CN117326720B - Phthalic anhydride chlorination wastewater treatment and recycling device and method - Google Patents
Phthalic anhydride chlorination wastewater treatment and recycling device and method Download PDFInfo
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- CN117326720B CN117326720B CN202311193248.XA CN202311193248A CN117326720B CN 117326720 B CN117326720 B CN 117326720B CN 202311193248 A CN202311193248 A CN 202311193248A CN 117326720 B CN117326720 B CN 117326720B
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- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 title claims abstract description 36
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 35
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 24
- 238000004064 recycling Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 149
- 238000006243 chemical reaction Methods 0.000 claims abstract description 104
- 238000007789 sealing Methods 0.000 claims abstract description 45
- 238000005303 weighing Methods 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 230000001502 supplementing effect Effects 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims description 43
- 239000006185 dispersion Substances 0.000 claims description 18
- 239000002351 wastewater Substances 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 16
- 238000003860 storage Methods 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 11
- 229910000564 Raney nickel Inorganic materials 0.000 claims description 11
- 238000004821 distillation Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 238000006722 reduction reaction Methods 0.000 claims description 11
- 230000003197 catalytic effect Effects 0.000 claims description 10
- 238000007790 scraping Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000006052 feed supplement Substances 0.000 claims description 7
- 230000005389 magnetism Effects 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 238000003916 acid precipitation Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000020477 pH reduction Effects 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 230000001360 synchronised effect Effects 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims description 2
- 238000005259 measurement Methods 0.000 abstract description 5
- 230000009469 supplementation Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 10
- 230000007246 mechanism Effects 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000008187 granular material Substances 0.000 description 6
- 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
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000011425 bamboo Substances 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 239000013589 supplement Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- BTTRMCQEPDPCPA-UHFFFAOYSA-N 4-chlorophthalic anhydride Chemical compound ClC1=CC=C2C(=O)OC(=O)C2=C1 BTTRMCQEPDPCPA-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000007868 Raney catalyst Substances 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000006114 decarboxylation reaction Methods 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction 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
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
-
- 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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Crystallography & Structural Chemistry (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention relates to the technical field of wastewater treatment, in particular to a phthalic anhydride chlorination wastewater treatment and recycling device and method, comprising a reaction kettle, wherein the top and the bottom of the reaction kettle are respectively provided with a sealing cover plate and a reaction output pipe, and the device further comprises: the central traction shaft is vertically arranged in the reaction kettle, a central sliding sleeve is rotatably connected with the center of the sealing cover plate, and the central traction shaft is in sliding connection with the sealing cover plate through the central sliding sleeve. According to the invention, the catalyst filter disc at the bottom side of the inside of the reaction kettle can be pulled to move upwards through the central pulling shaft so as to filter the internal liquid to separate the catalyst, and then the catalyst filter disc can be hung on the weighing press ring to be weighed through the weighing pressure gauge so as to measure the weight of the catalyst in the catalyst filter disc, so that the catalyst can be conveniently supplemented with the required catalyst through the vertical supplementing pipe according to the loss, the catalyst can be directly filtered and separated in the inside of the reaction kettle, and the measurement and the supplementation are convenient, and the overall reaction treatment efficiency is improved.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a phthalic anhydride chlorination wastewater treatment and recycling device and method.
Background
The 4-chlorophthalic anhydride or the derivative thereof is a main raw material for preparing polyimide monomer 3,3', 4' -biphenyl tetracarboxylic dianhydride, polyimide has a plurality of advantages of wide application temperature, high chemical corrosion resistance and the like, and is widely applied to the fields of aviation, aerospace and the like at present, various key intermediates for preparing polyimide are also in huge market demands, phthalic anhydride is taken as a raw material during production, chlorine or sodium hypochlorite is introduced into the phthalic anhydride for chlorination, wastewater is generated at the moment, the reaction depth of the synthesis process is difficult to control and the selectivity is low, only about 60% of products can be obtained, the remaining 40% of organic impurities are generated, the main pollutants are unreacted phthalic acid, 3-chlorinated products, polychlorinated products and the like, and the wastewater is directly discharged to pollute the environment and is wasted.
The patent with the application number of CN201921306976.6 discloses an organic wastewater degradation catalytic separation device, including diluting mechanism, degradation catalytic separation mechanism, first control module and second control module, diluting mechanism includes diluting case, rabbling mechanism and stirring actuating mechanism, degradation catalytic separation mechanism includes the base support, the separation chamber, catalytic mechanism and aeration mechanism, the separation chamber includes the separation chamber, well degradation catalytic chamber and retrieves the room, be provided with titanium dioxide granule catalyst in retrieving the room, upward be provided with separating mechanism in the separation chamber, it can be to organic wastewater's dilution, and carry out catalytic degradation to diluted organic wastewater, catalytic degradation efficiency has been improved, and can be to titanium dioxide granule catalyst separation recovery.
However, due to migration and aggregation of active components, deposition of pollutants and other reasons, the catalyst still has certain loss after each reaction is finished, so that the catalyst needs to be filtered and separated and taken out for measurement, and then is added into the reactor in a supplementing manner according to the loss amount for the next reaction treatment.
Disclosure of Invention
In view of the above, the invention aims to provide a phthalic anhydride chlorination wastewater treatment and recycling device and method, so as to solve the problems of complex overall operation and reduced reaction treatment efficiency caused by the need of filtering, separating, measuring and supplementing a catalyst after each reaction treatment.
