CN1053164C - Preparation process of alumina - Google Patents
Preparation process of alumina Download PDFInfo
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- CN1053164C CN1053164C CN97121771A CN97121771A CN1053164C CN 1053164 C CN1053164 C CN 1053164C CN 97121771 A CN97121771 A CN 97121771A CN 97121771 A CN97121771 A CN 97121771A CN 1053164 C CN1053164 C CN 1053164C
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Abstract
The present invention discloses an alumina preparation method, firstly adding aluminium compound and acid or alkali solution simultaneously and continuously, controlling pH at a certain constant value within the range of 6 to 11 and producing colloid in cocurrent flow to generate crystal seed aluminium hydroxide. Then noncrystalline aluminium hydroxide and fine particles are dissolved by adding acid or alkali solution to regulate pH value to greater than 11 or smaller than 4; finally, both dissolved and newly added aluminium ions re-precipitate under the action of seed crystal by re-adding acid or alkali solution to regulate pH value within 6 to 11, the steps are repeated for 1 to 20 times and alumina is produced through ageing, washing, filtration, drying, forming and roasting.
Description
The invention belongs to the preparation method of aluminium oxide, relate in particular to and after stream becomes glue to generate crystal kind aluminium hydroxide, PH swings into glue and prepares γ-Al again
2O
3Method.
As everyone knows, aluminum oxide is a kind of important catalyst carrier.The method for preparing aluminium oxide is a lot, and the method for preparing aluminium oxide with aluminate or aluminium salt can be divided into usually: 1. positive addition: alkaline material is progressively joined in the acid material, be settled out alumina gel in the medium that pH value constantly raises; 2. anti-addition: acid material is progressively joined in the alkaline material, in the medium that pH value constantly reduces, be settled out alumina gel; And stream become glue: acid and alkaline material is with the simultaneously continuously adding of certain velocity ratio, is settled out alumina gel in the constant medium of pH value.Front two kinds of methods are to become the pH value process, and alumina gel is to generate under the pH value that constantly changes, and is unfavorable for the generation of single crystal form, causes easily the inhomogeneous of particle.Rear a kind of method is to decide the pH value process, and alumina gel is to generate under constant pH value, is conducive to the generation of single crystal form, reduces the generation of fine particle, but still can be with the generation of amorphous hydroted alumina and fine particle.So, be difficult to prepare the aluminum oxide of crystallization purity height, macropore, pore distribution concentration with these methods.U.S. Pat 4248852 disclosed alumina preparation methods, be earlier neutralizing agent to be joined in the aluminum compound, make pH value to 6～10, generate seed crystal of aluminium hydroxide, alternately add aluminum compound and neutralizing agent then, pH value is alternately changed, i.e. the PH swing method in the soluble end and the areas of sedimentation of alumina gel, make pore distribution concentration, the aluminum oxide that aperture, pore volume can be controlled on demand.But this preparation method's complexity, solid content is low in the aging slurries, and production efficiency is low.The disclosed alumina preparation method of the clear 60-54917 of Japanese Patent is: make crystal seed with the alumina gel that the PH swing method makes, add simultaneously continuously aluminum compound then and make neutralizing agent, carry out and stream becomes glue, obtain macroporous aluminium oxide.The method with the generation of amorphous hydroted alumina and fine particle, affects crystallization purity and the pore size distribution of product easily when also stream becomes glue.
The object of the present invention is to provide a kind of work simplification, production efficiency height, alumina preparation method that product performance are good.
The preparation method of aluminum oxide of the present invention, its preparation process comprises:
1. in colloid generating kettle, add end water, be heated to 60～100 ℃, add continuously simultaneously aluminium compound and acidity or alkaline solution, pH value is controlled at a certain steady state value in 6～11 scopes, carries out and stream becomes glue, continues 5～120 minutes, stirred 5～30 minutes, and generated seed crystal of aluminium hydroxide.
2. add acidity or alkaline solution, transfer pH value to＜4 or＞11, stirred 5～20 minutes, dissolve amorphous hydroted alumina and fine particle.
3. adding acidity or alkaline solution are transferred pH value to 6～11, stir 5～20 minutes, and the aluminium ion of dissolving and the new aluminium ion that adds are precipitated under the crystal seed effect again.
4. repeat above-mentioned 2,3 step 1～20 time.
