CN221580580U - High-temperature reduction chlorination reaction device - Google Patents
High-temperature reduction chlorination reaction device Download PDFInfo
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- CN221580580U CN221580580U CN202420056005.5U CN202420056005U CN221580580U CN 221580580 U CN221580580 U CN 221580580U CN 202420056005 U CN202420056005 U CN 202420056005U CN 221580580 U CN221580580 U CN 221580580U
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- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 53
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 101
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- 238000001816 cooling Methods 0.000 claims abstract description 33
- 239000000919 ceramic Substances 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 19
- 239000000498 cooling water Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000002699 waste material Substances 0.000 claims abstract description 9
- 239000000571 coke Substances 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 29
- 239000007789 gas Substances 0.000 claims description 27
- 230000002829 reductive effect Effects 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 239000011148 porous material Substances 0.000 claims description 13
- 239000011521 glass Substances 0.000 claims description 9
- 239000004744 fabric Substances 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- 229940063656 aluminum chloride Drugs 0.000 abstract description 26
- 239000008188 pellet Substances 0.000 abstract description 18
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 abstract description 2
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 22
- 239000000463 material Substances 0.000 description 21
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 18
- 239000000460 chlorine Substances 0.000 description 18
- 229910052801 chlorine Inorganic materials 0.000 description 18
- 238000000034 method Methods 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 238000005406 washing Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- -1 imidazole aluminum chloride hydrate Chemical compound 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 238000010079 rubber tapping Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000012456 homogeneous solution Substances 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000010669 acid-base reaction Methods 0.000 description 1
- 238000005917 acylation reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- IMDXZWRLUZPMDH-UHFFFAOYSA-N dichlorophenylphosphine Chemical compound ClP(Cl)C1=CC=CC=C1 IMDXZWRLUZPMDH-UHFFFAOYSA-N 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 150000004687 hexahydrates Chemical class 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000011968 lewis acid catalyst Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229910001538 sodium tetrachloroaluminate Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
A high-temperature reduction chlorination reaction device is formed by cascading a tubular reactor and two water-cooling traps in sequence. The reaction tube of the tubular reactor is sleeved with a heating resistance wire, the reaction tube is filled with pellets made of spent catalyst aluminum chloride hexahydrate, coke and adhesive, and ceramic filler layers are arranged in the reaction tube above and below the pellets. The water-cooling catcher is as follows: the bottom of the outer tube is provided with a detachable blind plate, the inner tube with the bottom sealed is inserted into the outer tube, and cooling water is inserted into the inner tube; the cooling water flows out from the bottom to the top through the cooling water outlet pipe of the outer pipe through the bottom opening of the cooling water pipe. The gas generated by the tubular reactor enters through the lower air inlet pipe of the outer pipe, flows out from the upper air outlet pipe, and anhydrous aluminum trichloride cooled by cooling water is condensed on the inner wall of the outer pipe and the outer wall of the inner pipe. The invention has the characteristics of simple structure, high product purity, high product yield and the like. The invention directly recovers the anhydrous aluminum trichloride from the waste catalyst crystalline aluminum chloride, thereby realizing the utilization of the high added value of the catalyst circulation.
Description
Technical Field
The utility model relates to a chemical reaction device, in particular to a reaction device for preparing anhydrous aluminum chloride from crystalline aluminum chloride.
Background
The anhydrous aluminum trichloride is an important inorganic chemical product, is mainly used for organic synthesis catalysts and petroleum cracking catalysts, and is widely used for synthesis of detergents, pesticides, dyes, fragrances and the like. Anhydrous aluminum trichloride is the most widely used lewis acid catalyst in industry, and is mainly used for catalyzing alkylation reaction, acylation reaction, dichloro aryl phosphine intermediate, disproportionation reaction process of dimethyl dichlorosilane and the like. The anhydrous aluminum trichloride is used as a catalyst, the addition amount of the catalyst is relatively large (3% -10%) in actual industrial application, after the catalyst is used, the crystalline aluminum trichloride (AlCl 3.6H2O) containing six crystal waters is generally obtained by water dissolution and purification, and then the crystalline aluminum trichloride is converted into cheap polyaluminium chloride PAC as a water purifying agent, so that the economic benefit is poor, and the aluminum resource is wasted.
