CN102101686B - Process method for ultra-high purity alumina preparation by utilizing coal ash and comprehensive utilization of ultra-high purity alumina - Google Patents

Process method for ultra-high purity alumina preparation by utilizing coal ash and comprehensive utilization of ultra-high purity alumina Download PDF

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CN102101686B
CN102101686B CN2010106011904A CN201010601190A CN102101686B CN 102101686 B CN102101686 B CN 102101686B CN 2010106011904 A CN2010106011904 A CN 2010106011904A CN 201010601190 A CN201010601190 A CN 201010601190A CN 102101686 B CN102101686 B CN 102101686B
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flyash
ace
tai
high purity
ultra
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CN102101686A (en
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余红发
武金永
吴成友
麻海燕
王梅娟
董金美
李颖
李成栋
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Inner Mongolia Changtai Resourcs Circulation Regeneration Utilization Technology Development Co ltd
Nanjing University of Aeronautics and Astronautics
Qinghai Institute of Salt Lakes Research of CAS
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Inner Mongolia Changtai Resourcs Circulation Regeneration Utilization Technology Development Co ltd
Nanjing University of Aeronautics and Astronautics
Qinghai Institute of Salt Lakes Research of CAS
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Abstract

The invention discloses a process method for ultra-high purity alumina preparation by utilizing coal ash and comprehensive utilization of ultra-high purity alumina. In the process method, mechanical activation, flotation decarbonization, magnetic separation iron removal sulfuric acid aluminum lixiviation, solid-liquid separation, resin absorption iron removal, low-iron aluminum sulfate concentration, organic alcohol alcoholization acid washing, aluminum sulfate dehydration drying and aluminum sulfate high-temperature calcination are carried out on the coal ash so as to obtain ultra-high purity alpha-Al2O3, wherein the content of the Fe2O3 in the ultra-high purity alpha-Al2O3 is less than 2 ppm. By using the process method, the complicated purification problem that intermediate aluminum sulfate in the process of coal ash reclamation is necessarily subjected to a called Bayer circulation process is avoided, thereby simplifying the process flow, reducing the energy consumption, reducing the resource consumption and solving the technical problem of over-large secondary residue quantity accumulation. The process method has the advantages that the extraction efficiency is high, and the circulation recovery of organic alcohol and sulfuric acid and comprehensive utilization of byproducts such as resin and the like are achieved. In the invention, the process is simple, the process flow is short, the production process is easy to control, the content of the impurity in the product is low, and the quality of the product is stable.

Description

The process method of a kind of flyash production ultra-high purity aluminum oxide and comprehensive utilization thereof
Technical field
The present invention relates to the process method of Ash Utilization and comprehensive utilization, be specially the process method of a kind of flyash production ultra-high purity aluminum oxide and comprehensive utilization thereof.
Background technology
Flyash is remaining solid residue behind the coal combustion in the coal firing boiler, mainly comes from the by product of coal-burning power plant, and 1 ton of coal of every burning will produce the flyash of 230kg.According to incompletely statistics, national flyash accumulating amount reached 2,500,000,000 tons in 2007, expected the year two thousand twenty whole nation flyash accumulating amount and will reach 50～6,000,000,000 tons.The bulk deposition of flyash not only takies a large amount of land resources, also air, water, soil is caused serious pollution.The mode of conventional process flyash is to adopt the mode of landfill, but can't fundamentally solve flyash to pollution that environment caused.In recent years, flyash is obtaining application aspect building, the building materials, but because the technology that adopts is backward relatively, thereby this processing mode belongs to the utilization of extensive style.See that from chemical constitution flyash is a kind of aluminium ore that is rich in the medium-grade of silico-aluminate, and, utilize flyash to extract aluminium and have very wide application prospect along with the continuous exhaustion of China's alum clay resource.
The industrial use of aluminum oxide is very extensive, and metallurgical-grade aluminum oxide commonly used mainly is suitable for the dissolved salt electrolytic process and produces metallic aluminium, also is applicable to and produces corundum, pottery, refractory materials and other aluminum oxide chemical preparations.But; For the aluminum oxide that uses in fields such as fluorescent material, coating, jewel, high-pressure sodium fluorescent tube, glass additive, electronic ceramics, support of the catalyst; Its impurity requires strict more; Common metallurgical-grade aluminum oxide can not satisfy request for utilization, must adopt foreign matter contents such as Fe to be lower than the ultra-high purity aluminum oxide of 20ppm.At some special occasions, like military used in electronic ceramic high-purity superfine alumina powder material, foreign matter contents such as its impurity F e are in the scope of 3～10ppm in addition.
Although can adopt alkaline sintering method and pickling process from flyash, to extract aluminum oxide, its impurity removing technology remains the core technology that obtains the high-purity alpha-alumina product.Now, had report to adopt the alkaline sintering method to produce aluminum oxide, for example: number of patent application 200710150915.0 discloses a kind of method of from flyash, extracting high-purity ultra-fine alumina; Application number 200710017304.9 discloses a kind of method of extracting aluminum oxide and producing cement from fag end thereof from aluminous fly-ash; Application number 200410090949.1 discloses a kind of method of utilizing flyash and Wingdale combination producing aluminum oxide and cement etc.; But, produce a large amount of secondaries and pile up 1 ton of flyash of every processing because energy consumption is big; Will produce 10 tons residue; Can only be used to produce cement, therefore, limit it and applied.The production technique of pickling process is simple relatively; Has reasonable handiness; Its biggest advantage is can aluminum oxide in the flyash and silicon oxide be separated; And handle the quantity discharged that has reduced waste water, waste gas and waste residue in the process of flyash significantly, the residue of generation is rich in high silico-calcium, therefore can be directly as the active mineral admixture of high performance concrete etc.Adopt the number of patent application 200510048274.9 of vitriol lixiviation method to disclose a kind of method of alumina of from flyash, extracting; Application number 200610048295.5 discloses a kind ofly produces method of alumina by flyash; Application number 200710012997.2 discloses a kind of fly-ash Preparation method of alumina etc. of utilizing.
