CN100436324C - Method for preparing unformed aluminium hydroxide - Google Patents
Method for preparing unformed aluminium hydroxide Download PDFInfo
- Publication number
- CN100436324C CN100436324C CNB2006100792186A CN200610079218A CN100436324C CN 100436324 C CN100436324 C CN 100436324C CN B2006100792186 A CNB2006100792186 A CN B2006100792186A CN 200610079218 A CN200610079218 A CN 200610079218A CN 100436324 C CN100436324 C CN 100436324C
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- Prior art keywords
- aluminium hydroxide
- unformed
- aluminum hydroxide
- preparation
- reactor
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Abstract
The present invention discloses a method for preparing unformed aluminum hydroxide, which relates to aluminum hydroxide, particularly to a method for preparing aluminum hydroxide with high acid solubility and low-density; the present invention provides a method for preparing unformed aluminum hydroxide with high acid solubility and low-density. Gibbsite and sodium hydroxide are prepared into sodium metalluminate solution with high concentration, and the caustic ratio of the sodium metalluminate solution is controlled; deionized water is used for dilution, and hole enlarging agents are added; the deionized water is added to a reaction kettle at first; obtained raw material fliquid and CO2 gas flow into the reaction kettle; the glue forming temperature is controlled and the feeding flow quantity is regulated; serous fluid is filtered, washed and dried to obtain aluminum hydroxide. The present invention adopts continuous parallel-flow feeding and high concentration CO2 gas for glue formation, quickens the neutralization reaction rate and shortens the glued formation time; thereby, the generation of pseudo-boehmite is avoided or suppressed; cooling equipment is omitted, the equipment utilization is enhanced, or the volume of a glue kettle is reduce, and the cost is low. The aluminum hydroxide product has the characteristics of peracid solubility and low-density, and completely dissolves in excessive 20% of nitric acid solution; the bulk density is smaller than or equal to 0.4 g/ml.
Description
Technical field
The present invention relates to a kind of aluminium hydroxide, particularly relate to a kind of preparation method of high solubility in acid low density aluminium hydroxide.
Background technology
Activated alumina is to use the time the longest, most widely used a kind of synthetic vectors.It is aboundresources not only, and have crushing strength height, Heat stability is good, specific absorption is big, specific surface area is moderate and pore volume and the adjustable characteristic of pore size distribution, is the excellent carrier that is used for petrochemical complex and chemical fertilizer industry absorption and loaded catalyst.Because the employed alumina supporters of macromolecular reaction catalyzer such as residual hydrogenation must have enough big aperture and pore volume, but existing carrier is difficult to reach this requirement.Prior art generally is to make pseudo-boehmite earlier, and then the preparation alumina supporter.For example: Chinese patent CN 03101176.4 has described by CO
2In and sodium metaaluminate prepare the method for pseudo-boehmite.The product acid dissolubility that this method obtains is poor, can't the resolved vector physical strength and wide aperture, pore volume between contradiction.
Summary of the invention
Purpose of the present invention aims to provide the preparation method of a kind of high solubility in acid low density (being high hole) unformed aluminium hydroxide.But, and have the enough big aperture and the alumina supporter of pore volume by this aluminium hydroxide processing machinery intensity height.
Its step of the present invention is as follows:
1) be mixed with dense sodium aluminate solution with gibbsite and sodium hydroxide, the causticity of control solution is than [NaOH/Al (OH)
3] be 1.4～1.8mol/mol;
2) get the dense sodium aluminate solution for preparing, being diluted to concentration with deionized water is 5～30gAl
2O
3L
-1Be preferably 10～25gAl
2O
3L
-1
3) 5%～15% of the adding alumina weight expanding agent in the sodium aluminate solution of dilution, described expanding agent is selected from inorganic ammonium, preferred bicarbonate of ammonia or ammoniacal liquor etc.;
4) add the deionized water that accounts for reactor volume 1/2 earlier at reactor, will be by the stock liquid and the CO of step 3) gained
2Gas flows into reactor simultaneously, is controlled to the glue temperature at 15～40 ℃, is preferably 15～25 ℃, regulates the feed rate of the two, and making reactor discharge port product pH value is 9.0～12.0, is preferably 10.0～11.5;
5) with step 4) gained dope filtration, and with 40～70 ℃ deionized water wash filter cake;
6) at 50～90 ℃ of following drying step 5) the gained filter cake, promptly obtain unformed aluminium hydroxide.
