CN211645088U - Methyl phosphine dichloride serialization reaction unit - Google Patents
Methyl phosphine dichloride serialization reaction unit Download PDFInfo
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- CN211645088U CN211645088U CN201922360327.0U CN201922360327U CN211645088U CN 211645088 U CN211645088 U CN 211645088U CN 201922360327 U CN201922360327 U CN 201922360327U CN 211645088 U CN211645088 U CN 211645088U
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Abstract
The utility model provides a methyl phosphine dichloride serialization reaction unit, including chloromethane temporary storage device, phosphorus trichloride storage device, catalyst storage device, venturi mixing arrangement, counter-flow heat exchanger, tubular reactor, cyclone, first condenser, first vapour and liquid separator, compressor, second condenser, second vapour and liquid separator and distillation column. The utility model provides a methyl phosphine dichloride serialization reaction unit sets up the counter-current heat exchanger between venturi mixing arrangement and tubular reactor for the high temperature material of accomplishing the reaction in the tubular reactor can carry out the heat transfer with the low temperature solution in the heat transfer pipe, has effectively utilized the heat that produces in the reaction sequence.
Description
Technical Field
The utility model relates to a chemical synthesis equipment technical field especially relates to a methyl phosphine dichloride serialization reaction unit.
Background
The methyl phosphine dichloride is a basic organic phosphine compound with high reaction activity, has wide application field, and can be used as a raw material to synthesize products in the fields of flame retardants, herbicides, medicines, bactericides and the like. The synthesis difficulty of the methyl phosphine dichloride is higher, the methyl phosphine dichloride is mainly applied to the field of herbicides at home at present, and the glufosinate-ammonium is taken as the main raw material. The synthesis of methyl phosphine dichloride mainly comprises the following methods: 1. the method is a composite method taking phosphorus trichloride, aluminum trichloride, chloromethane, a reducing agent and sodium chloride as raw materials, and is long in production period and high in cost, and only a small part of manufacturers use the method; 2. the methylation method takes phosphorus trichloride, metallic aluminum, chloromethane and sodium chloride as raw materials, and because the intermediate methyl aluminum compound is extremely easy to burn and has danger of explosion when meeting water and the like, the method is almost used by no manufacturers at home; 3. the process for producing phosphine dichloride by using methane and phosphorus trichloride as raw materials and carbon tetrachloride, thionyl chloride, sulfone chloride and the like as catalysts through a gas phase method comprises the steps of mixing excessive methane with a mixture of phosphorus trichloride and catalysts according to a certain proportion through a mixer, feeding the mixture into a preheater, feeding the mixture into a reactor, passing through a dust remover, a packed tower, a quencher, a hydrogen chloride decontamination device, a methane drying device and a methane recovery device, and rectifying condensate in the quencher to obtain the phosphine dichloride.
Disclosure of Invention
In order to solve the problems of high energy consumption and high material consumption of gas phase method methyl phosphine dichloride, the utility model provides a continuous reaction device of methyl phosphine dichloride.
The utility model provides a methyl phosphine dichloride serialization reaction unit, including methyl chloride temporary storage device, phosphorus trichloride storage device, catalyst storage device, venturi mixing arrangement, counter-current heat exchanger, tubular reactor, cyclone, first condenser, first vapour and liquid separator, compressor, second condenser, second vapour and liquid separator and distillation column, methyl chloride temporary storage device, phosphorus trichloride storage device, catalyst storage device communicate with venturi mixing arrangement respectively, be equipped with second entry, second export, third entry, third export on the counter-current heat exchanger, the heat exchange tube has been laid to the inside of counter-current heat exchanger, the inlet and the second entry of heat exchange tube communicate, the liquid outlet and the second export of heat exchange tube communicate, the second entry still communicates with the liquid outlet of venturi mixing arrangement, the second export still communicates with the inlet of tubular reactor, the third entry communicates with tubular reactor's liquid outlet, the third export communicates with cyclone, the last fourth export that is equipped with of cyclone, the fourth export communicates with the inlet of first condenser, the liquid outlet and the first vapour and liquid separator intercommunication of first condenser, be equipped with the sixth export on the first vapour and liquid separator, the sixth export communicates with the air inlet of compressor, the gas outlet of compressor and the air inlet of second condenser intercommunication, the liquid outlet and the second vapour and liquid separator intercommunication of second condenser, be equipped with the ninth export on the second vapour and liquid separator, the inlet of ninth export and distillation column communicates, the liquid outlet of distillation column and methyl chloride temporary storage's inlet intercommunication.
