CN105924218B - A kind of preparation method of light porous aluminum phosphate-quartz-ceramics ball - Google Patents

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

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CN105924218B
CN105924218B CN201610283751.8A CN201610283751A CN105924218B CN 105924218 B CN105924218 B CN 105924218B CN 201610283751 A CN201610283751 A CN 201610283751A CN 105924218 B CN105924218 B CN 105924218B
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aluminum phosphate
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CN105924218A (en
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白佳海
高杰
刘俊成
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Shandong University of Technology
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Abstract

A kind of preparation method of light porous aluminum phosphate quartz Ceramic Balls, it is characterised in that using following steps:(1)SiO 2 powder, alumina powder, biphosphate aluminium powder, frit powder carries out dry-mixed;(2)It is granulated, shaping, cylindric green body is made;(3)After when 70 DEG C of dry base substrates 5 are small, green body is put into the alumina crucible that interior bottom is semicircle spherical shape, when heating to 150 DEG C and small heat preservation 2 under air atmosphere with the speed of 5 DEG C/min, 380 DEG C are heated to the speed of 10 20 DEG C/min and keep the temperature 1 hour again, when then heating to 680 DEG C and small heat preservation 2 with the speed of 1 DEG C/min, finally 1150 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, that is, light porous aluminum phosphate quartz Ceramic Balls are made.

Description

A kind of preparation method of light porous aluminum phosphate-quartz-ceramics ball
Technical field
The present invention is to provide a kind of preparation methods of light porous aluminum phosphate-quartz-ceramics ball, belong to special cermacis material Expect preparing technical field.
Technical field
The present invention is to provide a kind of preparation methods of light porous aluminum phosphate-quartz-ceramics ball, belong to special cermacis material Expect preparing technical field.
Background technology
Porous alumionphosphate (AlPO4)-quartz(SiO2) Ceramic Balls being widely used in the industrial production be general, it can conduct Catalyst carrier, chemical filler, heat preservation and refractory material etc..It is carried as carrier of photocatalyst and other liquid phase reactor catalyst Body and as in water during the adsorbent of noxious material, in order to ensure with efficient catalytic effect and(Or)Adsorption efficiency, it is past Toward requiring porous ceramic ball in water in suspended state, this just needs to prepare a kind of light porous ceramic ball.At present, both at home and abroad " core " of the sphere made of the organic matter for easily burning and losing as spherical green body is mainly used, it is then spherical organic by burning till removing " core ", so as to prepare a kind of suspensible porous ceramics hollow ball.The disadvantages of this method is:Shaping is more difficult, and in organic matter It burns during losing, easily lead to ceramics cracking or destroys, reduce the yield rate of product;In addition, this technical process is more complicated, into This higher, deficiency in economic performance, environment easy to pollute.In order to overcome above-mentioned problem, invention provides a kind of efficient, simple, peaces Entirely, operation, the preparation method of low-cost light porous aluminum phosphate-quartz-ceramics ball are reliable, easy to.
The content of the invention
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-quartz-ceramics ball, technical solution are:
A kind of preparation method of light porous aluminum phosphate-quartz-ceramics ball, it is characterised in that using following steps:(1) SiO 2 powder, alumina powder, biphosphate aluminium powder, frit powder are 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 that concentration is 8 wt%, the additive amount of binding agent is the 5% of blank gross mass as binding agent;Then make Grain, shaping, are made cylindric green body;(3)After when 70 DEG C of dry base substrates 5 are small, green body is put into interior bottom as semicircle spherical shape In alumina crucible, when heating to 150 DEG C and small heat preservation 2 under air atmosphere with the speed of 5 DEG C/min, 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 keep the temperature 2 it is small when, finally heat to 1150 DEG C with the speed of 5 DEG C/min and keep the temperature 2 hours, it is then natural Room temperature is cooled to, that is, light porous aluminum phosphate-quartz-ceramics ball is made.
A kind of preparation method of the light porous aluminum phosphate-quartz-ceramics ball, it is characterised in that:Step(1)In The average grain diameter of SiO 2 powder 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.
A kind of preparation method of the light porous aluminum phosphate-quartz-ceramics ball, it is characterised in that:Step(2)In Shaping refers to carrying out dry-pressing formed, briquetting pressure 10-25MPa to powder.
Fig. 1 is that light porous aluminum phosphate-quartz-ceramics ball prepared by the technology of the present invention floats on photo in water;From figure It can be seen that:Aluminum phosphate-quartz-ceramics ball is floated in water, illustrates that the bulk density of aluminum phosphate-quartz-ceramics ball is less than water Material prepared by density, i.e. 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, Keep the temperature 2 it is small when after, aluminium dihydrogen phosphate is changed into as liquid, be then heated rapidly to 380 DEG C and keep the temperature 1 it is small when, 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 as a kind of very big viscous body 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-stone with carbonic acid reactive magnesium English, and vapor and carbon dioxide etc. play an important role of pore-forming, can thus prepare light porous aluminum phosphate-quartz-ceramics.
Specific embodiment
Embodiment 1
SiO 2 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, 50 wt% lithias, the sodium oxide molybdena of 30 wt% and 20 wt% are contained in frit Silica;It is 0.6 micron to control the average grain diameter of SiO 2 powder and oxide powder, aluminium dihydrogen phosphate powder average particle size For 0.5 micron, the average grain diameter of frit powder is 0.7 micron;It adds the poly-vinyl alcohol solution that concentration is 8 wt% and is used as bonding Agent, the additive amount of binding agent are the 5% of blank gross mass;Then it is granulated, is dry-pressing formed with 10MPa pressure, cylindric base is made Body;After when 70 DEG C of dry base substrates 5 are small, green body is put into the alumina crucible that interior bottom is semicircle spherical shape, in air atmosphere Under with the speed of 5 DEG C/min heat to 150 DEG C and keep the temperature 2 it is small when, then heated to the speed of 10 DEG C/min 380 DEG C and 1 hour of heat preservation, when then heating to 680 DEG C and small heat preservation 2 with the speed of 1 DEG C/min, finally with 5 DEG C/speed of min heats to 1150 DEG C and keeps the temperature 2 hours, room temperature is then naturally cooled to, that is, is made light porous Aluminum phosphate-SiO 2-ceramic ball.The bulk density that porous ceramic ball is measured with Archimedes method is 0.96 g/cm3, open pore Rate is 32 %.The crystalline phase that Ceramic Balls are measured with XRD analysis is aluminum phosphate and silica.
Embodiment 2
SiO 2 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;Controlling the average grain diameter of SiO 2 powder and oxide powder, aluminium dihydrogen phosphate powder average particle size is 0.5 for 0.6 micron Micron, the average grain diameter of frit powder is 0.7 micron;The poly-vinyl alcohol solution that addition concentration is 8 wt% is bonded as binding agent The additive amount of agent is the 5% of blank gross mass;Then it is granulated, is dry-pressing formed with 20MPa pressure, cylindric green body is made;70 After when DEG C dry base substrate 5 is small, green body is put into the alumina crucible that interior bottom is semicircle spherical shape, with 5 under air atmosphere DEG C/speed of min heat to 150 DEG C and keep the temperature 2 it is small when, then heat to 380 DEG C simultaneously with the speed of 15 DEG C/min 1 hour is kept the temperature, when then heating to 680 DEG C and small heat preservation 2 with the speed of 1 DEG C/min, finally with 5 DEG C/min's Speed heats to 1150 DEG C and keeps the temperature 2 hours, then naturally cools to room temperature, that is, light porous aluminum phosphate-two is made Silicon oxide ceramics ball.The bulk density that porous ceramic ball is measured with Archimedes method is 0.93 g/cm3, open pore rate is 34 %. The crystalline phase that Ceramic Balls are measured with XRD analysis is aluminum phosphate and silica.
Embodiment 3
SiO 2 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 SiO 2 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;Poly-vinyl alcohol solution that concentration is 8 wt% is added as binding agent, The additive amount of binding 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; After when 70 DEG C of dry base substrates 5 are small, green body is put into the alumina crucible that interior bottom is semicircle spherical shape, under air atmosphere With the speed of 5 DEG C/min heat to 150 DEG C and keep the temperature 2 it is small when, then with the speed of 20 DEG C/min heat to 380 DEG C and keep the temperature 1 hour, then with the speed of 1 DEG C/min heat to 680 DEG C and keep the temperature 2 it is small when, finally with 5 DEG C/ The speed of min heats to 1150 DEG C and keeps the temperature 2 hours, then naturally cools to room temperature, that is, light porous phosphoric acid is made Aluminium-SiO 2-ceramic ball.The bulk density that porous ceramic ball is measured with Archimedes method is 0.94g/cm3, open pore rate is 35 %.The crystalline phase that Ceramic Balls are measured with XRD analysis is aluminum phosphate and silica.

