CN102320639A - 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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- CN102320639A CN102320639A CN201110265720A CN201110265720A CN102320639A CN 102320639 A CN102320639 A CN 102320639A CN 201110265720 A CN201110265720 A CN 201110265720A CN 201110265720 A CN201110265720 A CN 201110265720A CN 102320639 A CN102320639 A CN 102320639A
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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 ALUMNIUM 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
ALUMNIUM FLUORIDE (AlF
3) mainly as the fusing assistant of electrolysis of aluminum, can reduce electrolysis temperature, strengthen conductivity, adjustment electrolyte molecule ratio helps the electrolysis and the energy consumption that reduces in the electrolytic process of aluminum oxide.ALUMNIUM FLUORIDE also can be used as the suppressor factor of side fermentation in the ethanol produce, flux, ceramic glaze and the enamelled fusing assistant etc. of non-ferrous metal.
Domestic and international various ALUMNIUM FLUORIDE production technique can be divided into dry process and wet processing two big classes at present; Wet processing is at present domestic all basic identical; All be that to continue to use for five sixties be that raw material and white lake carry out liquid-solid reaction to produce ALUMNIUM FLUORIDE technological from the water hydrofluoric acid that has with fluorite production that the FSU introduces; Its technical process is long, equipment is many, seriously corroded, raw material consumption height, quality product are low; Be prone to cause downstream industry electrolysis of aluminum environmental pollution serious; Along with the development of low-carbon economy and recycling economy, this technology is regulation in 2007 No. 64 " aluminium industry access condition " of National Development and Reform Commission bulletin: forbid that wet processing production aluminium uses fluoride salt.And dry process mainly to be hydrogen fluoride with fluorite production be raw material and white lake carries out gas-solid reaction and produces ALUMNIUM FLUORIDE, can be divided into this technology of Switzerland's cloth that Hunan, domestic Hunan aluminium introduces, the German lurgi process of not introducing, French Bi Shinie technology, U.S. Unichem technology etc. again according to the flow process of reacted and equipment difference.The HF gas that does not purify that these technologies 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 the production capacity problem simultaneously; The at present domestic ALUMNIUM FLUORIDE that adopts is produced the most about 30,000 tons/year 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, reducing production costs and breaking through key takeaway that the fluidized-bed production capacity enlarges also is the main points that develop of fluoride salt industry and aluminum electrolysis industry from now on.
ALUMNIUM FLUORIDE is as one of solvent of electrolytic process, and still not electrolytical important component part influences electrolytical chemical physical property, and is the adjustment electrolyte molecule in normal electrolysis production process than, the thermally equilibrated important means of control electrolytic process.The ALUMNIUM FLUORIDE chemical physical property difference of producing with different methods is very big, directly influences operation, index, quality product and the environment of electrolysis production.Along with the raising of electrolysis production operant level and robotization control fineness, also increasingly high to the requirement of ALUMNIUM FLUORIDE quality.Improve and improve existing aluminum fluoride by dry process, the domestic high-performance of independent research is fluoridized aluminium product operational path, and producing high-quality aluminum fluoride by dry process is the most important thing that domestic from now on fluoride salt industry and aluminum electrolysis industry continue, stablize, develop 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 working method of Anhydrous Aluminium Chloride.
