CN105645446B - Carbonation method prepares the aging method of boehmite - Google Patents
Carbonation method prepares the aging method of boehmite Download PDFInfo
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- CN105645446B CN105645446B CN201610171887.XA CN201610171887A CN105645446B CN 105645446 B CN105645446 B CN 105645446B CN 201610171887 A CN201610171887 A CN 201610171887A CN 105645446 B CN105645446 B CN 105645446B
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- boehmite
- aging
- carbonation
- prepares
- filter cake
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- 238000000034 method Methods 0.000 title claims abstract description 71
- 230000032683 aging Effects 0.000 title claims abstract description 41
- 229910001593 boehmite Inorganic materials 0.000 title claims abstract description 28
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 title claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 22
- 239000012065 filter cake Substances 0.000 claims abstract description 12
- 239000004033 plastic Substances 0.000 claims abstract description 9
- 229920003023 plastic Polymers 0.000 claims abstract description 9
- 239000012452 mother liquor Substances 0.000 claims abstract description 3
- 239000002002 slurry Substances 0.000 claims description 27
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 11
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 10
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 10
- 239000001569 carbon dioxide Substances 0.000 claims description 10
- 238000005260 corrosion Methods 0.000 claims description 10
- 230000007797 corrosion Effects 0.000 claims description 10
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 238000001879 gelation Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 24
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 239000012535 impurity Substances 0.000 abstract description 11
- 238000001935 peptisation Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000001035 drying Methods 0.000 description 10
- 239000003513 alkali Substances 0.000 description 9
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 6
- 235000011941 Tilia x europaea Nutrition 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000004571 lime Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000003483 aging Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 210000000038 chest Anatomy 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910001648 diaspore Inorganic materials 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000005360 mashing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
- C01F7/142—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent with carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The invention discloses the aging method that a kind of carbonation method prepares boehmite, it is specially：Carbonation method is prepared after boehmite plastic, and solid-liquor separation is carried out rapidly, then will be adhered to the filter cake of mother liquor, is fitted into closed container, heat ageing.The aging method of the present invention, technique is simple, and energy consumption is low, and production capacity is big, and production cost is low；Obtained boehmite product, crystalline phase is pure, crystallinity is high, peptization is good, impurity is few, widely used.
Description
Technical field
The present invention relates to the preparation method of boehmite, more particularly to a kind of carbonation method prepares the old of boehmite
Change method.
Background technology
The preparation method of boehmite is varied, and domestic alumina by sintering factory is prepared using carbonation method mostly to be intended
Boehmite because grafting is on alumina production process flow, raw material sources are convenient, during accessory substance, waste liquid etc. all
Closed cycle can be realized with returning alumina flow, so product cost is low, non-environmental-pollution.Prepared by carbonation method intends thin water aluminium
Stone technical process includes dispensing, plastic, aging, washing, solid-liquor separation, drying and other steps successively.
Carbonation method prepares the aging technology in boehmite technique, and domestic and international patent and relevant report are a lot, but all
Be carbonating plastic after slurries or preparation alkaline solution in carry out, be properly termed as slurries state aging.For example,
CN85100161 discloses a kind of preparation process of pseudoboehmite, and aging method therein is：Plastic rear slurry is then heated to
70~100 DEG C, it is subject to aging in washing process after insulation aging 1~6 hour, or first directly progress solid-liquor separation；
Aging method disclosed in CN100999328 is：Unbodied hydrated alumina, at least one water miscible alkali of hydration are mixed
Close, pulp, slurries were in 20 DEG C to 90 DEG C agings 0.5 to 6 hour；CN101172631, which discloses a kind of carbonation method and prepared, intends thin
The preparation method of diaspore, its aging method is：After plastic, slurries separation is carried out first, then add wash water to mix mashing filter cake
Temperature raising aging is carried out afterwards, and temperature is 70 DEG C to 100 DEG C, and ageing time is 3~6 hours.In these methods, because ageing process is
Temperature raising and insulation are carried out to whole slurry system, therefore to expend a large amount of heat energy, and temperature raising process is longer, easily causes final production
There is dephasign in product, so as to influence the performance of product.