The cyclone separator is provided with a fifth outlet, the first gas-liquid separator is provided with a seventh outlet, and the fifth outlet and the seventh outlet are respectively communicated with the fractionating tower.
The hydrogen chloride absorption device is filled with water, an eighth outlet is formed in the second gas-liquid separator, and the eighth outlet is communicated with the hydrogen chloride absorption device.
Further, still include tail gas processing apparatus, place active carbon in the tail gas processing apparatus, be equipped with the tenth export on the hydrogen chloride absorbing device, the tenth export communicates with tail gas processing apparatus.
Furthermore, a methyl chloride pressurization metering device is arranged between the methyl chloride temporary storage device and the Venturi mixing device, and the methyl chloride pressurization metering device pressurizes and meters the methyl chloride.
Further, be equipped with phosphorus trichloride metering device between phosphorus trichloride storage device and the venturi mixing arrangement, phosphorus trichloride metering device measures phosphorus trichloride.
Further, a catalyst metering device is arranged between the catalyst storage device and the venturi mixing device, and the catalyst metering device meters the catalyst.
The utility model provides a beneficial effect that technical scheme brought is: the utility model provides a continuous reaction unit of methyl phosphine dichloride sets up the counter-current heat exchanger between venturi mixing arrangement and tubular reactor, make the high temperature material that finishes the reaction in the tubular reactor can carry on the heat transfer with the low temperature solution in the heat transfer pipe, have effectively utilized the heat that produces in the reaction process; the utility model provides a methyl phosphine dichloride serialization reaction unit sets up the compressor between first vapour and liquid separator and second condenser, has improved the pressure of methyl chloride gas and hydrogen chloride gas, makes the second condenser can be with the gaseous condensation of methyl chloride to the liquid under the lower temperature condition; the utility model provides a methyl phosphine dichloride serialization reaction unit sets up hydrogen chloride absorbing device, can realize hydrogen chloride gas's recycle.
Drawings
FIG. 1 is a schematic structural diagram of a continuous reaction device for methyl phosphine dichloride according to the present invention.
FIG. 2 is a schematic structural diagram of a counter-flow heat exchanger of the continuous reaction device for methyl phosphine dichloride of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, embodiments of the present invention will be further described below with reference to the accompanying drawings.
Referring to fig. 1, an embodiment of the present invention provides a methyl phosphine dichloride continuous reaction device, which includes a methyl chloride pressurization metering device 1, a phosphorus trichloride metering device 2, a catalyst metering device 3, a venturi mixing device 4, a counter-flow heat exchanger 5, a tubular reactor 6, a cyclone separator 7, a first condenser 8, a first gas-liquid separator 9, a compressor 10, a tail gas treatment device 11, a hydrogen chloride absorption device 12, a second condenser 13, a second gas-liquid separator 14, a distillation tower 15, a methyl chloride temporary storage device 16, a fractionation tower 17, a phosphorus trichloride storage device 18, and a catalyst storage device 19.
Methyl chloride temporary storage device 16 is used for storing methyl chloride, methyl chloride pressurization metering device 1 is last to set up first entry 101 and first export 102, first entry 101 passes through the liquid outlet intercommunication of pipeline with methyl chloride temporary storage device 16, methyl chloride pressurization metering device 1 is used for pressurizeing and measuring methyl chloride, phosphorus trichloride storage device 18 stores phosphorus trichloride, the liquid outlet of phosphorus trichloride storage device 18 passes through the pipeline and communicates with the inlet of phosphorus trichloride metering device 2, phosphorus trichloride metering device 2 is used for measuring phosphorus trichloride, catalyst storage device 19 stores the catalyst of reaction, catalyst storage device 19's liquid outlet passes through the pipeline and communicates with the inlet of catalyst metering device 3, catalyst metering device 3 is used for measuring the catalyst.