In order to realize above purpose; The technical scheme that the present invention adopted is: a kind of production system of Anhydrous Aluminium Chloride; Comprise the hydrofluoric acid vaporizer; Said hydrofluoric acid vaporizer is provided with hydrofluoric acid inlet and hydrogen fluoride gas first outlet, and the hydrogen fluoride gas first outlet string is provided with tail gas heat exchanger, and tail gas heat exchanger is provided with gas inlet, tail gas outlet and hydrogen fluoride gas second outlet; Said tail gas outlet string is provided with the washing tail gas device; The said hydrogen fluoride gas second outlet string is provided with gas mixing chamber, and gas mixing chamber is provided with hot air inlet and mixed gas outlet, and 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, and the bottom of said double-layer fluidized bed bioreactor is provided with the aluminium fluoride product outlet, and 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 first reacting material inlet, second reacting material inlet and the 3rd reacting material inlet on the double-layer fluidized bed bioreactor; First reacting material inlet is communicated with the upper bed layer of double-layer fluidized bed bioreactor, and second reacting material inlet and the 3rd reacting material inlet are communicated with the lower bed layer of double-layer fluidized bed bioreactor, and said 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; Said one-level gas-flow reactors is provided with white lake material inlet and one-level gas-flow reactors reacting material outlet, and one-level gas-flow reactors reacting material outlet is gone here and there successively and is provided with secondary air flow reactor drum, three grades of gas-flow reactors and level Four gas-flow reactors, and said secondary air flow reactor drum is communicated with said first reacting material inlet through a connecting tube; Said three grades of gas-flow reactors are communicated with said second reacting material inlet through a connecting tube; Said level Four gas-flow reactors is communicated with said the 3rd reacting material inlet through a connecting tube, and the level Four gas-flow reactors is provided with level Four gas-flow reactors tail gas and exports, said level Four gas-flow reactors tail gas export be arranged on tail gas heat exchanger on gas inlet be connected.
Further; Said washing tail gas device is made up of first Venturi scrubber, second Venturi scrubber and the 3rd Venturi scrubber established of string successively; First Venturi scrubber is provided with the first Venturi scrubber gas inlet; The said first Venturi scrubber gas inlet is connected with tail gas outlet on being arranged on tail gas heat exchanger; The 3rd Venturi scrubber is provided with the tail gas emptying pipe; Be provided with washings inlet and washings outlet on first Venturi scrubber, second Venturi scrubber and the 3rd Venturi scrubber, said washings inlet is connected with the washings storage tank through the total water inlet pipe of washings, and said washings outlet is connected with the total outlet conduit of washings.
Said aluminium fluoride product treatment unit is made up of cool furnace, induced draft fan, fly-ash separator and the ALUMNIUM FLUORIDE finished product bin established of string successively, and cool furnace exports with said aluminium fluoride product and is communicated with.
A kind of working method of Anhydrous Aluminium Chloride may further comprise the steps:
(1) anhydrous hydrofluoric acid charging
Anhydrous hydrofluoric acid gets into the hydrofluoric acid vaporizer through the hydrofluoric acid inlet; 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 gets into tail gas heat exchanger from hydrogen fluoride gas first back of coming out, and hydrogen fluoride gas carries out heat exchange with level Four gas-flow reactors tail gas from the level Four gas-flow reactors in tail gas heat exchanger, come out to get into gas mixing chamber from hydrogen fluoride gas second then; In gas mixing chamber, mix, send into the bottom of double-layer fluidized bed bioreactor afterwards through mixed gas outlet with warm air that hotblast stove provides;
(2) reaction of white lake
