CN105836770A - Preparation method of high-temperature-resistant boehmite - Google Patents
Preparation method of high-temperature-resistant boehmite Download PDFInfo
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- CN105836770A CN105836770A CN201610172756.3A CN201610172756A CN105836770A CN 105836770 A CN105836770 A CN 105836770A CN 201610172756 A CN201610172756 A CN 201610172756A CN 105836770 A CN105836770 A CN 105836770A
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- boehmite
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- temperature
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- 229910001593 boehmite Inorganic materials 0.000 title claims abstract description 68
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 31
- 238000005406 washing Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 229910001868 water Inorganic materials 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 31
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 30
- 150000001875 compounds Chemical class 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 17
- 239000002002 slurry Substances 0.000 claims description 15
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 13
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 12
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical group [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 9
- 239000001099 ammonium carbonate Substances 0.000 claims description 9
- 239000012498 ultrapure water Substances 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 8
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 claims description 8
- 229910001680 bayerite Inorganic materials 0.000 claims description 7
- 239000004411 aluminium Substances 0.000 claims description 5
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000001223 reverse osmosis Methods 0.000 claims description 4
- 238000004513 sizing Methods 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 abstract description 12
- 238000006297 dehydration reaction Methods 0.000 abstract description 12
- 239000013078 crystal Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 2
- 239000000654 additive Substances 0.000 abstract 1
- 230000000996 additive effect Effects 0.000 abstract 1
- -1 aluminum compound Chemical class 0.000 abstract 1
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 15
- 238000001816 cooling Methods 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000004575 stone Substances 0.000 description 4
- 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 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005201 scrubbing Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 238000004131 Bayer process Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000012776 electronic material Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 229910002706 AlOOH Inorganic materials 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910001648 diaspore Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000007701 flash-distillation Methods 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000004531 microgranule Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of high-temperature-resistant boehmite. The preparation method includes the steps of: slurrying an aluminum compound with water with addition of a crystal seeding agent and a washing additive, uniformly mixing the components and feeding the mixture into a high-pressure kettle, controlling the temperature increasing rate at 1-3 DEG C/min, and performing a reaction at 150-250 DEG C for 2-6 h, decreasing the temperature, and separating, washing and drying a product to obtain the high-temperature-resistant boehmite. The preparation method is simple and has high yield and low production cost. The boehmite is high in conversion rate, has concentrated particle distribution, is more than 350 DEG C in 1% dehydration temperature, has high chemical purity and is not more than 25 [mu]S/cm in electric conductivity.
Description
Technical field
The present invention relates to material and prepare synthesis technical field, be specifically related to the system of a kind of high temperature resistant boehmite
Preparation Method.
Background technology
Boehmite (Boehmite), also known as boehmite, boehmite etc., chemical formula is AlOOH
Or Al2O3·H2O, water insoluble, it is insoluble in soda acid, its powder body has using value widely.
