CN1307929A - Preparation process of alumina adsorbant - Google Patents
Preparation process of alumina adsorbant Download PDFInfo
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- CN1307929A CN1307929A CN 00136212 CN00136212A CN1307929A CN 1307929 A CN1307929 A CN 1307929A CN 00136212 CN00136212 CN 00136212 CN 00136212 A CN00136212 A CN 00136212A CN 1307929 A CN1307929 A CN 1307929A
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Abstract
The present invention relates to a preparation method of adsorbing agent, and is characterized by active aluminium hydroxide is used as raw material, and through the processes of drying and pulverizing to a certain mesh quickly dehydrating through the high-temp. air flow to obtain active aluminium oxide raw powder, placing the obtained raw powder in disk type pelletizer, and spraying aqueous solution of alkaline earth metal compound, rolling, forming and roasting so as to obtain finished product. Said product possesses higher adsorptivity, pore volume and specific surface area and crushing strength, and can obviously raise catalytic activity.
Description
The present invention relates to catalyst, adsorbent manufacturing technology field, exactly prepare the method for adsorbent for a kind of activated alumina load alkali (soil) components of metal compounds.
The present invention's technology in the past, the manufacturing of activated alumina generally have acid-base neutralization method, rapid dehydration method, aluminium alcoholates method etc.The activated alumina that is used in adsorbing domain is generally by rapid dehydration method production, and promptly aluminium hydroxide makes the active oxidation aluminium powder of porous through the high temperature gas flow fast dewatering, makes finished product through moulding, calcining again, the invention belongs to the expansion of this technology.
The present invention is directed to the problem of commercially available activated alumina in some absorption and catalytic field existence, a kind of preparation method of the activated alumina that contains alkali (soil) metallic compound of novelty is provided, product by this method preparation has higher adsorption capacity, pore volume and specific area and crushing strength, can significantly improve catalytic activity.
The present invention realizes in the following manner: be raw material with aluminium hydroxide, drying, be crushed to certain order number, in high temperature gas flow through fast dewatering, make the former powder of activated alumina, former powder is placed in the dribbling balling machine, sprays into the aqueous solution of alkali (soil) metallic compound, the rolling moulding, through calcining, get finished product again.
The technical process of preparation is:
(1) the aluminium hydrate powder bake out temperature is at 100 ℃-140 ℃, and is crushed to below 300 orders.
(2) in the high temperature gas flow with 380 ℃-1000 ℃ of aluminium hydroxide fine powder addings,, make the active oxidation aluminium powder of porous through instantaneous fast dewatering.
(3) aqueous solution of preparation alkali or strong base-weak acid salt is made adhesive, and control pH value is in the 11-14 scope.
(4) the active oxidation aluminium powder is put into dribbling balling machine, spray into the adhesive of above-mentioned (3) preparation, the rolling moulding.
(5) will become the semi-finished product of type to handle 3-16 hour down at 30 ℃-120 ℃, the calcining furnace of packing into was calcined 1-4 hour down at 300 ℃-450 ℃, made product of the present invention.
Aluminium hydroxide can adopt β-gibbsite, α-gibbsite or boehmite in above-mentioned (1), preferably adopts β-gibbsite or α-gibbsite.
In above-mentioned (2), when thin aluminium hydrate powder dewatered in thermal current, the time of staying was 0.1-5 second, and dehydration temperaturre is preferably in 380 ℃-9 00 ℃ at 300 ℃-1000 ℃.
In above-mentioned (3), alkali (soil) metallic compound calcining back exists with the metal oxide form on aluminium oxide.Concentration range is between 0.5-15%, and pH value scope is preferably between the 12-13.7.This aqueous solution can be one or more mixture.
In above-mentioned (5), the time of calcining generally between 0.5-4 hour, is preferably in 40 minutes to 2 hours.The temperature of calcining is preferably between 380 ℃-420 ℃.
The catalyst of the present invention's preparation has following performance:
Compressive resistance: 〉=60N/cm; Specific area: 〉=280m
2/ g;
Bulk specific weight: 0.6-0.9g/ml; Pore volume: 〉=0.40ml/g;
Burning decrement (1000 ℃, 2h): 3-9%, w/w;
Characteristic of the present invention is:
1. prepare certain density alkali (soil) metal compound solution, control pH value is between 12.7-13.5.
2. Pei Zhi the aqueous solution can be the solution that simple aqueous slkali, strong base weak acid salting liquid or aqueous slkali neutralizes with acid, it also can be the mixture of several solns, as sodium hydroxide solution, potassium hydroxide solution, magnesium hydroxide solution, aqua calcis, lithium hydroxide solution, sodium carbonate liquor, sodium acetate solution, sodium formate solution, or the solution that neutralizes with acid as nitric acid, carbon dioxide, organic acid of NaOH, potassium hydroxide solution.
3. alkali (soil) metallic compound is with aqueous solution form, and spraying adds during the rolling moulding in dribbling balling machine.
4. to have intensity good for the activated alumina of the present invention preparation, and pore volume, specific area increase, and simultaneously, adsorption capacity is significantly increased.
5. the product of the present invention's preparation is specially adapted to gas or the adsorbing and removing of other acidic materials and the regenerated catalysts of anthraquinone preparation hydrogen peroxide industry degradation product such as hydrogen chloride in the petro chemical industry, carbon dioxide, hydrogen sulfide.
That activated alumina production technology of the present invention has is simple to operate, product strength good, pore volume and specific area are big, characteristics such as result of use is good.
Embodiment 1
Do raw material with commercially available α-gibbsite, 120 ℃ of oven dry down, be crushed to 325 orders, through 450-780 ℃ of fast dewatering, get amorphous active oxidation aluminium powder, put into dribbling balling machine, spray into water and pH value respectively 12.0,13.0,13.5 sodium hydroxide solution, rolling is formed into Φ 1.5-2.9mm.Semi-finished product are 40 ℃ of following healths 11 hours, under 400 ℃, calcine the finished product activated alumina.