Based on the above purpose, the invention provides a phthalic anhydride chlorination wastewater treatment and recycling device, which comprises a reaction kettle, wherein the top and the bottom of the reaction kettle are respectively provided with a sealing cover plate and a reaction output pipe, and the device further comprises:
the central traction shaft is vertically arranged in the reaction kettle, a central sliding sleeve is rotationally connected to the center of the sealing cover plate, and the central traction shaft is in sliding connection with the sealing cover plate through the central sliding sleeve;
the vertical traction frame is arranged above the sealing cover plate, the top end of the central traction shaft is rotationally connected with the vertical traction frame, a lifting screw sleeve is arranged in the middle of the vertical traction frame, a lifting screw rod is nested on the inner side of the lifting screw sleeve, a lifting motor is arranged at the bottom end of the lifting screw rod, and the lifting motor is fixedly connected with the sealing cover plate;
the catalyst filter disc is embedded and slidingly arranged on the inner side of the reaction kettle, a filter screen is arranged at the bottom of the catalyst filter disc, a central plug bush is arranged at the center of the catalyst filter disc, a central clamping block is arranged at the bottom end of the central traction shaft, the central clamping block and the central plug bush are mutually matched in size, a connecting electromagnet is arranged in the middle of the central clamping block, and a hanging magnet is arranged on the inner side of the central plug bush;
the utility model provides a sealing cover plate, including sealing cover plate, weighing clamping ring, nested set up in the outside of being located the center traction shaft of sealing cover plate top, weighing clamping ring with be provided with weighing manometer between sealing cover plate's the top surface, the outside of weighing clamping ring evenly encircles perpendicularly and is provided with a plurality of traction bars that weigh, weighing traction bar's bottom runs through sealing cover plate connects and is provided with magnetism traction block, weighing clamping ring with magnetism traction block all passes through weighing traction bar with sealing cover plate synchronous sliding connection, the outside of center plug bush is encircleed and is provided with magnetic connection piece, sealing cover plate's the vertical feed supplement pipe that runs through in centre is provided with.
Further, the inside of sealed apron is provided with the cavity and disperses the storehouse, the bottom surface of sealed apron evenly is provided with a plurality of dispersion conveying holes, the outside connection in cavity disperses the storehouse is provided with the reaction conveyer pipe, the top connection of reaction conveyer pipe is provided with balanced blast pipe.
Further, the top of center traction shaft is provided with rotatory snap ring, the center department of vertical traction frame is provided with the traction connection cover, traction connection cover with size mutually support between the rotatory snap ring, the center traction shaft pass through rotatory snap ring with the traction connection cover that vertical traction frame center department set up rotates to be connected, traction connection cover's top is provided with rotatory gear, rotatory gear's outside meshing is provided with stirring gear, stirring gear's axle head is provided with agitator motor.
Further, a plurality of horizontal scraping plates are horizontally connected to the lower portion of the sealing cover plate, the horizontal scraping plates surround the vertical center line of the sealing cover plate in a circumferential mode, and the horizontal scraping plates are parallel to the catalyst filter discs.
Further, a plurality of center connecting sleeves are arranged on the outer side of the center traction shaft, a plurality of stirring blades are uniformly and circumferentially arranged on the outer side of the center connecting sleeve in a surrounding mode, a one-way ratchet wheel is arranged between the center connecting sleeve and the center traction shaft, and the center traction shaft drives the center connecting sleeve to rotate in a one-way mode through the one-way ratchet wheel so as to drive the stirring blades to rotate.
Further, the center connecting sleeves are in nested sliding connection with the center traction shaft, a plurality of center connecting sleeves are uniformly arranged along the vertical central line direction of the center traction shaft, folding stirring pieces are connected between adjacent center connecting sleeves, a distance is reserved between adjacent center connecting sleeves through the folding stirring pieces, a folding rotating shaft is arranged at the center of each folding stirring piece, and a supporting spring is arranged in the middle of each folding rotating shaft.
Further, the top connection of vertical feed supplement pipe is provided with sealed conveying feed bin, the inboard gomphosis of sealed conveying feed bin rotates and is provided with the level delivery tray, the axle head connection of level delivery tray is provided with the delivery motor, the centre of level delivery tray is circumference form evenly and encircles and be provided with a plurality of unit storage barrels, the upper and lower both ends of unit storage barrel are open structure, the top connection of sealed conveying feed bin is provided with vertical conveying pipe, vertical conveying pipe with the mutual misjoint setting of vertical feed supplement pipe, the top connection of vertical conveying pipe is provided with vertical storage silo.
Further, the below connection of catalyst filter disc is provided with the disc breather pipe, the vertical connection of outer end of disc breather pipe is provided with vertical breather pipe, the disc breather pipe is through the trompil of ventilating with inside intercommunication of reation kettle.
Further, the inside of center traction shaft is provided with vertical breather pipe, the bottom of vertical breather pipe is provided with attach fitting, the center department of disc-type breather pipe is provided with the interface of ventilating, attach fitting with correspond each other between the interface of ventilating and set up, when center traction shaft inserted center plug bush and catalyst filter disc interconnect through the center fixture block, attach fitting with interconnect between the interface of ventilating, vertical breather pipe passes through attach fitting with the interface of ventilating with disc-type breather pipe intercommunication each other.