White lake is sent into the one-level gas-flow reactors through the white lake material inlet; White lake is fluidization in the one-level gas-flow reactors; Contact with two-stage fluidized reactor high temperature tail gas from double-layer fluidized bed bioreactor; White lake realizes that dehydration obtains aluminum oxide fully; Hydrogen fluoride gas in partially oxidation aluminium and the two-stage fluidized reactor high temperature tail gas reacts; Reacted gas-solid mixture material gets into secondary air flow reactor drum, three grades of gas-flow reactors and level Four gas-flow reactors successively through one-level gas-flow reactors reacting material outlet; Realize separating of gas, two kinds of materials of solid when in secondary air flow reactor drum, three grades of gas-flow reactors and level Four gas-flow reactors, carrying out gas-solid reaction; The thick ALUMNIUM FLUORIDE of solid materials that comes out from the secondary air flow reactor drum is delivered to the upper bed layer of double-layer fluidized bed bioreactor through first reacting material inlet through connecting tube; The thick ALUMNIUM FLUORIDE of solid materials that comes out from three grades of gas-flow reactors and level Four gas-flow reactors is delivered to the lower bed layer of double-layer fluidized bed bioreactor respectively through second reacting material inlet and the 3rd reacting material inlet through connecting tube; The level Four gas-flow reactors tail gas that comes out from the level Four gas-flow reactors gets into tail gas heat exchanger; In tail gas heat exchanger, accomplish heat exchange; Get into first Venturi scrubber, second Venturi scrubber and the 3rd Venturi scrubber afterwards successively and cool off washing, the sodium aluminum fluoride mother liquor that the washings that first Venturi scrubber, second Venturi scrubber and the 3rd Venturi scrubber use obtains as the sodium aluminum fluoride workshop, sodium aluminum fluoride mother liquor are introduced into the washings storage tank after coming out in the sodium aluminum fluoride workshop and store; Get into the washings inlet through the total water inlet pipe of washings afterwards; Washings washs in first Venturi scrubber, second Venturi scrubber and the 3rd Venturi scrubber and finishes the back from washings outlet outflow, gets into the sodium aluminum fluoride workshop as sodium aluminum fluoride Workshop Production raw material through the total outlet conduit of washings then, and the tail gas that after first Venturi scrubber, second Venturi scrubber and three grades of cooling washings of the 3rd Venturi scrubber, obtains is through being arranged on the tail gas emptying pipe emptying on the 3rd Venturi scrubber;
(3) reaction of aluminum oxide
Mixed gas from gas mixing chamber evenly gets into the two-stage fluidized reactor lower part through 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 intact hydrogen fluoride gas of unreacted continues the top bed air distribution plate through 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 through upflow tube, and the aluminium fluoride product that reaction generates flows out from the bottom of double-layer fluidized bed bioreactor; Get into cool furnace; In cool furnace, carry out indirect heat exchange and cool off,, get into the ALUMNIUM FLUORIDE finished product bin afterwards again through induced draft fan, fly-ash separator with water coolant.
The working method of Anhydrous Aluminium Chloride provided by the invention has the following advantages: working method 1. of the present invention is carried out in two steps; Be the reaction of white lake 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, ALUMNIUM FLUORIDE master stable content is more than 90% in the product; 3. adopt double-layer fluidized bed bioreactor, gas-solid full contact 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. the washing tail gas 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. through the washing tail gas system HF in the tail gas and micro-solid aluminum hydroxide are collected; Raw material as sodium aluminum fluoride Workshop Production sodium aluminum fluoride; The mother liquor of sodium aluminum fluoride returns the washing tail gas system again as the washings of three grades of Venturi washing tail gas systems; Realized the closed cycle of fluoride waste, improved the utilization ratio of raw aluminum hydroxide and anhydrous hydrofluoric acid in two workshop sections in Anhydrous Aluminium Chloride workshop and sodium aluminum fluoride workshop; 7. there is not discharge of wastewater in the whole process of production of the working method of Anhydrous Aluminium Chloride provided by the invention.In sum, the working 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
Through specific embodiment technical scheme of the present invention is elaborated below.
