in organic synthesis, and is a raw material for producing medicines, dyes and chemical fibers, and is also a raw material for producing phosphonitrile chloride and phosphoryl chloride. The high-purity phosphorus pentachloride is mainly used for synthesizing medical intermediates and lithium hexafluorophosphate.
In the prior art, the production process of phosphorus pentachloride mainly comprises the reaction of phosphorus trichloride and chlorine, wherein the phosphorus trichloride and the chlorine react in a reaction kettle, the phosphorus pentachloride is generated by stirring through a stirring device, chlorine is gasified by chlorine water and is buffered before being added into the reaction kettle, and the phosphorus pentachloride is easy to react with the water, so that the chlorine can be subjected to drying treatment. During the production of the high-purity phosphorus pentachloride, the phosphorus pentachloride synthesized in the reaction kettle is gasified, and the gasified phosphorus pentachloride is coagulated again to obtain the high-purity phosphorus pentachloride.
In the prior art, when phosphorus pentachloride is prepared, phosphorus trichloride and chlorine are stirred by a stirring device, and when the stirring device is used for stirring and mixing the phosphorus trichloride and the chlorine, the reaction area is smaller when the phosphorus trichloride and the chlorine are contacted; secondly, after the phosphorus trichloride and the chlorine are directly connected into the reaction kettle, the uniformity after mixing is different; and finally, the stirring efficiency of the stirring device is reduced and the energy consumption is increased after solidification along with the reduction of the temperature of the reaction kettle after phosphorus pentachloride is generated. Therefore, the purity of the phosphorus pentachloride synthesized in the reaction kettle is low, and the purity of the phosphorus pentachloride obtained by gasifying and then condensing the phosphorus pentachloride is not up to the standard.
Therefore, in order to solve the above-mentioned problems, it is necessary to provide an energy-saving production device and production method for high-purity phosphorus pentachloride.
Disclosure of utility model
The invention aims to provide an energy-saving production device and a production method of high-purity phosphorus pentachloride, so as to solve the problems.
In order to achieve the above object, an embodiment of the present invention provides the following technical solution:
The utility model provides an energy-conserving apparatus for producing of high purity phosphorus pentachloride, includes reation kettle body, electromagnetic vibration board, phosphorus trichloride conveyor and chlorine conveyor, the reation kettle body includes first casing and second casing, electromagnetic vibration board sets up in this and is provided with a plurality of in the reation kettle, and is a plurality of electromagnetic vibration board alternately sets up, electromagnetic vibration board's lower extreme is provided with the base, electromagnetic vibration board's upper end is provided with the reaction plate, be provided with the heating plate in the reaction plate.
The one end of phosphorus trichloride conveyor installs first atomizing nozzle, first atomizing nozzle installs in the upper end of reation kettle body and the nozzle is arranged in the reation kettle body, install second atomizing nozzle and third atomizing nozzle on the chlorine conveyor, second atomizing nozzle and third atomizing nozzle are installed respectively on the lateral wall of reation kettle body.
The reaction kettle body is used for producing phosphorus pentachloride, the electromagnetic vibration plate is used for improving the speed of generating phosphorus pentachloride through the reaction of phosphorus trichloride and chlorine and improving the purity of generating phosphorus pentachloride, the phosphorus trichloride conveying device is used for atomizing the phosphorus trichloride, and the chlorine conveying device is used for forming a chlorine gas zone in the reaction kettle body.
As a further improvement of the present invention, the first housing is disposed inside the second housing, and a receiving chamber for storing cooling water is formed between the first housing and the second housing.
As a further improvement of the invention, the electromagnetic vibration plate is obliquely arranged in the reaction kettle body, a plurality of mounting plates are fixedly connected to the inner side wall of the first shell, the plurality of mounting plates are used for mounting the electromagnetic vibration plate, the lower end of the reaction plate is provided with an electromagnet, a plurality of resonance springs are mounted between the base and the reaction plate, and a plurality of guide plates are arranged on the reaction plate.
As a further improvement of the invention, the upper end of the reaction kettle body is provided with a first mounting pipe, the first atomizing nozzle is mounted on the reaction kettle body through the first mounting pipe, one end of the first atomizing nozzle, which is far away from the reaction kettle body, is provided with a first flow regulating valve, and one end of the first flow regulating valve, which is far away from the first atomizing nozzle, is provided with a pressurizing pipe.
As a further improvement of the invention, the upper end of the accommodating chamber is provided with a cooling water conveying device, the cooling water conveying device is provided with a water inlet pipe, a second flow regulating valve is arranged between the water inlet pipe and the accommodating chamber, a second mounting pipe is fixedly connected to the side wall of the upper end of the second shell, and a water return pipe is arranged on the second mounting pipe.
As a further improvement of the invention, the chlorine conveying device comprises an air inlet pipe and a branch pipe, a third flow regulating valve and a flowmeter are arranged between the air inlet pipe and the branch pipe, and the branch pipe penetrates through the accommodating cavity.
As a further improvement of the invention, the upper end of the reaction kettle body is provided with a phosphorus pentachloride gasification conveying device, the phosphorus pentachloride gasification conveying device is provided with a connecting pipe, and a check valve is arranged on the connecting pipe.
As a further improvement of the invention, the lower end of the reaction kettle body is provided with an emptying device, the emptying device is provided with an emptying pipe, and the emptying pipe is provided with a switch valve.
The energy-saving production process of high purity phosphorus pentachloride includes the steps of preparing phosphorus trichloride and chlorine water as material:
S1, phosphorus trichloride is taken from a phosphorus trichloride overhead tank, firstly, the phosphorus trichloride is filtered by a filtering device so as to increase the purity of the phosphorus trichloride, then the phosphorus trichloride is dehydrated by a dehydration device, and finally, the phosphorus trichloride is conveyed to a booster pump so as to be reserved;
s2, chlorine water is taken from a chlorine water tank, firstly, the chlorine water is gasified, the gasified chlorine water is filtered through a filtering device so as to improve the purity of chlorine, and then the chlorine is conveyed to a buffering device for buffering for standby.