The content of the invention
The technical problems to be solved by the invention are that the power consumption of existing aging technique is big, slurries temperature raising process is long, are easily caused
It is miscellaneous that there is provided the aging method that a kind of carbonation method prepares boehmite.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
Carbonation method prepares the aging method of boehmite, and carbonation method is prepared after boehmite plastic, entered rapidly
Row solid-liquor separation, then will adhere to the filter cake of mother liquor, is fitted into closed container, heat ageing.
Further, the closed container, it is desirable to high temperature resistant and acid and alkali-resistance, including polybag, glass container and stainless steel
Container.
Further, the heating, to directly heat or indirectly heat.
Further, the aging, temperature is 70-100 DEG C, and the time is 2-4h.
A kind of carbonation method that the present invention is provided prepares the aging method of boehmite, and technique is simple, energy-saving, carries
High production capacity, reduces production cost；Obtained boehmite product, crystalline phase is pure, crystallinity is high, peptization is good, impurity is few,
It is widely used as binding agent, dispersant, catalyst and catalyst support material.
Embodiment
A kind of carbonation method provided in an embodiment of the present invention prepares the aging method of boehmite, with soda lime sintering process
The sodium aluminate refined soln of production is raw material, adjusts its alumina content for 20-60g/l, and solution Crater corrosion is 1.3-1.6, is led to
Enter the industrial carbon dioxide gas that volumetric concentration is 30-40% and (may be from the centre that soda lime sintering process produces alumina technology
Product), gelation time 10-20min, plastic terminal slurry pH value 10-13 are controlled, obtained slurries are carried out rapidly to liquid and divided admittedly
From.The filter cake of separation is fitted into closed container, and closed container requires high temperature resistant, acid and alkali-resistance, including polybag, glass container, no
Become rusty steel container etc., to avoid adhering to mother liquid evaporation, then lifts temperature to 70-100 DEG C, can directly heat or indirectly heat, aging 2-
4h (can be described as the aging of solidification state).The filter cake of aging post processing, then stirred through hot water slurrying, washed repeatedly with 60-100 DEG C of hot water
After washing, dried through solid-liquor separation, using baking oven reinforcing drying or flash evaporation drying mode, produce boehmite product.
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
A kind of carbonation method that the embodiment of the present invention 1 is provided prepares the aging method of boehmite, specific as follows：With alkali
The sodium aluminate refined soln of lime sinter process production is raw material, adjusts its alumina content for 42g/l, Crater corrosion is 1.52, leads to
Enter the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 15 minutes, slurry pH value is 13, and obtained slurries are rapid
Carry out solid-liquor separation.The filter cake of separation loads sealing polybag, is put into after being incubated 2 hours in 70 DEG C of waters, adds 80 DEG C of hot water
Slurrying, carries out agitator treating removal of impurities repeatedly, and finally drying obtains qualified products in baking oven.Product index for details see attached table 1.
Embodiment 2
A kind of carbonation method that the embodiment of the present invention 2 is provided prepares the aging method of boehmite, specific as follows：With alkali
The sodium aluminate refined soln of lime sinter process production is raw material, adjusts its alumina content for 23g/l, Crater corrosion is 1.37, leads to
Enter the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 10.5 minutes, slurry pH value is 10.5, by obtained slurries
It is rapid to carry out solid-liquor separation.The filter cake of separation loads sealing polybag, is put into after being incubated 4 hours in 90 DEG C of waters, adds 75 DEG C
Hot water slurrying, carries out agitator treating removal of impurities repeatedly, and drying obtains qualified products in baking oven.Product index for details see attached table 1.
