CN101575112B - Method of preparing aluminum sulphate by utilizing fly ash - Google Patents
Method of preparing aluminum sulphate by utilizing fly ash Download PDFInfo
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- CN101575112B CN101575112B CN2008100113112A CN200810011311A CN101575112B CN 101575112 B CN101575112 B CN 101575112B CN 2008100113112 A CN2008100113112 A CN 2008100113112A CN 200810011311 A CN200810011311 A CN 200810011311A CN 101575112 B CN101575112 B CN 101575112B
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Abstract
The invention relates to a method of preparing aluminum sulphate by utilizing industrial solid waste, in particular to a method of preparing aluminum sulphate by utilizing fly ash. The method comprises the following steps: mechanically activating the fly ash; mixing the mechanically activated fly ash with water according to a weight ratio of 1: 0.5-2.5; adding concentrated sulfuric acid at a weight ratio of 0.3-2.2 : 1 to the fly ash to a reaction kettle to generate basic aluminum sulphate at a temperature of 120 to 230 DEG C kept for 1-8h and a pressure of 0.11 to 0.50 MPa; cooling the basic aluminum sulphate after a reaction, separating solid and liquid, adding sulfuric acid to the basic aluminum sulphate liquid, adjusting the system to have the basicity of 0.1 to 0.4 and the pH value of3 to 4 and converting the basic aluminum sulphate liquid into an aluminum sulphate solution; and evaporating and concentrating the aluminum sulphate solution to 110 to 120 DEG C and cooling and cryst allizing the aluminum sulphate solution to separate aluminum sulphate crystals.
Description
Technical field
The present invention relates to a kind of method of utilizing industrial solid castoff to prepare Tai-Ace S 150, relate in particular to a kind of method of utilizing fly-ash Preparation Tai-Ace S 150.
Background technology
Flyash is the solid waste that the coal-burning power plant discharges.At present, the more than one hundred million tons of China's flyash annual emissions, total volume of cargo in storage of China's flyash has tens00000000 tons.A large amount of soils are are not only occupied in the discharging of a large amount of flyash, and serious environment pollution, and ecological and environment are formed dual destruction.Therefore the comprehensive utilization of carrying out flyash has great realistic meaning and long-range strategic importance.
Tai-Ace S 150 can be done the scavenging agent that water source, service water or plant effluent are handled, paper sizing agent; The tannin of be used for flash arrestor, producing aluminum compound or white leather; Can be used as greasy finings, some catalyst for reaction or the like; It is important chemical material.The main method of producing at present Tai-Ace S 150 is to be raw material with bauxitic clay and sulfuric acid, reacts under certain condition to make.
Bauxite belongs to Nonrenewable resources, and along with China's aluminium industrial expansion, bauxite is deficient day by day, and the replacement resource of seeking bauxite is the only way of China's aluminium industrial development.Contain a large amount of aluminum oxide in the flyash, how content extracts Tai-Ace S 150 20%~60% from flyash, and it is very important maximally utilising flyash to the greatest extent.Because flyash is that so glassy phase accounts for significant proportion, its chemically reactive is very low through cooling rapidly behind the high-temp combustion.Therefore, the extraction yield that improve aluminum oxide in the flyash will be started with from the chemically reactive that improves flyash.The method of document announcement is to add the fluorochemical hydrotropy in acid-leaching reaction at present, silicon is combined with fluorine, reach and discharge the wherein purpose of aluminum oxide, but in the process of hydrotropy, may produce obnoxious flavoures such as HF, in the process of removing the fluorine purifying, can discharge fluorine-containing waste liquid and waste residue again, not only pollute the environment, and can cause potential safety hazard operator.
Summary of the invention
For solving the problems of the technologies described above a kind of method of utilizing fly-ash Preparation Tai-Ace S 150 that the invention provides, purpose is not add any auxiliary agent, improves the leaching yield of extracting aluminum oxide in the flyash.