The product that makes has following result after tested:
Lot number | Specific area (m 2/g) | Pore volume (ml/g) | Compression strength (N/) | Bulk specific weight (g/ml) |
Pure water | ????292 | ????0.39 | ????47 | ????0.77 |
??pH12.7 | ????298 | ????0.40 | ????55 | ????0.80 |
??pH13.0 | ????318 | ????0.41 | ????57 | ????0.82 |
??pH13.5 | ????332 | ????0.43 | ????66 | ????0.84 |
Embodiment 2
Do raw material with commercially available α-gibbsite, 120 ℃ of oven dry down, be crushed to 325 orders, through 450-780 ℃ of fast dewatering, amorphous active oxidation aluminium powder, put into dribbling balling machine, spray into water and 5%, 12% sodium hydroxide solution respectively, wherein 13.5, roll is formed into Φ 3.0-5.0mm to sodium hydroxide solution with rare nitre acid for adjusting pH value.Semi-finished product are 40 ℃ of following healths 11 hours, under 400 ℃, calcine the finished product activated alumina.
The product that makes has following result after tested:
Lot number | Specific area (m 2/g) | Pore volume (ml/g) | Compression strength (N/) | Bulk specific weight (g/ml) | Na 2O content (w/w, %) |
Pure water | ????287 | ????0.38 | ????147 | ????0.71 | ????0.41 |
??5% | ????311 | ????0.41 | ????183 | ????0.78 | ????1.62 |
??12% | ????290 | ????0.43 | ????195 | ????0.81 | ????3.77 |
Claims (7)
1. preparation method who contains the activated alumina adsorbents of alkali (soil), with aluminium hydroxide is raw material, and drying, pulverizing are dewatered in thermal current, make the former powder of activated alumina, former powder is placed in the dribbling balling machine, sprays into the aqueous solution of alkali (soil) metallic compound, the rolling moulding, again through calcining, finished product, it is characterized in that: (1) aluminium hydrate powder bake out temperature is at 100 ℃-140 ℃, and is crushed to 300 orders; (2) in the high temperature gas flow with 380 ℃-1000 ℃ of aluminium hydrate powder addings,, make the active oxidation aluminium powder of porous through dehydration; (3) aqueous solution of preparation alkali or strong base-weak acid salt is made adhesive, and its pH value is 11-14; (4) the active oxidation aluminium powder is put into dribbling balling machine, spray into the solution of (3), the rolling moulding; (5) be incubated 3-16 hour down at 30 ℃-120 ℃, the calcining furnace of packing into was calcined 0.5-4 hour down at 300 ℃-450 ℃, made product of the present invention.
2. according to the preparation method of claim 1, it is further characterized in that: aluminium hydroxide multiple crystalline forms such as β-gibbsite, α-gibbsite or boehmite.
3. according to the preparation method of claim 1, it is further characterized in that: the aqueous solution of preparation can be the solution that simple aqueous slkali, strong base weak acid salting liquid or aqueous slkali neutralizes with acid, it also can be the mixture of several solns, as sodium hydroxide solution, potassium hydroxide solution, magnesium hydroxide solution, aqua calcis, lithium hydroxide solution, sodium carbonate liquor, sodium acetate solution, sodium formate solution, or the solution that neutralizes with acid as nitric acid, carbon dioxide, organic acid of NaOH, potassium hydroxide solution.
4. according to the preparation method of claim 1, it is further characterized in that: the pH value of the solution of preparation is preferably in 12-13.7 in the scope of 11-14.
5. according to the preparation method of claim 1, it is further characterized in that: the solution of preparation adds when moulding, the adding of preferably spraying during the rolling moulding.
6. according to the preparation method of claim 1, it is further characterized in that: the time of hydrothermal treatment consists is preferably in more than 10 hours more than 5 hours.
7. according to the preparation method of claim 1, it is further characterized in that: the temperature of calcining is 300-550 ℃, is preferably 380-420 ℃.
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CN 00136212 CN1124879C (en) | 2000-12-25 | 2000-12-25 | Preparation process of alumina adsorbant |
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CN 00136212 CN1124879C (en) | 2000-12-25 | 2000-12-25 | Preparation process of alumina adsorbant |
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CN102658023A (en) * | 2012-05-17 | 2012-09-12 | 东南大学 | Carbon dioxide solid absorbent capable of effectively inhibiting active components from losing effect |
CN102872792A (en) * | 2012-08-28 | 2013-01-16 | 常州大学 | Composite adsorbing material for removing lithium ions in natural water and preparation method thereof |
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2000
- 2000-12-25 CN CN 00136212 patent/CN1124879C/en not_active Expired - Fee Related
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CN102029165B (en) * | 2010-11-09 | 2012-10-17 | 中国海洋石油总公司 | Method for preparing ozone catalytic oxidation catalyst for treating coking wastewater |
CN102617314A (en) * | 2012-02-22 | 2012-08-01 | 吉林化工学院 | Application of inorganic alkaline and fixed-bed adsorption technique to deacidification and purification of diisobutyl ketone |
CN102658023A (en) * | 2012-05-17 | 2012-09-12 | 东南大学 | Carbon dioxide solid absorbent capable of effectively inhibiting active components from losing effect |
CN102872792A (en) * | 2012-08-28 | 2013-01-16 | 常州大学 | Composite adsorbing material for removing lithium ions in natural water and preparation method thereof |
CN103480273A (en) * | 2013-09-30 | 2014-01-01 | 东南大学 | Highly-activity sodium-based solid carbon dioxide absorbent |
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