CN105540630A - Preparation method of catalyst carrier for glycol prepared from coal - Google Patents
Preparation method of catalyst carrier for glycol prepared from coal Download PDFInfo
- Publication number
- CN105540630A CN105540630A CN201510904473.9A CN201510904473A CN105540630A CN 105540630 A CN105540630 A CN 105540630A CN 201510904473 A CN201510904473 A CN 201510904473A CN 105540630 A CN105540630 A CN 105540630A
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- China
- Prior art keywords
- coal
- preparation
- ethylene glycol
- catalyst according
- drying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000003054 catalyst Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003245 coal Substances 0.000 title abstract description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 title abstract 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 230000004913 activation Effects 0.000 claims abstract description 8
- 238000001994 activation Methods 0.000 claims abstract description 8
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 7
- 238000012216 screening Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 230000036541 health Effects 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 229910001648 diaspore Inorganic materials 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 230000001788 irregular Effects 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 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 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000007493 shaping process Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007669 thermal treatment Methods 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004131 Bayer process Methods 0.000 description 1
- ZNZYKNKBJPZETN-WELNAUFTSA-N Dialdehyde 11678 Chemical compound N1C2=CC=CC=C2C2=C1[C@H](C[C@H](/C(=C/O)C(=O)OC)[C@@H](C=C)C=O)NCC2 ZNZYKNKBJPZETN-WELNAUFTSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000037351 starvation Effects 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
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/612—Surface area less than 10 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/633—Pore volume less than 0.5 ml/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
-
- 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
- C01P2006/12—Surface area
-
- 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
- C01P2006/16—Pore diameter
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Disclosed is a preparation method of a catalyst carrier for glycol prepared from coal. Aluminium hydroxide produced through a barer process is subjected to technical processes including drying, grinding, quick crystal water removal, mixing with a guiding agent, moulding with a forming agent, shaping, standing, heat treatment, drying, activation, treating with a processing agent, drying, and screening, thereby producing alpha activated aluminium oxide. The catalyst carrier is small in specific surface and hole volume and large in hole diameter, has an alpha-type crystal structure, and can be used as an effective catalyst carrier for glycol prepared from coal.
Description
Technical field
The present invention relates to field of inorganic materials, relate in particular to a kind of preparation method of coal-ethylene glycol support of the catalyst.
Background technology
Ethylene glycol is a kind of important large industrial chemicals, mainly for the production of polyester, also can produce Synolac, oxalic dialdehyde etc., also can be used as frostproofer.Within 2014, domestic ethylene glycol Apparent con-sumption is 1,210 ten thousand tons, import 8,450,000 tons, and external dependence degree reaches 70%, expects the year two thousand twenty demand and will reach 1,800 ten thousand tons.It is raw material that traditional ethylene glycol production must rely on oil ethene, and for the energy natural endowment feature of China due to " oil starvation, weak breath, rich coal ", Development of Coal preparing ethylene glycol has important practical significance and long-range strategic importance.Coal-ethylene glycol is one of five New Coal Chemical technology that in country 12 planning, emphasis advances.
In the preparation process of coal-ethylene glycol catalyzer, the activity and selectivity of character to catalyzer of carrier has considerable influence.The carrier surface character dispersity of remarkably influenced active ingredient at carrier surface and the Degree of interaction of active ingredient and carrier on the one hand, thus affect the activity of catalyzer; On the other hand, the pore structure of carrier affects the diffusion of reactant and product in reaction process, thus affects the activity and selectivity of catalyzer.Usually it is believed that gama-alumina is active, and Alpha-alumina is classified as inert alumina, so in the application of the catalytic field such as petrochemical complex and energy environment gama-alumina more than Alpha-alumina, but some are had to the catalyzed reaction of particular requirement, Alpha-alumina has its irreplaceable function.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the coal-ethylene glycol support of the catalyst that can solve the problems of the technologies described above.
A preparation method for coal-ethylene glycol support of the catalyst, comprises the steps: drying and grinding-de--directed agents mixing-forming agent configuration-mother bulb making-thermal treatment-drying soon--activation-cleaning-drying is screened.
Aluminium hydroxide after described grinding, moisture content is lower than 0.2%, and being ground to particle diameter D50 is 2.0 μ
M, particle diameter D97 are 4.0 μm.
Described forming agent collocation method is as follows: add water about 100 liters, slowly adds 10-12 kilogram of nitric acid,
Evenly add 6-8 kilogram of diaspore under stirring, after adding, continue stirring 10 minutes, get 50 kilograms and add in reactor, add water 50 kilograms, open and stir, make after evenly adding ammoniacal liquor 2Kg.
Described mother bulb making method is as follows: joined by forming agent in the aluminum hydroxide particles of mixed cylinder, makes it become
Half paste, and put into 12 order stainless (steel) wires, be twisted under irregular saccharoid falls into sieve with strength, put into plastics bag, mother bulb leaves standstill health 2-4 hour.
