CN115744952B - Continuous production system and method of aluminum trichloride - Google Patents
Continuous production system and method of aluminum trichloride Download PDFInfo
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- CN115744952B CN115744952B CN202211085569.3A CN202211085569A CN115744952B CN 115744952 B CN115744952 B CN 115744952B CN 202211085569 A CN202211085569 A CN 202211085569A CN 115744952 B CN115744952 B CN 115744952B
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- condenser
- aluminum trichloride
- solid separator
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- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 title claims abstract description 149
- 238000010924 continuous production Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims description 202
- 239000007787 solid Substances 0.000 claims description 138
- 239000000460 chlorine Substances 0.000 claims description 131
- 229910052801 chlorine Inorganic materials 0.000 claims description 131
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 128
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 99
- 238000005660 chlorination reaction Methods 0.000 claims description 86
- 238000003860 storage Methods 0.000 claims description 59
- 229910052757 nitrogen Inorganic materials 0.000 claims description 51
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 29
- 238000009833 condensation Methods 0.000 claims description 22
- 230000005494 condensation Effects 0.000 claims description 22
- 239000013078 crystal Substances 0.000 claims description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 18
- 229910052782 aluminium Inorganic materials 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 17
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 13
- 125000004122 cyclic group Chemical group 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000002425 crystallisation Methods 0.000 description 10
- 230000008025 crystallization Effects 0.000 description 10
- 239000006200 vaporizer Substances 0.000 description 10
- 239000012495 reaction gas Substances 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention belongs to the technical field of aluminum trichloride production, and particularly relates to a continuous production system and a continuous production method of aluminum trichloride. The invention provides a continuous production system of aluminum trichloride, which comprises a gas unit, a reaction unit and a circulation unit which are sequentially communicated. According to the invention, the circulating unit is arranged behind the reaction unit, and the reaction unit and the circulating unit form a closed loop, so that continuous production of aluminum trichloride is realized, and the production efficiency of the aluminum trichloride is improved.
Description
Technical Field
The invention belongs to the technical field of aluminum trichloride production, and particularly relates to a continuous production system and a continuous production method of aluminum trichloride.
Background
The anhydrous aluminum trichloride is widely applied to petroleum, chemical industry, medicines and other industrial processes, and is a catalyst, a flocculating agent, a preservative or a mordant for producing pigments, medicines and cosmetics.
The production process of anhydrous aluminum trichloride mainly comprises a metallic aluminum method, an alumina method, a crystalline hexahydrate aluminum chloride dehydration method and an electrochemical method. The electrochemical method is rarely used because of the problems of low product purity, high energy consumption and the like. The alumina method and the crystallization aluminum chloride hexahydrate dehydration method have the problems of long process route, difficult control of product quality and the like.
The metal aluminum method is to heat and melt aluminum ingots, introduce chlorine gas to generate aluminum trichloride gas for chlorination reaction, and condense the aluminum trichloride gas to obtain anhydrous aluminum trichloride. The process has the advantages of simple flow, less equipment, high product purity, small investment of unit products and low fixed cost, and is a production process commonly used in the industry at present.
However, in the actual production process, the gas-phase aluminum trichloride enters the catcher and is naturally condensed to sublimate on the condensing plate to generate anhydrous aluminum trichloride. The process is not a continuous process, the condensing plate is required to be periodically knocked and scraped to obtain the aluminum trichloride finished product, and the production efficiency is low.
Disclosure of Invention
The invention aims to provide a continuous production system and a continuous production method of aluminum trichloride, and the continuous production system can realize continuous production of aluminum trichloride and has high production efficiency.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a continuous production system of aluminum trichloride, which comprises a gas unit, a reaction unit and a circulation unit which are sequentially communicated;
the reaction unit comprises a chlorination reactor 1 and a condenser 2;
the chlorination reactor 1 is provided with a chlorination reactor air outlet 10 and a chlorination reactor air inlet 24;
the condenser 2 is provided with a condenser air inlet 11, a condenser air outlet 12 and a condenser feed inlet 13;
the air outlet 10 of the chlorination reactor is communicated with the air inlet 11 of the condenser;
the circulating unit comprises a gas-solid separator 3, wherein the gas-solid separator 3 is provided with a gas-solid separator discharge port 16 and a gas-solid separator gas inlet 17;
the condenser air outlet 12 is communicated with the air inlet 17 of the gas-solid separator;
the discharge port 16 of the gas-solid separator is communicated with the feed port 13 of the condenser.
Preferably, the gas unit comprises a chlorine system, or a chlorine system and a condensing system.
Preferably, when the gas unit comprises a chlorine system and a condensing system;
the chlorine system comprises a chlorine storage tank 5 and a chlorine gasifier 6 communicated with an air outlet of the chlorine storage tank 5;
the condensing system comprises a nitrogen storage tank 7 and a nitrogen gasifier 8 communicated with an air outlet of the nitrogen storage tank 7;
the nitrogen gasifier 8 is provided with a nitrogen gasifier air outlet 21, and the nitrogen gasifier air outlet 21 is communicated with the condenser feed inlet 13.
Preferably, when the gas unit comprises a chlorine system and a condensation system, the circulation unit further comprises a heat exchanger 9;
the heat exchanger 9 is provided with a heat exchanger air inlet 19 and a heat exchanger air outlet 20;
the gas-solid separator 3 is provided with a gas-solid separator gas outlet 18;
the gas outlet 18 of the gas-solid separator is communicated with the gas inlet 19 of the heat exchanger; the heat exchanger air outlet 20 is communicated with the condenser feed inlet 13.
Preferably, when the gas unit comprises a chlorine system;
the chlorine system comprises a chlorine storage tank 5 and a chlorine gasifier 6 communicated with an air outlet of the chlorine storage tank 5;
the chlorine gasifier 6 is provided with a chlorine gasifier air outlet 25; the chlorine storage tank air outlet 25 is communicated with the condenser feed inlet 13;
the gas-solid separator 3 is provided with a gas-solid separator gas outlet 18; the gas-solid separator outlet 18 communicates with the chlorination reactor inlet 24.
Preferably, the reaction unit further comprises an aluminum trichloride storage tank 4;
the aluminum trichloride storage tank 4 is provided with an aluminum trichloride storage tank feed inlet 15;
the condenser 2 is provided with a condenser discharge port 14;
the condenser discharge port 14 is communicated with the aluminum trichloride storage tank feed port 15 through a discharge valve 28.
The invention also provides a continuous production method of aluminum trichloride, which adopts the continuous production system of the technical scheme and comprises the following steps:
continuously inputting chlorine gas into the chlorination reactor 1 through a gas unit, mixing the chlorine gas with metal aluminum liquid, and carrying out chlorination reaction to obtain aluminum trichloride gas;
continuously introducing the aluminum trichloride gas into the condenser 2 for condensation to obtain a first aluminum trichloride solid and a first tail gas respectively; the first tail gas comprises uncondensed aluminum trichloride gas, second aluminum trichloride solids and chlorine gas; the grain diameter of the first aluminum trichloride solid is more than or equal to 1000 mu m; the particle size of the second aluminum trichloride solid is less than 1000 mu m;
continuously introducing the first tail gas into the gas-solid separator 3 for gas-solid separation to obtain aluminum trichloride seed crystals and second tail gas respectively; the second tail gas comprises uncondensed aluminum trichloride gas and chlorine gas;
and (3) introducing the aluminum trichloride seed crystal into the condenser 2 for cyclic condensation.
Preferably, when the gas unit comprises a chlorine system and a condensing system;
the chlorine is introduced into the chlorination reactor 1 by a chlorine system via the chlorination reactor gas inlet 24;
nitrogen in the condensing system is introduced into the condenser 2 through the condenser feed inlet 13, and heat exchange is carried out between the nitrogen and the aluminum trichloride gas; the flow of the nitrogen is 100-500 m 3 /h。
Preferably, when the gas unit comprises a chlorine system and a condensing system, the first tail gas and the second tail gas also independently comprise nitrogen;
the second tail gas is introduced into the condenser 2 after heat exchange to be used as condensing gas and aluminum trichloride gas for heat exchange;
the heat exchange is performed in the heat exchanger 9.
Preferably, when the gas unit comprises a chlorine system;
the chlorine is introduced into the condenser 2 from a chlorine system through the condenser feed inlet 13, flows out from the condenser air outlet 12, is introduced into the gas-solid separator 3 through the gas-solid separator air inlet 17, flows out from the gas-solid separator air outlet 18, and is introduced into the chlorination reactor 1 through the chlorine reactor air inlet 24;
the flow of the chlorine is 200-550 m 3 /h。
The invention provides a continuous production system of aluminum trichloride, which comprises a gas unit, a reaction unit and a circulation unit which are sequentially communicated; the reaction unit comprises a chlorination reactor 1 and a condenser 2; the chlorination reactor 1 is provided with a chlorination reactor air outlet 10 and a chlorination reactor air inlet 24; the condenser 2 is provided with a condenser air inlet 11, a condenser air outlet 12 and a condenser feed inlet 13; the air outlet 10 of the chlorination reactor is communicated with the air inlet 11 of the condenser; the circulating unit comprises a gas-solid separator 3, wherein the gas-solid separator 3 is provided with a gas-solid separator discharge port 16 and a gas-solid separator gas inlet 17; the condenser air outlet 12 is communicated with the air inlet 17 of the gas-solid separator; the discharge port 16 of the gas-solid separator is communicated with the feed port 13 of the condenser. According to the invention, the circulating unit is arranged behind the reaction unit, and the reaction unit and the circulating unit form a closed loop, so that continuous production of aluminum trichloride is realized, and the production efficiency of the aluminum trichloride is improved.
Drawings
FIG. 1 is a schematic diagram of a continuous production system for aluminum trichloride provided by the invention;
FIG. 2 is a schematic diagram of a continuous production system for aluminum trichloride provided in example 1;
FIG. 3 is a schematic view of a continuous production system for aluminum trichloride provided in example 2;
wherein, 1-chlorination reactor, 2-condenser, 3-gas-solid separator, 4-aluminum trichloride storage tank, 5-chlorine storage tank, 6-chlorine vaporizer, 7-nitrogen storage tank, 8-nitrogen vaporizer, 9-heat exchanger, 10-chlorination reactor gas outlet, 11-condenser gas inlet, 12-condenser gas outlet, 13-condenser feed inlet, 14-condenser discharge outlet, 15-aluminum trichloride storage tank feed inlet, 16-gas-solid separator discharge outlet, 17-gas-solid separator gas inlet, 18-gas-solid separator gas outlet, 19-heat exchanger gas inlet, 20-heat exchanger gas outlet, 21-nitrogen vaporizer gas outlet, 22-nitrogen vaporizer gas inlet, 23-nitrogen storage tank gas outlet, 24-chlorination reactor gas inlet, 25-chlorine vaporizer gas outlet, 26-vaporizer gas inlet, 27-storage tank gas outlet, 28-discharge valve.
Detailed Description
The invention provides a continuous production system of aluminum trichloride, which comprises a gas unit, a reaction unit and a circulation unit which are sequentially communicated;
the reaction unit comprises a chlorination reactor 1 and a condenser 2;
the chlorination reactor 1 is provided with a chlorination reactor air outlet 10 and a chlorination reactor air inlet 24;
the condenser 2 is provided with a condenser air inlet 11, a condenser air outlet 12 and a condenser feed inlet 13;
the air outlet 10 of the chlorination reactor is communicated with the air inlet 11 of the condenser;
the circulating unit comprises a gas-solid separator 3, wherein the gas-solid separator 3 is provided with a gas-solid separator discharge port 16 and a gas-solid separator gas inlet 17;
the condenser air outlet 12 is communicated with the air inlet 17 of the gas-solid separator;
the discharge port 16 of the gas-solid separator is communicated with the feed port 13 of the condenser.
As an embodiment of the invention, the reaction unit comprises a chlorination reactor 1 and a condenser 2.
As an embodiment of the invention, the chlorination reactor 1 is provided with a chlorination reactor outlet 10 and a chlorination reactor inlet 24.
As an embodiment of the present invention, the condenser 2 is provided with a condenser air inlet 11, a condenser air outlet 12, a condenser feed inlet 13 and a condenser discharge outlet 14.
As an embodiment of the invention, the circulation unit comprises a gas-solid separator 3.
As an embodiment of the present invention, the gas-solid separator 3 is provided with a gas-solid separator discharge port 16, a gas-solid separator gas inlet 17, and a gas-solid separator gas outlet 18.
As an embodiment of the present invention, the chlorination reactor gas outlet 10 and the condenser gas inlet 11 are communicated; the condenser air outlet 12 is communicated with the air inlet 17 of the gas-solid separator; the discharge port 16 of the gas-solid separator is communicated with the feed port 13 of the condenser.
As an embodiment of the invention, the gas unit comprises a chlorine system, or a chlorine system and a condensing system.
As an embodiment of the present invention, when the gas unit includes a chlorine system and a condensing system; the chlorine system comprises a chlorine storage tank 5 and a chlorine vaporizer 6 communicated with the air outlet of the chlorine storage tank 5.
As an embodiment of the present invention, the chlorine storage tank 5 is provided with a chlorine storage tank outlet 27; the chlorine gasifier 6 is provided with a chlorine gasifier air outlet 25 and a chlorine gasifier air inlet 26; the chlorine storage tank air outlet 27 is communicated with the chlorine vaporizer air inlet 26; the chlorine vaporizer outlet 25 is in communication with the chlorination reactor inlet 24.
As an embodiment of the present invention, when the gas unit includes a chlorine system and a condensing system; the condensing system comprises a nitrogen storage tank 7 and a nitrogen gasifier 8 communicated with an air outlet of the nitrogen storage tank 7.
As an embodiment of the present invention, the nitrogen tank 7 is provided with a nitrogen tank outlet 23; the nitrogen gasifier 8 is provided with a nitrogen gasifier air outlet 21 and a nitrogen gasifier air inlet 22; the nitrogen storage tank air outlet 23 is communicated with the nitrogen gasifier air inlet 22; the nitrogen gasifier gas outlet 21 is communicated with the condenser feed inlet 13.
As an embodiment of the invention, when the gas unit comprises a chlorine system and a condensation system, the circulation unit further comprises a heat exchanger 9; the heat exchanger 9 is provided with a heat exchanger air inlet 19 and a heat exchanger air outlet 20; the gas outlet 18 of the gas-solid separator is communicated with the gas inlet 19 of the heat exchanger; the heat exchanger air outlet 20 is communicated with the condenser feed inlet 13.
As an embodiment of the invention, when the gas unit comprises a chlorine system; the chlorine system comprises a chlorine storage tank 5 and a chlorine gasifier 6 communicated with an air outlet of the chlorine storage tank 5; the chlorine storage tank 5 is provided with a chlorine storage tank air outlet 27; the chlorine gasifier 6 is provided with a chlorine gasifier air outlet 25 and a chlorine gasifier air inlet 26; the chlorine storage tank air outlet 27 is communicated with the chlorine vaporizer air inlet 26; the chlorine storage tank air outlet 25 is communicated with the condenser feed inlet 13; the condenser air outlet 12 is communicated with the air inlet 17 of the gas-solid separator; the gas-solid separator discharge port 16 is communicated with the condenser feed port 13, and the gas-solid separator gas outlet 18 is communicated with the chlorination reactor gas inlet 24.
As an embodiment of the invention, the reaction unit further comprises an aluminum trichloride storage tank 4; the aluminum trichloride storage tank 4 is provided with an aluminum trichloride storage tank feed inlet 15; the condenser discharge port 14 is communicated with the aluminum trichloride storage tank feed port 15 through a discharge valve 28.
The invention also provides a continuous production method of aluminum trichloride, which adopts the continuous production system of the technical scheme and comprises the following steps:
continuously inputting chlorine gas into the chlorination reactor 1 through a gas unit, mixing the chlorine gas with metal aluminum liquid, and carrying out chlorination reaction to obtain aluminum trichloride gas;
continuously introducing the aluminum trichloride gas into the condenser 2 for condensation to obtain a first aluminum trichloride solid and a first tail gas respectively; the first tail gas comprises uncondensed aluminum trichloride gas, second aluminum trichloride solids and chlorine gas; the grain diameter of the first aluminum trichloride solid is more than or equal to 1000 mu m; the particle size of the second aluminum trichloride solid is less than 1000 mu m;
continuously introducing the first tail gas into the gas-solid separator 3 for gas-solid separation to obtain aluminum trichloride seed crystals and second tail gas respectively; the second tail gas comprises uncondensed aluminum trichloride gas and chlorine gas;
and (3) introducing the aluminum trichloride seed crystal into the condenser 2 for cyclic condensation.
Chlorine is continuously input into the chlorination reactor 1 from a gas unit and mixed with metal aluminum liquid to carry out chlorination reaction, so that aluminum trichloride gas is obtained.
In the present invention, the volume of the metal aluminum liquid is preferably 70 to 80%, more preferably 72 to 78%, and even more preferably 73 to 75% of the total volume of the chlorination reactor 1. In the present invention, the metal aluminum raw material is preferably liquefied by electric heating in the chlorination reactor 1 to obtain the metal aluminum liquid before the chlorination reaction.
In the present invention, the flow rate of the chlorine gas is preferably 200 to 550m 3 Preferably 250% to h500m 3 Preferably from 300 to 450m 3 And/h. In the present invention, the temperature of the chlorination reaction is preferably 780 to 850 ℃, and more preferably 800 to 820 ℃.
In the present invention, it is preferable that the electric heating of the chlorination reactor 1 is turned off during the chlorination reaction, and the temperature of the chlorination reaction is controlled by controlling the flow rate of chlorine gas while using the reaction heat of chlorine gas and the molten metal.
In the present invention, when the gas unit includes a chlorine system and a condensing system; the chlorine gas is introduced into the chlorination reactor 1 by a chlorine gas system via the chlorination reactor gas inlet 24.
In the specific embodiment of the invention, after the chlorine in the chlorine storage tank 5 is gasified by the chlorine gasifier 6, the chlorine flows out of the chlorine gasifier air outlet 25 and is introduced into the chlorination reactor 1 through the chlorination reactor air inlet 24.
In the present invention, when the gas unit includes a chlorine system, the chlorine is introduced into the condenser 2 from the chlorine system through the condenser feed inlet 13, flows out from the condenser gas outlet 12, is introduced into the gas-solid separator 3 through the gas-solid separator gas inlet 17, flows out from the gas-solid separator gas outlet 18, and is introduced into the chlorination reactor 1 through the chlorine reactor gas inlet 24.
In the specific embodiment of the invention, after being gasified by the chlorine gasifier 6, the chlorine in the chlorine storage tank 5 flows out from the chlorine gasifier air outlet 25, flows into the condenser 2 through the condenser feed inlet 13, flows out from the condenser air outlet 12, flows into the gas-solid separator 3 through the gas-solid separator air inlet 17, flows out from the gas-solid separator air outlet 18, and flows into the chlorination reactor 1 through the chlorine reactor air inlet 24.
After the aluminum trichloride gas is obtained, the aluminum trichloride gas is continuously introduced into the condenser 2 for condensation, and a first aluminum trichloride solid and a first tail gas are respectively obtained.
In the present invention, the temperature of the condenser 2 is preferably 180 to 190 ℃, more preferably 182 to 188 ℃, and even more preferably 183 to 185 ℃. In the present invention, the crystallization rate of the aluminum trichloride gas during the condensation is preferably 0.5 to 2.0kg/h, more preferably 1.0 to 1.8kg/h, and still more preferably 1.2 to 1.5kg/h.
In the present invention, the aluminum trichloride gas preferably flows out from the chlorination reactor gas outlet 10 and is introduced into the condenser 2 through the condenser gas inlet 11 to be condensed.
In the present invention, when the gas unit includes a chlorine system and a condensing system; nitrogen in the condensing system is introduced into the condenser 2 through the condenser feed inlet 13, and heat exchange with the aluminum trichloride gas occurs.
In the present invention, the temperature of the nitrogen gas is preferably 40 to 50 ℃, more preferably 42 to 48 ℃, and even more preferably 43 to 45 ℃. In the invention, the flow rate of the nitrogen is 100-500 m 3 Preferably 200 to 400m 3 Preferably from 250 to 350m 3 /h。
In the specific embodiment of the invention, after the nitrogen in the nitrogen storage tank 7 is gasified by the nitrogen gasifier 8, the nitrogen flows out from the air outlet 21 of the nitrogen gasifier, is introduced into the condenser 2 through the feed inlet 13 of the condenser, and exchanges heat with the aluminum trichloride gas, and the aluminum trichloride gas is condensed and crystallized.
In the present invention, when the gas unit includes a chlorine system, the chlorine is introduced into the condenser 2 from the chlorine system through the condenser feed inlet 13, flows out from the condenser gas outlet 12, is introduced into the gas-solid separator 3 through the gas-solid separator gas inlet 17, flows out from the gas-solid separator gas outlet 18, and is introduced into the chlorination reactor 1 through the chlorine reactor gas inlet 24.
In the present invention, when the gas unit includes a chlorine system, the chlorine gas is heat-exchanged as a condensed gas and the aluminum trichloride gas in the condenser 2; the chlorine gas is used as a reaction gas to carry out chlorination reaction with molten aluminum in the chlorination reactor 1. In the present invention, the temperature of the chlorine gas is preferably 40The temperature is preferably 42 to 48℃and more preferably 43 to 45 ℃. In the present invention, the flow rate of the chlorine gas is preferably 200 to 550m 3 Preferably 250 to 500m 3 Preferably from 300 to 450m 3 /h。
In the specific embodiment of the invention, after being gasified by the chlorine gasifier 6, the chlorine in the chlorine storage tank 5 flows out from the chlorine gasifier air outlet 25, flows into the condenser 2 through the condenser feed inlet 13, flows out from the condenser air outlet 12, flows into the gas-solid separator 3 through the gas-solid separator air inlet 17, flows out from the gas-solid separator air outlet 18, and flows into the chlorination reactor 1 through the chlorine reactor air inlet 24; the chlorine gas is taken as a reaction gas to carry out chlorination reaction with metal aluminum liquid in the chlorination reactor 1; the chlorine gas is heat-exchanged with the aluminum trichloride gas as a condensed gas in the condenser 2.
According to the invention, the chlorine is used as the reaction gas and the condensed gas at the same time, and the heating of the chlorine is realized while the aluminum trichloride gas is condensed by the chlorine; the heated chlorine is used as a reaction gas for chlorination reaction, so that the effective utilization of the condensation heat of the aluminum trichloride gas is realized.
In the present invention, the particle size of the first aluminum trichloride solid is preferably not less than 100. Mu.m, more preferably 1000 to 3000. Mu.m. In the present invention, the first aluminum trichloride solids are preferably discharged from the condenser discharge port 14 and fed to the aluminum trichloride tank 4 via the discharge valve 28 and the aluminum trichloride tank feed port 15 for storage.
In the present invention, the first tail gas preferably comprises uncondensed aluminum trichloride gas, second aluminum trichloride solids, and chlorine gas. In the present invention, the particle size of the second aluminum trichloride solid is preferably < 1000. Mu.m.
In the present invention, when the gas unit includes a chlorine system and a condensing system, the first tail gas also preferably includes nitrogen.
After the first tail gas is obtained, the first tail gas is continuously introduced into the gas-solid separator 3 for gas-solid separation, and aluminum trichloride seed crystal and second tail gas are respectively obtained.
In the present invention, the first tail gas flows out of the condenser exhaust port 12 and is introduced into the gas-solid separator 3 through the gas-solid separator intake port 17.
In the present invention, the cut particle diameter at the time of gas-solid separation is preferably 2 to 20. Mu.m, more preferably 5 to 15. Mu.m, still more preferably 8 to 10. Mu.m. In the present invention, the cut particle size of the gas-solid separator is 2 to 20 μm, that is, represents the second aluminum trichloride solid having a particle size of 2 to 20 μm in the first tail gas at the time of gas-solid separation, wherein 50wt% of the second aluminum trichloride solid is separated from the first tail gas and is returned to the condenser 2 as aluminum trichloride seed crystal for condensation.
In a specific embodiment of the present invention, the cutting particle size during the gas-solid separation is specifically 10 μm, that is, the second aluminum trichloride solid with the particle size of 10 μm in the first tail gas during the gas-solid separation is represented, wherein 50wt% of the second aluminum trichloride solid is separated from the first tail gas, and the second aluminum trichloride solid is used as aluminum trichloride seed crystal to be continuously returned to the condenser 2 for condensation.
In the present invention, the second off-gas preferably comprises uncondensed aluminum trichloride gas and chlorine gas.
In the present invention, when the gas unit includes a chlorine system and a condensing system, nitrogen is preferably also included in the second tail gas.
In the present invention, when the gas unit includes a chlorine system and a condensation system, the second tail gas is introduced into the condenser 2 after heat exchange to be used as a condensation gas and the aluminum trichloride gas for heat exchange. In the present invention, the heat exchange is preferably performed in the heat exchanger 9.
In the specific embodiment of the invention, the second tail gas flows out from the gas outlet 18 of the gas-solid reactor, enters the heat exchanger for heat exchange through the gas inlet 19 of the heat exchanger, then flows out from the gas outlet 20 of the heat exchanger, enters the condenser 2 through the feed inlet 13 of the condenser, and is used as condensed gas to exchange heat with aluminum trichloride gas.
In the present invention, when the gas unit includes a chlorine system, the second tail gas flows out from the gas-solid reactor outlet 18, and is introduced into the chlorination reactor 1 through the chlorination reactor inlet 24 as a reaction gas and a metal aluminum liquid to perform a chlorination reaction.
After the aluminum trichloride seed crystal is obtained, the aluminum trichloride seed crystal is introduced into the condenser 2 for cyclic condensation.
In the invention, the aluminum trichloride seed crystal is discharged from the discharge hole 16 of the gas-solid separator and enters the condenser 2 through the feed hole 13 of the condenser for circulating condensation.
According to the invention, after phosphorus trichloride gas is obtained, cooling crystallization is carried out in a mode of heat exchange with condensed gas, so that the problems that products are difficult to collect and possibly poor in quality due to traditional crystallization on the wall surface of a condenser are avoided; simultaneously, the particle size of the aluminum trichloride solid obtained by condensation can be precisely controlled by cooperatively controlling the flow rate and crystallization speed of the condensed gas, and a first aluminum trichloride solid with the particle size of more than or equal to 1000 mu m and a second aluminum trichloride solid with the particle size of less than 1000 mu m are respectively obtained; the first aluminum trichloride solid with the grain diameter of more than or equal to 1000 mu m is used as a finished product for recovery; the second aluminum trichloride solid with the grain diameter smaller than 1000 mu m is subjected to gas-solid separation to obtain an aluminum trichloride seed crystal, the aluminum trichloride seed crystal is returned to the condenser 2 for condensation crystallization, continuous production of aluminum trichloride is realized, and the production efficiency of the aluminum trichloride is improved.
For further explanation of the present invention, a continuous production system of aluminum trichloride and a continuous production method of aluminum trichloride according to the present invention will be described in detail with reference to the accompanying drawings and examples, which should not be construed as limiting the scope of the present invention.
Example 1
Gasifying the chlorine in the chlorine storage tank 5 through the chlorine gasifier 6, flowing out from the chlorine gasifier outlet 25, and introducing the chlorine into the chlorination reactor 1 through the chlorination reactor inlet 24 to perform chlorination reaction with the metal aluminum liquid to obtain aluminum trichloride gas; wherein the flow rate of chlorine is 350m 3 And/h, the volume of the metal aluminum liquid accounts for 80% of the total volume of the chlorination reactor 1, and the chlorination reaction temperature is 820 ℃;
the generated aluminum trichloride gas flows out from the air outlet 10 of the chlorination reactor and is introduced into the condenser 2 through the air inlet 11 of the condenser; after the nitrogen in the nitrogen storage tank 7 is gasified by the nitrogen gasifier 8, the nitrogen flows out from the nitrogen gasifier gas outlet 21 (wherein the nitrogen flow is 220m 3 And/h), introducing the aluminum trichloride gas into the condenser 2 through the condenser feed inlet 13 to perform heat exchange, and performing condensation crystallization (wherein the crystallization speed is 0.35 kg/s) to obtain a first aluminum trichloride solid and a first tail gas, wherein the particle size of the first aluminum trichloride solid is more than or equal to 1000 mu m; wherein the first tail gas comprises uncondensed aluminum trichloride gas, second aluminum trichloride solid with the particle size less than 1000 mu m, chlorine and nitrogen;
the obtained first aluminum trichloride solid is discharged from the condenser discharge port 14 and enters the aluminum trichloride storage tank 4 for storage through the discharge valve 28 and the aluminum trichloride storage tank feed port 15;
the obtained first tail gas flows out from the condenser exhaust port 12, is introduced into the gas-solid separator 3 through the gas-solid separator air inlet 17 for gas-solid separation, and the cutting grain diameter set in the gas-solid separation process is 10 mu m, so that aluminum trichloride seed crystals and second tail gas are respectively obtained; wherein the second tail gas comprises uncondensed aluminum trichloride gas, chlorine gas and nitrogen gas;
the obtained second tail gas flows out from the gas outlet 18 of the gas-solid separator, enters the heat exchanger through the gas inlet 19 of the heat exchanger to exchange heat, flows out from the gas outlet 20 of the heat exchanger, enters the condenser 2 through the feed inlet 13 of the condenser to be used as condensed gas and aluminum trichloride gas to exchange heat;
the obtained aluminum trichloride seed crystal is discharged from a discharge hole 16 of the gas-solid separator, enters the condenser 2 through a feed hole 13 of the condenser and is used as a crystal nucleus to be continuously circularly condensed.
Example 2
After being gasified by the chlorine gasifier 6, the chlorine in the chlorine storage tank 5 flows out from the air outlet 25 of the chlorine gasifier, is introduced into the condenser 2 through the feed inlet 13 of the condenser, flows out from the air outlet 12 of the condenser, and is introduced into the gas-solid separator 3 through the air inlet 17 of the gas-solid separatorFlowing out of the gas-solid separator gas outlet 18, and introducing the gas into the chlorination reactor 1 through the chlorine reactor gas inlet 24 to carry out chlorination reaction on the metal aluminum liquid so as to obtain aluminum trichloride gas; wherein the flow rate of chlorine is 400m 3 And/h, the volume of the metal aluminum liquid accounts for 83% of the total volume of the chlorination reactor 1, and the chlorination reaction temperature is 810 ℃;
the generated aluminum trichloride gas flows out from the air outlet 10 of the chlorination reactor and is introduced into the condenser 2 through the air inlet 11 of the condenser; chlorine gas (wherein the flow rate of the chlorine gas is 400 m) introduced into the condenser 2 from the condenser feed port 13 3 And/h) performing heat exchange between the condensed gas and aluminum trichloride gas therein, and performing condensation crystallization (the crystallization rate is 0.38 kg/s) to obtain a first aluminum trichloride solid and a first tail gas, wherein the particle size of the first aluminum trichloride solid is more than or equal to 1000 mu m; wherein the first tail gas comprises uncondensed aluminum trichloride gas, second aluminum trichloride solid with the particle size less than 1000 mu m and chlorine gas;
the obtained first aluminum trichloride solid is discharged from the condenser discharge port 14 and enters the aluminum trichloride storage tank 4 for storage through the discharge valve 28 and the aluminum trichloride storage tank feed port 15;
the obtained first tail gas flows out from the condenser exhaust port 12, is introduced into the gas-solid separator 3 through the gas-solid separator air inlet 17 for gas-solid separation, and the cutting grain diameter set in the gas-solid separation process is 10 mu m, so that aluminum trichloride seed crystals and second tail gas are respectively obtained; wherein the second tail gas comprises uncondensed aluminum trichloride gas and chlorine gas;
the obtained second tail gas flows out from the gas outlet 18 of the gas-solid separator, and is introduced into the chlorination reactor 1 through the gas inlet 24 of the chlorination reactor to be used as reaction gas and metal aluminum liquid for chlorination reaction;
the obtained aluminum trichloride seed crystal is discharged from a discharge hole 16 of the gas-solid separator, enters the condenser 2 through a feed hole 13 of the condenser and is used as a crystal nucleus to be continuously circularly condensed.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
Claims (10)
1. A continuous production system of aluminum trichloride is characterized by comprising a gas unit, a reaction unit and a circulation unit which are sequentially communicated;
the reaction unit comprises a chlorination reactor (1) and a condenser (2);
the chlorination reactor (1) is provided with a chlorination reactor air outlet (10) and a chlorination reactor air inlet (24);
the condenser (2) is provided with a condenser air inlet (11), a condenser air outlet (12) and a condenser feed inlet (13);
the air outlet (10) of the chlorination reactor is communicated with the air inlet (11) of the condenser;
the circulating unit comprises a gas-solid separator (3), wherein the gas-solid separator (3) is provided with a gas-solid separator discharge port (16) and a gas-solid separator air inlet (17);
the condenser air outlet (12) is communicated with the air inlet (17) of the gas-solid separator;
the discharge hole (16) of the gas-solid separator is communicated with the feed hole (13) of the condenser.
2. The continuous production system of claim 1, wherein the gas unit comprises a chlorine system, or a chlorine system and a condensing system.
3. The continuous production system of claim 2, wherein when the gas unit comprises a chlorine system and a condensing system;
the chlorine system comprises a chlorine storage tank (5) and a chlorine gasifier (6) communicated with an air outlet of the chlorine storage tank (5);
the condensing system comprises a nitrogen storage tank (7) and a nitrogen gasifier (8) communicated with an air outlet of the nitrogen storage tank (7);
the nitrogen gasifier (8) is provided with a nitrogen gasifier air outlet (21), and the nitrogen gasifier air outlet (21) is communicated with the condenser feed inlet (13).
4. A continuous production system according to claim 3, characterized in that when the gas unit comprises a chlorine system and a condensation system, the circulation unit further comprises a heat exchanger (9);
the heat exchanger (9) is provided with a heat exchanger air inlet (19) and a heat exchanger air outlet (20);
the gas-solid separator (3) is provided with a gas outlet (18) of the gas-solid separator;
the gas outlet (18) of the gas-solid separator is communicated with the gas inlet (19) of the heat exchanger; the air outlet (20) of the heat exchanger is communicated with the feeding port (13) of the condenser.
5. The continuous production system of claim 2, wherein when the gas unit comprises a chlorine system;
the chlorine system comprises a chlorine storage tank (5) and a chlorine gasifier (6) communicated with an air outlet of the chlorine storage tank (5);
the chlorine gasifier (6) is provided with a chlorine gasifier air outlet (25); the chlorine gasifier air outlet (25) is communicated with the condenser feed inlet (13);
the gas-solid separator (3) is provided with a gas outlet (18) of the gas-solid separator; the gas outlet (18) of the gas-solid separator is communicated with the gas inlet (24) of the chlorination reactor.
6. The continuous production system according to any one of claims 1 to 5, characterized in that the reaction unit further comprises an aluminum trichloride storage tank (4);
the aluminum trichloride storage tank (4) is provided with an aluminum trichloride storage tank feed inlet (15);
the condenser (2) is provided with a condenser discharge port (14);
the condenser discharge port (14) is communicated with the aluminum trichloride storage tank feed port (15) through a discharge valve (28).
7. A continuous production method of aluminum trichloride, characterized in that the continuous production system according to any one of claims 1 to 6 is employed, comprising the steps of:
continuously inputting chlorine into the chlorination reactor (1) from a gas unit, mixing with metal aluminum liquid, and carrying out chlorination reaction to obtain aluminum trichloride gas;
continuously introducing the aluminum trichloride gas into the condenser (2) for condensation to obtain a first aluminum trichloride solid and a first tail gas respectively; the first tail gas comprises uncondensed aluminum trichloride gas, second aluminum trichloride solids and chlorine gas; the grain diameter of the first aluminum trichloride solid is more than or equal to 1000 mu m; the particle size of the second aluminum trichloride solid is less than 1000 mu m;
continuously introducing the first tail gas into the gas-solid separator (3) to perform gas-solid separation to obtain aluminum trichloride seed crystals and second tail gas respectively; the second tail gas comprises uncondensed aluminum trichloride gas and chlorine gas;
and (3) introducing the aluminum trichloride seed crystal into the condenser (2) for cyclic condensation.
8. The continuous production method of claim 7, wherein when the gas unit comprises a chlorine system and a condensing system;
the chlorine is introduced into the chlorination reactor (1) by a chlorine system via the chlorination reactor gas inlet (24);
nitrogen in the condensing system is introduced into the condenser (2) through the condenser feed inlet (13) and is subjected to heat exchange with the aluminum trichloride gas; the flow of the nitrogen is 100-500 m 3 /h。
9. The continuous production process according to claim 7 or 8, wherein when the gas unit comprises a chlorine system and a condensing system, the recycle unit further comprises a heat exchanger (9), the first and second off-gases further independently comprise nitrogen;
the second tail gas is introduced into the condenser (2) after heat exchange to be used as condensed gas and aluminum trichloride gas for heat exchange;
the heat exchange is carried out in the heat exchanger (9).
10. The continuous production method of claim 7, wherein when the gas unit comprises a chlorine system;
the chlorine is introduced into the condenser (2) through the condenser feed inlet (13) by a chlorine system, flows out of the condenser air outlet (12), is introduced into the gas-solid separator (3) through the gas-solid separator air inlet (17), flows out of the gas-solid separator air outlet (18), and is introduced into the chlorination reactor (1) through the chlorination reactor air inlet (24);
the flow of the chlorine is 200-550 m 3 /h。
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1366845A (en) * | 1962-06-04 | 1964-07-17 | Aluminium Lab Ltd | Evaporation process of a solid aluminum trihalide |
| CN102179027A (en) * | 2010-09-16 | 2011-09-14 | 陕西坚瑞消防股份有限公司 | Ferrocene extinguishing composition |
| CN104817110A (en) * | 2015-03-04 | 2015-08-05 | 郭志斌 | Method for producing high-purity zirconium oxychloride and co-producing silicon tetrachloride through zircon sand boiling chlorination method |
| CN107983272A (en) * | 2016-10-26 | 2018-05-04 | 中国科学院化学研究所 | Sulfide encapsulated particles and preparation method and application |
| CN108751244A (en) * | 2018-07-06 | 2018-11-06 | 北京航天石化技术装备工程有限公司 | A kind of crystallization aluminium salt roasting prepares the integrating device of technical grade aluminium oxide |
| CN108862347A (en) * | 2018-08-01 | 2018-11-23 | 湖南恒光科技股份有限公司 | A kind of system and device and technique of industrial production alchlor |
| CN112520773A (en) * | 2020-11-19 | 2021-03-19 | 衡阳鸿宇化工有限责任公司 | Aluminum trichloride reaction furnace with good air tightness and use method thereof |
-
2022
- 2022-09-06 CN CN202211085569.3A patent/CN115744952B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1366845A (en) * | 1962-06-04 | 1964-07-17 | Aluminium Lab Ltd | Evaporation process of a solid aluminum trihalide |
| CN102179027A (en) * | 2010-09-16 | 2011-09-14 | 陕西坚瑞消防股份有限公司 | Ferrocene extinguishing composition |
| CN104817110A (en) * | 2015-03-04 | 2015-08-05 | 郭志斌 | Method for producing high-purity zirconium oxychloride and co-producing silicon tetrachloride through zircon sand boiling chlorination method |
| CN107983272A (en) * | 2016-10-26 | 2018-05-04 | 中国科学院化学研究所 | Sulfide encapsulated particles and preparation method and application |
| CN108751244A (en) * | 2018-07-06 | 2018-11-06 | 北京航天石化技术装备工程有限公司 | A kind of crystallization aluminium salt roasting prepares the integrating device of technical grade aluminium oxide |
| CN108862347A (en) * | 2018-08-01 | 2018-11-23 | 湖南恒光科技股份有限公司 | A kind of system and device and technique of industrial production alchlor |
| CN112520773A (en) * | 2020-11-19 | 2021-03-19 | 衡阳鸿宇化工有限责任公司 | Aluminum trichloride reaction furnace with good air tightness and use method thereof |
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