A phthalic anhydride chlorination wastewater treatment and reuse method comprises the following steps:
s1, alkali mixing of raw materials: adding phthalic anhydride chlorination wastewater to be treated into a reaction kettle, adding 3-5%o of auxiliary agent by mass concentration, and adjusting pH=9-10;
s2, catalytic treatment: adding Raney nickel catalyst, and heating the liquid to 50-120 ℃;
s3, introducing hydrogen for reduction: introducing hydrogen into the liquid of the reaction kettle to perform reduction reaction for 1-2h;
s4, filtering and separating: the catalyst filter disc at the bottom side of the inside of the reaction kettle is pulled to move upwards through the central pulling shaft, internal liquid is filtered, raney nickel catalyst particles are intercepted and filtered through the catalyst filter disc, and the catalyst particles are deposited in the catalyst filter disc so as to separate the catalyst;
s5, distillation and concentration: filtering out the catalyst, discharging the liquid from the reaction output pipe to the reaction kettle, and then distilling and concentrating to obtain water about 70%;
s6, acid precipitation and filtration: cooling the liquid after distillation and concentration to below 35 ℃, adding hydrochloric acid for acidification until the pH value is=1-2, and then filtering to obtain the phthalic acid with the purity of more than 99.5%.
The invention has the beneficial effects that: as can be seen from the above, the phthalic anhydride chlorination wastewater treatment and recycling device provided by the invention is characterized in that phthalic anhydride chlorination wastewater is contained in a reaction kettle, the phthalic anhydride chlorination wastewater is treated in the reaction kettle through catalytic reduction reaction of a catalyst, various chlorinated products in the phthalic anhydride chlorination wastewater are decomposed in a reaction manner, after the reaction is completed, a central traction shaft can drag a catalyst filter disc at the inner bottom side of the reaction kettle to move upwards so as to filter internal liquid, raney nickel catalyst particles are intercepted and filtered through the catalyst filter disc, so that the catalyst particles are deposited in the catalyst filter disc to separate the catalyst, the solution can be discharged out of the reaction kettle to carry out subsequent distillation concentration treatment, the catalyst filter disc is pulled to be adsorbed on a magnetic traction block through a magnetic connecting block, the whole catalyst filter disc is connected with a weighing pressure ring, and the catalyst filter disc is weighed through a weighing pressure gauge below the weighing pressure gauge so as to measure the weight of the catalyst in the catalyst filter disc, the catalyst is convenient to directly complete filtration and separation in the reaction kettle according to the loss, the new measurement and the whole reaction supplementing efficiency is improved.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only of the invention and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a schematic view of the internal structure of a reaction vessel according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the front structure of a reaction kettle according to an embodiment of the present invention;
FIG. 3 is a schematic view of a catalyst filter tray according to an embodiment of the present invention in a configuration at the bottom of a reaction vessel;
FIG. 4 is a schematic view of a catalyst filter tray according to an embodiment of the present invention after lifting and filtering;
FIG. 5 is a schematic view of the structure of a center traction axle according to an embodiment of the present invention;
FIG. 6 is a schematic view of a catalyst filter disk according to an embodiment of the present invention;
FIG. 7 is a schematic view showing the structure of a stirring blade according to an embodiment of the present invention;
FIG. 8 is a schematic view of a sealing cover plate according to an embodiment of the present invention;
FIG. 9 is a schematic view of a vertical traction frame according to an embodiment of the present invention;
fig. 10 is a schematic structural view of a sealed conveying bin according to an embodiment of the present invention.
Marked in the figure as:
1. a reaction kettle; 101. a reaction output pipe; 2. sealing the cover plate; 201. a central sliding sleeve; 202. a hollow dispersion bin; 203. dispersing and conveying holes; 204. a reaction delivery pipe; 205. balancing an exhaust pipe; 3. a central traction shaft; 301. a central clamping block; 302. connecting an electromagnet; 303. a rotating clasp; 304. a rotary gear; 4. a vertical traction frame; 401. lifting the screw sleeve; 402. lifting screw rods; 403. a lifting motor; 404. traction connecting sleeve; 405. a stirring motor; 406. a stirring gear; 5. stirring blades; 501. a central connecting sleeve; 502. a one-way ratchet; 503. folding the stirring sheet; 504. folding the rotating shaft; 505. a support spring; 6. a catalyst filter tray; 601. a filter screen; 602. a central plug bush; 603. a suspension magnet; 604. a magnetic connection block; 7. weighing the compression ring; 701. a weighing manometer; 702. a weighing traction rod; 703. a magnetic traction block; 8. a vertical material supplementing pipe; 801. sealing a conveying bin; 802. a horizontal feed tray; 803. a material conveying motor; 804. a unit storage cylinder; 805. a vertical material conveying pipe; 806. a vertical storage bin; 9. a disc-type breather pipe; 901. a vent opening; 902. a vertical vent pipe; 903. a connection joint; 904. a ventilation interface.
