CN105948789B - A kind of preparation method of light porous calcium phosphate-aluminum phosphate Ceramic Balls - Google Patents

A kind of preparation method of light porous calcium phosphate-aluminum phosphate Ceramic Balls Download PDF

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CN105948789B
CN105948789B CN201610283610.6A CN201610283610A CN105948789B CN 105948789 B CN105948789 B CN 105948789B CN 201610283610 A CN201610283610 A CN 201610283610A CN 105948789 B CN105948789 B CN 105948789B
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CN105948789A (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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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
    • C—CHEMISTRY; METALLURGY
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    • C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/057—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on calcium oxide
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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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing 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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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing 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
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • 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

A kind of preparation method of light porous calcium phosphate-aluminum phosphate Ceramic Balls, it is characterised in that use following steps：（1）Calcium carbonate, biphosphate aluminium powder, frit powder carries out dry-mixed；（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 calcium phosphate-aluminum phosphate Ceramic Balls.

Description

A kind of preparation method of light porous calcium phosphate-aluminum phosphate Ceramic Balls
Technical field
The present invention is to provide a kind of preparation methods of light porous calcium phosphate-aluminum phosphate Ceramic Balls, belong to special cermacis Technical field of material.
Background technology
Porous calcium phosphate（Ca3(PO4)2）- aluminum phosphate（AlPO4）Ceramic Balls being widely used in the industrial production is general, Catalyst carrier, high-temperature filter, chemical filler, heat preservation and refractory material etc. can be used as.As carrier of photocatalyst and Other liquid phase reactor catalyst carriers, and as in water when the adsorbent of noxious material, there is efficient catalysis in order to ensure Effect and（Or）Adsorption efficiency often requires that porous ceramic ball is in suspended state in water, this just needs to prepare a kind of lightweight Porous ceramic ball.Currently, both at home and abroad mainly using " core " of the sphere made of the organic matter lost as spherical green body is easily burnt, so Spherical organic " core " is removed by being burnt into afterwards, 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, and easily leads to ceramics cracking or destroys, reduces the yield rate of product；In addition, This technical process is more complex, and cost is higher, deficiency in economic performance, environment easy to pollute.In order to overcome above-mentioned problem, the present invention carries A kind of efficient, simple, safe and reliable, easily operated, low-cost light porous aluminum phosphate-calcium silicates Ceramic Balls are supplied Preparation method.
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-calcium phosphate ceramic ball, technical solution are：
A kind of preparation method of light porous calcium phosphate-aluminum phosphate Ceramic Balls, it is characterised in that use following steps：（1） Calcium carbonate, biphosphate aluminium powder, frit powder is 1 according to mass ratio：1.06：0.03 ratio carries out dry-mixed；Wherein, it melts The group of block becomes:50 wt% lithias, 30 wt% sodium oxide molybdena and 20 wt% silica；（2）Add a concentration of 8 wt% Poly-vinyl alcohol solution as binder, the additive amount of binder is the 5% of blank gross mass；Then it is granulated, is molded, circle is made Column 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, 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 Degree heats to 380 DEG C and keeps the temperature 1 hour, then heats to 680 DEG C with the speed of 1 DEG C/min and heat preservation 2 is small When, 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, that is, make Obtain light porous calcium phosphate-aluminum phosphate Ceramic Balls.
A kind of preparation method of the light porous calcium phosphate-aluminum phosphate Ceramic Balls, it is characterised in that：Step（1）In The average grain diameter of calcium carbonate powder be 0.6 micron, aluminium dihydrogen phosphate powder average particle size is 0.5 micron, frit powder it is flat Equal grain size is 0.7 micron.
A kind of preparation method of the light porous calcium phosphate-aluminum phosphate Ceramic Balls, 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 calcium phosphate-aluminum phosphate Ceramic Balls prepared by the technology of the present invention float in water；From It can see in figure：Calcium phosphate-aluminum phosphate Ceramic Balls float in water, illustrate that the volume of calcium phosphate-aluminum phosphate Ceramic Balls is close For degree 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 understands and calcium carbonate reaction generation calcium phosphate, and water Steam and carbon dioxide etc. have the function of pore-forming, can thus prepare light porous calcium phosphate-aluminum phosphate ceramics.
