CN102092749A - Preparation method of boehmite - Google Patents
Preparation method of boehmite Download PDFInfo
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- CN102092749A CN102092749A CN 201010587685 CN201010587685A CN102092749A CN 102092749 A CN102092749 A CN 102092749A CN 201010587685 CN201010587685 CN 201010587685 CN 201010587685 A CN201010587685 A CN 201010587685A CN 102092749 A CN102092749 A CN 102092749A
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- boehmite
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- aluminium hydroxide
- acid
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- 229910001593 boehmite Inorganic materials 0.000 title claims abstract description 65
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 39
- 239000002002 slurry Substances 0.000 claims description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 11
- 239000012065 filter cake Substances 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 8
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 150000007524 organic acids Chemical class 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- HIGRAKVNKLCVCA-UHFFFAOYSA-N alumine Chemical compound C1=CC=[Al]C=C1 HIGRAKVNKLCVCA-UHFFFAOYSA-N 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 claims description 2
- 239000000084 colloidal system Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000011734 sodium Substances 0.000 abstract description 30
- 229910052708 sodium Inorganic materials 0.000 abstract description 25
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 23
- 238000000034 method Methods 0.000 abstract description 19
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 230000002378 acidificating effect Effects 0.000 abstract description 6
- 239000003792 electrolyte Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 12
- 239000012535 impurity Substances 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 239000003513 alkali Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000010907 mechanical stirring Methods 0.000 description 5
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 5
- 229910001948 sodium oxide Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical class [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 1
- IOGARICUVYSYGI-UHFFFAOYSA-K azanium (4-oxo-1,3,2-dioxalumetan-2-yl) carbonate Chemical compound [NH4+].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O IOGARICUVYSYGI-UHFFFAOYSA-K 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
Abstract
The invention relates to a preparation method of boehmite, particularly a preparation method of ultralow-sodium boehmite. In the preparation process, aluminum hydroxide is used as the raw material. The preparation method is characterized by comprising the following steps: adding water into the raw material aluminum hydroxide to obtain a pulp, and carrying out hydrothermal treatment, wherein in the hydrothermal treatment process, boehmite and the like are added as seed crystals to control the granular form of the boehmite, and acid or acidic electrolyte is added to enable the pulp to be weakly acidic, thereby further reducing the sodium content in the boehmite; and filtering, washing and drying to obtain the boehmite. The method provided by the invention has the advantages of simple production technique, wide material source, low production cost and the like, and is an ideal method for preparing ultralow-sodium boehmite and aluminum oxide.
Description
Technical field
A kind of preparation method of boehmite, particularly a kind of preparation method of ultralow sodium boehmite.
Background technology
Boehmite is a kind of preparation activated alumina, support of the catalyst and calcining α-Al
2O
3Important source material, the physicochemical property of presoma boehmite directly has influence on the use properties of activated alumina and Calcined polishing aluminum oxide.Na
2O is one of impurity of harm maximum in the chemical aluminum oxide, when making heat resisting and pressure resisting insulation device, radioceramic, unicircuit ceramic substrate, resistance porcelain spare, high speed cutting sintex, sodium vapor lamp pipe, and impurity Na in all strict controlled oxidation aluminium
2The content of O.
Oxidation of impurities sodium content height in the boehmite, the γ-Al that generates after the roasting
2O
3Pore volume is less, influences the reactive behavior of catalyzer.Na in hydrated alumina
2O exists with the form of absorption alkali, intergranular alkali and crystalline alkali, waits the most of absorption of measure flush away alkali by strengthening washing, reduces the Na in the hydrated alumina
2O content DeGrain.Can produce the alumina product of ultralow sodium though adopt technologies such as aluminium carbonate ammonium pyrolysis method, aluminium alcoholates salt solution solution, spark-discharge method, spray pyrolysis, sol-gel method, but there are problems such as raw materials cost height, complex process, production cost height, and be that raw material adopts after the roasting pickling purifying process and adds when the high-temperature calcination and takes off the sodium agent and produce low sodium alumina and have environmental pollution, former crystalline substance problem such as easily grow up with metallurgical grade aluminium hydroxide, influence the use properties of product.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provides a kind of and can effectively reduce impurity Na
2The content of O is enhanced product performance, the preparation method of the boehmite that technology is simple, cost is low.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of boehmite, it is raw material that its preparation process adopts aluminium hydroxide, it is characterized in that preparation process at first adds water slurryization with the aluminium hydroxide raw material, carries out hydrothermal treatment consists, filter again, wash and drying after the boehmite produced.