As shown in Figure 1; A kind of production system of Anhydrous Aluminium Chloride; Comprise hydrofluoric acid vaporizer 2; Hydrofluoric acid vaporizer 2 is provided with hydrofluoric acid inlet 1 and hydrogen fluoride gas first outlet 3; Hydrogen fluoride gas first outlet 3 strings are provided with tail gas heat exchanger 6, and tail gas heat exchanger 6 is provided with gas inlet 27, tail gas outlet 5 and hydrogen fluoride gas second outlet 4, and tail gas outlet 5 strings are provided with washing tail gas device 7; Washing tail gas device 7 is provided with tail gas emptying pipe 8; Hydrogen fluoride gas second outlet 4 strings are provided with gas mixing chamber 21, and gas mixing chamber 21 is provided with hot air inlet 19 and mixed gas outlet 18, and 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, and the bottom of double-layer fluidized bed bioreactor 25 is provided with aluminium fluoride product outlet 16, and 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 first reacting material inlet 24, second reacting material inlet 23 and the 3rd reacting material inlet 22 on the double-layer fluidized bed bioreactor 25; First reacting material inlet 24 is communicated with the upper bed layer of double-layer fluidized bed bioreactor 25, and 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, and 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; One-level gas-flow reactors 14 is provided with white lake material inlet 11 and one-level gas-flow reactors reacting material outlet 13, and one-level gas-flow reactors reacting material outlet 13 go here and there successively and is provided with secondary air flow reactor drum 15, three grades of gas-flow reactors 12 and level Four gas-flow reactors 10, and secondary air flow reactor drum 15 passes through a connecting tube and is communicated with first reacting material inlet 24; Three grades of gas-flow reactors 12 are communicated with second reacting material inlet 23 through a connecting tube; Level Four gas-flow reactors 10 is communicated with the 3rd reacting material inlet 22 through a connecting tube, and level Four gas-flow reactors 10 is provided with level Four gas-flow reactors tail gas and exports 9, level Four gas-flow reactors tail gas export 9 be arranged on tail gas heat exchanger 6 on gas inlet 27 be connected.
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; Hydrofluoric acid vaporizer 2 is provided with hydrofluoric acid inlet 1 and hydrogen fluoride gas first outlet 3; Hydrogen fluoride gas first outlet 3 strings are provided with tail gas heat exchanger 6, and tail gas heat exchanger 6 is provided with gas inlet 27, tail gas outlet 5 and hydrogen fluoride gas second outlet 4, and tail gas outlet 5 string successively is provided with first Venturi scrubber 33, second Venturi scrubber 34 and the 3rd Venturi scrubber 35; First Venturi scrubber 33 is provided with the first Venturi scrubber gas inlet 32; The first Venturi scrubber gas inlet 32 is connected with tail gas outlet 5 on being arranged on tail gas heat exchanger 6, and the 3rd Venturi scrubber 35 is provided with and is provided with washings inlet 31 on tail gas emptying pipe 8, the first Venturi scrubbers 33, second Venturi scrubber 34 and the 3rd Venturi scrubber 35 and washings exports 30; Washings inlet 31 is connected with washings storage tank 36 through the total water inlet pipe 29 of washings; Washings outlet 30 is connected with the total outlet conduit 28 of washings, and hydrogen fluoride gas second outlet 4 is gone here and there and is provided with gas mixing chamber 21, and gas mixing chamber 21 is provided with hot air inlet 19 and mixed gas outlet 18; 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, and mixed gas outlet 18 is communicated with the bottom of double-layer fluidized bed bioreactor 25, and 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 first reacting material inlet 24, second reacting material inlet 23 and the 3rd reacting material inlet 22, the first reacting material inlets 24 on the double-layer fluidized bed bioreactor 25 and be communicated with the upper bed layer of double-layer fluidized bed bioreactor 25, 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 string successively is provided with cool furnace 40, induced draft fan 39, fly-ash separator 38 and ALUMNIUM FLUORIDE finished product bin 37; Cool furnace 40 is communicated with aluminium fluoride product outlet 16, and two-stage fluidized reactor high temperature tail gas outlet 26 strings are provided with one-level gas-flow reactors 14, and one-level gas-flow reactors 14 is provided with white lake material inlet 11 and one-level gas-flow reactors reacting material outlet 13; One-level gas-flow reactors reacting material outlet 13 is gone here and there successively and is provided with secondary air flow reactor drum 15, three grades of gas-flow reactors 12 and level Four gas-flow reactors 10; Secondary air flow reactor drum 15 is communicated with first reacting material inlet 24 through a connecting tube, and three grades of gas-flow reactors 12 are communicated with second reacting material inlet 23 through a connecting tube, and level Four gas-flow reactors 10 is communicated with the 3rd reacting material inlet 22 through a connecting tube; Level Four gas-flow reactors 10 is provided with level Four gas-flow reactors tail gas outlet 9, and level Four gas-flow reactors tail gas outlet 9 is connected with gas inlet 27 on being arranged on tail gas heat exchanger 6.
