CN105731508A - Method for preparing high-activity aluminum oxide powder using aluminum ash - Google Patents
Method for preparing high-activity aluminum oxide powder using aluminum ash Download PDFInfo
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- CN105731508A CN105731508A CN201610062816.6A CN201610062816A CN105731508A CN 105731508 A CN105731508 A CN 105731508A CN 201610062816 A CN201610062816 A CN 201610062816A CN 105731508 A CN105731508 A CN 105731508A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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Abstract
The invention discloses a method for preparing high-activity aluminum oxide powder using aluminum ash, and belongs to the preparation field of aluminum oxide powder. The method comprises the following steps: by using aluminum ash as a raw material, floating in water to remove slag, adding sulfuric acid solution and diisopropanolamine to remove insoluble matters in the aluminum ash, and then removing other metal impurities soluble in potassium hydroxide under the effect of carbon disulfide assisted by titanium dioxide, adding polyethylene glycol and ammonia water, stirring, filtering to obtain jelly, washing, drying, calcinating, and crushing to obtain the high-activity aluminum oxide powder. The method disclosed by the invention has the beneficial effects that aluminum ash is sufficiently utilized to prepare the high activity aluminum oxide powder, not only the environment pollution problem is solved, but also the sustainable utilization of the resource is realized; the prepared aluminum oxide powder is small in grain, uniform in grain size distribution and hard to unite, and the activity is more than or equal to 18% higher than that of the aluminum oxide powder prepared by other methods.
Description
Technical field
The present invention relates to a kind of method utilizing aluminum ash to prepare high-activity aluminium oxide powder body, belong to alumina powder jointed preparation field.
Background technology
Alumina powder jointed have excellent physics, chemistry, optics, mechanics and thermal property, has been widely used in the various fields such as chemical industry, electronics, machinery, special cermacis, and its important function in illumination and peninsula body industry also becomes increasingly conspicuous.At present, the method preparing ultra-fine alumina is a lot, is broadly divided into solid phase method, vapor phase method, liquid phase method and organic alkoxide Hydrolyze method according to reaction principle.But every kind of method has the limitation of himself, such as solid phase method, to there is complex process, alkoxide expensive, is difficult to the preparation little granule less than 100nnl, the problems such as granule crystal formation is undesirable；There is the limitation such as production efficiency is low, technological parameter is difficult to control to, device is huge, structure is complicated, the collection of apparatus expensive, powder difficulty in vapor phase method；In wet chemistry method, agglomeration traits is a difficult problem so far, and organic alkoxide Hydrolyze method is prepared alumina powder jointed, and complex process, alkoxide are expensive, and powder granule is relatively big, particle size distribution width and easily reuniting.Although many researcheres explore out numerous reducing or avoid the solution reunited, but also have the limitation of himself.Thus, explore preparation high-performance, soilless sticking, the technology of preparing that meets the market demand, caused the extensive concern of domestic and international researcher.
Aluminum ash mainly generates and produces in the process of aluminum in aluminium oxide through molten-salt electrolysis, due to operation and the carrying of measuring instrument, anode change, goes out the reasons such as aluminum, ingot casting and electrolytic cell overhaul, can produce substantial amounts of aluminum slag.1 ton of aluminum of general often production to produce 3050 kg aluminium slag aluminum ashes.In recent years, China's aluminum production capacity and yield increase considerably.Again, the response rate of aluminium scrap regeneration fabricated product again is generally 75%～85%.Regenerate 1 ton of aluminium scrap by generation 150～250 kg aluminium slag aluminum ash.Aluminum ash is a kind of Renewable resource, but does not obtain enough attention, one of factor becoming welding always.Along with expanding economy, aluminium scrap lime-ash accumulation increases considerably year by year, if the method not finding economical and effective and environmental protection is administered, the serious threat of environment will increasingly be highlighted by it.It is low that China's aluminum current ash processes the response rate, and energy expenditure is big, researches and develops to reclaim industrial aluminum lime-ash and prepares other materials, for increasing economic efficiency, preserves the ecological environment and have important practical significance and practical value.Therefore utilize aluminum ash to prepare high-activity aluminium oxide powder body on this basis, there is important social value and economic benefit.
