CN117819782A - Comprehensive utilization process and device for O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid - Google Patents
Comprehensive utilization process and device for O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid Download PDFInfo
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- CN117819782A CN117819782A CN202410249827.XA CN202410249827A CN117819782A CN 117819782 A CN117819782 A CN 117819782A CN 202410249827 A CN202410249827 A CN 202410249827A CN 117819782 A CN117819782 A CN 117819782A
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- silicon carbide
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- 239000007788 liquid Substances 0.000 title claims abstract description 145
- 238000004821 distillation Methods 0.000 title claims abstract description 74
- 239000002351 wastewater Substances 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 30
- WQYSXVGEZYESBR-UHFFFAOYSA-N thiophosphoryl chloride Chemical compound ClP(Cl)(Cl)=S WQYSXVGEZYESBR-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 230000008569 process Effects 0.000 title claims abstract description 26
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 88
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 69
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000000926 separation method Methods 0.000 claims abstract description 41
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 57
- 239000000460 chlorine Substances 0.000 claims description 57
- 229910052801 chlorine Inorganic materials 0.000 claims description 57
- 239000000126 substance Substances 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 39
- 238000007667 floating Methods 0.000 claims description 35
- 239000002699 waste material Substances 0.000 claims description 25
- 239000007787 solid Substances 0.000 claims description 24
- 238000002347 injection Methods 0.000 claims description 17
- 239000007924 injection Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 16
- 239000007791 liquid phase Substances 0.000 claims description 15
- 239000012071 phase Substances 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000003921 oil Substances 0.000 claims description 12
- 238000001802 infusion Methods 0.000 claims description 11
- 238000003860 storage Methods 0.000 claims description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 230000003197 catalytic effect Effects 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 6
- 230000007246 mechanism Effects 0.000 claims description 6
- 238000001944 continuous distillation Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 20
- 239000000047 product Substances 0.000 description 14
- 239000002253 acid Substances 0.000 description 10
- 150000003839 salts Chemical class 0.000 description 8
- 238000009423 ventilation Methods 0.000 description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- 230000000670 limiting effect Effects 0.000 description 6
- 239000007790 solid phase Substances 0.000 description 5
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 4
- 235000017491 Bambusa tulda Nutrition 0.000 description 4
- 241001330002 Bambuseae Species 0.000 description 4
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000011425 bamboo Substances 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000011343 solid material Substances 0.000 description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- KMJJJTCKNZYTEY-UHFFFAOYSA-N chloro-diethoxy-sulfanylidene-$l^{5}-phosphane Chemical compound CCOP(Cl)(=S)OCC KMJJJTCKNZYTEY-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 230000010412 perfusion Effects 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 230000032258 transport Effects 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- NQKSCAOXRSORTR-UHFFFAOYSA-N OP(O)(O)=S.Cl Chemical compound OP(O)(O)=S.Cl NQKSCAOXRSORTR-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229960003750 ethyl chloride Drugs 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010850 salt effect Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- -1 sodium chloride Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 150000003463 sulfur Chemical class 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 238000009280 upflow anaerobic sludge blanket technology Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
- C02F1/763—Devices for the addition of such compounds in gaseous form
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of production wastewater treatment, and discloses a comprehensive utilization process and a comprehensive utilization device of O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid, wherein the comprehensive utilization process and the comprehensive utilization device comprise a chlorination reaction kettle, an oil-water separator, a primary distillation refiner, a silicon carbide positive pressure reactor, a solid-liquid separation device and a continuous distiller; and the practicability is strong.
Description
Technical Field
The invention relates to the technical field of production wastewater treatment, in particular to a comprehensive utilization process and a comprehensive utilization device of O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid.
Background
At present, the domestic production process of O, O-dialkyl thiophosphoryl chloride can produce acid waste water in the production process and produce distillation residual liquid in the distillation process. The acidic waste water and the distillation residual liquid mainly contain chemical components of phosphoric acid, hydrochloric acid, phosphate and phosphorus oxychloride. The current treatment mode of the acid wastewater is as follows: adding solid sodium hydroxide into acidic wastewater, adjusting the pH value to 3-4, carrying out oxidation pretreatment by adopting a Fenton oxidation process, then continuously adding alkali for neutralization, adjusting the pH value to 6-8, forming salt-containing wastewater, feeding the salt-containing wastewater into a multi-effect evaporation device to remove salt such as sodium chloride, and after the first dephosphorization by adopting a dephosphorization agent, feeding the wastewater into a UASB high-efficiency anaerobic reactor, after the second dephosphorization, feeding the wastewater into a facultative aerobic treatment device, after the third dephosphorization, feeding the wastewater into a sewage treatment plant in a park, and discharging the wastewater reaching the standard after the treatment. The removed salts are managed according to hazardous waste and entrusted to a qualified third party for disposal. At present, distillation residual liquid is managed according to dangerous waste, and is entrusted to be disposed of by a qualified third party.
The invention discloses a method for treating O, O-diethyl thiophosphoryl chloride distillation raffinate in China patent with the application number of CN200710070720.5, which is characterized in that equimolar chlorine is introduced, a certain amount of fatty alcohol is added into a chlorinated solution, a crude product is quickly distilled out under reduced pressure, and a product is quickly distilled out under high vacuum condition in a rectifying tower. The technology of the invention is simple and convenient to implement, and O, O-diethyl thiophosphoryl chloride can be recovered from ethyl chloride distillation residual liquid in high yield and high purity, thereby changing waste into valuables, increasing income, reducing environmental protection treatment of waste liquid and meeting the requirement of green production.
