CN110386612A - A kind of preparation method of high purity aluminium oxide - Google Patents
A kind of preparation method of high purity aluminium oxide Download PDFInfo
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- CN110386612A CN110386612A CN201910656456.6A CN201910656456A CN110386612A CN 110386612 A CN110386612 A CN 110386612A CN 201910656456 A CN201910656456 A CN 201910656456A CN 110386612 A CN110386612 A CN 110386612A
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- high purity
- liquor alumini
- alumini chloridi
- aluminium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
Abstract
The invention discloses a kind of preparation methods of high purity aluminium oxide to obtain liquor alumini chloridi by reacting aluminium hydroxide of metallurgical grade with hydrochloric acid solution；Purified treatment is carried out to liquor alumini chloridi, makes the beavy metal impurity total amount in liquor alumini chloridi between 0.5~5ppm；Liquor alumini chloridi addition hydrogen chloride gas is once saltoutd, primary purification aluminum chloride crystals are obtained；The liquor alumini chloridi that weight is molten, after acquisition weight is molten is carried out to primary purification aluminum chloride crystals by high purity water；By weight it is molten after liquor alumini chloridi be added hydrogen chloride gas carry out it is secondary saltout, obtain secondary purification aluminum chloride crystals；Calcination process is carried out to secondary purification aluminium chloride crystal, obtains high purity aluminium oxide.In short, the present invention is using aluminium hydroxide of metallurgical grade as raw material, high-purity aluminium oxide is prepared in production, solves the problems, such as production technology complexity, the high production cost of existing aluminium oxide.
Description
Technical field
The invention belongs to the production technical fields of aluminium oxide, and in particular to a kind of preparation method of high purity aluminium oxide.
Background technique
Currently, there are many method for preparing high purity alumina powder both at home and abroad, mainly there are choline aluminum water solution, alum
Pyrolysismethod, aluminium carbonate ammonium pyrolysismethod, aluminium isopropoxide Hydrolyze method, aluminium hydroxide, high pure metal aluminum water method etc..
First the aluminium with a thickness of 0.1mm or so is made in the aluminium hydroxide that purity is 99.996% by choline aluminum water solution
Foil, and choline chloride is converted by choline using strong anion exchange resin；It is molten that choline is added in a certain amount of aluminium foil later
It is reacted in liquid.It is about 80 DEG C of the temperature of above-mentioned hydrolysis, anti-according to monitoring hydrogen evolution velocity estimated in reaction process
Speed is answered, when reaction speed is very low or stops, slurry is removed and is separated by solid-liquid separation, while aluminium hydroxide is periodically added and allows
Above process circulation carries out.The aluminium hydroxide that hydrolysis generates can obtain purity through filtering, spray drying, calcining and phase inversion
Up to 99.99% high-purity superfine alumina powder.The technology is the caustic alkali replaced in Bayer process alumina technology with choline
Circular response-precipitation process, compared with Bayer process, this technology is had a characteristic that by adjusting process conditions, can be produced
Varigrained high purity aluminium oxide product out；Using choline solution as reaction solution, reaction condition is mild, pollution-free；Choline circulation
It utilizes, advantage of lower cost；But it is easy to bring impurity into the process, product purity fluctuation is larger.
Alum pyrolysismethod is first made aluminum sulfate solution with sulfuric acid dissolution aluminium hydroxide, sulphur is added into solution later
Sour ammonium reacts obtained ammonia-alum, and cementing crystalline substance is repeatedly weighed further according to purity requirement, obtains purification ammonia-alum, then will obtain essence
Ammonia-alum processed decomposes at 1250 DEG C is made alumina powder.Its reaction equation is as follows: Al2(SO4)3+(NH4)2SO4+12H2O→
2NH4Al(SO4)2·12H2O, 2NH4Al(SO4)2·12H2O→Al2O3(amorphous)+2NH3+4SO3+13H2O.This method technique
Relatively simple, cost is relatively low, but the production cycle is long, and there are heat of solution phenomenons, and the NH generated in decomposable process3、
SO3Environment can be caused seriously to pollute.