Summary of the invention
The technical problem to be solved: process the response rate for aluminum current ash low, energy expenditure is big, contaminated environment, and at present method prepare alumina powder jointed, powder granule is bigger, particle size distribution width and the drawback easily reunited, provide a kind of with aluminum ash for raw material, water is floating to remove slag, add sulfuric acid solution and diisopropanolamine (DIPA) removes the insoluble matter in aluminum ash, again at Carbon bisulfide, the lower removal of effect being aided with titanium dioxide is dissolved in other metal impurities of potassium hydroxide, by filtering to obtain jelly after adding Polyethylene Glycol and ammonia stirring, scrubbed dry, calcining, pulverize the method preparing high-activity aluminium oxide powder body.Preparation method of the present invention is simple, not only reduces the pollution to environment of the aluminum ash, and achieves the sustainable use of resource, and products obtained therefrom granule is little, not easily reunites.
For solving above-mentioned technical problem, the present invention adopts the technical scheme as described below to be:
(1) take aluminum ash and put in container, it is added thereto to water logging and does not have aluminum ash 5～7cm, re-use agitator with 300～500r/min rotating speed, it is stirred 20～25min, then stand until deposit-free sinks, take out the impurity swimming in the water surface, then it is carried out filtration under diminished pressure, by the flushed screening of dehydrated alcohol 3～5 times, the aluminum ash after filtering is put in baking oven dry subsequently；
(2) the aluminum ash after being dried by above-mentioned 200～300g is put in 1L container, it is added thereto to the sulfuric acid solution that mass fraction is 40%, stirring is until solid not re-dissolved, stop adding sulfuric acid solution, filter subsequently, collect filtrate, be added thereto to the diisopropanolamine (DIPA) of aluminum ash quality 5～8%, 1L container is heated to 60～65 DEG C, is incubated 50～70min；
(3) after above-mentioned insulation terminates, stopping heating, be added thereto to the potassium hydroxide solution that mass fraction is 20%, regulating pH is 12.0～13.0, then 1L container is moved in ice bath pot, temperature is set as 4～6 DEG C, stands after 10～15min, the titanium dioxide of the aluminum ash quality 0.8～1.2% after being added thereto to the Carbon bisulfide of filtrate volume 3～5% and drying, after stirring, 1L container is heated to 75 DEG C, uses agitator to stir with rotating speed 120r/min, be incubated 1～2h；
(4) after above-mentioned insulation terminates, stop heating and stirring, naturally cool to room temperature, standing until producing without precipitation, collecting by filtration filtrate subsequently and putting in 500mL container, it is added thereto to the Polyethylene Glycol of the aluminum ash quality 4～6% after drying, moving in water-bath by container again, be heated to 50 DEG C, stirring is until Polyethylene Glycol is completely dissolved, being added thereto to the ammonia that mass fraction is 20% again, stirring is until giving birth to without gluey produce；
(5) after raw without gluey produce, carry out filtration under diminished pressure, using distilled water and dehydrated alcohol, the jelly after washing and filtering 4～6 times, then put into jelly in the baking oven of 85 DEG C and dry respectively, put it in the calcining furnace of 1150～1230 DEG C subsequently, after calcining 1～3h, it is cooled to room temperature with stove, takes out to put in ball mill by calcined material and pulverize, sieve, the high-activity aluminium oxide powder body of different-grain diameter can be obtained.
The high-activity aluminium oxide powder density that the present invention prepares is 4.01～4.05g/cm3, specific surface area is 29.8～32.1m2/ g, particle diameter is 0.46～0.53 μm, and bending strength is 748～752MPa, and hardness is 12.0～12.8GPa, and fracture toughness is 10.95～11.35MPa m1/2。
The present invention is compared with additive method, and Advantageous Effects is:
(1) present invention makes full use of aluminum ash and prepares high-activity aluminium oxide powder body, not only solves problem of environmental pollution, also achieves the sustainable use of resource；
(2) the alumina powder jointed granule of gained is little, and even particle size distribution is not easily reunited, and activity is higher than alumina powder jointed more than 18% that additive method prepares.
