CN102381722A - 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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- CN102381722A CN102381722A CN2011102288081A CN201110228808A CN102381722A CN 102381722 A CN102381722 A CN 102381722A CN 2011102288081 A CN2011102288081 A CN 2011102288081A CN 201110228808 A CN201110228808 A CN 201110228808A CN 102381722 A CN102381722 A CN 102381722A
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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 method comprises 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 this method, particularly a kind of preparation method of activated alumina reaches the product by this 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 bigger 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, removal of fluorine from water agent, industrial sewage and antiodorant etc.The inner crystal formation of activated alumina ball 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 white lake (chemical formula Al (OH) 3) is placed in 450～800 ℃ the stoving oven, and shower roasting 2～6 seconds promptly 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 this method, the technical problem that solve is to improve the absorption property of existing general activated alumina and the porousness and the bigger serface of catalytic activity.
The technical scheme that the present invention adopted 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 process step of its preparation method is following:
1) it is subsequent use the white lake fast dewatering to be made general active oxidation aluminium powder;
2) in the crystal seed preparation vessel, pseudo-boehmite is processed slurries, and add aluminum nitrate therein, pH value transfers to 6-9, feeds steam and carries out the hydration activation 2 hours, and it is subsequent use to make crystal seed;
3) in the hydration reaction groove, general active oxidation aluminium powder is added in the hot pure water, stir and process general active oxidation aluminum slurry;
4), add in the described general active oxidation aluminum slurry of step 3 and and carry out heated and stirred this mixed solution with the crystal seed for preparing;
5) mixed solution to step 4 gained washs, filters 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 is added 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 carry out heated and stirred, and stirring velocity is 145 rev/mins, and mixeding liquid temperature is 60-90 ℃, keep 2-4 hour.
Described oven dry is in stoving oven, the filter cake of slaking is dried about 10～20 seconds of drying time under 300 ℃ environment.
Described health is health under field conditions (factors), 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 carried out activation 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%, gipsite≤3%.
The present invention and prior art are relatively; Owing to adopted in that general active oxidation aluminum slurry is mid-to go into alumina seed and hydration reaction takes place betwixt once more; Thereby generate new hydrated aluminum oxide; This new hydrated aluminum oxide is through process 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 gipsite, technology of the present invention is simple, easy to operate, with low cost, environment is not produced pollution.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed description:
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 preparing method's step is following:
1) make general active oxidation aluminium powder (being ρ-Al2O3 powder) for preparing the raw material of activated alumina of the present invention:
With technical grade white lake (Aluminium hydroxide), chemical formula Al (OH) 3 (is a kind of alkali; Owing to show certain acidity again, thus can be referred to as aluminic acid (H3AlO3) again, but actual what generate during with alkali reaction is meta-aluminate; Therefore regard it as a hydration meta-aluminic acid (HAlO2H2O) usually), place in the common stoving oven, in 300～400 ℃ of scopes; Through flash baking in 15～20 seconds, place Raymond mill (device name: 3R60), rotated 15 minutes again with 280 rev/mins speed; With the granularity of having dried is the white lake of 45 μ m, and being crushed to granularity is 5 μ m white lake fine powders.
With 5 μ m white lake fine powders, add homemade taking off soon in the stove with hopper from furnace roof, the high-temperature hot-air in the stove is blown into from the stove bottom; Make the white lake 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; With the general active oxidation aluminium powder that has dewatered, get in cyclone and the bagroom through riser tube, lay in general activated alumina filler bin for use again.
2) the general activated alumina crystal seed of preparation:
In crystal seed preparation vessel (homemade, material is that stainless steel, volume are 17m3), put into 8 tons of pure water, water temperature at 50～60 ℃, be preferably 55 ℃; 350～400kg pseudo-boehmite (Shanxi Aluminium Plant production) put into wherein process slurries, and to add concentration therein be that 100g/l, quality are the aluminum nitrate (crystal formation changing agent) of the 6-10% of pseudo-boehmite, and add proper amount of sodium hydroxide; PH value is transferred to 6-9, be preferably 8.5, feed steam and carry out hydration reaction (steam adds from the sidepiece of bottom land); The hydration reaction time is 2 hours; Make 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, process general active oxidation aluminum slurry and deposit.
With the described crystal seed that has 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 high more, the foreign matter content in the gained activated alumina is just low more.Usually, mass ratio is 40% o'clock, and the quality of the activated alumina of gained is best; Mass ratio is 30% o'clock, and 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, stirring velocity are 145 rev/mins, and churning time is 2-4 hour; Temperature rise rate is in 2 hours, rises to 60-90 ℃, is preferably 80 ℃.General activated alumina reacts with water under hydrothermal condition, because crystal seed is gathering of colloidal particle, has certain clearance, under the effect of crystal seed, generates a kind of new hydrated aluminum oxide, promptly has the activated alumina of certain macropore and many micropores.
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 through extruding.