As a further improvement of the invention, the production method is as follows:
S1, controlling flow of the phosphorus trichloride after being pressurized by a booster pump through a first flow regulating valve, atomizing the pressurized phosphorus trichloride through a pressurizing pipe, and spraying the atomized phosphorus trichloride into a reaction kettle body; meanwhile, the chlorine in the buffer device is conveyed to a second atomizing nozzle and a third atomizing nozzle through the control flow of a third flow regulating valve, and the second atomizing nozzle and the third atomizing nozzle atomize the chlorine and then spray the chlorine into the reaction kettle body;
S2, firstly, phosphorus trichloride and chlorine on the uppermost layer are in contact reaction, the phosphorus trichloride falls onto the surface of a reaction plate on the uppermost layer, the vibration frequency of an electromagnetic vibration plate is controlled in a pulse mode, the phosphorus trichloride on the surface of the reaction plate is vibrated and floated by the vibration of the electromagnetic vibration plate, the phosphorus trichloride is continuously vibrated and floated by the vibration of the electromagnetic vibration plate so as to be in continuous contact with the phosphorus trichloride, the phosphorus trichloride and the synthesized phosphorus pentachloride can continuously move forwards due to the inclined arrangement of the electromagnetic vibration plate, finally falls onto an electromagnetic vibration plate on the lower layer from the edge, the phosphorus trichloride and the synthesized phosphorus pentachloride are continuously vibrated and floated again and contacted with the chlorine on the electromagnetic vibration plate on the lowermost layer, and repeated vibration falls onto the electromagnetic vibration plate on the lowermost layer, so that the phosphorus trichloride and the chlorine are fully contacted, and the purity of the finally generated phosphorus pentachloride is increased;
Wherein the mol ratio of the phosphorus trichloride to the chlorine is 1:1.05-1.15, the temperature in the reaction kettle body is controlled at 75-80 ℃, the pressure of the phosphorus trichloride after pressurization is controlled at 0.4-0.45 MPa, the pressure of the chlorine is controlled at 0.35-0.4 MPa, the reaction time of the phosphorus trichloride and the chlorine in the reaction kettle body is 1 hour, wherein the vibration frequency of an electromagnetic vibration plate in the first 0.8 hour is 0.4-0.6 Hz, and the vibration frequency of the electromagnetic vibration plate in the last 0.2 hour is 1-1.1 Hz;
s3, as the phosphorus trichloride and the chlorine react to release heat, the temperature in the reaction kettle body continuously rises, and in order to conveniently control the temperature in the reaction kettle body to 75-80 ℃, the water flow in the accommodating cavity is required to be controlled through a second flow regulating valve so as to control the temperature in the reaction kettle body;
S4, stopping adding phosphorus trichloride and chlorine into the reaction kettle body after the phosphorus pentachloride in the reaction kettle body is reacted, adjusting the temperature in the reaction kettle body through a second flow regulating valve, or opening a heating plate in a reaction plate so as to adjust the temperature in the reaction kettle body to 110-120 ℃, gasifying the phosphorus pentachloride, heating for 0.2 hours, and pumping the gasified phosphorus pentachloride in the reaction kettle body into a condensing device through a phosphorus pentachloride gasification conveying device through pumping equipment so as to condense the phosphorus pentachloride into high-purity phosphorus pentachloride in the condensing device;
wherein the gasified phosphorus pentachloride needs to be filtered by a filtering device before reaching the condensing device, and the temperature in the filtering device is close to the temperature of the gasified phosphorus pentachloride.
Compared with the prior art, the invention has the following advantages:
According to the invention, the plurality of electromagnetic vibrating plates are arranged in the reaction kettle, chlorine is atomized from the side wall of the reaction kettle through the plurality of nozzles and then sprayed into the reaction kettle, so that a plurality of chlorine gas areas are formed, dehydrated and pressurized phosphorus trichloride is sprayed into the reaction kettle through the atomizing nozzles at the top of the reaction kettle, the atomized phosphorus trichloride can be contacted with the chlorine gas in the reaction kettle, the electromagnetic vibrating plates vibrate the phosphorus trichloride so that the phosphorus trichloride jumps on the reaction plate, the phosphorus trichloride and the synthesized phosphorus pentachloride can be contacted with the chlorine gas quickly and uniformly, the phosphorus trichloride and the synthesized phosphorus pentachloride gradually move towards the lower electromagnetic vibrating plates along with the vibration of the electromagnetic vibrating plates, and each layer of vibrating plates vibrate the unreacted phosphorus trichloride and the generated phosphorus pentachloride so that the phosphorus pentachloride is contacted with the chlorine gas sufficiently and uniformly, the complete reaction of the chlorine gas and the phosphorus trichloride is ensured, and the synthesized phosphorus pentachloride has higher purity. And finally, gasifying the synthesized high-purity phosphorus pentachloride and conveying the gasified high-purity phosphorus pentachloride to a condensing device to obtain higher-purity phosphorus pentachloride so that the prepared phosphorus pentachloride reaches the standard.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings may be obtained according to the drawings without inventive effort to those skilled in the art.
FIG. 1 is a front view of an energy-saving production apparatus for high-purity phosphorus pentachloride according to an embodiment of the present invention;
FIG. 2 is a perspective view of an energy-saving production device for high-purity phosphorus pentachloride according to an embodiment of the present invention;
FIG. 3 is a top cross-sectional view of an energy-efficient apparatus for producing high purity phosphorus pentachloride according to one embodiment of the present invention;
FIG. 4 is a front cross-sectional view of an energy-saving apparatus for producing phosphorus pentachloride with high purity according to one embodiment of the present invention;
FIG. 5 is a front cross-sectional view of an energy-saving apparatus for producing phosphorus pentachloride of a first embodiment of the present invention;
fig. 6 is a front cross-sectional view of an energy-saving apparatus for producing phosphorus pentachloride of a type in accordance with an embodiment of the present invention.
In the figure: 100. the reactor comprises a reactor body, 101, a first shell, 102, a second shell, 103, a containing chamber, 200, an electromagnetic vibration plate, 201, a base, 202, an electromagnet, 203, a resonant spring, 204, a reaction plate, 205, a deflector, 206, a mounting plate, 300, a phosphorus trichloride delivery device, 301, a pressurizing pipe, 302, a first flow regulating valve, 303, a first atomizing nozzle, 304, a first mounting pipe, 400, a cooling water delivery device, 401, a water inlet pipe, 402, a second flow regulating valve, 403, a water return pipe, 404, a second mounting pipe, 500, a chlorine delivery device, 501, an air inlet pipe, 502, a third flow regulating valve, 503, a flowmeter, 504, a branch pipe, 505, a second atomizing nozzle, 506, a third atomizing nozzle, 600, a phosphorus pentachloride gasification delivery device, 601, 602, a check valve, 700, an evacuation device, 701, an evacuation pipe, 702, and a switching valve.