The preparation method of a kind of boehmite of the present invention is characterized in that the aluminium hydroxide raw material is added consolidating to contain and being 10-800g/L of aluminium hydroxide in the slurry of water slurryization.
The preparation method of a kind of boehmite of the present invention is characterized in that its temperature of carrying out heat treated is 160 ℃-260 ℃, and the treatment time is 10 minutes-12 hours.
The preparation method of a kind of boehmite of the present invention when it is characterized in that carrying out hydrothermal treatment consists, adds boehmite or alumine hydroxide colloid or activated alumina, aluminum nitrate as crystal seed, and the crystal seed amount is the 0.0001%-40% of aluminium hydroxide quality.
The preparation method of a kind of boehmite of the present invention before it is characterized in that carrying out hydrothermal treatment consists, stirs or ball milling, and aluminium hydroxide is levigate to 1-30 μ m.
The preparation method of a kind of boehmite of the present invention adds the mineral acid of hydrochloric acid, nitric acid, sulfuric acid or phosphoric acid, or is acetic acid, oxalic acid, tartaric organic acid, or is the acid salt of aluminum nitrate, Tai-Ace S 150, aluminum chloride when it is characterized in that carrying out hydrothermal treatment consists; The pH value of slurry is controlled between the 3-6.
The preparation method of a kind of boehmite of the present invention, it is characterized in that filtering, washing and drying process be with the filtration slurry with hot pure water drip washing filter cake, again filter cake is carried out drying and dehydrating, the exsiccant temperature is 60-150 ℃.
The preparation method of a kind of boehmite of the present invention is characterized in that the aluminium hydroxide raw material is an industrial aluminium hydroxide.
The preparation method of a kind of boehmite of the present invention is characterized in that its raw material is pseudo-boehmite, ρ aluminum oxide or gamma-alumina.
The preparation method of a kind of boehmite of the present invention, the hydrothermal method of employing be preparation ultra-fine, do not have to reunite or fewly reunite, a kind of technology of the powder body material of complete crystallization.Aluminium hydroxide changes boehmite under certain hydrothermal condition, can remove intergranular alkali effectively in the phase inversion process, obtains the hydrated alumina of ultralow sodium.The boehmite of Hydrothermal Preparation is the high quality raw material of preparation electronic ceramics, high-grade catalyzer and support of the catalyst.Compare with the low sodium alumina hydrate of other explained hereafter, the aluminium hydroxide raw material that alkaline process is produced is cheap and easy to get, aluminium hydroxide is carried out hydro-thermal take off sodium, can carry out hydrothermal treatment consists in conjunction with domestic alumina producing flow process and equipment, simplify production technique, reduce processing cost.
Advantages such as the boehmite of the ultralow sodium of hydrothermal treatment consists aluminium hydroxide feedstock production has raw material and is easy to get, and technology is simple, and production cost is relatively low have good market development prospect and competitive edge.
A kind of preparation method of boehmite, the industrial aluminium hydroxide of alkaline process production or pseudo-boehmite are made above-mentioned aluminum contained compound phase inversion under hydrothermal reaction condition be boehmite, in the phase inversion process, effectively reduce the sodium oxide content in the hydrated alumina, obtain the boehmite of low sodium.Add pseudo-boehmite or boehmite or aluminum nitrate (producing aluminium glue with the alkali reaction of separating out in the water-heat process) and be crystal seed in the phase inversion process, can effectively control the granule-morphology of boehmite, obtaining pattern is fiber, rhombus or prismatic boehmite.Preparation process is mixed with the slurry that necessarily contains admittedly with industrial aluminium hydroxide or pseudo-boehmite and pure water, can add crystal seed or acidic electrolyte bath as required, in hydro-thermal reaction devices such as autoclave or canalization, carry out hydro-thermal reaction, in hydro-thermal phase inversion process, remove the impurity such as sodium oxide, potassium oxide of the solubility of hydrated alumina inside, obtain the low sodium boehmite of various granule-morphology.
Method of the present invention, it is simple to have production technique, and raw material sources are extensive, advantages such as production cost is low, the boehmite of the ultralow sodium of hydrothermal treatment consists aluminium hydroxide feedstock production has raw material and is easy to get, advantages such as technology is simple, and production cost is relatively low have good market development prospect and competitive edge.
