CN114849630A - Recycling device and recycling method for dimethylamine in hexazinone production process - Google Patents
Recycling device and recycling method for dimethylamine in hexazinone production process Download PDFInfo
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- CN114849630A CN114849630A CN202210508170.5A CN202210508170A CN114849630A CN 114849630 A CN114849630 A CN 114849630A CN 202210508170 A CN202210508170 A CN 202210508170A CN 114849630 A CN114849630 A CN 114849630A
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- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 title claims abstract description 206
- CAWXEEYDBZRFPE-UHFFFAOYSA-N Hexazinone Chemical compound O=C1N(C)C(N(C)C)=NC(=O)N1C1CCCCC1 CAWXEEYDBZRFPE-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000004064 recycling Methods 0.000 title description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 99
- 238000005485 electric heating Methods 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000011084 recovery Methods 0.000 claims abstract description 23
- 238000009413 insulation Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 157
- 239000007864 aqueous solution Substances 0.000 claims description 56
- 230000007246 mechanism Effects 0.000 claims description 47
- 238000003756 stirring Methods 0.000 claims description 42
- 238000001514 detection method Methods 0.000 claims description 20
- 230000017525 heat dissipation Effects 0.000 claims description 20
- 238000005086 pumping Methods 0.000 claims description 18
- 239000000498 cooling water Substances 0.000 claims description 17
- 239000003814 drug Substances 0.000 claims description 17
- 239000007921 spray Substances 0.000 claims description 17
- 238000005507 spraying Methods 0.000 claims description 13
- 239000002351 wastewater Substances 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 11
- 210000000078 claw Anatomy 0.000 claims description 10
- 239000003651 drinking water Substances 0.000 claims description 8
- 235000020188 drinking water Nutrition 0.000 claims description 8
- 239000005457 ice water Substances 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 5
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 28
- 238000000605 extraction Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 description 8
- IQDGSYLLQPDQDV-UHFFFAOYSA-N dimethylazanium;chloride Chemical compound Cl.CNC IQDGSYLLQPDQDV-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- XHFGWHUWQXTGAT-UHFFFAOYSA-N dimethylamine hydrochloride Natural products CNC(C)C XHFGWHUWQXTGAT-UHFFFAOYSA-N 0.000 description 4
- 239000010842 industrial wastewater Substances 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 4
- 230000000149 penetrating effect Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000013040 rubber vulcanization Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- 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
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
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- 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
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- 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
- C02F2001/007—Processes including a sedimentation step
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical Kinetics & Catalysis (AREA)
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- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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Abstract
The invention discloses a dimethylamine recovery device and a dimethylamine recovery method in a hexazinone production process, wherein an equipment box and a reaction box are fixedly arranged at two ends of the bottom of the inner wall of the equipment box, movable sliding frames are fixed at two ends of the bottom of the equipment box, the output end of an electric cylinder is connected with a telescopic rod through a key groove, the other end of the telescopic rod is fixed with a movable plate, the lower ends of the front side and the rear side of the movable plate are rotatably connected with pulleys, one side of the movable plate is elastically connected with the equipment box through a telescopic spring, a heating box is fixed at the upper end of the movable plate, an electric heating wire is fixedly arranged at one side of the inner wall of the heating box, and a heat insulation plate is fixed at the other side of the inner wall of the heating box. The dimethylamine recovery device in the hexazinone production process has the advantages that the temperature rise of reaction materials can be accelerated to be reduced, the materials can reach a proper reaction temperature more quickly, the reaction time is shortened, and the extraction rate of dimethylamine is improved.
Description
Technical Field
The invention relates to the technical field of dimethylamine recovery, in particular to a device and a method for recovering dimethylamine in a hexazinone production process.