Detailed Description
The present invention will be described in detail below with reference to the embodiments shown in the drawings. The embodiments are not intended to limit the invention, but structural, methodological, or functional modifications of the invention from those skilled in the art are included within the scope of the invention.
The invention discloses an energy-saving production device for high-purity phosphorus pentachloride, which is shown in fig. 1-6, and comprises a reaction kettle body 100, an electromagnetic vibration plate 200, a phosphorus trichloride conveying device 300 and a chlorine conveying device 500, wherein when phosphorus pentachloride is produced, the phosphorus trichloride and the chlorine are generated through reaction, and the reaction of the phosphorus trichloride and the chlorine is carried out in the reaction kettle body 100.
Referring to fig. 3 to 6, the reaction kettle body 100 includes a first housing 101 and a second housing 102, the first housing 101 is disposed inside the second housing 102, a receiving chamber 103 is formed between the first housing 101 and the second housing 102, and the receiving chamber 103 is used for storing cooling water. The reaction kettle body 100 is provided with a first casing 101 and a second casing 102, the second casing 102 is arranged outside when arranged, the first casing 101 is arranged inside, the first casing 101 and the second casing 102 are integrally formed, and a containing chamber 103 is formed between the first casing 101 and the second casing 102. Since phosphorus trichloride and chlorine in the reaction kettle body 100 can release heat during reaction, in order to facilitate the control of the temperature in the reaction kettle body 100, the temperature in the reaction kettle body 100 is regulated by arranging the accommodating chamber 103 and introducing cooling water into the accommodating chamber 103.
Referring to fig. 3 to 6, a plurality of electromagnetic vibration plates 200 are provided in the reaction vessel body 100, and a plurality of electromagnetic vibration plates 200 are disposed to intersect. Since the conventional phosphorus trichloride and chlorine gas are stirred by the stirring device when they react in the reaction kettle body 100, the reaction rate of the phosphorus trichloride and the chlorine gas is increased, thereby generating phosphorus pentachloride. When the stirring device is used for stirring the phosphorus trichloride and the chlorine, the stirring device is not fully used for mixing the phosphorus trichloride and the chlorine, and after a large amount of phosphorus pentachloride is generated, the phosphorus pentachloride is solid at a low temperature, so that the resistance of the stirring device is large, the use of the stirring device is not facilitated, and the use energy consumption of the stirring device is increased. In order to solve the above-described problem, an electromagnetic vibration plate 200 is used instead of the stirring device.
Referring to fig. 6, the electromagnetic vibration plate 200 is obliquely disposed in the reaction kettle body 100, and a plurality of mounting plates 206 are fixedly connected to the inner sidewall of the first housing 101, and the plurality of mounting plates 206 are used for mounting the electromagnetic vibration plate 200. Since phosphorus trichloride and chlorine react on the electromagnetic vibration plate 200, in order to allow phosphorus trichloride and synthesized phosphorus pentachloride to move to the lower electromagnetic vibration plate 200 through the electromagnetic vibration plate 200 after the reaction, the electromagnetic vibration plate 200 is obliquely arranged, and the phosphorus trichloride and the synthesized phosphorus pentachloride move to one end of the lower position of the electromagnetic vibration plate 200 under the action of the vibration of the electromagnetic vibration plate 200. In order to facilitate the installation of the electromagnetic vibration plate 200, the installation plate 206 is fixedly connected to the inner side wall of the first housing 101, and the lower end of the electromagnetic vibration plate 200 is installed on the installation plate 206. Meanwhile, in order to stabilize the mounting of the electromagnetic vibration plate 200 on the mounting plate 206, the electromagnetic vibration plate 200 may be connected to the mounting plate 206 by a connector such as a bolt that is easy to mount and dismount and has good fixability.
The lower extreme of electromagnetic vibration board 200 is provided with base 201, and the upper end of electromagnetic vibration board 200 is provided with reaction plate 204, and the lower extreme of reaction plate 204 is provided with electro-magnet 202, installs a plurality of resonance springs 203 between base 201 and the reaction plate 204, is provided with a plurality of guide plates 205 on the reaction plate 204. The base 201 is a support for the electromagnetic vibration plate 200 for supporting the electromagnetic vibration plate 200 and mounting the electromagnetic vibration plate 200. When the electromagnet 202 is electrified, electromagnetic force can be generated, when the electromagnetic force is generated by the base 201, the base 201 is attracted, the electromagnet 202 can move downwards under the action of the electromagnetic force because the position of the base 201 is fixed, and the electromagnet 202 is arranged on the reaction plate 204, so that the electromagnet 202 can drive the reaction plate 204 to move downwards. The resonance spring 203 is disposed between the base 201 and the reaction plate 204, when the reaction plate 204 moves downward, the resonance spring 203 contracts, when the electromagnetic force is eliminated after the electromagnet 202 is powered off, the resonance spring 203 resets, and the reaction plate 204 is driven to move upward during resetting.
Preferably, the electromagnetic vibration plate 200 is electrically connected, and the electromagnetic vibration plate 200 is controlled to be on-off in a pulse mode, and the electromagnetic vibration plate 200 is controlled in a pulse mode, so that the electromagnetic vibration plate 200 is controlled by a DCS system or a PLC system. When the pulse-controlled electromagnetic vibration plate 200 is electrified, the electromagnet 202 generates electromagnetic force, so that the reaction plate 204 approaches the base 201, and the resonant spring 203 is compressed; when the pulse-controlled electromagnetic vibration plate 200 is powered off, the electromagnetic force on the electromagnet 202 disappears, the resonant spring 203 resets, and the reaction plate 204 is driven to move upwards during resetting. By such reciprocating control, frequent runout of the reaction plate 204 on the electromagnetic vibration plate 200 is realized, and vibration is realized.
