CN102381722B - Preparation method of activated aluminum oxide and product prepared by using same - Google Patents
Preparation method of activated aluminum oxide and product prepared by using same Download PDFInfo
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- CN102381722B CN102381722B CN 201110228808 CN201110228808A CN102381722B CN 102381722 B CN102381722 B CN 102381722B CN 201110228808 CN201110228808 CN 201110228808 CN 201110228808 A CN201110228808 A CN 201110228808A CN 102381722 B CN102381722 B CN 102381722B
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000013078 crystal Substances 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 39
- 238000006703 hydration reaction Methods 0.000 claims abstract description 27
- 239000002002 slurry Substances 0.000 claims abstract description 21
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000011148 porous material Substances 0.000 claims abstract description 14
- 229910001679 gibbsite Inorganic materials 0.000 claims abstract description 12
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 11
- 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 abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 38
- 229910052782 aluminium Inorganic materials 0.000 claims description 38
- 230000003647 oxidation Effects 0.000 claims description 31
- 238000007254 oxidation reaction Methods 0.000 claims description 31
- 239000004411 aluminium Substances 0.000 claims description 24
- 239000012065 filter cake Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000011734 sodium Substances 0.000 claims description 12
- 230000004913 activation Effects 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 230000036541 health Effects 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 5
- 230000001143 conditioned effect Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 14
- 239000000126 substance Substances 0.000 description 13
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 8
- 230000005070 ripening Effects 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 239000002594 sorbent Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 241000190022 Pilea cadierei Species 0.000 description 1
- 108010016634 Seed Storage Proteins Proteins 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000004682 monohydrates Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- -1 siccative Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of activated aluminum oxide and the activated aluminum oxide prepared by using the method, aiming to solve the technical problem on increasing the porosity and the large specific surface area of the traditional general activated aluminum oxide on the aspects of adsorptivity and catalytic activity. In the technical scheme disclosed by the invention, a seed crystal is prepared by using pseudo-boehmite, and then undergoes hydration reaction with general activated aluminum oxide powder to prepare the activated aluminum oxide; and the preparation methodcomprises the main steps of: rapidly dehydrating aluminum hydroxide to prepare the general activated aluminum oxide powder, adding aluminum nitrate into pseudo-boehmite slurry to prepare the seed crystal, then adding the prepared general activated aluminum oxide powder and the seed crystal into a hydration reaction tank for hydration reaction, and finally preparing the activated aluminum oxide powder with the specific surface area being not smaller than 400m<2>/g, the pore vloume of 0.4-0.6ml/g, the igloss being not more than 30%, Na2O being not more than 0.1%, and gibbsite being not more than 3%. The preparation method disclosed by the invention has the advantages of simple process, convenience for operation, low cost and no environment pollution.
Description
Technical field
The present invention relates to a kind of preparation method of aluminum oxide and the product that is prepared by the method, particularly a kind of preparation method of activated alumina reaches the product by the method preparation.
Background technology
Activated alumina (molecular formula Al2O (3-x) is 2x (OH), 0＜x＜0.8) is one of a large amount of inorganic chemical products that use on the our times.Because activated alumina has vesicular structure, high-specific surface area and be in unsettled transition state, thereby have larger activity.In petrochemical complex, chemical fertilizer industry, be widely used as catalyzer, support of the catalyst.Activated alumina has porousness, high degree of dispersion, the bigger serface of absorption property, catalytic activity, thereby as the color of the sorbent material of the siccative of gas and liquid, gas sweetening, Reducing Fluoride Materials In Drinkeng Water, industrial sewage and antiodorant etc.The crystal formation of activated alumina ball inside is γ type and χ-ρ type, can be divided into activated alumina ball sorbent material, activated alumina ball siccative and activated alumina sphere catalyst carrier by its purposes.