The preparation method of boehmite, lot of domestic and international patent documentation all reported, such as, US
Boehmite described in 4797139 is that the method processed by seeding is formed, and is confined to boehmite
Microgranule adapts to be formed in the scope in alumina abrasive, has the ball shape being especially desired to so that it is fitted
For abrasive application；R Bauer discloses a kind of seeded boehmite in Publication No. CN 1942398A
Microparticle material and preparation method, it is indicated that provide boeh-mite precursor and boehmite seed with the form of suspension,
Precursor uses conventional ATH (Alumina hydrate), and crystal seed is pseudobochmite and acid-base modifier,
Then it is carried out heat treatment, so that boeh-mite precursor is converted into the boehmite particulate of various draw ratio；
Cai Weiquan etc. disclose the preparation side of a kind of micrometre grade thin diaspore in Publication No. CN 1733607A
Method, it is indicated that first use H2O2The sodium aluminate solution precipitating certain alumina concentration obtains boehmite crystal seed,
Then its sodium aluminate solution with certain alumina concentration is carried out kind point, plant point rate up to more than 50%；
Jiang Qi etc., in ZL 200710031164.0, disclose the preparation method of a kind of nano crystal boehmite,
I.e. with aluminum isopropylate. hydrolyzate as precursor, then obtain the nanometer of good dispersion by hydro-thermal reaction vigorous
Nurse stone；In CN 102249270A, the method disclosing a kind of dry process big particle diameter boehmite, first
First by aluminium hydroxide under uniform temperature and pressure, it is converted into boehmite, is then milled to certain particle diameter,
Carry out nano silicon cladding process finally by wet method, obtain low oil absorbency, be widely used in electricity
The product of sub-Material Field；CN 102815733A discloses a kind of nm boehmite and preparation method thereof,
The boehmite of the most certain component, inorganic acid/base, auxiliary agent, deionized water etc. stir, and enter height
Pressure still carries out hydro-thermal reaction, is washed out, is spray-dried the nm boehmite obtaining different-shape；CN
102092749A discloses the preparation method of a kind of boehmite, and i.e. using aluminium hydroxide is raw material, water
In heat treatment process, add the crystal seeds such as boehmite and control the granule-morphology of product, add sour or alkaline
Electrolyte reduces the sodium content of product, thus obtains boehmite and the aluminium oxide of a kind of ultralow sodium；CN
101830491A discloses the preparation method of a kind of high heat-resistant boehmite, first by aluminium hydroxide >=
It is converted into boehmite at 350 DEG C, is then ground to certain particle diameter, then use and carry out under wet method high-speed stirred
Nano surface coated with silica processes, and is dried to obtain low oil absorbency, high fluidity after edulcoration purification
Boehmite product.
To sum up, the preparation method of high temperature resistant boehmite, related data is little.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is provided that the preparation method of a kind of high temperature resistant boehmite.
For achieving the above object, the technical solution used in the present invention is:
The preparation method of a kind of high temperature resistant boehmite, starches aluminum contained compound with aquation, adds seed content
And washing assisant, load after mix homogeneously in autoclave, controlling programming rate is 1～3 DEG C/min,
At 150～250 DEG C, lower the temperature after reaction 2～6h, separated washing, dried, obtain high temperature resistant suddenly
Nurse stone.
Further, the mass ratio of described aluminum contained compound, seed content and washing assisant be 1:0.05～
0.5:0.005～0.1.
Further, described aluminum contained compound, including soda lime sintering process aluminium hydroxide, intend thin water aluminum
One or more in stone, ρ-aluminium oxide or bayerite.
Further, described water includes distilled water, high purity water, deionized water or reverse osmosis water.
Further, described aluminum contained compound is 1～10 with the serosity liquid-solid ratio of aquation slurry.
Further, described seed content, including in unformed aluminium glue, alumina sol or boehmite
One or more.
Further, the moisture content 0.1～95%wt of described seed content.
Further, described washing assisant is the carbonate of ammonium, makes the pH value of serosity control 7～13
Between.
Further, described baking temperature is 100～220 DEG C.
Further, reaction temperature is 180～210 DEG C, and programming rate is 1.5～3 DEG C/min, reaction
Time is 2～4h.
The preparation method of a kind of high temperature resistant boehmite that the present invention provides, the boehmite conversion rate obtained
Height, distribution of particles concentration, 1% dehydration temperaturre reaches more than 350 DEG C, and chemical purity is high, electrical conductivity≤
25μs/cm；And preparation method is simple, production capacity is big, and production cost is low, is widely used as preparing high-purity
Aluminium oxide, the field such as high performance catalyst and carrier, high effect nontoxic fire retardant and electronic material.
Detailed description of the invention
The embodiment of the present invention provides the preparation method of a kind of high temperature resistant boehmite, by aluminum contained compound and water
Slurrying, adds seed content and washing assisant, loads in autoclave, control programming rate after mix homogeneously
Be 1～3 DEG C/min, at 150～250 DEG C, reaction 2～6h after lower the temperature, separated washing, be dried
After, obtain high temperature resistant boehmite.