In aforesaid patented claim, the midbody γ-Al of metallurgical-grade aluminum oxide process 2O 3Purifying technique all be to adopt Bayer process to handle, that is: the Tai-Ace S 150 crystal obtains midbody γ-Al through calcining once 2O 3, dissolve, plant branch, filtration, washing, secondary clacining through alkali then and obtain metallurgical grade α-Al 2O 3, but complex process, procedure links are many, have shortcomings such as energy consumption and resource consumption are big, production cost height, and are difficult to obtain the aluminum oxide of ultra-high purity, therefore promote to be difficult for.
Summary of the invention
The technical problem that the present invention will solve provides the process method of a kind of flyash production ultra-high purity aluminum oxide and comprehensive utilization thereof; Present method adopts finite concentration sulfuric acid heating and pressurizing to leach Tai-Ace S 150; After solid-liquid separation, feed the cationic exchange resin adsorption deironing; Can prepare the ultra-high purity Tai-Ace S 150 that Fe content is lower than 0.2ppm, Tai-Ace S 150 directly calcining obtains ultra-high purity α-Al that iron oxide content is lower than 2ppm 2O 3Present method has been cancelled midbody γ-Al 2O 3The Bayer process purifying technique of complicacy, have that technology is simple, flow process short, production process is easy to control, alumina extraction ratio is high, low, low, the stay-in-grade advantage of product foreign matter content of production cost, easy to utilize.
The technical problem that the present invention will solve is realized by following scheme:
Mechanical activation: with flyash process mechanical activation;
The flotation de-carbon: will pass through the flyash of mechanical activation, be to add water in 1: 1～1: 3 according to the mass ratio of flyash and water, fully stirs, and removes through flotation and do not fire clean carbon;
Iron removal by magnetic separation: remove red stone and obtain magnetite powder through magnetic separation;
Sulfuric acid lixiviate aluminium: will passing through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 30%～95% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 1～1: 15; In acid tolerance response equipment, carry out heating and pressurizing reaction 1～6h, the top temperature of reaction is 200 ℃～240 ℃;
Solid-liquid separation: after the reaction cooling, be to add water in 1: 10～1: 20 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 1～1: 2 water washing, obtains the pH value and be 1～3 the thick liquid of Tai-Ace S 150;
Resin absorption deironing: the thick liquid of gained Tai-Ace S 150 is fed the cation exchange resin column deironing, make low iron alum liquor;
Low iron alum liquor concentrates: low iron alum liquor after the cooling, obtains the Tai-Ace S 150 liquid concentrator at 1/10～1/20 of 90 ℃～130 ℃ of evaporation concentration to original volumes;
Acid is washed in organic alcohol alcoholization: in the Tai-Ace S 150 liquid concentrator, be to add organic alcohol in 1: 1～4: 1 according to the volume ratio of organic alcohol and Tai-Ace S 150 liquid concentrator, fully stir 1～4h, obtain hanging down iron Tai-Ace S 150 filter cake after filtering;
Tai-Ace S 150 dewatered drying: finally obtain low iron Tai-Ace S 150 filter cake through 70 ℃～100 ℃ oven dry, obtain the ultra-high purity Tai-Ace S 150 that Fe content is lower than 0.2ppm;
The Tai-Ace S 150 high-temperature calcination: resulting ultra-high purity Tai-Ace S 150 obtains Fe through 800 ℃～temperature more than 1200 ℃ calcining, 3～6h 2O 3Content is lower than ultra-high purity α-Al of 2ppm 2O 3
Described mechanical activation is that to adopt milling equipment to carry out levigate, and the grinding time is 0.5～6h.
In the described sulfuric acid lixiviate aluminium operation, concentration range the best of flyash sulfuric acid mixed solution is 40%～70%, the solid-to-liquid ratio of flyash and sulphuric acid soln preferably 1: 5～1: 10, and the heating and pressurizing reaction is 3～4h preferably.
In the described solid-liquid separation process, after the reaction cooling, in flyash, be to add water in 1: 12～1: 18 preferably according to the mass ratio of flyash and water.
Described resin is a large pores cation exchange resin, and treatment temp is room temperature～90 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 1～4 times of resin volume/h.
Described large pores cation exchange resin is selected from any one among D001, D001FC, D001MB, D001SC, D001TR, 732,742, JK008,7020H, 7120H and the SPC-1.
After large pores cation exchange resin absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration; Eluent employing water or concentration are 3%～15% hydrochloric acid, and the eluent consumption is 1～3 times of resin volume, and the eluent flow velocity is 1～3 times of resin volume/h; Eluting temperature is room temperature～60 ℃, and eluent passes through resin column from the enterprising mode that goes out down during wash-out; Adopting concentration during regeneration is 3%～15% hydrochloric acid, and the hydrochloric acid consumption is 1～2 times of resin volume, and the hydrochloric acid flow velocity is 1～3 times of resin volume/h, and regeneration temperature is room temperature～60 ℃, and hydrochloric acid passes through resin column from the enterprising mode that goes out down during regeneration.
The waste liquid of described resin in hydrochloric acid wash-out and regenerative process; Concentrate through 50 ℃～110 ℃, best 70 ℃～80 ℃, crystallization iron(ic)chloride is separated out in cooling, through conventional spinning or vacuum belt filter; After 70 ℃～100 ℃ dryings, obtain containing aluminium iron(ic)chloride product.