The liquid outlet of the chloromethane pressurizing and metering device 1, the liquid outlet of the phosphorus trichloride metering device 2 and the liquid outlet of the catalyst metering device 3 are respectively communicated with the Venturi mixing device 4 through pipelines, and the chloromethane, the phosphorus trichloride and the catalyst are mixed in the Venturi mixing device 4.
Here, it should be illustrated that the methyl chloride pressurization metering device 1, phosphorus trichloride metering device 2, catalyst metering device 3 that involve in this embodiment are current structure, and the corresponding metering device that uses when synthesizing methyl phosphine dichloride among the prior art is the utility model discloses well methyl chloride pressurization metering device 1, phosphorus trichloride metering device 2, catalyst metering device 3's specific embodiment, consequently, the utility model discloses no longer describe to its concrete structure and theory of operation.
Venturi mixing arrangement 4 that involves in this embodiment is current structure, and the venturi mixing arrangement that can realize solution mixing among the prior art is the utility model discloses well venturi mixing arrangement 4's specific embodiment, consequently, the utility model discloses no longer describe its concrete structure and theory of operation repeatedly.
Referring to fig. 2, a second inlet 501, a second outlet 502, a third inlet 503 and a third outlet 504 are arranged on the counter-flow heat exchanger 5, a heat exchange tube 505 is arranged inside the counter-flow heat exchanger 5, a liquid inlet of the heat exchange tube 505 is communicated with the second inlet 501, a liquid outlet of the heat exchange tube 505 is communicated with the second outlet 502, the second inlet 501 is communicated with a liquid outlet of the venturi mixing device 4 through a pipeline, the second outlet 502 is communicated with a liquid inlet of the tubular reactor 6 through a pipeline, and the third inlet 503 is communicated with a liquid outlet of the tubular reactor 6 through a pipeline.
The cyclone separator 7 is provided with a fourth inlet 701, a fourth outlet 702 and a fifth outlet 703, the fourth inlet 701 is communicated with the third outlet 504 through a pipeline, the fourth outlet 702 is communicated with a liquid inlet of the first condenser 8 through a pipeline, and the fifth outlet 703 is communicated with the fractionating tower 17 through a pipeline.
The first gas-liquid separator 9 is provided with a fifth inlet 901, a sixth outlet 902 and a seventh outlet 903, the fifth inlet 901 is communicated with a liquid outlet of the first condenser 8 through a pipeline, the sixth outlet 902 is communicated with a gas inlet of the compressor 10 through a pipeline, and the seventh outlet 903 is communicated with the fractionating tower 17 through a pipeline.
An air outlet of the compressor 10 is communicated with an air inlet of the second condenser 13 through a pipeline, a sixth inlet 1401, an eighth outlet 1402 and a ninth outlet 1403 are arranged on the second gas-liquid separator 14, the sixth inlet 1401 is communicated with an liquid outlet of the second condenser 13 through a pipeline, the ninth outlet 1403 is communicated with a liquid inlet of the distillation tower 15 through a pipeline, and a liquid outlet of the distillation tower 15 is communicated with a liquid inlet of the chloromethane temporary storage device 16 through a pipeline.
The hydrogen chloride absorption device 12 is provided with a seventh inlet 1201, a tenth outlet 1202 and an eleventh outlet 1203, the seventh inlet 1201 is communicated with the eighth outlet 1402 through a pipeline, and the tenth outlet 1202 is communicated with the tail gas treatment device 11 through a pipeline.