Embodiment
A kind of preparation method of boehmite at first puts into hydro-thermal containers such as autoclave with aluminium hydroxide and water, for further reducing the sodium oxide foreign matter content in the boehmite, can add a certain amount of acidic electrolyte bath class additive; Heating afterwards raises the hydrothermal system temperature, can prevent that by stirring aluminum hydroxide particles from precipitating in system, after the hydro-thermal reaction of certain hour, reduce the temperature of hydrothermal system by heat exchange, when temperature is reduced to below 100 ℃, the slurry after the filtered water thermal response, and with about pure water washing leaching cake secondary, with filtration cakes torrefaction, obtain the ultralow sodium boehmite of sodium oxide content afterwards less than 300ppm.
In hydrothermal system, the solid content of aluminium hydroxide is 10-800g/L in the water-based slurry, and solid content is more little, and it is good more to take off the sodium effect, but influences the production capacity of equipment; When solid content was too high, slurry viscosity height was unfavorable for the diffusion of ion in water, but production capacity height during the platform of equipment.
Hydrothermal temperature is 160 ℃-260 ℃, the temperature height, and hydro-thermal phase inversion speed of response is fast, and the needed hydro-thermal time is short, but the temperature height, the pressure of hydrothermal system is big, to the requirement of strength height of equipment.In addition, the temperature height, the former grain fineness number of the boehmite that obtains is big, and the former grain fineness number of the boehmite that obtains during low temperature is more tiny.
According to the height difference of hydrothermal temperature, it is also different to obtain the required hydro-thermal reaction time of ultralow sodium boehmite, is 10 minutes to 12 hours even longer reaction times of needs.
The adding acidic electrolyte bath helps further to reduce the content of sodium oxide impurity in the boehmite.Acidic electrolyte bath is organic acids such as mineral acids such as hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid or acetic acid, oxalic acid, tartrate, also can use bisalts such as aluminum nitrate, Tai-Ace S 150, aluminum chloride.In order to prevent the corrosion of acid to water heating apparatus, should control the add-on of acid, the pH value that makes slurry greater than 3 less than 7.
Add a small amount of boehmite, pseudo-boehmite etc. and contain the crystal seed of aluminum oxide as aluminium hydroxide hydro-thermal phase inversion, reaction has promoter action to the hydro-thermal phase inversion, and helps to obtain the boehmite of micron order or submicron order.
Embodiment 1
300 gram industrial aluminium hydroxides (mean particle size is 65 microns) are joined in the autoclave of 5L, the pure water that adds 3L, afterwards in autoclave in 220 ℃ of hydro-thermal reactions 3 hours, in order to guarantee that aluminium hydroxide fully suspends in slurry, need to adopt mechanical stirring to stir slurry, machinery back stirring velocity is not less than 80 rev/mins.After reaction finished, off-response still heating power supply when continuing to be stirred to temperature and being reduced to below 95 ℃, was opened autoclave, after taking out slurry and filtering, and washed about 3 liters of drip washing 3 times with 80 ℃ of hot pure water.Filter cake is dry under 110 ℃ afterwards, and the oxidation of impurities sodium content is 320ppm in the boehmite that obtains, and former grain fineness number is about 2.5 microns, and crystal morphology is a rhombus.
Embodiment 2
300 gram industrial aluminium hydroxides (mean particle size is 65 microns) are joined in the autoclave of 5L, the pure water that adds 3L, the concentration of pressing 2g/L adds acetic acid 6 grams, afterwards in autoclave in 220 ℃ of hydro-thermal reactions 3 hours, in order to guarantee that aluminium hydroxide fully suspends in slurry, need to adopt mechanical stirring to stir slurry, machinery back stirring velocity is not less than 80 rev/mins.After reaction finished, off-response still heating power supply when continuing to be stirred to temperature and being reduced to below 95 ℃, was opened autoclave, after taking out slurry and filtering, and washed about 3 liters of drip washing 3 times with 80 ℃ of hot pure water.Filter cake is dry under 110 ℃ afterwards, and the oxidation of impurities sodium content is 60ppm in the boehmite that obtains, and former grain fineness number is about 2.0 microns, and crystal morphology is a rhombus.