The Chinese patent literature discloses a method for preparing anhydrous aluminum chloride by dehydrating crystalline aluminum chloride by a double salt method: the method comprises the steps of taking amine substances, imidazole or pyridine as raw materials to synthesize organic hydrochloride, reacting the synthesized organic hydrochloride with crystalline aluminum chloride and water at 80-100 ℃, separating out crystals, drying to obtain ammonium chloride-containing water aluminum double salt, imidazole aluminum chloride hydrate double salt or pyridine aluminum chloride hydrate double salt, decomposing the double salt for two sections to remove the crystalline water, and capturing sublimated aluminum trichloride gas to obtain anhydrous aluminum chloride.
Dong Yanpeng, xie Chuang and the like are used for converting the aluminum chloride of a waste catalyst generated in the production process of dichlorophenyl phosphine into sodium tetrachloroaluminate (NaAlCl 4), then large-particle aluminum hydroxide is generated through acid-base reaction under the action of a polymeric flocculant, and aluminum oxide is prepared through high-temperature calcination, so that the recovery and circulation of anhydrous aluminum chloride can not be realized; the method has the advantages of long process route, complicated operation, large amount of industrial waste salt containing organic matters generated in the conversion process, great environmental problems and poor economical efficiency.
Anhydrous aluminum trichloride is produced by a high-temperature melt chlorination method of metallic aluminum adopted in industry. Namely, melting metal aluminum into liquid aluminum at a high temperature, and then introducing chlorine gas to the surface of the molten aluminum for quick chlorination reaction to release a large amount of heat; the generated aluminum chloride enters an aluminum chloride collector in a gas form and is sublimated. Aluminum trichloride is produced by a metal aluminum melt chlorination method, and has high purity and good quality, but the reaction is a strong exothermic reaction and has high requirements on process safety.
Disclosure of utility model
The utility model aims to provide a reaction device for anhydrous aluminum trichloride from crystalline aluminum chloride, which has the advantages of simple structure, high product purity and high recovery rate.
The purpose of the utility model is realized in the following way: the reaction device for anhydrous aluminum trichloride from crystalline aluminum chloride is characterized by comprising a tubular reactor and more than one water-cooling traps which are sequentially cascaded;
Tubular reactor: the reaction tube is arranged along the vertical direction, and a glass cloth wrapped ceramic chip packing layer and a ceramic chip packing layer are sequentially arranged on a supporting pore plate at the lower part of the inner cavity of the reaction tube from bottom to top; another ceramic chip filler layer and another glass cloth-wrapped ceramic chip filler layer are sequentially arranged on the support pore plate at the upper part of the inner cavity of the reaction tube from bottom to top, heating resistance wires or electromagnetic heaters are arranged on the periphery of the reaction tube corresponding to the position between the top of the ceramic chip layer wrapped by the other glass cloth and the support pore plate at the lower part of the inner cavity of the reaction tube, a nitrogen gas inlet pipe and a chlorine gas inlet pipe are arranged on the reaction tube corresponding to the position below the support pore plate at the lower part, a gas outlet pipeline is transversely arranged at the top of the reaction tube, and the inner cavity of the reaction tube is used for filling waste catalyst crystalline aluminum chloride and coke;
Water-cooled catcher: the lower part and the upper part of the outer tube arranged along the vertical direction are respectively provided with a horizontal air inlet tube and a horizontal air outlet tube, the bottom of the outer tube is provided with a detachable blind plate, the inner tube is inserted into the outer tube from top to bottom, the bottom of the inner tube is sealed and positioned below the horizontal air inlet tube, the inner tube and the outer tube are positioned on the same axis, the inner tube is fixed with the top end flange of the outer tube through bolts by a flange welded on the periphery of the upper part of the inner tube, the upper part of the inner tube is provided with a horizontal cooling water outlet tube, the cooling water tube is inserted into the inner tube from top to bottom and is adjacent to the bottom of the inner tube, and the cooling water tube is fixed with the top end flange of the inner tube through bolts by a flange welded on the periphery of the upper part of the inner tube; the gas outlet pipeline of the reactor is connected with the horizontal gas inlet pipe of the water-cooling catcher through a flange.
