CN105837249A - Preparation method of light porous aluminum phosphate-zinc ferrite ceramic balls - Google Patents

Preparation method of light porous aluminum phosphate-zinc ferrite ceramic balls Download PDF

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CN105837249A
CN105837249A CN201610283608.9A CN201610283608A CN105837249A CN 105837249 A CN105837249 A CN 105837249A CN 201610283608 A CN201610283608 A CN 201610283608A CN 105837249 A CN105837249 A CN 105837249A
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powder
zinc ferrite
speed
ceramic balls
aluminum phosphate
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CN105837249B (en
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白佳海
高杰
杜庆洋
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Shandong University of Technology
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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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
    • C04B35/26—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 ferrites
    • C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/447—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 phosphates, e.g. hydroxyapatite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • 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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Abstract

The invention discloses a preparation method of light porous aluminum phosphate-zinc ferrite ceramic balls .The preparation method is characterized by including the following steps that 1, zinc ferrite powder, aluminum oxide powder, aluminum dihydrogen phosphate powder and frit powder are subjected to dry mixing in proportion; 2, granulating and forming are carried out, and a cylindrical blank is obtained; 3, the blank is dried for 5 h at 70 DEG C and then put into an aluminum oxide crucible with the inner bottom in a hemisphere shape, the temperature is raised to 150 DEG C at the speed of 5 DEG C/min through heating under the air atmosphere and maintained for 2 h, then the temperature is raised to 380 DEG C at the speed of 10-20 DEG C/min through heating and maintained for 1 h, then the temperature is raised to 680 DEG C at the speed of 1 DEG C/min through heating and maintained for 2 h, finally the temperature is raised to 1150 DEG C at the speed of 5 DEG C/min through heating and maintained for 2 h, then the temperature is decreased to the room temperature through natural cooling, and the light porous aluminum phosphate-zinc ferrite ceramic balls are obtained.

Description

A kind of preparation method of light porous aluminum phosphate zinc ferrite Ceramic Balls
Technical field
The present invention is to provide the preparation method of a kind of light porous aluminum phosphate zinc ferrite Ceramic Balls, belong to special cermacis Technical field of material.
Background technology
Porous alumionphosphate (AlPO4) zinc ferrite (ZnFe2O4) Ceramic Balls application in the industrial production widely, can Using as catalyst carrier, chemical filler, insulation and refractory material etc..Urging as carrier of photocatalyst and other liquid phase reactors Agent carrier, and as in water during the adsorbent of noxious material, in order to ensure, there is efficient catalytic effect and (or) absorption Efficiency, often requires that porous ceramic ball is in suspended state in water, and this is accomplished by preparing a kind of light porous ceramic ball.Mesh Before, the domestic and international spheroid using the organic matter easily burning mistake to make that is mainly, as " core " of spherical base substrate, then passes through to burn till to remove Go spherical organic " core ", thus prepare a kind of suspensible porous ceramics hollow ball.The shortcoming of the method is: be molded more difficult, And during organic matter burns and loses, be easily caused pottery cracking or destroy, reducing the yield rate of product；Additionally, this technique mistake Journey is more complicated, relatively costly, deficiency in economic performance, easily pollutes environment.In order to overcome an above-mentioned difficult problem, invention provides a kind of high Effect, the preparation method of light porous aluminum phosphate zinc ferrite Ceramic Balls simple, safe and reliable, easily operated, with low cost.
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 aluminium zinc ferrite Ceramic Balls, its technical scheme is:
The preparation method of a kind of light porous aluminum phosphate zinc ferrite Ceramic Balls, it is characterised in that use following steps: (1) is iron Acid zinc 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% lithias, the sodium oxide molybdena of 30 wt% and the silica 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 granulation, 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 aluminium 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, the most naturally cooling To room temperature, i.e. prepare light porous aluminum phosphate zinc ferrite Ceramic Balls.
The preparation method of described a kind of light porous aluminum phosphate zinc ferrite Ceramic Balls, it is characterised in that: in step (1) Zinc ferrite powder and the average grain diameter of oxide powder be all 0.6 micron, aluminium dihydrogen phosphate powder average particle size is 0.5 micron, The average grain diameter of frit powder is 0.7 micron.
The preparation method of described a kind of light porous aluminum phosphate zinc ferrite Ceramic Balls, it is characterised in that: in step (2) Shaping refer to carry out dry-pressing formed to powder, briquetting pressure is 10-25MPa.
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 efficiency 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 phosphoric acid, the phosphoric acid of generation can react with magnesium carbonate and generate aluminum phosphate zinc ferrite, and steam and dioxy Change carbon etc. and there is the effect of pore-forming, thus can prepare light porous aluminum phosphate zinc ferrite pottery.
Detailed description of the invention
Embodiment 1
Zinc ferrite 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% lithias, the sodium oxide molybdena of 30 wt% and the silica of 20 wt% in frit； The average grain diameter controlling zinc ferrite powder and oxide powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, The average grain 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 granulation, 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 zinc ferrite Ceramic Balls.The bulk density recording porous ceramic ball with Archimedes method is 0.93 g/cm3, open pore rate is 38 %.Use XRD It is aluminum phosphate and zinc ferrite that analysis records the crystalline phase of Ceramic Balls.
Embodiment 2
Zinc ferrite 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% lithias, the sodium oxide molybdena of 30 wt% and the silica of 20 wt% in frit；Control The average grain diameter of zinc ferrite powder processed and oxide powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, molten The average grain 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 granulation, 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 zinc ferrite pottery Porcelain ball.The bulk density recording porous ceramic ball with Archimedes method is 0.93 g/cm3, open pore rate is 36 %.Divide with XRD It is aluminum phosphate zinc ferrite that analysis records the crystalline phase of Ceramic Balls.
Embodiment 3
Zinc ferrite 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% lithias, the sodium oxide molybdena of 30 wt% and the silica of 20 wt% in frit；Control The average grain diameter of zinc ferrite powder processed and oxide powder is all 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, The average grain 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 granulation, 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 zinc ferrite Ceramic Balls.The bulk density recording porous ceramic ball with Archimedes method is 0.95g/cm3, open pore rate is 34 %.Divide with XRD It is aluminum phosphate zinc ferrite that analysis records the crystalline phase of Ceramic Balls.

