CN108273566B - Preparation method of alumina microspheres - Google Patents
Preparation method of alumina microspheres Download PDFInfo
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- CN108273566B CN108273566B CN201810141700.0A CN201810141700A CN108273566B CN 108273566 B CN108273566 B CN 108273566B CN 201810141700 A CN201810141700 A CN 201810141700A CN 108273566 B CN108273566 B CN 108273566B
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- alumina
- oil
- aluminum
- sol
- aluminum source
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000004005 microsphere Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000084 colloidal system Substances 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- 238000001723 curing Methods 0.000 claims abstract description 4
- 239000003921 oil Substances 0.000 claims description 26
- 235000019198 oils Nutrition 0.000 claims description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 6
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 4
- 239000008158 vegetable oil Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910001593 boehmite Inorganic materials 0.000 claims description 2
- 229910001648 diaspore Inorganic materials 0.000 claims description 2
- 229910001679 gibbsite Inorganic materials 0.000 claims description 2
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 2
- 239000010687 lubricating oil Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 230000020477 pH reduction Effects 0.000 claims description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 abstract description 12
- 239000003054 catalyst Substances 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000007789 gas Substances 0.000 abstract description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000969 carrier Substances 0.000 abstract description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 6
- 239000008188 pellet Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 235000019253 formic acid Nutrition 0.000 description 3
- 239000007863 gel particle Substances 0.000 description 3
- -1 alkoxy aluminum Chemical compound 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 2
- 239000004312 hexamethylene tetramine Substances 0.000 description 2
- 229960004011 methenamine Drugs 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 241000219793 Trifolium Species 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- 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
- B01J35/615—100-500 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to the field of catalyst carriers, and particularly relates to a preparation method of an alumina microsphere, which comprises the following steps: mixing an aluminum source and water, grinding until the granularity D50 is less than or equal to 3 mu m, adding aluminum sol, continuously grinding and acidifying to prepare colloid; and (3) dripping the colloid into oil for forming, heating and curing, taking out the cured particles, washing, drying and roasting to obtain the alumina balls. The colloid is prepared from the aluminum sol, the aluminum source and the acid gel, and is formed and cured in oil, and no nitrogen-containing substance is used in the whole process, so that the subsequent generation of nitrogen oxide is avoided, the difficulty in tail gas treatment is reduced, and the cost is saved.
Description
Technical Field
The invention belongs to the field of catalyst carriers, and particularly relates to a preparation method of an alumina microsphere.
Background
The alumina is used as a common basic material of the catalyst and has wide application in the field of petrochemical industry, and the appearance forms of the alumina are about the following: microspheres, spheres, strips (cylinders, clover, etc.), or in the form of a medium matrix of the FCC catalyst. Wherein, the moving bed catalyst has higher requirement on the strength, and the spherical carrier prepared by the method also has higher strength.
The processes currently used for producing spherical alumina are classified into two types, one is mechanical forming such as rotary disc forming, extrusion forming (extruding, shaping) and the like, and the spherical alumina carrier produced by the processes relying on mechanical forming has natural defects in strength and sphericity, and the other is surface tension forming such as oil column method or oil amine method, and the spherical alumina carrier produced by the processes has better strength and sphericity than mechanical forming and can produce a carrier with a diameter of 1-2mm, which is difficult to achieve by mechanical forming.
CN105502447B discloses a method for preparing alumina pellets by hot oil column molding, comprising the steps of mixing pseudo-boehmite powder prepared by hydrolyzing alkoxy aluminum, urea and water to prepare alumina suspension, adding acid to obtain alumina slurry, adding hexamethylene tetramine to the alumina slurry to be uniformly mixed, then dripping the mixture into hot oil to form pellets, directly collecting the alumina pellets at the lower end of a hot oil column, and then washing, drying and roasting the collected alumina pellets. Although the method can prepare the alumina pellets with good quality, the hexamethylenetetramine is used in the production process, so that great peculiar smell and nitrogen oxide are generated, and the tail gas treatment is very difficult.
CN1204964C discloses a method for forming oil ammonia column of spherical alumina, alumina sol is dropped into oil ammonia column composed of 0.1-4.5mm upper layer oil phase and 10-300cm lower layer electrolyte solution to form spherical gel particles, then the gel particles are aged in the electrolyte solution phase for 0.5-15 hours, and then the gel particles are taken out, dried and roasted. The method avoids the use of organic amine, but does not laterally get rid of nitrogenous substances, and has the hidden danger of environmental pollution.