Embodiment 3
A kind of carbonation method that the embodiment of the present invention 3 is provided prepares the aging method of boehmite, specific as follows：With alkali
The sodium aluminate refined soln of lime sinter process production is raw material, adjusts its alumina content for 36g/l, Crater corrosion is 1.42, leads to
Enter the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 13 minutes, slurry pH value is 11, and obtained slurries are rapid
Carry out solid-liquor separation.The filter cake of separation is fitted into sealing flask, is put into after being incubated 3.5 hours in 95 DEG C of waters, adds 95 DEG C of heat
Aquation is starched, and carries out agitator treating removal of impurities repeatedly, and drying obtains qualified products in baking oven.Product index for details see attached table 1.
Embodiment 4
A kind of carbonation method that the embodiment of the present invention 4 is provided prepares the aging method of boehmite, specific as follows：With alkali
The sodium aluminate refined soln of lime sinter process production is raw material, adjusts its alumina content for 60g/l, Crater corrosion is 1.57, leads to
Enter the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 20 minutes, slurry pH value is 12, and obtained slurries are rapid
Carry out solid-liquor separation.The filter cake of separation is fitted into sealing flask, is put into after being incubated 3.5 hours in 95 DEG C of waters, adds 95 DEG C of heat
Aquation is starched, and carries out agitator treating removal of impurities repeatedly, and drying obtains qualified products in baking oven.Product index for details see attached table 1.
Embodiment 5
A kind of carbonation method that the embodiment of the present invention 5 is provided prepares the aging method of boehmite, specific as follows：With alkali
The sodium aluminate refined soln of lime sinter process production is raw material, adjusts its alumina content for 40g/l, Crater corrosion is 1.52, leads to
Enter the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 14 minutes, slurry pH value is 11.5, and obtained slurries are fast
Speed carries out solid-liquor separation.The filter cake of separation is fitted into sealing flask, is put into after being incubated 3 hours in 100 DEG C of steam chests, adds 85 DEG C
Hot water slurrying, carries out agitator treating removal of impurities repeatedly, and reinforcing is dried to obtain qualified products.
Embodiment 6
A kind of carbonation method that the embodiment of the present invention 6 is provided prepares the aging method of boehmite, specific as follows：With alkali
The sodium aluminate refined soln of lime sinter process production is raw material, adjusts its alumina content for 55g/l, Crater corrosion is 1.48, leads to
Enter the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 17 minutes, slurry pH value is 12.5, and obtained slurries are fast
Speed carries out solid-liquor separation.The filter cake of separation is fitted into stainless steel beaker with cover, is put into after 100 DEG C of steam chests are incubated 4 hours, adds
95 DEG C of hot water slurryings, carry out agitator treating removal of impurities repeatedly, and expansion drying obtains qualified products.Product index for details see attached table 1.
Comparative example 1~2 illustrates the boehmite property prepared without the aging method of the present invention.
Comparative example 1
A kind of carbonation method that comparative example 1 of the present invention is provided prepares the aging method of boehmite, is specially：With alkali stone
The sodium aluminate refined soln of grey sintering process production is raw material, adjusts its alumina content for 41g/l, Crater corrosion is 1.51, is passed through
Volumetric concentration is 30-40% industrial carbon dioxide gas, and after 15 minutes, slurry pH value is 11.5, by obtained carbonization slurries
85 DEG C are lifted temperature to, after being incubated 3 hours, solid-liquor separation is carried out, then 80 DEG C of hot water carry out agitator treating removal of impurities repeatedly, oven for drying
Obtain qualified products.Product index for details see attached table 1.
Comparative example 2
A kind of carbonation method that comparative example 2 of the present invention is provided prepares the aging method of boehmite, is specially：With alkali stone
The sodium aluminate refined soln of grey sintering process production is raw material, adjusts its alumina content for 50g/l, Crater corrosion is 1.46, is passed through
Volumetric concentration is 30-40% industrial carbon dioxide gas, and after 18 minutes, slurry pH value is 12, and obtained carbonization slurries are carried
Temperature is to 95 DEG C, after being incubated 3 hours, carries out solid-liquor separation, and then 80 DEG C of hot water carry out agitator treating removal of impurities repeatedly, and oven for drying is obtained
To qualified products.Product index for details see attached table 1.
