CN100337920C - Method of preparing active aluminium oxide from aluminium phosphide - Google Patents
Method of preparing active aluminium oxide from aluminium phosphide Download PDFInfo
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- CN100337920C CN100337920C CNB2004100203178A CN200410020317A CN100337920C CN 100337920 C CN100337920 C CN 100337920C CN B2004100203178 A CNB2004100203178 A CN B2004100203178A CN 200410020317 A CN200410020317 A CN 200410020317A CN 100337920 C CN100337920 C CN 100337920C
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- tower
- hydrolysis
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- aluminium phosphide
- aluminium
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Abstract
The present invention discloses a method for preparing active aluminium oxide from aluminium phosphide powder, which belongs to a preparing technique of active aluminium oxide. The method adopts an intermittent hydrolysis method or a continuous hydrolysis method. The method is characterized in that the intermittent hydrolysis method comprises: excessive water is added in a reaction vessel in advance, aluminium phosphide power is put into the water at uniform speed, reaction solution is stirred, generated hydrogen phosphide gas is collected, the reaction solution is filtered after the reaction is finished, and aluminium oxide is obtained after a filter cake is dried, ground and baked; the continuous hydrolysis method comprises: in a normal-pressure or a pressure-reducing hydrolysis tower, countercurrent operation is carried out to the aluminum phosphide powder fed from the middle upper part of the tower and water vapour led in from the bottom side of the tower to realize the hydrolysis reaction of the aluminium phosphide, the hydrogen phosphide gas is collected at the top of the tower, the reaction solution at the bottom of the tower is filtered, and the aluminum oxide is obtained after a filter cake is dried, ground and baked. The present invention has the advantages of simple aluminum oxide production process, low energy consumption, no pollution of 'three wastes', good performance of aluminum oxide hole texture and good high-temperature thermal stability.
Description
Technical field
The present invention relates to a kind ofly prepare the method for activated alumina, belong to the technology of preparing of activated alumina with aluminium phosphide.
Background technology
At present, about 100,000 tons of activated alumina whole world annual production, all be to produce resulting gibbsite or metallic aluminium is a raw material with Bayer process, take off the preparation of four kinds of different process such as method, acid system, alkaline process or aluminium alcoholates method and get through too fast, these method ubiquity technologies are comparatively complicated, the more high shortcoming of energy consumption.
Aluminium phosphide is often used as preparation fumigant PH
3Gas, if be the feedstock production activated alumina with it, because technological process is simple, alumina production cost descends greatly, and then will occupy a tiny space on market.Do not see at present bibliographical information with aluminium phosphide hydrolysis process path of preparing aluminum oxide.
Summary of the invention
The object of the present invention is to provide a kind ofly to prepare the method for activated alumina with aluminium phosphide, this method technological process is simple, energy consumption is low, raw materials cost is low.
The present invention realized by following technical proposals, a kind ofly prepares the method for activated alumina with aluminium phosphide, and this method comprises batch hydrolysis or continuous hydrolysis process, and its technical characterictic comprises following technological process.
Batch hydrolysis: add excessive water in the reaction vessel in advance, at the uniform velocity, quantitatively throw in the aluminium phosphide pulvis in water, temperature of reaction system remains on 25 ℃～80 ℃, adopts mechanical stirring or N
2Or CO
2Gas carries out continuously stirring to reaction soln; Collect the phosphine gas that hydrolysis reaction generates; Reaction finishes, filtering reacting solution, filtrate cycle is used, filter cake in 60 ℃～300 ℃ common dryings or vacuum-drying or supercritical drying 2～12h, pulverizing after 400 ℃～1300 ℃ roasting 1～5h obtain aluminum oxide.
Continuous hydrolysis process: in the ordinary-pressure hydrolysis tower,, under 20 ℃～120 ℃ tower temperature condition, carry out counter-current operation, realize the hydrolysis reaction of aluminium phosphide from the aluminium phosphide pulvis of tower middle and upper part charging and the water vapour that feeds from the tower bottom side; At the overhead collection phosphine gas, the reaction soln at the bottom of the filtration tank, filtrate cycle is used, filter cake in 60 ℃～300 ℃ common dryings or vacuum-drying or supercritical drying 2～12h, pulverizing after 400 ℃～1300 ℃ roasting 1～5h obtain aluminum oxide.
The invention has the advantages that process for making alumina is simple, energy consumption is low, do not have " three wastes " and pollute that the alumina pore texture property is good, high high-temp stability good.
