CN105948793A - Preparation method for preparing lightweight and porous aluminium phosphate-mullite ceramic ball - Google Patents
Preparation method for preparing lightweight and porous aluminium phosphate-mullite ceramic ball Download PDFInfo
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
Abstract
The invention provides a preparation method for preparing a lightweight and porous aluminium phosphate- mullite ceramic ball. The method is characterized by comprising the following steps: (1) conducting the dry blending of mullite powders, alumina powders, aluminium dihydrogen phosphate powders and frit powders proportionally; (2) granulating, molding and preparing a cylindrical green body; (3) drying the green body at 70 DEG C for 5 hours, placing the dried green body in an alumina crucible with the inner bottom thereof to be semi-spherical, heating the green body in the air atmosphere at a temperature rising speed of 5 DEG C per minute to 150 DEG C, maintaining the temperature for 2 hours, heating the green body again at a temperature rising speed of 10-20 DEG C per minute to 380 DEG C, maintaining the temperature for 1 hours, heating the green body again at a temperature rising speed of 1 DEG C per minute to 680 DEG C, maintaining the temperature for 2 hours, heating the green body again at a temperature rising speed of 5 DEG C per minute to 1150 DEG C, maintaining the temperature for 2 hours, and then naturally cooling the green body to the room temperature to obtain the lightweight and porous aluminium phosphate- mullite ceramic ball.
Description
Technical field
The present invention is to provide the preparation method of a kind of light porous aluminum phosphate mullite ceramic ball, belong to special cermacis
Technical field of material.
Background technology
Porous alumionphosphate (AlPO4) mullite (3Al2O3 .2SiO2) Ceramic Balls application in the industrial production is the widest
General, can be as catalyst carrier, chemical filler, insulation and refractory material etc..As carrier of photocatalyst and other liquid phases
Catalytic reaction agent carrier, and as in water during the adsorbent of noxious substance, in order to ensure have efficient catalytic effect and
(or) adsorption efficiency, often requiring that porous ceramic ball is in suspended state in water, this is accomplished by preparing a kind of light porous pottery
Porcelain ball.At present, the most mainly use the spheroid that the Organic substance that easily burning is lost is made as " core " of spherical base substrate, then pass through
Burn till removing spherical organic " core ", thus prepare a kind of suspensible porous ceramics hollow ball.The shortcoming of the method is: molding is relatively
Difficulty, and during Organic substance burns and loses, be easily caused pottery cracking or destroy, reducing the yield rate of product;Additionally, this work
Skill process is more complicated, relatively costly, deficiency in economic performance, easily pollutes environment.In order to overcome an above-mentioned difficult problem, invention provides one
Plant the preparation side of light porous aluminum phosphate mullite ceramic ball efficient, simple, safe and reliable, easily operated, with low cost
Method.
Summary of the invention
The technology of the present invention provides a kind of light porous phosphoric acid efficient, simple, safe and reliable, easily operated, with low cost
The preparation method of aluminum-containing mullite Ceramic Balls, its technical scheme is:
The preparation method of a kind of light porous aluminum phosphate mullite ceramic ball, it is characterised in that use following steps: (1) is not
Coming stone powder, alumina powder, biphosphate aluminium powder, frit powder enters according to the ratio that mass ratio is 2:1:3.11:0.03
Row is dry mixed;Wherein, containing 50 wt% lithium oxides, the sodium oxide of 30 wt% and the silicon dioxide of 20 wt% in frit;(2) add dense
Degree be the poly-vinyl alcohol solution of 8 wt% as binding agent, the addition of binding agent is the 5% of blank gross mass;Then pelletize, one-tenth
Type, prepares cylindric base substrate;(3) after 70 DEG C of dry base substrates 5 hours, it is the oxidation that semicircle is spherical that base substrate is put into inner bottom part
In aluminum crucible, under air atmosphere, heat to 150 DEG C with the speed of 5 DEG C/min and be incubated 2 hours, then with 10-20
DEG C/speed of min heats to 380 DEG C and is incubated 1 hour, then heats to 680 with the speed of 1 DEG C/min
DEG C and be incubated 2 hours, finally heat to 1150 DEG C with the speed of 5 DEG C/min and be incubated 2 hours, natural cooling subsequently
To room temperature, i.e. prepare light porous aluminum phosphate mullite ceramic ball.
The preparation method of described a kind of light porous aluminum phosphate mullite ceramic ball, it is characterised in that: in step (1)
Mullite Powder and the mean diameter of oxide powder be all 0.6 micron, aluminium dihydrogen phosphate powder average particle size is 0.5 micron,
The mean diameter of frit powder is 0.7 micron.
The preparation method of described a kind of light porous aluminum phosphate mullite ceramic ball, it is characterised in that: in step (2)
Molding refer to carry out dry-pressing formed to powder body, briquetting pressure is 10-25MPa.