The two water-cooling traps are arranged, and a horizontal air outlet pipe of the first water-cooling trap is communicated with a horizontal air inlet pipe of the second water-cooling trap through a flange; and the nitrogen inlet pipe and the chlorine inlet pipe are respectively provided with a mass flowmeter.
The device also comprises a frame: three rectangular frames which are sequentially arranged from left to right are formed by welding angle steel or rectangular pipes, the height of the third rectangular frame is larger than that of the second rectangular frame, and the height of the second rectangular frame is larger than that of the first rectangular frame;
The tubular reactor is arranged at the bottom of the first rectangular frame, the first water-cooling catcher and the second water-cooling catcher are respectively arranged on the second rectangular frame and the third rectangular frame, the height of a horizontal air inlet pipe of the first water-cooling catcher is adjacent to a gas outlet pipeline of the tubular reactor, and the height of a horizontal air inlet pipe of the second water-cooling catcher is adjacent to a horizontal air outlet pipe of the first water-cooling catcher.
Aiming at the practical problems of large aluminum chloride waste catalyst quantity, low recycling level, large aluminum resource waste, serious environmental impact and the like in the industrial production process, the utility model provides a method for directly crystallizing aluminum trichloride from the waste catalyst by using a high-temperature reduction chlorination technology and recycling the anhydrous aluminum trichloride catalyst, thereby realizing the recycling of the catalyst with high added value. The utility model has low requirement on process safety, and has the characteristics of simple reaction device, high product purity, high product recovery rate and the like.
Drawings
FIG. 1 is a schematic diagram of a high temperature reductive chlorination tubular reactor according to the present disclosure.
Fig. 2 is a structural diagram of a water-cooled trap.
FIG. 3 is a block diagram of a high temperature reductive chlorination reactor comprising the tubular reactor shown in FIG. 1 and the two-stage water-cooled trap shown in FIG. 2.
Fig. 4 is a top view of fig. 3.
Fig. 5 is a process flow diagram of the present utility model.
Detailed Description
In fig. 1, tubular reactor 100, feed 6, in fig. 2, water-cooled trap 200; in fig. 3, a mass flowmeter 17 and a connecting pipe 18 are provided.
FIG. 3 and FIG. 4 show a reaction apparatus for anhydrous aluminum trichloride from crystalline aluminum chloride, characterized by a sequential cascade of a tubular reactor 100 and one or more water-cooled traps 200;
Tubular reactor: the reaction tube 1 is arranged along the vertical direction, and a glass cloth-coated ceramic chip filler layer 4 and a ceramic chip filler layer 5 are sequentially arranged on a supporting pore plate at the lower part of the inner cavity of the reaction tube from bottom to top; another ceramic chip filler layer and another glass cloth-wrapped ceramic chip filler layer are sequentially arranged on the support pore plate at the upper part of the inner cavity of the reaction tube from bottom to top, a heating resistance wire 7 or an electromagnetic heater is arranged on the periphery of the reaction tube corresponding to the position between the top of the ceramic chip layer wrapped by the other glass cloth and the support pore plate at the lower part of the inner cavity of the reaction tube, a nitrogen gas inlet pipe 2 and a chlorine gas inlet pipe 3 are arranged on the reaction tube corresponding to the position below the support pore plate at the lower part, a gas outlet pipeline 8 is transversely arranged at the top of the reaction tube, and the inner cavity of the reaction tube is used for filling waste catalyst crystalline aluminum chloride and coke;
Water-cooled catcher: the lower part and the upper part of an outer pipe 12 arranged along the vertical direction are respectively provided with a horizontal air inlet pipe 13 and a horizontal air outlet pipe 14, the bottom of the outer pipe is provided with a detachable blind plate 15, an inner pipe 10 is inserted into the outer pipe from top to bottom, the bottom of the inner pipe is sealed and positioned below the horizontal air inlet pipe, the inner pipe and the outer pipe are positioned on the same axis, the inner pipe is fixed with the top end flange of the outer pipe through bolts by a flange welded on the periphery of the upper part of the inner pipe, the upper part of the inner pipe is provided with a horizontal cooling water outlet pipe 11, a cooling water pipe 9 is inserted into the inner pipe from top to bottom and is adjacent to the bottom of the inner pipe, and the cooling water pipe is fixed with the top end flange of the inner pipe through bolts by a flange welded on the periphery of the upper part of the inner pipe; the gas outlet pipe 8 of the reactor is connected with the horizontal gas inlet pipe 13 of the water-cooled catcher through a flange.