Claims (3)

1. the preparation method of a light porous aluminum phosphate zinc ferrite Ceramic Balls, it is characterised in that use following steps: (1) Zinc ferrite 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% lithias, the sodium oxide molybdena of 30 wt% and the silica 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 granulation, Shaping, 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 aluminium 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, the most naturally cooling To room temperature, i.e. prepare light porous aluminum phosphate zinc ferrite Ceramic Balls.
2. the preparation method of a kind of light porous aluminum phosphate zinc ferrite Ceramic Balls as described in claim 1, it is characterised in that: Zinc ferrite powder and the average grain 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 average grain diameter of frit powder is 0.7 micron.
3. the preparation method of a kind of light porous aluminum phosphate zinc ferrite Ceramic Balls as described in claim 1, it is characterised in that: Shaping in step (2) refers to carry out dry-pressing formed to powder, and briquetting pressure is 10-25MPa.
CN201610283608.9A 2016-05-04 2016-05-04 A kind of preparation method of light porous aluminum phosphate-zinc ferrite Ceramic Balls Expired - Fee Related CN105837249B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116477966A (en) * 2023-04-26 2023-07-25 深圳市博迪科技开发有限公司 Preparation method of hydroxyapatite-based porous ceramic without powder falling

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85100057A (en) * 1985-04-01 1986-07-23 清华大学 High-temperature strain sustainable adhesive
US6022513A (en) * 1996-10-31 2000-02-08 Pecoraro; Theresa A. Aluminophosphates and their method of preparation
CN101242948A (en) * 2005-06-27 2008-08-13 应用薄膜股份有限公司 Aluminum phosphate based microspheres
CN104311109A (en) * 2014-10-09 2015-01-28 山东理工大学 Method for preparing foamed ceramic through foaming, injection molding and cementing of aluminum dihydrogen phosphate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85100057A (en) * 1985-04-01 1986-07-23 清华大学 High-temperature strain sustainable adhesive
US6022513A (en) * 1996-10-31 2000-02-08 Pecoraro; Theresa A. Aluminophosphates and their method of preparation
CN101242948A (en) * 2005-06-27 2008-08-13 应用薄膜股份有限公司 Aluminum phosphate based microspheres
CN104311109A (en) * 2014-10-09 2015-01-28 山东理工大学 Method for preparing foamed ceramic through foaming, injection molding and cementing of aluminum dihydrogen phosphate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116477966A (en) * 2023-04-26 2023-07-25 深圳市博迪科技开发有限公司 Preparation method of hydroxyapatite-based porous ceramic without powder falling

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