The working process of the continuous reaction device for methyl phosphine dichloride provided by the embodiment is as follows:
methyl chloride in a methyl chloride temporary storage device 16 flows through a methyl chloride pressurizing and metering device 1 to be pressurized, the pressurized methyl chloride flows into a Venturi mixing device 4, phosphorus trichloride stored in a phosphorus trichloride storage device 18 flows into the Venturi mixing device 4 after flowing through a phosphorus trichloride metering device 2, a catalyst stored in a catalyst storage device 19 flows into the Venturi mixing device 4 after flowing through a catalyst metering device 3, the methyl chloride, the phosphorus trichloride and the catalyst are mixed in the Venturi mixing device 4, the mixed solution flows into a heat exchange tube 505 through a second inlet 501, then flows out through a second outlet 502, then flows into a tubular reactor 6 to be reacted, the reacted high-temperature material flows into a counter-flow heat exchanger 5 through a third inlet 503 to exchange heat with the solution in the heat exchange tube 505, the cooled material flows into a cyclone separator 7 through a third outlet 504 and a fourth inlet 701, the solution in the heat exchange tube 505 is heated and then flows into the tubular reactor 6 through the second outlet 502 to participate in the reaction, the cyclone separator 7 separates the cooled material, the liquid phase part and impurities are intercepted and separated and then flow into the fractionating tower 17 through the fifth outlet 703, the gas phase part flows into the first condenser 8 through the fourth outlet 702, the gas phase part is condensed by the first condenser 8 and then becomes the methyl phosphine dichloride liquid, the phosphorus trichloride liquid, the methyl chloride gas and the hydrogen chloride gas, the methyl phosphine dichloride liquid, the phosphorus trichloride liquid, the methyl chloride gas and the hydrogen chloride gas flow into the first gas-liquid separator 9 for gas-liquid separation, the methyl phosphine dichloride liquid and the phosphorus trichloride liquid flow into the fractionating tower 17 through the seventh outlet 903, the methyl chloride gas and the hydrogen chloride gas flow into the compressor 10 through the sixth outlet 902, the compressor 10 compresses the methyl chloride gas and the hydrogen chloride gas, and the compressed methyl chloride gas flow into the second condenser 13, the methyl chloride gas is condensed by the second condenser 13 and then becomes liquid, methyl chloride liquid and hydrogen chloride gas flow into the second gas-liquid separator 14 for gas-liquid separation, the methyl chloride liquid flows into the distillation tower 15 through the ninth outlet 1403 for distillation, the distilled methyl chloride liquid flows into the methyl chloride temporary storage device 16, the hydrogen chloride gas flows into the hydrogen chloride absorption device 12 through the eighth outlet 1402, water is contained in the hydrogen chloride absorption device 12, the hydrogen chloride gas is absorbed by the water to form a hydrochloric acid solution, the hydrochloric acid solution is discharged through the eleventh outlet 1203, waste gas which is not absorbed by the water is discharged to the tail gas treatment device 11 through the tenth outlet 1202, and activated carbon is placed in the tail gas treatment device 11 and used for adsorbing and purifying the waste gas.
In the fractionating tower 17, phosphorus trichloride and methyl phosphine dichloride are separated by distillation, the phosphorus trichloride obtained after separation is conveyed to a phosphorus trichloride storage device 18 for reuse, and the methyl phosphine dichloride obtained after separation is used for subsequent production.
The counterflow heat exchanger 5 that involves in this embodiment is current structure, and corresponding heat exchanger that can realize countercurrent flow among the prior art is the utility model discloses well counterflow heat exchanger 5's specific embodiment, consequently, the utility model discloses no longer describe its concrete structure and theory of operation repeatedly.
First condenser 8, second condenser 13 that involve in this embodiment are current structure, and the condenser that uses during the synthetic methyl phosphine dichloride among the prior art is the utility model discloses in the concrete embodiment of first condenser 8, second condenser 13, consequently, the utility model discloses no longer describe its concrete structure and theory of operation repeatedly.
