CN105948791B - A kind of preparation method of light porous aluminum phosphate-aluminium oxide ceramic ball - Google Patents

A kind of preparation method of light porous aluminum phosphate-aluminium oxide ceramic ball Download PDF

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CN105948791B
CN105948791B CN201610283623.3A CN201610283623A CN105948791B CN 105948791 B CN105948791 B CN 105948791B CN 201610283623 A CN201610283623 A CN 201610283623A CN 105948791 B CN105948791 B CN 105948791B
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白佳海
高杰
李国昌
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Shandong University of Technology
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    • C04B35/63Preparing 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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Abstract

A kind of preparation method of light porous aluminum phosphate-aluminium oxide ceramic ball, it is characterised in that using following steps:(1)Alumina powder, biphosphate aluminium powder, frit powder carries out dry-mixed in proportion;(2)It is granulated, molding, cylindric green body is made;(3)After 70 DEG C 5 hours dry, green body is put into the alumina crucible that interior bottom is semicircle spherical shape, 150 DEG C are heated to the speed of 5 DEG C/min and keep the temperature 2 hours under air atmosphere, reheating is warming up to 380 DEG C and keeps the temperature 1 hour, then 680 DEG C are heated to the speed of 1 DEG C/min and keeps the temperature 2 hours, finally 1150 DEG C are heated to the speed of 5 DEG C/min and keep the temperature 2 hours, then naturally cool to room temperature, obtain light porous aluminum phosphate-aluminium oxide ceramic ball.