Aluminium carbonate ammonium pyrolysismethod first alum is added in ammonium hydrogen carbonate, and reaction is converted into aluminum carbonate basic, then height
Alumina precursor can be made in pure aluminum carbonate basic ammonium heat resolve, and reaction equation is as follows: 4NH4HCO3+NH4Al(SO4)2→
NH4AlO(OH)HCO3+2(NH4)2SO4+3CO2+H2O, NH4AlO(OH)HCO3→Al2O3(amorphous)+2NH3+2CO2+3H2O.Heat
High purity alumina powder can be obtained through phase inversion and crushing again by solving amorphous precursors obtained.This method actually improves aluminum sulfate
Ammonium pyrolysismethod, although it overcomes alum pyrolysismethod discharge SO3The shortcomings that polluting environment, but the production cycle is lengthened, increase
Production cost is added.
Organic isopropanol water solution is to prepare the industrial production skill that high purity alumina powder mainly uses both at home and abroad at present
Art, Japan mainly produce high purity aluminium oxide using isopropanol water solution.This method is added aluminium and isopropanol using organic synthesis method
High-purity superfine alumina powder is made by techniques such as synthesis, purification, hydrolysis and roastings after catalyst.The oxygen of this method production
Change that aluminium powder body purity is high, partial size are small, but its production process is extremely complex, and process control is relatively difficult, and production cost compared with
Height, therefore the profit margin of enterprise is small.First reactive powder is made in the atomization of metallic aluminium chilling by the technique, later with simple
Al-H2O is reactant, activates its hydrolysis and maintains reaction, hydrolysis is as follows: 2Al+6H2O→2Al(OH)3+3H2
↑, 2Al (OH)3→Al2O3+3H2O.The aluminium hydroxide generated is hydrolyzed, through high-temperature calcination, the processing of phase inversion process, can be made high-purity super
Thin alumina powder.Compared with other traditional some processes, the technological principle and process be simple, in production process without dirt
Dye, is able to produce out 3N-5N aluminium oxide series of products.But the higher cost of production, needs using expensive refined aluminium or height
Fine aluminium, technical process requires strictly, and without special removal of impurities and purification process in production process, only part is soluble when hydrolysis
The impurity such as sodium oxide molybdena can remove, high purity aluminium oxide product purity is substantially dependent upon the purity of metal aluminum feedstock.
By the domestic and international main production process of the above high purity aluminium oxide, it was found that, aluminium isopropoxide method is that external production is high-purity
The main method of aluminium oxide, product purity is high, and the physical and chemical performance of product is stablized, but there are production technology complexity, productions
Problem at high cost.And other several methods all have that product quality is lower, and product physical and chemical performance is unstable, or there are rings
The problems such as border pollution, employment security hidden danger.
Summary of the invention
Place in view of the deficiency of the prior art, the present invention provides a kind of preparation methods of high purity aluminium oxide.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of preparation method of high purity aluminium oxide, comprising:
Aluminium hydroxide of metallurgical grade is reacted with hydrochloric acid solution, obtains liquor alumini chloridi；
Purified treatment is carried out to liquor alumini chloridi, make beavy metal impurity total amount in liquor alumini chloridi 0.5~5ppm it
Between；
Liquor alumini chloridi addition hydrogen chloride gas is once saltoutd, primary purification aluminum chloride crystals are obtained；
The liquor alumini chloridi that weight is molten, after acquisition weight is molten is carried out to primary purification aluminum chloride crystals by high purity water；
By weight it is molten after liquor alumini chloridi be added hydrogen chloride gas carry out it is secondary saltout, obtain secondary purification aluminium chloride knot
It is brilliant；
Calcination process is carried out to secondary purification aluminium chloride crystal, obtains high purity aluminium oxide.
Further, aluminium hydroxide of metallurgical grade is reacted with hydrochloric acid solution, comprising:
Aluminium hydroxide of metallurgical grade is mixed with the hydrochloric acid solution that mass fraction is 14~31%, obtains aluminium hydroxide and hydrochloric acid
Dissolution slurry；
Dissolution processing is carried out to dissolution slurry, obtains dissolution fluid；
Dissolution fluid is filtered processing, obtains liquor alumini chloridi.
Further, when carrying out dissolution processing to dissolution slurry, leaching temperature is 100~130 DEG C, dissolution pressure be 0~
0.3mpa, dissolution time 2~8 hours.