Further, under the vibration of the reaction plate 204, the phosphorus trichloride on the reaction plate 204 will follow the vibration, so that the phosphorus trichloride jumps on the reaction plate 204, so that the phosphorus trichloride and the chlorine can be fully contacted, and the reaction rate is promoted. And when the phosphorus trichloride vibrates on the electromagnetic vibration plate 200, the phosphorus trichloride gradually moves from the upper electromagnetic vibration plate 200 to the lower electromagnetic vibration plate 200 and descends layer by layer, and the phosphorus trichloride on each layer can jump on the reaction plate 204, so that the phosphorus trichloride is fully contacted with chlorine. And a plurality of baffles 205 are provided on the reaction plate 204, the baffles 205 will restrict the movement of phosphorus trichloride on the reaction plate 204 so that it will stay on each layer of the reaction plate 204 for a sufficient time to ensure the sufficiency of its reaction. Through the vibration of the electromagnetic vibration plate 200, the generated phosphorus pentachloride can easily jump on the electromagnetic vibration plate 200 after being vibrated, the jumping resistance can not be increased due to the phosphorus pentachloride, and the energy consumption is saved.
Referring to fig. 4 to 6, a first atomizing nozzle 303 is installed at one end of the phosphorus trichloride conveying apparatus 300, the first atomizing nozzle 303 is installed at the upper end of the reaction kettle body 100, and the nozzle is disposed in the reaction kettle body 100. In order to make the phosphorus trichloride added into the reaction kettle body 100 better contact with chlorine, the phosphorus trichloride is pressurized by the pressurizing device and then conveyed to the first atomizing nozzle 303 by the phosphorus trichloride conveying device 300, and then the pressurized phosphorus trichloride is atomized by the first atomizing nozzle 303 and then conveyed into the reaction kettle body 100, and the atomized phosphorus trichloride can be well contacted with the chlorine, so that the reaction rate of the phosphorus trichloride and the chlorine is greatly improved.
Referring to fig. 4 to 6, a first installation pipe 304 is provided at the upper end of the reaction vessel body 100, a first atomizing nozzle 303 is installed on the reaction vessel body 100 through the first installation pipe 304, a first flow rate adjusting valve 302 is installed at one end of the first atomizing nozzle 303 far from the reaction vessel body 100, and a pressurizing pipe 301 is installed at one end of the first flow rate adjusting valve 302 far from the first atomizing nozzle 303. In order to facilitate the installation of the first atomizing nozzle 303, the first atomizing nozzle 303 may be screwed to the first installation pipe 304 by providing the first installation pipe 304 on the reaction kettle body 100. Since the flow rate of the phosphorus trichloride to be conveyed into the reaction kettle body 100 needs to be controlled, in order to facilitate accurate control of the flow rate, the first flow rate regulating valve 302 can realize higher-accuracy control of the flow rate by arranging the first flow rate regulating valve 302 on the phosphorus trichloride conveying device 300. The first flow control valve 302 is electrically connected, and the first flow control valve 302 can be controlled by a DCS system or a PLC system.
Referring to fig. 1, 4,5 and 6, a cooling water delivery device 400 is disposed at the upper end of the accommodating chamber 103, a water inlet pipe 401 is disposed on the cooling water delivery device 400, a second flow regulating valve 402 is installed between the water inlet pipe 401 and the accommodating chamber 103, a second installation pipe 404 is fixedly connected to the upper end side wall of the second housing 102, and a water return pipe 403 is installed on the second installation pipe 404. In order to facilitate the control of the temperature in the reaction kettle body 100, the cooling water is supplied through the cooling water supply device 400 by introducing the cooling water into the accommodating chamber 103. Meanwhile, since the temperature control in the reaction kettle body 100 has a high requirement, the temperature needs to be ensured within a required range, and thus the flow rate of the cooling water needs to be controlled, the cooling water conveying device 400 is provided with the second flow rate regulating valve 402, and the flow rate of the cooling water can be controlled through the second flow rate regulating valve 402. The second flow regulating valve 402 is electrically connected, and the second flow regulating valve 402 can be controlled by a DCS system or a PLC system.
The switching value of the second flow regulating valve 402 is controlled by the set temperature, a temperature measuring element is arranged in the reaction kettle body 100, the temperature in the reaction kettle body 100 can be monitored in real time, and the detected temperature is interlocked with the second flow regulating valve 402. When the temperature in the reaction kettle body 100 is higher than the set value, the switching value of the second flow regulating valve 402 is increased so as to increase the flow rate of the cooling water, so that the speed of water replacement in the accommodating chamber 103 is increased, and the temperature in the reaction kettle body 100 is reduced by the cooling water; conversely, by decreasing the opening/closing amount of the second flow rate adjustment valve 402, the temperature in the reaction kettle body 100 can be increased.
Preferably, the water after cooling the accommodating chamber 103 is discharged through the water return pipe 403, so that the cooling water discharged from the water return pipe 403 is recycled for saving energy and reducing consumption, and the gasification device is needed to be used when the chlorine water is gasified, and the gasification of the chlorine gas needs to absorb heat, so that the gasification device which uses hot water as a heat source can be selected, the returned cooling water is conveyed to the gasification device, the chlorine water can be gasified through the returned water, the temperature of the cooling water after passing through the gasification device can be reduced, and the cooling water can be led into the accommodating chamber 103 again for cooling use, so that the circulation is performed, and the energy saving and the consumption reduction are realized.
Referring to fig. 1 to 6, the chlorine gas delivery apparatus 500 is provided with a second atomizing nozzle 505 and a third atomizing nozzle 506, the second atomizing nozzle 505 and the third atomizing nozzle 506 are respectively provided on the side wall of the reactor body 100, the chlorine gas delivery apparatus 500 includes an air inlet pipe 501 and a branch pipe 504, a third flow rate adjusting valve 502 and a flow meter 503 are provided between the air inlet pipe 501 and the branch pipe 504, and the branch pipe 504 penetrates through the accommodating chamber 103. In order to facilitate the dispersing and inputting of the chlorine into the reaction kettle body 100, the contact area between the chlorine and the phosphorus trichloride in the reaction kettle body 100 is increased, and the chlorine is atomized by the second atomizing nozzle 505 and the third atomizing nozzle 506 and then is conveyed into the reaction kettle body 100.