Embodiment 3
1200 gram industrial aluminium hydroxides (mean particle size is 65 microns) are joined in the autoclave of 5L, the pure water that adds 3L, press 10% of aluminium hydroxide quality and add 9 water aluminum nitrates, 12 grams, afterwards in autoclave in 200 ℃ of hydro-thermal reactions 4 hours, in order to guarantee that aluminium hydroxide fully suspends in slurry, need to adopt mechanical stirring to stir slurry, machinery back stirring velocity is not less than 80 rev/mins.After reaction finished, off-response still heating power supply when continuing to be stirred to temperature and being reduced to below 95 ℃, was opened autoclave, after taking out slurry and filtering, and washed about 3 liters of drip washing 3 times with 80 ℃ of hot pure water.Filter cake is dry under 110 ℃ afterwards, and the oxidation of impurities sodium content is 150ppm in the boehmite that obtains, and mean particle size is 1.5 microns, and crystal morphology is fibrous (length-to-diameter ratio is greater than 5).
Embodiment 4
1200 gram industrial aluminium hydroxides (mean particle size is 65 microns) are joined in the autoclave of 5L, the pure water that adds 3L, press 3% of aluminium hydroxide quality and add industrial pseudo-boehmite 36 grams, afterwards in autoclave in 240 ℃ of hydro-thermal reactions 1 hour, in order to guarantee that aluminium hydroxide fully suspends in slurry, need to adopt mechanical stirring to stir slurry, machinery back stirring velocity is not less than 80 rev/mins.After reaction finished, off-response still heating power supply when continuing to be stirred to temperature and being reduced to below 95 ℃, was opened autoclave, after taking out slurry and filtering, and washed about 3 liters of drip washing 3 times with 80 ℃ of hot pure water.Filter cake is dry under 110 ℃ afterwards, and the oxidation of impurities sodium content is 250ppm in the boehmite that obtains, and former grain fineness number is about 0.8 micron, and the mean particle size of boehmite is about 1.15 microns, and crystal morphology is prismatic.
Embodiment 5
2100 gram pseudo-boehmites are joined in the autoclave of 5L, the pure water that adds 3L, afterwards in autoclave in 160 ℃ of hydro-thermal reactions 10 hours, fully suspend in slurry in order to guarantee aluminium hydroxide, need to adopt mechanical stirring to stir slurry, machinery back stirring velocity is not less than 80 rev/mins.After reaction finished, off-response still heating power supply when continuing to be stirred to temperature and being reduced to below 95 ℃, was opened autoclave, after taking out slurry and filtering, and washed about 3 liters of drip washing 3 times with 80 ℃ of hot pure water.Filter cake is dry under 110 ℃ afterwards, and the oxidation of impurities sodium content is 250ppm in the boehmite that obtains.
Embodiment 6
200 gram ρ-aluminum oxide (mean particle size is 65 microns) are joined in the autoclave of 5L, the pure water that adds 3L, press 3% of aluminium hydroxide quality and add industrial pseudo-boehmite 36 grams, afterwards in autoclave in 260 ℃ of hydro-thermal reactions 0.5 hour, 85 rev/mins of machinery back stirring velocitys.After reaction finished, off-response still heating power supply when continuing to be stirred to temperature and being reduced to below 95 ℃, was opened autoclave, after taking out slurry and filtering, and washed about 3 liters of drip washing 3 times with 80 ℃ of hot pure water.Filter cake is dry under 110 ℃ afterwards, and the oxidation of impurities sodium content is 300ppm in the boehmite that obtains, and former grain fineness number is about 0.8 micron.
Claims (9)
1. the preparation method of a boehmite, it is raw material that its preparation process adopts aluminium hydroxide, it is characterized in that preparation process at first adds water slurryization with the aluminium hydroxide raw material, carries out hydrothermal treatment consists, filter again, wash and drying after produce boehmite.
2. the preparation method of a kind of boehmite according to claim 1 is characterized in that the aluminium hydroxide raw material is added consolidating to contain and being 10-800g/L of aluminium hydroxide in the slurry of water slurryization.
3. the preparation method of a kind of boehmite according to claim 1 is characterized in that its temperature of carrying out hydrothermal treatment consists is 160 ℃-260 ℃, and the treatment time is 10 minutes-12 hours.
4. the preparation method of a kind of boehmite according to claim 1 is characterized in that carrying out the hydrothermal treatment consists amount, adds boehmite or alumine hydroxide colloid or activated alumina, aluminum nitrate as crystal seed, and the crystal seed amount is the 0.0001%-40% of aluminium hydroxide quality.