The two water-cooling traps are arranged, and a horizontal air outlet pipe 14 of the first water-cooling trap is communicated with a horizontal air inlet pipe 13 of the second water-cooling trap through a flange; and the nitrogen inlet pipe and the chlorine inlet pipe are respectively provided with a mass flowmeter.
There is also a frame 16: three rectangular frames which are sequentially arranged from left to right are formed by welding angle steel or rectangular pipes, the height of the third rectangular frame is larger than that of the second rectangular frame, and the height of the second rectangular frame is larger than that of the first rectangular frame;
The tubular reactor is arranged at the bottom of the first rectangular frame, the first water-cooling catcher and the second water-cooling catcher are respectively arranged on the second rectangular frame and the third rectangular frame, the height of a horizontal air inlet pipe of the first water-cooling catcher is adjacent to a gas outlet pipeline 8 of the tubular reactor, and the height of a horizontal air inlet pipe of the second water-cooling catcher is adjacent to a horizontal air outlet pipe of the first water-cooling catcher. (see FIGS. 1 and 2). In fig. 2, a flange is welded on the opening at the lower part of the outer tube, and is fixed with the other flange through bolts, and the blind plate is clamped between the two flanges. The anhydrous aluminum trichloride is condensed on the inner wall of the outer tube and the outer wall of the inner tube. And (3) detaching the flange between the inner pipe and the outer pipe, and integrally extracting the inner pipe and the cooling water pipe from the outer pipe so as to recover the anhydrous aluminum chloride attached to the outer wall of the inner pipe. And then the blind plate at the bottom of the outer tube is disassembled, so that the anhydrous aluminum trichloride attached to the inner wall of the outer tube is recovered.
The reactor is a high-temperature reduction chlorination reactor and is mainly used for crystallizing aluminum chloride (aluminum chloride hexahydrate) to obtain an anhydrous aluminum trichloride product through one-step high-temperature reduction chlorination. Mixing crystal aluminum trichloride containing crystal water, coke, chlorine and the like according to a certain proportion, adding the mixture into a supporting plate in a reactor, introducing mixed gas of chlorine and air into the lower part of the reactor, reducing and chlorinating the mixture at a high temperature of between 500 and 800 ℃ by controlling the temperature of a material bed layer, wherein the crystal aluminum trichloride can completely remove crystal water in molecules and is converted into anhydrous aluminum trichloride, and the anhydrous aluminum trichloride is discharged from a gas phase outlet at the upper part of the reactor along with gases such as nitrogen, hydrogen chloride, carbon dioxide, carbon monoxide and the like in a gas form; the high-temperature gas-phase mixture passes through a circulating water-cooling wall of a catcher outside the reactor, wherein anhydrous aluminum trichloride is deposited on the water-cooling wall (the anhydrous aluminum trichloride is condensed on the water-cooling wall below 200 ℃ and is in a sublimated state when meeting the cold wall, and the anhydrous aluminum trichloride is more than 200 ℃), and the anhydrous aluminum trichloride and other carbon dioxide, carbon monoxide, hydrogen chloride and a small amount of chlorine continue to flow out from an outlet of the catcher, and are emptied after alkali washing, water washing and other treatments.
The high-temperature reduction chlorination reactor is successfully used for dehydrating crystalline aluminum trichloride at a high temperature by a one-step method to generate anhydrous aluminum trichloride, and plays a key role in high-value recycling of a large amount of waste aluminum chloride catalysts in industrial production.
The bed height of the high temperature reductive chlorination reactor depends on the crystalline aluminum trichloride treating capacity. The gas distributor, the material layer supporting pore plate, the inert filler layer, the reaction raw material layer, the inert filler layer and the gas phase space are respectively arranged from bottom to top
The inner diameter and the height of the material layer are determined according to the processing capacity, and the height-diameter ratio is between 4 and 15
The external catcher adopts a multi-layer sleeve form, and has simple structure and convenient maintenance. Circulating cooling water is introduced into the inner pipe, so that the wall of the inner pipe forms a cold wall, thereby effectively capturing anhydrous aluminum trichloride (purity is more than 98%) from high-temperature gas,
Example 1:
The recovered spent catalyst hexahydrated crystalline aluminum chloride, the coke powder with the granularity of 80 meshes, the polyacrylamide and the deionized water are fully and uniformly mixed according to the mass ratio of 100:250:20:50, formed into pellets with the diameter of 2-3 mm, and then fully dried for 10-15 hours at the temperature of 100 ℃ for standby.