Second reacting material inlet 23 and the 3rd reacting material inlet 22 also can be merged into same import.
A kind of working 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 after the anhydrous hydrofluoric acid of 1000kg is measured through under meter and valve; Anhydrous hydrofluoric acid is gasificated as hydrogen fluoride gas through the steam-heated cal(l)andria generation in hydrofluoric acid vaporizer 2; Hydrogen fluoride gas flows out from hydrogen fluoride gas first outlet 3 afterwards; Get into tail gas heat exchanger 6 through by-pass valve control, tail gas heat exchanger 6 in, carry out heat exchange, export 4 from hydrogen fluoride gas second then and come out to get into gas mixing chamber 21 with tail gas from level Four gas-flow reactors 10; The warm air that in gas mixing chamber 21, provides with hotblast stove 20 mixes, and sends into the bottom of double-layer fluidized bed bioreactor 25 afterwards through mixed gas outlet 18;
(2) reaction of white lake
The white lake of 1300kg is delivered to the white lake feed bin through band elevator; After the weighing belt metering; Send into one-level gas-flow reactors 14 through conveyor screw through white lake material inlet 11 again; White lake is fluidization in one-level gas-flow reactors 14; Fully contact with 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 ℃; Staple is unreacted HF, warm air and portion water steam; White lake dewaters fully in one-level gas-flow reactors 14; Obtain aluminum oxide; HF reaction in partially oxidation aluminium and the two-stage fluidized reactor high temperature tail gas; Reacted gas-solid mixture material gets into secondary air flow reactor drum 15, three grades of gas-flow reactors 12 and level Four gas-flow reactors 10 successively through one-level gas-flow reactors reacting material outlet 13, and the principle of work of secondary air flow reactor drum 15, 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; The thick ALUMNIUM FLUORIDE of solid materials that comes out from secondary air flow reactor drum 15 (fluorinated aluminium 1050kg wherein; The about 210kg of aluminum oxide) deliver to the upper bed layer of double-layer fluidized bed bioreactor 25 through the bottom conveyor screw through first reacting material inlet 24, the thick ALUMNIUM FLUORIDE of solid materials that comes out from three grades of gas-flow reactors 12 and level Four gas-flow reactors 10 is delivered to the lower bed layer of double-layer fluidized bed bioreactor 25 through second reacting material inlet 23 and the 3rd reacting material inlet 22, the level Four gas-flow reactors tail gas entering tail gas heat exchanger 6 of coming out from level Four gas-flow reactors 10; In tail gas heat exchanger, accomplish heat exchange; Get into first Venturi scrubber 33, second Venturi scrubber 34 and the 3rd Venturi scrubber 35 afterwards successively and cool off washing, the sodium aluminum fluoride mother liquor that the washings that first Venturi scrubber 33, second Venturi scrubber 34 and the 3rd Venturi scrubber 35 use obtains as the sodium aluminum fluoride workshop, the sodium aluminum fluoride mother liquor is introduced into after coming out in the sodium aluminum fluoride workshop the washings storage tank 36 and stores; Get into washings inlet 31 through the total water inlet pipe 29 of washings afterwards; Flow out from washings outlet 30 washings washing in first Venturi scrubber 33, second Venturi scrubber 34 and the 3rd Venturi scrubber 35 end back, gets into the sodium aluminum fluoride workshops as sodium aluminum fluoride Workshop Production raw material through the total outlet conduit 28 of washings then, and the tail gas that after first Venturi scrubber 33, second Venturi scrubber 34 and 35 3 grades of cooling washings of the 3rd Venturi scrubber, obtains passes through 8 emptyings of tail gas emptying pipe;
(3) reaction of aluminum oxide
Mixed gas from gas mixing chamber evenly gets into the two-stage fluidized reactor lower part through 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 intact hydrogen fluoride gas of unreacted continues the top bed air distribution plate through 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 through upflow tube, the ALUMNIUM FLUORIDE of the 1340kg that reaction generates (fluorinated aluminium 1280kg wherein; The about 64kg of aluminum oxide) flows out the back from the aluminium fluoride product outlet 16 of two-stage fluidized reactor bottom and get into cool furnace; In cool furnace, carry out indirect heat exchange and cool off, again through induced draft fan and fly-ash separator, be delivered to the ALUMNIUM FLUORIDE finished product bin after the cooling with water coolant.