For reaching a kind of method of utilizing fly-ash Preparation Tai-Ace S 150 of above-mentioned purpose the present invention, in may further comprise the steps: with the flyash mechanical activation; With the flyash behind the mechanical activation and water mixed according to weight 1: 0.5~2.5, the weight ratio that adds the vitriol oil and flyash is that 0.3~2.2: 1 the vitriol oil is in reactor, temperature is 120 ℃~230 ℃, pressure is 0.11MPa~0.50MPa, keep temperature 1h~8h, generate basic aluminium sulphate; Reaction cooling back solid-liquid separation adds sulfuric acid in basic aluminium sulphate liquid, regulation system basicity to 0.1~0.4, and pH value 3~4 makes it be converted into alum liquor; Alum liquor evaporation concentration to 110 ℃~120 ℃, crystallisation by cooling is separated out the Tai-Ace S 150 crystal.
The described method of utilizing fly-ash Preparation Tai-Ace S 150 comprises the steps: that also the Tai-Ace S 150 crystal promptly gets product through crushing packing.
Described mechanical activation adopts a kind of grinding the in vibration mill, vertical mill, planetary mills, high-energy ball milling or the Raymond mill.
Described 100~800 orders that are ground to.
Pipeline and valve are a kind of in acid-proof ceramic tile, enamel, glass, fluoroplastics or the tetrafluoroethylene between the liner of the reactor of described flyash and sulfuric acid reaction, whipping appts, reactor.
Behind described flyash and the sulfuric acid reaction, the solid-liquid separation of basic aluminium sulphate solution and slag adopts a kind of in natural subsidence, flocculating settling, pressure filtration or the filtration under diminished pressure.
The described sulfuric acid regulation system basicity that adds in basic aluminium sulphate solution, used sulfuric acid concentration is 10%~98%.
The residue hot water countercurrent washing of described reaction cooling back solid-liquid separation.
Described liquid aluminium sulfate evaporation concentration adopts a kind of in normal pressure or the reduction vaporization.
Described evaporation concentration equipment is for warding off lead or pottery or organic materials liner.
Described liquid aluminium sulfate evaporation concentration adopts directly or indirectly heating, and heating tube adopts the titanium material or wards off lead, and does anodic protection and handle.
Described crystallisation by cooling adopts a kind of in steel band crystallizer or the cylinder crystallizer.
It is heat-eliminating medium that described crystallisation by cooling adopts recirculated water.
Advantageous effect of the present invention:
The present invention adopts the flyash activating technology, does not add any auxiliary agent, can make that aluminum oxide effectively leaches in the flyash, and the leaching yield of aluminum oxide can reach more than 85%.
The present invention utilizes diluting concentrated sulfuric acid heat, and reactor temperature is raise, and forms high pressure, strengthens the leaching of aluminum oxide in the flyash, save energy.
The present invention makes it generate basic aluminium sulphate by control flyash and vitriolic ratio, enters solution thereby shielded impurity such as a large amount of iron, calcium, guarantees the quality of Tai-Ace S 150 product.
Reaction conditions of the present invention is a sulfuric acid concentration 20%~75%, 120 ℃~230 ℃ of temperature, and equipment solves easily under this condition, is beneficial to industrialization.
Embodiment
Below the invention will be further described.
Embodiment 1
The raw material powder coal ash consists of: Al
2O
3: 41%,, SiO
2: Fe 48%,
2O
3: 3.3%, CaO:3.3%, TiO
2: MgO:0.2% 1.3%.The composition of raw material powder coal ash also can adopt other moiety and concrete consumption, and the flyash of any routine is all passable, and this can not be used to limit protection scope of the present invention.