Background
The hexazinone is an organic matter, the chemical formula is C12H20N4O2, white crystalline solid, slightly harmful after being mixed with water, does not allow undiluted or massive products to contact underground water, water channels or sewage systems, if no government permits, does not discharge materials into the surrounding environment, the dimethylamine is an organic matter, the chemical formula is C2H7N, is colorless gas or liquid, has strong unpleasant ammonia odor when in high concentration or compression liquefaction, has the odor of fish oil when in extremely low concentration, and is used for producing medicaments, dyes, pesticides, leather dehairing agents, rubber vulcanization accelerators, rocket propellants and the like;
according to chinese patent No. CN 108752219 a, there is provided a method for recovering dimethylamine hydrochloride from industrial wastewater, the method for recovering dimethylamine hydrochloride comprises the following steps: 1) adjusting the pH value of the industrial wastewater to 7 by using acid; 2) carrying out reduced pressure distillation on the industrial wastewater treated in the step 1) to separate organic matters from water; 3) dissolving an organic matter by using an organic solvent, and cooling to 10-15 ℃ to salt out dimethylamine hydrochloric acid in the organic matter; 4) centrifugally separating and drying the mixture treated in the step 3) to obtain the high-purity dimethylamine hydrochloride. The method has simple flow and mature process, is suitable for industrial utilization, and can be used for treating high-salinity wastewater of hexazinone and even other industries;
the method for recovering dimethylamine hydrochloride from industrial wastewater provided by the patent has the advantages of simple flow and mature process, but the temperature of the existing recovery device in the reaction process is not well controlled, the temperature of the dimethylamine aqueous solution cannot be rapidly raised and lowered, the recovery rate of dimethylamine recovery can be influenced due to untimely temperature regulation, and the recovery rate of dimethylamine can also be adversely affected.
Disclosure of Invention
The invention aims to provide a device and a method for recovering dimethylamine in the production process of hexazinone, which are used for solving the problems that the temperature of the conventional recovery device in the background art is not well controlled in the reaction process, the temperature of a dimethylamine aqueous solution cannot be quickly raised and lowered, the recovery rate of dimethylamine is influenced due to untimely temperature regulation, and the recovery rate of dimethylamine is also adversely influenced.
In order to achieve the purpose, the invention provides the following technical scheme: a dimethylamine recovery device in the production process of hexazinone, which comprises an equipment box and a reaction box,
the electric cylinder is fixedly arranged at two ends of the bottom of the inner wall of the equipment box, the two ends of the bottom of the equipment box are fixedly provided with the movable sliding frames, the output end of the electric cylinder is connected with a telescopic rod through a key groove, the other end of the telescopic rod is fixedly provided with a movable plate, the lower ends of the front side and the rear side of the movable plate are rotatably connected with pulleys, one side of the movable plate is elastically connected with the equipment box through a telescopic spring, the upper end of the movable plate is fixedly provided with a heating box, one side of the inner wall of the heating box is fixedly provided with an electric heating wire, and the other side of the inner wall of the heating box is fixedly provided with a heat insulation plate;
the exhaust funnel is arranged on two sides of the top of the equipment box, the upper ends of two sides of the equipment box are embedded with the air inlet windows, the inner wall of the exhaust funnel is fixedly provided with the mounting rack, the inner wall of the mounting rack is fixedly provided with the heat dissipation motor, and the output end of the heat dissipation motor is connected with the fan through the key slot;
the water outlet pipes are arranged on two sides of the bottom of the inner wall of the reaction box, the upper ends of the water outlet pipes are fixedly communicated with spray pipes, and spray heads are fixedly communicated in an array mode on one side of each spray pipe;
the temperature guide plate is embedded at the upper end of the reaction box, flow guide grooves are longitudinally arrayed on the inner side of the temperature guide plate, a cooling water pipe is spirally fixed on the outer wall of the temperature guide plate, and two ends of the cooling water pipe penetrate through and extend to the outer wall of the equipment box;
the rectifying tower is fixedly arranged on one side of the equipment box, the water outlet end of the rectifying tower is communicated with the top of the reaction box through a water outlet pipe of the rectifying tower, and the water outlet pipe of the rectifying tower extends to the upper end in the reaction box;
and the sedimentation tank is fixedly arranged on the other side of the equipment box, a suction filter is fixedly arranged at the lower end of the sedimentation tank, and a water inlet of the suction filter is communicated with a water outlet of the sedimentation tank through a pipeline.
Further, the bottom of the equipment box is fixed with the support frame, support frame lower extreme one side fixed mounting has a water pump, a water pump water outlet head link up and is fixed with the water outlet house steward, the water outlet pipe lower extreme link up fixed connection with the water outlet house steward, a water pump water inlet head passes through the drinking-water pipe through connection with the reaction box.
Further, support frame lower extreme has agitator motor along a water pump one side fixed mounting, the agitator motor output is connected with the puddler through the keyway, the puddler upper end extends to the reaction box inner wall, and the puddler passes through the bearing rotation with equipment box and reaction box and is connected, the puddler array is fixed with the stirring claw.
Further, the bottom of the reaction box is fixedly provided with a second water pump water pumping pipe along one side of the stirring motor in a penetrating manner, and the second water pump water pumping pipe penetrates through the equipment box and extends to one side of the bottom of the equipment box.