Firstly filling a ceramic filler layer with the length of 2-3 cm in a high-temperature reduction chlorination reactor, and then adding 600 g of raw material pellets; tapping the outer tube of the reactor to uniformly fill the raw material layer; then a ceramic filler layer with the height of 2-3 cm is filled on the material layer. And pressing an upper cover of the high-temperature reduction chlorination reactor, and connecting a temperature and pressure sensor, an anhydrous aluminum chloride catcher and a tail gas washing system. And introducing nitrogen from a gas raw material inlet at the lower part of the high-temperature reduction chlorination reactor, and checking the air tightness of the system.
And starting a heating system of the high-temperature reduction chlorination reactor, heating the reactor materials, switching nitrogen into chlorine, and controlling the flow of the chlorine to be 1.0L/min before the temperature of a material layer is lower than 200 ℃. When the temperature of the material layer reaches 200 ℃, the chlorine flow is regulated to 3.0L/min, the temperature rising speed of the material layer is kept at 15 ℃/min, and the material is heated to 500 ℃ for reductive chlorination.
The temperature is controlled at 500 ℃, and the chlorine flow is 3.0L/min, and the reaction is finished after 1.0 hour of high-temperature reaction. 65.0 g of yellow-gray anhydrous aluminum trichloride was collected in a trap in 82.2% yield
Example 2:
The raw material pellets and the high-temperature reductive chlorination reaction were operated similarly to example 1, and the reaction was terminated by maintaining the high-temperature chlorination reaction temperature at 600℃for 1 hour. 68 g of yellow-gray anhydrous aluminum trichloride was collected in a trap, and the yield was 86.0%.
Example 3:
The raw material pellets and the high-temperature reductive chlorination reaction were operated similarly to example 1, and the reaction was terminated by maintaining the high-temperature reductive chlorination reaction temperature at 750℃for 1 hour. 69.2 g of yellow-white anhydrous aluminum trichloride was collected in a trap, and the yield was 88.7%.
Example 4:
the raw material pellets and the high-temperature reductive chlorination reaction were operated similarly to example 1, and the reaction was terminated by maintaining the high-temperature reductive chlorination reaction temperature at 900℃for 1 hour. 65.2 g of yellow-white anhydrous aluminum trichloride was collected in a trap, and the yield was 82.3%.
Example 5:
The operation of the raw material pellet and the high-temperature reduction chlorination reaction is similar to that of the example 1, the temperature of the raw material reaches 200 ℃, the flow rate of chlorine is kept at 1.5L/min, the high-temperature chlorination reaction temperature is 700 ℃, and the reaction is finished after 1 hour. 64.2 g of yellow-white anhydrous aluminum trichloride was collected in a trap, and the yield was 82.3%.
Example 6:
The recovered spent catalyst hexahydrated crystalline aluminum chloride, coke powder with granularity of 80 meshes, carboxymethyl cellulose and deionized water are fully and uniformly mixed according to the mass ratio of 100:200:30:50, formed into pellets with the diameter of 2-3 mm, and then fully dried for 10-15 hours at the temperature of 100 ℃ for standby.
Firstly filling a ceramic filler layer with the length of 2-3 cm in a high-temperature reduction chlorination reactor, and then adding 600 g of raw material pellets; tapping the outer tube of the reactor to uniformly fill the raw material layer; then a ceramic filler layer with the height of 2-3 cm is filled on the material layer. And pressing an upper cover of the high-temperature reduction chlorination reactor, and connecting a temperature and pressure sensor, an anhydrous aluminum chloride catcher and a tail gas washing system. And introducing nitrogen from a gas raw material inlet at the lower part of the high-temperature reduction chlorination reactor, and checking the air tightness of the system.