The invention discloses a waste acid recovery method for treating chlorination distillation residual liquid, which combines a pressure swing distillation process and a salt adding extraction distillation process, and adds salt into a chlorination distillation waste acid, and combines a negative pressure environment to enable hydrochloric acid in the chlorination distillation waste acid to be resolved in a gas form, and then the concentrated hydrochloric acid and the dilute hydrochloric acid are obtained through a heat exchanger and an absorption tower, so that the chlorination distillation waste acid is efficiently recovered and reused, and the aspects of the concentration, the impurity content and the like of the recovered hydrochloric acid meet the index requirements of hydrochloric acid reuse, and the method has the advantages of low energy consumption, simplicity in operation, low running cost and the like, meanwhile, the waste acid recovery method for treating the chlorination distillation residual liquid provided by the invention has the advantages that on one hand, the salt is added into a hydrochloric acid-water system, the salt effect can cause very remarkable influence on vapor-liquid balance of the hydrochloric acid-water system, thereby changing the relative volatility between HCl-H2O components, destroying the original constant boiling composition, and solving the technical problem of secondary pollution caused by the by-product treatment of the chlorination distillation waste acid in the recovery process due to the non-volatility of the salt, and recycling technology can be repeatedly utilized in the recovery process; on the other hand, the reduced pressure distillation is performed based on the difference of the azeotropic points of hydrochloric acid under different pressures, and the purpose of further removing HCl is achieved by changing the rectification pressure. However, the following problems still exist in practical applications, in particular:
1. Although the acid waste liquid and the chlorination distillation residual liquid are treated and utilized, the O, O-dialkyl thiophosphoryl chloride production waste water and the distillation residual liquid cannot be comprehensively treated, and meanwhile, the fixed asset investment is large, the process is complex, the operation cost is high, secondary pollution is generated, the dangerous waste is large in production amount and high in disposal cost, and a plurality of chemical components which can be recycled are changed into wastes, so that social resources are wasted, and the requirements of improving the chemical conversion rate, the atom utilization rate, saving energy, reducing consumption and reducing emission are not met;
2. in the process of treating the acidic waste liquid and the distillation residual liquid, chlorine is required to be added for oxidation reaction, and a certain catalyst is required to be added for reaction, so that stirring can not be realized while feeding materials, and the uniform stability of chlorine supply can not be ensured;
3. in the process of oil-liquid separation, liquid is directly introduced into an oil-liquid separation device, so that liquid fluctuation is large, meanwhile, the oil-liquid separation boundary is not obvious, and the problems of incomplete separation in the oil-liquid separation process and micro-mixing of oil liquid in the classified discharge process are caused;
4. in the acid waste liquid treatment process, effective mixing among all components is not convenient to ensure, meanwhile, the supply range of chlorine is not convenient to control, the full mixing reaction of the chlorine can not be effectively ensured, and resource waste is caused.
Therefore, the invention provides a comprehensive utilization process and a device for O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid to solve the problems.
Disclosure of Invention
Aiming at the situation, in order to overcome the defects of the prior art, the invention provides a comprehensive utilization process and a device for the O, O-dialkyl thiophosphoryl chloride production wastewater and the distillation residual liquid, which effectively solve the problems of comprehensively treating and utilizing the O, O-dialkyl thiophosphoryl chloride production wastewater and the distillation residual liquid, reducing the emission of harmful substances and ensuring the efficient chlorination catalytic treatment of the production wastewater and the distillation residual liquid.
The invention relates to a comprehensive utilization process and a device of O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid, comprising a chlorination reaction kettle, an oil-water separator, a primary distillation refiner, a silicon carbide positive pressure reactor, a solid-liquid separation device and a continuous distiller, wherein a primary infusion tube is connected between the chlorination reaction kettle and the oil-water separator, two symmetrically distributed feeding tubes are connected to the upper side of the chlorination reaction kettle, one ends of the feeding tubes, far away from the chlorination reaction kettle, are connected with a storage cylinder, the chlorination reaction kettle is connected with a chlorine supply device connected to the upper end of the chlorination reaction kettle, and the chlorination reaction kettle is connected with an external waste liquid conveying device;
The oil-water separator is internally and vertically coaxially connected with a lifting floating plate in a sliding manner, an adjusting bin is arranged in the lifting floating plate, the adjusting bin is connected with a liquid inlet pipe connected to the upper end of the lifting floating plate, a liquid through hole is formed in the lifting floating plate, the upper end of the liquid inlet pipe is connected with a liquid inlet valve, the upper end of the lifting floating plate is connected with a first-stage telescopic pipe, the lower end of the first-stage telescopic pipe is arranged at the upper end of the lifting floating plate, a second-stage telescopic pipe penetrates through the lifting floating plate, the lower end of the second-stage telescopic pipe is arranged at the lower end of the lifting floating plate, the second-stage telescopic pipe is connected with a silicon carbide positive pressure reactor through a guide pipe, the guide pipe is connected with a first-stage pump connected to the inside of the silicon carbide positive pressure reactor, and the first-stage telescopic pipe is connected with a second-stage pump arranged inside the first-stage distillation refiner through the guide pipe;
the silicon carbide positive pressure reactor is fixedly connected with a material injection pipe and a chlorine introducing pipe, the material injection pipe is connected with an external feeding device, and the chlorine introducing pipe is connected with an external chlorine supply device;
the solid-liquid separation device is arranged in the continuous distiller, three-stage pumps in the continuous distiller are connected through a guide pipe, and the lower end of the continuous distiller is connected with a silicon carbide membrane component.
Preferably, the silicon carbide positive pressure reactor is internally provided with a lifting air supply disc in a vertically coaxial sliding manner, the lifting air supply disc is in threaded connection with an adjusting reciprocating screw rod rotationally connected in the silicon carbide positive pressure reactor, and the adjusting reciprocating screw rod is connected with an external driving device;
the lifting air supply disc is of a hollow structure, a plurality of through holes are formed in the lifting air supply disc, one-way air vent valves are fixedly connected in the through holes, the one-way air vent valves are communicated with the inside of the lifting air supply disc, lifting corrugated pipes are coaxially and fixedly communicated with the upper end of the lifting air supply disc, and the lifting corrugated pipes are communicated with the chlorine communication pipe.
Preferably, the solid-liquid separation device comprises a guide bent pipe communicated with the lower end of the silicon carbide positive pressure reactor, a separation pipe is fixedly communicated with one end of the guide bent pipe far away from the silicon carbide positive pressure reactor, the separation pipe comprises a filter pipe communicated with the guide bent pipe, the filter pipe is matched with the guide bent pipe, and the filter pipe is in a state of being in a downward-upward direction from the guide bent pipe to one end far away from the guide bent pipe;
The filter tube is characterized in that a material conveying and conveying paddle is rotationally connected inside the guide bent tube, a solid conveying paddle is rotationally connected inside the filter tube, the material conveying and conveying paddle is coaxially and fixedly connected with the solid conveying paddle, the material conveying and conveying paddle is attached to the inner wall of the guide bent tube, the solid conveying paddle is attached to the inner wall of the filter tube, and the solid conveying paddle is connected with an external driving device;
one end of the filter pipe, which is far away from the diversion elbow, is fixedly connected with a discharge elbow, and the lower end of the discharge elbow is fixedly connected with a storage barrel;
the filter tube lower extreme fixedly connected with water conservancy diversion semicircle pipe, the filter tube with water conservancy diversion semicircle pipe between be connected with the arc filter screen, the arc filter screen with the filter tube inner wall cooperate, water conservancy diversion semicircle pipe be close to water conservancy diversion return bend one side pass through the pipe with continuous distiller be linked together, continuous distiller inside be equipped with the quaternary pump.
