CN104973613A - Method for continuously producing aluminum oxide by using carbonation method - Google Patents
Method for continuously producing aluminum oxide by using carbonation method Download PDFInfo
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- CN104973613A CN104973613A CN201510355201.8A CN201510355201A CN104973613A CN 104973613 A CN104973613 A CN 104973613A CN 201510355201 A CN201510355201 A CN 201510355201A CN 104973613 A CN104973613 A CN 104973613A
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- aluminum oxide
- carborization
- continuous seepage
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Abstract
A method for continuously producing aluminum oxide by using a carbonation method relates to aluminum oxide. The method comprises the following steps of: (1) continuously adding a sodium metaaluminate solution into a reaction device, introducing mixed gas of air and carbon dioxide and carrying out gel forming to obtain slurry with the pH value of 9-12; and (2) carrying out aging on the slurry obtained by the step (1) and carrying out solid-liquid separation, and drying and baking an obtained solid to obtain the aluminum oxide. The sodium metaaluminate solution is continuously added into the reaction device so that the gas and the liquid are in sufficient contact, and the defect of using an interval method to produce the aluminum oxide is overcome. The preparation method has the advantages of stable production process, high production efficiency, low cost, easiness of washing a device and the like; and the prepared aluminum oxide has a large specific surface area and a suitable pore capacity.
Description
Technical field
The present invention relates to aluminum oxide, particularly a kind of method adopting carborization continuous seepage aluminum oxide.
Background technology
Aluminum oxide, also known as aluminium sesquioxide, is a kind of porous solid material, has the features such as specific surface area is high, pore volume large, pore distribution controllable, physical strength are high, Heat stability is good, in catalytic field, is commonly used for support of the catalyst.The method of industrial production aluminum oxide comprises aluminate or aluminium salt precipitation method, aluminium salt neutralisation, aluminium alcoholates hydrolysis method, carborization etc., and wherein carborization preparation technology equipment requirements is low, route is simple, with low cost, environment friendly and pollution-free.Current carborization is prepared on aluminum oxide technology more ripe, the open carborization in Chinese patent CN1250746A such as Yang Qinghe prepares aluminum oxide, the aluminum oxide that pore volume is 0.5 ~ 2.0mL/g can be prepared, but need to add alkaline matter regulation and control pH extraly after stopping plastic, comparatively loaded down with trivial details, and the specific surface area of products obtained therefrom and pore volume are not concentrated, fluctuate larger; The open carborization in Chinese patent CN1583568A such as Yuan Chongliang prepares aluminum oxide, and need pass into carbon dioxide at twice to regulate and control the pH change of solution, process is comparatively loaded down with trivial details, is not easy to control; The open carborization in Chinese patent CN101665262A such as Liu Yandong prepares aluminum oxide, and described method need add seed precipitation solution or plant point washing lotion in slurries, and process is comparatively complicated.
Above-mentioned aluminum oxide industry preparation method often adopts interrupter method, and processing unit falls behind, CO
2specific absorption is low, and preparation cycle is longer, and quality product fluctuation is large, constrains the development of enterprise to scale operation direction.
Summary of the invention
The object of the invention is to overcome prior art above shortcomings, a kind of a kind of method adopting carborization continuous seepage aluminum oxide that production efficiency is high, stable production process, technique are simple, with low cost is provided.
Adopt a method for carborization continuous seepage aluminum oxide, comprise the following steps:
1) sodium aluminate solution is joined in reaction unit continuously, pass into air and carbon dioxide gas mixture, carry out plastic, obtain the slurries that pH value is 9 ~ 12;
2) by step 1) gained slurries carry out aging rear solid-liquid separation, by gained solid drying, roasting, obtain aluminum oxide.
In step 1) in, described being joined continuously in reaction unit by sodium aluminate solution is joined continuously in reaction unit by sodium aluminate solution by volume pump; The mass concentration of described sodium aluminate solution can be 15 ~ 80g/L by aluminum oxide, preferably 20 ~ 50g/L; Described sodium aluminate solution also can add auxiliary element, and described auxiliary element can be selected from least one in phosphorus, silicon, boron, titanium, zirconium etc.; Described reaction unit can adopt glass sphere, and described glass sphere is provided with liquid-inlet, product exit, enterprising gas port, lower inlet mouth, circulating water outlet, circulating water intake; The described air that passes into can be with the method for carbon dioxide gas mixture and by described reaction unit, air is contacted with sodium aluminate solution with carbon dioxide gas mixture at the same time or separately; The flow ratio of described mixed gas and sodium aluminate solution can be 50 ~ 100, in described air and carbon dioxide gas mixture, the volume fraction of carbonic acid gas can be 20% ~ 100%, the pressure of air and carbon dioxide gas mixture can be 0.1 ~ 2MPa, preferably 0.1 ~ 0.5MPa; The temperature of described plastic can be 20 ~ 90 DEG C, preferably 30 ~ 50 DEG C.
