CN105948796B - A kind of preparation method of light porous aluminum phosphate-alumina titanate ceramics ball - Google Patents

A kind of preparation method of light porous aluminum phosphate-alumina titanate ceramics ball Download PDF

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CN105948796B
CN105948796B CN201610283698.1A CN201610283698A CN105948796B CN 105948796 B CN105948796 B CN 105948796B CN 201610283698 A CN201610283698 A CN 201610283698A CN 105948796 B CN105948796 B CN 105948796B
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白佳海
高杰
何静
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Shandong University of Technology
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Abstract

A kind of preparation method of light porous aluminum phosphate-alumina titanate ceramics ball, it is characterised in that using following steps:(1)Aluminum titanate powder, 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 of dry base substrates 5 hours, 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, 380 DEG C are heated to the speed of 10 20 DEG C/min and keep the temperature 1 hour again, then 680 DEG C are heated to the speed of 1 DEG C/min and keeps the temperature 2 hours, finally 1100 DEG C are heated to the speed of 5 DEG C/min and keep the temperature 2 hours, room temperature then is naturally cooled to, obtains light porous aluminum phosphate-alumina titanate ceramics ball.

Description

A kind of preparation method of light porous aluminum phosphate-alumina titanate ceramics ball
Technical field
The present invention is to provide a kind of preparation methods of light porous aluminum phosphate-alumina titanate ceramics ball, belong to special cermacis Technical field of material.
Background technology
Porous alumionphosphate(AlPO4)- aluminium titanates(Al2TiO5) Ceramic Balls being widely used in the industrial production be general, it can Using as catalyst carrier, chemical filler, heat preservation and refractory material etc..It is urged 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 with efficient catalytic effect and(Or)Absorption Efficiency often requires that porous ceramic ball in water in suspended state, this just needs to prepare a kind of light porous ceramic ball.Mesh Before, it is mainly then removed both at home and abroad using " core " of the sphere made of the organic matter lost as spherical green body is easily burnt by firing 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 more difficult, And during organic matter burns and loses, easily lead to ceramics cracking or destroy, reduce the yield rate of product;In addition, this technique mistake Journey is more complicated, and cost is higher, deficiency in economic performance, environment easy to pollute.In order to overcome above-mentioned problem, invention provides a kind of high Effect, the preparation method of simple, safe and reliable, easily operated, low-cost light porous aluminum phosphate-alumina titanate ceramics ball.
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-alumina titanate ceramics ball, technical solution are:
A kind of preparation method of light porous aluminum phosphate-alumina titanate ceramics ball, it is characterised in that using following steps:(1) Aluminum titanate powder, alumina powder, biphosphate aluminium powder, frit powder is 2 according to mass ratio:1:3.11:0.03 ratio Example 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 Adding the poly-vinyl alcohol solution of a concentration of 8 wt%, the additive amount of binding agent is the 5% of blank gross mass as binding agent;Then it makes Grain, molding, are made cylindric green body;(3)After 70 DEG C of dry base substrates 5 hours, it is for semicircle spherical that green body is put into interior bottom In alumina crucible, 150 DEG C are heated to the speed of 5 DEG C/min under air atmosphere and keep the temperature 2 hours, then with 10- The speed of 20 DEG C/min heats to 380 DEG C and keeps the temperature 1 hour, is then heated to the speed of 1 DEG C/min 680 DEG C and 2 hours are kept the temperature, finally heat to 1100 DEG C with the speed of 5 DEG C/min and keeps the temperature 2 hours, it is then natural Room temperature is cooled to, obtains light porous aluminum phosphate-alumina titanate ceramics ball.
A kind of preparation method of the light porous aluminum phosphate-alumina titanate ceramics ball, it is characterised in that:Step(1)In Aluminum titanate powder and oxide powder average grain diameter all for 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.
A kind of preparation method of the light porous aluminum phosphate-alumina titanate ceramics ball, it is characterised in that:Step(2)In Molding refer to powder carry out dry-pressing formed, briquetting pressure 10-25MPa.
Fig. 1 is the photo that light porous aluminum phosphate-alumina titanate ceramics ball prepared by the technology of the present invention floats on the water surface;From It can see in figure:Aluminum phosphate-alumina titanate ceramics ball is floated in water, illustrates that the volume of aluminum phosphate-alumina titanate ceramics 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 phosphoric acid are decomposed into, the phosphoric acid of generation can be reacted with magnesium carbonate generates aluminum phosphate-aluminium titanates, and vapor There is pore-forming with carbon dioxide etc., can thus prepare light porous aluminum phosphate-alumina titanate ceramics.
Specific embodiment
Embodiment 1
Aluminum titanate powder, alumina powder, biphosphate aluminium powder, frit powder is 2 according to mass ratio:1:3.11: 0.03 ratio carries out dry-mixed;Wherein, the titanium dioxide containing 50 wt% lithias, the sodium oxide molybdena of 30 wt% and 20 wt% in frit Silicon;It is 0.6 micron to control the average grain diameter of aluminum titanate powder and oxide powder, and aluminium dihydrogen phosphate powder average particle size is micro- for 0.5 Rice, the average grain diameter of frit powder is 0.7 micron;The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binding agent, binding agent Additive amount be the 5% of blank gross mass;Then it is granulated, is dry-pressing formed with 10MPa pressure, cylindric green body is made;At 70 DEG C After dry base substrate 5 hours, green body be put into interior bottom be semicircle spherical shape alumina crucible in, under air atmosphere with 5 DEG C/ The speed of min heats to 150 DEG C and keeps the temperature 2 hours, then heat to 380 DEG C with the speed of 10 DEG C/min and protect Then warm 1 hour heats to 680 DEG C with the speed of 1 DEG C/min and keeps the temperature 2 hours, finally with the speed of 5 DEG C/min Degree heats to 1100 DEG C and keeps the temperature 2 hours, then naturally cools to room temperature, obtains light porous aluminum phosphate-titanium Sour aluminium Ceramic Balls.The bulk density that porous ceramic ball is measured with Archimedes method is 0.94 g/cm3, open pore rate is 36 %.With The crystalline phase that XRD analysis measures Ceramic Balls is aluminum phosphate-aluminium titanates.
Embodiment 2
Aluminum titanate powder, alumina powder, biphosphate aluminium powder, frit powder are 2 according to mass ratio:1:3.11: 0.03 ratio carries out dry-mixed;Wherein, the titanium dioxide containing 50 wt% lithias, the sodium oxide molybdena of 30 wt% and 20 wt% in frit Silicon;It is 0.6 micron to control the average grain diameter of aluminum titanate powder and oxide powder, and aluminium dihydrogen phosphate powder average particle size is micro- for 0.5 Rice, the average grain diameter of frit powder is 0.7 micron;The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binding agent, binding agent Additive amount be the 5% of blank gross mass;Then it is granulated, is dry-pressing formed with 20MPa pressure, cylindric green body is made;At 70 DEG C After dry base substrate 5 hours, green body be put into interior bottom be semicircle spherical shape alumina crucible in, under air atmosphere with 5 DEG C/ The speed of min heats to 150 DEG C and keeps the temperature 2 hours, then heat to 380 DEG C with the speed of 15 DEG C/min and protect Then warm 1 hour heats to 680 DEG C with the speed of 1 DEG C/min and keeps the temperature 2 hours, finally with the speed of 5 DEG C/min Degree heats to 1100 DEG C and keeps the temperature 2 hours, then naturally cools to room temperature, obtains light porous aluminum phosphate-titanium Sour aluminium Ceramic Balls.The bulk density that porous ceramic ball is measured with Archimedes method is 0.95 g/cm3, open pore rate 35%.With The crystalline phase that XRD analysis measures Ceramic Balls is aluminum phosphate-aluminium titanates.
Embodiment 3
Aluminum titanate powder, alumina powder, biphosphate aluminium powder, frit powder are 2 according to mass ratio:1:3.11: 0.03 ratio carries out dry-mixed;Wherein, the titanium dioxide containing 50 wt% lithias, the sodium oxide molybdena of 30 wt% and 20 wt% in frit Silicon;It is all 0.6 micron to control the average grain diameter of aluminum titanate powder and oxide powder, and aluminium dihydrogen phosphate powder average particle size is 0.5 Micron, the average grain diameter of frit powder is 0.7 micron;The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binding agent, is bonded The additive amount of agent is the 5% of blank gross mass;Then it is granulated, is dry-pressing formed with 25 MPa pressure, cylindric green body is made;70 DEG C dry base substrate is put into green body in the alumina crucible that interior bottom is semicircle spherical shape, after 5 hours with 5 under air atmosphere DEG C/speed of min heats to 150 DEG C and keeps the temperature 2 hours, then heat to 380 DEG C simultaneously with the speed of 20 DEG C/min 1 hour is kept the temperature, then heat to 680 DEG C with the speed of 1 DEG C/min and keeps the temperature 2 hours, finally with 5 DEG C/min's Speed heat to 1100 DEG C and keep the temperature 2 hours, then naturally cool to room temperature, obtain light porous aluminum phosphate- Alumina titanate ceramics ball.The bulk density that porous ceramic ball is measured with Archimedes method is 0.96g/cm3, open pore rate is 36 %. The crystalline phase that Ceramic Balls are measured with XRD analysis is aluminum phosphate-aluminium titanates.