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
It is to be noted that unless otherwise defined, technical or scientific terms used herein should be taken in a general sense as understood by one of ordinary skill in the art to which the present invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
As shown in fig. 1, fig. 2, fig. 3, fig. 4, fig. 5, fig. 6, fig. 7, fig. 8 and fig. 9, a phthalic anhydride chlorination wastewater treatment and reuse device, including a reaction kettle 1, the top and the bottom of the reaction kettle 1 are respectively provided with a sealing cover plate 2 and a reaction output pipe 101, and further include:
the central traction shaft 3 is vertically arranged in the reaction kettle 1, a central sliding sleeve 201 is rotatably connected at the center of the sealing cover plate 2, and the central traction shaft 3 is in sliding connection with the sealing cover plate 2 through the central sliding sleeve 201;
the vertical traction frame 4 is arranged above the sealing cover plate 2, the top end of the central traction shaft 3 is rotationally connected with the vertical traction frame 4, a lifting screw sleeve 401 is arranged in the middle of the vertical traction frame 4, a lifting screw 402 is nested on the inner side of the lifting screw sleeve 401, a lifting motor 403 is arranged at the bottom end of the lifting screw 402, and the lifting motor 403 is fixedly connected with the sealing cover plate 2;
the catalyst filter disc 6 is embedded and slidingly arranged on the inner side of the reaction kettle 1, a filter screen 601 is arranged at the bottom of the catalyst filter disc 6, a central plug bush 602 is arranged at the center of the catalyst filter disc 6, a central clamping block 301 is arranged at the bottom end of the central traction shaft 3, the central clamping block 301 and the central plug bush 602 are mutually matched in size, a connecting electromagnet 302 is arranged in the middle of the central clamping block 301, and a hanging magnet 603 is arranged on the inner side of the central plug bush 602;
the weighing press ring 7 is nested to be set up in the outside that is located the central traction shaft 3 of sealed apron 2 top, be provided with weighing manometer 701 between the top surface of weighing press ring 7 and sealed apron 2, the outside of weighing press ring 7 evenly encircles perpendicularly and is provided with a plurality of traction bars 702 of weighing, the bottom of traction bar 702 of weighing is run through sealed apron 2 and is connected and be provided with magnetism traction block 703, weighing press ring 7 and magnetism traction block 703 are all through the synchronous sliding connection of traction bar 702 and sealed apron 2, the outside of center plug bush 602 is encircleed and is provided with magnetism connecting block 604, the vertical feed tube 8 that runs through in centre of sealed apron 2.
In this embodiment, the apparatus accommodates phthalic anhydride chlorination wastewater through the reaction kettle 1, the phthalic anhydride chlorination wastewater is treated by reduction reaction through catalyst catalysis in the reaction kettle 1, so as to decompose various chlorinated products in the phthalic anhydride chlorination wastewater, when the reaction is performed, the catalyst filter disc 6 is positioned at the bottom of the reaction kettle 1, the inside of the reaction kettle 1 is provided with a central traction shaft 3, the central traction shaft 3 is slidably connected with the sealing cover plate 2 through a central sliding sleeve 201, after the reaction is completed, the central traction shaft 3 can move downwards, the central clamping block 301 is embedded into the central plug 602 through the central clamping block 301, and is electrified through the connecting electromagnet 302 to attract a hanging magnet 603 in the central plug 602, the top end of the central traction shaft 3 is rotationally connected with the vertical traction frame 4, the lifting motor 403 can drive the vertical traction frame 4 to move up and down through the lifting screw sleeve 401 and the lifting screw 402, and then drive the central traction shaft 3 to move synchronously, so that the catalyst filter disc 6 at the inner bottom side of the reaction kettle 1 can be pulled through the central traction shaft 3, internal liquid is filtered, the Raney nickel catalyst is intercepted and filtered by the catalyst filter disc 6, the catalyst particles are separated in the catalyst filter disc 6, the catalyst filter disc 6 is separated from the catalyst filter disc 6 at this time, the time is separated from the catalyst filter disc 6, and the catalyst filter disc is separated by the catalyst filter disc 6, and the whole is separated by the catalyst filter disc 6, and the catalyst is separated by the magnetic filter disc 6, and the magnetic filter disc is mutually attached to the magnetic filter disc 6, and the magnetic filter disc is attached to the magnetic disc 4, and the magnetic filter disc is attached to the magnetic filter disc attached to the magnetic disc 4 and the magnetic filter disc 4 and the magnetic disc attached to the magnetic filter frame and the magnetic filter frame is attached to the magnetic filter frame and the magnetic filter frame. The catalyst filter disc 6 is weighed by the weighing pressure gauge 701 below the weighing press ring 7, so that the weight of the catalyst in the catalyst filter disc 6 is measured, the catalyst is convenient to supplement the required catalyst through the vertical feed supplement pipe 8 according to loss, and the catalyst is directly filtered and separated and is measured and supplemented in the reaction kettle 1, thereby being beneficial to improving the overall reaction treatment efficiency.
As shown in fig. 1, fig. 2, fig. 3, fig. 4, fig. 8 and fig. 9, preferably, the top of the reaction kettle 1 is sealed by a sealing cover plate 2, a hollow dispersion bin 202 is arranged in the sealing cover plate 2, a plurality of dispersion conveying holes 203 are uniformly formed in the bottom surface of the sealing cover plate 2, a reaction conveying pipe 204 is connected and arranged on the outer side of the hollow dispersion bin 202, liquid raw materials can be conveyed into the hollow dispersion bin 202 through the reaction conveying pipe 204, then the hollow dispersion bin 202 is uniformly conveyed into the reaction kettle 1 below through the dispersion conveying holes 203, so that the raw materials are uniformly mixed and conveyed, the reaction uniformity and the reaction effect are improved, and when the catalyst filter plate 6 is lifted to the lower part of the sealing cover plate 2, water can be conveyed into the hollow dispersion bin 202 through the reaction conveying pipe 204 and is uniformly sprayed onto the catalyst filter plate 6 below through the dispersion conveying holes 203, so as to wash the catalyst, residual reaction liquid between catalyst residues is avoided, and meanwhile, the top end of the reaction conveying pipe 204 is connected and is provided with a balance exhaust pipe 205 so that the exhaust balance air pressure during the reduction reaction of hydrogen is convenient.