Preferably, the chlorination reaction kettle is internally and rotatably connected with a vent pipe, a plurality of air ejector pipes are fixedly communicated with the vent pipe, and air ejector check valves are fixedly connected with the air ejector pipes;
The chlorine supply device comprises an air supply box connected to the upper end of the chlorination reaction kettle, the air supply box is rotationally connected with the vent pipe, the upper end of the air supply box is connected with an external air supply device, and the upper end of the vent pipe is connected with a flow meter;
the vent pipe is coaxially and fixedly connected with a driven gear which is rotationally connected with the upper end of the chlorination reaction kettle, a driving gear which is rotationally connected with the chlorination reaction kettle is meshed beside the driven gear, and the driving gear is connected with a driving motor which is connected with the lower end of the air supply box.
Preferably, the feeding pipes are rotationally connected with feeding conveying paddles, and the feeding conveying paddles are attached to the inner walls of the feeding pipes;
and the side of the feeding conveying paddle, which is close to the vent pipe, is coaxially and fixedly connected with a driven bevel gear, and the driven bevel gear is meshed with a driving bevel gear which is coaxially and fixedly connected to the vent pipe.
Preferably, the primary transfer line inside rotate and be connected with the primary transfer rake, the primary transfer rake with the primary transfer line inside laminate mutually, the breather pipe lower extreme run through the chlorination reaction kettle lower extreme, the primary transfer rake with the lower extreme of breather pipe link to each other through bevel gear drive mechanism, the primary transfer line be close to chlorination reaction kettle one end fixedly connected with solenoid valve.
Preferably, an umbrella-shaped shunt is fixedly connected in the oil-water separator, the lower end of the umbrella-shaped shunt is communicated with the primary infusion tube, the upper end face of the umbrella-shaped shunt is fixedly connected with a plurality of shunt tubes, the shunt tubes are communicated with the interior of the umbrella-shaped shunt, and stirring paddles are rotatably connected in the shunt tubes;
the oil-water separator is characterized in that a steady flow screen plate is coaxially and fixedly connected inside the oil-water separator, a buffer screen plate is arranged between the steady flow screen plate and the umbrella-shaped flow dividing plate, and the buffer screen plate is connected with the steady flow screen plate through a spring.
Preferably, the accommodating cylinder is internally connected with a disassembling cylinder in a threaded manner, and the lower end of the disassembling cylinder is fixedly connected with an operation bracelet.
Preferably, the adjusting reciprocating screw is connected with the material conveying paddle through a bevel gear transmission mechanism, and the adjusting reciprocating screw is externally connected with a driving source.
The treatment process of the comprehensive utilization device for the O, O-dialkyl thiophosphoryl chloride production wastewater and the distillation residual liquid comprises the following steps:
step one: firstly, introducing the production wastewater and the distillation waste liquid into the chlorination reaction kettle, and simultaneously adding a chlorination catalytic reactant into the chlorination reaction kettle through the feeding pipe;
Step two: after the chlorination catalytic reaction in the chlorination reaction kettle, the electromagnetic valve is opened, and the reacted liquid is introduced into the oil-water separator through the primary infusion tube;
step three: the liquid entering the oil-water separator is separated into oil phase substances and liquid phase substances after oil liquid is separated, the oil phase substances enter the primary distillation refiner, and the liquid phase substances enter the silicon carbide positive pressure reactor;
step four: then, while inputting the liquid phase substances into the silicon carbide positive pressure reactor, adding an acidified water phase catalyst into the silicon carbide positive pressure reactor through the feeding pipe, and simultaneously, slowly introducing chlorine into the silicon carbide positive pressure reactor through the chlorine introducing pipe;
step five: then, substances treated by the silicon carbide positive pressure reaction kettle enter the filter pipe;
step six: the solid-liquid separation is realized through the filtration of the arc-shaped filter screen in the filter pipe;
step seven: the separated solids are conveyed into the disassembly cylinder for collection, and meanwhile, liquid enters the continuous distiller;
step eight: after the continuous distillation is completed, the distillation residues are separated by the silicon carbide film, and a phosphoric acid product is obtained.
The invention improves the existing treatment device of the production wastewater and the distillation residual liquid generated in the production process of O, O-dialkyl thiophosphoryl chloride, and has the following beneficial effects:
1. the problems that the production wastewater and the distillation residual liquid generated in the production process of O, O-dialkyl thiophosphoryl chloride are effectively and comprehensively treated, the emission of harmful substances is reduced and the utilization rate of resources is improved are effectively solved;
2. the lifting floating plate, the adjusting bin, the primary telescopic pipe, the secondary telescopic pipe, the liquid inlet valve and other structures are arranged, so that the problem that the density of the lifting floating plate is adjusted and is ensured to be between oil-liquid separation densities is effectively solved;
3. the structure of the lifting air supply disc, the adjusting reciprocating screw, the one-way vent valve, the lifting corrugated pipe, the chlorine pipe and the like effectively realize the problems of slowly introducing chlorine and guaranteeing uniform distribution of the chlorine while stirring the liquid in the silicon carbide positive pressure reactor;
4. through setting up breather pipe, jet-propelled check valve, air feed box, driven gear, driving gear's isotructure, realized that chlorination reaction kettle is inside to carry out the omnidirectional and lead to chlorine and carry out the problem of intensive mixing to the reaction process.
Drawings
Fig. 1 is a schematic perspective view of the present invention.
FIG. 2 is a schematic cross-sectional view of the present invention.
Fig. 3 is an enlarged partial schematic view of fig. 2 at a in accordance with the present invention.
Fig. 4 is an enlarged partial schematic view of fig. 2B in accordance with the present invention.
FIG. 5 is a schematic diagram of the internal cross-sectional structure of a silicon carbide positive pressure reactor according to the present invention.
Fig. 6 is an enlarged partial schematic view of fig. 5 at C in accordance with the present invention.
Fig. 7 is an enlarged partial schematic view of fig. 5 at D in accordance with the present invention.
FIG. 8 is a schematic diagram of the internal structure of the oil-water separator of the present invention.
Fig. 9 is an enlarged partial schematic view of fig. 8 at E in accordance with the present invention.
FIG. 10 is a schematic view showing the internal structure of a silicon carbide positive pressure reactor according to the present invention.
FIG. 11 is a process flow diagram of the present invention.