Further, purified treatment is carried out using resin adsorption method to liquor alumini chloridi.
Further, further includes: crystallization steaming is carried out to liquor alumini chloridi of the beavy metal impurity total amount between 0.5~5ppm
Hair processing comprising:
The steam for being 0.2~0.8mpa using pressure carries out 1~4 effect to liquor alumini chloridi and evaporates, tied as heat medium
Brilliant aluminium chloride；
High-temperature roasting processing is carried out to crystal aluminum chloride, obtains 3N crystalline aluminum oxide.
Further, when liquor alumini chloridi addition hydrogen chloride gas is once saltoutd, comprising:
Under conditions of salt-out temperature is 50~100 DEG C, once saltoutd by hydrogen chloride gas liquor alumini chloridi,
The salting-out crystallization rate of aluminium chloride is set to reach 88~94%, wherein the time of saltouing is 1~4 hour, and controls the salt in final solution
Acid concentration is 28~35%.
Further, further includes: high-temperature roasting processing is carried out to primary purification aluminum chloride crystals, obtains 4N crystallization oxidation
Aluminium.
Further, when carrying out heavy molten to primary purification aluminum chloride crystals by high purity water, the additional amount of high purity water makes
The concentration of aluminium chloride is 100~230g/l, and primary purification aluminum chloride crystals are carried out with the leaching temperature 40~80 of the molten processing of weight
DEG C, dissolution time be 1~5 hour.
Further, conductivity 16~20M Ω cm of the high purity water.
Further, when the liquor alumini chloridi addition hydrogen chloride gas by weight after molten carries out secondary saltout, comprising:
Under conditions of salt-out temperature is 50~100 DEG C, carried out by liquor alumini chloridi of the hydrogen chloride gas counterweight after molten
It is secondary to saltout, so that the salting-out crystallization rate of aluminium chloride is reached 88~94%, wherein the time of saltouing is 1~4 hour, and is controlled final
The mass fraction of hydrochloric acid in solution is 28~35%.
The preparation method of a kind of high purity aluminium oxide provided by the invention, by the way that aluminium hydroxide of metallurgical grade is anti-with hydrochloric acid solution
It answers, obtains liquor alumini chloridi；Purified treatment is carried out to liquor alumini chloridi, the beavy metal impurity total amount in liquor alumini chloridi is made to exist
Between 0.5~5ppm；Liquor alumini chloridi addition hydrogen chloride gas is once saltoutd, primary purification aluminum chloride crystals are obtained；
The liquor alumini chloridi that weight is molten, after acquisition weight is molten is carried out to primary purification aluminum chloride crystals by high purity water；By chlorination of the weight after molten
Aluminum solutions addition hydrogen chloride gas progress is secondary to saltout, and obtains secondary purification aluminum chloride crystals；To secondary purification aluminium chloride crystal
Calcination process is carried out, high purity aluminium oxide is obtained.In short, the present invention is using aluminium hydroxide of metallurgical grade as raw material, height is prepared in production
Pure aluminium oxide solves the problems, such as production technology complexity, the high production cost of existing aluminium oxide.
Detailed description of the invention
Fig. 1 is a kind of process flow chart of the preparation method of high purity aluminium oxide of exemplary embodiment of the present；
Fig. 2 is the process flow chart of the preparation method of another high purity aluminium oxide of exemplary embodiment of the present；
Fig. 3 is the process flow chart of the preparation method of another high purity aluminium oxide of exemplary embodiment of the present；
Fig. 4 is the process flow chart of the preparation method of another high purity aluminium oxide of exemplary embodiment of the present.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
As shown in Figure 1, a kind of preparation method of high purity aluminium oxide, comprising:
S100, aluminium hydroxide of metallurgical grade is reacted with hydrochloric acid solution, obtains liquor alumini chloridi.
As a preferred embodiment, as shown in Fig. 2, aluminium hydroxide of metallurgical grade is reacted with hydrochloric acid solution, comprising:
S101, aluminium hydroxide of metallurgical grade is mixed with the hydrochloric acid solution that mass fraction is 14~31%, obtains aluminium hydroxide
With the dissolution slurry of hydrochloric acid；
S102, dissolution processing is carried out to dissolution slurry, obtains dissolution fluid, wherein leaching temperature is 100~130 DEG C, dissolves out
Pressure be 0~0.3mpa, dissolution time 2~8 hours；
S103, dissolution fluid is filtered to processing, obtains liquor alumini chloridi.