As shown in fig. 1, fig. 2, fig. 3, fig. 4, fig. 5, fig. 6, fig. 8 and fig. 9, preferably, the device drives the central traction shaft 3 to move through the vertical traction frame 4, and then pulls the catalyst filter disc 6 to move through the central traction shaft 3, so as to filter and separate the catalyst from the internal liquid, and the traction connection sleeve 404 arranged at the center of the vertical traction frame 4 through the rotary clamping ring 303 of the central traction shaft 3 is rotationally connected, a rotary gear 304 is arranged above the traction connection sleeve 404, a stirring gear 406 is arranged on the outer side of the rotary gear 304 in a meshed manner, a stirring motor 405 is arranged at the shaft end of the stirring gear 406, the central traction shaft 3 can be driven to rotate through the stirring motor 405, and then the catalyst filter disc 6 in traction connection is driven to synchronously rotate, a plurality of horizontal scraping plates are arranged below the sealing cover plate 2 in a circumferential manner and surround the vertical center line of the sealing cover plate 2, and the horizontal scraping plates and the catalyst filter disc 6 are mutually parallel to each other, so that when the catalyst filter disc 6 moves to the lower part of the horizontal scraping plates, the catalyst filter disc 6 is rotated, the stirring motor is arranged, the catalyst 6 can be uniformly distributed in the horizontal scraping plates 6, and the catalyst is uniformly distributed in the filter disc 6, and the catalyst is conveniently and evenly measured, and the catalyst is well and the weighing is convenient.
As shown in fig. 1, 3, 4, 5 and 7, preferably, a plurality of central connecting sleeves 501 are arranged on the outer side of a central traction shaft 3 of the device, a plurality of stirring blades 5 are uniformly and circumferentially arranged on the outer side of the central connecting sleeve 501 in a surrounding manner, a one-way ratchet wheel 502 is arranged between the central connecting sleeve 501 and the central traction shaft 3, the central traction shaft 3 drives the central connecting sleeve 501 to rotate in a one-way manner through the one-way ratchet wheel 502 so as to drive the stirring blades 5 to rotate, so that the solution in the reaction kettle 1 is stirred, the uniformity and the efficiency of the reaction are improved, the central connecting sleeve 501 cannot be driven to rotate when the central traction shaft 3 rotates reversely due to the one-way transmission of the one-way ratchet wheel 502, the stirring blades 5 are prevented from being clamped, the central connecting sleeve 501 is in nested sliding connection with the central traction shaft 3, a folding stirring piece 503 is arranged between the adjacent central connecting sleeves 501, the center of the folding stirring piece 503 is provided with a folding rotating shaft 504, the middle of the folding rotating shaft 504 is provided with a supporting spring 505, the folding stirring piece 503 can be folded through the folding rotating shaft 504 and kept in an extending state through the supporting spring 505, so that adjacent center connecting sleeves 501 are mutually separated by a distance through the folding stirring piece 503, the stirring range and uniformity are further improved, when the center traction shaft 3 moves upwards, the center connecting sleeves 501 are blocked by the center sliding sleeve 201 to slide downwards, so as to compress the folding stirring piece 503, the folding stirring piece 503 is folded through the folding rotating shaft 504, the blocking of the center traction shaft 3 is avoided, meanwhile, the bottom end of the center traction shaft 3 is provided with a limiting structure, the separation of the center connecting sleeves 501 from the lower end is avoided, meanwhile, the folding stirring piece 503 also rotates along with the center traction shaft 3, the stirring treatment of an internal solution can be carried out, the stirring gap of the stirring blade 5 is filled, further improving the stirring efficiency.
As shown in fig. 1, 2, 3, 4, 8, 9 and 10, preferably, the device can supplement catalyst particles in the catalyst filter disc 6 through the vertical feed supplementing pipe 8, the top end of the vertical feed supplementing pipe 8 is connected with a sealed feed delivering bin 801, the inner side of the sealed feed delivering bin 801 is provided with a horizontal feed delivering disc 802 in a jogged and rotating manner, the shaft end of the horizontal feed delivering disc 802 is connected with a feed delivering motor 803, the middle of the horizontal feed delivering disc 802 is uniformly and circumferentially provided with a plurality of unit feed storing barrels 804 in a surrounding manner, the upper end and the lower end of the unit feed storing barrel 804 are both in an open structure, the upper part of the sealed feed delivering bin 801 is provided with a vertical feed delivering pipe 805, the vertical feed delivering pipe 805 and the vertical feed supplementing pipe 8 are mutually staggered, the top connection of vertical conveying pipeline 805 is provided with vertical storage silo 806 to store required catalyst granule through vertical storage silo 806, catalyst granule is carried downwards through vertical conveying pipeline 805, and conveying motor 803 can drive horizontal delivery tray 802 rotation, make unit storage section of thick bamboo 804 pass through vertical conveying pipeline 805 in proper order under, catalyst granule just gets into in the unit storage section of thick bamboo 804, then the unit storage section of thick bamboo 804 that fills with catalyst granule continues to rotate to vertical feed supplement pipe 8 top, carry downwards through vertical feed supplement pipe 8 and fall into the catalyst and strain, and unit storage section of thick bamboo 804 size is invariable, the single transport catalyst quantity of being convenient for control, and then the catalyst quantity of being convenient for accurate control of supplement.