Reference numerals: 1. a chlorination reaction kettle; 2. an oil-water separator; 3. a primary distillation refiner; 4. a silicon carbide positive pressure reactor; 5. a continuous distiller; 6. a primary infusion tube; 7. a feeding pipe; 8. a storage cylinder; 9. lifting the floating plate; 10. adjusting the bin; 11. a liquid inlet pipe; 12. a liquid-permeable hole; 14. a first-stage telescopic pipe; 15. a second-stage telescopic tube; 18. a material injection pipe; 19. a chlorine introducing pipe; 21. lifting the air supply disc; 22. adjusting a reciprocating screw; 23. a through hole; 24. a one-way vent valve; 25. lifting the corrugated pipe; 26. a diversion elbow; 27. a filter tube; 28. a material conveying paddle; 29. solid conveying paddles; 30. a discharge elbow; 31. a storage barrel; 32. a diversion semicircle tube; 33. an arc-shaped filter screen; 35. a vent pipe; 36. a gas lance; 37. an air supply box; 38. a driven gear; 39. a drive gear; 40. a driving motor; 41. a feeding and conveying paddle; 42. a driven bevel gear; 43. driving a bevel gear; 44. a first stage conveying paddle; 45. an umbrella-shaped shunt; 46. a shunt; 47. stirring paddles; 48. a steady flow screen plate; 49. a buffer screen; 50. disassembling the cylinder; 51. the bracelet is operated.
Detailed Description
The foregoing and other features, aspects and advantages of the present invention will become more apparent from the following detailed description of the embodiments with reference to the accompanying drawings, 1-11. The following embodiments are described in detail with reference to the drawings.
Exemplary embodiments of the present invention will be described below with reference to the accompanying drawings.
The invention relates to a comprehensive utilization process and a device of O, O-dialkyl thiophosphoryl chloride production wastewater and distillation raffinate, comprising a chlorination reaction kettle 1, an oil-water separator 2, a primary distillation refiner 3, a silicon carbide positive pressure reactor 4, a solid-liquid separation device and a continuous distiller 5, wherein the chlorination reaction kettle 1 is used for realizing chlorination catalytic treatment of the production wastewater and the distillation raffinate, a primary infusion tube 6 is connected between the chlorination reaction kettle 1 and the oil-water separator 2, a liquid pump is arranged in the primary infusion tube 6 in the embodiment, the liquid in the chlorination reaction kettle 1 is conveyed into the oil-water separator 2 through the liquid pump and the primary infusion tube 6, two symmetrically distributed feeding tubes 7 are connected to the upper side of the chlorination reaction kettle 1, catalysts (catalyst loading 16 mol%) and sodium vanadate (0.2%) are respectively fed into the chlorination reaction kettle 1 through the two feeding tubes 7, one end of the chlorination reaction kettle 7 is far away from the chlorination reaction kettle 1, the catalyst loading 8 is respectively connected with the sodium vanadate (0.2%) and the chlorine storage tube 1 is respectively connected with the chlorine storage device (the chlorine storage device is connected with the chlorine storage device 1) which is used for realizing the continuous loading of the catalyst 1) and the catalyst 1 at the two ends of the two sides of the chlorination reaction kettle 1, the production wastewater and the distillation waste liquid are input into the chlorination reaction kettle 1 through an external waste liquid conveying device, meanwhile, chlorine is supplied to the interior of the chlorination reaction kettle 1 through the chlorine supply device, so that the production wastewater and the distillation waste liquid realize chlorination catalytic reaction in the chlorination reaction kettle 1, the chlorine supply device in the embodiment comprises a guide pipe arranged in the chlorination reaction kettle 1, the other end of the guide pipe is connected with an external air supply device, air is supplied to the interior of the chlorination reaction kettle 1 through the guide pipe, a quantitative catalyst DMSO (catalyst load amount 16 mol%) and sodium vanadate (0.2 mol%) are added into the distillation residual liquid, and after the complete stirring, chlorine is introduced, so that phosphate compounds and polysulfide (chain sulfur) compounds in the distillation residual liquid undergo catalytic chlorination reaction, and the distillation residual liquid is converted into O, O-dialkyl phosphorothioate chloride (the conversion rate is about 78%), sulfur, hydrochloric acid, phosphoric acid and a small amount of catalyst residues.
In order to realize the effective separation of oil with different densities, the oil-water separator 2 is internally provided with a lifting floating plate 9 which is coaxially and slidably connected up and down, the liquid inlet pipe 11 connected to the upper end of the lifting floating plate 9 is communicated with the lifting floating plate 10, the liquid inlet pipe 11 is filled with liquid to the inside of the lifting floating plate 9, the lifting floating plate 9 is provided with a liquid permeable hole 12 which is convenient for the effective control and adjustment of the density of the lifting floating plate 9, the inside of the lifting floating plate 9 is provided with an adjusting bin 10 which is used for filling liquid, the inside of the adjusting bin 10 is filled with liquid by filling liquid into the lifting floating plate 9, the liquid inlet pipe 11 connected to the upper end of the lifting floating plate 9 is connected with a liquid inlet pipe 14 which is connected to the upper end of the lifting floating plate 9 by a valve, the liquid inlet pipe 11 is connected to the upper end of the lifting floating plate 4 by a positive pressure pipe 15 which is connected to the lower end of the silicon carbide guide pipe 4, the air inlet pipe 15 is connected to the upper end of the lifting floating plate 9 by a positive pressure pipe 15, the guide pipe is connected with a secondary pump arranged in the primary distillation refiner 3, liquid above the lifting floating plate 9 is pumped into the silicon carbide positive pressure reactor 4 through the primary telescopic pipe 14, and liquid below the lifting floating plate 9 is pumped into the primary distillation refiner 3 through the secondary telescopic pipe 15.
The silicon carbide positive pressure reactor 4 is fixedly connected with a material injection pipe 18 and a chlorine introducing pipe 19, the material injection pipe 7 is connected with an external feeding device, a water phase catalyst is added into the silicon carbide positive pressure reactor 4 through the material injection pipe 18, the chlorine introducing pipe 19 is connected with an external chlorine supply device, chlorine is introduced into the silicon carbide positive pressure reactor 4 through the chlorine introducing pipe 19, and sulfide substances and other organic matters in a reaction system are all oxidized to generate solid-phase sulfur and liquid-phase products.
The solid-liquid separation device is connected with a three-stage pump arranged in the continuous distiller 5 through a conduit, the solid-liquid separation device in the embodiment is an existing solid-liquid separation device, and is not described in detail herein, the lower end of the continuous distiller 5 is connected with a silicon carbide membrane component, after solid-liquid separation, liquid phase substances enter the continuous distiller 5, reduced pressure distillation is carried out under the negative pressure condition of 750mmhg, and gas phase products are collected to prepare high-quality hydrochloric acid products; heating distillation residues to 185-195 ℃, and separating by a silicon carbide film to obtain phosphoric acid products with the content of more than 80%; about 2% of the organic remainder remains to be disposed of as hazardous waste.