The mass ratio of described aluminum contained compound, seed content and washing assisant is 1:0.05～0.5:
0.005～0.1.The serosity liquid-solid ratio of described aluminum contained compound and aquation slurry is 1～10, preferably 1.5～
4.The moisture content 0.1～95%wt of described seed content, preferably 30～80%wt.
Described aluminum contained compound includes soda lime sintering process aluminium hydroxide, boehmite, ρ-aluminium oxide
Or/and bayerite, aluminum contained compound can be that one can also multiple be simultaneously introduced, and does not limit it and adds
Ratio.
Described seed content, including unformed aluminium glue, alumina sol and boehmite, seed content is permissible
It is that one can also multiple be simultaneously introduced, does not limit its additional proportion.
Described washing assisant, including one or more in the carbonate of the ammonium such as ammonium carbonate, ammonium hydrogen carbonate,
The pH value making serosity controls 7～13.
Described dry, the filter cake after separated washing is qualified, use baking oven, expansion drying or spraying
Being dried, baking temperature is 100～220 DEG C, preferably 150～210 DEG C.
The creativeness of the present invention is, uses soda lime sintering process aluminium hydroxide and the centre thereof of low cost
The aluminum contained compounds such as product are raw material, by adding seed content and washing assisant, can obtain high-purity
High heat-resistant boehmite (1% dehydration temperaturre reaches more than 350 DEG C).Wherein, seed content can effectively be controlled
The crystal morphology of boehmite processed and granularity and distribution, washing assisant is conducive to being converted into the sodium in raw material
Soluble sodium salt, it is easy to washing removes.The preparation method that the present invention provides is simple, and production capacity is big, produces
Low cost, this product is widely used as preparing high purity aluminium oxide, high performance catalyst and carrier, efficiently
The fields such as nontoxic fire retardant and electronic material.
Embodiment 1
The preparation method of a kind of high temperature resistant boehmite that the embodiment of the present invention 1 provides, specific as follows: to take
0.7kg soda lime sintering process aluminium hydroxide and 0.3kg ρ-aluminium oxide, by 2.5kg distilled water stirringization
Uniformly, aluminum contained compound is 2.5 with the serosity liquid-solid ratio of aquation slurry to slurry, add seed content 0.5kg without
Sizing aluminium glue (moisture content is 65%), and after 5g scrubbing with ammonium carbonate auxiliary agent, serosity pH is about 7.5,
Loading in autoclave, the speed controlling 1.5 DEG C/min rises to 180 DEG C, is incubated 2.5 hours.Cooling
Rear filtration separates, and with distilled water wash, is dried at 180 DEG C of baking oven.Product boehmite conversion rate is 98%,
1% dehydration temperaturre 381 DEG C, electrical conductivity 24 μ s/cm.
Embodiment 2
The preparation method of a kind of high temperature resistant boehmite that the embodiment of the present invention 2 provides, specific as follows: to take
0.5kg soda lime sintering process aluminium hydroxide and 0.5kg bayerite, stir slurrying with 1.5kg high purity water
Uniformly, aluminum contained compound is 1.5 with the serosity liquid-solid ratio of aquation slurry, adds the thin water of seed content 0.4kg
Aluminum stone (moisture content 50%), and after 50g scrubbing with ammonium carbonate auxiliary agent, serosity pH is about 11.5, loads
In autoclave, the speed controlling 1.5 DEG C/min rises to 190 DEG C, is incubated 2 hours.Filter after cooling
Separate, wash with high purity water, be dried at 150 DEG C of baking oven.Product boehmite conversion rate is 97.5%, 1%
Dehydration temperaturre 352 DEG C, electrical conductivity 20 μ s/cm.