In " Shandong Aluminium Industrial Corp's company standard " of Shandong Aluminium Industrial Corp's issue on February 1st, 2000, the physical and chemical index of general activated alumina: specific surface area is 200～350m
2/ g, pore volume are 0.3～0.45ml/g, igloss≤7%, Na
2O≤0.45%.Usually, its making method is that aluminium hydroxide (chemical formula Al (OH) 3) is placed in 450～800 ℃ the stoving oven, and shower roasting 2～6 seconds namely obtains general activated alumina (ρ-AL2O3).
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of activated alumina and the activated alumina that is obtained by the method, the technical problem that solve is to improve the absorption property of existing general activated alumina and porousness and the bigger serface of catalytic activity.
The technical solution adopted in the present invention is:
The preparation method of activated alumina of the present invention makes crystal seed by pseudo-boehmite, carries out hydration reaction with general active oxidation aluminium powder again and makes activated alumina, and the processing step of its preparation method is as follows:
1) the aluminium hydroxide fast dewatering is made general active oxidation aluminium powder for subsequent use;
2) in the crystal seed preparation vessel, pseudo-boehmite is made slurries, and add aluminum nitrate therein, the pH value transfers to 6-9, passes into steam and carries out Hydration Activation 2 hours, makes crystal seed for subsequent use;
3) in the hydration reaction groove, general active oxidation aluminium powder is added in the hot pure water, stir and make general active oxidation aluminum slurry;
4) with the crystal seed for preparing, add in the described general active oxidation aluminum slurry of step 3 and to this mixed solution and carry out heated and stirred;
5) mixed solution of step 4 gained washed, filtered and be pressed into filter cake;
6) below 100 ℃ filter cake is being carried out slaking;
7) filter cake of slaking is dried or health, activation.
The aluminum nitrate concentration that adds is 100g/l, and the amount of adding is the 6-10% of pseudo-boehmite quality.
In the hydration reaction groove, the crystal seed quality is the 25%-40% of general activated alumina opaque amount in the general active oxidation aluminum slurry.
General active oxidation aluminium powder slurry and crystal seed mixed solution in the hydration reaction groove are carried out heated and stirred, and stirring velocity is 145 rev/mins, and mixeding liquid temperature is 60-90 ℃, keeps 2-4 hour.
Described oven dry is in stoving oven, the filter cake of slaking is dried drying time approximately 10～20 seconds under 300 ℃ environment.
Described health is under field conditions (factors) health, and the envrionment temperature of health is not less than 20 ℃, and conditioned time is 10～15 hours.
Described activation is in activation furnace, and the filter cake of slaking is activated under 500 ℃ environment, and soak time is 6 hours.
The activated alumina that makes according to above-mentioned preparation method of the present invention, its specific surface area 〉=400m
2/ g, pore volume be at 0.4～0.6ml/g, igloss≤30%, Na
2O≤0.1%, gibbsite≤3%.
The present invention compared with the prior art, owing to having adopted general active oxidation aluminum slurry is mid-to enter alumina seed and hydration reaction occurs betwixt again, thereby generate new hydrated aluminum oxide, this new hydrated aluminum oxide is through processing steps such as press filtration washing, slaking, health, activation, finally make have high absorption property, the activated alumina of large pore volume that catalytic activity is stronger, bigger serface, low gibbsite, technique of the present invention is simple, easy to operate, with low cost, environment is not produced pollution.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples:
As shown in Figure 1, the preparation method of activated alumina of the present invention is to make crystal seed by pseudo-boehmite (having another name called monohydrate alumina, molecular formula Al2O3H2O), carry out hydration reaction with general active oxidation aluminium powder again and make activated alumina, this preparation method's step is as follows:
1) make general active oxidation aluminium powder (be ρ--Al2O3 powder, for preparing the raw material of activated alumina of the present invention):
With technical grade aluminium hydroxide (Aluminium hydroxide), chemical formula Al (OH) 3, (be a kind of alkali, owing to showing again certain acidity, so can be referred to as again aluminic acid (H3AlO3), but what generate when actual and alkali reaction is meta-aluminate, therefore usually it is regarded as a hydration meta-aluminic acid (HAlO2H2O)), place in the common stoving oven, in 300～400 ℃ of scopes, through flash baking in 15～20 seconds, place again Raymond mill (device name: 3R60) with 280 rev/mins speed, rotating 15 minutes, is the aluminium hydroxide of 45 μ m with the granularity of having dried, and being crushed to granularity is 5 μ m aluminium hydroxide fine powders.