In the described low iron alum liquor enrichment process, preferably 100～120 ℃ of evaporation concentration.
Organic alcohol that described organic alcohol alcoholization is washed in the sour operation is any one or more than one the mixture of methyl alcohol, ethanol, Virahol, n-propyl alcohol.
Described organic alcohol alcoholization is washed in the sour operation, and preferably the volume ratio according to organic alcohol and low iron Tai-Ace S 150 liquid concentrator is 2: 1～3: the 1 organic alcohol of adding, and abundant churning time is 2～3h preferably.
In the described Tai-Ace S 150 dewatered drying operation, the best bake out temperature that finally obtains low iron Tai-Ace S 150 filter cake is 80 ℃～90 ℃.
In the described Tai-Ace S 150 high-temperature calcination operation, the optimum calcinating temperature of resulting ultra-high purity Tai-Ace S 150 is at 1000 ℃～1200 ℃, and best calcination time is 4～5h.
Flyash adopts wet magnetic separation to remove magnetite after the flotation de-carbon.
Do not fire clean carbon through what flotation was removed, be used to make carbon black or directly burning produce heat.
Through the magnetite powder that magnetic separation obtains, be used to produce cement, make iron oxide black pigment or ironmaking.
Described organic alcohol alcoholization wash in the sour operation filtrating below 100 ℃ through distillation, reclaim organic alcohol, turn back to organic alcohol alcoholization again and wash in the sour operation and use, realize the recycling of organic alcohol.
To pass through distillation and reclaim organic alcohol second aqueous afterwards, and continue to be heated to distillation more than 120 ℃, concentrate, deposition is separated out in cooling; Sulphuric acid soln after filtering and the sulfuric acid that distills out; Obtain dilute sulphuric acid through mix, continue on for sulfuric acid lixiviate aluminium operation, realize the vitriolic recycling.
Described throw out of separating out after filtering obtains the Aluminum Sulfate Solution crystal after 80 ℃～120 ℃ oven dry.
Described ultra-high purity Tai-Ace S 150 is through 1000 ℃～temperature more than 1200 ℃ calcining, 4～5h, and that obtain is ultra-high purity α-Al 2O 3And SO 3
Described SO 3With through distillation, concentrate, cooling, filter, mix the dilution heat of sulfuric acid that is reclaimed and absorb, the preparation vitriol oil turns back to sulfuric acid lixiviate aluminium operation, realizes the vitriolic recycling.
The SiO of described solid-liquid separation process gained 2The solid residue that content is high after 70 ℃～120 ℃ oven dry, obtains high silicon ash.
Described high silicon ash directly is mixed together as the active mineral admixture of high performance concrete or with light dolomite, light calcined magnesia and is mixed with Si-Mg cement.
The invention has the advantages that:
1, adopt the vitriol lixiviation method to extract the aluminium in the flyash, the process energy consumption of preparation Tai-Ace S 150 is low, simple to operate.
2, adopt the method for purification of magnetic separation and resin absorption associating deironing, be easy to the industriallization deironing of Tai-Ace S 150, de-ironing efficiency is high, and its cost is lower, and technology is simple, obtains ultra-high purity Tai-Ace S 150.
3, the ultra-high purity Tai-Ace S 150 of preparing can directly be calcined and prepare ultra-high purity α-Al 2O 3, need not that adopting process complicacy, procedure links are many, energy consumption and resource consumption is big, production cost is high Bayer process circular treatment midbody γ-Al 2O 3Ultra-high purity α-Al 2O 3Fe content be lower than 0.2ppm; Can be used for fields such as chemical reagent, fine chemistry industry; Use as aluminum oxide such as fluorescent material, coating, jewel, high-pressure sodium fluorescent tube, glass additive, electronic ceramics, support of the catalyst, especially can be used in the high-purity superfine alumina powder material that military electronic ceramics is made in deep processing.
4, the cationic exchange resin adsorption in the resin absorption iron removal step saturated after, make resin recover adsorptive power through hydrochloric acid wash-out and regeneration, realize the recycling of resin; Waste liquid in hydrochloric acid wash-out and the regenerative process is separated out deposition, solid-liquid separation and drying through concentrating, cooling off, and obtains to contain aluminium iron(ic)chloride crystal.
5, the filtrating in the sour operation is washed in organic alcohol alcoholization, through the distillation of differing temps, concentrate, deposition is separated out in cooling, filter, and realizes organic pure and mild vitriolic recycling successively, and acquisition high ferro Tai-Ace S 150 crystal.
6, the present invention does not pursue the highest aluminium extraction yield, is target but fully utilize with 100% of fly ash, has realized the resource utilization of flyash all the components, removes and can produce ultra-high purity Tai-Ace S 150 and α-Al 2O 3Beyond the product, can also obtain not fire products such as clean carbon, magnetite powder, high ferro Tai-Ace S 150, high silicon ash, comprehensive utilization benefit is remarkable.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention
Embodiment
Below further set forth the present invention through embodiment, these embodiment are only presented for purposes of illustration, do not limit scope of the present invention.The experimental technique of unreceipted actual conditions in the following example is usually according to normal condition.
Embodiment 1: the raw material powder coal ash consists of: Al 2O 3Content 37.7%, Fe 2O 3Content 4.38%, CaO content 3.74%, MgO content 0.54%, SiO 2Content 49.9%, loss on ignition 1.92%.The raw material powder coal ash also can adopt other compositions and corresponding amount thereof.