Embodiment 3
The preparation method of a kind of high temperature resistant boehmite that the embodiment of the present invention 3 provides, specific as follows: to take
1.0kg bayerite, uniform by 2.5kg deionized water stirring slurrying, aluminum contained compound and aquation slurry
Serosity liquid-solid ratio is 2.5, adds seed content 0.25kg alumina sol (moisture content 80%) and 10g
After ammonium hydrogen carbonate washing assisant, serosity pH is about 8, loads in autoclave, controls 1.8 DEG C/min
Speed rises to 198 DEG C, is incubated 3 hours.Filter after cooling and separate, be washed with deionized, spraying
It is dried at 198 DEG C of exsiccator.Product boehmite conversion rate is 98.5%, 1% dehydration temperaturre 358 DEG C, electricity
Conductance 20 μ s/cm.
Embodiment 4
The preparation method of a kind of high temperature resistant boehmite that the embodiment of the present invention 4 provides, specific as follows: to take
1kg ρ-aluminium oxide, uniform by 2kg reverse osmosis water stirring slurrying, aluminum contained compound and the slurry of aquation slurry
Liquid-liquid-solid ratio is 2.0, adds seed content 0.75kg boehmite (moisture content is 0.5%), and 100g
After ammonium hydrogen carbonate washing assisant, serosity pH is about 13, loads in autoclave, controls 2.0 DEG C/min
Speed rise to 205 DEG C, be incubated 2 hours.Filter after cooling and separate, wash with reverse osmosis water, dodge
Steam and be dried at 220 DEG C of exsiccator.Product boehmite conversion rate is 97.8%, 1% dehydration temperaturre 365 DEG C,
Electrical conductivity 21 μ s/cm.
Embodiment 5
The preparation method of a kind of high temperature resistant boehmite that the embodiment of the present invention 5 provides, specific as follows: to take
0.6kg boehmite and 0.4kg soda lime sintering process aluminium hydroxide, by 4kg high purity water stirringization
Uniformly, aluminum contained compound is 4.0 with the serosity liquid-solid ratio of aquation slurry to slurry, adds seed content 1.65kg oxygen
Change Alumina gel (moisture content is 70%), and after 100g ammonium hydrogen carbonate washing assisant, serosity pH is about
13, load in autoclave, the speed controlling 2 DEG C/min rises to 205 DEG C, is incubated 3 hours.Cooling
Rear filtration separates, and washs with high purity water, is dried at spray dryer 190 DEG C.Product boehmite conversion
Rate is 98.5%, 1% dehydration temperaturre 358 DEG C, electrical conductivity 18 μ s/cm.
Embodiment 6
The preparation method of a kind of high temperature resistant boehmite that the embodiment of the present invention 6 provides, specific as follows: to take
0.6kg bayerite, 0.2kg ρ-aluminium oxide and 0.2kg soda lime sintering process aluminium hydroxide, use 3kg
Deionized water stirring slurrying is uniform, and aluminum contained compound is 3.0 with the serosity liquid-solid ratio of aquation slurry, adds
After the unformed aluminium glue of 0.5kg seed content (moisture content is 80%) and 70g scrubbing with ammonium carbonate auxiliary agent, serosity
PH is about 9, loads in autoclave, and the speed controlling 2.0 DEG C/min rises to 198 DEG C, and insulation 4 is little
Time.Filter after cooling and separate, be washed with deionized, be dried at flash distillation dryer 205 DEG C.Product
Boehmite conversion rate is 98.3%, 1% dehydration temperaturre 355 DEG C, electrical conductivity 15 μ s/cm.
Comparative example 1
The preparation method of a kind of high temperature resistant boehmite that comparative example 1 of the present invention provides, specific as follows:
Taking with 1kg Bayer process aluminium hydroxide, it is uniform to add 3kg high purity water stirring slurrying, aluminum contained compound with
The serosity liquid-solid ratio of aquation slurry is 3.0, loads in autoclave, and the speed controlling 3.5 DEG C/min rises to
190 DEG C, it is incubated 2 hours.Filter after cooling and separate, washing, it is dried at 120 DEG C.Product boehmite
Conversion ratio is 94.3%, 1% dehydration temperaturre 281 DEG C, electrical conductivity 215 μ s/cm.