Described heat treating method is as follows: add suitable quantity of water in a kettle., and the masterbatch that health is good is added in reactor,
Add to after tank mouth 40cm, cover tightly lid, be incubated 1 hour when being warmed up to 120 DEG C, then be warmed up to 290 ± 5 DEG C, pressure-controlling is at 3 ± 0.05MPa, and soaking time 1 hour, last naturally cooling at least 10 hours, Pressure Drop, to normal pressure, starts blowing.
Described dry activation method is as follows: after work in-process drying thermal treatment obtained, then activate, activation
Temperature is raised to 300 DEG C, insulation 0.5-1 hour, is more progressively warmed up to 650-700 DEG C, is incubated 1 hour, then naturally cooling.
Described dry sieve detecting method is as follows: temperature remains on 180-200 DEG C, adopt after dry 2 hours machine or
Artificial screening, particle ensures at 2-4mm.
The Alpha-alumina specific surface area that the present invention prepares is less than 10m
2/ g, pore volume is less than 0.01cm
2/ g, hole
Footpath is greater than 7nm, and the mass ratio of sodium is less than 0.001%.
The Alpha-alumina that the present invention prepares is as the application of coal-ethylene glycol support of the catalyst.
The beneficial effect that tool of the present invention brings:
1) that production process of the present invention adopts is particle diameter D50 is 2.0 μm, D97 is that the aluminium hydroxide of 4.0 μm is as raw material production activated alumina, the aluminum hydroxide particles being less than 2.0 μm accounts for 50%, the aluminum hydroxide particles being less than 4.0 μm accounts for 97%, meets the condition that crystalline form is changed and specific physicochemical property is necessary.
2) specific directed agents is adopted to be that the conversion of Alpha-alumina crystalline structure provides safeguard.
3) after adopting thermal treatment, the technique of dry activation again ensures the physical and chemical performance of Alpha-alumina.
4) Alpha-alumina specific surface area is minimum.
5) when Alpha-alumina pore volume is minimum, aperture reaches maximization.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but not as limitation of the present invention:
A preparation method for coal-ethylene glycol support of the catalyst, preparation process is as follows:
(1) dry: aluminium hydroxide Bayer process produced, biodiversity content is lower than 0.2%.
(2) grind: it is 2.0 μm that dried aluminium hydroxide is ground to D50, and D97 is 4.0 μm.
(3) take off soon: more than 800 DEG C, high temperature sloughs the crystal water in aluminium hydroxide.
(4) directed agents mixing: by directed agents all be mixed in aluminum oxide.
(5) forming agent configuration: add water about 100 liters, slowly add 10-12 kilogram of nitric acid, under agitation evenly add 6-8 kilogram of diaspore, after adding, continues stirring 10 minutes.Get 50 kilograms to add in middle reactor, add water 50 kilograms, open and stir, evenly add ammoniacal liquor 2Kg.
(6) mother bulb makes: joined by forming agent solution from the fast shedding of the aluminium hydroxide of mixed cylinder, make it become half paste to put into 12 order stainless (steel) wires, is twisted under irregular saccharoid falls into sieve with strength, puts into plastics bag.
(7) mother bulb is put into bowling machine add fast shedding and forming agent shaping, then shaping.
(8) health: mother bulb leaves standstill 2-4 hour.
(9) thermal treatment: add half water in a kettle., then masterbatch is added in reactor, add to after tank mouth 40cm, cover tightly lid, can heat up, when being warmed up to 120 DEG C, be incubated 1 hour, be warmed up to 290 ± 5 DEG C again, pressure-controlling was 3 ± 0.05MPa soaking time 1 hour.Naturally cooling at least 10 hours, Pressure Drop, to normal pressure, starts blowing.
(10) dry activation: by after the work in-process drying that obtains, then activate, activation temperature is raised to 300 DEG C, insulation 0.5-1 hour, is more progressively warmed up to technological temperature (650-700 DEG C), is incubated 1 hour, then naturally cooling.
(11) clean: repeatedly clean with ionized water.
(12) dry: temperature remains on 180-200 DEG C, dry 2 hours.
(13) screening: adopt machine and artificial screening, particle ensures at 2-4mm.
(14) pack: pack according to the requirement of client.
Feature performance benefit of the present invention
Project | The present invention | HG/T3297 2 --> |
Crystalline structure | α type | No requirement (NR) |
Specific surface area/(m 2/g) | Maximum 10 | >=200(is minimum) |
Pore volume/(cm 2/g) | Maximum 0.007 | >=0.35(is minimum) |
Aperture nm | Minimum 7.0 | No requirement (NR) |
The above embodiment of the present invention; it is only the citing clearly illustrating that the present invention does; but be not used for limiting the scope of the invention, all equivalent technical schemes also belong to category of the present invention, and scope of patent protection of the present invention should be limited by every claim.