And starting a heating system of the high-temperature reduction chlorination reactor, heating the reactor materials, switching nitrogen into chlorine, and controlling the flow of the chlorine to be 1.0L/min before the temperature of a material layer is lower than 200 ℃. When the temperature of the material layer reaches 200 ℃, the chlorine flow is regulated to 3.0L/min, the temperature rising speed of the material layer is kept at 15 ℃/min, and the material is heated to 500 ℃ for reductive chlorination.
The temperature is controlled at 550 ℃, and the chlorine flow is 3.0L/min, and the reaction is finished after 1.0 hour of high-temperature reaction. 67.0 g of yellow-gray anhydrous aluminum trichloride was collected in a trap in a yield of 85.6%
Example 7:
The raw material pellets and the high-temperature reductive chlorination reaction were operated similarly to example 6, and the reaction was terminated by maintaining the high-temperature chlorination reaction temperature at 650℃for 1 hour. 70 g of yellow-gray anhydrous aluminum trichloride were collected in a trap, with a yield of 89.7%.
Example 8:
The raw material pellets and the high-temperature reductive chlorination reaction were operated similarly to example 6, and the reaction was terminated by maintaining the high-temperature reductive chlorination reaction temperature at 750℃for 1 hour. 69.0 g of yellow-white anhydrous aluminum trichloride was collected in a trap, and the yield was 88.2%.
Example 9:
The raw material pellets and the high-temperature reductive chlorination reaction were operated similarly to example 6, and the reaction was terminated by maintaining the high-temperature reductive chlorination reaction temperature at 850℃for 1 hour. 66.2 g of yellow-white anhydrous aluminum trichloride was collected in a trap, with a yield of 84.3%.
Example 10:
The recovered spent catalyst hexahydrate crystalline aluminum chloride, the coke powder with granularity of 80 meshes and the epoxy resin are fully and uniformly mixed according to the mass ratio of 100:250:30, formed into pellets with the diameter of 2-3 mm, and then fully dried for 10-15 hours at the temperature of 110 ℃ for standby.
Firstly filling a ceramic filler layer with the length of 2-3 cm in a high-temperature reduction chlorination reactor, and then adding 600 g of raw material pellets; tapping the outer tube of the reactor to uniformly fill the raw material layer; then a ceramic filler layer with the height of 2-3 cm is filled on the material layer. And pressing an upper cover of the high-temperature reduction chlorination reactor, and connecting a temperature and pressure sensor, an anhydrous aluminum chloride catcher and a tail gas washing system. And introducing nitrogen from a gas raw material inlet at the lower part of the high-temperature reduction chlorination reactor, and checking the air tightness of the system.
And starting a heating system of the high-temperature reduction chlorination reactor, heating the reactor materials, switching nitrogen into chlorine, and controlling the flow of the chlorine to be 1.0L/min before the temperature of a material layer is lower than 200 ℃. When the temperature of the material layer reaches 200 ℃, the chlorine flow is regulated to 3.0L/min, the temperature rising speed of the material layer is kept at 15 ℃/min, and the material is heated to 500 ℃ for reductive chlorination.
The temperature is controlled at 600 ℃, and the chlorine flow is 3.0L/min, and the reaction is finished after 1.0 hour of high-temperature reaction. 65.0 g of yellow-gray anhydrous aluminum trichloride was collected in a trap in a yield of 83.3%
Example 11:
The raw material pellets and the high-temperature reductive chlorination reaction were operated similarly to example 10, and the reaction was terminated by maintaining the high-temperature chlorination reaction temperature at 700℃for 1 hour. 70.2 g of yellow-gray anhydrous aluminum trichloride was collected in a trap in 89.8% yield.
Example 12:
The raw material pellets and the high-temperature reductive chlorination reaction were operated similarly to example 10, and the reaction was terminated by maintaining the high-temperature reductive chlorination reaction temperature at 750℃for 1 hour. 69.0 g of yellow-white anhydrous aluminum trichloride was collected in a trap, and the yield was 88.2%.
Example 13:
The raw material pellets and the high-temperature reductive chlorination reaction were operated similarly to example 10, and the reaction was terminated by maintaining the high-temperature reductive chlorination reaction temperature at 800℃for 1 hour. 66.0 g of yellow-white anhydrous aluminum trichloride was collected in a trap, and the yield was 84.0%.