Further, support frame one side fixed mounting has No. two water pumps, No. two water pump drinking-water pipe other ends link up fixed connection with No. two water pump water inlets, No. two water pump water outlets link up and are fixed with No. two water pump outlet pipes, No. two water pump outlet pipe other ends link up fixed connection with settling tank one side upper end.
Further, reaction box inner wall bottom fixed mounting has temperature-detecting mechanism, temperature-detecting mechanism is located No. two water pump drinking-water pipe top one sides, temperature-detecting mechanism includes temperature sensor, treater and display screen, and treater and display screen fixed mounting are in equipment box outer wall front side.
Further, the reaction box is provided with a medicine feeding mechanism along the upper part of the temperature detection mechanism, the number of the medicine feeding mechanisms is two, and the medicine feeding mechanisms are communicated and fixedly connected with the reaction box.
A recovery method of a dimethylamine recovery device in a hexazinone production process comprises the following steps:
the method comprises the following steps: introducing the hexazinone production wastewater containing dimethylamine into a rectifying tower from the water inlet end of the rectifying tower, starting the rectifying tower, rectifying the hexazinone production wastewater containing dimethylamine by the rectifying tower, and obtaining a dimethylamine aqueous solution after rectification;
step two: then introducing a dimethylamine aqueous solution into the reaction box through a water outlet pipe of the rectifying tower, starting a stirring motor, a temperature detection mechanism and an electric heating wire, driving a stirring rod to rotate by an output end of the stirring motor, stirring the dimethylamine aqueous solution by using a stirring claw, controlling the power of the electric heating wire by using the temperature detection mechanism, and controlling the temperature of the dimethylamine aqueous solution to be-20-30 ℃;
step three: dropwise adding concentrated sulfuric acid into the reaction tank through the feeding mechanism on one side, reacting for a period of time, then increasing the power of an electric heating wire, adjusting the temperature of the dimethylamine aqueous solution to 20-100 ℃, and dropwise adding the cyanamide aqueous solution into the reaction tank through the feeding mechanism on the other side;
step four: after reacting for a period of time, closing the electric heating wire, starting the electric cylinder, extending out the output end of the electric cylinder, driving the movable plate at the lower end of the heating box to move in the movable sliding frame, keeping the heating box away from the reaction box, and simultaneously introducing ice water at 0 ℃ into the cooling water pipe;
step five: the method comprises the following steps that a first water pump is started, the first water pump pumps out dimethylamine aqueous solution in a reaction box through a water pumping pipe, dimethylamine aqueous solution is sprayed on a heat conducting plate through a water outlet main pipe, a water outlet pipe, a spraying pipe and a spray head, the heat conducting plate conducts heat conduction on the dimethylamine aqueous solution and ice water in a cooling water pipe, the dimethylamine aqueous solution sprayed on the heat conducting plate is cooled, meanwhile, a heat dissipation motor is started and drives a heat dissipation fan to rotate, air enters from an air inlet window and is discharged through an exhaust funnel, and a temperature detection mechanism controls the dimethylamine aqueous solution to be at 0 ℃ along with spraying and maintains for a period of time;
step six: and then starting a second water pump, introducing the dimethylamine aqueous solution into the precipitation tank through a second water pump water suction pipe and a second water pump water outlet pipe by the second water pump, precipitating for a period of time, and introducing the dimethylamine aqueous solution into a suction filter for suction filtration to obtain the dimethylamine mixed salt.
Compared with the prior art, the invention has the beneficial effects that: the device comprises an electric heating wire, a movable sliding frame, an electric cylinder, a movable plate and a heating box, wherein the electric heating wire is used for heating materials in a reaction box, the movable sliding frame, the electric cylinder, the movable plate and the heating box are used for controlling the distance between the electric heating wire and the reaction box, the materials can keep proper reaction temperature by matching the electric heating wire and the reaction box, the recovery rate of dimethylamine is improved, a cooling water pipe is arranged for cooling a heat guide plate, the heat guide plate is used for carrying out heat exchange on the materials sprayed on the heat guide plate, a water pump is arranged for circularly spraying the materials in the reaction box, a spray pipe is arranged for spraying the materials in the reaction box on the heat guide plate, the cold and heat circulation of the materials in the reaction box is accelerated by matching with the water pump, and an air inlet window, an exhaust funnel and a heat dissipation motor are arranged, the air circulation in the equipment box can be accelerated, the reduction of the temperature of the materials in the reaction box is accelerated, and the materials can reach proper reaction temperature more quickly, the reaction time is shortened, and the extraction rate of dimethylamine is improved;
the rectification tower is used for rectifying the hexazinone production wastewater of dimethylamine, removing impurities, obtaining dimethylamine aqueous solution after rectification, facilitating the subsequent reaction, the stirring motor, the stirring rod and the stirring claw are used for stirring the materials in the reaction box, accelerating the reaction, the temperature detection mechanism is arranged, the device is used for monitoring the temperature of materials in the reaction box in real time to ensure that the temperature of the materials in the reaction box is always at the optimal reaction temperature, the arranged medicine feeding mechanism can conveniently add reaction solution into the reaction box to ensure that the recovery process is kept complete, the arranged water pumping pipe of a second water pump is used for discharging water in the reaction box, the arranged settling tank is used for layering mixed liquid containing dimethylamine mixed salt, the dimethylamine mixed salt is filtered out through a suction filter, so that the filtering efficiency of the dimethylamine mixed salt is accelerated, and the treatment time of the wastewater is further shortened.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a perspective view of the present invention;
FIG. 3 is a perspective view of the temperature guide plate of the present invention;
FIG. 4 is an enlarged view of structure A of the present invention;
FIG. 5 is an enlarged view of the structure B of the present invention.