With flyash ball milling 1h in ball mill, carry out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 3, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 40% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 8; In acid tolerance response equipment, carry out heating and pressurizing reaction 3h, the top temperature of reaction is 240 ℃; After the reaction cooling, be to add water at 1: 10 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 2 water washing, obtains pH value and be 3 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 72%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that D001 macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 65 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 4 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing concentration is 10% hydrochloric acid, and eluting temperature is 50 ℃; The hydrochloric acid flow velocity is 1 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 10% hydrochloric acid during regeneration, and temperature is 40 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 1 times of resin volume to regenerate altogether.
Low iron alum liquor at 1/10 of 100 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add absolute ethyl alcohol at 1: 1 according to the volume ratio of ethanol and Tai-Ace S 150 liquid concentrator, fully stir 2h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 85 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, at 1200 ℃ of calcining 3h, obtain ultra-high purity α-Al then 2O 3, analyze Fe wherein 2O 3Content is 1.6ppm, SiO 2Content is 0.018%, Na 2O content is 0.25%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
The sub product of gained comprehensive utilization comprises: flyash is not fired clean carbon at the flotation de-carbon; Adopt the wet magnetic separation deironing to obtain magnetite powder; The waste liquid of resin in hydrochloric acid wash-out and regenerative process concentrates through 75 ℃, and crystallization iron(ic)chloride is separated out in cooling, and spinning or vacuum belt filter through conventional after 90 ℃ of dryings, obtain containing aluminium iron(ic)chloride product; The SiO of solid-liquid separation process gained 2The solid residue that content is high after 100 ℃ of oven dry, obtains high silicon ash, directly is used as the active mineral admixture of high performance concrete; Perhaps be mixed together and be mixed with novel Si-Mg cement with light dolomite, light calcined magnesia.
Ethanol is distilled, reclaimed to the filtrating of washing in the sour operation in the ethanol alcoholization in addition, in process below 100 ℃; Continue to be heated to distillation more than 120 ℃, concentrate, deposition is separated out in cooling, and sulphuric acid soln after filtering and the sulfuric acid that distills out obtain dilute sulphuric acid through mix; The throw out of separating out after filtering obtains the Aluminum Sulfate Solution crystal after 100 ℃ of oven dry; The SO that the high-temperature calcination of ultra-high purity Tai-Ace S 150 obtains 3Absorb the preparation vitriol oil with the dilution heat of sulfuric acid that obtains through aforementioned recovery; Ethanol and vitriolic recycling have been realized.
Embodiment 2: the thick liquid of gained Tai-Ace S 150 is pressed into the resin column that JK008 macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 90 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 2 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing concentration is 8% hydrochloric acid, and eluting temperature is 30 ℃; The hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 1 times of resin volume to carry out wash-out altogether; Employing concentration is 8% hydrochloric acid during regeneration, and temperature is 20 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 1 times of resin volume to regenerate altogether.
Low iron alum liquor at 1/10 of 110 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add absolute ethyl alcohol at 1.5: 1 according to the volume ratio of ethanol and Tai-Ace S 150 liquid concentrator, fully stir 2h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 85 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, at 1100 ℃ of calcining 4h, obtain ultra-high purity α-Al then 2O 3, analyze Fe wherein 2O 3Content is 1.1ppm, SiO 2Content is 0.014%, Na 2O content is 0.20%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Ethanol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 3: with the flyash among the embodiment 1, ball milling 3h in ball mill carries out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 2, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 80% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 6; In acid tolerance response equipment, carry out heating and pressurizing reaction 5h, the top temperature of reaction is 240 ℃; After the reaction cooling, be to add water at 1: 10 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 2 water washing, obtains pH value and be 1 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 74%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that SPC-1 macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 70 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 3 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent adopts water, and eluting temperature is 60 ℃, and water flow velocity is 1 times of resin volume/h, adopts the water of 3 times of resin volumes to carry out wash-out altogether; Employing concentration is 6% hydrochloric acid during regeneration, and temperature is 50 ℃, and the hydrochloric acid flow velocity is 3 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to regenerate altogether.
Low iron alum liquor at 1/10 of 100 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add absolute ethyl alcohol at 3: 1 according to the volume ratio of ethanol and Tai-Ace S 150 liquid concentrator, fully stir 3h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 100 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, calcine 2h respectively at 810 ℃ and 1200 ℃ then, obtain ultra-high purity α-Al 2O 3, analyze Fe wherein 2O 3Content is 1.7ppm, SiO 2Content is 0.013%, Na 2O content is 0.17%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Ethanol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 4: with the flyash among the embodiment 1, ball milling 4h in ball mill carries out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 2, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 95% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 4; In acid tolerance response equipment, carry out heating and pressurizing reaction 5h, the top temperature of reaction is 240 ℃; After the reaction cooling, be to add water at 1: 20 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 1 water washing, obtains pH value and be 2 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 81%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that 732 macroporous type resin cation(R.C.)s are housed with noncorrosive pump carries out deironing, treatment temp is 90 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 1 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing concentration is 4% hydrochloric acid, and eluting temperature is 50 ℃; The hydrochloric acid flow velocity is 1 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 10% hydrochloric acid during regeneration, and temperature is 40 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 1 times of resin volume to regenerate altogether.
Low iron alum liquor at 1/20 of 110 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add absolute ethyl alcohol at 4: 1 according to the volume ratio of ethanol and Tai-Ace S 150 liquid concentrator, fully stir 2h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 90 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, calcine 5h respectively at 1000 ℃ then, obtain ultra-high purity α-Al 2O 3, analyze Fe wherein 2O 3Content is 1.5ppm, SiO 2Content is 0.013%, Na 2O content is 0.17%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Ethanol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 5: the raw material powder coal ash consist of Fe 2O 3Content is 3.66%, Al 2O 3Content is 40.88%, and CaO content is 2.96%, and MgO content is 0.36%, SiO 2Content is 42.7%, loss on ignition 5.46%.
