CN1286726C - Preparation of pseudo thinolite - Google Patents
Preparation of pseudo thinolite Download PDFInfo
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- CN1286726C CN1286726C CN 200410024185 CN200410024185A CN1286726C CN 1286726 C CN1286726 C CN 1286726C CN 200410024185 CN200410024185 CN 200410024185 CN 200410024185 A CN200410024185 A CN 200410024185A CN 1286726 C CN1286726 C CN 1286726C
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- sodium aluminate
- carbonic acid
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 38
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 6
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 29
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 29
- 235000011089 carbon dioxide Nutrition 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 4
- 238000001640 fractional crystallisation Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 19
- 239000011148 porous material Substances 0.000 abstract description 17
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000009826 distribution Methods 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 7
- 239000001569 carbon dioxide Substances 0.000 abstract description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 5
- 229910052708 sodium Inorganic materials 0.000 abstract description 5
- 239000011734 sodium Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000012066 reaction slurry Substances 0.000 abstract 2
- 239000013078 crystal Substances 0.000 abstract 1
- 238000005194 fractionation Methods 0.000 abstract 1
- 238000005272 metallurgy Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 21
- 239000000047 product Substances 0.000 description 18
- 238000003763 carbonization Methods 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000005245 sintering Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 238000006386 neutralization reaction Methods 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005255 carburizing Methods 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
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Abstract
The present invention relates to an improved method for preparing pseudo-boehmite, which belongs to the technical field of preparing non-metallurgy aluminum oxides. The present invention comprises: carbonating decomposition is carried out for solution of sodium metaaluminate, fractionation is carried out for reaction slurry, and fractional crystals are cleaned, dried and treated to obtain products. The present invention is characterized in that the control of the carbonating decomposition of the solution of sodium metaaluminate comprises: the solution of sodium metaaluminate is added into water into which carbon dioxide is induced, the pH value of the solution is controlled by controlling the flow of the carbon dioxide, the flow of the carbon dioxide is increased immediately after the addition of the solution of sodium metaaluminate to make the pH value of the solution drop to 9.5 to 10.5 so as to obtain the reaction slurry. With the present invention, the variation range of the pH value in the carbonating and gelatinizing process is small, the gelatinizing time is short, obtained pseudo-boehmite particles are uniform, the pore size distribution is centralized, and meanwhile, the product yield is increased; the present invention has simple preparation process, easy implementation and operation, combination with the actual production of aluminum oxides, no waste exhausting in the production process, environmental protection and easy popularization and application.
Description
Technical field
The present invention relates to a kind of preparation method of improved pseudo-boehmite, belong to the preparing technical field of non-metallurgical aluminum oxide.
Background technology
Pseudo-boehmite belongs to the incomplete boehmite of crystallization, and its performance is just closely related with its crystallization degree.
The method of producing pseudo-boehmite is a lot, is divided into aluminium alcoholates hydrolysis method and neutralisation generally.Adopt sodium aluminate solution and carbon dioxide reaction to generate the method for pseudo-boehmite, can be regarded as and adopt the neutralisation of carbonic acid gas as acid source, the difference of it and neutralisation is that reaction process can not carried out under acidic conditions.Sodium metaaluminate-carbonic acid gas (carborization) is produced pseudo-boehmite, relatively be fit to graft in aluminum oxide, the particularly production of alumina by sintering, because raw material sources are convenient, the by product of production process, waste liquid etc. can return the Production Flow Chart of aluminum oxide and reuse, whole process of preparation does not have the discharge of other material, is " green " industry.
The Carbonization Preparation pseudo-boehmite has comprised following chemical reaction:
Formula (1)～formula (5) formula has related to the formation mechanism of carborization pseudo-boehmite, they additions, obtains a net reaction:
(6)
Formula (6) is exactly the reaction formula of Carbonization Preparation pseudo-boehmite.