Flyash is carried out mechanical activation with vibration mill, be ground to 100 orders, mix according to 1: 1 with water and to place acidproof autoclave, with the grey weight ratio of acid is that 0.8: 1 the vitriol oil places in another pressure vessel that is connected with reactor, making the vitriol oil flow into flyash after the sealing of reactor and pressure vessel high-pressure system mixes with water, temperature is 172 ℃, and pressure is 0.32MPa, reaction 6h.Reaction cooling back solid-liquid separation adopts natural subsidence to obtain basic aluminium sulphate liquid, the residue hot water countercurrent washing of reaction cooling back solid-liquid separation, improve the rate of recovery of aluminium, adding concentration and be 10% sulfuric acid, to regulate its basicity be 0.1, and pH value 3.2 obtains alum liquor; Evaporation concentration postcooling to 120 ℃ is separated out the Tai-Ace S 150 crystal, and the Tai-Ace S 150 crystal promptly gets product through crushing packing, and Tai-Ace S 150 liquid decrease temperature crystalline adopts the steel band crystallizer after the evaporation concentration, and employing recirculated water is heat-eliminating medium; The liquid aluminium sulfate evaporation concentration adopts the normal pressure direct evaporation, and evaporation concentration equipment is for warding off lead, and the heating tube of evaporation equipment is the titanium material, and does anodic protection and handle; Pipeline and valve are acid-proof ceramic tile between the liner of the reactor of flyash and sulfuric acid reaction, whipping appts, reactor.Product meets national standard.Get part leaching back wash heat and wash, analyze wherein Al to neutrality
2O
3And SiO
2Content, the leaching yield of calculating aluminum oxide in the flyash reaches 88.2%.
Embodiment 2
Raw material powder coal ash among the embodiment 1 is carried out mechanical activation with vertical mill, be ground to 300 orders, mix according to 1: 1.5 with water and to place acidproof autoclave, with the grey weight ratio of acid is that 0.7: 1 the vitriol oil places in another pressure vessel that is connected with reactor, making the vitriol oil flow into flyash after the sealing of reactor and pressure vessel high-pressure system mixes with water, temperature is 120 ℃, and pressure is 0.5MPa, reaction 8h.Reaction cooling back solid-liquid separation adopts flocculating settling to obtain basic aluminium sulphate liquid, the residue hot water countercurrent washing of reaction cooling back solid-liquid separation, improve the rate of recovery of aluminium, adding concentration and be 50% sulfuric acid, to regulate its basicity be 0.3, and pH value 3.5 obtains alum liquor.Evaporation concentration postcooling to 110 ℃ is separated out the Tai-Ace S 150 crystal, and the Tai-Ace S 150 crystal promptly gets product through crushing packing, and Tai-Ace S 150 liquid decrease temperature crystalline adopts the cylinder crystallizer after the evaporation concentration, and employing recirculated water is heat-eliminating medium.The liquid aluminium sulfate evaporation concentration adopts the decompression indirect evaporation, and the liner of evaporation concentration equipment is an organic materials, and the heating tube of evaporation equipment is for warding off lead, and does the anodic protection processing.Pipeline and valve are enamel between the liner of the reactor of flyash and sulfuric acid reaction, whipping appts, reactor.Product meets national standard.Get part leaching back wash heat and wash, analyze wherein Al to neutrality
2O
3And SiO
2Content, the leaching yield of calculating aluminum oxide in the flyash reaches 80.6%.
Embodiment 3
Raw material powder coal ash among the embodiment 1 is carried out mechanical activation with planetary mills, be ground to 800 orders, mix according to 1: 0.5 with water and to place acidproof autoclave, with the grey weight ratio of acid is that 1.5: 1 the vitriol oil places in another pressure vessel that is connected with reactor, making the vitriol oil flow into flyash after the sealing of reactor and pressure vessel high-pressure system mixes with water, temperature is 230 ℃, and pressure is 0.11MPa, reaction 4h.Reaction cooling back solid-liquid separation adopts pressure filtration to obtain basic aluminium sulphate liquid, the residue hot water countercurrent washing of reaction cooling back solid-liquid separation, improve the rate of recovery of aluminium, adding concentration and be 98% sulfuric acid, to regulate its basicity be 0.4, and pH value 4 obtains alum liquor.Evaporation concentration postcooling to 115 ℃ is separated out the Tai-Ace S 150 crystal, and the Tai-Ace S 150 crystal promptly gets product through crushing packing, and Tai-Ace S 150 liquid decrease temperature crystalline adopts the cylinder crystallizer after the evaporation concentration, and employing recirculated water is heat-eliminating medium.The liquid aluminium sulfate evaporation concentration adopts the normal pressure indirect evaporation, and the liner of evaporation concentration equipment is an organic materials, and the heating tube of evaporation equipment is the titanium material, and does anodic protection and handle.Pipeline and valve are fluoroplastics between the liner of the reactor of flyash and sulfuric acid reaction, whipping appts, reactor.Product meets national standard.Get part leaching back wash heat and wash, analyze wherein Al to neutrality
2O
3And SiO
2Content, the leaching yield of calculating aluminum oxide in the flyash reaches 85.2%.