A kind of working 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 after the anhydrous hydrofluoric acid of 500kg is measured through under meter and valve; Anhydrous hydrofluoric acid is gasificated as hydrogen fluoride gas through the steam-heated cal(l)andria generation in hydrofluoric acid vaporizer 2; Hydrogen fluoride gas flows out from hydrogen fluoride gas first outlet 3 afterwards; Get into tail gas heat exchanger 6 through by-pass valve control, tail gas heat exchanger 6 in, carry out heat exchange, export 4 from hydrogen fluoride gas second then and come out to get into gas mixing chamber 21 with tail gas from level Four gas-flow reactors 10; The warm air that in gas mixing chamber 21, provides with hotblast stove 20 mixes, and sends into the bottom of double-layer fluidized bed bioreactor 25 afterwards through mixed gas outlet 18;
(2) reaction of white lake
The white lake of 650kg is delivered to the white lake feed bin through band elevator; After the weighing belt metering; Send into one-level gas-flow reactors 14 through conveyor screw through white lake material inlet 11 again; White lake is fluidization in one-level gas-flow reactors 14; Fully contact with 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 ℃; Staple is unreacted HF, warm air and portion water steam; White lake dewaters fully in one-level gas-flow reactors 14; Obtain aluminum oxide; HF reaction in partially oxidation aluminium and the two-stage fluidized reactor high temperature tail gas; Reacted gas-solid mixture material gets into secondary air flow reactor drum 15, three grades of gas-flow reactors 12 and level Four gas-flow reactors 10 successively through one-level gas-flow reactors reacting material outlet 13, and the principle of work of secondary air flow reactor drum 15, 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; The thick ALUMNIUM FLUORIDE of solid materials that comes out from secondary air flow reactor drum 15 (fluorinated aluminium 1050kg wherein; The about 210kg of aluminum oxide) deliver to the upper bed layer of double-layer fluidized bed bioreactor 25 through the bottom conveyor screw through first reacting material inlet 24, the thick ALUMNIUM FLUORIDE of solid materials that comes out from three grades of gas-flow reactors 12 and level Four gas-flow reactors 10 is delivered to the lower bed layer of double-layer fluidized bed bioreactor 25 through second reacting material inlet 23 and the 3rd reacting material inlet 22, the level Four gas-flow reactors tail gas entering tail gas heat exchanger 6 of coming out from level Four gas-flow reactors 10; In tail gas heat exchanger, accomplish heat exchange; Get into first Venturi scrubber 33, second Venturi scrubber 34 and the 3rd Venturi scrubber 35 afterwards successively and cool off washing, the sodium aluminum fluoride mother liquor that the washings that first Venturi scrubber 33, second Venturi scrubber 34 and the 3rd Venturi scrubber 35 use obtains as the sodium aluminum fluoride workshop, the sodium aluminum fluoride mother liquor is introduced into after coming out in the sodium aluminum fluoride workshop the washings storage tank 36 and stores; Get into washings inlet 31 through the total water inlet pipe 29 of washings afterwards; Flow out from washings outlet 30 washings washing in first Venturi scrubber 33, second Venturi scrubber 34 and the 3rd Venturi scrubber 35 end back, gets into the sodium aluminum fluoride workshops as sodium aluminum fluoride Workshop Production raw material through the total outlet conduit 28 of washings then, and the tail gas that after first Venturi scrubber 33, second Venturi scrubber 34 and 35 3 grades of cooling washings of the 3rd Venturi scrubber, obtains passes through 8 emptyings of tail gas emptying pipe;
(3) reaction of aluminum oxide
Mixed gas from gas mixing chamber evenly gets into the two-stage fluidized reactor lower part through 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 intact hydrogen fluoride gas of unreacted continues the top bed air distribution plate through 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 through upflow tube, the ALUMNIUM FLUORIDE of the 690kg that reaction generates (fluorinated aluminium 645kg wherein; The about 45kg of aluminum oxide) flows out the back from the aluminium fluoride product outlet 16 of two-stage fluidized reactor bottom and get into cool furnace; In cool furnace, carry out indirect heat exchange and cool off, again through induced draft fan and fly-ash separator, be delivered to the ALUMNIUM FLUORIDE finished product bin after the cooling with water coolant.