Detailed description of the invention
First take aluminum ash and put in container, it is added thereto to water logging and does not have aluminum ash 5～7cm, re-use agitator with 300～500r/min rotating speed, it is stirred 20～25min, then stand until deposit-free sinks, take out the impurity swimming in the water surface, then it is carried out filtration under diminished pressure, by the flushed screening of dehydrated alcohol 3～5 times, the aluminum ash after filtering is put in baking oven dry subsequently；Then the aluminum ash after being dried by above-mentioned 200～300g is put in 1L container, it is added thereto to the sulfuric acid solution that mass fraction is 40%, stirring is until solid not re-dissolved, stop adding sulfuric acid solution, filter subsequently, collect filtrate, be added thereto to the diisopropanolamine (DIPA) of aluminum ash quality 5～8%, 1L container is heated to 60～65 DEG C, is incubated 50～70min；After above-mentioned insulation terminates, stopping heating, be added thereto to the potassium hydroxide solution that mass fraction is 20%, regulating pH is 12.0～13.0, then 1L container is moved in ice bath pot, temperature is set as 4～6 DEG C, stands after 10～15min, the titanium dioxide of the aluminum ash quality 0.8～1.2% after being added thereto to the Carbon bisulfide of filtrate volume 3～5% and drying, after stirring, 1L container is heated to 75 DEG C, uses agitator to stir with rotating speed 120r/min, be incubated 1～2h；After above-mentioned insulation terminates, stop heating and stirring, naturally cool to room temperature, standing until producing without precipitation, collecting by filtration filtrate subsequently and putting in 500mL container, it is added thereto to the Polyethylene Glycol of the aluminum ash quality 4～6% after drying, moving in water-bath by container again, be heated to 50 DEG C, stirring is until Polyethylene Glycol is completely dissolved, being added thereto to the ammonia that mass fraction is 20% again, stirring is until giving birth to without gluey produce；Finally after raw without gluey produce, carry out filtration under diminished pressure, using distilled water and dehydrated alcohol, the jelly after washing and filtering 4～6 times, then put into jelly in the baking oven of 85 DEG C and dry respectively, put it in the calcining furnace of 1150～1230 DEG C subsequently, after calcining 1～3h, it is cooled to room temperature with stove, takes out to put in ball mill by calcined material and pulverize, sieve, the high-activity aluminium oxide powder body of different-grain diameter can be obtained.
Example 1
First take aluminum ash and put in container, it is added thereto to water logging and does not have aluminum ash 5cm, re-use agitator with 300r/min rotating speed, it is stirred 20min, then stand until deposit-free sinks, take out the impurity swimming in the water surface, then it is carried out filtration under diminished pressure, by the flushed screening of dehydrated alcohol 3 times, the aluminum ash after filtering is put in baking oven dry subsequently；Then the aluminum ash after being dried by above-mentioned 200g is put in 1L container, it is added thereto to the sulfuric acid solution that mass fraction is 40%, stirring is until solid not re-dissolved, stop adding sulfuric acid solution, filter subsequently, collect filtrate, be added thereto to the diisopropanolamine (DIPA) of aluminum ash quality 5%, 1L container is heated to 60 DEG C, is incubated 50min；After above-mentioned insulation terminates, stopping heating, be added thereto to the potassium hydroxide solution that mass fraction is 20%, regulating pH is 12.0, then 1L container is moved in ice bath pot, temperature is set as 4 DEG C, stands after 10min, the titanium dioxide of the aluminum ash quality 0.8% after being added thereto to the Carbon bisulfide of filtrate volume 3% and drying, after stirring, 1L container is heated to 75 DEG C, uses agitator to stir with rotating speed 120r/min, be incubated 1h；After above-mentioned insulation terminates, stop heating and stirring, naturally cool to room temperature, standing until producing without precipitation, collecting by filtration filtrate subsequently and putting in 500mL container, it is added thereto to the Polyethylene Glycol of the aluminum ash quality 4% after drying, moving in water-bath by container again, be heated to 50 DEG C, stirring is until Polyethylene Glycol is completely dissolved, being added thereto to the ammonia that mass fraction is 20% again, stirring is until giving birth to without gluey produce；Finally after raw without gluey produce, carry out filtration under diminished pressure, using distilled water and dehydrated alcohol, the jelly after washing and filtering 4 times, then put into jelly in the baking oven of 85 DEG C and dry respectively, put it in the calcining furnace of 1150 DEG C subsequently, after calcining 1h, it is cooled to room temperature with stove, takes out to put in ball mill by calcined material and pulverize, sieve, the high-activity aluminium oxide powder body of different-grain diameter can be obtained.The present invention makes full use of aluminum ash and prepares high-activity aluminium oxide powder body, not only solves problem of environmental pollution, also achieves the sustainable use of resource；The alumina powder jointed granule of gained is little, and even particle size distribution is not easily reunited, and activity is higher than alumina powder jointed 18.2% that additive method prepares；The high-activity aluminium oxide powder density prepared is 4.01g/cm3, specific surface area is 29.8m2/ g, particle diameter is 0.46 μm, and bending strength is 748MPa, and hardness is 12.0GPa, and fracture toughness is 10.95MPa m1/2。