As shown in fig. 1, 2, 3, 4, 5 and 6, preferably, a disc-shaped breather pipe 9 is connected and arranged below a catalyst filter disc 6 of the device, a plurality of breather holes 901 are uniformly formed in the outer wall of the disc-shaped breather pipe 9 in a penetrating manner, a vertical breather pipe 902 is arranged in the central traction shaft 3, a connecting joint 903 is arranged at the bottom end of the vertical breather pipe 902, a breather port 904 is arranged at the center of the disc-shaped breather pipe 9, the connecting joint 903 and the breather port 904 are correspondingly arranged, when the central traction shaft 3 is inserted into a central plug bush 602 through a central clamping block 301 to be connected with the catalyst filter disc 6, the connecting joint 903 and the breather port 904 are connected with each other, the vertical breather pipe 902 and the breather pipe 904 are communicated with each other through the connecting joint 903, when the reaction treatment is carried out, reducing agent hydrogen can be conveyed through the vertical breather pipe 902 and the disc-shaped breather pipe 9, the hydrogen is evenly conveyed into the reaction kettle 1 through the disc-type breather pipe 9 and the ventilation openings 901 so as to carry out reaction treatment, so that the uniformity of conveying the hydrogen is improved, meanwhile, as the disc-type breather pipe 9 is positioned below the catalyst filter disc 6, bubbles generated by the hydrogen float upwards through the catalyst filter disc 6, and the bubbles are divided into smaller bubbles when passing through the filter screen 601 of the catalyst filter disc 6 so as to improve the contact reaction efficiency of gas and liquid, meanwhile, the bubbles can impact the filter screen 601 of the catalyst filter disc 6 in the rising process of the bubbles, catalyst particles are prevented from being deposited on the filter screen 601, the catalyst is conveniently and evenly dispersed into the reaction kettle 1, the uniformity and the efficiency of the reaction treatment are conveniently improved, after the following disc-type breather pipe 9 moves along the catalyst filter disc 6 to be close to the lower part of the sealing cover plate 2, the water can be conveyed into the hollow dispersion bin 202 through the reaction conveying pipe 204, the water is uniformly sprayed onto the catalyst filter disc 6 below through the dispersion conveying holes 203 to wash the catalyst, and then the drying gas can be conveyed through the disc type breather pipe 9 to be sprayed out through the breather holes 901, so that the catalyst on the catalyst filter disc 6 is dried, and the interference of residual liquid between the catalyst filter disc 6 and the catalyst on the subsequent weighing measurement is avoided.
When in use, corresponding pipelines of the device are connected, liquid raw materials are conveyed into the hollow dispersion bin 202 through the reaction conveying pipe 204, the hollow dispersion bin 202 is uniformly conveyed into the reaction kettle 1 below through the dispersion conveying holes 203, so that the raw materials are uniformly mixed and conveyed into the reaction kettle 1, catalyst particles are added, the catalyst filter disc 6 is kept at the bottom of the reaction kettle 1, meanwhile, the central traction shaft 3 is driven to rotate through the stirring motor 405, the central traction shaft 3 drives the central connecting sleeve 501 to rotate unidirectionally through the unidirectional ratchet 502, the stirring blades 5 are driven to rotate, so that the solution in the reaction kettle 1 is stirred, the uniformity and efficiency of reaction treatment are improved, when the reduction reaction is carried out, the top end of the central traction shaft 3 is rotationally connected with the vertical traction frame 4, the lifting motor 403 drives the vertical traction frame 4 to move up and down through the lifting screw sleeve 401 and the lifting screw 402, and then the central traction shaft 3 is driven to synchronously move, the central traction shaft 3 moves downwards, the central plug bush 602 is embedded through the central clamping block 301, then reducing agent hydrogen is conveyed through the vertical vent pipe 902 and the disc vent pipe 9, the hydrogen is uniformly conveyed into the reaction kettle 1 through the disc vent pipe 9 and the vent holes 901 for reduction reaction treatment, after the reaction treatment is finished, the electromagnet 302 is electrified to attract the hanging magnet 603 in the central plug bush 602, so that the catalyst filter disc 6 at the bottom side of the inner part of the reaction kettle 1 is pulled by the central traction shaft 3 to upwards move for filtering internal liquid, raney nickel catalyst particles are intercepted and filtered through the catalyst filter disc 6, so that the catalyst particles are deposited in the catalyst filter disc 6 for separating catalyst, and then the solution can be discharged out of the reaction kettle 1 for subsequent distillation concentration treatment, the catalyst filter disc 6 is pulled to move to the position close to the position passing through the lower part of the sealing cover plate 2, the magnetic connecting block 604 is adsorbed to the magnetic pulling block 703, then the central pulling shaft 3 is connected with the electromagnet 302 to be powered off and moves upwards so as to be separated from the catalyst filter disc 6, at the moment, the catalyst filter disc 6 is suspended by the magnetic connecting block 604 and the magnetic pulling block 703, the whole catalyst filter disc 6 is connected with the weighing press ring 7, the catalyst filter disc 6 is weighed by the weighing press ring 7 through the weighing press gauge 701 below the weighing press ring 7, the weight of the catalyst in the catalyst filter disc 6 is measured, then the required catalyst is replenished through the vertical replenishing pipe 8 according to the loss, and the catalyst is directly filtered and separated in the reaction kettle 1, and the measurement replenishing is completed.
