CN105645446A - Aging method of pseudo-boehmite prepared by carbonation method - Google Patents
Aging method of pseudo-boehmite prepared by carbonation method Download PDFInfo
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- CN105645446A CN105645446A CN201610171887.XA CN201610171887A CN105645446A CN 105645446 A CN105645446 A CN 105645446A CN 201610171887 A CN201610171887 A CN 201610171887A CN 105645446 A CN105645446 A CN 105645446A
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- aging
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- 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
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- 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
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- 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
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses an aging method of pseudo-boehmite prepared by a carbonation method. The method concretely comprises the steps of enabling the pseudo-boehmite prepared by the carbonation method to form gel, and then rapidly carrying out on solid-liquid separation; after that, putting a filter cake attached with mother liquor into a closed container, heating and aging. The aging method is simple in technology, low in energy consumption, high in productivity and low in production cost; the prepared pseudo-boehmite product is pure in crystalline phase, high in degree of crystallinity, good in gel dissolubility, less in impurity and wide in use.
Description
Technical field
The preparation method that the present invention relates to boehmite, prepares the aging method of boehmite particularly to a kind of carbonation method.
Background technology
The preparation method of boehmite is varied, domestic alumina by sintering factory adopts carbonation method to prepare boehmite mostly, because grafting is on alumina production process flow, raw material sources are convenient, by-product in process, waste liquid etc. returning alumina flow process can realize closed cycle, so product cost is low, non-environmental-pollution. Carbonation method is prepared boehmite technical process and is included dispensing, plastic, aging, washing, solid-liquor separation, drying and other steps successively.
It is a lot of that carbonation method prepares the aging technology in boehmite technique, domestic and international patent and relevant report, but is all carry out in the alkaline solution of the serosity after carbonating plastic or preparation, it is possible to is called that serosity state is aging. Such as, 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, is incubated aging 1��6 hour, or it is in addition aging to be first made directly after solid-liquor separation in washing process; Aging method disclosed in CN100999328 is: by unbodied hydrated alumina, at least one water miscible alkali mixing of hydration, pulp, serosity in 20 DEG C to 90 DEG C aging 0.5 to 6 hour; CN101172631 discloses the preparation method that a kind of carbonation method prepares boehmite, its aging method is: after plastic, first carries out serosity separation, then it is aging to carry out temperature raising after filter cake adds wash water mixing making beating, temperature is 70 DEG C to 100 DEG C, and ageing time is 3��6 hours. In these methods, owing to ageing process is that whole slurry system carries out temperature raising and insulation, therefore to expend a large amount of heat energy, and temperature raising process is longer, easily cause final products that dephasign occurs, thus affecting the serviceability of product.
Summary of the invention
The technical problem to be solved is that the power consumption of existing aging technique is big, serosity temperature raising process is long, it is easy to cause miscellaneous, it is provided that a kind of carbonation method prepares the aging method of boehmite.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
Carbonation method prepares the aging method of boehmite, after carbonation method prepares boehmite plastic, carries out rapidly solid-liquor separation, then by the filter cake of attachment mother solution, loads in hermetic container, heat ageing.
Further, described hermetic container, it is desirable to high temperature resistant and acid and alkali-resistance, including plastic bag, glass container and rustless steel container.
Further, described heating, for directly heating or indirectly heating.
Further, described aging, temperature is 70-100 DEG C, and the time is 2-4h.
A kind of carbonation method provided by the invention prepares the aging method of boehmite, and technique is simple, energy-saving and cost-reducing, improves production capacity, reduces production cost; The boehmite product prepared, crystalline phase is pure, degree of crystallinity is high, peptization is good, impurity is few, be widely used as binding agent, dispersant, catalyst and catalyst support material.