Comparative example 2
The preparation method of a kind of high temperature resistant boehmite that comparative example 2 of the present invention provides, specific as follows:
Take with 1kg bayerite, add 4kg high purity water stirring slurrying uniformly, aluminum contained compound and aquation slurry
Serosity liquid-solid ratio is 4.0, loads in autoclave, and the speed controlling 3.5 DEG C/min rises to 200 DEG C,
It is incubated 3 hours.Filter separation, washing after cooling, be dried at 120 DEG C.Product boehmite conversion rate is
97.6%, 1% dehydration temperaturre 272 DEG C, electrical conductivity 198 μ s/cm.
Comparative example 3
The preparation method of a kind of high temperature resistant boehmite that comparative example 3 of the present invention provides, specific as follows:
Taking with 1kg Bayer process aluminium hydroxide, it is uniform to add 3kg high purity water stirring slurrying, aluminum contained compound with
The serosity liquid-solid ratio of aquation slurry is 3.0, adds 100g seed content boehmite, loads high pressure together
In still, the speed controlling 3.5 DEG C/min rises to 190 DEG C, is incubated 2 hours.Filter after cooling and separate,
Washing, is dried at 120 DEG C.Product boehmite conversion rate is 95.3%, 1% dehydration temperaturre 275 DEG C, electricity
Conductance 208 μ s/cm.
It should be noted last that, above detailed description of the invention only in order to technical scheme to be described and
Unrestricted, although the present invention being described in detail with reference to example, those of ordinary skill in the art
Should be appreciated that and technical scheme can be modified or equivalent, without deviating from this
The spirit and scope of inventive technique scheme, it all should be contained in the middle of scope of the presently claimed invention.
Claims (10)
1. the preparation method of a high temperature resistant boehmite, it is characterised in that: by aluminum contained compound and aquation
Slurry, adds seed content and washing assisant, loads in autoclave after mix homogeneously, controls programming rate and is
1～3 DEG C/min, at 150～250 DEG C, lower the temperature after reaction 2～6h, separated washing, dried,
Obtain high temperature resistant boehmite.
2. preparation method as claimed in claim 1, it is characterised in that: described aluminum contained compound, draw
The mass ratio of brilliant agent and washing assisant is 1:0.05～0.5:0.005～0.1.
3. preparation method as claimed in claim 1, it is characterised in that: described aluminum contained compound,
Including the one in soda lime sintering process aluminium hydroxide, boehmite, ρ-aluminium oxide or bayerite or
Multiple.
4. preparation method as claimed in claim 1, it is characterised in that: described water include distilled water,
High purity water, deionized water or reverse osmosis water.
5. preparation method as claimed in claim 1, it is characterised in that: described aluminum contained compound and water
The serosity liquid-solid ratio of slurrying is 1～10.
6. preparation method as claimed in claim 1, it is characterised in that: described seed content, including nothing
One or more in sizing aluminium glue, alumina sol or boehmite.
7. preparation method as claimed in claim 6, it is characterised in that: the moisture content of described seed content
0.1～95%wt.
8. preparation method as claimed in claim 1, it is characterised in that: described washing assisant is ammonium
Carbonate, makes the pH value of serosity control between 7～13.