The Carbonization Preparation pseudo-boehmite is divided into carborization and two modes of continuous carbonization method of being interrupted.Be interrupted carborization and be meant that sodium aluminate solution forms towards rare, steps such as carbonization is decomposed, aging or aging, separating, washing, drying and crushing through cooling, filtering.The pH value of carbonization decomposition course control reaction end is between 9～12, because the pH value of reaction process progressively reduces, the time that the feasible pseudo-boehmite particle that forms stops in reaction solution is inconsistent, and the formation of pseudo-boehmite particle has run through entire reaction course.Like this, particle that carburizing reagent forms in earlier stage and the performance generation difference of decomposing the particle that forms when finishing, the pore size distribution that causes final pseudo-boehmite product is not very concentrated than disperse; The continuous carbonization method is to enter reactor continuously to certain density sodium aluminate solution towards rare, the control residence time, obtain the pseudo-boehmite product continuously, and the pH value of control reaction system also is between 9～12.This method, because the residence time is meant mean residence time, the stop of some single pseudo-boehmite particle might depart from far away this time in the reaction system, also can cause the difference of the performance of these particles, and the pore size distribution that is reacted to the pseudo-boehmite product is not very concentrated.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of pseudo-boehmite of the pore size distribution scattering problem that solves pseudo-boehmite.
The preparation method of pseudo-boehmite of the present invention, sodium aluminate solution is carried out carbonating to be decomposed, reacting slurry is separated, fractional crystallization is got product through washing, dry aftertreatment, what its sodium aluminate solution carbonating was decomposed is controlled to be: add sodium aluminate solution in the water that feeds carbonic acid gas, the pH value of controlling solution by the air flow of control carbonic acid gas is 10～13, preferred 10.5～12.5, best 11～12, after interpolation finishes, increase rapidly the air flow of carbonic acid gas, making the pH value of solution reduce to 9.5～10.5 rapidly must reacting slurry.
Increase the carbonic acid gas air flow, make the pH value of reacting slurry in 4～12 minutes, reduce to 9.5～10.5.
Among the present invention:
The used sodium aluminate solution of the present invention can be the solution of any concentration, and it is good, convenient and practical especially selecting the product in the industrial alumina by sintering production for use, and its concentration is Al
2O
3Content 70～200g/l, preferred 70～180g/l, best 90～150g/l, causticity is 1.1～1.8 than (molecular ratio of sodium oxide and aluminum oxide), preferred 1.2～1.7, best 1.3～1.6.
The interpolation time of sodium aluminate solution is controlled to be 0.5～10 minute, best 4～8 minutes.
The control of used carbon dioxide requires selected getting final product according to the carbonating control in present technique field, can be that volumetric concentration is 10～50% industrial gas mixture, it also can be pure carbon dioxide, can be that to be deployed into volumetric concentration with pressurized air be any concentration more than 20%, preferred 30～90%, the best 35～60%, the feeding of carbon dioxide can also be played the effect of pneumatic blending when satisfying the participation reaction.Equally, material temperature and carbonating decomposition reaction temperature get final product according to the popular response situation, as: the temperature of water is 10～35 ℃, and the temperature of sodium aluminate solution is controlled to be 5～60 ℃, preferred 10～35 ℃.
The AUTOSORB low temperature n2 absorption apparatus of the U.S. is adopted in the test of the pore volume of pseudo-boehmite product of the present invention, specific surface area, pore size distribution.
The present invention is compared with prior art:
Carbonization of the present invention becomes the pH value variation range of glue process to diminish, and gelation time is short, and the pseudo-boehmite particle that obtains is even, and pore size distribution is concentrated, and also helps improving simultaneously the production capacity of product.And technology is simple, and easy implementation and operation combines the production reality of aluminum oxide again, has reached the production process no waste and has discharged, and environmental protection is beneficial to and applies.
Description of drawings
Fig. 1, product of the present invention and ordinary method product pore size distribution comparison diagram.
Among the figure: 1, the product pore size distribution curve 2 that obtains of the present invention, the product pore size distribution curve that ordinary method obtains.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Get the sodium aluminate solution in the alumina by sintering production, the concentration of this solution is Al
2O
3Content 110g/l, causticity is filtered than 1.45, and cooling is standby.
In the 5L reactor, add the 2L temperature and be 15 ℃, pH value and be 7 deionized water, feeding volumetric concentration from reactor bottom is 50% carbonic acid gas, be 23 ℃ above-mentioned sodium aluminate solution immediately to reactor adding 400ml temperature, added in 4.5 minutes that this moment, the pH value of reaction system was 11.0, increase air flow rapidly, make to be reflected at and reduce to pH value 9.5 in 6 minutes, separate, with 80 ℃ deionized water wash three times, 110 ℃ of oven dry obtain pseudo-boehmite.Product pore volume 1.106ml/g, specific surface area 406.4m
2/ g, the hole 92.5% between 40～150 dusts.