Example 2
First take aluminum ash and put in container, it is added thereto to water logging and does not have aluminum ash 6cm, re-use agitator with 400r/min rotating speed, it is stirred 23min, then stand until deposit-free sinks, take out the impurity swimming in the water surface, then it is carried out filtration under diminished pressure, by the flushed screening of dehydrated alcohol 4 times, the aluminum ash after filtering is put in baking oven dry subsequently；Then the aluminum ash after being dried by above-mentioned 250g is put in 1L container, it is added thereto to the sulfuric acid solution that mass fraction is 40%, stirring is until solid not re-dissolved, stop adding sulfuric acid solution, filter subsequently, collect filtrate, be added thereto to the diisopropanolamine (DIPA) of aluminum ash quality 7%, 1L container is heated to 63 DEG C, is incubated 60min；After above-mentioned insulation terminates, stopping heating, be added thereto to the potassium hydroxide solution that mass fraction is 20%, regulating pH is 12.5, then 1L container is moved in ice bath pot, temperature is set as 5 DEG C, stands after 13min, the titanium dioxide of the aluminum ash quality 1.0% after being added thereto to the Carbon bisulfide of filtrate volume 4% and drying, after stirring, 1L container is heated to 75 DEG C, uses agitator to stir with rotating speed 120r/min, be incubated 1.5h；After above-mentioned insulation terminates, stop heating and stirring, naturally cool to room temperature, standing until producing without precipitation, collecting by filtration filtrate subsequently and putting in 500mL container, it is added thereto to the Polyethylene Glycol of the aluminum ash quality 5% after drying, moving in water-bath by container again, be heated to 50 DEG C, stirring is until Polyethylene Glycol is completely dissolved, being added thereto to the ammonia that mass fraction is 20% again, stirring is until giving birth to without gluey produce；Finally after raw without gluey produce, carry out filtration under diminished pressure, using distilled water and dehydrated alcohol, the jelly after washing and filtering 5 times, then put into jelly in the baking oven of 85 DEG C and dry respectively, put it in the calcining furnace of 1190 DEG C subsequently, after calcining 2h, it is cooled to room temperature with stove, takes out to put in ball mill by calcined material and pulverize, sieve, the high-activity aluminium oxide powder body of different-grain diameter can be obtained.The present invention makes full use of aluminum ash and prepares high-activity aluminium oxide powder body, not only solves problem of environmental pollution, also achieves the sustainable use of resource；The alumina powder jointed granule of gained is little, and even particle size distribution is not easily reunited, and activity is higher than alumina powder jointed 19.0% that additive method prepares；The high-activity aluminium oxide powder density prepared is 4.03g/cm3, specific surface area is 30.9m2/ g, particle diameter is 0.49 μm, and bending strength is 750MPa, and hardness is 12.4GPa, and fracture toughness is 11.15MPa m1/2。
Example 3
First take aluminum ash and put in container, it is added thereto to water logging and does not have aluminum ash 7cm, re-use agitator with 500r/min rotating speed, it is stirred 25min, then stand until deposit-free sinks, take out the impurity swimming in the water surface, then it is carried out filtration under diminished pressure, by the flushed screening of dehydrated alcohol 5 times, the aluminum ash after filtering is put in baking oven dry subsequently；Then the aluminum ash after being dried by above-mentioned 300g is put in 1L container, it is added thereto to the sulfuric acid solution that mass fraction is 40%, stirring is until solid not re-dissolved, stop adding sulfuric acid solution, filter subsequently, collect filtrate, be added thereto to the diisopropanolamine (DIPA) of aluminum ash quality 8%, 1L container is heated to 65 DEG C, is incubated 70min；After above-mentioned insulation terminates, stopping heating, be added thereto to the potassium hydroxide solution that mass fraction is 20%, regulating pH is 13.0, then 1L container is moved in ice bath pot, temperature is set as 6 DEG C, stands after 15min, the titanium dioxide of the aluminum ash quality 1.2% after being added thereto to the Carbon bisulfide of filtrate volume 5% and drying, after stirring, 1L container is heated to 75 DEG C, uses agitator to stir with rotating speed 120r/min, be incubated 2h；After above-mentioned insulation terminates, stop heating and