In step (2), described aging temperature can be 20 ~ 120 DEG C, preferably 40 ~ 60 DEG C; The temperature of described roasting can be 500 ~ 900 DEG C, and the time of described roasting can be 2 ~ 6h; The temperature of described roasting is preferably 550 ~ 700 DEG C, and the time of described roasting is preferably 3 ~ 5h.
The present invention, by being joined continuously in reaction unit by sodium aluminate solution, makes gas-liquid fully contact, and overcomes the defect that interrupter method produces aluminum oxide.The present invention has that stable production process, production efficiency are high, with low cost, device is easy to the advantages such as cleaning, and the alumina ratio surface-area prepared is large, pore volume is suitable for.
Accompanying drawing explanation
Fig. 1 is the reaction unit schematic diagram of the embodiment of the present invention.In FIG, be respectively labeled as: 1, liquid-inlet; 2, product exit; 3, enterprising gas port; 4, lower inlet mouth; 5, circulating water outlet; 6, circulating water intake.
The XRD figure of the aluminum oxide of Fig. 2 prepared by embodiment of the present invention 1-.
Embodiment
Following examples will the present invention will be further described by reference to the accompanying drawings.Adopt the reaction unit that Fig. 1 provides.
Embodiment 1
The sodium aluminate solution by aluminum oxide concentration being 15g/L is joined in reaction unit by liquid-inlet 1 by volume pump continuously; Air and carbon dioxide gas mixture is passed into from enterprising gas port 3, the volume fraction of carbon dioxide in gas mixture is 40%, the pressure of mixed gas is 0.1MPa, by reaction unit, gas-liquid is fully contacted, controlling gas-liquid flow ratio is 50, gas-to-liquid contact temperature is 25 DEG C and pH stops plastic when being 9.50, and product aging temperature is 25 DEG C; Slurry with water after aging is washed till neutrality, then filter cake is carried out drying, temperature is 40 DEG C.Dried product exhibited carries out roasting, and maturing temperature is 550 DEG C, and roasting time is 3h, finally obtains aluminum oxide.Its physico-chemical property is in table 1.
Embodiment 2
The sodium aluminate solution by aluminum oxide concentration being 25g/L is joined in reaction unit by liquid-inlet 1 by volume pump continuously, the mixed gas of air and carbonic acid gas is passed into from lower inlet mouth 4, the volume fraction of carbon dioxide in gas mixture is 40%, the pressure of mixed gas is 0.1MPa, by reaction unit, gas-liquid is fully contacted, controlling gas-liquid flow ratio is 60, and gas-to-liquid contact temperature is 40 DEG C and pH stops plastic when being 9.50, and product aging temperature is 40 DEG C; Slurry with water after aging is washed till neutrality, then filter cake is carried out drying, temperature is 60 DEG C.Dried product exhibited carries out roasting, and maturing temperature is 550 DEG C, and roasting time is 4h, finally obtains aluminum oxide.Its physico-chemical property is in table 1.
Embodiment 3
The sodium aluminate solution by aluminum oxide concentration being 35g/L is joined in reaction unit by liquid-inlet 1 by volume pump continuously, the mixed gas of air and carbonic acid gas is passed into from lower inlet mouth 4, the volume fraction of carbon dioxide in gas mixture is 40%, the pressure of mixed gas is 0.1MPa, by reaction unit, gas-liquid is fully contacted, controlling gas-liquid flow ratio is 70, and gas-to-liquid contact temperature is 60 DEG C and pH stops plastic when being 10.0, and product aging temperature is 60 DEG C; Slurry with water after aging is washed till neutrality, then filter cake is carried out drying, temperature is 80 DEG C.Dried product exhibited carries out roasting, and maturing temperature is 550 DEG C, and roasting time is 3h, finally obtains aluminum oxide.Its physico-chemical property is in table 1.
Embodiment 4
The sodium aluminate solution by aluminum oxide concentration being 45g/L is joined in reaction unit by liquid-inlet 1 by volume pump continuously, the mixed gas of air and carbonic acid gas is passed into from lower inlet mouth 4, the volume fraction of carbon dioxide in gas mixture is 99%, the pressure of mixed gas is 0.3MPa, by reaction unit, gas-liquid is fully contacted, controlling gas-liquid flow ratio is 80, and gas-to-liquid contact temperature is 60 DEG C and pH stops plastic when being 10.5, and product aging temperature is 60 DEG C; Slurry with water after aging is washed till neutrality, then filter cake is carried out drying, temperature is 100 DEG C.Dried product exhibited carries out roasting, and maturing temperature is 550 DEG C, and roasting time is 3h, finally obtains aluminum oxide.Its physico-chemical property is in table 1.