Claims (2)

1. a kind of preparation method of light porous aluminum phosphate-alumina titanate ceramics ball, it is characterised in that using following steps:(1) Aluminum titanate powder, alumina powder, biphosphate aluminium powder, frit powder are 2 according to mass ratio:1:3.11:0.03 ratio It carries out dry-mixed;Wherein, the silica containing 50 wt% lithias, the sodium oxide molybdena of 30 wt% and 20 wt% in frit;Control titanium The average grain diameter of sour aluminium powder and alumina powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, frit The average grain diameter of powder is 0.7 micron;(2)The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binding agent, binding agent Additive amount is the 5% of blank gross mass;Then it is granulated, is molded, cylindric green body is made;(3)In 70 DEG C of dry base substrates 5 hours Afterwards, green 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 It is warming up to 150 DEG C and keeps the temperature 2 hours, then heat to 380 DEG C with the speed of 10-20 DEG C/min and keep 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 with the speed heat temperature raising of 5 DEG C/min To 1100 DEG C and 2 hours are kept the temperature, room temperature is then naturally cooled to, obtains light porous aluminum phosphate-alumina titanate ceramics ball.
2. a kind of preparation method of light porous aluminum phosphate-alumina titanate ceramics 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.
CN201610283698.1A 2016-05-04 2016-05-04 A kind of preparation method of light porous aluminum phosphate-alumina titanate ceramics ball Expired - Fee Related CN105948796B (en)

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Citations (3)

* 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
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 (3)

* 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
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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