CN102320638A - Preparation method of low-sodium fine grain alumina - Google Patents
Preparation method of low-sodium fine grain alumina Download PDFInfo
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Abstract
The invention relates to a preparation method of low-sodium fine grain alumina, in particular to a preparation method of low-sodium submicro grain alumina used for electronic ceramics, microcrystalline ceramics, fine polishing, catalyst carriers and the like. The preparation method is characterized by taking industrial aluminium hydroxide as a raw material in the preparation process and comprising the following steps of: firstly carrying out hydrothermal phase inversion processing on aluminium hydroxide to obtain low-sodium fine grain alumina monohydrate with sodium oxide content being less than 500ppm; briquetting the obtained low-sodium fine grain alumina monohydrate, and then roasting to obtain low-sodium fine grain alumina; and finally grinding and grading, thus obtaining low-sodium submicro alumina. The preparation method of low-sodium fine grain alumina has the advantages of simple production process, wide raw material sources, low production cost, environment friendliness and the like, and can combine with the existing alumina production process and equipment to carry out hydrothermal processing, thus effectively simplifying the production process and lowering the production cost. The method is ideal for preparing ultra-low-sodium boehmite and alumina.
Description
Technical field
A kind of preparation method of low sodium fine-grained alumina relates to the preparation method of the low sodium sub-micron crystal alumina of usefulness such as a kind of electronic ceramics, micro-crystalline ceramic, meticulous polishing, catalyzer and carrier thereof.
Background technology
Thin brilliant (former grain fineness number is less than the 2 microns) aluminum oxide of low sodium have resistance to wear, the characteristic of corrosion-resistant, high-insulativity, easy-sintering etc., obtained application widely at micro-crystalline ceramic, high technology ceramics, foamed ceramics, IC chip, aviation light source device, electronic ceramics and semiconductor substrate, rigid disk substrate and LED with aspects such as the meticulous polishings of sapphire substrate at present.
Though adopt technologies such as aluminium carbonate ammonium pyrogenic silica, aluminium salt solution solution, spark-discharge method, spray pyrolysis, sol-gel method can produce the thin brilliant alumina product of low sodium of high conversion, have problems such as complex process, production cost height, contaminate environment.
At present a lot of enterprises are raw material with metallurgical-grade aluminum oxide or white lake, take off the sodium agent through interpolation and carry out high temperature and take off sodium and produce low sodium alumina.Because sodium oxide content is higher in commercial alumina or the white lake; Need to make the sodium oxide volatilization obtain low sodium alumina through high-temperature calcination through adding boride or halogenide etc.; Not only contaminate environment and etching apparatus, and, cause alumina grain thick because high temperature takes off in the sodium process alumina grain grows up fast; Former grain fineness number is difficult to prepare the alumina powder jointed of thin crystalline substance usually greater than 2 microns.In addition, the most of compounds containing sodium that volatilizees away in the pyroprocess is oxidized once more aluminium absorption in process of cooling, causes the sodium oxide content in the finished product higher, needs just can obtain through processes such as further pickling the sodium oxide powder of low sodium.CN 1189475A discloses the preparation method of the no reunion submicron alumina of a kind of low-cost preparation; The metallurgical aluminum oxide of producing with commercially available αYang Hualv powder or Bayer process is a raw material; After grinding, dispersion agent obtains submicron alumina through adding, but the aluminum oxide powder Na that this method obtains
2O content is higher, products such as inapplicable manufacturing electronic ceramics.CN1565975A discloses the method that salting-out process prepares submicron alumina that improves; Adopt the salt acid system to produce submicron alumina, can make the aluminum oxide of low sodium through saltouing, but adopt acid system to require high the corrosion resistance nature of equipment; And the purifying technique complicacy of saltouing, production cost is high.CN1342609A discloses the loose submicron of a kind of form, nano aluminium oxide technology of preparing; With aluminium and alcohol is that feedstock production goes out organic aluminium alcoholates salt; Obtain the high purity aluminium oxide hydrate through hydrolysis again, further obtain superfine alumina powder after the calcining, there is the high problem of raw materials cost in this method.CN200910168548.6 discloses the method for manufacture of a kind of boehmite particle and aluminium oxide particles; This patent is a raw material with the white lake of thin crystalline substance; Specific conductivity through control white lake slurry; And add the nucleus forming agent, preparing second particle is a water aluminum oxide of submicron order, through further preparing the submicron alumina that is fit to fine grinding polishing usefulness after the calcining.Though the method that adopts this patent to provide can be prepared the alumina powder jointed of thin crystalline substance; But this patent must be prepared the boehmite of submicron earlier; Because there are problems such as filtration, washing, dry difficulty in tiny causing of particle in the wet production process, cause production cost of products higher.