5.60 wore out 10～60 minutes under～100 ℃ of temperature, filter.
6. chemical water purification washing is 2～8 times, and is dry under 100～140 ℃ of temperature, gets aluminum hydroxide solid elastomer.
7. behind the crushing screening, extruded moulding, 450～700 ℃ of roasting temperatures 1～8 hour get γ-Al
2O
3
The effect that the present invention reached:
1. adopt elder generation and stream to become glue, can prepare good seed crystal of aluminium hydroxide.As everyone knows, γ-Al
2O
3Precursor---boehmite (α-Al
2O
3H
2O) preparation is the process of a complexity, and influence factor is numerous, and boehmite has its optimum formation condition.And stream becomes glue can select to be conducive to most to carry out under the condition that boehmite generates, and becomes the adhesive tape part constant.Therefore the seed crystal of aluminium hydroxide crystallization purity that generates is higher, granularity more greatly and more even, crystallization purity (pseudo-boehmite/dry glue powder weight percent) is at 50～70wt%, about grain fineness number 40A.The aluminium hydroxide that generates like this is good seed crystal of aluminium hydroxide, in PH swing process subsequently, can play good guide effect.
2. simplified preparation process, the production efficiency height.Because this method gained seed crystal of aluminium hydroxide crystallization purity is higher, particle is bigger, in the PH swing process, can play good crystal seed guide effect, and germination is few to the required PH number of oscillations of expection size, has simplified preparation process.Amorphous or the fine particle aluminium hydroxide that produces in present method crystal seed forming process is less, and its aluminum ion that dissolves again in the rear slurry reduces.Again because seeded crystallization purity height, show that crystal seed quantity is many, the aluminum ion during redeposition in the slurries mainly is deposited on the crystal seed, has reduced the generation of newborn amorphous or fine particle aluminium hydroxide, make the solid content in the final aging slurries to increase, improved production efficiency.
3. product crystallization purity height.Adopt the aluminum hydroxide solid elastomer powder of the inventive method preparation, pseudo-boehmite content is at 75～98wt%.
4. the product pore structure is good.Pore structure has material impact to activity of such catalysts, selectivity, life-span.Adopt the prepared aluminum oxide of the inventive method, can satisfy the requirement of different catalysts pore structure, specific surface area 160～400 meters squared per gram, 0.4～1.1 milliliter/gram of pore volume, pore distribution concentration, aperture, pore volume can be controlled as required.If by changing preparation condition, can make the aluminum oxide of following pore diameter range: the I. pore diameter range is at the aluminum oxide of 40～100A smaller aperture due; II. pore diameter range is at the intermediate pore size aluminum oxide of 100～300A; III. pore diameter range is at the larger aperture aluminum oxide of 200～600A.The pore volume of above-mentioned three kinds of pore diameter ranges all accounts for more than 70% of total pore volume.
Aluminum oxide with the inventive method preparation is applicable to catalyzer, support of the catalyst, sorbent material, binding agent, siccative etc., be specially adapted to catalyzer and support of the catalyst, be particularly useful for the carrier of hydrodemetallation (HDM), hydrotreatment, hydrofining, hydrocracking and reformation, isomerization catalyst.