Further, the second atomizing nozzle 505 and the third atomizing nozzle 506 are different in size, the second atomizing nozzle 505 is larger than the third atomizing nozzle 506, so that the chlorine gas input through the second atomizing nozzle 505 is more than the chlorine gas conveyed by the third atomizing nozzle 506, the chlorine gas conveyed through the second atomizing nozzle 505 and the third atomizing nozzle 506 forms a chlorine gas zone in the reaction kettle body 100, the chlorine gas content of the upper layer is larger than the chlorine gas content of the lower layer, and after the phosphorus trichloride is added into the reaction kettle body 100, the reaction rate of the upper layer is larger than the reaction rate of the lower layer, so that the chlorine gas content of the upper layer is large. The input of chlorine is controlled by a third flow rate adjusting valve 502, wherein the third flow rate adjusting valve 502 is electrically connected with a flow meter 503, and the third flow rate adjusting valve 502 can be controlled by a DCS system or a PLC system.
Referring to fig. 1 and 6, a phosphorus pentachloride gasification conveyor 600 is provided at the upper end of the reaction vessel body 100, the phosphorus pentachloride gasification conveyor 600 is provided with a connection pipe 601, and a check valve 602 is installed on the connection pipe 601. After phosphorus trichloride and chlorine gas react in the reactor body 100 to produce phosphorus pentachloride, the produced phosphorus pentachloride is gasified by heating, and the gasified phosphorus pentachloride is transported by the phosphorus pentachloride gasification transport device 600 in order to obtain high-purity phosphorus pentachloride. The phosphorus pentachloride gasification conveying device 600 is connected with the condensing device, and a pumping device is arranged between the phosphorus pentachloride gasification conveying device 600 and the condensing device, and phosphorus pentachloride is conveyed into the condensing device through the pumping device. The phosphorus pentachloride gasification conveyor 600 is provided with a check valve 602, so that the gasified phosphorus pentachloride can be prevented from returning to the reactor body 100.
Referring to fig. 1 to 6, an evacuation device 700 is provided at the lower end of the reaction vessel body 100, the evacuation device 700 is provided with an evacuation pipe 701, and the evacuation pipe 701 is provided with an on-off valve 702. After the high-purity phosphorus pentachloride is prepared through the reaction kettle body 100, impurities and the like can remain in the reaction kettle body 100, and in order to facilitate the discharge of the impurities in the reaction kettle body 100, an evacuating device 700 is arranged at the lower end of the reaction kettle body 100, and the impurities are discharged through the evacuating device 700. The evacuation device 700 is provided with the on-off valve 702, the on-off valve 702 is electrically connected, and the on-off valve 702 can be controlled by a DCS system or a PLC system.
The energy-saving production process of high purity phosphorus pentachloride includes the steps of preparing phosphorus trichloride and chlorine water as material:
S1, phosphorus trichloride is taken from a phosphorus trichloride overhead tank, firstly, the phosphorus trichloride is filtered by a filtering device so as to increase the purity of the phosphorus trichloride, then the phosphorus trichloride is dehydrated by a dehydration device, and finally, the phosphorus trichloride is conveyed to a booster pump so as to be reserved;
s2, chlorine water is taken from a chlorine water tank, firstly, the chlorine water is gasified, the gasified chlorine water is filtered through a filtering device so as to improve the purity of chlorine, and then the chlorine is conveyed to a buffering device for buffering for standby.
The production method of the high-purity phosphorus pentachloride comprises the following steps:
S1, controlling flow of the phosphorus trichloride after being pressurized by a booster pump through a first flow regulating valve 302, atomizing the pressurized phosphorus trichloride through a pressurizing pipe 301, and spraying the atomized phosphorus trichloride into a reaction kettle body 100; meanwhile, the chlorine in the buffer device is conveyed to the second atomizing nozzle 505 and the third atomizing nozzle 506 through the control flow of the third flow regulating valve 502, and the second atomizing nozzle 505 and the third atomizing nozzle 506 atomize the chlorine and then spray the atomized chlorine into the reaction kettle body 100, and as the second atomizing nozzle 505 and the third atomizing nozzle 506 are different in size and the second atomizing nozzle 505 is larger than the third atomizing nozzle 506, different atomizing areas are formed in the reaction kettle body 100;
S2, firstly, phosphorus trichloride reacts with chlorine gas at the uppermost layer in a contact way, the phosphorus trichloride falls onto the surface of a reaction plate 204 at the uppermost layer, the vibration frequency of an electromagnetic vibration plate 200 is controlled in a pulse way, the vibration of the electromagnetic vibration plate 200 can enable the phosphorus trichloride at the surface of the reaction plate 204 to float in a vibration way, the phosphorus trichloride continuously floats in a vibration way through the continuous vibration of the electromagnetic vibration plate 200 so as to enable the chlorine gas to be continuously contacted with the phosphorus trichloride, and the phosphorus trichloride and the synthesized phosphorus pentachloride continuously move forwards and finally fall onto the electromagnetic vibration plate 200 at the lower layer from the edge, the phosphorus trichloride and the synthesized phosphorus pentachloride continuously float in a vibration way again and contact with the chlorine gas on the electromagnetic vibration plate 200 at the lowermost layer in a repeated vibration way, so that the phosphorus trichloride and the chlorine gas are fully contacted, and the purity of the phosphorus pentachloride finally generated is increased;
Wherein, the mol ratio of the phosphorus trichloride to the chlorine is 1:1.05-1.15, the temperature in the reaction kettle body 100 is controlled at 75-80 ℃, the pressure of the phosphorus trichloride after pressurization is controlled at 0.4-0.45 MPa, the pressure of the chlorine is controlled at 0.35-0.4 MPa, the reaction time of the phosphorus trichloride and the chlorine in the reaction kettle body 100 is 1 hour, wherein the vibration frequency of the electromagnetic vibration plate 200 in the first 0.8 hour is 0.4-0.6 Hz, and the vibration frequency of the electromagnetic vibration plate 200 in the last 0.2 hour is 1-1.1 Hz;
S3, as the phosphorus trichloride and the chlorine react to release heat, the temperature in the reaction kettle body 100 continuously rises, and in order to conveniently control the temperature in the reaction kettle body 100 to be 75-80 ℃, the water flow in the accommodating chamber 103 needs to be controlled through the second flow regulating valve 402 so as to control the temperature in the reaction kettle body 100;
S4, stopping adding phosphorus trichloride and chlorine into the reaction kettle body 100 after the phosphorus pentachloride in the reaction kettle body 100 is reacted, adjusting the temperature in the reaction kettle body 100 through a second flow regulating valve 402, or opening a heating plate in a reaction plate 204 so as to adjust the temperature in the reaction kettle body 100 to 110-120 ℃, gasifying the phosphorus pentachloride, heating for 0.2 hours, and pumping the gasified phosphorus pentachloride in the reaction kettle body 100 into a condensing device through a phosphorus pentachloride gasification conveying device 600 through a pumping device so as to condense the phosphorus pentachloride into high-purity phosphorus pentachloride in the condensing device;
Wherein the gasified phosphorus pentachloride needs to be filtered by a filtering device before reaching the condensing device, and the temperature in the filtering device is close to the temperature of the gasified phosphorus pentachloride. The temperature of the device for filtering the gasified phosphorus pentachloride is set to be close to the temperature of the gasified phosphorus pentachloride, so as to avoid condensation of the phosphorus pentachloride in the filtering device caused by low temperature of the filtering device.