Embodiment 4
Flyash among the embodiment 1 carries out mechanical activation with high-energy ball milling, be ground to 500 orders, mix according to 1: 2.5 with water and to place acidproof autoclave, with the grey weight ratio of acid is that 2.2: 1 the vitriol oil places in another pressure vessel that is connected with reactor, making the vitriol oil flow into flyash after the sealing of reactor and pressure vessel high-pressure system mixes with water, temperature is 190 ℃, and pressure is 0.4MPa, reaction 1h.Reaction cooling back solid-liquid separation adopts filtration under diminished pressure to obtain basic aluminium sulphate liquid, the residue hot water countercurrent washing of reaction cooling back solid-liquid separation, improve the rate of recovery of aluminium, adding concentration and be 70% sulfuric acid, to regulate its basicity be 0.3, and pH value 3.8 obtains alum liquor.Evaporation concentration postcooling to 119 ℃ is separated out the Tai-Ace S 150 crystal, and the Tai-Ace S 150 crystal promptly gets product through crushing packing, and Tai-Ace S 150 liquid decrease temperature crystalline adopts the steel band crystallizer after the evaporation concentration, and employing recirculated water is heat-eliminating medium.The liquid aluminium sulfate evaporation concentration adopts the decompression direct evaporation, and the liner of evaporation concentration equipment is an organic materials, and the heating tube of evaporation equipment is the titanium material, and does anodic protection and handle.Pipeline and valve are glass between the liner of the reactor of flyash and sulfuric acid reaction, whipping appts, reactor.Product meets national standard.Get part leaching back wash heat and wash, analyze wherein Al to neutrality
2O
3And SiO
2Content, the leaching yield of calculating aluminum oxide in the flyash reaches 91.4%.
Embodiment 5
Flyash among the embodiment 1 carries out mechanical activation with Raymond mill, be ground to 600 orders, mix according to 1: 2 with water and to place acidproof autoclave, with the grey weight ratio of acid is that 1.8: 1 the vitriol oil places in another pressure vessel that is connected with reactor, making the vitriol oil flow into flyash after the sealing of reactor and pressure vessel high-pressure system mixes with water, temperature is 140 ℃, and pressure is 0.3MPa, reaction 3h.Reaction cooling back solid-liquid separation adopts filtration under diminished pressure to obtain basic aluminium sulphate liquid, the residue hot water countercurrent washing of reaction cooling back solid-liquid separation, improve the rate of recovery of aluminium, adding concentration and be 70% sulfuric acid, to regulate its basicity be 0.2, and pH value 3 obtains alum liquor.Evaporation concentration postcooling to 112 ℃ is separated out the Tai-Ace S 150 crystal, and the Tai-Ace S 150 crystal promptly gets product through crushing packing, and Tai-Ace S 150 liquid decrease temperature crystalline adopts the steel band crystallizer after the evaporation concentration, and employing recirculated water is heat-eliminating medium.The liquid aluminium sulfate evaporation concentration adopts the decompression direct evaporation, and the liner of evaporation concentration equipment is an organic materials, and the heating tube of evaporation equipment is the titanium material, and does anodic protection and handle.Pipeline and valve are tetrafluoroethylene between the liner of the reactor of flyash and sulfuric acid reaction, whipping appts, reactor.Product meets national standard.Get part leaching back wash heat and wash, analyze wherein Al to neutrality
2O
3And SiO
2Content, the leaching yield of calculating aluminum oxide in the flyash reaches 90%.