With above-mentioned flyash ball milling 5h in ball mill, carry out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 1, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 30% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 10; In acid tolerance response equipment, carry out heating and pressurizing reaction 1.5h, the top temperature of reaction is 200 ℃; After the reaction cooling, be to add water at 1: 20 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 1 water washing, obtains pH value and be 3 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 76%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that 742 macroporous type resin cation(R.C.)s are housed with noncorrosive pump carries out deironing, treatment temp is 70 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 3 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing concentration is 7% hydrochloric acid, and eluting temperature is 60 ℃; The hydrochloric acid flow velocity is 1 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 7% hydrochloric acid during regeneration, and temperature is 30 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 1 times of resin volume to regenerate altogether.
Low iron alum liquor at 1/10 of 100 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add absolute ethyl alcohol at 2: 1 according to the volume ratio of ethanol and Tai-Ace S 150 liquid concentrator, fully stir 1h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 88 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, calcine 3h respectively at 1200 ℃ then, obtain ultra-high purity α-Al 2O 3, analyze Fe wherein 2O 3Content is 1.1ppm, SiO 2Content is 0.016%, Na 2O content is 0.21%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Ethanol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 6: with the flyash among the embodiment 5, ball milling 2h in ball mill carries out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 1, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 60% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 5; In acid tolerance response equipment, carry out heating and pressurizing reaction 1.4h, the top temperature of reaction is 240 ℃; After the reaction cooling, be to add water at 1: 20 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 1 water washing, obtains pH value and be 1 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 71%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that 7120H macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 50 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 3 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent adopts water, and eluting temperature is 50 ℃, and water flow velocity is 1 times of resin volume/h, adopts the water of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 8% hydrochloric acid during regeneration, and temperature is 40 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to regenerate altogether.
Low iron alum liquor at 1/20 of 110 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add absolute ethyl alcohol at 3: 1 according to the volume ratio of ethanol and Tai-Ace S 150 liquid concentrator, fully stir 1h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 100 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, calcine 4h respectively at 1100 ℃ then, obtain ultra-high purity α-Al 2O 3, analyze Fe wherein 2O 3Content is 0.9ppm, SiO 2Content is 0.013%, Na 2O content is 0.18%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Ethanol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 7: the raw material powder coal ash consist of Fe 2O 3Content is 2.72%, Al 2O 3Content is 41.67%, and CaO content is 2.39%, and MgO content is 0.43%, SiO 2Content is 46.21%, loss on ignition 3.07%.
With flyash ball milling 2h in ball mill, carry out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 2, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 70% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 4; In acid tolerance response equipment, carry out heating and pressurizing reaction 3h, the top temperature of reaction is 220 ℃; After the reaction cooling, be to add water at 1: 15 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 2 water washing, obtains pH value and be 2 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 76%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that 7020H macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 70 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 2 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing concentration is 9% hydrochloric acid, and eluting temperature is 50 ℃; The hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 1 times of resin volume to carry out wash-out altogether; Employing concentration is 9% hydrochloric acid during regeneration, and temperature is 40 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to regenerate altogether.
Low iron alum liquor at 1/15 of 100 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add absolute ethyl alcohol at 2: 1 according to the volume ratio of ethanol and Tai-Ace S 150 liquid concentrator, fully stir 1h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 90 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, calcine 2h respectively at 900 ℃ and 1200 ℃ then, obtain ultra-high purity α-Al 2O 3, analyze Fe wherein 2O 3Content is 1.5ppm, SiO 2Content is 0.013%, Na 2O content is 0.24%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Ethanol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 8: with the flyash among the embodiment 7, ball milling 6h in ball mill carries out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 1, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 90% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 3; In acid tolerance response equipment, carry out heating and pressurizing reaction 2h, the top temperature of reaction is 240 ℃; After the reaction cooling, be to add water at 1: 20 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 2 water washing, obtains pH value and be 2 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 82%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that D001TR macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 80 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 2 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing concentration is 7% hydrochloric acid, and eluting temperature is 60 ℃; The hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 8% hydrochloric acid during regeneration, and temperature is 50 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 1 times of resin volume to regenerate altogether.
Low iron alum liquor at 1/20 of 100 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add absolute ethyl alcohol at 4: 1 according to the volume ratio of ethanol and Tai-Ace S 150 liquid concentrator, fully stir 1h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 90 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, at 1200 ℃ of calcining 3h, obtain ultra-high purity α-Al then 2O 3, analyze Fe wherein 2O 3Content is 1.2ppm, SiO 2Content is 0.012%, Na 2O content is 0.13%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Ethanol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 9: the raw material powder coal ash consist of Fe 2O 3Content is 4.39%, Al 2O 3Content is 28.7%, and CaO content is 5.38%, and MgO content is 1.28%, SiO 2Content is 52.51%, loss on ignition 4.29%.
With flyash ball milling 3h in ball mill, carry out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 1, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 50% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 6; In acid tolerance response equipment, carry out heating and pressurizing reaction 2h, the top temperature of reaction is 240 ℃; After the reaction cooling, be to add water at 1: 20 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 1 water washing, obtains pH value and be 3 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 75%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that D001SC macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 50 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 2 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent adopts water, and eluting temperature is 40 ℃, and water flow velocity is 2 times of resin volume/h, adopts the water of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 8% hydrochloric acid during regeneration, and temperature is 40 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to regenerate altogether.