With 5 μ m aluminium hydroxide fine powders, take off soon in the stove with hopper from the furnace roof adding is homemade, high-temperature hot-air in the stove is blown into from the stove bottom, make the aluminium hydroxide powder and fine powder be in boiling state, in 600～800 ℃ of scopes, the quick roasting dehydration through 2～6 seconds, make general active oxidation aluminium powder, general active oxidation aluminium powder with having dewatered enters in cyclone and the bagroom through riser tube, lays in general activated alumina filler bin stand-by again.
2) the general activated alumina crystal seed of preparation:
(homemade at the crystal seed preparation vessel, material is stainless steel, volume is 17m3) in, put into 8 tons of pure water, water temperature is at 50～60 ℃, be preferably 55 ℃, 350～400kg pseudo-boehmite (Shanxi Aluminium Plant production) put into wherein make slurries, and to add therein concentration be 100g/l, quality is the aluminum nitrate (crystal formation changing agent) of the 6-10% of pseudo-boehmite, and add an amount of sodium hydroxide, the pH value is transferred to 6-9, be preferably 8.5, pass into steam and carry out hydration reaction (steam adds from the sidepiece of bottom land), the hydration reaction time is 2 hours, makes crystal seed, through the press filtration washing, remove the NO in the crystal seed again
3 -And Na
+After, crystal seed deposited in the crystal seed storage tank preserve.
3) preparation active oxidation aluminum slurry:
In hydration reaction groove (homemade, material is that stainless steel, volume are 17m3), put into 12m
3Hot pure water, water temperature transfer to 70～80 ℃, are preferably 75 ℃, with the described general active oxidation aluminium powder of 1000～1200kg, add in the groove, stir 2 hours with 145 rev/mins speed again, make general active oxidation aluminum slurry and deposit.
With the described crystal seed that prepared [ratio that adds crystal seed quality and general activated alumina opaque amount in the hydration reaction groove is: 25%≤mass ratio≤40%, its mass ratio is higher, the foreign matter content in the gained activated alumina is just lower.Usually, when mass ratio was 40%, the quality of the activated alumina of gained was best, when mass ratio is 30%, the integrated quality of the activated alumina of gained is (cost is lower) better], concentrated adding is deposited in the general active oxidation aluminum slurry in the hydration reaction groove, warming while stirring, and stirring velocity is 145 rev/mins, churning time is 2-4 hour, temperature rise rate is in 2 hours, rises to 60-90 ℃, is preferably 80 ℃.General activated alumina is given birth to reaction with steeping in water for reconstitution under hydrothermal condition, because crystal seed is gathering of colloidal particle, have certain gap, under the effect of crystal seed, generates a kind of new hydrated aluminum oxide, namely has certain macropore and is permitted microporous activated alumina.
4) press filtration washing:
The slurry that will contain new hydrated aluminum oxide is squeezed into filter press with the slag stock pump, carry out reverse 3 times the washing after, obtain filter cake by extruding.
5) filter cake slaking:
With described filter cake, place the ripening tank of being made by stainless steel, pass into steam, make that temperature remains on 70～80 ℃ in the ripening tank, and filter cake was carried out slaking 20 hours, thereby the crystal formation of described new hydrated aluminum oxide filter cake is transformed fully and keep stable.
6) acquisition of active oxidation aluminium powder:
With the filter cake of slaking, under 300 ℃ environment, dry, drying time approximately 10～20 seconds, drying places filler bin, packs when being cooled to 40～50 ℃, namely obtains active oxidation aluminium powder of the present invention, i.e. " SA " powder product.
