CN105924214B - A kind of preparation method of light porous aluminum phosphate-forsterite ceramics ball - Google Patents

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

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CN105924214B
CN105924214B CN201610283639.4A CN201610283639A CN105924214B CN 105924214 B CN105924214 B CN 105924214B CN 201610283639 A CN201610283639 A CN 201610283639A CN 105924214 B CN105924214 B CN 105924214B
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forsterite
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CN105924214A (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 aluminium phosphate magnesium olivine Ceramic Balls, it is characterised in that use following steps：（1）Forsterite 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 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, obtains light porous aluminium phosphate magnesium olivine Ceramic Balls.

Description

A kind of preparation method of light porous aluminum phosphate-forsterite ceramics ball
Technical field
The present invention is to provide a kind of preparation methods of light porous aluminum phosphate-forsterite ceramics ball, belong to Special clay Ceramic material preparing technical field.
Background technology
Porous forsterite（ZrSi2O4)-aluminum phosphate（AlPO4）Ceramic Balls being widely used in the industrial production is general, 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 when the adsorbent of noxious material, in order to ensure with efficient catalytic effect and（Or）Absorption Efficiency often requires that porous ceramic ball is in suspended state in water, this just needs to prepare a kind of light porous ceramic ball.Mesh Before, it is mainly then removed both at home and abroad by firing using " core " of the sphere made of the organic matter lost as spherical green body is easily burnt Spherical organic " core " is removed, 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 leads to ceramics cracking or destroy, reduce the yield rate of product；In addition, this technique mistake Journey is more complex, 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-forsterite 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-forsterite ceramics ball, technical solution are：
A kind of preparation method of light porous aluminum phosphate-forsterite ceramics ball, it is characterised in that use following steps： （1）Forsterite powder, alumina powder, biphosphate aluminium powder, frit powder is 2 according to mass ratio：1：3.11：0.03 Ratio carry out it is dry-mixed；Wherein, the silica containing 50 wt% lithias, the sodium oxide molybdena and 20 wt% of 30 wt% in frit； （2）The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binder, the additive amount of binder 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, it is semi-round ball that green body, which is put into interior bottom, 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 It so is cooled to room temperature, obtains light porous aluminum phosphate-forsterite ceramics ball.
A kind of preparation method of the light porous aluminum phosphate-forsterite ceramics ball, it is characterised in that：Step（1） In forsterite powder and the average grain diameter of oxide powder be all 0.6 micron, aluminium dihydrogen phosphate powder average particle size is 0.5 micro- The average grain diameter of rice, frit powder is 0.7 micron.
A kind of preparation method of the light porous aluminum phosphate-forsterite ceramics 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-forsterite ceramics ball prepared by the technology of the present invention floats in water；From It can see in figure：Aluminum phosphate-forsterite ceramics ball floats in water, illustrates the volume of aluminum phosphate-forsterite ceramics ball Density 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：
Using aluminium dihydrogen phosphate it is fusible at a lower temperature be liquid, then at relatively high temperatures again solidifiable property 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 prodigious viscous body of viscosity at such a temperature.The effect that frit is added is on the one hand can to promote raw material Melting be a kind of prodigious 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 It is decomposed into aluminum phosphate, vapor and phosphorus pentoxide, the phosphorus pentoxide of generation can generate aluminum phosphate-magnesium olive with magnesium carbonate reaction Olive stone, and vapor and carbon dioxide etc. have the function of pore-forming, can thus prepare light porous aluminum phosphate-forsterite pottery Porcelain.
Specific implementation mode
Embodiment 1
Forsterite 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；The average grain diameter for controlling forsterite powder and oxide powder is 0.6 micron, aluminium dihydrogen phosphate powder average particle size It it 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 bonding Agent, the additive amount of binder are the 5% of blank gross mass；Then it is granulated, is dry-pressing formed with 10MPa pressure, cylindric base is made Body；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, in air atmosphere Under heat to 150 DEG C with the speed of 5 DEG C/min and keep the temperature 2 hours, then heated to the speed of 10 DEG C/min Then 380 DEG C and 1 hour of heat preservation heat to 680 DEG C with the speed of 1 DEG C/min and keep the temperature 2 hours, 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, is obtained light porous Aluminum phosphate-forsterite ceramics ball.The bulk density that porous ceramic ball is measured with Archimedes method is 0.96 g/cm3, open pore Rate is 35 %.The crystalline phase that Ceramic Balls are measured with XRD analysis is aluminum phosphate and forsterite.
Embodiment 2
Forsterite 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 and 20 wt% of 30 wt% in frit Silicon；The average grain diameter for controlling forsterite powder and oxide powder is 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 The average grain diameter of micron, frit powder is 0.7 micron；The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binder, is bonded 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 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 15 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 heats to 1150 DEG C and keeps the temperature 2 hours, then naturally cools to room temperature, obtains light porous aluminum phosphate-magnesium Olivine Ceramic Balls.The bulk density that porous ceramic ball is measured with Archimedes method is 0.93 g/cm3, open pore rate is 37 %. The crystalline phase that Ceramic Balls are measured with XRD analysis is aluminum phosphate and forsterite.
Embodiment 3
Forsterite 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 and 20 wt% of 30 wt% in frit Silicon；The average grain diameter for controlling forsterite 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；The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binder, The additive amount of binder 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 70 DEG C of dry base substrates 5 hours, green body is put into the alumina crucible that interior bottom is semicircle spherical shape, under air atmosphere 150 DEG C are heated to the speed of 5 DEG C/min and keeps the temperature 2 hours, then heat to 380 with the speed of 20 DEG C/min 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 hours, 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, obtains light porous phosphoric acid Aluminium-forsterite ceramics ball.The bulk density that porous ceramic ball is measured with Archimedes method is 0.94g/cm3, open pore rate is 38 %.The crystalline phase that Ceramic Balls are measured with XRD analysis is aluminum phosphate and forsterite.

Claims (2)

1. a kind of preparation method of light porous aluminum phosphate-forsterite ceramics ball, it is characterised in that use following steps：（1） Forsterite 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 silica containing 50 wt% lithias, the sodium oxide molybdena and 20 wt% of 30 wt% in frit；Control The average grain diameter of forsterite powder and alumina powder processed is all 0.6 micron, and aluminium dihydrogen phosphate powder average particle size is 0.5 micro- The average grain diameter of rice, frit powder is 0.7 micron；（2）The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binder, is glued The additive amount for tying agent 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 After hour, green body is put into the alumina crucible that interior bottom is semicircle spherical shape, with the speed of 5 DEG C/min under air atmosphere It heats 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 small When, then 680 DEG C are heated to the speed of 1 DEG C/min and keep the temperature 2 hours, finally heated and risen with the speed of 5 DEG C/min Temperature is to 1150 DEG C and keeps the temperature 2 hours, then naturally cools to room temperature, obtains light porous aluminum phosphate-forsterite ceramics Ball.
2. a kind of preparation method of light porous aluminum phosphate-forsterite ceramics ball as described in claim 1, feature exist In：Step（2）In molding refer to powder carry out dry-pressing formed, briquetting pressure 10-25MPa.
CN201610283639.4A 2016-05-04 2016-05-04 A kind of preparation method of light porous aluminum phosphate-forsterite ceramics ball Expired - Fee Related CN105924214B (en)

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CN101928155A (en) * 2010-09-01 2010-12-29 中国地质大学（北京） Cordierite porous fireproofing material and preparation method thereof
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
CN101928155A (en) * 2010-09-01 2010-12-29 中国地质大学（北京） Cordierite porous fireproofing material and preparation method thereof
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