In step 4), be provided with strong mixer in the reactor.
The present invention adopts continuously and flows to material and high concentration CO
2Gas becomes glue, accelerates neutralization reaction speed, shortens gelation time, thereby avoids or suppress the generation of pseudo-boehmite.Because gelation time shortens, the restriction of temperature of reaction is relaxed simultaneously, save the cooling apparatus of production process; It is continuous and flow to the volume that the material mode has also improved plant factor or reduced colloid generating kettle, and then reduces cost.Products obtained therefrom has high solubility in acid and low-density characteristics, is in particular in that product sample is dissolved in 20% excessive salpeter solution fully, and its tap density≤0.4g/ml.
Embodiment
Below by specific embodiment the present invention is elaborated.
Embodiment 1
Get industrial one-level gibbsite and [contain Al
2O
363% (w)] 152.4g and NaOH aqueous solution 273g (w), add deionized water 150g, under agitation be heated to 100 ℃, constant temperature 120min dissolves fully to aluminium hydroxide and to obtain concentration and be about 400gAl
2O
3L
-1Sodium aluminate solution [NaOH/Al (OH)
3The mol ratio is 1.4], being diluted to concentration with deionized water again is 15g Al
2O
3L
-1Sodium aluminate solution, add 8% ammonium bicarbonate soln; Add the deionized water that accounts for reactor volume 1/2 earlier at reactor then, open valve, stock liquid (above-mentioned rare sodium metaaluminate mixing solutions) and CO
2[98% (V)] gas flows into reactor simultaneously, and the two mixes in the reactor bottom, is provided with strong mixer in the reactor, and reactant flow forms a kind of helical flow that makes progress under brute force stirs, flowed out by exit, reactor top at last; Be controlled to 25 ℃ of glue temperature, CO
2Flow is 600ml/min, regulates the feed rate of stock liquid, and making reactor discharge port product pH value is 11.0; With the gained dope filtration, and with 60 ℃ of deionized water wash; At 70 ℃ of following dry cakes, the time is 7h, promptly gets unformed aluminium hydroxide, and its main character is listed in table 1.
Embodiment 2,3
The preparation method is identical with embodiment 1, and dense sodium aluminate solution is diluted to 5gAl
2O
3L
-1And 30gAl
2O
3L
-1, the products obtained therefrom main character is listed in table 1.
Reference example 1
In embodiment 1, dense sodium aluminate solution is diluted to 40gAl
2O
3L
-1, the products obtained therefrom main character is listed in table 1.
Table 1. embodiment 1～3 and reference example 1 products made thereby main character
| Sample | Sodium aluminate solution concentration/g Al 2O 3·L -1 | Solubility in acid 5ml 20% (v) nitric acid | Tap density/gml -1 | The thing phase |
| Embodiment 1 | 15 | CL | 0.352 | Unformed |
| Embodiment 2 | 5 | CL | 0.340 | Unformed |
| Embodiment 3 | 30 | CL | 0.369 | Unformed |
| Reference example 1 | 40 | CL not | 0.552 | Pseudo-boehmite+unformed |
Embodiment 4,5
Change NaOH/Al (OH)
3The mol ratio is 1.6,1.8, and all the other are with embodiment 1, products obtained therefrom main character such as table 2.
Table 2. embodiment 1,4 and 5 products made thereby main character
| Sample | NaOH/Al(OH) 3The mol ratio | Solubility in acid 5ml 20% (v) nitric acid | Tap density/gml -1 | The thing phase |
| Embodiment 1 | 14 | CL | 0.352 | Unformed |
| Embodiment 4 | 1.6 | CL | 0.359 | Unformed |
| Embodiment 5 | 1.8 | CL | 0.388 | Unformed |
Embodiment 6,7
In embodiment 1, change change pH values and be respectively 10.0 and 9.5, be controlled to the glue temperature at 35 ℃, products obtained therefrom main character such as table 3.