In the embodiment, firstly, the pre-determined catalyst DMSO catalyst loading (16 mol%) and sodium vanadate (0.2 mol%) and production wastewater are put into the chlorination reaction kettle 1 to realize chlorination catalytic treatment of the production wastewater and distillation waste liquid, then the treated liquid enters the oil-water separator 2, and after oil-water separation treatment in the oil-water separator 2, the oil phase O, O-dialkyl thiophosphoryl chloride enters the first-stage distillation refiner 3 to be distilled and refined, so as to prepare a finished product, and meanwhile, the water phase remainder is taken as wastewater to be introduced into the silicon carbide positive pressure reactor 4 to be subjected to subsequent treatment;
simultaneously, an acidified water phase catalyst is added into the silicon carbide positive pressure reactor 4, meanwhile, chlorine is slowly introduced into the silicon carbide positive pressure reactor 4 through the chlorine introducing pipe 19, all thioether substances and other organic matters in a reaction system are oxidized to generate solid-phase sulfur and liquid-phase products, then the solid-phase sulfur and liquid-phase products are separated through the solid-liquid separation device, meanwhile, the liquid-phase products enter the continuous distiller 5 for reduced pressure distillation, further, gas-phase products are collected to prepare high-quality hydrochloric acid products, and distilled residues are treated through a silicon carbide membrane group to separate phosphoric acid products.
In order to stir substances in the silicon carbide positive pressure reactor 4 and ensure that chlorine is slowly and uniformly introduced into the silicon carbide positive pressure reactor 4, the silicon carbide positive pressure reactor 4 is internally and coaxially connected with a lifting air supply disc 21 in a sliding manner up and down, a limiting arc-shaped strip is fixedly connected with the silicon carbide positive pressure reactor 4, the lifting air supply disc 21 is provided with a limiting arc-shaped groove matched with the limiting arc-shaped strip, the lifting air supply disc 21 slides up and down in the silicon carbide positive pressure reactor 4 under the limiting action of the limiting arc-shaped groove and the limiting arc-shaped strip, the lifting air supply disc 21 is in threaded connection with an adjusting reciprocating screw 22 rotationally connected in the silicon carbide positive pressure reactor 4, the adjusting reciprocating screw 22 is connected with an external driving device, and the lifting air supply disc 21 is driven to reciprocate up and down in the rotating process of the adjusting reciprocating screw 22, so that the stirring of liquid in the silicon carbide positive pressure reactor 4 is accelerated;
meanwhile, in order to ensure that chlorine can be uniformly and slowly introduced into the silicon carbide positive pressure reactor 4, the lifting air supply disc 21 is of a hollow structure, a plurality of through holes 23 are formed in the lifting air supply disc 21, one-way vent valves 24 are fixedly connected in the through holes 23, the one-way vent valves 24 are communicated with the inside of the lifting air supply disc 21, so that the chlorine entering the inside of the lifting air supply disc 21 enters the silicon carbide positive pressure reactor 4 through the one-way vent valves 24, lifting corrugated pipes 25 are fixedly communicated with the upper ends of the lifting air supply disc 21 coaxially, the lifting corrugated pipes 25 are communicated with the chlorine introducing pipes 19, the chlorine is supplied to the inside of the lifting air supply disc 21 through the chlorine introducing pipes 19 and the lifting corrugated pipes 25, and simultaneously, the chlorine introducing pipes 19 are connected with flow meters, and the chlorine amount entering the inside of the silicon carbide positive pressure reactor 4 is monitored through the flow meters.
In order to effectively realize solid-liquid separation and simultaneously ensure that different substances can be classified and collected during separation, the solid-liquid separation device comprises a guide bent pipe 26 communicated with the lower end of the silicon carbide positive pressure reactor 4, solid substances and liquid substances processed by the silicon carbide positive pressure reactor 4 enter the guide bent pipe 26, meanwhile, one end of the guide bent pipe 26, which is far away from the silicon carbide positive pressure reactor 4, is fixedly communicated with a separation pipe, the separation pipe comprises a filter pipe 27 communicated with the guide bent pipe 26, the filter pipe 27 is matched with the guide bent pipe 26, solid substances and liquid substances entering the guide bent pipe 26 enter the filter pipe 27, the filter pipe 27 is in a self-downward upward state from one end of the guide bent pipe 26, and the filter pipe 27 is preferentially filled near one end of the guide bent pipe 26 under the inclined state of the filter pipe 27.
The inside rotation of water conservancy diversion return bend 26 be connected with defeated material and carry oar 28, the inside rotation of filter tube 27 be connected with solid and carry oar 29, defeated material carry oar 28 and solid and carry oar 29 coaxial fixed connection, defeated material carry oar 28 with the water conservancy diversion return bend 26 inner wall laminating mutually, solid carry oar 29 with filter tube 27 inner wall laminating mutually, solid carry oar 29 and external drive device link to each other, through defeated material carry oar 28 with solid carry oar 29's rotation, realize the transportation to the material inside water conservancy diversion return bend 26, filter tube 27, guarantee that solid phase material, liquid phase material can get into smoothly inside the filter tube 27, be in the process of solid carry oar 29 rotation realization simultaneously to the inside material of filter tube 27, will pass through the solid phase material after the filtration simultaneously carry out the filter tube 27.
The filter tube 27 keep away from water conservancy diversion return bend 26 one end fixedly connected with row material return bend 30, row material return bend 30 lower extreme fixedly connected with receiving vessel 31, through the transport of solid conveying oar 29, carry the solid material to row material return bend 30 inside, and then fall into receiving vessel 31 inside, realize the collection of solid material and store.
In order to improve the solid-liquid separation effect, effectively collect liquid substance simultaneously, filter tube 27 lower extreme fixedly connected with water conservancy diversion semicircle pipe 32, filter tube 27 with water conservancy diversion semicircle pipe 32 between be connected with arc filter screen 33, arc filter screen 33 with filter tube 27 inner wall cooperate, realize the separation filtration to solid substance and liquid substance through arc filter screen 33, and then guarantee that liquid substance is through arc filter screen 33 get into water conservancy diversion semicircle pipe 32 inside, realize solid-liquid effective separation, water conservancy diversion semicircle pipe 32 be close to water conservancy diversion return bend 26 one side be linked together through pipe and continuous distiller 5, continuous distiller 5 inside be provided with the quaternary pump, through the quaternary pump with the liquid substance in the water conservancy diversion semicircle pipe 32 carry to continuous distiller 5 inside, realize effectively distilling liquid substance through continuous distiller 5 simultaneously.