In the figure: 1. an equipment box; 2. a reaction box; 3. a support frame; 4. a stirring motor; 5. a stirring rod; 6. a stirring claw; 7. a water pump I; 8. a water outlet main pipe; 9. a water outlet pipe; 10. a shower pipe; 11. a temperature detection mechanism; 12. a water pumping pipe; 13. a spray head; 14. a heat conducting plate; 15. a cooling water pipe; 16. an air inlet window; 17. an exhaust funnel; 18. a mounting frame; 19. a heat dissipation motor; 20. a heating box; 21. a heat insulation plate; 22. an electric heating wire; 23. moving the plate; 24. a tension spring; 25. moving the sliding frame; 26. a pulley; 27. an electric cylinder; 28. a medicine feeding mechanism; 29. a rectifying tower; 30. a second water pump; 31. a settling tank; 32. a suction filter; 33. a second water pump pumping pipe; 34. a water outlet pipe of a second water pump; 35. and a water outlet pipe of the rectifying tower.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-5, the present invention provides a technical solution: a recovery unit of dimethylamine in hexazinone production process includes: an equipment box 1 and a reaction box 2,
an electric cylinder 27 fixedly installed at both ends of the bottom of the inner wall of the equipment box 1, and both ends of the bottom of the equipment box 1 are fixed with a movable sliding frame 25, and the output end of the electric cylinder 27 is connected with a telescopic rod through a key slot, and the other end of the telescopic rod is fixed with a movable plate 23, and the lower ends of the front and rear sides of the movable plate 23 are rotatably connected with pulleys 26, and one side of the movable plate 23 is elastically connected with the equipment box 1 through a telescopic spring 24, and the upper end of the movable plate 23 is fixed with a heating box 20, and one side of the inner wall of the heating box 20 is fixedly provided with an electric heating wire 22, and the other side of the inner wall of the heating box 20 is fixed with a heat insulation plate 21, the movable sliding frame 25, the electric cylinder 27, the movable plate 23 and the heating box 20 are arranged for controlling the distance between the electric heating wire 22 and the reaction box 2, the electric heating wire 22 is arranged for heating the materials in the reaction box 2, and the materials can keep a proper reaction temperature by matching with each other, the recovery rate of dimethylamine is improved;
the exhaust funnel 17 is arranged on two sides of the top of the equipment box 1, the upper ends of two sides of the equipment box 1 are embedded with the air inlet windows 16, the mounting frame 18 is fixed on the inner wall of the exhaust funnel 17, the heat dissipation motor 19 is fixedly arranged on the inner wall of the mounting frame 18, the output end of the heat dissipation motor 19 is connected with a fan through a key slot, and the arranged air inlet windows 16, the exhaust funnel 17 and the heat dissipation motor 19 can accelerate air circulation in the equipment box 1, accelerate the reduction of the temperature of materials in the reaction box 2 and enable the materials to reach proper reaction temperature more quickly;
the water outlet pipes 9 are arranged on two sides of the bottom of the inner wall of the reaction box 2, the upper ends of the water outlet pipes 9 are fixedly communicated with the spray pipes 10, the spray heads 13 are fixedly communicated with one side of the spray pipes 10 in an array mode, the arranged spray pipes 10 are used for spraying the materials in the reaction box 2 onto the temperature guide plate 14, and the first water pump 7 is matched to accelerate the cold and hot circulation of the materials in the reaction box 2;
the temperature guide plate 14 is embedded at the upper end of the reaction box 2, flow guide grooves are longitudinally arranged on the inner side of the temperature guide plate 14 in an array mode, a cooling water pipe 15 is spirally fixed on the outer wall of the temperature guide plate 14, two ends of the cooling water pipe 15 penetrate through and extend to the outer wall of the equipment box 1, the arranged cooling water pipe 15 can cool the temperature guide plate 14, and the temperature guide plate 14 is used for carrying out heat exchange on materials sprayed on the temperature guide plate 14, so that the cooling speed of the materials in the reaction box 2 is increased, the reaction time is shortened, and the extraction rate of dimethylamine is improved;