9. preparation method as claimed in claim 1, it is characterised in that: described baking temperature be 100～
220℃。
10. preparation method as claimed in claim 1, it is characterised in that: reaction temperature is 180～210
DEG C, programming rate is 1.5～3 DEG C/min, and the response time is 2～4h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610172756.3A CN105836770B (en) | 2016-03-24 | 2016-03-24 | A kind of preparation method of high temperature resistant boehmite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610172756.3A CN105836770B (en) | 2016-03-24 | 2016-03-24 | A kind of preparation method of high temperature resistant boehmite |
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| Publication Number | Publication Date |
|---|---|
| CN105836770A true CN105836770A (en) | 2016-08-10 |
| CN105836770B CN105836770B (en) | 2017-11-21 |
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| 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 |
| 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 |
| CN112551563A (en) * | 2020-12-30 | 2021-03-26 | 宣城晶瑞新材料有限公司 | Preparation method of boehmite liquid |
| CN113479919A (en) * | 2021-08-24 | 2021-10-08 | 安徽壹石通材料科技股份有限公司 | Low-conductivity boehmite and preparation method thereof |
| CN113860340A (en) * | 2021-10-28 | 2021-12-31 | 中化学科学技术研究有限公司 | Method for preparing high-purity granular boehmite by dry method and boehmite |
| CN113860342A (en) * | 2021-11-05 | 2021-12-31 | 中化学科学技术研究有限公司 | Method for preparing high-purity parallelepipedal boehmite and high-purity parallelepipedal boehmite |
| CN113860341A (en) * | 2021-10-28 | 2021-12-31 | 中化学科学技术研究有限公司 | High-purity flaky boehmite and preparation method thereof |
| CN113955779A (en) * | 2021-11-05 | 2022-01-21 | 中化学科学技术研究有限公司 | Method for preparing high-purity boehmite by dry method and high-purity 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 |
| CN115245798A (en) * | 2022-07-20 | 2022-10-28 | 山东大学 | Gamma-AlOOH sol and preparation method and application thereof |
| CN115353133A (en) * | 2022-09-02 | 2022-11-18 | 宁波大浦新材料科技有限公司 | Preparation method of high-purity boehmite |
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| 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 |
| 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 |
| CN112551563A (en) * | 2020-12-30 | 2021-03-26 | 宣城晶瑞新材料有限公司 | Preparation method of boehmite liquid |
| CN112551563B (en) * | 2020-12-30 | 2024-02-02 | 宣城晶瑞新材料有限公司 | Preparation method of boehmite liquid |
| CN113479919A (en) * | 2021-08-24 | 2021-10-08 | 安徽壹石通材料科技股份有限公司 | Low-conductivity boehmite and preparation method thereof |
| CN113860341A (en) * | 2021-10-28 | 2021-12-31 | 中化学科学技术研究有限公司 | High-purity flaky boehmite and preparation method thereof |
| CN113860340B (en) * | 2021-10-28 | 2023-10-27 | 中化学科学技术研究有限公司 | Method for preparing high-purity granular boehmite by dry method and boehmite |
| CN113860341B (en) * | 2021-10-28 | 2023-10-27 | 中化学科学技术研究有限公司 | High-purity platy boehmite and preparation method thereof |
| CN113860340A (en) * | 2021-10-28 | 2021-12-31 | 中化学科学技术研究有限公司 | Method for preparing high-purity granular boehmite by dry method and boehmite |
| CN113860342A (en) * | 2021-11-05 | 2021-12-31 | 中化学科学技术研究有限公司 | Method for preparing high-purity parallelepipedal boehmite and high-purity parallelepipedal boehmite |
| CN113955779A (en) * | 2021-11-05 | 2022-01-21 | 中化学科学技术研究有限公司 | Method for preparing high-purity boehmite by dry method and high-purity boehmite |
| CN113860342B (en) * | 2021-11-05 | 2023-08-08 | 中化学科学技术研究有限公司 | Method for preparing high-purity parallelepiped boehmite and high-purity parallelepiped boehmite |
| CN113955779B (en) * | 2021-11-05 | 2023-10-27 | 中化学科学技术研究有限公司 | Method for preparing high-purity boehmite by dry method and high-purity 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 |
| CN115245798A (en) * | 2022-07-20 | 2022-10-28 | 山东大学 | Gamma-AlOOH sol and preparation method and application thereof |
| CN115353133A (en) * | 2022-09-02 | 2022-11-18 | 宁波大浦新材料科技有限公司 | Preparation method of high-purity boehmite |
| CN115353133B (en) * | 2022-09-02 | 2023-12-26 | 宁波大浦新材料科技有限公司 | Preparation method of high-purity boehmite |
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