In order to realize the effective stirring of the reaction substances in the chlorination reaction kettle 1, the chlorine gas supply treatment is realized in the chlorination reaction kettle 1 while stirring, the ventilation pipe 35 is rotationally connected in the chlorination reaction kettle 1, a plurality of air injection pipes 36 are fixedly communicated on the ventilation pipe 35, air injection check valves are fixedly connected on the air injection pipes 36, the air injection pipes 36 are driven to synchronously rotate in the rotation process of the ventilation pipe 35, the effective stirring of the position in the chlorination reaction kettle 1 is realized in the rotation process of the air injection pipes 36, and meanwhile, the chlorine gas supply is realized in the chlorination reaction kettle 1 through the ventilation pipe 35 and the air injection pipes 36.
The chlorine supply device comprises a gas supply box 37 connected to the upper end of the chlorination reaction kettle 1, the gas supply box 37 is rotationally connected with a vent pipe 35, the gas supply to the vent pipe 35 is realized through the gas supply box 37, the upper end of the gas supply box 37 is connected with an external gas supply device, the upper end of the vent pipe 35 is fixedly connected with a flow meter, chlorine is introduced into the gas supply box 37 through the gas supply device, and meanwhile, the detection of the introduced amount of the chlorine is realized through the flow meter.
The device is characterized in that the vent pipe 35 is connected with the driven gear 38 at the upper end of the chlorination reaction kettle 1 in a rotating way, the driven gear 38 is connected with the driven gear 38 in a coaxial and fixed way, the vent pipe 35 is driven to rotate synchronously, the vent pipe 35 rotates to stir substances in the chlorination reaction kettle 1, the driven gear 38 is meshed with the driving gear 39 connected with the chlorination reaction kettle 1 in a rotating way, the driving gear 39 is connected with the driving motor 40 at the lower end of the air supply box 37, the driving motor 40 rotates to drive the driving gear 39 to rotate, and the driving gear 39 rotates to drive the driven gear 38, so that the vent pipe 35 is driven to rotate.
In order to ensure the effective transportation of the materials in the storage cylinder 8, the materials can smoothly enter the chlorination reaction kettle 1, so the feeding pipe 7 is internally and rotatably connected with a feeding transportation paddle 41, the feeding transportation paddle 41 is attached to the inner wall of the feeding pipe 7, and the materials in the feeding pipe 7 are transported to the chlorination reaction kettle 1 through the seasoning transportation paddle.
The material feeding and conveying paddle 41 is coaxially and fixedly connected with a driven bevel gear 42 on one side, close to the vent pipe 35, of the driven bevel gear 42, and a driving bevel gear 43 coaxially and fixedly connected to the vent pipe 35 are meshed, the vent pipe 35 rotates and drives the driving bevel gear 43 to rotate, the driving bevel gear 43 rotates and drives the driven bevel gear 42 to rotate, and the driven bevel gear 42 rotates and drives the corresponding material feeding and conveying paddle 41 to rotate, so that conveying of materials is achieved.
In order to realize that substances after the completion of the reaction in the chlorination reaction kettle 1 are conveyed into the oil-water separator 2, a first-stage conveying paddle 44 is rotatably connected in the first-stage conveying pipe 6, the first-stage conveying paddle 44 is attached to the inside of the first-stage conveying pipe 6, the lower end of the ventilation pipe 35 penetrates through the lower end of the chlorination reaction kettle 1, the lower ends of the first-stage conveying paddle 44 and the ventilation pipe 35 are connected through a bevel gear transmission mechanism, the ventilation pipe 35 rotates to drive the first-stage conveying paddle 44 to synchronously rotate through the bevel gear transmission, further the driving of the first-stage conveying paddle 44 is realized in the rotation process of the driving motor 40, the first-stage conveying pipe 6 is close to one end of the chlorination reaction kettle 1 and is fixedly connected with an electromagnetic valve, and the opening and closing of the electromagnetic valve is used for controlling the opening and closing of the lower end of the chlorination reaction kettle 1 to flow between the oil-water separator 2, so that the unloading control of the chlorination reaction kettle 1 is realized.
When the liquid is supplied to the oil-water separator 2 through the first-stage perfusion tube 6, the liquid level inside the oil-water separator 2 can generate larger fluctuation, so that the oil-water separator 2 is not thoroughly separated, so in the embodiment, the inside of the oil-water separator 2 is fixedly connected with an umbrella-shaped shunt 45, the lower end of the umbrella-shaped shunt 45 is communicated with the first-stage perfusion tube 6, the liquid is slowly slowed down through the umbrella-shaped shunt 45, the upper end surface of the umbrella-shaped shunt 45 is fixedly connected with a plurality of shunt tubes 46, the liquid is uniformly distributed inside the oil-water separator 2 through the shunt tubes 46, the shunt tubes 46 and the inside of the umbrella-shaped shunt 45 are communicated, stirring paddles 47 are all rotationally connected inside the liquid in the process of the inside of the shunt tubes 46, the stirring paddles 47 are driven, the stirring process of the liquid is realized, the stirring of the liquid is further facilitated, the liquid is further prevented from entering the screen plate 48, the flow stabilizing plate is further connected with the liquid through the baffle-plate 48, the baffle-plate 48 is further connected with the liquid-plate 48, and the flow stabilizing plate 48 is effectively prevented from entering the baffle-plate 48, and the baffle-plate 48 is stably connected with the liquid-plate 48, and the liquid is stably-flowing through the baffle-plate 48, and the liquid is stably-separated through the baffle-plate 48.
The inside threaded connection of receiving section of thick bamboo 31 have and dismantle section of thick bamboo 50, dismantlement section of thick bamboo 50 lower extreme fixedly connected with operation bracelet 51, through dismantlement section of thick bamboo 50 collect solid material, convenient to detach transports simultaneously.
The adjusting reciprocating screw 22 is connected with the material conveying and conveying paddle 28 through a bevel gear transmission mechanism, the adjusting reciprocating screw 22 is externally connected with a driving source, the material conveying and conveying paddle 28 is driven to rotate while the adjusting reciprocating screw 22 rotates, so that solid-liquid separation is achieved, meanwhile, an electromagnetic valve is connected between the lower end of the silicon carbide positive pressure reaction kettle and the flow guide bent pipe 26, and the flow direction of liquid inside the silicon carbide positive pressure reactor 4 is controlled through the opening and closing of the electromagnetic valve.