Description

A kind of preparation method of light porous aluminum phosphate-aluminium oxide ceramic ball
Technical field
The present invention is to provide a kind of preparation methods of light porous aluminum phosphate-aluminium oxide ceramic ball, belong to special cermacis Technical field of material.
Background technology
Porous light porous alumionphosphate-aluminium oxide ceramic ball being widely used in the industrial production is general, can be used as and urge Agent carrier, high-temperature filter, chemical filler, heat preservation and refractory material etc..Anti- as carrier of photocatalyst and other liquid phases Answer catalyst carrier and as in water during the adsorbent of noxious material, in order to ensure with efficient catalytic effect and(Or) Adsorption efficiency often requires that porous ceramic ball in water in suspended state, this just needs to prepare a kind of light porous ceramic ball. At present, then pass through firing mainly using " core " of the sphere made of the organic matter lost as spherical green body is easily burnt both at home and abroad Spherical organic " core " is removed, so as to prepare a kind of suspensible porous ceramics hollow ball.The disadvantages of this method is:Molding is relatively tired Difficulty, and during organic matter burns and loses, easily lead to ceramics cracking or destroy, reduce the yield rate of product;In addition, this technique Process is more complicated, and cost is higher, deficiency in economic performance, environment easy to pollute.In order to overcome above-mentioned problem, invention provides one kind Efficiently, the preparation method of simple, safe and reliable, easily operated, low-cost light porous aluminum phosphate-calcium silicates Ceramic Balls.
Invention content
The technology of the present invention provides a kind of efficient, simple, safe and reliable, easily operated, low-cost light porous phosphoric acid The preparation method of aluminium-aluminium oxide ceramic ball, technical solution are:
A kind of preparation method of light porous aluminum phosphate-aluminium oxide ceramic ball, it is characterised in that using following steps:(1) Alumina powder, biphosphate aluminium powder, frit powder is 3 according to mass ratio: 3.11:0.03 ratio carries out dry-mixed; Wherein, the silica containing 50 wt% lithias, the sodium oxide molybdena of 30 wt% and 20 wt% in frit;(2)Add a concentration of 8 For the poly-vinyl alcohol solution of wt% as binding agent, the additive amount of binding agent is the 5% of blank gross mass;Then it is granulated, is molded, be made Cylindric green body;(3)After 70 DEG C of dry base substrates 5 hours, green body is put into the alumina crucible that interior bottom is semicircle spherical shape It is interior, 150 DEG C are heated to the speed of 5 DEG C/min and keep the temperature 2 hours, then with 10-20 DEG C/min's under air atmosphere Speed heats to 380 DEG C and keeps the temperature 1 hour, then heats to 680 DEG C and heat preservation 2 with the speed of 1 DEG C/min Hour, finally 1150 DEG C are heated to the speed of 5 DEG C/min and keep the temperature 2 hours, then naturally cool to room temperature, i.e., Light porous aluminum phosphate-aluminium oxide ceramic ball is made.
A kind of preparation method of the light porous aluminum phosphate-alumina ball, it is characterised in that:Step(1)In The average grain diameter of alumina powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, and frit powder is averaged Grain size is 0.7 micron.
A kind of preparation method of the light porous aluminum phosphate-aluminium oxide ceramic ball, it is characterised in that:Step(2)In Molding refer to powder carry out dry-pressing formed, briquetting pressure 10-25MPa.
Description of the drawings
Fig. 1 is the photo that light porous aluminum phosphate-aluminium oxide ceramic ball prepared by the technology of the present invention suspends in water;From It can see in figure:Aluminum phosphate-aluminium oxide ceramic ball is floated in water, illustrates that the volume of aluminum phosphate-aluminium oxide ceramic ball is close Degree is less than the density of water, i.e., the material that prepared by the technology of the present invention belongs to light porous ceramic material.
The principle of this technology invention is as follows:
It is fusible at a lower temperature for liquid using aluminium dihydrogen phosphate, the then property of solidifiable again at relatively high temperatures It can so that green body is spontaneously formed in sintering process as sphere, and concrete principle is as follows:Aluminium dihydrogen phosphate be heated to 150 DEG C, After heat preservation 2 hours, aluminium dihydrogen phosphate is changed into as liquid, is then heated rapidly to 380 DEG C and keeps the temperature 1 hour, the purpose is to make Various raw materials form a kind of very big viscous body of viscosity at such a temperature.The effect for adding in frit is on the one hand can to promote raw material Melt the viscous body very big for a kind of viscosity, on the other hand can also increase surface tension so that viscous physical efficiency spontaneously form for Sphere.It is heated slowly to during 680 DEG C, aluminium dihydrogen phosphate is gradually solidified as solid;In temperature-rise period, aluminium dihydrogen phosphate meeting Aluminum phosphate, vapor and phosphorus pentoxide are decomposed into, the phosphorus pentoxide of generation can generate aluminum phosphate with partial oxidation reactive aluminum, And vapor has the function of pore-forming, can thus prepare light porous aluminum phosphate-aluminium oxide ceramic ball.
Specific embodiment
Embodiment 1
Alumina powder, biphosphate aluminium powder, frit powder is 3 according to mass ratio: 3.11:0.03 ratio into Row is dry-mixed;Wherein, the silica containing 50 wt% lithias, the sodium oxide molybdena of 30 wt% and 20 wt% in frit;Control oxidation The average grain diameter of aluminium powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, the average grain diameter of frit powder It is 0.7 micron;The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binding agent, the additive amount of binding agent is blank gross mass 5%;Then it is granulated, is dry-pressing formed with 10MPa pressure, cylindric green body is made;After 70 DEG C of dry base substrates 5 hours, base Body is put into the alumina crucible that interior bottom is semicircle spherical shape, is heated under air atmosphere with the speed of 5 DEG C/min 150 DEG C and keep the temperature 2 hours, then with the speed of 10 DEG C/min heat to 380 DEG C and keep the temperature 1 hour, then with 1 DEG C/speed of min heats to 680 DEG C and keeps the temperature 2 hours, finally 1150 DEG C are heated to the speed of 5 DEG C/min And 2 hours are kept the temperature, room temperature is then naturally cooled to, obtains light porous aluminum phosphate-aluminium oxide ceramic ball.Use A Ji meter The bulk density that moral method measures porous ceramic ball is 0.90 g/cm3, open pore rate is 36.5 %.Ceramic Balls are measured with XRD analysis Crystalline phase be aluminum phosphate and aluminium oxide.
Embodiment 2
Alumina powder, biphosphate aluminium powder, frit powder is 3 according to mass ratio: 3.11:0.03 ratio into Row is dry-mixed;Wherein, the silica containing 50 wt% lithias, the sodium oxide molybdena of 30 wt% and 20 wt% in frit;Control oxidation The average grain diameter of aluminium powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, the average grain diameter of frit powder It is 0.7 micron;The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binding agent, the additive amount of binding agent is blank gross mass 5%;Then it is granulated, is dry-pressing formed with 20MPa pressure, cylindric green body is made;After 70 DEG C of dry base substrates 5 hours, base Body is put into the alumina crucible that interior bottom is semicircle spherical shape, is heated under air atmosphere with the speed of 5 DEG C/min 150 DEG C and keep the temperature 2 hours, then with the speed of 15 DEG C/min heat to 380 DEG C and keep the temperature 1 hour, then with 1 DEG C/speed of min heats to 680 DEG C and keeps the temperature 2 hours, finally 1150 DEG C are heated to the speed of 5 DEG C/min And 2 hours are kept the temperature, room temperature is then naturally cooled to, obtains light porous aluminum phosphate-aluminium oxide ceramic ball.Use A Ji meter The bulk density that moral method measures porous ceramic ball is 0.91 g/cm3, open pore rate is 35.4 %.XRD analysis the result shows that:Pottery The crystalline phase of porcelain ball is aluminum phosphate and aluminium oxide.
Embodiment 3
Alumina powder, biphosphate aluminium powder, frit powder is 3 according to mass ratio: 3.11:0.03 ratio into Row is dry-mixed;Wherein, the silica containing 50 wt% lithias, the sodium oxide molybdena of 30 wt% and 20 wt% in frit;Control oxidation The average grain diameter of aluminium powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, the average grain diameter of frit powder It is 0.7 micron;The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binding agent, the additive amount of binding agent is blank gross mass 5%;Then it is granulated, is dry-pressing formed with 25 MPa pressure, cylindric green body is made;After 70 DEG C of dry base substrates 5 hours, base Body is put into the alumina crucible that interior bottom is semicircle spherical shape, is heated under air atmosphere with the speed of 5 DEG C/min 150 DEG C and keep the temperature 2 hours, then with the speed of 20 DEG C/min heat to 380 DEG C and keep the temperature 1 hour, then with 1 DEG C/speed of min heats to 680 DEG C and keeps the temperature 2 hours, finally 1150 DEG C are heated to the speed of 5 DEG C/min And 2 hours are kept the temperature, room temperature is then naturally cooled to, obtains light porous aluminum phosphate-aluminium oxide ceramic ball.Use A Ji meter The bulk density that moral method measures porous ceramic ball is 0.93 g/cm3, open pore rate is 34.3 %.Ceramic Balls are measured with XRD analysis Crystalline phase be aluminum phosphate and aluminium oxide.