According to the method for embodiment 1, different is the sodium aluminate solution that begins to add 500ml behind the feeding carbonic acid gas, adds in 6 minutes, this moment, the pH value of reaction system was 11.4, increase the carbonic acid gas air flow, make to be reflected at and reduce to pH value 9.8 in 8 minutes, obtain pseudo-boehmite.Product pore volume 1.080ml/g, specific surface area 396.0m
2/ g, the hole 91.4% between 40～150 dusts.
Embodiment 3
According to the method for embodiment 1, different is the sodium aluminate solution that begins to add 800ml behind the feeding carbonic acid gas, adds in 7.5 minutes, this moment, the pH value of reaction system was 12.0, increase the carbonic acid gas air flow, make to be reflected at and reduce to pH value 10.2 in 10 minutes, obtain pseudo-boehmite.Product pore volume 0.995ml/g, specific surface area 385.6m
2/ g, the hole 88.9% between 40～150 dusts.
Embodiment 4
Method according to embodiment 1, different is adds the washing lotion that the pH value is 7.5 pseudo-boehmite in the reactor, begin to add the sodium aluminate solution of 700ml behind the feeding carbonic acid gas, added in 6 minutes, this moment, the pH value of reaction system was 11.8, increase the carbonic acid gas air flow, make to be reflected at and reduce to pH value 10.5 in 9 minutes, obtain pseudo-boehmite 4.Product pore volume 1.032ml/g, specific surface area 392.7m
2/ g, the hole 93.7% between 40～150 dusts.
Embodiment 5
Get sintering process aluminium hydroxide, being dissolved into concentration with caustic solution is Al
2O
3Content 140g/l, causticity is filtered than 1.31, and cooling is standby.
In the 5L reactor, add the 2L temperature and be 15 ℃, pH value and be 7 deionized water, feeding volumetric concentration from reactor bottom is 40% carbonic acid gas, be 20 ℃ above-mentioned sodium aluminate solution immediately to reactor adding 300ml temperature, added in 4 minutes, this moment, the pH value of reaction system was 11.0, increase air flow rapidly, make to be reflected at and reduce to pH value 9.5 in 5 minutes.From, with 80 ℃ deionized water wash three times, 110 ℃ of oven dry obtain pseudo-boehmite 5.Product pore volume 1.146ml/g, specific surface area 412.2m
2/ g, the hole 90.1% between 40～150 dusts.
According to the method for embodiment 5, the volumetric concentration that different is feeds carbonic acid gas is 51%, and the 500ml sodium aluminate solution added in 5.5 minutes, this moment reaction system pH value 11.2, increase air flow, make to be reflected at and reduce to pH value 9.8 in 8 minutes, obtain pseudo-boehmite.Product pore volume 1.075ml/g, specific surface area 395.9m
2/ g, the hole 89.8% between 40～150 dusts.
Embodiment 7
According to the method for embodiment 5, the volumetric concentration that different is feeds carbonic acid gas is 60%, and the 700ml sodium aluminate solution added in 6.5 minutes, this moment reaction system pH value 11.5, increase air flow, make to be reflected at and reduce to pH value 10.0 in 8.5 minutes, obtain pseudo-boehmite.Product pore volume 0.970ml/g, specific surface area 386.4m
2/ g, the hole 89.0% between 40～150 dusts.
Embodiment 8
Get the sodium aluminate solution in the alumina by sintering production, the concentration of this solution is Al
2O
3Content 150g/l, causticity is filtered than 1.5, and cooling is standby.
Adding 2L temperature is 15 ℃ a deionized water in the 5L reactor, feeding volumetric concentration from reactor bottom is 35% carbonic acid gas, be 23 ℃ above-mentioned sodium aluminate solution immediately to reactor adding 400ml temperature, added in 6 minutes that this moment, the pH value of reaction system was 11.0, increase air flow rapidly, make to be reflected at and reduce to pH value 9.5 in 7 minutes, separate, with 80 ℃ deionized water wash three times, 105 ℃ of oven dry obtain pseudo-boehmite.