The treatment process of the comprehensive utilization device for the O, O-dialkyl thiophosphoryl chloride production wastewater and the distillation residual liquid comprises the following steps:
step one: firstly, introducing the production wastewater and the distillation waste liquid into the chlorination reaction kettle 1, and simultaneously adding a chlorination catalytic reactant into the chlorination reaction kettle 1 through the feeding pipe 7;
step two: after the chlorination catalytic reaction in the chlorination reaction kettle 1, the electromagnetic valve is opened, and the reacted liquid is introduced into the oil-water separator 2 through the primary infusion tube 6;
Step three: the liquid entering the oil-water separator 2 is separated into oil phase substances and liquid phase substances after oil liquid separation, the oil phase substances enter the primary distillation refiner 3, and the liquid phase substances enter the silicon carbide positive pressure reactor 4;
step four: then, while inputting the liquid phase substances into the silicon carbide positive pressure reactor 4, adding an acidified water phase catalyst into the silicon carbide positive pressure reactor 4 through the feeding pipe 18, and simultaneously slowly introducing chlorine into the silicon carbide positive pressure reactor 4 through the chlorine introducing pipe 19;
step five: then the substances treated by the silicon carbide positive pressure reaction kettle enter the filter tube 27;
step six: the solid-liquid separation is realized through the filtration of the arc-shaped filter screen 33 in the filter pipe 27;
step seven: the separated solids are conveyed into the disassembly cylinder 50 for collection, and meanwhile, liquid enters the continuous distiller 5;
step eight: after the continuous distillation is completed, the distillation residues are separated by the silicon carbide film, and a phosphoric acid product is obtained.
The invention improves the existing comprehensive treatment device of O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid, and effectively solves the problems of converting and utilizing harmful substances in the O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid, saving resources and reducing the discharge of wastes by arranging structures such as a chlorination reaction kettle, an oil-water separator, a primary distillation refiner, a silicon carbide positive pressure reactor, a solid-liquid separation device, a continuous distiller and the like; the lifting floating plate, the adjusting bin, the primary telescopic pipe, the secondary telescopic pipe, the liquid inlet valve and other structures are arranged, so that the problem that the density of the lifting floating plate is adjusted and is ensured to be between oil-liquid separation densities is effectively solved; the structure of the lifting air supply disc, the adjusting reciprocating screw, the one-way vent valve, the lifting corrugated pipe, the chlorine pipe and the like effectively realize the problems of slowly introducing chlorine and guaranteeing uniform distribution of the chlorine while stirring the liquid in the silicon carbide positive pressure reactor; the problems of solid-liquid separation are solved by arranging the structures such as the separating pipe, the diversion bent pipe, the material conveying paddle, the solid conveying paddle and the like; has extremely high universality.
Claims (10)
- The comprehensive utilization device of the O, O-dialkyl thiophosphoryl chloride production wastewater and the distillation residual liquid is characterized by comprising a chlorination reaction kettle (1), an oil-water separator (2), a primary distillation refiner (3), a silicon carbide positive pressure reactor (4), a solid-liquid separation device and a continuous distiller (5), wherein a primary infusion tube (6) is connected between the chlorination reaction kettle (1) and the oil-water separator (2), two symmetrically distributed feeding tubes (7) are connected to the upper side of the chlorination reaction kettle (1), a storage cylinder (8) is connected to one end, far away from the chlorination reaction kettle (1), of each feeding tube (7), the chlorination reaction kettle (1) is connected with a chlorine supply device connected to the upper end of the chlorination reaction kettle (1), and the chlorination reaction kettle (1) is connected with an external waste liquid conveying device;the oil-water separator (2) is internally and vertically coaxially connected with a lifting floating plate (9) in a sliding manner, an adjusting bin (10) is arranged in the lifting floating plate (9), the adjusting bin (10) is communicated with a liquid inlet pipe (11) connected with the upper end of the lifting floating plate (9), a liquid permeable hole (12) is formed in the lifting floating plate (9), the upper end of the liquid inlet pipe (11) is connected with a liquid inlet valve, the upper end of the lifting floating plate (9) is connected with a first-stage telescopic pipe (14), the lower end of the first-stage telescopic pipe (14) is arranged at the upper end of the lifting floating plate (9), a second-stage telescopic pipe (15) penetrates through the lifting floating plate (9), the lower end of the second-stage telescopic pipe (15) is arranged at the lower end of the lifting floating plate (9), the second-stage telescopic pipe (15) is connected with a silicon carbide positive pressure reactor (4) through a guide pipe, the guide pipe is connected with a first-stage pump connected with the first-stage positive pressure reactor (4), and the first-stage telescopic pipe (14) is connected with a first-stage distiller (3) through the guide pipe, and the first-stage distiller (3) is connected with the first-stage distiller (3);The silicon carbide positive pressure reactor (4) is fixedly connected with a material injection pipe (18) and a chlorine introducing pipe (19), the material injection pipe (7) is connected with an external feeding device, and the chlorine introducing pipe (19) is connected with an external chlorine supply device;the solid-liquid separation device is connected with a three-stage pump arranged in the continuous distiller (5) through a guide pipe, and the lower end of the continuous distiller (5) is connected with a silicon carbide membrane component.
- 2. The comprehensive utilization device of O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid according to claim 1, wherein a lifting air supply disc (21) is coaxially and slidingly connected up and down in the silicon carbide positive pressure reactor (4), the lifting air supply disc (21) is in threaded connection with an adjusting reciprocating screw (22) rotatably connected in the silicon carbide positive pressure reactor (4), and the adjusting reciprocating screw (22) is connected with an external driving device;the lifting air supply disc (21) is of a hollow structure, a plurality of through holes (23) are formed in the lifting air supply disc (21), one-way air vent valves (24) are fixedly connected in the through holes (23), the one-way air vent valves (24) are communicated with the inside of the lifting air supply disc (21), lifting corrugated pipes (25) are fixedly communicated with the upper ends of the lifting air supply disc (21) coaxially, and the lifting corrugated pipes (25) are communicated with chlorine communication pipes (19).