Summary of the invention
The object of the invention is exactly the deficiency that exists to above-mentioned prior art, provides that a kind of raw material sources are wide, the preparation method of environmental friendliness, technology is simple and production cost is low low sodium fine-grained alumina.
The objective of the invention is to realize through following technical scheme.
A kind of preparation method of low sodium fine-grained alumina; It is characterized in that the preparation process is raw material with the industrial aluminium hydroxide; At first white lake is carried out the hydro-thermal phase inversion and handle, obtain the low sodium thin brilliant water aluminum oxide of sodium oxide content, the thin brilliant water aluminum oxide briquetting of the low sodium that will obtain again less than 500ppm; Roasting afterwards obtains the thin brilliant aluminum oxide of low sodium, after grind, obtain after the classification low sodium alumina of submicron.
The preparation method of a kind of low sodium fine-grained alumina of the present invention is characterized in that white lake is carried out hydro-thermal phase inversion treating processes is to use hydro-thermal devices such as canalization to carry out hydrothermal treatment consists continuously.
The preparation method of a kind of low sodium fine-grained alumina of the present invention; It is characterized in that white lake is carried out in the hydro-thermal phase inversion treating processes; The white lake water-based slurry is preheating to employing canalization hydro-thermal device or a little more than hydrothermal temperature, slurry is fed directly in the autoclave series that has whipping appts and carries out abundant hydro-thermal reaction afterwards, and the slurry after reaction finishes is through flash tank flash distillation recovery waste heat; Slurry temperature is reduced to below 100 ℃, and slurry is carried out liquid-solid separation and washing.
The preparation method of a kind of low sodium fine-grained alumina of the present invention; It is characterized in that it is to adopt autoclave to carry out hydrothermal treatment consists continuously that white lake is carried out hydro-thermal phase inversion treating processes, also can adopt other hydro-thermal devices such as pure canalization hydro-thermal reaction device or autoclave to produce.
The preparation method of a kind of low sodium fine-grained alumina of the present invention is characterized in that white lake is carried out in the hydrothermal system of hydro-thermal phase inversion treating processes, and white lake consolidates to contain and be 10-800g/L in the water-based slurry.
The preparation method of a kind of low sodium fine-grained alumina of the present invention, the hydrothermal temperature that it is characterized in that white lake is carried out hydro-thermal phase inversion treating processes is 150 ℃ to 260 ℃, the hydro-thermal reaction time is 10 minutes to 12 hours.
The preparation method of a kind of low sodium fine-grained alumina of the present invention is characterized in that white lake is carried out hydro-thermal phase inversion treating processes, in hydro-thermal reaction system, adds mineral acid, organic acid or acidic electrolyte bath and makes the pH value of slurry be 3-7.
The preparation method of a kind of low sodium fine-grained alumina of the present invention is characterized in that white lake is carried out hydro-thermal phase inversion treating processes, and the mineral acid that in hydro-thermal reaction system, adds is hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid; Organic acid is acetic acid, oxalic acid, tartrate; Acidic electrolyte bath is aluminum nitrate, Tai-Ace S 150, aluminum chloride hydrogen salt.
The preparation method of a kind of low sodium fine-grained alumina of the present invention; It is characterized in that white lake is carried out hydro-thermal phase inversion treating processes; Adding pseudo-boehmite or superfine boehmite are crystal seed in hydro-thermal reaction system, and seed load is the 0.001%-30% of white lake quality.
The preparation method of a kind of low sodium fine-grained alumina of the present invention; It is characterized in that the thin brilliant water aluminum oxide briquetting process of the low sodium that will obtain adopts brick press or nodulizer shaped device to carry out; Obtain a water alumina brick or a ball; With pack into saggar or be placed on the refractory slabs such as SiC of the brick after the moulding or ball, in high temperature kilns such as shuttle kiln or flint road kiln, calcine afterwards; In one water that maybe will obtain alumina powder jointed directly pack into saggar or the crucible or be placed in the high temperature kiln, calcine on the refractory slab obtain alumina powder jointed.
The preparation method of a kind of low sodium fine-grained alumina of the present invention, when it is characterized in that in high temperature kilns such as shuttle kiln or flint road kiln, calcining, calcining temperature is 800-1500 ℃, the soaking time under calcining temperature is 0.5-20 hour.When calcining temperature is hanged down, obtain the activated alumina of low α phase content; Calcining temperature is higher than 1000 ℃, can obtain the high temperature alumina of high α phase content.