7) acquisition of activated alumina end product:
With the filter cake of slaking, after banded extruder is made rod-shaped objects, put into frame of plastic, carry out natural Health preservation with the plastic cloth sealing, the envrionment temperature of health must not be lower than 20 ℃, and conditioned time is 10～15 hours; Afterwards, insert in the activation furnace again and activate, rod-shaped objects adds from activation furnace top hopper, its state in stove is top-down flowing, and heating duct is 2/3 (being added with sleeve pipe) in stove is inserted at the activation furnace top outside the heating duct, and hot blast is blown in the stove from the pipe end opening, hot blast temperature is 550 ℃, temperature remains 500 ℃ of degree in the stove, and the hot and humid gas in the stove is discharged from furnace roof section with induced draft fan, soak time approximately 6 hours; By activation, make the moisture evaporation in the rod-shaped objects, the formation micropore is also gained in strength, thereby obtains activated alumina end product of the present invention, i.e. " SA " rod-shaped objects.
(be called for short " SA "-English full name: Swell aluminum means the oxide molecule of dilated aluminium to end product of the present invention " SA " rod-shaped objects.In other words, the oxide molecule of aluminium is through transformation of crystal, hydration reaction, and volumetric expansion has become a kind of macropore, porous, high-specific surface area, highly active molecular structure.Simultaneously, the symbol of element of aluminium is " Al ", generally all uses " A " expression aluminium), be white in color, nontoxic, odorless, be the strip porous material, not efflorescence, water insoluble is mainly used to do catalyzer and carrier;
The activated alumina of " SA " of the present invention powder (being called for short " SA " powder) is mainly used to the raw material of the product of making " SA " bar shaped and other shapes, also can be used for making the raw material of the deep processed products such as other catalyzer, support of the catalyst, siccative, sorbent material, detoxifying agent.
(molecular formula: Al2O3nH2O) physico-chemical parameter of powder is as follows: specific surface area 〉=400m for activated alumina of the present invention
2/ g, pore volume be at 0.4～0.6ml/g, igloss≤30%, Na
2O≤0.1%, gibbsite≤3%.
Embodiment 1
The first step: preparation crystal seed:
Put into the crystal seed preparation vessel, make crystal seed.
Second step: get general active oxidation aluminium powder 1100kg and 12 tons of pure water, put into the hydration reaction groove, water temperature is controlled at 75 degree, stirs 2 hours with 145 rev/mins speed, makes general active oxidation aluminum slurry.
The 3rd step: the crystal seed and the general active oxidation aluminum slurry (the crystal seed quality is about 32% with the ratio of general activated alumina opaque amount) that make are added in the hydration reaction groove, and temperature rises to 80 degree, with 145 rev/mins speed, stirs 4 hours.
The 4th step: afterwards, will contain the slurry of new hydrated aluminum oxide, and squeeze into filter press with the slag stock pump, after carrying out reverse 3 washings, obtain filter cake by extruding, filter cake is placed ripening tank again, make the interior temperature of ripening tank remain on 70～80 ℃, and to filter cake slaking 20 hours.
The 5th step: afterwards, with the filter cake of slaking, under 300 ℃ environment, dry, drying time approximately 10～20 seconds, drying places filler bin, pack when being cooled to 40～50 ℃, namely obtain active oxidation aluminium powder of the present invention, be i.e. " SA " powder product.Its physico-chemical parameter is: 350m
2/ g≤specific surface area≤400m
2/ g, pore volume 0.38～0.46ml/g, igloss≤25%, Na
2O≤0.1%, gibbsite 〉=9%.
Embodiment 2
Repeat embodiment 1 by described same steps as, but the institute add aluminum nitrate (concentration is 100g/l), increase to 21kg (for pseudo-boehmite 6%), the pH value transfers to 7, the physico-chemical parameter of gained " SA " powder product is: specific surface area 〉=450m
2/ g, pore volume 0.45～0.58ml/g, igloss≤30%, Na
2O≤0.1%, gibbsite≤3%.
Embodiment 3
Repeat embodiment 1 by described same steps as, but the institute add aluminum nitrate (concentration is 100g/l), increase to 28kg (for pseudo-boehmite 8%), the pH value transfers to 8.5,, the physico-chemical parameter of gained " SA " powder product is: specific surface area 〉=450m
2/ g, pore volume 0.46～0.6ml/g, igloss≤30%, Na
2O≤0.1%, gibbsite≤3%.