More specifically, dissolution processing being carried out to mixed liquor, leaching temperature is 100~130 DEG C, dissolution pressure is 0~
0.3mpa, dissolution time are 2~8 hours, and chemical equation is as follows:
Al(OH)3+ 3HCl=AlCl3+3H2O
Then to the insoluble matter impurity in aluminium hydroxide of metallurgical grade successively after being filtered, lime etc. is added into solution
Alkaline matter is neutralized, and makes the pH value 7 or so of impurity, cinder field is sent to store up.
S200, purified treatment is carried out using resin adsorption method to liquor alumini chloridi, keeps the heavy metal in liquor alumini chloridi miscellaneous
Matter total amount between 0.5~5ppm, and using using the resin eluent after resin adsorption method purified treatment as producing water purification agent
Byproduct.
As a preferred embodiment, as shown in Figure 3, further includes: counterweight metal impurities total amount is between 0.5~5ppm
Liquor alumini chloridi carries out crystallization and evaporation processing comprising:
S201, the steam for being 0.2~0.8mpa using pressure carry out 1~4 effect to liquor alumini chloridi and evaporate as heat medium,
Obtain crystal aluminum chloride；
S202, to crystal aluminum chloride 1200-1450 DEG C at a temperature of, carry out high-temperature roasting processing, obtain 3N crystallize oxygen
Change aluminium.
S300, liquor alumini chloridi addition hydrogen chloride gas is once saltoutd, obtains primary purification aluminum chloride crystals.
As a preferred embodiment, when liquor alumini chloridi addition hydrogen chloride gas is once saltoutd, comprising:
Under conditions of salt-out temperature is 50~100 DEG C, once saltoutd by hydrogen chloride gas liquor alumini chloridi,
The salting-out crystallization rate of aluminium chloride is set to reach 88~94%, wherein the time of saltouing is 1~4 hour, and controls the salt in final solution
Acid concentration is 28~35%.
As a preferred embodiment, further includes: to primary purification aluminum chloride crystals 1200-1450 DEG C at a temperature of,
High-temperature roasting processing is carried out, 4N crystalline aluminum oxide is obtained.
S400, the liquor alumini chloridi that weight is molten, after acquisition weight is molten is carried out to primary purification aluminum chloride crystals by high purity water.
As a preferred embodiment, when carrying out heavy molten to primary purification aluminum chloride crystals by high purity water, high purity water
Additional amount make 100~230g/l of solution concentration of aluminium chloride, and the molten processing of weight is carried out to primary purification aluminum chloride crystals
40~80 DEG C of leaching temperature, dissolution time are 1~5 hour, conductivity 16~20M Ω cm of high purity water.
S500, by weight it is molten after liquor alumini chloridi be added hydrogen chloride gas carry out it is secondary saltout, obtain secondary purification chlorination
Crystalline aluminophosphate.
As a preferred embodiment, when liquor alumini chloridi addition hydrogen chloride gas of the weight after molten is carried out secondary saltout,
Include:
Under conditions of salt-out temperature is 50~100 DEG C, carried out by liquor alumini chloridi of the hydrogen chloride gas counterweight after molten
It is secondary to saltout, so that the salting-out crystallization rate of aluminium chloride is reached 88~94%, wherein the time of saltouing is 1~4 hour, and is controlled final
The mass fraction of hydrochloric acid in solution is 28~35%.
S600, calcination process is carried out to secondary purification aluminium chloride crystal, obtains high purity aluminium oxide, as acquisition 5N crystallizes oxygen
Change aluminium.