Claims (2)

1. a kind of preparation method of light porous aluminum phosphate-quartz-ceramics ball, it is characterised in that using following steps:(1)Two Silicon oxide 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 two The average grain diameter of silicon oxide powder and alumina powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micron, is melted The average grain diameter of block powder is 0.7 micron;(2)Addition concentration is the poly-vinyl alcohol solution of 8 wt% as binding agent, binding agent Additive amount be the 5% of blank gross mass;Then it is granulated, is molded, cylindric green body is made;(3)When 70 DEG C of dry base substrates 5 are small 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 When being warming up to 150 DEG C and small heat preservation 2, then heat to 380 DEG C with the speed of 10-20 DEG C/min and keep the temperature 1 hour, When then heating to 680 DEG C and small heat preservation 2 with the speed of 1 DEG C/min, finally with the speed heat temperature raising of 5 DEG C/min To 1150 DEG C and 2 hours are kept the temperature, then naturally cool to room temperature, that is, light porous aluminum phosphate-quartz-ceramics ball is made.
2. a kind of preparation method of light porous aluminum phosphate-quartz-ceramics ball as described in claim 1, it is characterised in that:Step Suddenly(2)In shaping refer to powder carry out dry-pressing formed, briquetting pressure 10-25MPa.
CN201610283751.8A 2016-05-04 2016-05-04 A kind of preparation method of light porous aluminum phosphate-quartz-ceramics ball Expired - Fee Related CN105924218B (en)

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CN116082030A (en) * 2022-12-26 2023-05-09 广西产研院新型功能材料研究所有限公司 Aluminum phosphate ceramic produced by using unpurified wet-process phosphoric acid, and method and application thereof

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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