Reference example 2
In embodiment 1, changing change pH values is 8.0, products obtained therefrom main character such as table 3.
Table 3. embodiment 1,6～7 and reference example 2 products made thereby main character
| Sample | The pH value | Solubility in acid 5ml 20% (v) nitric acid | Tap density/gml -1 | The thing phase |
| Embodiment 1 | 11.0 | CL | 0.352 | Unformed |
| Embodiment 6 | 10.0 | CL | 0.394 | Unformed |
| Embodiment 7 | 9.5 | CL | 0.400 | Unformed |
| Reference example 2 | 8.0 | CL not | 0.600 | Pseudo-boehmite+unformed |
Embodiment 8
Change NaOH/Al (OH)
3The mol ratio is 1.8, expanding agent NH
4HCO
3Consumption is 12gL
-1, being controlled to the glue temperature at 15 ℃, all the other are with embodiment 1, products obtained therefrom main character such as table 4.
Embodiment 9
Change NaOH/Al (OH)
3The mol ratio is 1.8, and expanding agent liquefied ammonia consumption is 8gL
-1, being controlled to the glue temperature at 15 ℃, all the other are with embodiment 1, products obtained therefrom main character such as table 4.
Table 4. embodiment 1,8 and reference example 3～4 products made thereby main character
| Sample | Expanding agent consumption gL -1 | Solubility in acid 5ml 20% (v) nitric acid | Tap density/gml -1 | The thing phase |
| Embodiment 8 | NH 4HCO 3：12 | CL | 0.346 | Unformed |
| Embodiment 9 | NH 3：8 | CL | 0.350 | Unformed |
Embodiment 10
Get embodiment 1 made unformed aluminium hydroxide 100g, add carbon black 25g, mix, add 4%HNO again
3Solution 70g puddles extrusion, dry 4h under 120 ℃, and 850 ℃ of following roasting 3h, the products obtained therefrom main character is listed in table 5.
Reference example 5
With embodiment 10 made unformed aluminium hydroxide 100g, change the obtained pseudo-boehmite of describing by patent ZL03101176.4 of method into, all the other are identical, and the products obtained therefrom main character is listed in table 5.
Table 5. embodiment 10 and reference example 5 products made thereby main character
| Sample | Pore volume/cm 3·g -1 | Specific surface/m 2·g -1 | Crushing strength/Ncm -1 |
| Embodiment 9 | 1.02 | 135 | 72 |
| Reference example 5 | 0.98 | 140 | 35 |
Claims (6)
1. the preparation method of a unformed aluminium hydroxide makes aluminium hydroxide with carbonic acid gas by sodium aluminate solution after becoming the glue reaction, it is characterized in that its step is as follows:
1) be mixed with dense sodium aluminate solution with gibbsite and sodium hydroxide, the causticity of control solution is than [NaOH/Al (OH)
3] be 1.4～1.8mol/mol;
2) get the dense sodium aluminate solution for preparing, being diluted to concentration with deionized water is 5～30gAl
2O
3L
-1
3) agitation and dropping is gone into 5%～15% expanding agent of alumina weight in the sodium aluminate solution of dilution;
4) add the deionized water that accounts for reactor volume 1/2 earlier at reactor, will be by the stock liquid and the CO of step 3 gained
2Gas flows into reactor simultaneously, is controlled to the glue temperature at 15～40 ℃, regulates the feed rate of the two, and making reactor discharge port product pH value is 9.0～12.0, is provided with strong mixer in the reactor;
5) with step 4 gained dope filtration, and with 40～70 ℃ deionized water wash filter cake;
6) at 50～90 ℃ of following drying step 5 gained filter cakes, promptly obtain unformed aluminium hydroxide.