Embodiment 1
As shown in figure 4, a kind of preparation method of high purity aluminium oxide, comprising:
(1) 180kg aluminium hydroxide of metallurgical grade is mixed with the 1263kg hydrochloric acid solution that mass fraction is 20%, obtains hydrogen-oxygen
Change the dissolution slurry of aluminium and hydrochloric acid, wherein when aluminum hydroxide solution is mixed with hydrochloric acid solution, to the matter of aluminium hydroxide and hydrochloric acid
Amount selection is chemically reacted by the participation of aluminium hydroxide 100%, is generated liquor alumini chloridi and is calculated；Dissolution slurry pump is added
Enter into reactor for leaching, leaching temperature is 125 DEG C, and dissolution pressure is 0.3mpa, and dissolution time is 2 hours, is carried out at dissolution
Reason obtains dissolution fluid；By dissolution fluid after filter filters, filtrate floating material content 1mg/l is carried out with pumping liquor alumini chloridi
Purified treatment, filter cake are insoluble matter impurity；By filter cake after lime neutralisation treatment to pH value 7.0, it is sent to cinder field stockpiling.
(2) purified treatment is carried out using resin adsorption method to liquor alumini chloridi, makes the beavy metal impurity in liquor alumini chloridi
Total amount in 2ppm, and using using the resin eluent after resin adsorption method purified treatment as the byproduct for producing water purification agent；With
The steam that pressure is 0.2mpa is heat medium, and 50% purified treated liquor alumini chloridi is carried out 2 effects and is evaporated, is obtained
245kg crystal aluminum chloride；To crystal aluminum chloride 1350 DEG C at a temperature of, carry out high-temperature roasting processing, obtain 50kg 3N knot
Crystal alumina, and the hydrogen chloride flue gas that calcination process is generated produce hydrochloric acid using 2-3 grades of concatenated hydrogen chloride absorption towers.
(3) by the liquor alumini chloridi after remaining 50% purified treatment, salt-out temperature is 60 DEG C, the time of saltouing is 3 small
When under conditions of, once saltoutd by hydrogen chloride gas liquor alumini chloridi, reach the salting-out crystallization rate of aluminium chloride
94%, 245kg primary purification aluminum chloride crystals, the 4N crystal aluminum chloride of as 245kg are obtained, and control the salt in final solution
Acid concentration is 28%；By the primary purification aluminum chloride crystals of 196kg in 1350 DEG C of quartzy rotary kiln, carry out at high-temperature roasting
Reason, obtains the 4N crystalline aluminum oxide of 40kg；And the hydrogen chloride flue gas for generating calcination process, using 2-3 grades of concatenated hydrogen chloride
Absorption tower produces hydrochloric acid.
(4) by remaining 49kg primary purification aluminum chloride crystals (crystal aluminum chloride), it is added to conductivity 18M Ω .cm's
In high purity water, and the additional amount of high purity water makes the concentration 150g/l of aluminium chloride, with leaching temperature for 70 DEG C, dissolution time 2
Hour, carry out the liquor alumini chloridi that weight is molten, after acquisition weight is molten.
(5) salt-out temperature is 70 DEG C, the time of saltouing is 2 hours, under conditions of, liquor alumini chloridi of the weight after molten is added
Hydrogen chloride gas progress is secondary to saltout, and so that the salting-out crystallization rate of aluminium chloride is reached 94%, obtains the secondary purification aluminium chloride of 49kg
Crystallization.
(6) to the secondary purification aluminium chloride crystal of 49kg 1350 DEG C at a temperature of, carry out calcination process, obtain 10kg's
High purity aluminium oxide, as acquisition 5N crystalline aluminum oxide, and the hydrogen chloride flue gas that calcination process is generated are concatenated using 2-3 grades
Hydrogen chloride absorption tower produces hydrochloric acid.
Embodiment 2
A kind of preparation method of high purity aluminium oxide, comprising:
(1) 180kg aluminium hydroxide of metallurgical grade is mixed with the 1014kg hydrochloric acid solution that mass fraction is 14%, obtains hydrogen-oxygen
Change the dissolution slurry of aluminium and hydrochloric acid, wherein when aluminum hydroxide solution is mixed with hydrochloric acid solution, to the matter of aluminium hydroxide and hydrochloric acid
Amount selection is chemically reacted by the participation of aluminium hydroxide 100%, is generated liquor alumini chloridi and is calculated；Dissolution slurry pump is added
Enter into reactor for leaching, leaching temperature is 100 DEG C, and dissolution pressure is 0.2mpa, and dissolution time is 6 hours, is carried out at dissolution
Reason obtains dissolution fluid；By dissolution fluid after filter filters, filtrate floating material content 1.2mg/l, with pumping liquor alumini chloridi into
Row purified treatment, filter cake are insoluble matter impurity；By filter cake after lime neutralisation treatment to pH value 7.0, it is sent to cinder field stockpiling.