The preparation method of a kind of low sodium fine-grained alumina of the present invention; The low fine-grained alumina of receiving that obtains after it is characterized in that calcining; After airflow milling, stirring mill, ball milling or vibration mill are further levigate; After adopting air classification or hydraulic classification to remove macrobead, obtain submicron alumina or ultra-fine alumina.
The preparation method of a kind of low sodium fine-grained alumina of the present invention, it is simple to have production technique, and raw material sources are extensive; Low and the advantages of environment protection of production cost; And can combine existing alumina producing flow process and equipment to carry out hydrothermal treatment consists, and effectively simplified production technique, reduced production cost.It is a kind of Perfected process for preparing ultralow sodium boehmite and aluminum oxide.
Description of drawings
Fig. 1 is the process flow sheet of the inventive method.
Embodiment
A kind of preparation method of low sodium fine-grained alumina; Industrial aluminium hydroxide and pseudo-boehmite (or boehmite) crystal seed thorough mixing are processed slurry; In the hydro-thermal reaction device, under certain temperature, carry out hydro-thermal reaction, afterwards with slurry filter, wash, drying, obtain the thin brilliant water aluminum oxide of low sodium; Then a water aluminum oxide being adopted presses brick or apparatus for making pearl ball to be pressed into fragment of brick or ball; Be placed on and powder calcined in certain temperature in flint road kiln, shuttle kiln or other calcining kiln, be prepared into the thin brilliant aluminum oxide of low sodium, through further grinding, can obtain hanging down after the classification submicron alumina powder of sodium.
Its process is: at first industrial aluminium hydroxide and pure water or tap water are mixed with the slurry that necessarily contains admittedly; Can add crystal seed and the pH value of regulating slurry as required; In autoclave or in the hydro-thermal reaction device such as canalization, carry out hydro-thermal reaction; In hydro-thermal phase inversion process, remove impurity such as hydrated alumina interior oxidation sodium, potassium oxide, and be converted into former grain fineness number less than a water aluminum oxide agglomerate of 1 micron by the white lake of big crystal grain.A water aluminum oxide water-based slurry that obtains after the hydro-thermal reaction carries out liquid-solid separation; And adopt the alkali that attaches in pure water or the tap water washing leaching cake of heat; It is alumina powder jointed that filtration cakes torrefaction is obtained a water; Be pressed into brick or directly with the water aluminum oxide powder saggar of packing into, in flint road kiln, shuttle kiln, calcine afterwards again a water is alumina powder jointed, directly calcining one water is alumina powder jointed also can to adopt rotary kiln; Prepare low sodium thin brilliant high temperature alumina or activated alumina product, after further grinding, can make submicron or micron-sized superfine alumina powder.
Embodiment 1
10 tons of industrial aluminium hydroxides (mean particle size is 65 microns) are joined in the dosing vessel; The tap water that adds 50 cubic metres makes the slurry thorough mixing after stirring, by surge pump slurry is transported in the canalization device afterwards; After in pipeline, slip progressively being preheating to 220 ℃; Enter into autoclave and carry out hydro-thermal reaction, slurry residence time in autoclave is 60 minutes, and slurry cools to 98 ℃ through the flash tank flash distillation afterwards.Reaction back slurry gets into dashpot, through shurry pump slurry is delivered to vacuum band-type filter machine and carries out filtration washing, and a water aluminum oxide that obtains adopts brick pressing machine compression moulding; Put into afterwards on the SiC refractory slab, in 1250 ℃ of calcinings down, 1250 ℃ are incubated 6 hours in shuttle kiln; Obtain α inversion of phases rate greater than 95% high temperature alumina; Through scanning electron microscopic observation, former grain fineness number is about 0.8 micron, and sodium oxide content is 500ppm.
Embodiment 2
10 tons of industrial aluminium hydroxides (mean particle size is 65 microns) are joined in the dosing vessel; The tap water that adds 50 cubic metres makes the slurry thorough mixing after stirring, by surge pump slurry is transported in the canalization device afterwards; After in pipeline, slip progressively being preheating to 240 ℃; Enter into autoclave and carry out hydro-thermal reaction, slurry residence time in autoclave is 30 minutes, and slurry cools to 98 ℃ through the flash tank flash distillation afterwards.Reaction back slurry gets into dashpot, through shurry pump slurry is delivered to vacuum band-type filter machine and carries out filtration washing, and a water aluminum oxide that obtains adopts brick pressing machine compression moulding; Put into afterwards on the SiC refractory slab, in 1250 ℃ of calcinings down, 1350 ℃ are incubated 6 hours in shuttle kiln; Obtain α inversion of phases rate greater than 95% high temperature alumina; Through scanning electron microscopic observation, former grain fineness number is about 1.0 microns, and sodium oxide content is 400ppm.