Embodiment 9
Get the sodium aluminate solution in the alumina by sintering production, the concentration of this solution is Al
2O
3Content 90g/l, causticity is filtered than 1.45, and cooling is standby.
The deionized water that in the 5L reactor, adds 2L, feeding volumetric concentration from reactor bottom is 55% carbonic acid gas, be 20 ℃ above-mentioned sodium aluminate solution immediately to reactor adding 400ml temperature, added in 5 minutes that this moment, the pH value of reaction system was 11.5, increase air flow rapidly, make to be reflected at and reduce to pH value 10 in 9 minutes, separate, with 82 ℃ deionized water wash, 115 ℃ of oven dry obtain pseudo-boehmite.
Claims (9)
1, a kind of preparation method of pseudo-boehmite, sodium aluminate solution is carried out carbonating to be decomposed, reacting slurry is separated, fractional crystallization is got product through washing, dry aftertreatment, it is characterized in that being controlled to be of sodium aluminate solution carbonating decomposition: in the water that feeds carbonic acid gas, add sodium aluminate solution, the pH value of controlling solution by the air flow of control carbonic acid gas is 10～13, after interpolation finishes, increase rapidly the air flow of carbonic acid gas, making the pH value of solution reduce to 9.5～10.5 rapidly must reacting slurry.
2, preparation method according to claim 1 is characterized in that adding sodium aluminate solution in the water that feeds carbonic acid gas, and the pH value of controlling solution by the air flow of control carbonic acid gas is 11～12.
3, preparation method according to claim 1 is characterized in that increasing the carbonic acid gas air flow, makes the pH value of reacting slurry reduce to 9.5～10.5 in 4～12 minutes.
4, according to claim 1,2 or 3 described preparation methods, the concentration that it is characterized in that sodium aluminate solution is Al
2O
3Content 70～200g/l, the causticity ratio is 1.1～1.8.
5, preparation method according to claim 4, the concentration that it is characterized in that sodium aluminate solution is Al
2O
3Content 90～150g/l, the causticity ratio is 1.3～1.6.
6, preparation method according to claim 4, the interpolation time that it is characterized in that sodium aluminate solution is 0.5～10 minute.
7, preparation method according to claim 6, the interpolation time that it is characterized in that sodium aluminate solution is 4～8 minutes.
8, preparation method according to claim 1, the gas volume concentration that it is characterized in that carbonic acid gas is 35～60%.
9, preparation method according to claim 1 is characterized in that carbonating decomposition reaction temperature is 10～35 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410024185 CN1286726C (en) | 2004-06-03 | 2004-06-03 | Preparation of pseudo thinolite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410024185 CN1286726C (en) | 2004-06-03 | 2004-06-03 | Preparation of pseudo thinolite |
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| Publication Number | Publication Date |
|---|---|
| CN1583568A CN1583568A (en) | 2005-02-23 |
| CN1286726C true CN1286726C (en) | 2006-11-29 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348493C (en) * | 2005-05-10 | 2007-11-14 | 中国石油天然气股份有限公司 | Preparation tech. for producing pseudoboehmite |
| CN100363261C (en) * | 2006-06-22 | 2008-01-23 | 武汉理工大学 | Method for preparing pseudo-boehmite with large pore volume and high specific surface area |
| CN100457626C (en) * | 2006-12-18 | 2009-02-04 | 天津理工大学 | Prepn process of quasi-crystal and micron crystal pseudoboehmite |
| CN103449485B (en) * | 2013-08-23 | 2015-09-02 | 中国铝业股份有限公司 | A kind of method utilizing ejector continuous seepage pseudo-boehmite |
| CN103449484B (en) * | 2013-08-23 | 2015-07-08 | 中国铝业股份有限公司 | Method for continuously producing pseudoboehmite |
| CN105347374B (en) * | 2015-11-20 | 2017-05-24 | 中国石油化工股份有限公司 | production method of pseudo-boehmite |
| CN106946278B (en) * | 2016-01-07 | 2019-01-25 | 中国石油化工股份有限公司 | A kind of boehmite and preparation method thereof |
| CN108910924B (en) * | 2018-09-11 | 2020-07-31 | 淄博齐茂催化剂有限公司 | Precipitation energy-saving preparation method of pseudo-boehmite |
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