The application method of the phthalic anhydride chlorination wastewater treatment and reuse device comprises the following steps:
s1, alkali mixing of raw materials: adding phthalic anhydride chlorination wastewater to be treated into a reaction kettle 1, adding 3-5%o of auxiliary agents such as potassium carbonate, and adjusting pH to be 9-10 by alkali;
s2, catalytic treatment: adding Raney nickel catalyst, and heating the liquid to 50-120 ℃;
s3, introducing hydrogen for reduction: introducing hydrogen into the liquid of the reaction kettle 1 to perform reduction reaction for 1-2h;
s4, filtering and separating: the catalyst filter disc 6 at the bottom side in the reaction kettle 1 is pulled by the central pulling shaft 3 to move upwards, internal liquid is filtered, raney nickel catalyst particles are intercepted and filtered by the catalyst filter disc 6, and the catalyst particles are deposited in the catalyst filter disc 6 to separate the catalyst;
s5, distillation and concentration: after filtering out the catalyst, discharging the liquid from the reaction output pipe 101 to the reaction kettle 1, and then carrying out distillation concentration to obtain about 70% of distilled water;
s6, acid precipitation and filtration: cooling the liquid after distillation and concentration to below 35 ℃, adding hydrochloric acid for acidification until the pH value is=1-2, and then filtering to obtain the phthalic acid with the purity of more than 99.5%.
In the method, the catalyst is easy to obtain and can be repeated (1-3% of the catalyst is replaced every time), and the post-treatment is simple. The auxiliary agent plays a key role in the method, the dechlorination of Raney nickel alone is difficult to complete, and a decarboxylation product benzoic acid is easy to generate, so that the defects can be overcome after the auxiliary agent is adopted.
According to the phthalic anhydride chlorination wastewater treatment and recycling device provided by the invention, phthalic anhydride chlorination wastewater is contained in the reaction kettle 1, the phthalic anhydride chlorination wastewater is treated through reduction reaction under catalysis of the catalyst, so that various chlorinated products in the phthalic anhydride chlorination wastewater are decomposed in a reaction way, after the reaction is finished, the central traction shaft 3 can drag the catalyst filter disc 6 at the inner bottom side of the reaction kettle 1 to move upwards, so that internal liquid is filtered, raney nickel catalyst particles are intercepted and filtered through the catalyst filter disc 6, so that the catalyst particles are deposited in the catalyst filter disc 6, so that the catalyst is separated, a solution can be discharged out of the reaction kettle 1 for subsequent distillation concentration treatment, the catalyst filter disc 6 is pulled and adsorbed onto the magnetic traction block 703 through the magnetic connecting block 604, the whole of the catalyst filter disc 6 is connected with the weighing press ring 7, and the weighing press ring 701 below the weighing press ring 7 is used for weighing the catalyst filter disc 6, so that the catalyst in the catalyst filter disc 6 is conveniently supplemented with the required catalyst through the vertical feed pipe 8 according to loss, the whole reaction is directly filtered and the reaction is finished, and the whole reaction efficiency is improved.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of the invention (including the claims) is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the invention, the steps may be implemented in any order and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
The present invention is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the scope of the present invention.
Claims (10)
1. The utility model provides a phthalic anhydride chlorination waste water treatment recycling device, is including reation kettle (1), the top and the bottom of reation kettle (1) are provided with sealed apron (2) and reaction output tube (101) respectively, its characterized in that still includes:
the central traction shaft (3) is vertically arranged in the reaction kettle (1), a central sliding sleeve (201) is rotatably connected to the center of the sealing cover plate (2), and the central traction shaft (3) is in sliding connection with the sealing cover plate (2) through the central sliding sleeve (201);
the vertical traction frame (4) is arranged above the sealing cover plate (2), the top end of the central traction shaft (3) is rotationally connected with the vertical traction frame (4), a lifting screw sleeve (401) is arranged in the middle of the vertical traction frame (4), a lifting screw rod (402) is arranged on the inner side of the lifting screw sleeve (401) in a nested mode, a lifting motor (403) is arranged at the bottom end of the lifting screw rod (402), and the lifting motor (403) is fixedly connected with the sealing cover plate (2);
the catalyst filter disc (6) is embedded and slidingly arranged on the inner side of the reaction kettle (1), a filter screen (601) is arranged at the bottom of the catalyst filter disc (6), a center plug bush (602) is arranged at the center of the catalyst filter disc (6), a center clamping block (301) is arranged at the bottom end of the center traction shaft (3), the center clamping block (301) and the center plug bush (602) are mutually matched in size, a connecting electromagnet (302) is arranged in the middle of the center clamping block (301), and a hanging magnet (603) is arranged on the inner side of the center plug bush (602);
weighing press ring (7), the nested setting in be located the outside of the center traction shaft (3) of sealed apron (2) top, weighing press ring (7) with be provided with weighing press gauge (701) between the top surface of sealed apron (2), evenly encircle perpendicularly in the outside of weighing press ring (7) and be provided with a plurality of traction bars (702), the bottom of weighing traction bar (702) is run through sealed apron (2) are connected and are provided with magnetism traction block (703), weighing press ring (7) with magnetism traction block (703) all pass through weighing traction bar (702) with sealed apron (2) synchronous sliding connection, the outside of center plug bush (602) is encircleed and is provided with magnetic connection piece (604), the middle vertical of sealed apron (2) is run through and is provided with vertical feed supplement pipe (8).
2. The phthalic anhydride chlorination wastewater treatment and recycling device according to claim 1, wherein a hollow dispersion bin (202) is arranged in the sealing cover plate (2), a plurality of dispersion conveying holes (203) are uniformly formed in the bottom surface of the sealing cover plate (2), a reaction conveying pipe (204) is connected and arranged on the outer side of the hollow dispersion bin (202), and a balance exhaust pipe (205) is connected and arranged on the top end of the reaction conveying pipe (204).