Embodiment 5
The sodium aluminate solution by aluminum oxide concentration being 55g/L is joined in reaction unit by liquid-inlet 1 by volume pump continuously, the mixed gas of air and carbonic acid gas is passed into from lower inlet mouth 4, the volume fraction of carbon dioxide in gas mixture is 99%, the pressure of mixed gas is 0.5MPa, by reaction unit, gas-liquid is fully contacted, controlling gas-liquid flow ratio is 100, and gas-to-liquid contact temperature is 60 DEG C and pH stops plastic when being 11.00, and product aging temperature is 60 DEG C; Slurry with water after aging is washed till neutrality, then filter cake is carried out drying, temperature is 120 DEG C.Dried product exhibited carries out roasting, and maturing temperature is 550 DEG C, and roasting time is 3h, finally obtains aluminum oxide.Its physico-chemical property is in table 1.
Embodiment 6
The sodium aluminate solution by aluminum oxide concentration being 65g/L is joined in reaction unit by liquid-inlet 1 by volume pump continuously, the mixed gas of air and carbonic acid gas is passed into from lower inlet mouth 4, the volume fraction of carbon dioxide in gas mixture is 99%, the pressure of mixed gas is 2MPa, by glass sphere, gas-liquid is fully contacted, control gas-liquid flow ratio 100, gas-to-liquid contact temperature is 60 DEG C and pH stops plastic when being 11.00, and product aging temperature is 60 DEG C; Slurry with water after aging is washed till neutrality, then filter cake is carried out drying, temperature is 120 DEG C.Dried product exhibited carries out roasting, and maturing temperature is 550 DEG C, and roasting time is 3 hours, finally obtains aluminum oxide.Its physico-chemical property is in table 1.
Embodiment 7
To be the sodium aluminate solution of 45g/L and the sodium silicate solution equal-volume mixing of 27.5g/L by aluminum oxide concentration, join in reaction unit by liquid-inlet 1 continuously by volume pump, the mixed gas of air and carbonic acid gas is passed into from lower inlet mouth 4, the volume fraction of carbon dioxide in gas mixture is 99%, the pressure of mixed gas is 0.3MPa, by reaction unit, gas-liquid is fully contacted, controlling gas-liquid flow ratio is 80, gas-to-liquid contact temperature is 60 DEG C and pH stops plastic when being 10.50, and product aging temperature is 60 DEG C; Slurry with water after aging is washed till neutrality, then filter cake is carried out drying, temperature is 120 DEG C.Dried product exhibited carries out roasting, and maturing temperature is 550 DEG C, and roasting time is 3h, finally obtains aluminum oxide.Its physico-chemical property is in table 1.
Comparative example 1
Interrupter method is used to prepare aluminum oxide with reference to method disclosed in Chinese patent CN02158286.The sodium aluminate solution by aluminum oxide concentration being 35g/L is placed in reactor, the mixed gas of air and carbonic acid gas is passed into bottom reactor, the volume fraction of carbon dioxide in gas mixture is 40%, the pressure of mixed gas is 0.1MPa, to control solution temperature be 60 DEG C and pH stops plastic when being 10.0, and product aging temperature is 60 DEG C; Slurry with water after aging is washed till neutrality, then filter cake is carried out drying, temperature is 120 DEG C.Dried product exhibited carries out roasting, and maturing temperature is 550 DEG C, and roasting time is 3h, finally obtains aluminum oxide.Its physico-chemical property is in table 1.
Table 1
| Embodiment/comparative example | Specific surface area (m 2/g) | Pore volume (ml/g) |
| Embodiment 1 | 287 | 0.68 |
| Embodiment 2 | 320 | 0.62 |
| Embodiment 3 | 275 | 0.75 |
| Embodiment 4 | 330 | 0.57 |
| Embodiment 5 | 280 | 0.60 |
| Embodiment 6 | 297 | 0.65 |
| Embodiment 7 | 340 | 0.67 |
| Comparative example 1 | 268 | 0.55 |
As can be seen from Table 1, by the aluminum oxide prepared by the present invention, the aluminum oxide that specific surface area and pore volume all prepare than comparative example 1 is large.
Claims (10)
1. adopt a method for carborization continuous seepage aluminum oxide, it is characterized in that comprising the following steps:
1) sodium aluminate solution is joined in reaction unit continuously, pass into air and carbon dioxide gas mixture, carry out plastic, obtain the slurries that pH value is 9 ~ 12;
2) by step 1) gained slurries carry out aging rear solid-liquid separation, by gained solid drying, roasting, obtain aluminum oxide.
2. a kind of method adopting carborization continuous seepage aluminum oxide as claimed in claim 1, it is characterized in that in step 1) in, described being joined continuously in reaction unit by sodium aluminate solution is joined continuously in reaction unit by sodium aluminate solution by volume pump.