2. the preparation method of a kind of unformed aluminium hydroxide as claimed in claim 1, the concentration that it is characterized in that the sodium aluminate solution in the step 2 is 10～25g Al
2O
3L
-1
3. the preparation method of a kind of unformed aluminium hydroxide as claimed in claim 1 is characterized in that the expanding agent in the step 3 is inorganic ammonium.
4. the preparation method of a kind of unformed aluminium hydroxide as claimed in claim 3 is characterized in that said expanding agent is bicarbonate of ammonia or ammoniacal liquor.
5. the preparation method of a kind of unformed aluminium hydroxide as claimed in claim 1 is characterized in that the one-tenth glue temperature in the step 4 is 15～25 ℃.
6. the preparation method of a kind of unformed aluminium hydroxide as claimed in claim 1 is characterized in that the reactor discharge port product pH value in the step 4 is 10.0～11.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100792186A CN100436324C (en) | 2006-04-17 | 2006-04-17 | Method for preparing unformed aluminium hydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100792186A CN100436324C (en) | 2006-04-17 | 2006-04-17 | Method for preparing unformed aluminium hydroxide |
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| Publication Number | Publication Date |
|---|---|
| CN1843924A CN1843924A (en) | 2006-10-11 |
| CN100436324C true CN100436324C (en) | 2008-11-26 |
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ID=37062895
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100792186A Expired - Fee Related CN100436324C (en) | 2006-04-17 | 2006-04-17 | Method for preparing unformed aluminium hydroxide |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102039195B (en) * | 2009-10-16 | 2013-01-09 | 中国石油化工股份有限公司 | Preparation method of alumina carrier |
| CN102452678B (en) * | 2010-10-15 | 2013-06-19 | 中国石油化工股份有限公司 | Method for preparing aluminum hydroxide through carbonization |
| CN106335913B (en) * | 2016-08-16 | 2018-05-01 | 中铝山东新材料有限公司 | Amorphous hydroted alumina, its preparation method and preparation facilities |
| CN106984296B (en) * | 2017-04-24 | 2019-06-18 | 西南化工研究设计院有限公司 | A kind of preparation method of vapor phase method methyl alcohol to dimethyl ether catalyst |
| CN108356943A (en) * | 2018-01-31 | 2018-08-03 | 中国科学院理化技术研究所 | A kind of high thermal conductivity coefficient timber and the preparation method and application thereof |
| CN110304644B (en) * | 2019-07-01 | 2022-03-25 | 中铝山东有限公司 | Method for producing high-purity high-viscosity pseudo-boehmite |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4292295A (en) * | 1978-07-26 | 1981-09-29 | Rhone-Poulenc Industries | Highly reactive alumina and process for the preparation thereof |
| CN1254684A (en) * | 1998-11-21 | 2000-05-31 | 中国石化齐鲁石油化工公司 | Process for preparing active alumina by sodium metaaluminate-carbon dioxide method |
| CN1420082A (en) * | 2002-12-19 | 2003-05-28 | 厦门大学 | Process for preparing active alumina |
| CN1425612A (en) * | 2003-01-16 | 2003-06-25 | 厦门大学 | Process for preparing active aluminium oxide |
-
2006
- 2006-04-17 CN CNB2006100792186A patent/CN100436324C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4292295A (en) * | 1978-07-26 | 1981-09-29 | Rhone-Poulenc Industries | Highly reactive alumina and process for the preparation thereof |
| CN1254684A (en) * | 1998-11-21 | 2000-05-31 | 中国石化齐鲁石油化工公司 | Process for preparing active alumina by sodium metaaluminate-carbon dioxide method |
| CN1420082A (en) * | 2002-12-19 | 2003-05-28 | 厦门大学 | Process for preparing active alumina |
| CN1425612A (en) * | 2003-01-16 | 2003-06-25 | 厦门大学 | Process for preparing active aluminium oxide |
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| CN1843924A (en) | 2006-10-11 |
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Granted publication date: 20081126 Termination date: 20110417 |