Detailed description of the invention
A kind of carbonation method that the embodiment of the present invention provides prepares the aging method of boehmite, with the sodium aluminate refined soln of soda lime sintering process production for raw material, adjusting its alumina content is 20-60g/l, solution Crater corrosion is 1.3-1.6, pass into the industrial carbon dioxide gas (may be from soda lime sintering process and produce the intermediate product of alumina technology) that volumetric concentration is 30-40%, control gelation time 10-20min, plastic terminal slurry pH value 10-13, carries out rapidly solid-liquor separation by the serosity obtained. The filter cake separated loads in hermetic container, hermetic container requires high temperature resistant, acid and alkali-resistance, including plastic bag, glass container, rustless steel container etc., to avoid attachment mother liquid evaporation, then 70-100 DEG C is lifted temperature to, can directly heating or indirectly heat, aging 2-4h (can be described as solidification state aging). The filter cake of aging post processing, then through hot waterization slurry stirring, after the hot water cyclic washing of 60-100 DEG C, through solid-liquor separation, adopts baking oven strengthening drying or flash evaporation drying mode to dry, obtains 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 provides prepares the aging method of boehmite, specific as follows: with the sodium aluminate refined soln of soda lime sintering process production for raw material, adjusting its alumina content is 42g/l, Crater corrosion is 1.52, pass into the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 15 minutes, slurry pH value is 13, and the serosity obtained is carried out rapidly solid-liquor separation. The filter cake separated loads sealing plastic bag, puts into after being incubated 2 hours in 70 DEG C of waters, adds 80 DEG C of hot waterization slurries, carries out agitator treating remove impurity repeatedly, finally dries in baking oven and obtains qualified products. Product index for details see attached table 1.
Embodiment 2
A kind of carbonation method that the embodiment of the present invention 2 provides prepares the aging method of boehmite, specific as follows: with the sodium aluminate refined soln of soda lime sintering process production for raw material, adjusting its alumina content is 23g/l, Crater corrosion is 1.37, pass into the industrial carbon dioxide gas that volumetric concentration is 30-40%, 10.5 after minute, slurry pH value is 10.5, the serosity obtained is carried out rapidly solid-liquor separation. The filter cake separated loads sealing plastic bag, puts into after being incubated 4 hours in 90 DEG C of waters, adds 75 DEG C of hot waterization slurries, carries out agitator treating remove impurity repeatedly, dries and obtain 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 provides prepares the aging method of boehmite, specific as follows: with the sodium aluminate refined soln of soda lime sintering process production for raw material, adjusting its alumina content is 36g/l, Crater corrosion is 1.42, pass into the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 13 minutes, slurry pH value is 11, and the serosity obtained is carried out rapidly solid-liquor separation.The filter cake separated loads in sealing flask, puts into after being incubated 3.5 hours in 95 DEG C of waters, adds 95 DEG C of hot waterization slurries, carries out agitator treating remove impurity repeatedly, dries and obtain 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 provides prepares the aging method of boehmite, specific as follows: with the sodium aluminate refined soln of soda lime sintering process production for raw material, adjusting its alumina content is 60g/l, Crater corrosion is 1.57, pass into the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 20 minutes, slurry pH value is 12, and the serosity obtained is carried out rapidly solid-liquor separation. The filter cake separated loads in sealing flask, puts into after being incubated 3.5 hours in 95 DEG C of waters, adds 95 DEG C of hot waterization slurries, carries out agitator treating remove impurity repeatedly, dries and obtain 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 provides prepares the aging method of boehmite, specific as follows: with the sodium aluminate refined soln of soda lime sintering process production for raw material, adjusting its alumina content is 40g/l, Crater corrosion is 1.52, pass into the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 14 minutes, slurry pH value is 11.5, and the serosity obtained is carried out rapidly solid-liquor separation. The filter cake separated loads in sealing flask, puts into after being incubated 3 hours in 100 DEG C of steam boxs, adds 85 DEG C of hot waterization slurries, carries out agitator treating remove impurity repeatedly, and strengthening is dry obtains qualified products.
Embodiment 6
A kind of carbonation method that the embodiment of the present invention 6 provides prepares the aging method of boehmite, specific as follows: with the sodium aluminate refined soln of soda lime sintering process production for raw material, adjusting its alumina content is 55g/l, Crater corrosion is 1.48, pass into the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 17 minutes, slurry pH value is 12.5, and the serosity obtained is carried out rapidly solid-liquor separation. The filter cake separated loads in rustless steel beaker with cover, after putting into 100 DEG C of steam boxs insulations 4 hours, adds 95 DEG C of hot waterization slurries, carries out agitator treating remove impurity repeatedly, and expansion drying obtains qualified products. Product index for details see attached table 1.