stirring, naturally cool to room temperature, standing until producing without precipitation, collecting by filtration filtrate subsequently and putting in 500mL container, it is added thereto to the Polyethylene Glycol of the aluminum ash quality 6% after drying, moving in water-bath by container again, be heated to 50 DEG C, stirring is until Polyethylene Glycol is completely dissolved, being added thereto to the ammonia that mass fraction is 20% again, stirring is until giving birth to without gluey produce；Finally after raw without gluey produce, carry out filtration under diminished pressure, using distilled water and dehydrated alcohol, the jelly after washing and filtering 6 times, then put into jelly in the baking oven of 85 DEG C and dry respectively, put it in the calcining furnace of 1230 DEG C subsequently, after calcining 3h, it is cooled to room temperature with stove, takes out to put in ball mill by calcined material and pulverize, sieve, the high-activity aluminium oxide powder body of different-grain diameter can be obtained.The present invention makes full use of aluminum ash and prepares high-activity aluminium oxide powder body, not only solves problem of environmental pollution, also achieves the sustainable use of resource；The alumina powder jointed granule of gained is little, and even particle size distribution is not easily reunited, and activity is higher than alumina powder jointed 19.9% that additive method prepares；The high-activity aluminium oxide powder density prepared is 4.05g/cm3, specific surface area is 32.1m2/ g, particle diameter is 0.53 μm, and bending strength is 752MPa, and hardness is 12.8GPa, and fracture toughness is 11.35MPa m1/2。
Claims (1)
1. one kind utilizes the method that aluminum ash prepares high-activity aluminium oxide powder body, it is characterised in that concrete preparation process is:
(1) take aluminum ash and put in container, it is added thereto to water logging and does not have aluminum ash 5～7cm, re-use agitator with 300～500r/min rotating speed, it is stirred 20～25min, then stand until deposit-free sinks, take out the impurity swimming in the water surface, then it is carried out filtration under diminished pressure, by the flushed screening of dehydrated alcohol 3～5 times, the aluminum ash after filtering is put in baking oven dry subsequently；
(2) the aluminum ash after being dried by above-mentioned 200～300g is put in 1L container, it is added thereto to the sulfuric acid solution that mass fraction is 40%, stirring is until solid not re-dissolved, stop adding sulfuric acid solution, filter subsequently, collect filtrate, be added thereto to the diisopropanolamine (DIPA) of aluminum ash quality 5～8%, 1L container is heated to 60～65 DEG C, is incubated 50～70min；
(3) after above-mentioned insulation terminates, stop heating, be added thereto to the potassium hydroxide solution that mass fraction is 20%, regulate pH to 12.0～13.0, then 1L container is moved in ice bath pot, temperature is set as 4～6 DEG C, stands after 10～15min, the titanium dioxide of the aluminum ash quality 0.8～1.2% after being added thereto to the Carbon bisulfide of filtrate volume 3～5% and drying, after stirring, 1L container is heated to 75 DEG C, uses agitator to stir with rotating speed 120r/min, be incubated 1～2h；
(4) after above-mentioned insulation terminates, stop heating and stirring, naturally cool to room temperature, standing until producing without precipitation, collecting by filtration filtrate subsequently and putting in 500mL container, it is added thereto to the Polyethylene Glycol of the aluminum ash quality 4～6% after drying, moving in water-bath by container again, be heated to 50 DEG C, stirring is until Polyethylene Glycol is completely dissolved, being added thereto to the ammonia that mass fraction is 20% again, stirring is until giving birth to without gluey produce；
(5) after raw without gluey produce, carry out filtration under diminished pressure, using distilled water and dehydrated alcohol, the jelly after washing and filtering 4～6 times, then put into jelly in the baking oven of 85 DEG C and dry respectively, put it in the calcining furnace of 1150～1230 DEG C subsequently, after calcining 1～3h, it is cooled to room temperature with stove, takes out to put in ball mill by calcined material and pulverize, sieve, the high-activity aluminium oxide powder body of different-grain diameter can be obtained.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106830025A (en) * | 2017-02-24 | 2017-06-13 | 南通大学 | aluminium ash recycling method |
| CN109665550A (en) * | 2018-11-20 | 2019-04-23 | 南通特乃博高新材料有限公司 | A kind of high-activity aluminium oxide powder and preparation method thereof |
| TWI760226B (en) * | 2021-05-19 | 2022-04-01 | 釔銪鑫應用材料有限公司 | Treatment method of metal oxide slag |
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| CN109665550A (en) * | 2018-11-20 | 2019-04-23 | 南通特乃博高新材料有限公司 | A kind of high-activity aluminium oxide powder and preparation method thereof |
| TWI760226B (en) * | 2021-05-19 | 2022-04-01 | 釔銪鑫應用材料有限公司 | Treatment method of metal oxide slag |
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Application publication date: 20160706 |