Claims (2)

1. a kind of preparation method of light porous aluminum phosphate-aluminium oxide ceramic ball, it is characterised in that using following steps:(1) Alumina powder, biphosphate aluminium powder, frit powder are 3 according to mass ratio: 3.11:0.03 ratio carries out dry-mixed;Its In, the silica containing 50 wt% lithias, the sodium oxide molybdena of 30 wt% and 20 wt% in frit;Control the flat of alumina powder Equal grain size is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, and the average grain diameter of frit powder is 0.7 micron; (2)The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binding agent, the additive amount of binding agent is the 5% of blank gross mass;So It is granulated, is molded afterwards, cylindric green body is made;(3)After 70 DEG C of dry base substrates 5 hours, green body is put into interior bottom as semi-round ball In the alumina crucible of shape, 150 DEG C are heated to the speed of 5 DEG C/min under air atmosphere and keep the temperature 2 hours, then with The speed of 10-20 DEG C/min heats to 380 DEG C and keeps the temperature 1 hour, then with the speed heat temperature raising of 1 DEG C/min To 680 DEG C and 2 hours are kept the temperature, finally heat to 1150 DEG C with the speed of 5 DEG C/min and keeps the temperature 2 hours, then certainly Room temperature so is cooled to, obtains light porous aluminum phosphate-aluminium oxide ceramic ball.
2. a kind of preparation method of light porous aluminum phosphate-aluminium oxide ceramic ball as described in claim 1, it is characterised in that: Step(2)In molding refer to powder carry out dry-pressing formed, briquetting pressure 10-25MPa.
CN201610283623.3A 2016-05-04 2016-05-04 A kind of preparation method of light porous aluminum phosphate-aluminium oxide ceramic ball Expired - Fee Related CN105948791B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN105481464A (en) * 2014-09-19 2016-04-13 青岛百键城环保科技有限公司 Porous refractory material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN105481464A (en) * 2014-09-19 2016-04-13 青岛百键城环保科技有限公司 Porous refractory material and preparation method thereof

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