Claims (10)
1. a preparation method for coal-ethylene glycol support of the catalyst, is characterized in that, comprises the steps: drying and grinding-de--directed agents mixing-forming agent configuration-mother bulb making-thermal treatment-drying-activation-cleaning soon-drying screening.
2. the preparation method of a kind of coal-ethylene glycol support of the catalyst according to claim 1, is characterized in that, the aluminium hydroxide after described drying and grinding, and moisture content is lower than 0.2%, and being ground to particle diameter D50 is 2.0 μm, and particle diameter D97 is 4.0 μm.
3. the preparation method of a kind of coal-ethylene glycol support of the catalyst according to claim 1, it is characterized in that, described forming agent collocation method is as follows: add water about 100 liters, slowly adds 10-12 kilogram of nitric acid, under agitation evenly adds 6-8 kilogram of diaspore, after adding, continue stirring 10 minutes, get 50 kilograms and add in reactor, add water 50 kilograms, open and stir, make after evenly adding ammoniacal liquor 2Kg.
4. the preparation method of a kind of coal-ethylene glycol support of the catalyst according to claim 1, it is characterized in that, described mother bulb making method is as follows: joined by forming agent in the aluminum hydroxide particles of mixed cylinder, it is made to become half paste, and put into 12 order stainless (steel) wires, be twisted under irregular saccharoid falls into sieve with strength, put into plastics bag, mother bulb leaves standstill health 2-4 hour.
5. the preparation method of a kind of coal-ethylene glycol support of the catalyst according to claim 1, it is characterized in that, described heat treating method is as follows: add suitable quantity of water in a kettle., the masterbatch that health is good is added in reactor, add to after tank mouth 40cm, cover tightly lid, when being warmed up to 120 DEG C, be incubated 1 hour, be warmed up to 290 ± 5 DEG C again, pressure-controlling at 3 ± 0.05MPa, soaking time 1 hour, last naturally cooling at least 10 hours, Pressure Drop, to normal pressure, starts blowing.
6. the preparation method of a kind of coal-ethylene glycol support of the catalyst according to claim 1, it is characterized in that, described activation method is as follows: activation temperature is raised to 300 DEG C, insulation 0.5-1 hour, progressively be warmed up to 650-700 DEG C again, be incubated 1 hour, then naturally cooling.
7. the preparation method of a kind of coal-ethylene glycol support of the catalyst according to claim 1, is characterized in that, described dry sieve detecting method is as follows: temperature remains on 180-200 DEG C, and adopt machine or artificial screening after dry 2 hours, particle ensures at 2-4mm.
8. the preparation method of a kind of coal-ethylene glycol support of the catalyst according to any one of claim 1-7, is characterized in that: the Alpha-alumina specific surface area prepared is less than 10m
2/ g, pore volume is less than 0.01cm
2/ g, aperture is greater than 7nm.
9. the preparation method of a kind of coal-ethylene glycol support of the catalyst according to any one of claim 1-7, is characterized in that: in the Alpha-alumina prepared, the mass ratio of sodium is less than 0.001%.
10. the preparation method of a kind of coal-ethylene glycol support of the catalyst according to claim 1, is characterized in that: the Alpha-alumina prepared is as the method for coal-ethylene glycol support of the catalyst.
Priority Applications (1)
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CN201510904473.9A CN105540630B (en) | 2015-12-09 | 2015-12-09 | A kind of preparation method of coal-ethylene glycol catalyst carrier |
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CN201510904473.9A CN105540630B (en) | 2015-12-09 | 2015-12-09 | A kind of preparation method of coal-ethylene glycol catalyst carrier |
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CN105540630A true CN105540630A (en) | 2016-05-04 |
CN105540630B CN105540630B (en) | 2017-03-29 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113247930A (en) * | 2021-06-30 | 2021-08-13 | 上海交通大学 | Alpha-alumina and preparation method thereof |
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CN1258567A (en) * | 1998-12-30 | 2000-07-05 | 中国石油化工集团公司 | Macroporous Alpha-alumina and its preparation and application |
CN1307929A (en) * | 2000-12-25 | 2001-08-15 | 化学工业部天津化工研究设计院 | Preparation process of alumina adsorbant |
CN103818939A (en) * | 2014-01-14 | 2014-05-28 | 淄博贝格工贸有限公司 | Aluminum oxide specially used for hydrogen peroxide fluidized bed and production technology for aluminum oxide |
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2015
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Patent Citations (3)
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CN1258567A (en) * | 1998-12-30 | 2000-07-05 | 中国石油化工集团公司 | Macroporous Alpha-alumina and its preparation and application |
CN1307929A (en) * | 2000-12-25 | 2001-08-15 | 化学工业部天津化工研究设计院 | Preparation process of alumina adsorbant |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113247930A (en) * | 2021-06-30 | 2021-08-13 | 上海交通大学 | Alpha-alumina and preparation method thereof |
CN113247930B (en) * | 2021-06-30 | 2022-04-01 | 上海交通大学 | Alpha-alumina and preparation method thereof |
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