The present invention is further illustrated for the following examples:
Comparative example 1
Adding 20 liter deionized waters in colloid generating kettle, be heated to 90 ℃, is that 200 gram/liters are (with Al with concentration
2O
3Meter) sodium aluminate solution and concentration are that 50 gram/liters are (with Al
2O
3Meter) aluminum sulfate solution, at different charge doors, respectively with 3 liters/hour and 5 liters/hour simultaneously continuously adding of flow velocity, pH value is controlled at 10 ± 0.2, continuous charging 2 hours.Stop reinforced back and continue to stir, aging 30 minutes after-filtration.Filter cake is with deionized water washing 4 times, 120 ℃ of dryings 4 hours, and crushing screening is extruded into φ 1.2 clover bars, and dry rear 550 ℃ of roastings 4 hours make γ-Al
2O
3Product R
1
Comparative example 2
Adding 20 liter deionized waters and 1 liter concentration are that 40 gram/liters are (with Al in colloid generating kettle
2O
3Meter) aluminum nitrate solution is heated to 90 ℃, and under fully stirring, adding concentration is that 70 gram/liters are (with Al
2O
3Meter) sodium aluminate solution stops to feed in raw material to pH value=10, obtains the milky slurries, as aluminium hydroxide crystal seed.Stir after 10 minutes, add aluminum nitrate solution to pH value=2.5～3.0, stir after 10 minutes, add sodium aluminate solution to pH value=10, stirred 10 minutes.So repeat aforesaid operations 4 times, 90 ℃ were stirred aging 20 minutes.Other makes γ-Al with comparative example 1
2O
3Product R
2
Comparative example 3
With the identical method of comparative example 2, the aluminum hydroxide slurry that the pH value swing makes for 4 times is as seed crystal of aluminium hydroxide.Stir down, at different charging openings, respectively with 1.5 liters/hour and 1.0 liters/hour flow velocity, adding aluminum nitrate and sodium aluminate solution continuously simultaneously, pH value is controlled at 10 ± 0.2,90 ℃ of temperature, continuous charging 2 hours.After stopping to feed in raw material, stirred aging 20 minutes, other logical comparative example 1 makes γ-Al
2O
3Product R
3
Embodiment 1
In colloid generating kettle, add 20 liter deionized waters, be heated to 90 ℃, fully stir lower, at different charge doors, respectively with 4 liters/hour and 2 liters/hour flow velocity, adding concentration is that 17wt% salpeter solution and concentration are that 180 gram/liters are (with Al
2O
3Meter) sodium aluminate solution, pH value is controlled at 10.0 ± 0.2, and continuous 30 minutes, stop to feed in raw material, obtain seed crystal of aluminium hydroxide.Stir after 10 minutes, add salpeter solution to pH value=2.5, stir after 5 minutes, add sodium aluminate solution to PH=10, stirred 5 minutes.Repeat aforesaid operations 2 times.Stirred under 90 ℃ of temperature aging 20 minutes.Other makes γ-Al with comparative example 1
2O
3Product A.
Embodiment 2
The preparation method after difference is to make seed crystal of aluminium hydroxide, adds sodium aluminate solution to PH=11.5 with embodiment 1, stirs after 5 minutes, adds salpeter solution to PH=10, stirs 5 minutes.Repeat operation 4 times, make γ-Al
2O
3Product B.
Embodiment 3
In colloid generating kettle, add 20 liter deionized waters, be heated to 95 ℃, fully stir lower, at different charge doors, respectively with 3.0 liters/hour and 2.0 liters/hour flow velocity, adding concentration is that 40 gram/liters are (with Al
2O
3Meter) aluminum nitrate solution and concentration are that 180 gram/liters are (with Al
2O
3Meter) sodium aluminate solution, pH value is controlled at 10.0 ± 0.2, continues 20 minutes, stops to feed in raw material, and obtains seed crystal of aluminium hydroxide.Stir after 10 minutes, add above-mentioned aluminum nitrate solution to pH value=2.5, stir after 5 minutes, add above-mentioned sodium aluminate solution to PH=10, stirred 5 minutes.Repeat aforesaid operations 8 times.95 ℃ lower aging 20 minutes.Other makes γ-Al with embodiment 1
2O
3Products C.
Above-mentioned 6 kinds of alumina product physico-chemical properties are listed in table 1.