Embodiment 4
Repeat embodiment 1 by described same steps as, but the institute add aluminum nitrate (concentration is 100g/l), increase to 35kg (for pseudo-boehmite 10%), the pH value transfers to 9, the physico-chemical parameter of gained " SA " powder product is: specific surface area 〉=450m
2/ g, pore volume 0.45～0.55ml/g, igloss≤30%, Na
2O≤0.12%, gibbsite≤3%.
Embodiment 5
The first step: preparation crystal seed:
Get pseudo-boehmite 350kg and 8 tons of pure water, put into the crystal seed preparation vessel, water temperature is controlled at 55 degree, and add therein concentration be 100g/l, quality be 21kg aluminum nitrate (for pseudo-boehmite 6%), and add an amount of sodium hydroxide, and the pH value is transferred to 8, be preferably 8.5, hydration reaction 2 hours makes crystal seed.
Second step: get general active oxidation aluminium powder 1100kg and 12 tons of pure water, put into the hydration reaction groove, water temperature is controlled at 75 degree, stirs 2 hours with 145 rev/mins speed, makes general active oxidation aluminum slurry.
The 3rd step: take the ratio of general activated alumina quality/crystal seed quality as 4 (added crystal seed as general activated alumina 25%), with crystal seed and the general active oxidation aluminum slurry that makes, add in the hydration reaction groove and carry out hydration reaction, temperature keeps 80 degree, with 145 rev/mins speed, stirred 4 hours.
The 4th step: afterwards, will contain the slurry of new hydrated aluminum oxide, and squeeze into filter press with the slag stock pump, after carrying out reverse 3 washings, obtain filter cake by extruding, filter cake is placed ripening tank again, make the interior temperature of ripening tank remain on 70～80 ℃, and to filter cake slaking 20 hours.
The 5th step: with the filter cake of slaking, under 300 ℃ environment, dry, drying time approximately 10～20 seconds, drying, place filler bin, pack when being cooled to 40～50 ℃, namely obtain active oxidation aluminium powder of the present invention, i.e. " SA " powder product, its physico-chemical parameter is: specific surface area 〉=400m
2/ g, pore volume 0.35～0.55ml/g, igloss≤30%, Na
2O≤0.1%, gibbsite 〉=4%.
Embodiment 6
Repeat embodiment 5 by described same steps as, but in the 3rd step, general activated alumina quality/crystal seed quality reduce to 3 ratio (add crystal seed be general activated alumina 33%), the physico-chemical parameter of gained " SA " powder product is: specific surface area 〉=430m
2/ g, pore volume 0.45～0.6ml/g, igloss≤30%, Na
2O≤0.1%, gibbsite≤3%.
Embodiment 7
Repeat embodiment 5 by described same steps as, but in the 3rd step, general activated alumina quality/crystal seed quality reduce to 2.5 ratio (add crystal seed be general activated alumina 40%), the physico-chemical parameter of gained " SA " powder product is: specific surface area 〉=450m
2/ g, pore volume 0.46～0.6ml/g, igloss≤30%, Na
2O≤0.1%, gibbsite≤3%.