the rectifying tower 29 is fixedly installed on one side of the equipment box 1, the water outlet end of the rectifying tower 29 is communicated with the top of the reaction box 2 through a rectifying tower water outlet pipe 35, the rectifying tower water outlet pipe 35 extends to the upper end inside the reaction box 2, and the rectifying tower 29 is used for rectifying the hexazinone production wastewater of dimethylamine to remove impurities, so that a dimethylamine aqueous solution is obtained after rectification, and subsequent reactions are facilitated;
and the settling tank 31 is fixedly arranged on the other side of the equipment box 1, a suction filter 32 is fixedly arranged at the lower end of the settling tank 31, a water inlet of the suction filter 32 is communicated with a water outlet of the settling tank 31 through a pipeline, the set settling tank 31 is used for layering mixed liquid containing dimethylamine mixed salt, and the dimethylamine mixed salt is filtered out through the suction filter 32, so that the filtering efficiency of the dimethylamine mixed salt is improved, and the treatment time of wastewater is further shortened.
Referring to fig. 1 and 2, a support frame 3 is fixed at the bottom of an equipment box 1, a first water pump 7 is fixedly installed on one side of the lower end of the support frame 3, a water outlet head of the first water pump 7 is fixedly communicated with a water outlet main pipe 8, the lower end of a water outlet pipe 9 is fixedly communicated with the water outlet main pipe 8, a water inlet head of the first water pump 7 is fixedly communicated with a reaction box 2 through a water pumping pipe 12, and the first water pump 7 is used for circularly spraying materials in the reaction box 2;
referring to fig. 1 and 2, a stirring motor 4 is fixedly installed at the lower end of the support frame 3 along one side of a first water pump 7, an output end of the stirring motor 4 is connected with a stirring rod 5 through a key slot, the upper end of the stirring rod 5 extends to the inner wall of the reaction box 2, the stirring rod 5 is rotatably connected with the equipment box 1 and the reaction box 2 through bearings, stirring claws 6 are fixed on the stirring rod 5 in an array manner, and the stirring motor 4, the stirring rod 5 and the stirring claws 6 are arranged to stir materials in the reaction box 2, so that the reaction is accelerated;
referring to fig. 1 and 2, a second water pumping pipe 33 is fixedly arranged at the bottom of the reaction box 2 along one side of the stirring motor 4, the second water pumping pipe 33 penetrates through the equipment box 1 and extends to one side of the bottom of the equipment box 1, and the second water pumping pipe 33 is used for discharging water in the reaction box 2;
referring to fig. 1 and 2, a second water pump 30 is fixedly installed on one side of the support frame 3, the other end of a water pumping pipe 33 of the second water pump is fixedly connected with a water inlet head of the second water pump 30 in a penetrating manner, a water outlet head of the second water pump 30 is fixedly connected with a water outlet pipe 34 of the second water pump in a penetrating manner, the other end of the water outlet pipe 34 of the second water pump is fixedly connected with the upper end of one side of the settling tank 31 in a penetrating manner, and the second water pump 30 is used for pumping the materials in the reaction tank 2 into the settling tank 31, so that the settling tank 31 can further process the materials;
referring to fig. 1 and 2, a temperature detection mechanism 11 is fixedly installed at the bottom of the inner wall of the reaction box 2, the temperature detection mechanism 11 is located on one side of the top of the second water pump water pumping pipe 33, the temperature detection mechanism 11 comprises a temperature sensor, a processor and a display screen, the processor and the display screen are fixedly installed on the front side of the outer wall of the equipment box 1, and the temperature detection mechanism 11 is arranged and used for monitoring the temperature of the materials in the reaction box 2 in real time so that the temperature of the materials in the reaction box 2 is always at the optimal reaction temperature;
referring to fig. 1 and 2, a medicine feeding mechanism 28 is disposed above the temperature detection mechanism 11 of the reaction box 2, the number of the medicine feeding mechanisms 28 is two, the medicine feeding mechanism 28 is fixedly connected with the reaction box 2, and the disposed medicine feeding mechanism 28 can conveniently add reaction solution into the reaction box 2, so that the recovery process is kept complete.