The technical scheme shows that the invention has the following beneficial effects:
According to the invention, the plurality of electromagnetic vibrating plates are arranged in the reaction kettle, chlorine is atomized from the side wall of the reaction kettle through the plurality of nozzles and then sprayed into the reaction kettle, so that a plurality of chlorine gas areas are formed, dehydrated and pressurized phosphorus trichloride is sprayed into the reaction kettle through the atomizing nozzles at the top of the reaction kettle, the atomized phosphorus trichloride can be contacted with the chlorine gas in the reaction kettle, the electromagnetic vibrating plates vibrate the phosphorus trichloride so that the phosphorus trichloride jumps on the reaction plate, the phosphorus trichloride and the synthesized phosphorus pentachloride can be contacted with the chlorine gas quickly and uniformly, the phosphorus trichloride and the synthesized phosphorus pentachloride gradually move towards the lower electromagnetic vibrating plates along with the vibration of the electromagnetic vibrating plates, and each layer of vibrating plates vibrate the unreacted phosphorus trichloride and the generated phosphorus pentachloride so that the phosphorus pentachloride is contacted with the chlorine gas sufficiently and uniformly, the complete reaction of the chlorine gas and the phosphorus trichloride is ensured, and the synthesized phosphorus pentachloride has higher purity. And finally, gasifying the synthesized high-purity phosphorus pentachloride and conveying the gasified high-purity phosphorus pentachloride to a condensing device to obtain higher-purity phosphorus pentachloride so that the prepared phosphorus pentachloride reaches the standard.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment contains only one independent technical solution, and that such description is provided for clarity only, and that the technical solutions of the embodiments may be appropriately combined to form other embodiments that will be understood by those skilled in the art.
Claims (10)
1. An energy-saving production device for high-purity phosphorus pentachloride, which is characterized by comprising:
the reaction kettle body comprises a first shell and a second shell;
The electromagnetic vibration plates are arranged in the reaction kettle body and are in cross arrangement, the lower ends of the electromagnetic vibration plates are provided with bases, the upper ends of the electromagnetic vibration plates are provided with reaction plates, and heating discs are arranged in the reaction plates;
The device comprises a phosphorus trichloride conveying device, wherein a first atomizing nozzle is arranged at one end of the phosphorus trichloride conveying device, and is arranged at the upper end of a reaction kettle body, and the nozzle is arranged in the reaction kettle body;
the chlorine conveying device is provided with a second atomizing nozzle and a third atomizing nozzle, and the second atomizing nozzle and the third atomizing nozzle are respectively arranged on the side wall of the reaction kettle body;
The reaction kettle body is used for producing phosphorus pentachloride, the electromagnetic vibration plate is used for improving the speed of generating phosphorus pentachloride through the reaction of phosphorus trichloride and chlorine and improving the purity of generating phosphorus pentachloride, the phosphorus trichloride conveying device is used for atomizing the phosphorus trichloride, and the chlorine conveying device is used for forming a chlorine gas zone in the reaction kettle body.
2. The energy-saving production device and the production method for the high-purity phosphorus pentachloride according to claim 1, wherein the first shell is arranged on the inner side of the second shell, a containing cavity is formed between the first shell and the second shell, and the containing cavity is used for storing cooling water.
3. The energy-saving production device for high-purity phosphorus pentachloride according to claim 2, wherein the electromagnetic vibration plate is obliquely arranged in the reaction kettle body, a plurality of mounting plates are fixedly connected to the inner side wall of the first shell, the plurality of mounting plates are used for mounting the electromagnetic vibration plate, an electromagnet is arranged at the lower end of the reaction plate, a plurality of resonant springs are mounted between the base and the reaction plate, and a plurality of guide plates are arranged on the reaction plate.
4. The energy-saving production device for high-purity phosphorus pentachloride according to claim 1, wherein a first installation pipe is arranged at the upper end of the reaction kettle body, the first atomizing nozzle is installed on the reaction kettle body through the first installation pipe, a first flow regulating valve is installed at one end, far away from the reaction kettle body, of the first atomizing nozzle, and a pressurizing pipe is installed at one end, far away from the first atomizing nozzle, of the first flow regulating valve.
5. The energy-saving production device of high-purity phosphorus pentachloride according to claim 2, wherein a cooling water conveying device is arranged at the upper end of the accommodating chamber, a water inlet pipe is arranged on the cooling water conveying device, a second flow regulating valve is arranged between the water inlet pipe and the accommodating chamber, a second installation pipe is fixedly connected to the side wall of the upper end of the second shell, and a water return pipe is arranged on the second installation pipe.
6. The energy-saving production device of high-purity phosphorus pentachloride according to claim 2, wherein the chlorine conveying device comprises an air inlet pipe and a branch pipe, a third flow regulating valve and a flow meter are arranged between the air inlet pipe and the branch pipe, and the branch pipe penetrates through the accommodating cavity.
7. The energy-saving production device of high-purity phosphorus pentachloride according to claim 1, wherein the upper end of the reaction kettle body is provided with a phosphorus pentachloride gasification conveying device, the phosphorus pentachloride gasification conveying device is provided with a connecting pipe, and a check valve is arranged on the connecting pipe.
8. The energy-saving production device for high-purity phosphorus pentachloride according to claim 7, wherein an evacuating device is arranged at the lower end of the reaction kettle body, an evacuating pipe is arranged on the evacuating device, and a switch valve is arranged on the evacuating pipe.