5. the preparation method of a kind of boehmite according to claim 1 when it is characterized in that carrying out hydrothermal treatment consists, stirs or ball milling, and aluminium hydroxide is levigate to 1-30 μ m.
6. the preparation method of a kind of boehmite according to claim 1, the mineral acid that adds hydrochloric acid, nitric acid, sulfuric acid or phosphoric acid when it is characterized in that carrying out hydrothermal treatment consists, or be acetic acid, oxalic acid, tartaric organic acid, or be the acid salt of aluminum nitrate, Tai-Ace S 150, aluminum chloride; The pH value of slurry is controlled between the 3-6.
7. the preparation method of a kind of boehmite according to claim 1, it is characterized in that filtering, washing and drying process be with the filtration slurry with hot pure water drip washing filter cake, again filter cake is carried out drying and dehydrating, the exsiccant temperature is 60-150 ℃.
8. the preparation method of a kind of boehmite according to claim 1 is characterized in that the aluminium hydroxide raw material is an industrial aluminium hydroxide.
9. the preparation method of a kind of boehmite according to claim 1 is characterized in that its raw material is pseudo-boehmite, ρ aluminum oxide or gamma-alumina.
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| CN 201010587685 CN102092749A (en) | 2010-12-15 | 2010-12-15 | Preparation method of boehmite |
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| CN 201010587685 CN102092749A (en) | 2010-12-15 | 2010-12-15 | Preparation method of boehmite |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320638A (en) * | 2011-08-04 | 2012-01-18 | 中国铝业股份有限公司 | Preparation method of low-sodium fine grain alumina |
| CN102815733A (en) * | 2012-09-20 | 2012-12-12 | 天津博苑高新材料有限公司 | Nanometer boehmite and preparation method thereof |
| CN102815732A (en) * | 2012-09-20 | 2012-12-12 | 天津碧海蓝天水性高分子材料有限公司 | Nanometer boehmite having high dispersion performance, and preparation method and application of nanometer boehmite |
| CN102910655A (en) * | 2012-11-20 | 2013-02-06 | 中国海洋石油总公司 | Method for preparing pseudoboehmite by quick removal powder |
| CN105836770A (en) * | 2016-03-24 | 2016-08-10 | 中国铝业股份有限公司 | Preparation method of high-temperature-resistant boehmite |
| CN106517280A (en) * | 2016-11-02 | 2017-03-22 | 齐鲁工业大学 | Technology for preparing boehmite microcrystal powder only through adjusting pressure |
| CN106517273A (en) * | 2016-11-02 | 2017-03-22 | 齐鲁工业大学 | Production method used for preparing low sodium boehmite |
| CN107298453A (en) * | 2017-07-03 | 2017-10-27 | 中国科学院青海盐湖研究所 | The nanocrystalline preparation method of boehmite |
| CN107416875A (en) * | 2017-08-16 | 2017-12-01 | 云南冶金集团创能金属燃料电池股份有限公司 | The method for preparing high purity aluminium oxide |
| CN109179461A (en) * | 2018-09-19 | 2019-01-11 | 孝义市泰兴铝镁有限公司 | A kind of low sodium boehmite and preparation method thereof, device |
| CN109336145A (en) * | 2018-11-09 | 2019-02-15 | 大连交通大学 | A kind of preparation method of boehmite |
| CN109534376A (en) * | 2019-01-17 | 2019-03-29 | 滨州市金毅设备有限公司 | A kind of high purification preparation method of boehmite |
| CN112062144A (en) * | 2020-09-19 | 2020-12-11 | 河津市炬华铝业有限公司 | Large-pore-volume pseudo-boehmite and preparation method thereof |
| CN112479240A (en) * | 2020-11-30 | 2021-03-12 | 上海簇睿低碳能源技术有限公司 | Preparation method of high-viscosity pseudo-boehmite |
| CN113023757A (en) * | 2021-01-27 | 2021-06-25 | 三门峡义翔铝业有限公司 | Process for preparing ultralow-sodium boehmite by hydrothermal method and ultralow-sodium boehmite |