A recovery method of a dimethylamine recovery device in a hexazinone production process comprises the following steps:
the method comprises the following steps: introducing the hexazinone production wastewater containing dimethylamine into a rectifying tower 29 from the water inlet end of the rectifying tower 29, starting the rectifying tower 29, rectifying the hexazinone production wastewater containing dimethylamine by the rectifying tower 29 to obtain a dimethylamine aqueous solution after rectification;
step two: then introducing a dimethylamine aqueous solution into the reaction box 2 through a water outlet pipe 35 of the rectifying tower, starting the stirring motor 4, the temperature detection mechanism 11 and the electric heating wire 22, driving the stirring rod 5 to rotate by the output end of the stirring motor 4, stirring the dimethylamine aqueous solution by using the stirring claw 6, controlling the power of the electric heating wire 22 by using the temperature detection mechanism 11, and controlling the temperature of the dimethylamine aqueous solution to be-20-30 ℃;
step three: dropwise adding concentrated sulfuric acid into the reaction box 2 through the feeding mechanism 28 on one side, reacting for a period of time, then increasing the power of the electric heating wire 22, adjusting the temperature of the dimethylamine aqueous solution to 20-100 ℃, and dropwise adding the cyanamide aqueous solution into the reaction box 2 through the feeding mechanism on the other side;
step four: after reacting for a period of time, closing the electric heating wire 22, starting the electric cylinder 27, extending the output end of the electric cylinder 27, driving the movable plate 23 at the lower end of the heating box 20 to move in the movable sliding frame 25, keeping the heating box 20 away from the reaction box 2, and simultaneously introducing ice water at 0 ℃ into the cooling water pipe 15;
step five: the first water pump 7 is turned on, the first water pump 7 pumps the dimethylamine aqueous solution in the reaction box 2 through the water pumping pipe 12, dimethylamine aqueous solution is sprayed on the temperature guide plate 14 through the water outlet main pipe 8, the water outlet pipe 9, the spray pipe 10 and the spray head 13, the temperature guide plate 14 conducts heat on the dimethylamine aqueous solution and ice water in the cooling water pipe 15, the dimethylamine aqueous solution sprayed on the temperature guide plate 14 is cooled, meanwhile, the heat dissipation motor 19 is turned on, the heat dissipation motor 19 drives the heat dissipation fan to rotate, so that air enters from the air inlet window 16 and is discharged through the exhaust pipe 17, and the temperature detection mechanism 11 controls the dimethylamine aqueous solution to be at 0 ℃ for a period of time along with the spraying;
step six: and then, starting the second water pump 30, introducing the dimethylamine aqueous solution into the precipitation tank 31 through the second water pump water suction pipe 33 and the second water pump water outlet pipe 34 by the second water pump 30, precipitating for a period of time, and then introducing the dimethylamine aqueous solution into the suction filter 32 for suction filtration, thereby obtaining the dimethylamine mixed salt.
The working principle is as follows: introducing hexazinone production wastewater containing dimethylamine into a rectifying tower 29 from a water inlet end of the rectifying tower 29, starting the rectifying tower 29, rectifying the hexazinone production wastewater containing dimethylamine by the rectifying tower 29 to obtain dimethylamine aqueous solution after rectification, introducing the dimethylamine aqueous solution into a reaction box 2 through a water outlet pipe 35 of the rectifying tower, starting a stirring motor 4, a temperature detection mechanism 11 and an electric heating wire 22, driving an output end of the stirring motor 4 to rotate a stirring rod 5, stirring the dimethylamine aqueous solution by using a stirring claw 6, controlling the power of the electric heating wire 22 by using the temperature detection mechanism 11, controlling the temperature of the dimethylamine aqueous solution to be-20-30 ℃, dropwise adding concentrated sulfuric acid into the reaction box 2 by using a medicine feeding mechanism 28 on one side, reacting for a period of time, increasing the power of the electric heating wire 22, regulating the temperature of the dimethylamine aqueous solution to be 20-100 ℃, dropwise adding a cyanamide aqueous solution into the reaction box 2 by using a medicine feeding mechanism on the other side, after reacting for a period of time, closing the electric heating wire 22, starting the electric cylinder 27, extending the output end of the electric cylinder 27, driving the moving plate 23 at the lower end of the heating box 20 to move in the moving sliding frame 25, keeping the heating box 20 away from the reaction box 2, simultaneously introducing ice water of 0 ℃ into the cooling water pipe 15, opening the water pump 7, pumping out the dimethylamine aqueous solution in the reaction box 2 by the water pump 7 through the water pumping pipe 12, spraying the dimethylamine aqueous solution on the temperature guide plate 14 through the water outlet header pipe 8, the water outlet pipe 9, the spraying pipe 10 and the spray head 13, carrying out heat conduction on the dimethylamine aqueous solution and the ice water in the cooling water pipe 15 by the temperature guide plate 14, cooling the dimethylamine aqueous solution on the temperature guide plate 14 through spraying, simultaneously, starting the heat dissipation motor 19, driving the heat dissipation motor 19 to rotate the heat dissipation fan, enabling air to enter from the air inlet window 16, then being discharged through the exhaust pipe 17 along with the spraying, the temperature detection mechanism 11 controls the dimethylamine aqueous solution to be at 0 ℃ for a period of time, then the second water pump 30 is started, the second water pump 30 pumps the dimethylamine aqueous solution into the precipitation tank 31 through the second water pump pumping pipe 33 and the second water pump discharging pipe 34, and after a period of precipitation, the dimethylamine aqueous solution is pumped into the suction filter 32 for suction filtration, so that the dimethylamine mixed salt is obtained.