Embodiment
The following stated embodiment describes the present invention in detail.In these embodiments, unless otherwise indicated beyond, all per-cents are all by weight.
Embodiment 1
Add 50L water in the reactor in advance, heating also keeps water temperature at 40 ℃; At first in reactor, feed CO
2Gas treats that entire reaction still and circulating line all are full of CO
2Behind the gas, quantitatively at the uniform velocity drop into the aluminium phosphide pulvis, during keep CO
2Gas uninterruptedly stirs; Reaction dropped into aluminium phosphide pulvis 6kg in lasting 2 hours altogether; Filtering reacting solution adopts common desiccating method in 120 ℃, 2h dry cake, and in 500 ℃ of roasting 3h, gets activated alumina, and the tem analysis sample is the acicular structure of diameter 1～2nm, length 30～40nm, and the BET specific surface area is 280.0m
2.g
-1, pore volume is 0.8cm
3.g
-1
Embodiment 2
Add 50L water in the reactor in advance, heating also keeps water temperature at 30 ℃; At first in reactor, feed N
2Gas treats that entire reaction still and circulating line all are full of N
2Behind the gas, quantitatively at the uniform velocity drop into the aluminium phosphide pulvis, during keep N
2Gas uninterruptedly stirs; Reaction dropped into aluminium phosphide pulvis 6kg in lasting 2 hours altogether; Filtering reacting solution adopts the supercritical drying dry cake 2h of ethanol medium, and in 550 ℃ of roasting 1h, gets activated alumina; The properties of sample basically identical that makes among aluminum oxide performance that this method makes and the embodiment 1.
Embodiment 3
Add 50L water in the reactor in advance, heating also keeps water temperature at 60 ℃; At first in reactor, feed CO
2Gas treats that entire reaction still and circulating line all are full of CO
2Behind the gas, quantitatively at the uniform velocity drop into the aluminium phosphide pulvis, during keep CO
2Gas uninterruptedly stirs; Reaction dropped into aluminium phosphide pulvis 6kg in lasting 2 hours altogether; Filtering reacting solution at 60 ℃ of vacuum-drying filter cake 5h, and in 500 ℃ of roasting 5h, gets activated alumina; The properties of sample basically identical that makes among aluminum oxide performance that this method makes and the embodiment 1.
Embodiment 4
Add 50L water in the reactor in advance, heating also keeps water temperature at 80 ℃; Quantitatively at the uniform velocity drop into the aluminium phosphide pulvis, during reaction soln is carried out continual mechanical stirring; Reaction dropped into aluminium phosphide pulvis 6kg in lasting 2 hours altogether; Filtering reacting solution adopts common desiccating method in 100 ℃, 12h dry cake, and in 500 ℃ of roasting 3h, gets activated alumina; The properties of sample basically identical that makes among aluminum oxide performance that this method makes and the embodiment 1.
Embodiment 5
Add 50L water in the reactor in advance, heating also keeps water temperature at 40 ℃; Quantitatively at the uniform velocity drop into the aluminium phosphide pulvis, during reaction soln is carried out continual mechanical stirring; Reaction dropped into aluminium phosphide pulvis 6kg in lasting 2 hours altogether; Filtering reacting solution adopts common desiccating method in 130 ℃, 2h dry cake, and in 1000 ℃ of roasting 3h, gets activated alumina; The tem analysis sample is the acicular structure of diameter 2～4nm, length 40～60nm, and the BET specific surface area is 160.0m
2.g
-1, pore volume is 0.6cm
3.g
-1
Embodiment 6
In the atmospheric operation tower, keep 90 ℃ tower temperature, make that aluminium phosphide pulvis and water vapour are reverse to contact that both throughput ratios and charge ratio are 1: 3; Filtering reacting solution adopts common desiccating method in 100 ℃, 12h dry cake, and in 1000 ℃ of roasting 3h, gets activated alumina; The tem analysis sample is the acicular structure of diameter 2～4nm, length 40～60nm, and the BET specific surface area is 155.0m
2.g
-1, pore volume is 0.6cm
3.g
-1
Embodiment 7
In the atmospheric operation tower, keep 80 ℃ tower temperature, make that aluminium phosphide pulvis and water vapour are reverse to contact that both throughput ratios and charge ratio are 1: 3; Adopt common desiccating method in 100 ℃, 12h dry cake, and, get aluminum oxide in 1300 ℃ of roasting 3h; The tem analysis sample is the sheet structure of diameter 50～60nm.