Disclosure of Invention
The invention provides a preparation method of alumina microspheres for solving the problems in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of alumina microspheres comprises the following steps: mixing an aluminum source and water, grinding until the granularity D50 is less than or equal to 3 mu m, adding aluminum sol, continuously grinding and acidifying to prepare colloid; and (3) dripping the colloid into oil for forming, heating and curing, taking out the cured particles, washing, drying and roasting to obtain the alumina balls.
Further, the aluminum source is one or more of pseudoboehmite, gibbsite, boehmite, diaspore and alumina powder.
Further, the content of chloride ions in the aluminum sol is 10-15 wt%.
Furthermore, the sum of the mass of the alumina provided by the alumina sol and the mass of the alumina provided by the aluminum source is 20-30% of the sum of the weight of the alumina sol, the weight of the aluminum source and the weight of the water.
Further, the mass ratio of the alumina provided by the aluminum sol to the alumina provided by the aluminum source is 1-20: 80-99.
Further, the pH value after acidification is 3.0-3.2.
Further, the oil is one or more of transformer oil, medical lubricating oil, vegetable oil and heat conducting oil. Further selected from the group consisting of thermal oils.
Further, the temperature is 150-.
Further, the washing process is washing by using 0.1-1mol/L dilute hydrochloric acid.
Further, the drying temperature is 50-100 ℃, the roasting temperature is 500-700 ℃, and the roasting time is 1-2 h.
The invention has the beneficial effects that:
firstly, colloid is prepared by adopting aluminum sol, an aluminum source and acid gel, and is formed and cured in oil, no nitrogen-containing substance is used in the whole process, so that the subsequent generation of nitrogen oxide is avoided, the difficulty in tail gas treatment is reduced, and the cost is saved.
Secondly, the method for preparing the alumina ball by the oil column forming comprises the steps of mixing and grinding an aluminum source and water to enable aluminum source particles to be smaller and prepare more uniform slurry, mixing and grinding the slurry and aluminum sol to enable the aluminum source particles and aluminum ions to be more uniformly mixed, adding an acid solution to prepare uniform colloid, dropping gel into oil for forming and heating for curing, avoiding using organic amine or ammonium salt, and effectively avoiding the generation of nitrogen oxide.
The invention reasonably optimizes the use amount of each component, controls the solid content and the pH value of the colloid, and grinds to the degree of the invention, so that the colloid is more uniform, the performance of the prepared product is more excellent, and the zero use of harmful substances ensures that the preparation process and the prepared product are more environment-friendly.
Detailed Description
The present invention is further described in detail below by way of specific examples, which will enable one skilled in the art to more fully understand the present invention, but which are not intended to limit the invention in any way.
Example 1
Weighing 146.2g of pseudo-boehmite, mixing with 331.74 g of water, grinding in a JM-L100 type colloid mill, adding 22.06g of alumina sol when the particle size D50 of the pseudo-boehmite is less than or equal to 3 mu m, grinding for 10min, slowly adding 30% hydrochloric acid until the pH value is 3.10, dripping the mixture into vegetable oil to form balls, heating the oil to 120 ℃, keeping the temperature for 300min, taking out the alumina balls, washing in 0.1mol/L diluted hydrochloric acid, drying at 80 ℃ for 120min, and roasting at 600 ℃ for 120min to obtain the alumina balls.
Example 2
Alumina spheres were prepared by following the procedure of example 1 except that the weight of pseudoboehmite was 141.5g, the weight of water was 223.2g, and the weight of alumina sol was 35.3 g. Slowly adding formic acid until the pH value is 3.10, dripping the formic acid into heat conduction oil to form balls, heating the oil to 150 ℃, keeping the temperature for 240min, taking out the alumina balls, washing the alumina balls in 0.1mol/L diluted hydrochloric acid, drying the alumina balls at 80 ℃ for 120min, and roasting the alumina balls at 600 ℃ for 120min to obtain the alumina balls.
Example 3
Alumina spheres were prepared by following the procedure of example 2 except that 30% hydrochloric acid was added to a pH of 3.10, dropped into vegetable oil to form spheres, the oil was heated to 180 ℃ and kept at a constant temperature for 120min, the alumina spheres were taken out and washed with 0.1mol/L diluted hydrochloric acid, dried at 80 ℃ for 120min and then calcined at 600 ℃ for 120min to obtain alumina spheres.