Fig. 1 is the photo that light porous aluminum phosphate mullite ceramic ball prepared by the technology of the present invention floats in water;From
Figure can be seen that, aluminum phosphate mullite ceramic ball floats in water, illustrates that the volume of aluminum phosphate mullite ceramic ball is close
Degree is less than the density of water, and the material that i.e. prepared by the technology of the present invention belongs to light porous ceramic material.
The principle of this technological invention is as follows:
Utilizing aluminium dihydrogen phosphate melting at a lower temperature is liquid, and the most coagulable performance makes
Base substrate spontaneously forms as spheroid in sintering process, concrete principle is as follows: aluminium dihydrogen phosphate is heated to 150 DEG C, insulation 2
After hour, aluminium dihydrogen phosphate is changed into as liquid, is then heated rapidly to 380 DEG C and is incubated 1 hour, its objective is to make various
Raw material forms the viscous body that a kind of viscosity is the biggest at such a temperature.The effect adding frit is on the one hand can to promote raw materials melt
For the viscous body that a kind of viscosity is the biggest, on the other hand surface tension can also be increased so that viscous physical ability spontaneously forms as spheroid.
During being heated slowly to 680 DEG C, aluminium dihydrogen phosphate is gradually solidified as solid;In temperature-rise period, aluminium dihydrogen phosphate can be decomposed into
Aluminum phosphate, steam and phosphorus pentoxide, the phosphorus pentoxide of generation can generate aluminum phosphate mullite with magnesium carbonate reaction, and
Steam and carbon dioxide etc. have the effect of pore-forming, thus can prepare light porous aluminum phosphate mullite ceramic.
Detailed description of the invention
Embodiment 1
Mullite Powder, alumina powder, biphosphate aluminium powder, frit powder is 2:1:3.11:0.03 according to mass ratio
Ratio be dry mixed;Wherein, containing 50 wt% lithium oxides, the sodium oxide of 30 wt% and the silicon dioxide of 20 wt% in frit;
The mean diameter controlling Mullite Powder and oxide powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron,
The mean diameter of frit powder is 0.7 micron;Add concentration be the poly-vinyl alcohol solution of 8 wt% as binding agent, binding agent
Addition is the 5% of blank gross mass;Then pelletize, with 10MPa pressure dry-pressing formed, prepare cylindric base substrate;Do at 70 DEG C
Dry base substrate is after 5 hours, base substrate is put in inner bottom part is the alumina crucible that semicircle is spherical, with 5 DEG C/min under air atmosphere
Speed heat to 150 DEG C and be incubated 2 hours, then heat to 380 DEG C with the speed of 10 DEG C/min and be incubated 1
Individual hour, then heat to 680 DEG C with the speed of 1 DEG C/min and be incubated 2 hours, finally adding with the speed of 5 DEG C/min
Heat is warmed up to 1150 DEG C and is incubated 2 hours, naturally cools to room temperature subsequently, i.e. prepares light porous aluminum phosphate mullite
Ceramic Balls.The bulk density recording porous ceramic ball with Archimedes method is 0.89 g/cm3, open pore rate is 35 %.Use XRD
It is aluminum phosphate mullite that analysis records the crystalline phase of Ceramic Balls.
Embodiment 2
Mullite Powder, alumina powder, biphosphate aluminium powder, frit powder is 2:1:3.11:0.03's according to mass ratio
Ratio is dry mixed;Wherein, containing 50 wt% lithium oxides, the sodium oxide of 30 wt% and the silicon dioxide of 20 wt% in frit;Control
The mean diameter of Mullite Powder processed and oxide powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, molten
The mean diameter of block powder is 0.7 micron;Adding concentration is that the poly-vinyl alcohol solution of 8 wt% is as binding agent, adding of binding agent
Dosage is the 5% of blank gross mass;Then pelletize, with 20MPa pressure dry-pressing formed, prepare cylindric base substrate;It is dried at 70 DEG C
After base substrate 5 hours, base substrate is put in inner bottom part is the alumina crucible that semicircle is spherical, with 5 DEG C/min's under air atmosphere
Speed heats to 150 DEG C and is incubated 2 hours, then heats to 380 DEG C with the speed of 15 DEG C/min and be incubated 1
Hour, then heat to 680 DEG C with the speed of 1 DEG C/min and be incubated 2 hours, finally heating with the speed of 5 DEG C/min
It is warmed up to 1150 DEG C and is incubated 2 hours, naturally cooling to room temperature subsequently, i.e. preparing light porous aluminum phosphate mullite pottery
Porcelain ball.The bulk density recording porous ceramic ball with Archimedes method is 0.90 g/cm3, open pore rate is 34 %.Divide with XRD
It is aluminum phosphate mullite that analysis records the crystalline phase of Ceramic Balls.