The embodiment 3 and the mass analysis result of the Anhydrous Aluminium Chloride finished product that embodiment 4 makes see shown in the table 1.
The mass analysis result of table 1 Anhydrous Aluminium Chloride finished product
Claims (4)
1. the production system of an Anhydrous Aluminium Chloride; It is characterized in that; Comprise the hydrofluoric acid vaporizer; Said hydrofluoric acid vaporizer is provided with hydrofluoric acid inlet and hydrogen fluoride gas first outlet, and the hydrogen fluoride gas first outlet string is provided with tail gas heat exchanger, and tail gas heat exchanger is provided with gas inlet, tail gas outlet and hydrogen fluoride gas second outlet; Said tail gas outlet string is provided with the washing tail gas device; The said hydrogen fluoride gas second outlet string is provided with gas mixing chamber, and gas mixing chamber is provided with hot air inlet and mixed gas outlet, and 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, and the bottom of said double-layer fluidized bed bioreactor is provided with the aluminium fluoride product outlet, and 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 first reacting material inlet, second reacting material inlet and the 3rd reacting material inlet on the double-layer fluidized bed bioreactor; First reacting material inlet is communicated with the upper bed layer of double-layer fluidized bed bioreactor, and second reacting material inlet and the 3rd reacting material inlet are communicated with the lower bed layer of double-layer fluidized bed bioreactor, and said 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; Said one-level gas-flow reactors is provided with white lake material inlet and one-level gas-flow reactors reacting material outlet, and one-level gas-flow reactors reacting material outlet is gone here and there successively and is provided with secondary air flow reactor drum, three grades of gas-flow reactors and level Four gas-flow reactors, and said secondary air flow reactor drum is communicated with said first reacting material inlet through a connecting tube; Said three grades of gas-flow reactors are communicated with said second reacting material inlet through a connecting tube; Said level Four gas-flow reactors is communicated with said the 3rd reacting material inlet through a connecting tube, and the level Four gas-flow reactors is provided with level Four gas-flow reactors tail gas and exports, said level Four gas-flow reactors tail gas export be arranged on tail gas heat exchanger on gas inlet be connected.
2. the production system of Anhydrous Aluminium Chloride according to claim 1; It is characterized in that; Said washing tail gas device is made up of first Venturi scrubber, second Venturi scrubber and the 3rd Venturi scrubber established of string successively; First Venturi scrubber is provided with the first Venturi scrubber gas inlet; The said first Venturi scrubber gas inlet is connected with tail gas outlet on being arranged on tail gas heat exchanger, and the 3rd Venturi scrubber is provided with the tail gas emptying pipe, is provided with washings inlet and washings on first Venturi scrubber, second Venturi scrubber and the 3rd Venturi scrubber and exports; Said washings inlet is connected with the washings storage tank through the total water inlet pipe of washings, and said washings outlet is connected with the total outlet conduit of washings.
3. the production system of Anhydrous Aluminium Chloride according to claim 1 and 2; It is characterized in that; Said aluminium fluoride product treatment unit is made up of cool furnace, induced draft fan, fly-ash separator and the ALUMNIUM FLUORIDE finished product bin established of string successively, and cool furnace exports with said aluminium fluoride product and is communicated with.