Claims (1)
1. one kind prepares method of alumina with aluminium phosphide, this method adopts batch hydrolysis or continuous hydrolysis process, its feature comprises following technological process, batch hydrolysis: add excessive water in the reaction vessel in advance, at the uniform velocity, quantitatively in water, throw in the aluminium phosphide pulvis, add aluminium phosphide 6kg metering by 50L water, temperature of reaction system remains on 25 ℃～80 ℃, adopts mechanical stirring or N
2Or CO
2Gas carries out continuously stirring to reaction soln, collect the phosphine gas that the aluminium phosphide hydrolysis reaction generates, reaction finishes, filtering reacting solution, filtrate cycle is used, filter cake in 60 ℃～300 ℃ common dryings or vacuum-drying or supercritical drying 2～12h, pulverizing after 400 ℃～1300 ℃ roasting 1～5h obtain aluminum oxide; Continuous hydrolysis process: in the ordinary-pressure hydrolysis tower, press the mass ratio 1: 3 of aluminium phosphide and water, from tower middle and upper part charging aluminium phosphide pulvis and the water vapour that feeds from the tower bottom side, under 20 ℃～120 ℃ tower temperature condition, carry out counter-current operation, realize the hydrolysis reaction of aluminium phosphide, at the overhead collection phosphine gas, reaction soln at the bottom of the filtration tank, filtrate cycle is used, filter cake 60 ℃～300 ℃ with common drying or vacuum-drying or supercritical drying 2～12h, pulverizing after 400 ℃～1300 ℃ roasting 1～5h obtain aluminum oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100203178A CN100337920C (en) | 2004-08-16 | 2004-08-16 | Method of preparing active aluminium oxide from aluminium phosphide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100203178A CN100337920C (en) | 2004-08-16 | 2004-08-16 | Method of preparing active aluminium oxide from aluminium phosphide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1597522A CN1597522A (en) | 2005-03-23 |
| CN100337920C true CN100337920C (en) | 2007-09-19 |
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ID=34663197
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|---|---|---|---|
| CNB2004100203178A Expired - Fee Related CN100337920C (en) | 2004-08-16 | 2004-08-16 | Method of preparing active aluminium oxide from aluminium phosphide |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428836B (en) * | 2008-12-17 | 2011-02-02 | 天津大学 | Process and apparatus for producing active aluminum oxide with discontinuous fluidized bed aluminium phosphide hydrolysis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4333989A (en) * | 1974-10-26 | 1982-06-08 | Semiconductor Research Foundation | Sapphire single crystal substrate consisting essentially of Ga2 O.sub.3 |
| US5993981A (en) * | 1997-04-18 | 1999-11-30 | Raytheon Company | Broadband protective optical window coating |
| CN2402144Y (en) * | 2000-01-13 | 2000-10-25 | 沈美庆 | High-efficiency fumigant producing and delivery and dispensing device |
-
2004
- 2004-08-16 CN CNB2004100203178A patent/CN100337920C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4333989A (en) * | 1974-10-26 | 1982-06-08 | Semiconductor Research Foundation | Sapphire single crystal substrate consisting essentially of Ga2 O.sub.3 |
| US5993981A (en) * | 1997-04-18 | 1999-11-30 | Raytheon Company | Broadband protective optical window coating |
| CN2402144Y (en) * | 2000-01-13 | 2000-10-25 | 沈美庆 | High-efficiency fumigant producing and delivery and dispensing device |
Non-Patent Citations (1)
| Title |
|---|
| 磷化氢熏蒸剂的研究进展 翟燕萍等，化学工业与工程，第20卷第4期 2003 * |
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|---|---|
| CN1597522A (en) | 2005-03-23 |
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Assignee: Linhai Bondlye Motor Vehicle Environmental Technology Co., Ltd. Assignor: Tianjin University Contract fulfillment period: 2007.12.1 to 2014.12.1 contract change Contract record no.: 2009330001705 Denomination of invention: Method of preparing active aluminium oxide from aluminium phosphide Granted publication date: 20070919 License type: Exclusive license Record date: 2009.7.27 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.12.1 TO 2014.12.1; CHANGE OF CONTRACT Name of requester: LINHAI CITY BONDLYE CAR ENVIRONMENT PROTECTION TEC Effective date: 20090727 |
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Granted publication date: 20070919 Termination date: 20120816 |