Those not described in detail in this specification are within the skill of the art.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The utility model provides a recovery unit of dimethylamine in hexazinone production process, includes equipment box (1) and reaction box (2), its characterized in that:
the electric air cylinders (27) are fixedly installed at two ends of the bottom of the inner wall of the equipment box (1), the two ends of the bottom of the equipment box (1) are fixedly provided with movable sliding frames (25), the output ends of the electric air cylinders (27) are connected with telescopic rods through key slots, the other ends of the telescopic rods are fixedly provided with movable plates (23), the lower ends of the front side and the rear side of each movable plate (23) are rotatably connected with pulleys (26), one sides of the movable plates (23) are elastically connected with the equipment box (1) through telescopic springs (24), the upper ends of the movable plates (23) are fixedly provided with heating boxes (20), one sides of the inner walls of the heating boxes (20) are fixedly provided with electric heating wires (22), and the other sides of the inner walls of the heating boxes (20) are fixedly provided with heat insulation plates (21);
the air exhausting cylinder (17) is arranged on two sides of the top of the equipment box (1), air inlet windows (16) are embedded in the upper ends of the two sides of the equipment box (1), a mounting frame (18) is fixed on the inner wall of the air exhausting cylinder (17), a heat dissipation motor (19) is fixedly mounted on the inner wall of the mounting frame (18), and the output end of the heat dissipation motor (19) is connected with a fan through a key slot;
the water outlet pipes (9) are arranged on two sides of the bottom of the inner wall of the reaction box (2), the upper ends of the water outlet pipes (9) are fixedly communicated with the spray pipes (10), and the spray heads (13) are fixedly communicated with one side of each spray pipe (10) in an array manner;
the temperature guide plate (14) is embedded at the upper end of the reaction box (2), flow guide grooves are longitudinally arranged on the inner side of the temperature guide plate (14) in an array mode, a cooling water pipe (15) is spirally fixed on the outer wall of the temperature guide plate (14), and two ends of the cooling water pipe (15) penetrate through and extend to the outer wall of the equipment box (1);
the rectifying tower (29) is fixedly arranged on one side of the equipment box (1), the water outlet end of the rectifying tower (29) is communicated with the top of the reaction box (2) through a rectifying tower water outlet pipe (35), and the rectifying tower water outlet pipe (35) extends to the upper end inside the reaction box (2);
and the sedimentation tank (31) is fixedly arranged on the other side of the equipment box (1), a suction filter (32) is fixedly arranged at the lower end of the sedimentation tank (31), and a water inlet of the suction filter (32) is communicated with a water outlet of the sedimentation tank (31) through a pipeline.
2. The apparatus for recovering dimethylamine during the production of hexazinone according to claim 1, wherein: the utility model discloses a water pump, including equipment box (1), support frame (3) lower extreme one side fixed mounting have water pump (7) No. one, water pump (7) play flood peak link up and is fixed with water header (8), outlet pipe (9) lower extreme link up fixed connection with water header (8), water pump (7) are intake the head and are passed through drinking-water pipe (12) through connection with reaction box (2).
3. The apparatus for recovering dimethylamine during the production of hexazinone according to claim 2, wherein: support frame (3) lower extreme has agitator motor (4) along a water pump (7) one side fixed mounting, agitator motor (4) output is connected with puddler (5) through the keyway, puddler (5) upper end extends to reaction box (2) inner wall, and puddler (5) and equipment box (1) and reaction box (2) rotate through the bearing and be connected, puddler (5) array is fixed with stirring claw (6).