The physicochemical property of table 1 product
| A | B | C | R 1 | R 2 | R 3 | ||
| Crystallization purity wt% | 83 | 81 | 88 | 60 | 82 | 79 | |
| Specific surface area (m 2/g) | 265 | 210 | 170 | 270 | 260 | 210 | |
| Pore volume (ml/g) | 0.60 | 0.83 | 0.95 | 0.55 | 0.58 | 0.80 | |
| 20～40A | 4.8 | 1.6 | 1.5 | 10.4 | 5.1 | 1.7 | |
| The hole | 40～100A | 83.9 | 12.2 | 2.6 | 57.6 | 80.4 | 14.3 |
| Body | 100～200A | 6.2 | 56.0 | 8.2 | 11.9 | 8.2 | 52.4 |
| Long-pending | 200～300A | 2.2 | 24.1 | 19.4 | 7.1 | 2.8 | 22.4 |
| ％ | 300～600A | 2.5 | 5.2 | 64.2 | 9.4 | 3.4 | 6.2 |
| ＞600A | 0.4 | 0.9 | 4.1 | 3.6 | 0.4 | 3.0 | |
| Pore diameter range A | 40～100 | 100～300 | 200～600 | 40～100 | 40～100 | 100～300 | |
| Account for total pore volume percentage ratio % | 83.9 | 80.1 | 83.6 | 57.6 | 80.4 | 74.8 | |
| (g/l is with Al for aging slurry solid content 2O 3Meter) | 43.2 | 45.5 | 40.3 | 49.5 | 11.9 | 15.5 | |
By table 1 as seen, adopt aluminum oxide A, B that the present invention makes, C crystallization purity at 83～88wt%.Different preparation conditions can make pore volume at 0.60～0.95ml/g.The aperture concentrates on 40～100A respectively, 100～300A, and 200～600A, and all account for more than 80% of total pore volume, pore distribution concentration.Solid content in the aging slurries at 40.3～45.5 grams per liters (with Al
2O
3Meter).With and stream become the aluminum oxide R of glue method preparation
1, crystallization purity has only 65wt%, and pore distribution is not concentrated.Adopt the aluminium oxide R of PH swing method preparation
2, to the aluminium oxide A of similar pore structure, the PH number of oscillations is many twice, and the solid content in the aging slurries only has 11.9 grams per liters (with Al
2O
3Meter).Stream becomes the method for glue to prepare aluminium oxide R to adopt PH to swing also again
3, crystallization purity is 79wt%, it is total long-pending 74.8% that the hole of 100～300A accounts for, the solid content in the aging slurries at 15.5 gram/liters (with Al
2O
3Meter).The alumina product function admirable that this explanation makes with the present invention, and simplified preparation process, improved production efficiency.
Claims (5)
1, a kind of preparation method of aluminum oxide is characterized in that:
1) add end water in colloid generating kettle, be heated to 60～100 ℃, add continuously simultaneously aluminium compound and acidity or alkaline solution, pH value is controlled at a certain steady state value in 6～11 scopes, carries out and stream becomes glue, stirs the generation seed crystal of aluminium hydroxide 5～30 minutes;
2) add acidity or alkaline solution, transfer pH value to＜4 or＞11, stirred 5～20 minutes;
3) add alkalescence or acid solution, transfer pH value to 6～11, stirred 5～20 minutes;
4) repeat above-mentioned 2), 3) step 1～20 time;
5) 60～100 ℃ were worn out 10～60 minutes down, filtered;
6) chemical water purification washing is 2～8 times, and 100～140 ℃ lower dry, gets aluminum hydroxide solid elastomer;
7) behind the crushing screening, extruded moulding, 450～700 ℃ of lower roastings 1～8 hour get γ-Al
2O
3
2, method according to claim 1 is characterized in that described aluminum compound is aluminum nitrate, Tai-Ace S 150, aluminum chloride, sodium metaaluminate.
3, method according to claim 1 is characterized in that described acidic solution is one or more the mixture in nitric acid, sulfuric acid, hydrochloric acid, aluminum nitrate, Tai-Ace S 150, the aluminum chloride.
4, method according to claim 1 is characterized in that described basic solution is one or more the mixture in sodium metaaluminate, ammoniacal liquor, yellow soda ash, the sodium hydroxide.
5, method according to claim 1 is characterized in that described and the stream gelation time is 5～90 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121771A CN1053164C (en) | 1997-12-19 | 1997-12-19 | Preparation process of alumina |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97121771A CN1053164C (en) | 1997-12-19 | 1997-12-19 | Preparation process of alumina |
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| Publication Number | Publication Date |
|---|---|
| CN1184078A CN1184078A (en) | 1998-06-10 |
| CN1053164C true CN1053164C (en) | 2000-06-07 |
Family
ID=5176431
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97121771A Expired - Fee Related CN1053164C (en) | 1997-12-19 | 1997-12-19 | Preparation process of alumina |
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-
1997
- 1997-12-19 CN CN97121771A patent/CN1053164C/en not_active Expired - Fee Related
Patent Citations (3)
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|---|---|---|---|---|
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| US4562059A (en) * | 1984-06-08 | 1985-12-31 | Chiyoda Chemical Engineering & Construction Co., Ltd. | Method of preparing alumina |
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|---|---|
| CN1184078A (en) | 1998-06-10 |
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