(2) purified treatment is carried out using resin adsorption method to liquor alumini chloridi, makes the beavy metal impurity in liquor alumini chloridi
Total amount in 0.5ppm, and using using the resin eluent after resin adsorption method purified treatment as the byproduct for producing water purification agent；
Using pressure for 0.6mpa steam as heat medium, 50% purified treated liquor alumini chloridi is subjected to 3 effects and is evaporated, is obtained
Obtain 2450kg crystal aluminum chloride；To crystal aluminum chloride 1400 DEG C at a temperature of, carry out high-temperature roasting processing, obtain 500kg's
3N crystalline aluminum oxide, and the hydrogen chloride flue gas that calcination process is generated produce salt using 2-3 grades of concatenated hydrogen chloride absorption towers
Acid.
(3) by the liquor alumini chloridi after remaining 50% purified treatment, salt-out temperature is 50 DEG C, the time of saltouing is 4 small
When under conditions of, once saltoutd by hydrogen chloride gas liquor alumini chloridi, reach the salting-out crystallization rate of aluminium chloride
88%, 2450kg primary purification aluminum chloride crystals, the 4N crystal aluminum chloride of as 2450kg are obtained, and control in final solution
Concentration of hydrochloric acid is 30%；By the primary purification aluminum chloride crystals of 1960kg in 1450 DEG C of quartzy rotary kiln, high temperature roasting is carried out
Burning processing, obtains the 4N crystalline aluminum oxide of 400kg；And the hydrogen chloride flue gas for generating calcination process, using 2-3 grades of concatenated chlorine
Change hydrogen absorption tower, produces hydrochloric acid.
(4) by remaining 490kg primary purification aluminum chloride crystals (crystal aluminum chloride), it is added to conductivity 16M Ω .cm's
In high purity water, and the additional amount of high purity water makes the concentration 230g/l of aluminium chloride, with leaching temperature for 40 DEG C, dissolution time 2
Hour, carry out the liquor alumini chloridi that weight is molten, after acquisition weight is molten.
(5) salt-out temperature is 70 DEG C, the time of saltouing is 4 hours, under conditions of, liquor alumini chloridi of the weight after molten is added
Hydrogen chloride gas progress is secondary to saltout, and so that the salting-out crystallization rate of aluminium chloride is reached 88%, obtains the secondary purification aluminium chloride of 490kg
Crystallization.
(6) to the secondary purification aluminium chloride crystal of 490kg 1450 DEG C at a temperature of, carry out calcination process, obtain 100kg
High purity aluminium oxide, as acquisition 5N crystalline aluminum oxide, and by calcination process generate hydrogen chloride flue gas, using 2-3 grade series connection
Hydrogen chloride absorption tower, produce hydrochloric acid.
Embodiment 3
A kind of preparation method of high purity aluminium oxide, comprising:
(1) 900kg aluminium hydroxide of metallurgical grade is mixed with the 4210kg hydrochloric acid solution that mass fraction is 31%, obtains hydrogen-oxygen
Change the dissolution slurry of aluminium and hydrochloric acid, wherein when aluminum hydroxide solution is mixed with hydrochloric acid solution, to the matter of aluminium hydroxide and hydrochloric acid
Amount selection is chemically reacted by the participation of aluminium hydroxide 100%, is generated liquor alumini chloridi and is calculated；Dissolution slurry pump is added
Entering into reactor for leaching, leaching temperature is 130 DEG C, and dissolution pressure is 0mpa, and dissolution time is 8 hours, dissolution processing is carried out,
Obtain dissolution fluid；By dissolution fluid after filter filters, filtrate floating material content 1.1mg/l is carried out with pumping liquor alumini chloridi
Purified treatment, filter cake are insoluble matter impurity；By filter cake after lime neutralisation treatment to pH value 7.0, it is sent to cinder field stockpiling.