9. An energy-saving production method of high-purity phosphorus pentachloride is characterized by comprising the following steps of:
S1, controlling flow of the phosphorus trichloride after being pressurized by a booster pump through a first flow regulating valve, atomizing the pressurized phosphorus trichloride through a pressurizing pipe, and spraying the atomized phosphorus trichloride into a reaction kettle body; meanwhile, the chlorine in the buffer device is conveyed to a second atomizing nozzle and a third atomizing nozzle through the control flow of a third flow regulating valve, and the second atomizing nozzle and the third atomizing nozzle atomize the chlorine and then spray the chlorine into the reaction kettle body;
S2, firstly, phosphorus trichloride and chlorine on the uppermost layer are in contact reaction, the phosphorus trichloride falls onto the surface of a reaction plate on the uppermost layer, the vibration frequency of an electromagnetic vibration plate is controlled in a pulse mode, the phosphorus trichloride on the surface of the reaction plate is vibrated and floated by the vibration of the electromagnetic vibration plate, the phosphorus trichloride is continuously vibrated and floated by the vibration of the electromagnetic vibration plate so as to be in continuous contact with the phosphorus trichloride, the phosphorus trichloride and the synthesized phosphorus pentachloride can continuously move forwards due to the inclined arrangement of the electromagnetic vibration plate, finally falls onto an electromagnetic vibration plate on the lower layer from the edge, the phosphorus trichloride and the synthesized phosphorus pentachloride are continuously vibrated and floated again and contacted with the chlorine on the electromagnetic vibration plate on the lowermost layer, and repeated vibration falls onto the electromagnetic vibration plate on the lowermost layer, so that the phosphorus trichloride and the chlorine are fully contacted, and the purity of the finally generated phosphorus pentachloride is increased;
Wherein the mol ratio of the phosphorus trichloride to the chlorine is 1:1.05-1.15, the temperature in the reaction kettle body is controlled at 75-80 ℃, the pressure of the phosphorus trichloride after pressurization is controlled at 0.4-0.45 MPa, the pressure of the chlorine is controlled at 0.35-0.4 MPa, the reaction time of the phosphorus trichloride and the chlorine in the reaction kettle body is 1 hour, wherein the vibration frequency of an electromagnetic vibration plate in the first 0.8 hour is 0.4-0.6 Hz, and the vibration frequency of the electromagnetic vibration plate in the last 0.2 hour is 1-1.1 Hz;
s3, as the phosphorus trichloride and the chlorine react to release heat, the temperature in the reaction kettle body continuously rises, and in order to conveniently control the temperature in the reaction kettle body to 75-80 ℃, the water flow in the accommodating cavity is required to be controlled through a second flow regulating valve so as to control the temperature in the reaction kettle body;
S4, stopping adding phosphorus trichloride and chlorine into the reaction kettle body after the phosphorus pentachloride in the reaction kettle body is reacted, adjusting the temperature in the reaction kettle body through a second flow regulating valve, or opening a heating plate in a reaction plate so as to adjust the temperature in the reaction kettle body to 110-120 ℃, gasifying the phosphorus pentachloride, heating for 0.2 hours, and pumping the gasified phosphorus pentachloride in the reaction kettle body into a condensing device through a phosphorus pentachloride gasification conveying device through pumping equipment so as to condense the phosphorus pentachloride into high-purity phosphorus pentachloride in the condensing device;
wherein the gasified phosphorus pentachloride needs to be filtered by a filtering device before reaching the condensing device, and the temperature in the filtering device is close to the temperature of the gasified phosphorus pentachloride.
10. The energy-saving production method of high-purity phosphorus pentachloride according to claim 9, wherein the phosphorus trichloride and the chlorine water are produced as raw materials, and the raw materials are prepared by the following steps:
S1, phosphorus trichloride is taken from a phosphorus trichloride overhead tank, firstly, the phosphorus trichloride is filtered by a filtering device so as to increase the purity of the phosphorus trichloride, then the phosphorus trichloride is dehydrated by a dehydration device, and finally, the phosphorus trichloride is conveyed to a booster pump so as to be reserved;
s2, chlorine water is taken from a chlorine water tank, firstly, the chlorine water is gasified, the gasified chlorine water is filtered through a filtering device so as to improve the purity of chlorine, and then the chlorine is conveyed to a buffering device for buffering for standby.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310324464.7A CN116237006B (en) | 2023-03-30 | 2023-03-30 | Energy-saving production device and production method for high-purity phosphorus pentachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310324464.7A CN116237006B (en) | 2023-03-30 | 2023-03-30 | Energy-saving production device and production method for high-purity phosphorus pentachloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116237006A CN116237006A (en) | 2023-06-09 |
| CN116237006B true CN116237006B (en) | 2024-05-24 |
Family
ID=86633315
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310324464.7A Active CN116237006B (en) | 2023-03-30 | 2023-03-30 | Energy-saving production device and production method for high-purity phosphorus pentachloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116237006B (en) |
Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1210810A (en) * | 1997-06-06 | 1999-03-17 | 埃勒夫阿托化学有限公司 | Process for manufacture of lithium hexafluorophosphate |
| JP2007069139A (en) * | 2005-09-08 | 2007-03-22 | Yayoi Chemical Industry Co Ltd | Stirring impeller for mixing apparatus |
| CN201437505U (en) * | 2009-07-03 | 2010-04-14 | 中国石油天然气股份有限公司 | Inclined plate chlorine dioxide reactor |