Comparative example 1��2 describes the boehmite character 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 provides prepares the aging method of boehmite, particularly as follows: with soda lime sintering process produce sodium aluminate refined soln for raw material, adjusting its alumina content is 41g/l, Crater corrosion is 1.51, pass into the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 15 minutes, slurry pH value is 11.5, the carbonization serosity obtained is lifted temperature to 85 DEG C, after being incubated 3 hours, carrying out solid-liquor separation, then 80 DEG C of hot water carry out agitator treating remove impurity repeatedly, and oven for drying obtains 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 provides prepares the aging method of boehmite, particularly as follows: with soda lime sintering process produce sodium aluminate refined soln for raw material, adjusting its alumina content is 50g/l, Crater corrosion is 1.46, pass into the industrial carbon dioxide gas that volumetric concentration is 30-40%, after 18 minutes, slurry pH value is 12, the carbonization serosity obtained is lifted temperature to 95 DEG C, after being incubated 3 hours, carrying out solid-liquor separation, then 80 DEG C of hot water carry out agitator treating remove impurity repeatedly, and oven for drying obtains qualified products. Product index for details see attached table 1.
As it can be seen from table 1 adopt the embodiment of the present invention 1-6 carbonation method provided to prepare the product that the aging method of boehmite prepares, the miscellaneous content of its gibbsite is few, degree of crystallinity is high, pore volume is big, and peptization performance is good, Na2The objectionable impurities content such as O are few.
The properties of product that table 1 embodiment 1-6 aging method and comparative example's 1-2 aging method obtain
It should be noted last that, above detailed description of the invention is only in order to illustrate technical scheme and unrestricted, although the present invention being described in detail with reference to example, it will be understood by those within the art that, technical scheme can be modified or equivalent replacement, without deviating from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of scope of the presently claimed invention.
Claims (4)
1. carbonation method prepares the aging method of boehmite, it is characterised in that after carbonation method prepares boehmite plastic, carries out rapidly solid-liquor separation, then by the filter cake of attachment mother solution, loads in hermetic container, heat ageing.
2. method as claimed in claim 1, it is characterised in that described hermetic container, it is desirable to high temperature resistant and acid and alkali-resistance, including plastic bag, glass container and rustless steel container.
3. method as claimed in claim 1, it is characterised in that described heating, for directly heating or indirectly heating.
4. method as claimed in claim 1, it is characterised in that described aging, temperature is 70-100 DEG C, and the time is 2-4h.
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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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| CN105645446B CN105645446B (en) | 2017-07-28 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108627411A (en) * | 2017-03-20 | 2018-10-09 | 中国石油化工股份有限公司 | Measure the method and the method for peptization acid dosage and the preparation method of catalytic cracking catalyst of carbonate content in boehmite |
| CN112744845A (en) * | 2019-10-29 | 2021-05-04 | 中国石油化工股份有限公司 | Pseudo-boehmite, preparation method and application thereof |
| CN114506867A (en) * | 2020-10-29 | 2022-05-17 | 中国石油化工股份有限公司 | Silicon-containing pseudo-boehmite as well as preparation method and application thereof |
| CN114522693A (en) * | 2020-10-30 | 2022-05-24 | 中国石油化工股份有限公司 | Boron-containing heavy oil hydrotreating catalyst and heavy oil hydrotreating method |
| CN114524447A (en) * | 2020-10-30 | 2022-05-24 | 中国石油化工股份有限公司 | Pseudo-boehmite, preparation method thereof and alumina |
| CN114522692A (en) * | 2020-10-30 | 2022-05-24 | 中国石油化工股份有限公司 | Heavy oil hydrotreating catalyst and heavy oil hydrotreating method |
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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 |
| 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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2016
- 2016-03-24 CN CN201610171887.XA patent/CN105645446B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| 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 |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108627411A (en) * | 2017-03-20 | 2018-10-09 | 中国石油化工股份有限公司 | Measure the method and the method for peptization acid dosage and the preparation method of catalytic cracking catalyst of carbonate content in boehmite |
| 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 |
| CN112744845A (en) * | 2019-10-29 | 2021-05-04 | 中国石油化工股份有限公司 | Pseudo-boehmite, preparation method and application thereof |
| 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 |
| CN114506867A (en) * | 2020-10-29 | 2022-05-17 | 中国石油化工股份有限公司 | Silicon-containing pseudo-boehmite as well as 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 |
| CN114522693A (en) * | 2020-10-30 | 2022-05-24 | 中国石油化工股份有限公司 | Boron-containing heavy oil hydrotreating catalyst and heavy oil hydrotreating method |
| CN114524447A (en) * | 2020-10-30 | 2022-05-24 | 中国石油化工股份有限公司 | Pseudo-boehmite, preparation method thereof and alumina |
| CN114522692A (en) * | 2020-10-30 | 2022-05-24 | 中国石油化工股份有限公司 | 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 |
| 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 |
| 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 |
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| CN105645446B (en) | 2017-07-28 |
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