Claims (14)
1. method of utilizing fly-ash Preparation Tai-Ace S 150 is characterized in that may further comprise the steps:
With the flyash mechanical activation;
With the flyash behind the mechanical activation and water mixed according to weight 1: 0.5~2.5, the weight ratio that adds the vitriol oil and flyash is that 0.3~2.2: 1 the vitriol oil is in reactor, temperature is 120 ℃~230 ℃, pressure is 0.11MPa~0.50MPa, keep temperature 1h~8h, generate basic aluminium sulphate;
Reaction cooling back solid-liquid separation adds sulfuric acid in basic aluminium sulphate liquid, regulation system basicity to 0.1~0.4, and pH value 3~4 makes it be converted into alum liquor;
Alum liquor evaporation concentration to 110 ℃~120 ℃, crystallisation by cooling is separated out the Tai-Ace S 150 crystal.
2. the method for utilizing fly-ash Preparation Tai-Ace S 150 according to claim 1 is characterized in that also comprising the steps: that the Tai-Ace S 150 crystal promptly gets product through crushing packing.
3. the method for utilizing fly-ash Preparation Tai-Ace S 150 according to claim 1 is characterized in that described mechanical activation adopts a kind of grinding the in vibration mill, vertical mill, planetary mills, high-energy ball milling or the Raymond mill.
4. the method for utilizing fly-ash Preparation Tai-Ace S 150 according to claim 3 is characterized in that described 100~800 orders that are ground to.
5. the method for utilizing fly-ash Preparation Tai-Ace S 150 according to claim 1 is characterized in that pipeline and valve between the liner, whipping appts, reactor of the reactor of described flyash and sulfuric acid reaction are a kind of in acid-proof ceramic tile, enamel, glass, fluoroplastics or the tetrafluoroethylene.
6. the method for utilizing fly-ash Preparation Tai-Ace S 150 according to claim 1, after it is characterized in that described flyash and sulfuric acid reaction, the solid-liquid separation of basic aluminium sulphate solution and slag adopts a kind of in natural subsidence, flocculating settling, pressure filtration or the filtration under diminished pressure.
7. the method for utilizing fly-ash Preparation Tai-Ace S 150 according to claim 1 is characterized in that the described sulfuric acid regulation system basicity that adds in basic aluminium sulphate solution, used sulfuric acid concentration is 10%~98%.
8. the method for utilizing fly-ash Preparation Tai-Ace S 150 according to claim 1 is characterized in that the residue hot water countercurrent washing of described reaction cooling back solid-liquid separation.
9. the method for utilizing fly-ash Preparation Tai-Ace S 150 according to claim 1 is characterized in that described liquid aluminium sulfate evaporation concentration adopts a kind of in normal pressure or the reduction vaporization.
10. the method for utilizing fly-ash Preparation Tai-Ace S 150 according to claim 9 is characterized in that described evaporation concentration equipment is for warding off lead or pottery or organic materials liner.
11. a kind of method of utilizing fly-ash Preparation Tai-Ace S 150 according to claim 1 is characterized in that described liquid aluminium sulfate evaporation concentration adopts directly or indirectly heating, heating tube adopts the titanium material or wards off lead, and does anodic protection and handle.
12. a kind of method of utilizing fly-ash Preparation Tai-Ace S 150 according to claim 1 is characterized in that described crystallisation by cooling adopts a kind of in steel band crystallizer or the cylinder crystallizer.
13. a kind of method of utilizing fly-ash Preparation Tai-Ace S 150 according to claim 10 is characterized in that it is heat-eliminating medium that described crystallisation by cooling adopts recirculated water.
14. a kind of method of utilizing fly-ash Preparation Tai-Ace S 150 according to claim 1 is characterized in that described mixing afterreaction sulfuric acid concentration is 20~75%.
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CN103936040A (en) * | 2013-01-18 | 2014-07-23 | 新疆大学 | Ultrasonic wave acid method for extracting aluminum oxide from fly ash |
CN103936045B (en) * | 2014-04-01 | 2016-02-10 | 王宝冬 | A kind of method extracting aluminum oxide from flyash |
CN104445329B (en) * | 2014-12-10 | 2016-03-16 | 兴安宸亿工贸有限公司 | A kind of production equipment of Tai-Ace S 150 and production method |
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CN116040670B (en) * | 2023-03-31 | 2023-08-08 | 内蒙古蒙泰集团有限公司 | Method for producing polyaluminum chloride in process of preparing aluminum silicon oxide from fly ash |
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