Embodiment 3
Mullite Powder, alumina powder, biphosphate aluminium powder, frit powder is 2:1:3.11:0.03's according to mass ratio
Ratio is dry mixed;Wherein, containing 50 wt% lithium oxides, the sodium oxide of 30 wt% and the silicon dioxide of 20 wt% in frit;Control
The mean diameter of Mullite Powder processed and oxide powder is all 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron,
The mean diameter of frit powder is 0.7 micron;Add concentration be the poly-vinyl alcohol solution of 8 wt% as binding agent, binding agent
Addition is the 5% of blank gross mass;Then pelletize, dry-pressing formed with 25 MPa pressure, prepare cylindric base substrate;Do at 70 DEG C
Dry base substrate is after 5 hours, base substrate is put in inner bottom part is the alumina crucible that semicircle is spherical, with 5 DEG C/min under air atmosphere
Speed heat to 150 DEG C and be incubated 2 hours, then heat to 380 DEG C with the speed of 20 DEG C/min and be incubated 1
Individual hour, then heat to 680 DEG C with the speed of 1 DEG C/min and be incubated 2 hours, finally adding with the speed of 5 DEG C/min
Heat is warmed up to 1150 DEG C and is incubated 2 hours, naturally cools to room temperature subsequently, i.e. prepares light porous aluminum phosphate mullite
Ceramic Balls.The bulk density recording porous ceramic ball with Archimedes method is 0.91g/cm3, open pore rate is 32 %.Divide with XRD
It is aluminum phosphate mullite that analysis records the crystalline phase of Ceramic Balls.
Claims (3)
1. the preparation method of a light porous aluminum phosphate mullite ceramic ball, it is characterised in that use following steps: (1)
Mullite Powder, alumina powder, biphosphate aluminium powder, frit powder is the ratio of 2:1:3.11:0.03 according to mass ratio
It is dry mixed;Wherein, containing 50 wt% lithium oxides, the sodium oxide of 30 wt% and the silicon dioxide of 20 wt% in frit;(2) add
Concentration be the poly-vinyl alcohol solution of 8 wt% as binding agent, the addition of binding agent is the 5% of blank gross mass;Then pelletize,
Molding, prepares cylindric base substrate;(3) after 70 DEG C of dry base substrates 5 hours, it is the oxygen that semicircle is spherical that base substrate is put into inner bottom part
Change in aluminum crucible, under air atmosphere, heat to 150 DEG C with the speed of 5 DEG C/min and be incubated 2 hours, then with 10-20
DEG C/speed of min heats to 380 DEG C and is incubated 1 hour, then heats to 680 with the speed of 1 DEG C/min
DEG C and be incubated 2 hours, finally heat to 1150 DEG C with the speed of 5 DEG C/min and be incubated 2 hours, natural cooling subsequently
To room temperature, i.e. prepare light porous aluminum phosphate mullite ceramic ball.
The preparation method of a kind of light porous aluminum phosphate mullite ceramic ball the most as claimed in claim 1, it is characterised in that:
Mullite Powder and the mean diameter of oxide powder in step (1) are all 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is
0.5 micron, the mean diameter of frit powder is 0.7 micron.
The preparation method of a kind of light porous aluminum phosphate mullite ceramic ball the most as claimed in claim 1, it is characterised in that:
Molding in step (2) refers to carry out dry-pressing formed to powder body, and briquetting pressure is 10-25MPa.
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CN112299833A (en) * | 2020-09-30 | 2021-02-02 | 蒙娜丽莎集团股份有限公司 | High-strength high-toughness mullite ceramic sheet and preparation method thereof |
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CN1091764A (en) * | 1993-02-19 | 1994-09-07 | 胡小弟 | The high temperature compound binding agent |
CN102503510A (en) * | 2011-11-03 | 2012-06-20 | 杭州中亚新材料科技有限公司 | Production process for firing alumina foamed ceramic filter board in roller kiln |
CN103396150A (en) * | 2013-07-30 | 2013-11-20 | 河南煤业化工集团研究院有限责任公司 | Method for preparing foam ceramic self-insulation wall material by utilizing solid wastes |
CN103467123A (en) * | 2013-09-02 | 2013-12-25 | 安徽瑞泰新材料科技有限公司 | Silicon-rich mullite lightweight aggregate and preparation method thereof |
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- 2016-05-04 CN CN201610283659.1A patent/CN105948793B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1091764A (en) * | 1993-02-19 | 1994-09-07 | 胡小弟 | The high temperature compound binding agent |
CN102503510A (en) * | 2011-11-03 | 2012-06-20 | 杭州中亚新材料科技有限公司 | Production process for firing alumina foamed ceramic filter board in roller kiln |
CN103396150A (en) * | 2013-07-30 | 2013-11-20 | 河南煤业化工集团研究院有限责任公司 | Method for preparing foam ceramic self-insulation wall material by utilizing solid wastes |
CN103467123A (en) * | 2013-09-02 | 2013-12-25 | 安徽瑞泰新材料科技有限公司 | Silicon-rich mullite lightweight aggregate and preparation method thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112299833A (en) * | 2020-09-30 | 2021-02-02 | 蒙娜丽莎集团股份有限公司 | High-strength high-toughness mullite ceramic sheet and preparation method thereof |
CN112299833B (en) * | 2020-09-30 | 2022-06-17 | 蒙娜丽莎集团股份有限公司 | High-strength high-toughness mullite ceramic sheet and preparation method thereof |
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