First vapour and liquid separator 9, second vapour and liquid separator 14 that involve in this embodiment are current structure, and the vapour and liquid separator that uses during the synthetic methyl phosphine dichloride among the prior art is the utility model discloses well first vapour and liquid separator 9, second vapour and liquid separator 14's specific embodiment, consequently, the utility model discloses no longer describe its specific structure and theory of operation repeatedly.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included within the protection scope of the present invention.
Claims (7)
1. A methyl phosphine dichloride serialization reaction unit, characterized in that, including methyl chloride temporary storage device, phosphorus trichloride storage device, catalyst storage device, venturi mixing arrangement, counter-current heat exchanger, tubular reactor, cyclone, first condenser, first vapour and liquid separator, compressor, second condenser, second vapour and liquid separator and distillation column, methyl chloride temporary storage device, phosphorus trichloride storage device, catalyst storage device communicate with venturi mixing arrangement respectively, be equipped with second entry, second export, third entry, third export on the counter-current heat exchanger, the heat exchange tube is laid to the inside of counter-current heat exchanger, the inlet and the second entry intercommunication of heat exchange tube, the liquid outlet and the second export intercommunication of heat exchange tube, the second entry still communicates with venturi mixing arrangement's liquid outlet, the second export still communicates with tubular reactor's inlet, the third entry communicates with tubular reactor's liquid outlet, third export and cyclone intercommunication, the last fourth export that is equipped with of cyclone, the inlet of fourth export and first condenser communicates, the liquid outlet and the first vapour and liquid separator intercommunication of first condenser, be equipped with the sixth export on the first vapour and liquid separator, the air inlet intercommunication of sixth export and compressor, the gas outlet of compressor and the air inlet intercommunication of second condenser, the liquid outlet and the second vapour and liquid separator intercommunication of second condenser, be equipped with the ninth export on the second vapour and liquid separator, the ninth export communicates with the inlet of distillation column, the liquid outlet of distillation column communicates with chloromethane temporary storage's inlet.
2. The continuous reaction device for phosphine methyldichloride according to claim 1, further comprising a fractionating tower, wherein a fifth outlet is arranged on the cyclone separator, a seventh outlet is arranged on the first gas-liquid separator, and the fifth outlet and the seventh outlet are respectively communicated with the fractionating tower.
3. The continuous reaction device for phosphine methyldichloride according to claim 1, further comprising a hydrogen chloride absorption device, wherein water is contained in the hydrogen chloride absorption device, the second gas-liquid separator is provided with an eighth outlet, and the eighth outlet is communicated with the hydrogen chloride absorption device.
4. The continuous reaction device for phosphine methyldichloride according to claim 3, further comprising a tail gas treatment device, wherein activated carbon is placed in the tail gas treatment device, a tenth outlet is arranged on the hydrogen chloride absorption device, and the tenth outlet is communicated with the tail gas treatment device.
5. The continuous reaction device for methyl phosphine dichloride according to claim 1, wherein a methyl chloride pressurization and metering device is arranged between the methyl chloride temporary storage device and the venturi mixing device, and the methyl chloride pressurization and metering device pressurizes and meters methyl chloride.
6. The continuous reaction device of phosphine methyldichloride according to claim 1, wherein a phosphorus trichloride metering device is arranged between the phosphorus trichloride storage device and the venturi mixing device, and the phosphorus trichloride metering device meters phosphorus trichloride.
7. The continuous reaction device for the phosphine methyldichloride according to claim 1, wherein a catalyst metering device is arranged between the catalyst storage device and the venturi mixing device, and the catalyst metering device meters the catalyst.
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| CN201922360327.0U CN211645088U (en) | 2019-12-24 | 2019-12-24 | Methyl phosphine dichloride serialization reaction unit |
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| CN201922360327.0U CN211645088U (en) | 2019-12-24 | 2019-12-24 | Methyl phosphine dichloride serialization reaction unit |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113680307A (en) * | 2021-09-09 | 2021-11-23 | 金川集团股份有限公司 | Horizontal rotary reaction device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113680307A (en) * | 2021-09-09 | 2021-11-23 | 金川集团股份有限公司 | Horizontal rotary reaction device |
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