Embodiment 3
10 tons of industrial aluminium hydroxides (mean particle size is 65 microns) are joined in the dosing vessel, add 50 cubic metres tap water, add 0.5 ton pseudo-boehmite; After stirring, make the slurry thorough mixing; By surge pump slurry is transported in the canalization device afterwards, in pipeline, slip progressively is preheating to 220 ℃ after, enter into autoclave and carry out hydro-thermal reaction; Slurry residence time in autoclave is 60 minutes, and slurry cools to 98 ℃ through the flash tank flash distillation afterwards.Reaction back slurry gets into dashpot, through shurry pump slurry is delivered to vacuum band-type filter machine and carries out filtration washing, and a water aluminum oxide that obtains adopts brick pressing machine compression moulding; Put into afterwards on the SiC refractory slab, in 1250 ℃ of calcinings down, 1250 ℃ are incubated 6 hours in shuttle kiln; Obtain α inversion of phases rate greater than 95% high temperature alumina; Through scanning electron microscopic observation, former grain fineness number is about 0.6 micron, and sodium oxide content is 450ppm.
Embodiment 4
10 tons of industrial aluminium hydroxides (mean particle size is 65 microns) are joined in the dosing vessel; The tap water that adds 50 cubic metres adds the pH value that about 16 liters industrial sulphuric acid is adjusted slurry, after stirring, makes the slurry thorough mixing; PH value through detecting slurry is about 4; By surge pump slurry is transported in the canalization device afterwards, in pipeline, slip progressively is preheating to 220 ℃ after, enter into autoclave and carry out hydro-thermal reaction; Slurry residence time in autoclave is 60 minutes, and slurry cools to 98 ℃ through the flash tank flash distillation afterwards.Reaction back slurry gets into dashpot, through shurry pump slurry is delivered to vacuum band-type filter machine and carries out filtration washing, and a water aluminum oxide that obtains adopts brick pressing machine compression moulding; Put into afterwards on the SiC refractory slab, in 1250 ℃ of calcinings down, 1250 ℃ are incubated 6 hours in shuttle kiln; Obtain α inversion of phases rate greater than 95% high temperature alumina; Through scanning electron microscopic observation, former grain fineness number is about 0.8 micron, and sodium oxide content is 200ppm.
Embodiment 5
10 tons of industrial aluminium hydroxides (mean particle size is 65 microns) are joined in the dosing vessel; The tap water that adds 50 cubic metres adds about 100 kilograms industrial nitric acid aluminium, after stirring, makes the slurry thorough mixing; PH value through detecting slurry is about 6.5; By surge pump slurry is transported in the canalization device afterwards, in pipeline, slip progressively is preheating to 220 ℃ after, enter into autoclave and carry out hydro-thermal reaction; Slurry residence time in autoclave is 60 minutes, and slurry cools to 98 ℃ through the flash tank flash distillation afterwards.Reaction back slurry gets into dashpot, through shurry pump slurry is delivered to vacuum band-type filter machine and carries out filtration washing, a water aluminum oxide that the obtains saggar of packing into; In flint road kiln, calcine afterwards; In 1450 ℃ of insulations 6 hours, obtain α inversion of phases rate greater than 95% high temperature alumina, through scanning electron microscopic observation; Former grain fineness number is about 0.9 micron, and sodium oxide content is 300ppm.
Embodiment 6
10 tons of industrial aluminium hydroxides (mean particle size is 65 microns) are joined in the dosing vessel; The tap water that adds 50 cubic metres adds about 100 kilograms industrial nitric acid aluminium, after stirring, makes the slurry thorough mixing; PH value through detecting slurry is about 6.5; By surge pump slurry is transported in the canalization device afterwards, in pipeline, slip progressively is preheating to 220 ℃ after, enter into autoclave and carry out hydro-thermal reaction; Slurry residence time in autoclave is 60 minutes, and slurry cools to 98 ℃ through the flash tank flash distillation afterwards.Reaction back slurry gets into dashpot; Through shurry pump slurry being delivered to vacuum band-type filter machine filters, washs; A water aluminum oxide that the obtains saggar of packing into is calcined in shuttle kiln afterwards, in 900 ℃ of insulations 4 hours down; The former grain fineness number that obtains is about 0.75 micron activated alumina, and sodium oxide content is 300ppm.