(2) purified treatment is carried out using resin adsorption method to liquor alumini chloridi, makes the beavy metal impurity in liquor alumini chloridi
Total amount in 5ppm, and using using the resin eluent after resin adsorption method purified treatment as the byproduct for producing water purification agent；With
The steam that pressure is 0.2mpa is heat medium, and 50% purified treated liquor alumini chloridi is carried out 1 effect and is evaporated, is obtained
1225kg crystal aluminum chloride；To crystal aluminum chloride 1200 DEG C at a temperature of, carry out high-temperature roasting processing, obtain the 3N of 250kg
Crystalline aluminum oxide, and the hydrogen chloride flue gas that calcination process is generated produce hydrochloric acid using 2-3 grades of concatenated hydrogen chloride absorption towers.
(3) by the liquor alumini chloridi after remaining 50% purified treatment, salt-out temperature is 100 DEG C, the time of saltouing is 1 small
When under conditions of, once saltoutd by hydrogen chloride gas liquor alumini chloridi, reach the salting-out crystallization rate of aluminium chloride
90%, 1225kg primary purification aluminum chloride crystals, the 4N crystal aluminum chloride of as 1225kg are obtained, and control in final solution
Concentration of hydrochloric acid is 35%；By the primary purification aluminum chloride crystals of 980kg in 1200 DEG C of quartzy rotary kiln, high-temperature roasting is carried out
Processing, obtains the 4N crystalline aluminum oxide of 160kg；And the hydrogen chloride flue gas for generating calcination process, using 2-3 grades of concatenated chlorinations
Hydrogen absorption tower produces hydrochloric acid.
(4) by remaining 245kg primary purification aluminum chloride crystals (crystal aluminum chloride), it is added to conductivity 20M Ω .cm's
In high purity water, and the additional amount of high purity water makes the concentration 100g/l of aluminium chloride, with leaching temperature for 80 DEG C, dissolution time 1
Hour, carry out the liquor alumini chloridi that weight is molten, after acquisition weight is molten.
(5) salt-out temperature is 50 DEG C, the time of saltouing is 4 hours, under conditions of, liquor alumini chloridi of the weight after molten is added
Hydrogen chloride gas progress is secondary to saltout, and so that the salting-out crystallization rate of aluminium chloride is reached 90%, obtains the secondary purification aluminium chloride of 245kg
Crystallization.
(6) to the secondary purification aluminium chloride crystal of 245kg 1200 DEG C at a temperature of, carry out calcination process, obtain 50kg
High purity aluminium oxide, as acquisition 5N crystalline aluminum oxide, and by calcination process generate hydrogen chloride flue gas, using 2-3 grade series connection
Hydrogen chloride absorption tower, produce hydrochloric acid.
The preparation method of a kind of high purity aluminium oxide provided by the invention, by the way that aluminium hydroxide of metallurgical grade is anti-with hydrochloric acid solution
It answers, obtains liquor alumini chloridi；Purified treatment is carried out to liquor alumini chloridi, the beavy metal impurity total amount in liquor alumini chloridi is made to exist
Between 0.5~5ppm；Liquor alumini chloridi addition hydrogen chloride gas is once saltoutd, primary purification aluminum chloride crystals are obtained；
The liquor alumini chloridi that weight is molten, after acquisition weight is molten is carried out to primary purification aluminum chloride crystals by high purity water；By chlorination of the weight after molten
Aluminum solutions addition hydrogen chloride gas progress is secondary to saltout, and obtains secondary purification aluminum chloride crystals；To secondary purification aluminium chloride crystal
Calcination process is carried out, high purity aluminium oxide is obtained.In short, the present invention is using aluminium hydroxide of metallurgical grade as raw material, height is prepared in production
Pure aluminium oxide solves the problems, such as production technology complexity, the high production cost of existing aluminium oxide；Also, from 3N, 4N,
The hydrogen chloride flue gas that the calcination steps of 5N aluminium oxide generate is all made of 2-3 grades of concatenated hydrogen chloride absorption towers, produces hydrochloric acid, this
The hydrochloric acid that step obtains returns to the aluminium hydroxide dissolution step of front, forms the closed cycle of steps flow chart of the present invention；Primary
Saltout, the aluminium chloride that secondary salting-out crystallization generates is saltoutd raffinate, and resolving hydrochloric acid is carried out, the hydrogen chloride gas of generation can be used for tying
Brilliant liquor alumini chloridi once saltout, secondary analyzing step, organize cost steps flow chart closed cycle.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (10)
1. a kind of preparation method of high purity aluminium oxide characterized by comprising
Aluminium hydroxide of metallurgical grade is reacted with hydrochloric acid solution, obtains liquor alumini chloridi；
Purified treatment is carried out to liquor alumini chloridi, makes the beavy metal impurity total amount in liquor alumini chloridi between 0.5~5ppm；
Liquor alumini chloridi addition hydrogen chloride gas is once saltoutd, primary purification aluminum chloride crystals are obtained；
The liquor alumini chloridi that weight is molten, after acquisition weight is molten is carried out to primary purification aluminum chloride crystals by high purity water；
By weight it is molten after liquor alumini chloridi be added hydrogen chloride gas carry out it is secondary saltout, obtain secondary purification aluminum chloride crystals；
Calcination process is carried out to secondary purification aluminium chloride crystal, obtains high purity aluminium oxide.