5) filter cake slaking:
With described filter cake, place the ripening tank of making by stainless steel, feed 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, to dry, about 10～20 seconds of drying time through oven dry, places filler bin, packs when being cooled to 40～50 ℃, promptly 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 activation in the activation furnace again, hopper adds rod-shaped objects from the activation furnace top; 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 portion with induced draft fan, about 6 hours of soak time; Through 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 through crystal formation transform, hydration reaction, volumetric expansion, 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 mainly is used for doing catalyzer and carrier; The activated alumina of " SA " of the present invention powder (be called for short " SA " powder) mainly is used for making the raw material of the product of " SA " bar shaped and other shapes, also can be used for making the raw material of 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 following: 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%, gipsite≤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, processes general active oxidation aluminum slurry.
The 3rd step: crystal seed that makes and general active oxidation aluminum slurry (the crystal seed quality is about 32% with the ratio of general activated alumina opaque amount) 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, filter cake is placed ripening tank again through extruding; Make the interior temperature of ripening tank remain on 70～80 ℃, and to filter cake slaking 20 hours.
The 5th step: afterwards,, under 300 ℃ environment, dry with the filter cake of slaking; About 10～20 seconds of drying time through oven dry, places filler bin; Pack when being cooled to 40～50 ℃, promptly 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%, gipsite>=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%), 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%, gipsite≤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%), 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%, gipsite≤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%), 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%, gipsite≤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 the adding proper amount of sodium hydroxide, 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, processes general active oxidation aluminum slurry.
The 3rd step: with general activated alumina quality/crystal seed quality be 4 ratio (added crystal seed be general activated alumina 25%); With crystal seed that makes and general active oxidation aluminum slurry; Add in the hydration reaction groove and carry out hydration reaction; Temperature keeps 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, filter cake is placed ripening tank again through extruding; Make the interior temperature of ripening tank remain on 70～80 ℃, and to filter cake slaking 20 hours.
The 5th step:, under 300 ℃ environment, dry about 10～20 seconds of drying time with the filter cake of slaking; Through oven dry; Place filler bin, pack when being cooled to 40～50 ℃, promptly 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%, gipsite>=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%, gipsite≤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%, gipsite≤3%.
Claims (8)
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: said preparing method's step is following:
1) it is subsequent use the white lake fast dewatering to be made general active oxidation aluminium powder;
2) in the crystal seed preparation vessel, pseudo-boehmite is processed slurries, and add aluminum nitrate therein, pH value transfers to 6-9, feeds steam and carries out the hydration activation 2 hours, and it is subsequent use to make crystal seed;
3) in the hydration reaction groove, general active oxidation aluminium powder is added in the hot pure water, stir and process general active oxidation aluminum slurry;
4), add in the described general active oxidation aluminum slurry of step 3 and and carry out heated and stirred this mixed solution with the crystal seed for preparing;
5) mixed solution to step 4 gained washs, filters 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.
2. the preparation method of activated alumina according to claim 1, it is characterized in that: the aluminum nitrate concentration that is added is 100g/l, the amount of adding is the 6-10% of pseudo-boehmite quality.
3. the preparation method of activated alumina according to claim 1 is characterized in that: 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.
4. the preparation method of activated alumina according to claim 1; It is characterized in that: general active oxidation aluminium powder slurry and crystal seed mixed solution in the hydration reaction groove carry out heated and stirred; Stirring velocity is 145 rev/mins, and mixeding liquid temperature is 60-90 ℃, keeps 2-4 hour.
5. the preparation method of activated alumina according to claim 1, it is characterized in that: described oven dry is in stoving oven, the filter cake of slaking is dried about 10～20 seconds of drying time under 300 ℃ environment.
6. the preparation method of activated alumina according to claim 1, it is characterized in that: described health is health under field conditions (factors), and the envrionment temperature of health is not less than 20 ℃, and conditioned time is 10～15 hours.
7. the preparation method of activated alumina according to claim 1, it is characterized in that: described activation is in activation furnace, and the filter cake of slaking is carried out activation under 500 ℃ environment, soak time is 6 hours.
8. an activated alumina of making according to the said method of claim 1 is characterized in that: its specific surface area>=400m
2/ g, pore volume be at 0.4～0.6ml/g, igloss≤30%, Na
2O≤0.1%, gipsite≤3%.
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| CN103818938A (en) * | 2014-02-27 | 2014-05-28 | 昆明铂生金属材料加工有限公司 | Preparation method for modified alumina supporter with high thermal stability |
| CN104961146A (en) * | 2015-06-26 | 2015-10-07 | 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 |
| CN114599444A (en) * | 2019-08-26 | 2022-06-07 | 河北立车卓格新材料有限公司 | Solid material for purifying air and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103818939A (en) * | 2014-01-14 | 2014-05-28 | 淄博贝格工贸有限公司 | Aluminum oxide specially used for hydrogen peroxide fluidized bed and production technology for aluminum oxide |
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| CN114599444A (en) * | 2019-08-26 | 2022-06-07 | 河北立车卓格新材料有限公司 | Solid material for purifying air and preparation method and application thereof |
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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 |
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