Claims (13)
1. the preparation method of a low sodium fine-grained alumina; It is characterized in that the preparation process is raw material with the industrial aluminium hydroxide; At first white lake is carried out the hydro-thermal phase inversion and handle, obtain the low sodium thin brilliant water aluminum oxide of sodium oxide content, the thin brilliant water aluminum oxide briquetting of the low sodium that will obtain again less than 500ppm; Roasting afterwards obtains the thin brilliant aluminum oxide of low sodium, after grind, obtain after the classification low sodium alumina of submicron.
2. the preparation method of a kind of low sodium fine-grained alumina according to claim 1 is characterized in that white lake is carried out hydro-thermal phase inversion treating processes is to use canalization hydro-thermal device to carry out hydrothermal treatment consists continuously.
3. the preparation method of a kind of low sodium fine-grained alumina according to claim 1; It is characterized in that white lake is carried out in the hydro-thermal phase inversion treating processes; Adopt canalization hydro-thermal device that the white lake water-based slurry is preheating to or a little more than hydrothermal temperature; Slurry is fed directly in the autoclave series that has whipping appts and carries out abundant hydro-thermal reaction afterwards; Slurry after reaction finishes is through flash tank flash distillation recovery waste heat, and slurry temperature is reduced to below 100 ℃, and slurry is carried out liquid-solid separation and washing.
4. the preparation method of a kind of low sodium fine-grained alumina according to claim 1 is characterized in that it is to adopt autoclave to carry out hydrothermal treatment consists continuously that white lake is carried out hydro-thermal phase inversion treating processes.
5. the preparation method of a kind of low sodium fine-grained alumina according to claim 1, described hydrothermal treatment device comprise the canalization preheating hydro-thermal reaction devices such as reaction kettle treatment system, pure canalization hydrothermal treatment consists system or autoclave that add high pressure.
6. the preparation method of a kind of low sodium fine-grained alumina according to claim 1 is characterized in that white lake is carried out in the hydrothermal system of hydro-thermal phase inversion treating processes, and white lake consolidates to contain and be 10-800g/L in the water-based slurry.
7. the preparation method of a kind of low sodium fine-grained alumina according to claim 1, the hydrothermal temperature that it is characterized in that white lake is carried out hydro-thermal phase inversion treating processes is 150 ℃ to 260 ℃, the hydro-thermal reaction time is 10 minutes to 12 hours.
8. the preparation method of a kind of low sodium fine-grained alumina according to claim 1 is characterized in that white lake is carried out hydro-thermal phase inversion treating processes, in hydro-thermal reaction system, adds mineral acid, organic acid or acidic electrolyte bath and makes the pH value of slurry be 3-7.
9. the preparation method of a kind of low sodium fine-grained alumina according to claim 1 is characterized in that white lake is carried out hydro-thermal phase inversion treating processes, and the mineral acid that in hydro-thermal reaction system, adds is hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid; Organic acid is acetic acid, oxalic acid, tartrate; Acidic electrolyte bath is aluminum nitrate, Tai-Ace S 150, aluminum chloride hydrogen salt.
10. the preparation method of a kind of low sodium fine-grained alumina according to claim 1; It is characterized in that white lake is carried out hydro-thermal phase inversion treating processes; Adding pseudo-boehmite or superfine boehmite are crystal seed in hydro-thermal reaction system, and seed load is the 0.001%-30% of white lake quality.
11. the preparation method of a kind of low sodium fine-grained alumina according to claim 1; It is characterized in that the thin brilliant water aluminum oxide briquetting process of the low sodium that will obtain adopts brick press or nodulizer shaped device to carry out; Obtain a water alumina brick or a ball; With pack into saggar or be placed on the refractory slabs such as SiC of the brick after the moulding or ball, in high temperature kilns such as shuttle kiln or flint road kiln, calcine afterwards; In one water that maybe will obtain alumina powder jointed directly pack into saggar or the crucible or be placed in the high temperature kiln, calcine on the refractory slab obtain alumina powder jointed.
12. the preparation method of a kind of low sodium fine-grained alumina according to claim 1, when it is characterized in that in high temperature kilns such as shuttle kiln or flint road kiln, calcining, calcining temperature is 800-1500 ℃, and the soaking time under calcining temperature is 0.5-20 hour.When calcining temperature is hanged down, obtain the activated alumina of low α phase content; Calcining temperature is higher than 1000 ℃, can obtain the high temperature alumina of high α phase content.
13. the preparation method of a kind of low sodium fine-grained alumina according to claim 1; The low fine-grained alumina of receiving that obtains after it is characterized in that calcining; After airflow milling, stirring mill, ball milling or vibration mill are further levigate; After adopting air classification or hydraulic classification to remove macrobead, obtain submicron alumina or ultra-fine alumina.
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