Example 14
100 G of yellow gray anhydrous aluminum trichloride obtained by the high-temperature reduction chlorination reaction is added into 300 ml of absolute ethyl alcohol, stirred at 60 ℃ for 30 minutes, stirred and stopped, and subjected to nitrogen pressure filtration; an absolute ethanol homogeneous solution was obtained and solvent ethanol was recovered by evaporation in a rotary evaporator to yield 97.5 g of a white yellow anhydrous aluminum trichloride product.
Example 15
100 G of yellow gray anhydrous aluminum trichloride obtained by the high-temperature reduction chlorination reaction is added into 300 ml of absolute ethyl alcohol, stirred for 30 minutes under the reflux condition, and then the stirring is stopped, and the nitrogen filter pressing is performed; an absolute ethanol homogeneous solution was obtained, and solvent ethanol was recovered by evaporation in a rotary evaporator to obtain 98 g of a white yellow absolute aluminum trichloride product.
Claims (3)
1. The high-temperature reduction chlorination reaction device is characterized by comprising a tubular reactor (100) and more than one water-cooling traps (200) which are sequentially cascaded;
Tubular reactor: the reaction tube (1) is arranged along the vertical direction, and a glass cloth wrapped ceramic chip filler layer (4) and a ceramic chip filler layer (5) are sequentially arranged on a supporting pore plate at the lower part of the inner cavity of the reaction tube from bottom to top; another ceramic chip filler layer and another glass cloth-wrapped ceramic chip filler layer are sequentially arranged on the support pore plate at the upper part of the inner cavity of the reaction tube from bottom to top, heating resistance wires (7) or electromagnetic heaters are arranged on the periphery of the reaction tube corresponding to the position between the top of the ceramic chip layer wrapped by the other glass cloth and the support pore plate at the lower part of the inner cavity of the reaction tube, a nitrogen gas inlet pipe (2) and a chlorine gas inlet pipe (3) are arranged on the reaction tube corresponding to the position below the support pore plate at the lower part, a gas outlet pipeline (8) is transversely arranged at the top of the reaction tube, and the inner cavity of the reaction tube is used for filling waste catalyst crystalline aluminum chloride and coke;
Water-cooled catcher: the lower part and the upper part of an outer pipe (12) arranged along the vertical direction are respectively provided with a horizontal air inlet pipe (13) and a horizontal air outlet pipe (14), the bottom of the outer pipe is provided with a detachable blind plate (15), an inner pipe (10) is inserted into the outer pipe from top to bottom, the bottom of the inner pipe is sealed and positioned below the horizontal air inlet pipe, the inner pipe and the outer pipe are positioned on the same axis, the inner pipe is fixed with the top end flange of the outer pipe through a welded flange on the periphery of the upper part of the inner pipe through bolts, the upper part of the inner pipe is provided with a horizontal cooling water outlet pipe (11), a cooling water pipe (9) is inserted into the inner pipe from top to bottom and is adjacent to the bottom of the inner pipe, and the cooling water pipe is fixed with the top end flange of the inner pipe through the welded flange on the periphery of the upper part of the inner pipe through bolts; the gas outlet pipeline (8) of the reactor is connected with the horizontal gas inlet pipe (13) of the water-cooling catcher through a flange.
2. The high-temperature reduction chlorination reaction device according to claim 1, wherein the number of the water-cooling traps is two, and a horizontal air outlet pipe (14) of the first water-cooling trap is connected with a horizontal air inlet pipe (13) of the second water-cooling trap through a flange; and the nitrogen inlet pipe and the nitrogen outlet pipe are respectively provided with a mass flowmeter.
3. A high temperature reductive chlorination reaction device according to claim 2, further comprising a frame (16): three rectangular frames which are sequentially arranged from left to right are formed by welding angle steel or rectangular pipes, the height of the third rectangular frame is larger than that of the second rectangular frame, and the height of the second rectangular frame is larger than that of the first rectangular frame;
The tubular reactor is arranged at the bottom of the first rectangular frame, the first water-cooling catcher and the second water-cooling catcher are respectively arranged on the second rectangular frame and the third rectangular frame, the height of a horizontal air inlet pipe of the first water-cooling catcher is adjacent to a gas outlet pipeline (8) of the tubular reactor, and the height of a horizontal air inlet pipe of the second water-cooling catcher is adjacent to a horizontal air outlet pipe of the first water-cooling catcher.
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