| CN201945216U (en) * | 2010-07-06 | 2011-08-24 | 路辉 | Totally-enclosed channel continuous type centerless pipe spiral baffle heat exchanger |
| CN202107526U (en) * | 2011-06-16 | 2012-01-11 | 江苏大明科技有限公司 | Circulation process system for producing phosphorus oxychloride by pure oxygen oxidation of phosphorus trichloride |
| CN204661329U (en) * | 2015-04-01 | 2015-09-23 | 徐州市建平化工有限公司 | Phosphorus pentachloride production device |
| CN204661328U (en) * | 2015-04-01 | 2015-09-23 | 徐州市建平化工有限公司 | Modified version phosphorus pentachloride production device |
| CN105195064A (en) * | 2015-09-15 | 2015-12-30 | 沅江华龙催化科技有限公司 | Improved reaction and separation synchronous reactor |
| CN108975293A (en) * | 2018-09-11 | 2018-12-11 | 安徽东至广信农化有限公司 | A kind of synthetic method of high purity phosphorus pentachloride |
| CN113941238A (en) * | 2021-03-22 | 2022-01-18 | 青岛大学 | Integrated control method for low-temperature smoke pollutants |
| CN113976012A (en) * | 2021-11-09 | 2022-01-28 | 孙丽 | Pollutant detects uses processing apparatus |
| CN216296320U (en) * | 2021-10-13 | 2022-04-15 | 徐州宏达新能源科技有限公司 | Phosphorus pentachloride is agitating unit for preparation |
| CN115121145A (en) * | 2022-06-23 | 2022-09-30 | 安徽尘缘节能环保科技有限公司 | High-concentration explosive organic gas thermal oxidation air premixing explosion-proof system |
| CN115382492A (en) * | 2022-08-23 | 2022-11-25 | 湖北航欧新材料科技有限公司 | Continuous preparation device and preparation method of phosphorus pentachloride |
| CN115646806A (en) * | 2022-11-14 | 2023-01-31 | 深圳市一个玉米科技有限公司 | Multistage sieve separator of processing usefulness is squeezed to maize |
| CN116553497A (en) * | 2023-05-24 | 2023-08-08 | 徐州宏达新能源科技有限公司 | Full-automatic control process for producing high-purity phosphorus pentachloride |
-
2023
- 2023-03-30 CN CN202310324464.7A patent/CN116237006B/en active Active
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1210810A (en) * | 1997-06-06 | 1999-03-17 | 埃勒夫阿托化学有限公司 | Process for manufacture of lithium hexafluorophosphate |
| JP2007069139A (en) * | 2005-09-08 | 2007-03-22 | Yayoi Chemical Industry Co Ltd | Stirring impeller for mixing apparatus |
| CN201437505U (en) * | 2009-07-03 | 2010-04-14 | 中国石油天然气股份有限公司 | Inclined plate chlorine dioxide reactor |
| CN201945216U (en) * | 2010-07-06 | 2011-08-24 | 路辉 | Totally-enclosed channel continuous type centerless pipe spiral baffle heat exchanger |
| CN202107526U (en) * | 2011-06-16 | 2012-01-11 | 江苏大明科技有限公司 | Circulation process system for producing phosphorus oxychloride by pure oxygen oxidation of phosphorus trichloride |
| CN204661329U (en) * | 2015-04-01 | 2015-09-23 | 徐州市建平化工有限公司 | Phosphorus pentachloride production device |
| CN204661328U (en) * | 2015-04-01 | 2015-09-23 | 徐州市建平化工有限公司 | Modified version phosphorus pentachloride production device |
| CN105195064A (en) * | 2015-09-15 | 2015-12-30 | 沅江华龙催化科技有限公司 | Improved reaction and separation synchronous reactor |
| CN108975293A (en) * | 2018-09-11 | 2018-12-11 | 安徽东至广信农化有限公司 | A kind of synthetic method of high purity phosphorus pentachloride |
| CN113941238A (en) * | 2021-03-22 | 2022-01-18 | 青岛大学 | Integrated control method for low-temperature smoke pollutants |
| CN216296320U (en) * | 2021-10-13 | 2022-04-15 | 徐州宏达新能源科技有限公司 | Phosphorus pentachloride is agitating unit for preparation |
| CN113976012A (en) * | 2021-11-09 | 2022-01-28 | 孙丽 | Pollutant detects uses processing apparatus |
| CN115121145A (en) * | 2022-06-23 | 2022-09-30 | 安徽尘缘节能环保科技有限公司 | High-concentration explosive organic gas thermal oxidation air premixing explosion-proof system |
| CN115382492A (en) * | 2022-08-23 | 2022-11-25 | 湖北航欧新材料科技有限公司 | Continuous preparation device and preparation method of phosphorus pentachloride |
| CN115646806A (en) * | 2022-11-14 | 2023-01-31 | 深圳市一个玉米科技有限公司 | Multistage sieve separator of processing usefulness is squeezed to maize |
| CN116553497A (en) * | 2023-05-24 | 2023-08-08 | 徐州宏达新能源科技有限公司 | Full-automatic control process for producing high-purity phosphorus pentachloride |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116237006A (en) | 2023-06-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN116237006B (en) | Energy-saving production device and production method for high-purity phosphorus pentachloride | |
| CN101696038A (en) | Method for preparing carbonyl iron powder in high-pressure circulating way | |
| JP2009544640A (en) | Method for producing α-hydroxycarboxylic acid ester | |
| WO2007145261A1 (en) | Hydrate production apparatus | |
| CN201079737Y (en) | Three-phase internal circulation fluidized bed photocatalysis reactor | |
| CN101613272B (en) | Device for continuously producing esters by atomizing raw materials | |
| CN101948384B (en) | Device and method for preparing medium and high-carbon aliphatic ester by continuous etherification method | |
| CN100393613C (en) | Reactor for synthesizing phosphorus pentachloride | |
| CN103318860B (en) | Phosphorous acid pyrolysis is utilized to produce the method for phosphuret-(t)ed hydrogen | |
| CN100404137C (en) | Industrial reduction method of particle iron-base fischer-tropsch synthesis catalyst | |
| CN101791484A (en) | Film-falling scraping plate type multitubular evaporation concentrator | |
| CN202478617U (en) | Novel falling-film evaporator | |
| CN102229524A (en) | Reaction device for synthesizing levo terpineol | |
| CN201850135U (en) | Hydrogen chloride gas drying device | |
| CN102887884B (en) | Method for producing 2-acetylthiophene with trickle bed reactor | |
| CN101337904B (en) | Synthesis of DMF and device | |
| CN217221502U (en) | Carbonization reaction system of nano calcium carbonate | |
| CN208975758U (en) | A kind of fluidization equipment producing aniline-acetonitrile | |
| CN211913719U (en) | Converter is used in chloroethylene production | |
| CN212700570U (en) | Combined methanol evaporator | |
| CN212669230U (en) | Hydrolysis structure for titanium dioxide production | |
| CN215464285U (en) | Reactor for synthesizing trioxymethylene by fixed bed method | |
| CN103408016B (en) | Prepare method and the fluidized-bed reactor thereof of silicon grain | |
| CN201271578Y (en) | Reactor for continuously synthesizing polyvinyl chloride | |
| CN217568385U (en) | Turnover kettle for synthetic spice production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |