CN102320639B - Production system and production method for anhydrous aluminum fluoride - Google Patents
Production system and production method for anhydrous aluminum fluoride Download PDFInfo
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- CN102320639B CN102320639B CN 201110265720 CN201110265720A CN102320639B CN 102320639 B CN102320639 B CN 102320639B CN 201110265720 CN201110265720 CN 201110265720 CN 201110265720 A CN201110265720 A CN 201110265720A CN 102320639 B CN102320639 B CN 102320639B
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Abstract
The invention belongs to the technical field of aluminum fluoride production, concretely discloses a production system and a production method for anhydrous aluminum fluoride. The anhydrous aluminum fluoride production system comprises a hydrofluoric acid evaporator, wherein the hydrofluoric acid evaporator is connected in series to a tail gas heat exchanger, a tail gas outlet and a hydrogen fluoride gas outlet are provided with the tail gas heat exchanger, a tail gas washing apparatus is provided with the tail gas outlet, a gas mixing chamber is provided with the hydrogen fluoride gas outlet, a double-layer fluidized bed reactor is provided with a gas mixture outlet of the gas mixing chamber, the bottom of the double-layer fluidized bed reactor is provided with an aluminum fluoride product outlet, a high temperature tail gas outlet of the double-layer fluidized bed reactor is provided on the top, a reaction material inlet is provided on the double-layer fluidized bed reactor, a first order gas flow reactor is provided at the high temperature tail gas outlet of the double-layer fluidized bed reactor, the first order gas flow reactor is connected in series to a second order gas flow reactor, a third order gas flow reactor and a fourth order gas flow reactor, the second order gas flow reactor, the third order gas flow reactor and the fourth order gas flow reactor are communicated with the double-layer fluidized bed reactor, the fourth order gas flow reactor is communicated with the tail gas heat exchanger.
Description
Technical field
The present invention relates to the aluminum fluoride production technical field, be specifically related to a kind of production system of Anhydrous Aluminium Chloride and adopt this system to produce the method for Anhydrous Aluminium Chloride.
Background technology
Aluminum fluoride (AlF
3) mainly as the fusing assistant of electrolysis of aluminum, can reduce electrolysis temperature, strengthen conductivity, adjust the electrolyte molecule ratio, be conducive to the electrolysis of aluminum oxide and the energy consumption in the reduction electrolytic process.Aluminum fluoride also can be used as the fusing assistant etc. of flux, ceramic glaze and enamel of inhibitor, the non-ferrous metal of side fermentation in the Alcohol Production.
Domestic and international various aluminum fluoride production technique can be divided into dry process and wet processing two large classes at present, wet processing is at present domestic all basic identical, all be to continue to use the water hydrofluoric acid that has take fluorite production that five sixties introduced from USSR (Union of Soviet Socialist Republics) to produce the aluminum fluoride technology as raw material and aluminium hydroxide carry out liquid-solid reaction, its technical process is long, equipment is many, seriously corroded, raw material consumption is high, quality product is low, easily cause downstream industry electrolysis of aluminum environmental pollution serious, along with the development of low-carbon economy and recycling economy, this technique is regulation in 2007 No. 64 " aluminium industry access condition " of National Development and Reform Commission's bulletin: forbid wet processing production aluminium fluoride salt.And dry process mainly is take the hydrogen fluoride of fluorite production as raw material and aluminium hydroxide carries out gas-solid reaction and produces aluminum fluoride, and the flow process of producing according to reaction and equipment difference can be divided into again this technique of Switzerland's cloth that Hunan, domestic Hunan aluminium introduces, the German lurgi process of not introducing, French Bi Shinie technique, U.S. Unichem technique etc.The HF gas that does not purify that these techniques use the higher-grade fluorite to produce mostly, cause the raw materials used cost height of aluminium fluoride product, product foreign matter content height, also there is simultaneously the production capacity problem, the at present domestic aluminum fluoride that adopts is produced the most about 30,000 ton/years of separate unit production capacity, and its major equipment fluidized-bed is crucial.Open up low-grade fluorite, production higher-grade anhydrous hydrogen fluoride, Anhydrous Aluminium Chloride reduce production costs and break through the main points that key takeaway that the fluidized-bed production capacity enlarges also is from now on fluoride salt industry and aluminum electrolysis industry development.
Aluminum fluoride is as one of solvent of electrolytic process, and still electrolytical important component part does not affect electrolytical chemical physical property, and is to adjust electrolyte molecule ratio, the thermally equilibrated important means of control electrolytic process in normal electrolysis production process.The aluminum fluoride chemical physical property difference of producing with different methods is very large, directly affects operation, index, quality product and the environment of electrolysis production.Along with the raising of electrolysis production operant level and automatization control fineness, also more and more higher to the requirement of aluminum fluoride quality.Improvement and perfection has aluminum fluoride by dry process now, and the domestic high-performance of independent research is fluoridized aluminium Product Process route, produces high-quality aluminum fluoride by dry process and be from now on that domestic fluoride salt industry and aluminum electrolysis industry continue, stable, the most important thing that develops in a healthy way.
Summary of the invention
The object of the present invention is to provide a kind of production system of Anhydrous Aluminium Chloride.
The present invention also aims to provide a kind of production method of Anhydrous Aluminium Chloride.
In order to realize above purpose, the technical solution adopted in the present invention is: a kind of production system of Anhydrous Aluminium Chloride, comprise the hydrofluoric acid vaporizer, be provided with hydrofluoric acid entrance and hydrogen fluoride gas the first outlet on the described hydrofluoric acid vaporizer, hydrogen fluoride gas the first outlet string is provided with tail gas heat exchanger, be provided with gas inlet on the tail gas heat exchanger, tail gas outlet and hydrogen fluoride gas the second outlet, described tail gas outlet string is provided with the washing tail gas device, described hydrogen fluoride gas the second outlet string is provided with gas mixing chamber, be provided with hot air inlet and mixed gas outlet on the gas mixing chamber, hot air inlet is connected in series with a hotblast stove, the mixed gas outlet string is provided with double-layer fluidized bed bioreactor, mixed gas outlet is communicated with the bottom of double-layer fluidized bed bioreactor, the bottom of described double-layer fluidized bed bioreactor is provided with the aluminium fluoride product outlet, the top of double-layer fluidized bed bioreactor is provided with the outlet of two-stage fluidized reactor high temperature tail gas, also be provided with the first reacting material inlet on the double-layer fluidized bed bioreactor, the second reacting material inlet and the 3rd reacting material inlet, the first reacting material inlet is communicated with the upper bed layer of double-layer fluidized bed bioreactor, the second reacting material inlet and the 3rd reacting material inlet are communicated with the lower bed layer of double-layer fluidized bed bioreactor, described aluminium fluoride product outlet string is provided with the aluminium fluoride product treatment unit, two-stage fluidized reactor high temperature tail gas outlet string is provided with the one-level gas-flow reactors, be provided with aluminium hydroxide material inlet and one-level gas-flow reactors reacting material outlet on the described one-level gas-flow reactors, one-level gas-flow reactors reacting material outlet is gone here and there successively and is provided with the secondary air flow reactor, three grades of gas-flow reactors and level Four gas-flow reactors, described secondary air flow reactor is communicated with described the first reacting material inlet by a connecting tube, described three grades of gas-flow reactors are communicated with described the second reacting material inlet by a connecting tube, described level Four gas-flow reactors is communicated with described the 3rd reacting material inlet by a connecting tube, be provided with level Four gas-flow reactors tail gas outlet on the level Four gas-flow reactors, described level Four gas-flow reactors tail gas outlet is connected with gas inlet on being arranged on tail gas heat exchanger.
Further, described washing tail gas device is by going here and there successively the first Venturi scrubber of establishing, the second Venturi scrubber and the 3rd Venturi scrubber consist of, be provided with the first Venturi scrubber gas inlet on the first Venturi scrubber, described the first Venturi scrubber gas inlet is connected with tail gas outlet on being arranged on tail gas heat exchanger, be provided with the tail gas emptying pipe on the 3rd Venturi scrubber, the first Venturi scrubber, be provided with the outlet of washings entrance and washings on the second Venturi scrubber and the 3rd Venturi scrubber, described washings entrance is connected with the washings storage tank by the total water inlet pipe of washings, and described washings outlet is connected with the total outlet conduit of washings.
Described aluminium fluoride product treatment unit is made of cool furnace, induced draft fan, fly-ash separator and the aluminum fluoride finished product bin established of string successively, and cool furnace exports with described aluminium fluoride product and is communicated with.
A kind of production method of Anhydrous Aluminium Chloride may further comprise the steps:
(1) anhydrous hydrofluoric acid charging
Anhydrous hydrofluoric acid enters the hydrofluoric acid vaporizer by the hydrofluoric acid entrance, anhydrous hydrofluoric acid passes through the steam-heated cal(l)andria generating gasification in the hydrofluoric acid vaporizer, obtain hydrogen fluoride gas, hydrogen fluoride gas out enters tail gas heat exchanger afterwards from hydrogen fluoride gas the first outlet, hydrogen fluoride gas carries out heat exchange in tail gas heat exchanger with from the level Four gas-flow reactors tail gas of level Four gas-flow reactors, then out enter gas mixing chamber from hydrogen fluoride gas the second outlet, in gas mixing chamber, mix with warm air that hotblast stove provides, send into afterwards the bottom of double-layer fluidized bed bioreactor through mixed gas outlet;
(2) reaction of aluminium hydroxide
Aluminium hydroxide is sent into the one-level gas-flow reactors by the aluminium hydroxide material inlet, aluminium hydroxide is fluidization in the one-level gas-flow reactors, contact with the two-stage fluidized reactor high temperature tail gas from double-layer fluidized bed bioreactor, aluminium hydroxide realizes that dehydration obtains aluminum oxide fully, hydrogen fluoride gas in partial oxidation aluminium and the two-stage fluidized reactor high temperature tail gas reacts, reacted gas-solid mixture material enters the secondary air flow reactor successively by one-level gas-flow reactors reacting material outlet, three grades of gas-flow reactors and level Four gas-flow reactors, at the secondary air flow reactor, realize gas when carrying out gas-solid reaction in three grades of gas-flow reactors and the level Four gas-flow reactors, the separation of two kinds of materials of solid, deliver to the upper bed layer of double-layer fluidized bed bioreactor through the first reacting material inlet by connecting tube from the thick aluminum fluoride of secondary air flow reactor solid materials out, deliver to respectively the lower bed layer of double-layer fluidized bed bioreactor through the second reacting material inlet and the 3rd reacting material inlet by connecting tube from three grades of gas-flow reactors and the thick aluminum fluoride of level Four gas-flow reactors solid materials out, enter tail gas heat exchanger from level Four gas-flow reactors level Four gas-flow reactors tail gas out, in tail gas heat exchanger, finish heat exchange, enter successively afterwards the first Venturi scrubber, the second Venturi scrubber and the 3rd Venturi scrubber cool off washing, the first Venturi scrubber, the sodium aluminum fluoride mother liquor that the washings that the second Venturi scrubber and the 3rd Venturi scrubber use obtains as the sodium aluminum fluoride workshop, the sodium aluminum fluoride mother liquor out is introduced into afterwards the washings storage tank from the sodium aluminum fluoride workshop and stores, enter the washings entrance by the total water inlet pipe of washings afterwards, washings is at the first Venturi scrubber, flow out from the washings outlet after washing finishes in the second Venturi scrubber and the 3rd Venturi scrubber, then enter the sodium aluminum fluoride workshop as sodium aluminum fluoride Workshop Production raw material, through the first Venturi scrubber through the total outlet conduit of washings, the tail gas that obtains after three grades of cooling washings of the second Venturi scrubber and the 3rd Venturi scrubber is emptying by the tail gas emptying pipe that is arranged on the 3rd Venturi scrubber;
(3) reaction of aluminum oxide
Mixed gas from gas mixing chamber evenly enters the two-stage fluidized reactor lower part by the air distribution plate that is arranged on the two-stage fluidized reactor bottom, react with the material on the double-layer fluidized bed bioreactor lower bed layer, the complete hydrogen fluoride gas of unreacted continues the top bed air distribution plate by setting in the double-layer fluidized bed bioreactor in the mixed gas, react with the material on the double-layer fluidized bed bioreactor upper bed layer, the material of upper bed layer is delivered to lower bed layer by upflow tube, the aluminium fluoride product that reaction generates flows out from the bottom of double-layer fluidized bed bioreactor, enter cool furnace, carrying out indirect heat exchange with water coolant in cool furnace cools off, afterwards again through induced draft fan, fly-ash separator enters the aluminum fluoride finished product bin.
The production method of Anhydrous Aluminium Chloride provided by the invention has the following advantages: 1. production method of the present invention is carried out in two steps, be the reaction of aluminium hydroxide and two steps of reaction of aluminum oxide, so feed stock conversion improve the consumption reduction, yield is more than 99%, and production cost is relatively low; 2. the steady quality of aluminium fluoride product, aluminum fluoride master stable content is more than 90% in the product; 3. adopt double-layer fluidized bed bioreactor, gas-solid contact is abundant, has guaranteed the abundant reaction of anhydrous hydrofluoric acid, constant product quality; 4. heat utilization efficiency is high, and energy consumption is low, and the intensification of anhydrous hydrogen fluoride gas utilizes the waste heat of the high-temperature tail gas of Anhydrous Aluminium Chloride reaction unit generation, has reduced the energy expenditure of Anhydrous Aluminium Chloride; 5. vent gas washing system adopts three grades of Venturi scrubbings, has improved the assimilation effect to HF in the tail gas, has guaranteed the qualified discharging of HF in the tail gas; 6. by vent gas washing system the HF in the tail gas and trace solid aluminium hydroxide are collected, raw material as sodium aluminum fluoride Workshop Production sodium aluminum fluoride, the mother liquor of sodium aluminum fluoride returns to vent gas washing system as the washings of three grades of Venturi vent gas washing systems, realize the closed cycle of fluoride waste in two workshop sections in Anhydrous Aluminium Chloride workshop and sodium aluminum fluoride workshop, improved the utilization ratio of raw aluminum hydroxide and anhydrous hydrofluoric acid; 7. there is not discharge of wastewater in the whole production process of the production method of Anhydrous Aluminium Chloride provided by the invention.In sum, the production method of Anhydrous Aluminium Chloride provided by the invention meets the recycling economy that country advocates, and economic benefit, social benefit and environmental benefit are remarkable, belongs to process for cleanly preparing.
Description of drawings
The structural representation of the Anhydrous Aluminium Chloride production system that Fig. 1 provides for the embodiment of the invention 1;
The structural representation of the Anhydrous Aluminium Chloride production system that Fig. 2 provides for the embodiment of the invention 2.
Embodiment
Below by specific embodiment technical scheme of the present invention is elaborated.
As shown in Figure 1, a kind of production system of Anhydrous Aluminium Chloride, comprise hydrofluoric acid vaporizer 2, be provided with hydrofluoric acid entrance 1 and hydrogen fluoride gas the first outlet 3 on the hydrofluoric acid vaporizer 2, hydrogen fluoride gas the first outlet 3 strings are provided with tail gas heat exchanger 6, be provided with gas inlet 27 on the tail gas heat exchanger 6, tail gas outlet 5 and hydrogen fluoride gas the second outlet 4, tail gas outlet 5 strings are provided with washing tail gas device 7, be provided with tail gas emptying pipe 8 on the washing tail gas device 7, hydrogen fluoride gas the second outlet 4 strings are provided with gas mixing chamber 21, be provided with hot air inlet 19 and mixed gas outlet 18 on the gas mixing chamber 21, hot air inlet 19 is connected in series with a hotblast stove 20, mixed gas outlet 18 strings are provided with double-layer fluidized bed bioreactor 25, mixed gas outlet 18 is communicated with the bottom of double-layer fluidized bed bioreactor 25, the bottom of double-layer fluidized bed bioreactor 25 is provided with aluminium fluoride product outlet 16, the top of double-layer fluidized bed bioreactor 25 is provided with two-stage fluidized reactor high temperature tail gas outlet 26, also be provided with the first reacting material inlet 24 on the double-layer fluidized bed bioreactor 25, the second reacting material inlet 23 and the 3rd reacting material inlet 22, the first reacting material inlet 24 is communicated with the upper bed layer of double-layer fluidized bed bioreactor 25, the second reacting material inlet 23 and the 3rd reacting material inlet 22 are communicated with the lower bed layer of double-layer fluidized bed bioreactor 25, aluminium fluoride product outlet 16 strings are provided with aluminium fluoride product treatment unit 17, two-stage fluidized reactor high temperature tail gas outlet 26 strings are provided with one-level gas-flow reactors 14, be provided with aluminium hydroxide material inlet 11 and one-level gas-flow reactors reacting material outlet 13 on the one-level gas-flow reactors 14, one-level gas-flow reactors reacting material outlet 13 is gone here and there successively and is provided with secondary air flow reactor 15, three grades of gas-flow reactors 12 and level Four gas-flow reactors 10, secondary air flow reactor 15 is communicated with the first reacting material inlet 24 by a connecting tube, three grades of gas-flow reactors 12 are communicated with the second reacting material inlet 23 by a connecting tube, level Four gas-flow reactors 10 is communicated with the 3rd reacting material inlet 22 by a connecting tube, be provided with level Four gas-flow reactors tail gas outlet 9 on the level Four gas-flow reactors 10, level Four gas-flow reactors tail gas outlet 9 is connected with gas inlet 27 on being arranged on tail gas heat exchanger 6.
The second reacting material inlet 23 and the 3rd reacting material inlet 22 also can be merged into same import.
As shown in Figure 2, a kind of production system of Anhydrous Aluminium Chloride, comprise hydrofluoric acid vaporizer 2, be provided with hydrofluoric acid entrance 1 and hydrogen fluoride gas the first outlet 3 on the hydrofluoric acid vaporizer 2, hydrogen fluoride gas the first outlet 3 strings are provided with tail gas heat exchanger 6, be provided with gas inlet 27 on the tail gas heat exchanger 6, tail gas outlet 5 and hydrogen fluoride gas the second outlet 4, tail gas outlet 5 successively string is provided with the first Venturi scrubber 33, the second Venturi scrubber 34 and the 3rd Venturi scrubber 35, be provided with the first Venturi scrubber gas inlet 32 on the first Venturi scrubber 33, the first Venturi scrubber gas inlet 32 is connected with tail gas outlet 5 on being arranged on tail gas heat exchanger 6, be provided with tail gas emptying pipe 8 on the 3rd Venturi scrubber 35, the first Venturi scrubber 33, be provided with washings entrance 31 and washings outlet 30 on the second Venturi scrubber 34 and the 3rd Venturi scrubber 35, washings entrance 31 is connected with washings storage tank 36 by the total water inlet pipe 29 of washings, washings outlet 30 is connected with the total outlet conduit 28 of washings, hydrogen fluoride gas the second outlet 4 strings are provided with gas mixing chamber 21, be provided with hot air inlet 19 and mixed gas outlet 18 on the gas mixing chamber 21, hot air inlet 19 is connected in series with a hotblast stove 20, mixed gas outlet 18 strings are provided with double-layer fluidized bed bioreactor 25, mixed gas outlet 18 is communicated with the bottom of double-layer fluidized bed bioreactor 25, the bottom of double-layer fluidized bed bioreactor 25 is provided with aluminium fluoride product outlet 16, the top of double-layer fluidized bed bioreactor 25 is provided with two-stage fluidized reactor high temperature tail gas outlet 26, also be provided with the first reacting material inlet 24 on the double-layer fluidized bed bioreactor 25, the second reacting material inlet 23 and the 3rd reacting material inlet 22, the first reacting material inlet 24 is communicated with the upper bed layer of double-layer fluidized bed bioreactor 25, the second reacting material inlet 23 and the 3rd reacting material inlet 22 are communicated with the lower bed layer of double-layer fluidized bed bioreactor 25, aluminium fluoride product outlet 16 successively string is provided with cool furnace 40, induced draft fan 39, fly-ash separator 38 and aluminum fluoride finished product bin 37, cool furnace 40 is communicated with aluminium fluoride product outlet 16, two-stage fluidized reactor high temperature tail gas outlet 26 strings are provided with one-level gas-flow reactors 14, be provided with aluminium hydroxide material inlet 11 and one-level gas-flow reactors reacting material outlet 13 on the one-level gas-flow reactors 14, one-level gas-flow reactors reacting material outlet 13 is gone here and there successively and is provided with secondary air flow reactor 15, three grades of gas-flow reactors 12 and level Four gas-flow reactors 10, secondary air flow reactor 15 is communicated with the first reacting material inlet 24 by a connecting tube, three grades of gas-flow reactors 12 are communicated with the second reacting material inlet 23 by a connecting tube, level Four gas-flow reactors 10 is communicated with the 3rd reacting material inlet 22 by a connecting tube, be provided with level Four gas-flow reactors tail gas outlet 9 on the level Four gas-flow reactors 10, level Four gas-flow reactors tail gas outlet 9 is connected with gas inlet 27 on being arranged on tail gas heat exchanger 6.
The second reacting material inlet 23 and the 3rd reacting material inlet 22 also can be merged into same import.
A kind of production method of Anhydrous Aluminium Chloride, concrete steps are:
(1) anhydrous hydrofluoric acid charging
The anhydrous hydrofluoric acid pump is sent into hydrofluoric acid vaporizer 2 with the anhydrous hydrofluoric acid of 1000kg after through under meter and control valve metering, anhydrous hydrofluoric acid is gasificated as hydrogen fluoride gas by the steam-heated cal(l)andria generation in hydrofluoric acid vaporizer 2, hydrogen fluoride gas flows out from hydrogen fluoride gas the first outlet 3 afterwards, enter tail gas heat exchanger 6 by by-pass valve control, in tail gas heat exchanger 6 with from the tail gas of level Four gas-flow reactors 10, carry out heat exchange, then out enter gas mixing chamber 21 from hydrogen fluoride gas the second outlet 4, the warm air that provides with hotblast stove 20 in gas mixing chamber 21 mixes, and sends into afterwards the bottom of double-layer fluidized bed bioreactor 25 through mixed gas outlet 18;
(2) reaction of aluminium hydroxide
The aluminium hydroxide of 1300kg is delivered to the aluminium hydroxide feed bin by band elevator, through behind the belt scale metering, send into one-level gas-flow reactors 14 by conveyor screw through aluminium hydroxide material inlet 11 again, aluminium hydroxide is fluidization in one-level gas-flow reactors 14, fully contact with the two-stage fluidized reactor high temperature tail gas from double-layer fluidized bed bioreactor 25, the temperature of two-stage fluidized reactor high temperature tail gas is about 500～600 ℃, main component is unreacted HF, warm air and part water vapor, aluminium hydroxide dewaters fully in one-level gas-flow reactors 14, obtain aluminum oxide, HF reaction in partial oxidation aluminium and the two-stage fluidized reactor high temperature tail gas, reacted gas-solid mixture material enters secondary air flow reactor 15 successively by one-level gas-flow reactors reacting material outlet 13, three grades of gas-flow reactors 12 and level Four gas-flow reactors 10, secondary air flow reactor 15, the principle of work of three grades of gas-flow reactors 12 and level Four gas-flow reactors 10 is identical with cyclonic separator, when carrying out gas-solid reaction, can also realize separating of gas and two kinds of materials of solid, from the thick aluminum fluoride of secondary air flow reactor 15 solid materials out (fluorinated aluminium 1050kg wherein, the about 210kg of aluminum oxide) delivers to the upper bed layer of double-layer fluidized bed bioreactor 25 through the first reacting material inlet 24 by the bottom conveyor screw, deliver to the lower bed layer of double-layer fluidized bed bioreactor 25 through the second reacting material inlet 23 and the 3rd reacting material inlet 22 from three grades of gas-flow reactors 12 and the thick aluminum fluoride of level Four gas-flow reactors 10 solid materials out, enter tail gas heat exchanger 6 from level Four gas-flow reactors 10 level Four gas-flow reactors tail gas out, in tail gas heat exchanger, finish heat exchange, enter successively afterwards the first Venturi scrubber 33, the second Venturi scrubber 34 and the 3rd Venturi scrubber 35 cool off washing, the first Venturi scrubber 33, the sodium aluminum fluoride mother liquor that the washings that the second Venturi scrubber 34 and the 3rd Venturi scrubber 35 use obtains as the sodium aluminum fluoride workshop, the sodium aluminum fluoride mother liquor out is introduced into afterwards from the sodium aluminum fluoride workshop the washings storage tank 36 and stores, enter washings entrance 31 by the total water inlet pipe 29 of washings afterwards, washings is at the first Venturi scrubber 33, flow out from washings outlet 30 after washing finishes in the second Venturi scrubber 34 and the 3rd Venturi scrubber 35, then enter the sodium aluminum fluoride workshop as sodium aluminum fluoride Workshop Production raw material through the total outlet conduit 28 of washings, through the first Venturi scrubber 33, the tail gas that obtains after 35 3 grades of cooling washings of the second Venturi scrubber 34 and the 3rd Venturi scrubber is emptying by tail gas emptying pipe 8;
(3) reaction of aluminum oxide
Mixed gas from gas mixing chamber evenly enters the two-stage fluidized reactor lower part by the air distribution plate that is arranged on the two-stage fluidized reactor bottom, react with the material on the double-layer fluidized bed bioreactor lower bed layer, the complete hydrogen fluoride gas of unreacted continues the top bed air distribution plate by setting in the double-layer fluidized bed bioreactor in the mixed gas, react with the material on the double-layer fluidized bed bioreactor upper bed layer, the material of upper bed layer is delivered to lower bed layer by upflow tube, the aluminum fluoride of the 1340kg that reaction generates (fluorinated aluminium 1280kg wherein, the about 64kg of aluminum oxide) after flowing out, the aluminium fluoride product outlet 16 of two-stage fluidized reactor bottom enters cool furnace, carrying out indirect heat exchange with water coolant in cool furnace cools off, again through induced draft fan and fly-ash separator, be delivered to the aluminum fluoride finished product bin after the cooling.
A kind of production method of Anhydrous Aluminium Chloride, concrete steps are:
(1) anhydrous hydrofluoric acid charging
The anhydrous hydrofluoric acid pump is sent into hydrofluoric acid vaporizer 2 with the anhydrous hydrofluoric acid of 500kg after through under meter and control valve metering, anhydrous hydrofluoric acid is gasificated as hydrogen fluoride gas by the steam-heated cal(l)andria generation in hydrofluoric acid vaporizer 2, hydrogen fluoride gas flows out from hydrogen fluoride gas the first outlet 3 afterwards, enter tail gas heat exchanger 6 by by-pass valve control, in tail gas heat exchanger 6 with from the tail gas of level Four gas-flow reactors 10, carry out heat exchange, then out enter gas mixing chamber 21 from hydrogen fluoride gas the second outlet 4, the warm air that provides with hotblast stove 20 in gas mixing chamber 21 mixes, and sends into afterwards the bottom of double-layer fluidized bed bioreactor 25 through mixed gas outlet 18;
(2) reaction of aluminium hydroxide
The aluminium hydroxide of 650kg is delivered to the aluminium hydroxide feed bin by band elevator, through behind the belt scale metering, send into one-level gas-flow reactors 14 by conveyor screw through aluminium hydroxide material inlet 11 again, aluminium hydroxide is fluidization in one-level gas-flow reactors 14, fully contact with the two-stage fluidized reactor high temperature tail gas from double-layer fluidized bed bioreactor 25, the temperature of two-stage fluidized reactor high temperature tail gas is about 500～600 ℃, main component is unreacted HF, warm air and part water vapor, aluminium hydroxide dewaters fully in one-level gas-flow reactors 14, obtain aluminum oxide, HF reaction in partial oxidation aluminium and the two-stage fluidized reactor high temperature tail gas, reacted gas-solid mixture material enters secondary air flow reactor 15 successively by one-level gas-flow reactors reacting material outlet 13, three grades of gas-flow reactors 12 and level Four gas-flow reactors 10, secondary air flow reactor 15, the principle of work of three grades of gas-flow reactors 12 and level Four gas-flow reactors 10 is identical with cyclonic separator, when carrying out gas-solid reaction, can also realize separating of gas and two kinds of materials of solid, from the thick aluminum fluoride of secondary air flow reactor 15 solid materials out (fluorinated aluminium 1050kg wherein, the about 210kg of aluminum oxide) delivers to the upper bed layer of double-layer fluidized bed bioreactor 25 through the first reacting material inlet 24 by the bottom conveyor screw, deliver to the lower bed layer of double-layer fluidized bed bioreactor 25 through the second reacting material inlet 23 and the 3rd reacting material inlet 22 from three grades of gas-flow reactors 12 and the thick aluminum fluoride of level Four gas-flow reactors 10 solid materials out, enter tail gas heat exchanger 6 from level Four gas-flow reactors 10 level Four gas-flow reactors tail gas out, in tail gas heat exchanger, finish heat exchange, enter successively afterwards the first Venturi scrubber 33, the second Venturi scrubber 34 and the 3rd Venturi scrubber 35 cool off washing, the first Venturi scrubber 33, the sodium aluminum fluoride mother liquor that the washings that the second Venturi scrubber 34 and the 3rd Venturi scrubber 35 use obtains as the sodium aluminum fluoride workshop, the sodium aluminum fluoride mother liquor out is introduced into afterwards from the sodium aluminum fluoride workshop the washings storage tank 36 and stores, enter washings entrance 31 by the total water inlet pipe 29 of washings afterwards, washings is at the first Venturi scrubber 33, flow out from washings outlet 30 after washing finishes in the second Venturi scrubber 34 and the 3rd Venturi scrubber 35, then enter the sodium aluminum fluoride workshop as sodium aluminum fluoride Workshop Production raw material through the total outlet conduit 28 of washings, through the first Venturi scrubber 33, the tail gas that obtains after 35 3 grades of cooling washings of the second Venturi scrubber 34 and the 3rd Venturi scrubber is emptying by tail gas emptying pipe 8;
(3) reaction of aluminum oxide
Mixed gas from gas mixing chamber evenly enters the two-stage fluidized reactor lower part by the air distribution plate that is arranged on the two-stage fluidized reactor bottom, react with the material on the double-layer fluidized bed bioreactor lower bed layer, the complete hydrogen fluoride gas of unreacted continues the top bed air distribution plate by setting in the double-layer fluidized bed bioreactor in the mixed gas, react with the material on the double-layer fluidized bed bioreactor upper bed layer, the material of upper bed layer is delivered to lower bed layer by upflow tube, the aluminum fluoride of the 690kg that reaction generates (fluorinated aluminium 645kg wherein, the about 45kg of aluminum oxide) after flowing out, the aluminium fluoride product outlet 16 of two-stage fluidized reactor bottom enters cool furnace, carrying out indirect heat exchange with water coolant in cool furnace cools off, again through induced draft fan and fly-ash separator, be delivered to the aluminum fluoride finished product bin after the cooling.
The mass analysis of the Anhydrous Aluminium Chloride finished product that embodiment 3 and embodiment 4 make the results are shown in Table shown in 1.
The mass analysis result of table 1 Anhydrous Aluminium Chloride finished product
Claims (3)
1. the production system of an Anhydrous Aluminium Chloride, it is characterized in that, comprise the hydrofluoric acid vaporizer, be provided with hydrofluoric acid entrance and hydrogen fluoride gas the first outlet on the described hydrofluoric acid vaporizer, hydrogen fluoride gas the first outlet string is provided with tail gas heat exchanger, be provided with gas inlet on the tail gas heat exchanger, tail gas outlet and hydrogen fluoride gas the second outlet, described tail gas outlet string is provided with the washing tail gas device, described hydrogen fluoride gas the second outlet string is provided with gas mixing chamber, be provided with hot air inlet and mixed gas outlet on the gas mixing chamber, hot air inlet is connected in series with a hotblast stove, the mixed gas outlet string is provided with double-layer fluidized bed bioreactor, mixed gas outlet is communicated with the bottom of double-layer fluidized bed bioreactor, the bottom of described double-layer fluidized bed bioreactor is provided with the aluminium fluoride product outlet, the top of double-layer fluidized bed bioreactor is provided with the outlet of two-stage fluidized reactor high temperature tail gas, also be provided with the first reacting material inlet on the double-layer fluidized bed bioreactor, the second reacting material inlet and the 3rd reacting material inlet, the first reacting material inlet is communicated with the upper bed layer of double-layer fluidized bed bioreactor, the second reacting material inlet and the 3rd reacting material inlet are communicated with the lower bed layer of double-layer fluidized bed bioreactor, described aluminium fluoride product outlet string is provided with the aluminium fluoride product treatment unit, two-stage fluidized reactor high temperature tail gas outlet string is provided with the one-level gas-flow reactors, be provided with aluminium hydroxide material inlet and one-level gas-flow reactors reacting material outlet on the described one-level gas-flow reactors, one-level gas-flow reactors reacting material outlet is gone here and there successively and is provided with the secondary air flow reactor, three grades of gas-flow reactors and level Four gas-flow reactors, described secondary air flow reactor is communicated with described the first reacting material inlet by a connecting tube, described three grades of gas-flow reactors are communicated with described the second reacting material inlet by a connecting tube, described level Four gas-flow reactors is communicated with described the 3rd reacting material inlet by a connecting tube, be provided with level Four gas-flow reactors tail gas outlet on the level Four gas-flow reactors, described level Four gas-flow reactors tail gas outlet is connected with gas inlet on being arranged on tail gas heat exchanger; Described washing tail gas device is by going here and there successively the first Venturi scrubber of establishing, the second Venturi scrubber and the 3rd Venturi scrubber consist of, be provided with the first Venturi scrubber gas inlet on the first Venturi scrubber, described the first Venturi scrubber gas inlet is connected with tail gas outlet on being arranged on tail gas heat exchanger, be provided with the tail gas emptying pipe on the 3rd Venturi scrubber, the first Venturi scrubber, be provided with the outlet of washings entrance and washings on the second Venturi scrubber and the 3rd Venturi scrubber, described washings entrance is connected with the washings storage tank by the total water inlet pipe of washings, and described washings outlet is connected with the total outlet conduit of washings.
2. the production system of Anhydrous Aluminium Chloride according to claim 1, it is characterized in that, described aluminium fluoride product treatment unit is made of cool furnace, induced draft fan, fly-ash separator and the aluminum fluoride finished product bin established of string successively, and cool furnace exports with described aluminium fluoride product and is communicated with.
3. the production method of an Anhydrous Aluminium Chloride is characterized in that, may further comprise the steps:
(1) anhydrous hydrofluoric acid charging
Anhydrous hydrofluoric acid enters the hydrofluoric acid vaporizer by the hydrofluoric acid entrance, anhydrous hydrofluoric acid passes through the steam-heated cal(l)andria generating gasification in the hydrofluoric acid vaporizer, obtain hydrogen fluoride gas, hydrogen fluoride gas out enters tail gas heat exchanger afterwards from hydrogen fluoride gas the first outlet, hydrogen fluoride gas carries out heat exchange in tail gas heat exchanger with from the level Four gas-flow reactors tail gas of level Four gas-flow reactors, then out enter gas mixing chamber from hydrogen fluoride gas the second outlet, in gas mixing chamber, mix with warm air that hotblast stove provides, send into afterwards the bottom of double-layer fluidized bed bioreactor through mixed gas outlet;
(2) reaction of aluminium hydroxide
Aluminium hydroxide is sent into the one-level gas-flow reactors by the aluminium hydroxide material inlet, aluminium hydroxide is fluidization in the one-level gas-flow reactors, contact with the two-stage fluidized reactor high temperature tail gas from double-layer fluidized bed bioreactor, aluminium hydroxide realizes that dehydration obtains aluminum oxide fully, hydrogen fluoride gas in partial oxidation aluminium and the two-stage fluidized reactor high temperature tail gas reacts, reacted gas-solid mixture material enters the secondary air flow reactor successively by one-level gas-flow reactors reacting material outlet, three grades of gas-flow reactors and level Four gas-flow reactors, at the secondary air flow reactor, realize gas when carrying out gas-solid reaction in three grades of gas-flow reactors and the level Four gas-flow reactors, the separation of two kinds of materials of solid, deliver to the upper bed layer of double-layer fluidized bed bioreactor through the first reacting material inlet by connecting tube from the thick aluminum fluoride of secondary air flow reactor solid materials out, deliver to respectively the lower bed layer of double-layer fluidized bed bioreactor through the second reacting material inlet and the 3rd reacting material inlet by connecting tube from three grades of gas-flow reactors and the thick aluminum fluoride of level Four gas-flow reactors solid materials out, enter tail gas heat exchanger from level Four gas-flow reactors level Four gas-flow reactors tail gas out, in tail gas heat exchanger, finish heat exchange, enter successively afterwards the first Venturi scrubber, the second Venturi scrubber and the 3rd Venturi scrubber cool off washing, the first Venturi scrubber, the sodium aluminum fluoride mother liquor that the washings that the second Venturi scrubber and the 3rd Venturi scrubber use obtains as the sodium aluminum fluoride workshop, washings is at the first Venturi scrubber, flow out from the washings outlet after washing finishes in the second Venturi scrubber and the 3rd Venturi scrubber, then enter the sodium aluminum fluoride workshop as sodium aluminum fluoride Workshop Production raw material, through the first Venturi scrubber through the total outlet conduit of washings, the tail gas that obtains after three grades of cooling washings of the second Venturi scrubber and the 3rd Venturi scrubber is emptying by the tail gas emptying pipe that is arranged on the 3rd Venturi scrubber;
(3) reaction of aluminum oxide
Mixed gas from gas mixing chamber evenly enters the two-stage fluidized reactor lower part by the air distribution plate that is arranged on the two-stage fluidized reactor bottom, react with the material on the double-layer fluidized bed bioreactor lower bed layer, the complete hydrogen fluoride gas of unreacted continues the top bed air distribution plate by setting in the double-layer fluidized bed bioreactor in the mixed gas, react with the material on the double-layer fluidized bed bioreactor upper bed layer, the material of upper bed layer is delivered to lower bed layer by upflow tube, the aluminium fluoride product that reaction generates flows out from the bottom of double-layer fluidized bed bioreactor, enter cool furnace, carrying out indirect heat exchange with water coolant in cool furnace cools off, afterwards again through induced draft fan, fly-ash separator enters the aluminum fluoride finished product bin.
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| CN102631819A (en) * | 2012-05-08 | 2012-08-15 | 江西六国化工有限责任公司 | Tail gas washing method for reducing ammonia consumption |
| CN104714507A (en) * | 2013-12-17 | 2015-06-17 | 天津金牛电源材料有限责任公司 | Automatic anhydrous hydrofluoric acid measuring and feeding system |
| CN103877916B (en) * | 2014-03-15 | 2015-08-12 | 宜章弘源化工有限责任公司 | Fluidized bed tail gas utilization method and equipment in dry-method aluminum fluoride production |
| CN106830034A (en) * | 2017-02-09 | 2017-06-13 | 武汉工程大学 | A kind of utilization fluoride waste prepares the method and device of sand like synthetic cryolite |
| CN108840358B (en) * | 2018-09-13 | 2023-07-18 | 衢州市鼎盛化工科技有限公司 | Device and method for preparing anhydrous aluminum fluoride |
| CN111517348A (en) * | 2020-04-01 | 2020-08-11 | 白银中天化工有限责任公司 | Production process for regenerating aluminum fluoride by using aluminum fluoride production tail gas washing liquid |
| CN115869864B (en) * | 2022-12-27 | 2024-06-25 | 兰州理工大学 | Production system and method of anhydrous aluminum fluoride |
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| CN101077786A (en) * | 2006-05-22 | 2007-11-28 | 多氟多化工股份有限公司 | Method for preparing aluminum fluoride |
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