As it can be seen from table 1 preparing the aging side of boehmite using 1-6 of the embodiment of the present invention carbonation methods provided
Product made from method, the miscellaneous content of its gibbsite is few, crystallinity is high, pore volume is big, and peptization performance is good, Na2The objectionable impurities such as O
Content is few.
The properties of product that the embodiment 1-6 aging methods of table 1 and comparative example 1-2 aging methods are obtained
It should be noted last that, above embodiment is merely illustrative of the technical solution of the present invention and unrestricted,
Although the present invention is described in detail with reference to example, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, it all should cover
Among scope of the presently claimed invention.
Claims (3)
1. carbonation method prepares the aging method of boehmite, it is characterised in that the sodium aluminate produced with soda lime sintering process
Refined soln is raw material, adjusts its alumina content for 20-60g/l, solution Crater corrosion is 1.3-1.6, and being passed through volumetric concentration is
30-40% industrial carbon dioxide gas, controls gelation time 10-20min, plastic terminal slurry pH value 10-13, by what is obtained
Slurries carry out rapidly solid-liquor separation, then will adhere to the filter cake of mother liquor, are fitted into closed container, 70-100 DEG C of heat ageing 2-
4h。
2. method as claimed in claim 1, it is characterised in that the closed container, it is desirable to high temperature resistant and acid and alkali-resistance, including plastics
Bag, glass container and rustless steel container.
3. method as claimed in claim 1, it is characterised in that the heating, to directly heat or indirectly heat.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610171887.XA CN105645446B (en) | 2016-03-24 | 2016-03-24 | Carbonation method prepares the aging method of boehmite |
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| CN201610171887.XA CN105645446B (en) | 2016-03-24 | 2016-03-24 | Carbonation method prepares the aging method of boehmite |
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| CN105645446A CN105645446A (en) | 2016-06-08 |
| CN105645446B true CN105645446B (en) | 2017-07-28 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108627411B (en) * | 2017-03-20 | 2020-07-31 | 中国石油化工股份有限公司 | Method for determining carbonate content in pseudo-boehmite, method for determining peptized acid using amount and preparation method of catalytic cracking catalyst |
| CN112744845B (en) * | 2019-10-29 | 2023-01-10 | 中国石油化工股份有限公司 | Pseudo-boehmite, preparation method and application thereof |
| CN114506867B (en) * | 2020-10-29 | 2023-07-28 | 中国石油化工股份有限公司 | Silicon-containing pseudo-boehmite and preparation method and application thereof |
| CN114522693B (en) * | 2020-10-30 | 2023-07-14 | 中国石油化工股份有限公司 | Boron-containing heavy oil hydrotreating catalyst and heavy oil hydrotreating method |
| CN114522692B (en) * | 2020-10-30 | 2023-07-11 | 中国石油化工股份有限公司 | Heavy oil hydrotreating catalyst and heavy oil hydrotreating method |
| CN114524447B (en) * | 2020-10-30 | 2023-10-10 | 中国石油化工股份有限公司 | Pseudo-boehmite, preparation method thereof and alumina |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102910656A (en) * | 2011-08-01 | 2013-02-06 | 中国石油化工股份有限公司 | Preparation method of pseudo-boehmite and porous alumina |
| CN105174293A (en) * | 2015-09-10 | 2015-12-23 | 中国海洋石油总公司 | Preparation method of pseudo-boehmite with centralized pore size distribution |
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| JPH07172823A (en) * | 1993-12-17 | 1995-07-11 | Sumitomo Chem Co Ltd | Production of aluminum hydroxide having low degree of flocculation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102910656A (en) * | 2011-08-01 | 2013-02-06 | 中国石油化工股份有限公司 | Preparation method of pseudo-boehmite and porous alumina |
| CN105174293A (en) * | 2015-09-10 | 2015-12-23 | 中国海洋石油总公司 | Preparation method of pseudo-boehmite with centralized pore size distribution |
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