2. a kind of preparation method of high purity aluminium oxide according to claim 1, which is characterized in that by aluminium hydroxide of metallurgical grade
It is reacted with hydrochloric acid solution, comprising:
The hydrochloric acid solution that aluminium hydroxide of metallurgical grade and mass fraction are 14~31% mix, acquisition aluminium hydroxide and hydrochloric acid it is molten
Slurry out；
Dissolution processing is carried out to dissolution slurry, obtains dissolution fluid；
Dissolution fluid is filtered processing, obtains liquor alumini chloridi.
3. a kind of preparation method of high purity aluminium oxide according to claim 2, which is characterized in that carried out to dissolution slurry molten
When handling out, leaching temperature is 100~130 DEG C, dissolution pressure is 0~0.3mpa, dissolution time 2~8 hours.
4. a kind of preparation method of high purity aluminium oxide according to claim 1, which is characterized in that used to liquor alumini chloridi
Resin adsorption method carries out purified treatment.
5. a kind of preparation method of high purity aluminium oxide according to claim 1, which is characterized in that further include: to heavy metal
Liquor alumini chloridi of the total impurities between 0.5~5ppm carries out crystallization and evaporation processing comprising:
The steam for being 0.2~0.8mpa using pressure carries out 1~4 effect to liquor alumini chloridi and evaporates, obtain crystallization chlorine as heat medium
Change aluminium；
High-temperature roasting processing is carried out to crystal aluminum chloride, obtains 3N crystalline aluminum oxide.
6. a kind of preparation method of high purity aluminium oxide according to claim 1, which is characterized in that add by liquor alumini chloridi
When entering hydrogen chloride gas and once being saltoutd, comprising:
Under conditions of salt-out temperature is 50~100 DEG C, is once saltoutd by hydrogen chloride gas liquor alumini chloridi, make chlorine
The salting-out crystallization rate for changing aluminium reaches 88~94%, wherein the time of saltouing is 1~4 hour, and the hydrochloric acid controlled in final solution is dense
Degree is 28~35%.
7. a kind of preparation method of high purity aluminium oxide according to claim 1, which is characterized in that further include: to once mentioning
Pure aluminum chloride crystals carry out high-temperature roasting processing, obtain 4N crystalline aluminum oxide.
8. a kind of preparation method of high purity aluminium oxide according to claim 1, which is characterized in that passing through high purity water to one
When secondary purification aluminum chloride crystals carry out heavy molten, the additional amount of high purity water makes 100~230g/l of concentration of aluminium chloride, and to primary
Purification aluminum chloride crystals carry out 40~80 DEG C of the leaching temperature of the molten processing of weight, dissolution time is 1~5 hour.
9. a kind of preparation method of high purity aluminium oxide according to claim 8, which is characterized in that the conductance of the high purity water
Rate 16~20M Ω cm.
10. a kind of preparation method of high purity aluminium oxide according to claim 1, which is characterized in that by chlorination of the weight after molten
When aluminum solutions addition hydrogen chloride gas carries out secondary saltout, comprising:
Under conditions of salt-out temperature is 50~100 DEG C, carried out by liquor alumini chloridi of the hydrogen chloride gas counterweight after molten secondary
It saltouts, the salting-out crystallization rate of aluminium chloride is made to reach 88~94%, wherein the time of saltouing is 1~4 hour, and controls final solution
In hydrochloric acid mass fraction be 28~35%.
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