3. The phthalic anhydride chlorination wastewater treatment and recycling device according to claim 1, wherein a rotating clamping ring (303) is arranged at the top end of the central traction shaft (3), a traction connecting sleeve (404) is arranged at the center of the vertical traction frame (4), the traction connecting sleeve (404) and the rotating clamping ring (303) are mutually matched in size, the central traction shaft (3) is rotatably connected with the traction connecting sleeve (404) arranged at the center of the vertical traction frame (4) through the rotating clamping ring (303), a rotating gear (304) is arranged above the traction connecting sleeve (404), a stirring gear (406) is arranged on the outer side of the rotating gear (304) in a meshed mode, and a stirring motor (405) is arranged at the shaft end of the stirring gear (406).
4. The phthalic anhydride chlorination wastewater treatment and recycling device according to claim 1, wherein a plurality of horizontal scraping plates are horizontally connected below the sealing cover plate (2), the plurality of horizontal scraping plates are circumferentially arranged around the vertical center line of the sealing cover plate (2), and the horizontal scraping plates and the catalyst filter discs (6) are mutually parallel.
5. The phthalic anhydride chlorination wastewater treatment and recycling device according to claim 1, wherein a plurality of central connecting sleeves (501) are arranged on the outer side of the central traction shaft (3), a plurality of stirring blades (5) are uniformly and circumferentially arranged on the outer side of the central connecting sleeve (501), a one-way ratchet wheel (502) is arranged between the central connecting sleeve (501) and the central traction shaft (3), and the central traction shaft (3) drives the central connecting sleeve (501) to rotate in a one-way manner through the one-way ratchet wheel (502) so as to drive the stirring blades (5) to rotate.
6. The phthalic anhydride chlorination wastewater treatment and recycling device according to claim 5, wherein the central connecting sleeve (501) is in nested sliding connection with the central traction shaft (3), a plurality of central connecting sleeves (501) are uniformly arranged along the vertical central line direction of the central traction shaft (3), folding stirring sheets (503) are connected between adjacent central connecting sleeves (501), a distance is reserved between adjacent central connecting sleeves (501) through the folding stirring sheets (503), a folding rotating shaft (504) is arranged at the center of the folding stirring sheets (503), and a supporting spring (505) is arranged in the middle of the folding rotating shaft (504).
7. The phthalic anhydride chlorination wastewater treatment and recycling device according to claim 1, wherein a sealing conveying bin (801) is connected and arranged at the top end of the vertical material supplementing bin (8), a horizontal conveying tray (802) is arranged on the inner side of the sealing conveying bin (801) in a jogged mode, a conveying motor (803) is arranged on the shaft end of the horizontal conveying tray (802) in a connected mode, a plurality of unit material storage barrels (804) are uniformly and circumferentially arranged in the middle of the horizontal conveying tray (802) in a surrounding mode, the upper end and the lower end of the unit material storage barrels (804) are of an open structure, a vertical material conveying pipe (805) is arranged above the sealing conveying bin (801) in a connected mode, the vertical material conveying pipe (805) and the vertical material supplementing bin (8) are arranged in a staggered mode, and a vertical material storage bin (806) is arranged on the top end of the vertical material conveying pipe (805) in a connected mode.
8. The phthalic anhydride chlorination wastewater treatment and recycling device according to claim 1, wherein a disc-type vent pipe (9) is connected and arranged below the catalyst filter disc (6), a plurality of vent holes (901) are uniformly formed in the outer wall of the disc-type vent pipe (9) in a penetrating mode, and the disc-type vent pipe (9) is communicated with the inside of the reaction kettle (1) through the vent holes (901).
9. The phthalic anhydride chlorination wastewater treatment and recycling device according to claim 8, wherein a vertical vent pipe (902) is arranged in the central traction shaft (3), a connecting joint (903) is arranged at the bottom end of the vertical vent pipe (902), a vent interface (904) is arranged at the center of the disc-type vent pipe (9), the connecting joint (903) and the vent interface (904) are correspondingly arranged, and when the central traction shaft (3) is inserted into the central plug bush (602) through the central clamping block (301) to be connected with the catalyst filter disc (6), the connecting joint (903) is connected with the vent interface (904), and the vertical vent pipe (902) is mutually communicated with the disc-type vent pipe (9) through the connecting joint (903) and the vent interface (904).
10. A phthalic anhydride chlorination wastewater treatment and reuse method, adopting the phthalic anhydride chlorination wastewater treatment and reuse device according to any one of claims 1 to 9, characterized by comprising the following steps:
s1, alkali mixing of raw materials: adding phthalic anhydride chlorination wastewater to be treated into a reaction kettle (1), adding 3-5%o of auxiliary agent with mass concentration, and adjusting pH=9-10;
s2, catalytic treatment: adding Raney nickel catalyst, and heating the liquid to 50-120 ℃;
s3, introducing hydrogen for reduction: introducing hydrogen into the liquid of the reaction kettle (1) to perform a reduction reaction for 1-2h;
s4, filtering and separating: the catalyst filter disc (6) at the bottom side inside the reaction kettle (1) is pulled by the central pulling shaft (3) to move upwards, internal liquid is filtered, raney nickel catalyst particles are intercepted and filtered by the catalyst filter disc (6), and the catalyst particles are deposited in the catalyst filter disc (6) to separate the catalyst;
s5, distillation and concentration: after filtering out the catalyst, discharging the liquid from the reaction output pipe (101) to the reaction kettle (1), and then carrying out distillation concentration to obtain 70% of distilled water;
s6, acid precipitation and filtration: cooling the liquid after distillation and concentration to below 35 ℃, adding hydrochloric acid for acidification until the pH value is=1-2, and then filtering to obtain the phthalic acid with the purity of more than 99.5%.
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