4. the working method of an Anhydrous Aluminium Chloride is characterized in that, may further comprise the steps:
(1) anhydrous hydrofluoric acid charging
Anhydrous hydrofluoric acid gets into the hydrofluoric acid vaporizer through the hydrofluoric acid inlet; 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 gets into tail gas heat exchanger from hydrogen fluoride gas first back of coming out, and hydrogen fluoride gas carries out heat exchange with level Four gas-flow reactors tail gas from the level Four gas-flow reactors in tail gas heat exchanger, come out to get into gas mixing chamber from hydrogen fluoride gas second then; In gas mixing chamber, mix, send into the bottom of double-layer fluidized bed bioreactor afterwards through mixed gas outlet with warm air that hotblast stove provides;
(2) reaction of white lake
White lake is sent into the one-level gas-flow reactors through the white lake material inlet; White lake is fluidization in the one-level gas-flow reactors; Contact with two-stage fluidized reactor high temperature tail gas from double-layer fluidized bed bioreactor; White lake realizes that dehydration obtains aluminum oxide fully; Hydrogen fluoride gas in partially oxidation aluminium and the two-stage fluidized reactor high temperature tail gas reacts; Reacted gas-solid mixture material gets into secondary air flow reactor drum, three grades of gas-flow reactors and level Four gas-flow reactors successively through one-level gas-flow reactors reacting material outlet; Realize separating of gas, two kinds of materials of solid when in secondary air flow reactor drum, three grades of gas-flow reactors and level Four gas-flow reactors, carrying out gas-solid reaction; The thick ALUMNIUM FLUORIDE of solid materials that comes out from the secondary air flow reactor drum is delivered to the upper bed layer of double-layer fluidized bed bioreactor through first reacting material inlet through connecting tube; The thick ALUMNIUM FLUORIDE of solid materials that comes out from three grades of gas-flow reactors and level Four gas-flow reactors is delivered to the lower bed layer of double-layer fluidized bed bioreactor respectively through second reacting material inlet and the 3rd reacting material inlet through connecting tube; The level Four gas-flow reactors tail gas that comes out from the level Four gas-flow reactors gets into tail gas heat exchanger; In tail gas heat exchanger, accomplish heat exchange; Get into first Venturi scrubber, second Venturi scrubber and the 3rd Venturi scrubber afterwards successively and cool off washing, the sodium aluminum fluoride mother liquor that the washings that first Venturi scrubber, second Venturi scrubber and the 3rd Venturi scrubber use obtains as the sodium aluminum fluoride workshop, washings wash in first Venturi scrubber, second Venturi scrubber and the 3rd Venturi scrubber and finish the back from washings outlet outflow; Get into the sodium aluminum fluoride workshop as sodium aluminum fluoride Workshop Production raw material through the total outlet conduit of washings then, the tail gas that after first Venturi scrubber, second Venturi scrubber and three grades of cooling washings of the 3rd Venturi scrubber, obtains is through being arranged on the tail gas emptying pipe emptying on the 3rd Venturi scrubber;
(3) reaction of aluminum oxide
Mixed gas from gas mixing chamber evenly gets into the two-stage fluidized reactor lower part through 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 intact hydrogen fluoride gas of unreacted continues the top bed air distribution plate through 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 through upflow tube, and the aluminium fluoride product that reaction generates flows out from the bottom of double-layer fluidized bed bioreactor; Get into cool furnace; In cool furnace, carry out indirect heat exchange and cool off,, get into the ALUMNIUM FLUORIDE finished product bin afterwards again through induced draft fan, fly-ash separator with water coolant.
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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 |
CN103877916A (en) * | 2014-03-15 | 2014-06-25 | 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 |
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 |
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 |
CN108840358A (en) * | 2018-09-13 | 2018-11-20 | 衢州市鼎盛化工科技有限公司 | A kind of devices and methods therefor preparing aluminum fouoride |
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