| CN113060748A (en) * | 2021-04-15 | 2021-07-02 | 洛阳中超新材料股份有限公司 | Submicron boehmite and preparation method |
| CN113800543A (en) * | 2021-09-23 | 2021-12-17 | 大连理工大学 | Method for accelerating hydrothermal conversion rate of aluminum hydroxide into boehmite |
| CN114560482A (en) * | 2022-02-08 | 2022-05-31 | 中铝山东有限公司 | Pseudo-boehmite powder, forming carrier and preparation method thereof |
| CN114772615A (en) * | 2022-04-24 | 2022-07-22 | 郑州原发精细微粉材料技术有限公司 | Production method of heavy rhombohedral boehmite |
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| CN102320638A (en) * | 2011-08-04 | 2012-01-18 | 中国铝业股份有限公司 | Preparation method of low-sodium fine grain alumina |
| CN102815733A (en) * | 2012-09-20 | 2012-12-12 | 天津博苑高新材料有限公司 | Nanometer boehmite and preparation method thereof |
| CN102815732A (en) * | 2012-09-20 | 2012-12-12 | 天津碧海蓝天水性高分子材料有限公司 | Nanometer boehmite having high dispersion performance, and preparation method and application of nanometer boehmite |
| CN102910655A (en) * | 2012-11-20 | 2013-02-06 | 中国海洋石油总公司 | Method for preparing pseudoboehmite by quick removal powder |
| CN105836770A (en) * | 2016-03-24 | 2016-08-10 | 中国铝业股份有限公司 | Preparation method of high-temperature-resistant boehmite |
| CN106517280A (en) * | 2016-11-02 | 2017-03-22 | 齐鲁工业大学 | Technology for preparing boehmite microcrystal powder only through adjusting pressure |
| CN106517273A (en) * | 2016-11-02 | 2017-03-22 | 齐鲁工业大学 | Production method used for preparing low sodium boehmite |
| CN107298453A (en) * | 2017-07-03 | 2017-10-27 | 中国科学院青海盐湖研究所 | The nanocrystalline preparation method of boehmite |
| CN107416875B (en) * | 2017-08-16 | 2019-09-03 | 云南创能斐源金属燃料电池有限公司 | The method for preparing high purity aluminium oxide |
| CN107416875A (en) * | 2017-08-16 | 2017-12-01 | 云南冶金集团创能金属燃料电池股份有限公司 | The method for preparing high purity aluminium oxide |
| CN109179461B (en) * | 2018-09-19 | 2021-03-23 | 孝义市泰兴铝镁有限公司 | Low-sodium pseudo-boehmite, preparation method and device thereof |
| CN109179461A (en) * | 2018-09-19 | 2019-01-11 | 孝义市泰兴铝镁有限公司 | A kind of low sodium boehmite and preparation method thereof, device |
| CN109336145A (en) * | 2018-11-09 | 2019-02-15 | 大连交通大学 | A kind of preparation method of boehmite |
| CN109534376A (en) * | 2019-01-17 | 2019-03-29 | 滨州市金毅设备有限公司 | A kind of high purification preparation method of boehmite |
| CN112062144A (en) * | 2020-09-19 | 2020-12-11 | 河津市炬华铝业有限公司 | Large-pore-volume pseudo-boehmite and preparation method thereof |
| CN112062144B (en) * | 2020-09-19 | 2021-05-18 | 河津市炬华铝业有限公司 | Large-pore-volume pseudo-boehmite and preparation method thereof |
| CN112479240A (en) * | 2020-11-30 | 2021-03-12 | 上海簇睿低碳能源技术有限公司 | Preparation method of high-viscosity pseudo-boehmite |
| CN113023757A (en) * | 2021-01-27 | 2021-06-25 | 三门峡义翔铝业有限公司 | Process for preparing ultralow-sodium boehmite by hydrothermal method and ultralow-sodium boehmite |
| CN113060748A (en) * | 2021-04-15 | 2021-07-02 | 洛阳中超新材料股份有限公司 | Submicron boehmite and preparation method |
| CN113800543A (en) * | 2021-09-23 | 2021-12-17 | 大连理工大学 | Method for accelerating hydrothermal conversion rate of aluminum hydroxide into boehmite |
| CN114560482A (en) * | 2022-02-08 | 2022-05-31 | 中铝山东有限公司 | Pseudo-boehmite powder, forming carrier and preparation method thereof |
| CN114772615A (en) * | 2022-04-24 | 2022-07-22 | 郑州原发精细微粉材料技术有限公司 | Production method of heavy rhombohedral boehmite |
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