- 3. The comprehensive utilization device for the O, O-dialkylthiophosphoryl chloride production wastewater and the distillation residual liquid according to claim 2, wherein the solid-liquid separation device comprises a guide elbow pipe (26) communicated with the lower end of the silicon carbide positive pressure reactor (4), a separation pipe is fixedly communicated with one end of the guide elbow pipe (26) far away from the silicon carbide positive pressure reactor (4), the separation pipe comprises a filter pipe (27) communicated with the guide elbow pipe (26), the filter pipe (27) is matched with the guide elbow pipe (26), the filter pipe (27) is in a state of inclining from bottom to top, and the position of the filter pipe (27) close to one end of the guide elbow pipe (26) is lower than the position of the end far away from the guide elbow pipe (26);the inside of the diversion elbow pipe (26) is rotationally connected with a material conveying and conveying paddle (28), the inside of the filter pipe (27) is rotationally connected with a solid conveying paddle (29), the material conveying and conveying paddle (28) and the solid conveying paddle (29) are coaxially and fixedly connected, the material conveying and conveying paddle (28) is attached to the inner wall of the diversion elbow pipe (26), the solid conveying paddle (29) is attached to the inner wall of the filter pipe (27), and the solid conveying paddle (29) is connected with an external driving device;One end of the filter pipe (27) far away from the guide elbow pipe (26) is fixedly connected with a discharge elbow pipe (30), and the lower end of the discharge elbow pipe (30) is fixedly connected with a storage barrel (31);the utility model discloses a filter tube, including filter tube (27), filter tube (32) between be connected with arc filter screen (33), arc filter screen (33) with filter tube (27) inner wall cooperate, filter tube (32) be close to water conservancy diversion return bend (26) one side pass through the pipe with continuous distillation ware (5) are linked together, continuous distillation ware (5) inside be equipped with the quaternary pump.
- 4. The comprehensive utilization device for the O, O-dialkyl thiophosphoryl chloride production wastewater and the distillation residual liquid according to claim 3, wherein a vent pipe (35) is rotationally connected inside the chlorination reaction kettle (1), a plurality of air injection pipes (36) are fixedly communicated with the vent pipe (35), and an air injection one-way valve is fixedly connected with the air injection pipes (36);the chlorine supply device comprises an air supply box (37) connected to the upper end of the chlorination reaction kettle (1), the air supply box (37) is rotationally connected with the vent pipe (35), the upper end of the air supply box (37) is connected with an external air supply device, and the upper end of the vent pipe (35) is fixedly connected with a flow meter;The device is characterized in that the vent pipe (35) is coaxially and fixedly connected with a driven gear (38) which is rotatably connected with the upper end of the chlorination reaction kettle (1), a driving gear (39) which is rotatably connected with the chlorination reaction kettle (1) is meshed beside the driven gear (38), and the driving gear (39) is connected with a driving motor (40) which is connected with the lower end of the air supply box (37).
- 5. The comprehensive utilization device for the O, O-dialkyl thiophosphoryl chloride production wastewater and the distillation residual liquid according to claim 4 is characterized in that a feeding conveying paddle (41) is rotationally connected in the feeding pipe (7), and the feeding conveying paddle (41) is attached to the inner wall of the feeding pipe (7);and a driven bevel gear (42) is coaxially and fixedly connected to one side of the feeding conveying paddle (41) close to the vent pipe (35), and the driven bevel gear (42) is meshed with a driving bevel gear (43) coaxially and fixedly connected to the vent pipe (35).
- 6. The comprehensive utilization device for O, O-dialkylthiophosphoryl chloride production wastewater and distillation residual liquid according to claim 5, wherein a primary conveying paddle (44) is rotationally connected inside a primary conveying pipe (6), the primary conveying paddle (44) is attached to the inside of the primary conveying pipe (6), the lower end of a vent pipe (35) penetrates through the lower end of the chlorination reaction kettle (1), the lower ends of the primary conveying paddle (44) and the vent pipe (35) are connected through a bevel gear transmission mechanism, and an electromagnetic valve is fixedly connected to one end of the primary conveying pipe (6) close to the chlorination reaction kettle (1).
- 7. The comprehensive utilization device for O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid according to claim 6, wherein an umbrella-shaped shunt (45) is fixedly connected inside the oil-water separator (2), the lower end of the umbrella-shaped shunt (45) is communicated with the primary infusion tube (6), a plurality of shunt tubes (46) are fixedly connected to the upper end surface of the umbrella-shaped shunt (45), the shunt tubes (46) are communicated with the inside of the umbrella-shaped shunt (45), and stirring paddles (47) are rotatably connected inside the shunt tubes (46);the oil-water separator (2) is internally and fixedly connected with a steady flow screen plate (48) in a coaxial manner, a buffer screen plate (49) is arranged between the steady flow screen plate (48) and the umbrella-shaped flow dividing plate, and the buffer screen plate (49) is connected with the steady flow screen plate (48) through springs.
- 8. The comprehensive utilization device for O, O-dialkyl thiophosphoryl chloride production wastewater and distillation residual liquid according to claim 3, wherein the accommodating cylinder (31) is internally connected with a disassembling cylinder (50) in a threaded manner, and the lower end of the disassembling cylinder (50) is fixedly connected with an operation bracelet (51).
- 9. The comprehensive utilization device for the O, O-dialkyl thiophosphoryl chloride production wastewater and the distillation residual liquid according to claim 7, wherein the adjusting reciprocating screw (22) is connected with the material conveying propeller (28) through a bevel gear transmission mechanism, and the adjusting reciprocating screw (22) is externally connected with a driving source.
- The comprehensive utilization process of the O, O-dialkyl thiophosphoryl chloride production wastewater and the distillation residual liquid is characterized in that the comprehensive utilization device of the O, O-dialkyl thiophosphoryl chloride production wastewater and the distillation residual liquid is used, which comprises the following steps:step one: firstly, introducing the production wastewater and the distillation waste liquid into the chlorination reaction kettle (1), and simultaneously adding a chlorination catalytic reactant into the chlorination reaction kettle (1) through the feeding pipe (7);step two: after the chlorination catalytic reaction in the chlorination reaction kettle (1), the electromagnetic valve is opened, and the reacted liquid is introduced into the oil-water separator (2) through the primary infusion tube (6);step three: the liquid entering the oil-water separator (2) is separated into oil phase substances and liquid phase substances after oil liquid is separated, the oil phase substances enter the primary distillation refiner (3), and the liquid phase substances enter the silicon carbide positive pressure reactor (4);Step four: then, while inputting the liquid phase substances into the silicon carbide positive pressure reactor (4), adding an acidified water phase catalyst into the silicon carbide positive pressure reactor (4) through the feeding pipe (18), and simultaneously slowly introducing chlorine into the silicon carbide positive pressure reactor (4) through the chlorine introducing pipe (19);step five: then, the substances treated by the silicon carbide positive pressure reaction kettle enter the filter pipe (27);step six: the solid-liquid separation is realized through the filtration of an arc-shaped filter screen (33) in the filter pipe (27);step seven: the separated solids are conveyed into the disassembly cylinder (50) for collection, and meanwhile, liquid enters the continuous distiller (5);step eight: after the continuous distillation is completed, the distillation residues are separated by the silicon carbide film, and a phosphoric acid product is obtained.
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