Low iron alum liquor at 1/20 of 100 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add absolute ethyl alcohol at 2: 1 according to the volume ratio of ethanol and Tai-Ace S 150 liquid concentrator, fully stir 1h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 90 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, at 1000 ℃ of calcining 6h, obtain ultra-high purity α-Al then 2O 3, analyze Fe wherein 2O 3Content is 0.3ppm, SiO 2Content is 0.016%, Na 2O content is 0.13%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Ethanol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 10: with the flyash among the embodiment 9, ball milling 3h in ball mill carries out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 2, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 70% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 5; In acid tolerance response equipment, carry out heating and pressurizing reaction 2h, the top temperature of reaction is 240 ℃; After the reaction cooling, be to add water at 1: 10 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 2 water washing, obtains pH value and be 1 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 73%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that D001MB macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 60 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 2 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing concentration is 7% hydrochloric acid, and eluting temperature is 50 ℃; The hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 8% hydrochloric acid during regeneration, and temperature is 40 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 1 times of resin volume to regenerate altogether.
Low iron alum liquor at 1/10 of 110 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add absolute ethyl alcohol at 2: 1 according to the volume ratio of ethanol and Tai-Ace S 150 liquid concentrator, fully stir 2h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 100 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, at 1200 ℃ of calcining 3h, obtain ultra-high purity α-Al then 2O 3, analyze Fe wherein 2O 3Content is 0.8ppm, SiO 2Content is 0.014%, Na 2O content is 0.27%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Ethanol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 11: with the flyash among the embodiment 1, ball milling 4h in ball mill carries out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 2, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 70% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 6; In acid tolerance response equipment, carry out heating and pressurizing reaction 3h, the top temperature of reaction is 220 ℃; After the reaction cooling, be to add water at 1: 20 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 1 water washing, obtains pH value and be 2 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 77%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that D001FC macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 60 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 2 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing concentration is 11% hydrochloric acid, and eluting temperature is 50 ℃; The hydrochloric acid flow velocity is 3 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 8% hydrochloric acid during regeneration, and temperature is 40 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 1 times of resin volume to regenerate altogether.
Low iron alum liquor at 1/15 of 120 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add anhydrous methanol at 2: 1 according to the volume ratio of methyl alcohol and Tai-Ace S 150 liquid concentrator, fully stir 1h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 95 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, at 1100 ℃ of calcining 4h, obtain ultra-high purity α-Al then 2O 3, analyze Fe wherein 2O 3Content is 1.2ppm, SiO 2Content is 0.015%, Na 2O content is 0.26%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Methyl alcohol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 12: with the flyash among the embodiment 1, ball milling 3h in ball mill carries out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 2, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 80% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 6; In acid tolerance response equipment, carry out heating and pressurizing reaction 5h, the top temperature of reaction is 240 ℃; After the reaction cooling, be to add water at 1: 10 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 2 water washing, obtains pH value and be 1 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 85%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that D001 macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 50 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 2 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent adopts water, and eluting temperature is 60 ℃, and water flow velocity is 2 times of resin volume/h, adopts the water of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 7% hydrochloric acid during regeneration, and temperature is 40 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to regenerate altogether.
Low iron alum liquor at 1/20 of 100 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add anhydrous methanol at 3: 1 according to the volume ratio of methyl alcohol and Tai-Ace S 150 liquid concentrator, fully stir 2h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 100 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, at 1200 ℃ of calcining 4h, obtain ultra-high purity α-Al then 2O 3, analyze Fe wherein 2O 3Content is 1.7ppm, SiO 2Content is 0.015%, Na 2O content is 0.23%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Methyl alcohol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 13: with the flyash among the embodiment 5, ball milling 2h in ball mill carries out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 1, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 60% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 5; In acid tolerance response equipment, carry out heating and pressurizing reaction 1.4h, the top temperature of reaction is 240 ℃; After the reaction cooling, be to add water at 1: 20 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 1 water washing, obtains pH value and be 2 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 82%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that 742 macroporous type resin cation(R.C.)s are housed with noncorrosive pump carries out deironing, treatment temp is 40 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 2 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing concentration is 11% hydrochloric acid, and eluting temperature is 60 ℃; The hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 7% hydrochloric acid during regeneration, and temperature is 40 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to regenerate altogether.
Low iron alum liquor at 1/20 of 110 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add anhydrous isopropyl alcohol at 3: 1 according to the volume ratio of Virahol and Tai-Ace S 150 liquid concentrator, fully stir 1h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 100 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, calcine 4h respectively at 1100 ℃ then, obtain ultra-high purity α-Al 2O 3, analyze Fe wherein 2O 3Content is 0.9ppm, SiO 2Content is 0.017%, Na 2O content is 0.26%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
Virahol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 14: with the flyash among the embodiment 7, ball milling 6h in ball mill carries out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 1, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 90% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 3; In acid tolerance response equipment, carry out heating and pressurizing reaction 2h, the top temperature of reaction is 240 ℃; After the reaction cooling, be to add water at 1: 20 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 2 water washing, obtains pH value and be 3 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 83%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that D001 macroporous type resin cation(R.C.) is housed with noncorrosive pump carries out deironing, treatment temp is 70 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 2 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent adopts water, and eluting temperature is 50 ℃, and water flow velocity is 2 times of resin volume/h, adopts the water of 3 times of resin volumes to carry out wash-out altogether; Employing concentration is 7% hydrochloric acid during regeneration, and temperature is 50 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to regenerate altogether.
Low iron alum liquor at 1/20 of 100 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add anhydrous n-propyl alcohol at 4: 1 according to the volume ratio of n-propyl alcohol and Tai-Ace S 150 liquid concentrator, fully stir 1h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 90 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, at 1200 ℃ of calcining 3h, obtain ultra-high purity α-Al then 2O 3, analyze Fe wherein 2O 3Content is 1.3ppm, SiO 2Content is 0.010%, Na 2O content is 0.15%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
N-propyl alcohol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.