Example 4
Alumina spheres were prepared as in example 1, except that formic acid was added to a pH of 3.10, dropped into transformer oil to form spheres, the oil was heated to 180 ℃ and kept at a constant temperature for 180min, the alumina spheres were taken out, washed with 0.1mol/L diluted hydrochloric acid, dried at 80 ℃ for 120min and then calcined at 600 ℃ for 120min to obtain alumina spheres.
Sample analysis meter
| Numbering | Diameter mm | Content of alumina% | Strength N | Specific surface m2/g | Pore volume ml/g |
| Example 1 | 1-2 | 99.97 | 58.15 | 241 | 0.44 |
| Example 2 | 1-2 | 99.95 | 60.43 | 233 | 0.45 |
| Example 3 | 1-2 | 99.94 | 62.28 | 236 | 0.44 |
| Example 4 | 1-2 | 99.96 | 59.16 | 240 | 0.45 |
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be made by those skilled in the art without inventive work within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (5)
1. The preparation method of the alumina microspheres is characterized by comprising the following steps: mixing an aluminum source and water, grinding until the granularity D50 is less than or equal to 3 mu m, adding aluminum sol, continuously grinding and acidifying to prepare colloid; dripping the colloid into oil for molding, heating and curing, taking out the cured particles, washing, drying and roasting to obtain alumina balls;
the aluminum source is one or more of pseudo boehmite, gibbsite, boehmite, diaspore and alumina powder;
the sum of the mass of the alumina provided by the alumina sol and the mass of the alumina provided by the aluminum source is 20-30% of the sum of the weight of the alumina sol, the weight of the aluminum source and the weight of the water; the content of chloride ions in the aluminum sol is 10-15 wt%;
the mass ratio of the alumina provided by the aluminum sol to the alumina provided by the aluminum source is 1-20: 80-99 parts of;
the pH value after acidification is 3.0-3.2.
2. The method for preparing alumina microspheres according to claim 1, wherein: the oil is one or more of transformer oil, medical lubricating oil, vegetable oil and heat conducting oil.
3. The method for producing the alumina microspheres according to claim 1, wherein: the temperature is 150-.
4. The method for preparing alumina microspheres according to claim 1, wherein: the washing process adopts 0.1-1mol/L dilute hydrochloric acid for washing.
5. The method for preparing alumina microspheres according to claim 1, wherein: the drying temperature is 50-100 ℃, the roasting temperature is 500-700 ℃, and the roasting time is 1-2 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810141700.0A CN108273566B (en) | 2018-02-11 | 2018-02-11 | Preparation method of alumina microspheres |
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| CN201810141700.0A CN108273566B (en) | 2018-02-11 | 2018-02-11 | Preparation method of alumina microspheres |
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| CN108273566B true CN108273566B (en) | 2021-03-23 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108947570A (en) * | 2018-09-07 | 2018-12-07 | 长沙理工大学 | A kind of porous ceramics microballoon and preparation method thereof |
| CN111468048A (en) * | 2020-04-13 | 2020-07-31 | 邹凌峰 | Preparation method of high-strength gamma-alumina microspheres |
| CN114180608A (en) * | 2020-08-24 | 2022-03-15 | 中国石油化工股份有限公司 | Preparation method of alumina pellets |
| CN117735961B (en) * | 2023-12-21 | 2024-05-31 | 任红波 | Method for preparing alumina grinding medium by titration method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1040845C (en) * | 1993-07-16 | 1998-11-25 | 中国石油化工总公司 | Preparation of micro-ball gamma aluminum oxide |
| CN104418371B (en) * | 2013-08-20 | 2016-04-27 | 中国石油化工股份有限公司 | A kind of preparation method of ball-aluminium oxide |
| CN103922373A (en) * | 2014-04-14 | 2014-07-16 | 浙江大学 | Preparation method of alumina porous microsphere |
| CN106745121B (en) * | 2016-12-23 | 2017-12-19 | 鲁西催化剂有限公司 | A kind of preparation method of high-performance active oxidation aluminium ball |
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| CN108273566A (en) | 2018-07-13 |
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Effective date of registration: 20240429 Address after: No.23 Yongning Road, Gudao Town, Hekou District, Dongying City, Shandong Province, 257000 Patentee after: Dongying Junlin New Material Co.,Ltd. Country or region after: China Address before: 614000 group 3, Miaoer village, Jinsu Town, Wutongqiao District, Leshan City, Sichuan Province Patentee before: Runhe catalyst Co.,Ltd. Country or region before: China |
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