3. a kind of method adopting carborization continuous seepage aluminum oxide as claimed in claim 1, is characterized in that in step 1) in, the mass concentration of described sodium aluminate solution counts 15 ~ 80g/L by aluminum oxide, preferably 20 ~ 50g/L.
4. a kind of method adopting carborization continuous seepage aluminum oxide as claimed in claim 1, is characterized in that in step 1) in, described sodium aluminate solution also adds auxiliary element, and described auxiliary element can be selected from least one in phosphorus, silicon, boron, titanium, zirconium.
5. a kind of method adopting carborization continuous seepage aluminum oxide as claimed in claim 1, it is characterized in that in step 1) in, described reaction unit adopts glass sphere, and described glass sphere is provided with liquid-inlet, product exit, enterprising gas port, lower inlet mouth, circulating water outlet, circulating water intake.
6. a kind of method adopting carborization continuous seepage aluminum oxide as claimed in claim 1, it is characterized in that in step 1) in, described in pass into the method for air and carbon dioxide gas mixture for make air contact with sodium aluminate solution with carbon dioxide gas mixture by described reaction unit at the same time or separately.
7. a kind of method adopting carborization continuous seepage aluminum oxide as claimed in claim 1, it is characterized in that in step 1) in, the flow ratio of described mixed gas and sodium aluminate solution is 50 ~ 100, in described air and carbon dioxide gas mixture, the volume fraction of carbonic acid gas can be 20% ~ 100%, the pressure of air and carbon dioxide gas mixture can be 0.1 ~ 2MPa, preferably 0.1 ~ 0.5MPa.
8. a kind of method adopting carborization continuous seepage aluminum oxide as claimed in claim 1, is characterized in that in step 1) in, the temperature of described plastic is 20 ~ 90 DEG C, preferably 30 ~ 50 DEG C.
9. a kind of method adopting carborization continuous seepage aluminum oxide as claimed in claim 1, is characterized in that in step 2) in, described aging temperature is 20 ~ 120 DEG C, preferably 40 ~ 60 DEG C.
10. a kind of method adopting carborization continuous seepage aluminum oxide as claimed in claim 1, is characterized in that in step 2) in, the temperature of described roasting is 500 ~ 900 DEG C, and the time of described roasting is 2 ~ 6h; The temperature of described roasting is preferably 550 ~ 700 DEG C, and the time of described roasting is preferably 3 ~ 5h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114426298A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | System for carbonization method preparation aluminium hydroxide and carbonization reactor thereof |
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| CN1485275A (en) * | 2003-09-02 | 2004-03-31 | 中国铝业股份有限公司 | Continuously carbonation decompsition process for preparing sand-shape alumina |
| JP4021513B2 (en) * | 1997-02-21 | 2007-12-12 | 水澤化学工業株式会社 | Alumina or alumina hydrate having ultra-low bulk density, high specific surface area, and high porosity, production method and use thereof |
| CN102139204A (en) * | 2010-02-03 | 2011-08-03 | 中国石油天然气股份有限公司 | Pseudo-boehmite containing amorphous silica-alumina and preparation method thereof |
| CN103449484A (en) * | 2013-08-23 | 2013-12-18 | 中国铝业股份有限公司 | Method for continuously producing pseudoboehmite |
| CN102807242B (en) * | 2012-08-22 | 2014-09-10 | 中国铝业股份有限公司 | Method for producing aluminium hydroxide micro powder by continuous decomposition |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4021513B2 (en) * | 1997-02-21 | 2007-12-12 | 水澤化学工業株式会社 | Alumina or alumina hydrate having ultra-low bulk density, high specific surface area, and high porosity, production method and use thereof |
| CN1485275A (en) * | 2003-09-02 | 2004-03-31 | 中国铝业股份有限公司 | Continuously carbonation decompsition process for preparing sand-shape alumina |
| CN102139204A (en) * | 2010-02-03 | 2011-08-03 | 中国石油天然气股份有限公司 | Pseudo-boehmite containing amorphous silica-alumina and preparation method thereof |
| CN102807242B (en) * | 2012-08-22 | 2014-09-10 | 中国铝业股份有限公司 | Method for producing aluminium hydroxide micro powder by continuous decomposition |
| CN103449484A (en) * | 2013-08-23 | 2013-12-18 | 中国铝业股份有限公司 | Method for continuously producing pseudoboehmite |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114426298A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | System for carbonization method preparation aluminium hydroxide and carbonization reactor thereof |
| CN114426298B (en) * | 2020-10-29 | 2023-08-01 | 中国石油化工股份有限公司 | System for preparing aluminum hydroxide by carbonization method and carbonization reactor thereof |
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