Embodiment 15: with the flyash among the embodiment 9, ball milling 2h in ball mill carries out mechanical activation; According to the mass ratio of flyash and water is to add water at 1: 2, fully stirs, and removes through flotation and does not fire clean carbon; Remove red stone through magnetic separation again; To pass through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 70% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 5; In acid tolerance response equipment, carry out heating and pressurizing reaction 2h, the top temperature of reaction is 220 ℃; After the reaction cooling, be to add water at 1: 10 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 1 water washing, obtains pH value and be 2 the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 84%.
The thick liquid of gained Tai-Ace S 150 is pressed into the resin column that 732 macroporous type resin cation(R.C.)s are housed with noncorrosive pump carries out deironing, treatment temp is 50 ℃, and the flow velocity of the thick liquid of Tai-Ace S 150 is 2 times of resin volume/h during processing, obtains low iron alum liquor.
After said macroporous type resin cation(R.C.) absorption is saturated; Make resin recover adsorptive power through wash-out and regeneration, elution requirement is: eluent employing concentration is 10% hydrochloric acid, and eluting temperature is 50 ℃; The hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 2 times of resin volumes to carry out wash-out altogether; Employing concentration is 7% hydrochloric acid during regeneration, and temperature is 30 ℃, and the hydrochloric acid flow velocity is 2 times of resin volume/h, adopts the hydrochloric acid of 1 times of resin volume to regenerate altogether.
Low iron alum liquor at 1/15 of 110 ℃ of evaporation concentration to original volumes, after the cooling, is obtained the Tai-Ace S 150 liquid concentrator; In the Tai-Ace S 150 liquid concentrator, be to add anhydrous n-propyl alcohol at 2: 1 according to the volume ratio of n-propyl alcohol and Tai-Ace S 150 liquid concentrator, fully stir 1h, obtain low iron Tai-Ace S 150 filter cake after filtering; The low iron Tai-Ace S 150 filter cake that finally obtains through 100 ℃ of oven dry, is obtained ultra-high purity Tai-Ace S 150, at 1200 ℃ of calcining 3h, obtain ultra-high purity α-Al then 2O 3, analyze Fe wherein 2O 3Content is 0.8ppm, SiO 2Content is 0.012%, Na 2O content is 0.25%; Be superior to the strictest technical requirements of GB/T24487-2009 " aluminum oxide ", reach among the SJ20608-1996 " military alumina powder jointed MAT'L specification " 4 types (high-purity superfine alumina powder material) fully the strictest chemical ingredients requirement of Fe to the AO-1 metallurgical-grade aluminum oxide.
N-propyl alcohol, SO 3Recycle with not fire clean sub products such as carbon identical with embodiment 1.

Claims (21)

1. the process method of flyash production ultra-high purity aluminum oxide and comprehensive utilization thereof is characterized in that may further comprise the steps:
Mechanical activation: with flyash process mechanical activation;
The flotation de-carbon: will pass through the flyash of mechanical activation, be to add water in 1: 1～1: 3 according to the mass ratio of flyash and water, fully stirs, and removes through flotation and do not fire clean carbon;
Iron removal by magnetic separation: remove red stone and obtain magnetite powder through magnetic separation;
Sulfuric acid lixiviate aluminium: will passing through flyash raffinate and the vitriol oil after the flotation de-carbon, iron removal by magnetic separation, to be made into sulfuric acid concentration be 30%～95% mixing solutions; The solid-to-liquid ratio of control flyash and mixing solutions is 1: 1～1: 15; In acid tolerance response equipment, carry out heating and pressurizing reaction 1～6h, the top temperature of reaction is 200 ℃～240 ℃;
Solid-liquid separation: after the reaction cooling, be to add water in 1: 10～1: 20 according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and the mass ratio of use flyash and water is 1: 1～1: 2 water washing, obtains the pH value and be 1～3 the thick liquid of Tai-Ace S 150;
Resin absorption deironing: the thick liquid of gained Tai-Ace S 150 is fed the cation exchange resin column deironing, make low iron alum liquor;
Low iron alum liquor concentrates: low iron alum liquor after the cooling, obtains the Tai-Ace S 150 liquid concentrator at 1/10～1/20 of 90 ℃～130 ℃ of evaporation concentration to original volumes;
Acid is washed in organic alcohol alcoholization: in the Tai-Ace S 150 liquid concentrator, be to add organic alcohol in 1: 1～4: 1 according to the volume ratio of organic alcohol and Tai-Ace S 150 liquid concentrator, fully stir 1～4h, obtain hanging down iron Tai-Ace S 150 filter cake after filtering;
Tai-Ace S 150 dewatered drying: finally obtain low iron Tai-Ace S 150 filter cake through 70 ℃～100 ℃ oven dry, obtain the ultra-high purity Tai-Ace S 150 that Fe content is lower than 0.2ppm;
The Tai-Ace S 150 high-temperature calcination: resulting ultra-high purity Tai-Ace S 150 is calcined 3～6h through 800 ℃～1200 ℃ temperature, obtains Fe 2O 3Content is lower than ultra-high purity α-Al of 2ppm 2O 3
2. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 1 and comprehensive utilization thereof is characterized in that described mechanical activation is that to adopt milling equipment to carry out levigate, and the grinding time is 0.5～6h.
3. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 1 and comprehensive utilization thereof; It is characterized in that in the described sulfuric acid lixiviate aluminium operation; Concentration range the best of flyash sulfuric acid mixed solution is 40%～70%; The solid-to-liquid ratio of flyash and sulphuric acid soln preferably 1: 5～1: 10, the heating and pressurizing reaction is 3～4h preferably.
4. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 1 and comprehensive utilization thereof; It is characterized in that in the described solid-liquid separation process; After the reaction cooling, in flyash, be to add water in 1: 12～1: 18 preferably according to the mass ratio of flyash and water.
5. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 1 and comprehensive utilization thereof; It is characterized in that described resin is a large pores cation exchange resin, treatment temp is that the flow velocity of room temperature～90 ℃, the thick liquid of Tai-Ace S 150 is 1～4 times of resin volume/h.
6. according to the process method of claim 1 or 5 described a kind of flyash production ultra-high purity aluminum oxide and comprehensive utilization thereof, it is characterized in that described large pores cation exchange resin is selected from any one among D001, D001FC, D001MB, D001SC, D001TR, 732,742, JK008,7020H, 7120H and the SPC-1.
7. according to the process method of claim 1 or 5 described a kind of flyash production ultra-high purity aluminum oxide and comprehensive utilization thereof; It is characterized in that; After large pores cation exchange resin absorption is saturated, make resin recover adsorptive power through wash-out and regeneration, eluent employing water or concentration are 3%～15% hydrochloric acid; The eluent consumption is 1～3 times of resin volume; The eluent flow velocity is 1～3 times of resin volume/h, and eluting temperature is room temperature～60 ℃, and eluent passes through resin column from the enterprising mode that goes out down during wash-out; Adopting concentration during regeneration is 3%～15% hydrochloric acid, and the hydrochloric acid consumption is 1～2 times of resin volume, and the hydrochloric acid flow velocity is 1～3 times of resin volume/h, and regeneration temperature is room temperature～60 ℃, and hydrochloric acid passes through resin column from the enterprising mode that goes out down during regeneration.
8. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 7 and comprehensive utilization thereof; It is characterized in that the waste liquid of described resin in hydrochloric acid wash-out and regenerative process; Concentrate through 50 ℃～110 ℃, crystallization iron(ic)chloride is separated out in cooling, through conventional spinning or vacuum belt filter; After 70 ℃～100 ℃ dryings, obtain containing aluminium iron(ic)chloride product.
9. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 1 and comprehensive utilization thereof is characterized in that in the described low iron alum liquor enrichment process, preferably 100～120 ℃ of evaporation concentration.
10. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 1 and comprehensive utilization thereof is characterized in that organic alcohol that described organic alcohol alcoholization is washed in the sour operation is any one or more than one the mixture of methyl alcohol, ethanol, Virahol, n-propyl alcohol.
11. process method according to claim 1 or 10 described a kind of flyash production ultra-high purity aluminum oxide and comprehensive utilization thereof; It is characterized in that described organic alcohol alcoholization washes in the sour operation; Preferably the volume ratio according to organic alcohol and low iron Tai-Ace S 150 liquid concentrator is 2: 1～3: the 1 organic alcohol of adding, and abundant churning time is 2～3h preferably.
12. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 1 and comprehensive utilization thereof; It is characterized in that in the described Tai-Ace S 150 dewatered drying operation that the best bake out temperature that finally obtains low iron Tai-Ace S 150 filter cake is 80 ℃～90 ℃.
13. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 1 and comprehensive utilization thereof; It is characterized in that in the described Tai-Ace S 150 high-temperature calcination operation; The optimum calcinating temperature of resulting ultra-high purity Tai-Ace S 150 is at 1000 ℃～1200 ℃, and best calcination time is 4～5h.
14. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 1 and comprehensive utilization thereof is characterized in that flyash after the flotation de-carbon, adopts wet magnetic separation to remove magnetite.
15. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 11 and comprehensive utilization thereof; It is characterized in that described organic alcohol refines the filtrating of washing in the sour operation and distills, reclaims organic alcohol in process below 100 ℃; Turn back to organic alcohol alcoholization again and wash in the sour operation and use, realize the recycling of organic alcohol.
16. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 15 and comprehensive utilization thereof; It is characterized in that passing through distillation and reclaim organic alcohol second aqueous afterwards, continue to be heated to distillation more than 120 ℃, concentrate, deposition is separated out in cooling; Sulphuric acid soln after filtering and the sulfuric acid that distills out; Obtain dilute sulphuric acid through mix, continue on for sulfuric acid lixiviate aluminium operation, realize the vitriolic recycling.
17. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 16 and comprehensive utilization thereof is characterized in that described throw out of separating out after filtering after 80 ℃～120 ℃ oven dry, obtains the Aluminum Sulfate Solution crystal.
18. process method according to claim 1 or 13 described a kind of flyash production ultra-high purity aluminum oxide and comprehensive utilization thereof; It is characterized in that described ultra-high purity Tai-Ace S 150 through 1000 ℃～1200 ℃ temperature calcining, 4～5h, that obtain is ultra-high purity α-Al 2O 3And SO 3
19. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 18 and comprehensive utilization thereof is characterized in that described SO 3With through distillation, concentrate, cooling, filter, mix the dilution heat of sulfuric acid that is reclaimed and absorb, the preparation vitriol oil turns back to sulfuric acid lixiviate aluminium operation, realizes the vitriolic recycling.
20. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 1 and comprehensive utilization thereof is characterized in that the SiO of described solid-liquid separation process gained 2The solid residue that content is high after 70 ℃～120 ℃ oven dry, obtains high silicon ash.
21. the process method of a kind of flyash production ultra-high purity aluminum oxide according to claim 20 and comprehensive utilization thereof is characterized in that direct being mixed together as the active mineral admixture of high performance concrete or with light dolomite, light calcined magnesia of described high silicon ash is mixed with Si-Mg cement.
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