Claims (2)
1. the preparation method of an activated alumina makes crystal seed by pseudo-boehmite, carries out hydration reaction with general active oxidation aluminium powder again and makes activated alumina, and it is characterized in that: described preparation method's step is as follows:
1) with technical grade aluminium hydroxide under 300～400 ℃, through 15～20 seconds the oven dry, being crushed to granularity is 5 μ m aluminium hydroxide fine powders again, places under 600～800 ℃, fast dewatering made general active oxidation aluminium powder for subsequent use after 2～6 seconds;
2) in the crystal seed preparation vessel, put into pure water, water temperature at 50～60 ℃, pseudo-boehmite put into wherein make slurries, and to add therein concentration be that 100g/l, quality are the aluminum nitrate of the 6-10% of pseudo-boehmite, and add an amount of sodium hydroxide, the pH value is transferred to 6-9, pass into steam and carried out hydration reaction 2 hours, make crystal seed for subsequent use;
3) in the hydration reaction groove, general active oxidation aluminium powder is added temperature in 70～80 ℃ hot pure water, stir and made general active oxidation aluminum slurry in 2 hours;
4) with the crystal seed for preparing, take the mass ratio of crystal seed quality and the general activated alumina opaque amount step 3 as 40%) described in general active oxidation aluminum slurry be put in the hydration reaction groove, take stirring velocity as 145 rev/mins, churning time is 2-4 hour, temperature rise rate is in 2 hours, rise to 60-90 ℃, generate the mixed solution that has certain macropore and permitted microporous activated alumina;
5) to step 4) mixed solution of gained washs, filter and be pressed into filter cake;
6) below 100 ℃ filter cake is being carried out slaking;
7) to the filter cake of slaking dry, health, activation, bake out temperature is under 300 ℃ the environment, drying time approximately 10～20 seconds; Be not less than in 20 ℃ of situations in envrionment temperature, conditioned time is 10～15 hours; Activation is 6 hours under 500 ℃.
2. preparation method according to claim 1, it is characterized in that: the parameter of prepared activated alumina is that specific surface area is 450m
2/ g, pore volume 0.45～0.58ml/g, igloss≤30%, Na
2O≤0.1%, gibbsite≤3%.
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| CN103818939B (en) * | 2014-01-14 | 2016-06-08 | 杜云峰 | Hydrogen peroxide fluid bed special aluminium oxide and production technology |
| CN103818938B (en) * | 2014-02-27 | 2016-05-04 | 昆明铂生金属材料加工有限公司 | A kind of preparation method of high thermal stability modified aluminium oxide supports |
| CN104961146B (en) * | 2015-06-26 | 2017-04-12 | 吉林大学 | Nanometer sheet aluminum hydroxide gel and preparation method thereof |
| CN109485079A (en) * | 2018-12-27 | 2019-03-19 | 中国铝业股份有限公司 | A kind of method of lithium content in reduction alumina product |
| CN110508128A (en) | 2019-08-26 | 2019-11-29 | 李迎九 | A kind of preparation and application of solid air scavenging material |
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| CN1434745A (en) * | 1999-12-21 | 2003-08-06 | 格雷斯公司 | Alumina trihydrated derived high pore volume, high surface area aluminum oxide composites and methods of their preparation and use |
| CN1506163A (en) * | 2002-12-06 | 2004-06-23 | 石油大学(北京) | Alumina carrier and hydrogenation catalyst obtained by using the carrier |
| CN102070169A (en) * | 2010-12-15 | 2011-05-25 | 中国铝业股份有限公司 | Preparation method of low-sodium active aluminum oxide |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1434745A (en) * | 1999-12-21 | 2003-08-06 | 格雷斯公司 | Alumina trihydrated derived high pore volume, high surface area aluminum oxide composites and methods of their preparation and use |
| CN1506163A (en) * | 2002-12-06 | 2004-06-23 | 石油大学(北京) | Alumina carrier and hydrogenation catalyst obtained by using the carrier |
| CN102070169A (en) * | 2010-12-15 | 2011-05-25 | 中国铝业股份有限公司 | Preparation method of low-sodium active aluminum oxide |
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| Title |
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| 生产活性氧化铝的原料和技术条件;黄德修等;《轻金属》;19991231(第2期);全文 * |
| 黄德修等.生产活性氧化铝的原料和技术条件.《轻金属》.1999,(第2期),全文. |
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Effective date of registration: 20180629 Address after: 043300 opposite the gas section of the north section of No. nine road, Shanxi aluminum plant, Hejin, Shanxi. Patentee after: Hejin torch Aluminium Industry Co., Ltd. Address before: 043300 2 3 gates 4 in the Southern District of Hejin, Shanxi. Patentee before: Guo Wanli |