4. The apparatus for recovering dimethylamine during the production of hexazinone according to claim 3, wherein: reaction box (2) bottom is link up along agitator motor (4) one side and is fixed with No. two water pump drinking-water pipes (33), No. two water pump drinking-water pipes (33) run through equipment box (1) and extend to equipment box (1) bottom one side.
5. The apparatus for recovering dimethylamine during the production of hexazinone according to claim 4, wherein: support frame (3) one side fixed mounting has No. two water pumps (30), No. two water pump drinking-water pipe (33) other ends and No. two water pumps (30) are intake the head and are link up fixed connection, No. two water pumps (30) are gone out the water head and are link up and be fixed with No. two water pump outlet pipe (34), No. two water pump outlet pipe (34) other ends link up fixed connection with setting tank (31) one side upper end.
6. The apparatus for recovering dimethylamine during the production of hexazinone according to claim 5, wherein: reaction box (2) inner wall bottom fixed mounting has temperature-detecting mechanism (11), temperature-detecting mechanism (11) are located No. two water pump drinking-water pipes (33) top one side, temperature-detecting mechanism (11) include temperature sensor, treater and display screen, and treater and display screen fixed mounting are in equipment box (1) outer wall front side.
7. The apparatus for recovering dimethylamine during the production of hexazinone according to claim 6, wherein: reaction box (2) are provided with into medicine mechanism (28) along temperature-detecting mechanism (11) top, it has two to advance medicine mechanism (28), it link up fixed connection with reaction box (2) to advance medicine mechanism (28).
8. A method for recovering a dimethylamine in a hexazinone production process, which is realized based on the dimethylamine recovery apparatus in the hexazinone production process of claim 7, and comprises the following steps:
the method comprises the following steps: introducing the hexazinone production wastewater containing dimethylamine into a rectifying tower (29) from the water inlet end of the rectifying tower (29), starting the rectifying tower (29), rectifying the hexazinone production wastewater containing dimethylamine by the rectifying tower (29), and obtaining a dimethylamine aqueous solution after rectification;
step two: then introducing a dimethylamine aqueous solution into the reaction box (2) through a water outlet pipe (35) of the rectifying tower, starting the stirring motor (4), the temperature detection mechanism (11) and the electric heating wire (22), driving the stirring rod (5) to rotate by the output end of the stirring motor (4), stirring the dimethylamine aqueous solution by using the stirring claw (6), controlling the power of the electric heating wire (22) by using the temperature detection mechanism (11), and controlling the temperature of the dimethylamine aqueous solution to be-20-30 ℃;
step three: concentrated sulfuric acid is dripped into the reaction box (2) through the medicine feeding mechanism (28) on one side to react for a period of time, then the power of the electric heating wire (22) is increased, the temperature of the dimethylamine aqueous solution is increased to 20-100 ℃, and the cyanamide aqueous solution is dripped into the reaction box (2) through the medicine feeding mechanism on the other side;
step four: after reacting for a period of time, closing the electric heating wire (22), starting the electric cylinder (27), extending the output end of the electric cylinder (27), driving the moving plate (23) at the lower end of the heating box (20) to move in the moving sliding frame (25), keeping the heating box (20) away from the reaction box (2), and simultaneously introducing ice water with the temperature of 0 ℃ into the cooling water pipe (15);
step five: a first water pump (7) is turned on, the first water pump (7) pumps the dimethylamine aqueous solution in the reaction box (2) through a water pumping pipe (12), dimethylamine aqueous solution is sprayed on a heat conducting plate (14) through a water outlet main pipe (8), a water outlet pipe (9), a spraying pipe (10) and a spray head (13), the heat conducting plate (14) conducts heat on the dimethylamine aqueous solution and ice water in a cooling water pipe (15), the dimethylamine aqueous solution sprayed on the heat conducting plate (14) is cooled, meanwhile, a heat dissipation motor (19) is turned on, the heat dissipation motor (19) drives a heat dissipation fan to rotate, air enters from an air inlet window (16) and is discharged through an exhaust pipe (17), and a temperature detection mechanism (11) controls the dimethylamine aqueous solution to be at 0 ℃ for a period of time along with the spraying;
step six: and then starting a second water pump (30), introducing the dimethylamine aqueous solution into a precipitation tank (31) through a second water pump water suction pipe (33) and a second water pump water outlet pipe (34) by the second water pump (30), precipitating for a period of time, and then introducing the dimethylamine aqueous solution into a suction filter (32) for suction filtration, thereby obtaining the dimethylamine mixed salt.
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