Specific implementation mode
Embodiment 1
Calcium carbonate powder, biphosphate aluminium powder, frit powder is 1 according to mass ratio：1.06：0.03 ratio carries out It is dry-mixed；Wherein, the silica containing 50 wt% lithias, the sodium oxide molybdena and 20 wt% of 30 wt% in frit；Control calcium carbonate The average grain diameter of powder 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；The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binder, the additive amount of binder 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, green body It is put into the alumina crucible that interior bottom is semicircle spherical shape, 150 is heated to the speed of 5 DEG C/min under air atmosphere 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/min Speed heat to 680 DEG C and keep the temperature 2 hours, finally heat to 1150 DEG C with the speed of 5 DEG C/min and keep the temperature 2 hours, room temperature is then naturally cooled to, obtains light porous calcium phosphate-aluminum phosphate Ceramic Balls.It is surveyed with Archimedes method The bulk density for obtaining porous ceramic ball is 0.89 g/cm3, open pore rate is 34 %.The crystalline phase that Ceramic Balls are measured with XRD analysis is Calcium phosphate and aluminum phosphate.
Embodiment 2
Calcium carbonate powder, biphosphate aluminium powder, frit powder is 1 according to mass ratio：1.06：0.03 ratio carries out It is dry-mixed；Wherein, the silica containing 50 wt% lithias, the sodium oxide molybdena and 20 wt% of 30 wt% in frit；Control calcium carbonate The average grain diameter of powder 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；The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binder, the additive amount of binder 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, green body It is put into the alumina crucible that interior bottom is semicircle spherical shape, 150 is heated to the speed of 5 DEG C/min under air atmosphere 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/min Speed heat to 680 DEG C and keep the temperature 2 hours, finally heat to 1150 DEG C with the speed of 5 DEG C/min and keep the temperature 2 hours, room temperature is then naturally cooled to, obtains light porous calcium phosphate-aluminum phosphate Ceramic Balls.It is surveyed with Archimedes method The bulk density for obtaining porous ceramic ball is 0.91 g/cm3, open pore rate 33%.The crystalline phase that Ceramic Balls are measured with XRD analysis is Calcium phosphate and aluminum phosphate.
Embodiment 3
Calcium carbonate powder, biphosphate aluminium powder, frit powder is 1 according to mass ratio：1.06：0.03 ratio carries out It is dry-mixed；Wherein, the silica containing 50 wt% lithias, the sodium oxide molybdena and 20 wt% of 30 wt% in frit；Control calcium carbonate The average grain diameter of powder 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；The poly-vinyl alcohol solution of a concentration of 8 wt% is added as binder, the additive amount of binder 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, green body It is put into the alumina crucible that interior bottom is semicircle spherical shape, 150 is heated to the speed of 5 DEG C/min under air atmosphere 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/min Speed heat to 680 DEG C and keep the temperature 2 hours, finally heat to 1150 DEG C with the speed of 5 DEG C/min and keep the temperature 2 hours, room temperature is then naturally cooled to, obtains light porous calcium phosphate-aluminum phosphate Ceramic Balls.It is surveyed with Archimedes method The bulk density for obtaining porous ceramic ball is 0.90g/cm3, open pore rate is 32 %.The crystalline phase that Ceramic Balls are measured with XRD analysis is Calcium phosphate and aluminum phosphate.

Claims (2)

1. a kind of preparation method of light porous calcium phosphate-aluminum phosphate Ceramic Balls, it is characterised in that use following steps：（1） Calcium carbonate, biphosphate aluminium powder, frit powder are 1 according to mass ratio：1.06：0.03 ratio carries out dry-mixed；Wherein, frit Group become:50 wt% lithias, 30 wt% sodium oxide molybdena and 20 wt% silica；Control calcium carbonate powder is averaged 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 binder, the additive amount of binder is the 5% of blank gross mass；Then it makes Grain, molding, are made cylindric green body；（3）After 70 DEG C of dry base substrates 5 hours, it is that semicircle is spherical that green body, which 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 1150 DEG C with the speed of 5 DEG C/min and keeps the temperature 2 hours, it is then natural It is cooled to room temperature, obtains light porous calcium phosphate-aluminum phosphate Ceramic Balls.
2. a kind of preparation method of light porous calcium phosphate-aluminum phosphate Ceramic Balls 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.
CN201610283610.6A 2016-05-04 2016-05-04 A kind of preparation method of light porous calcium phosphate-aluminum phosphate Ceramic Balls Expired - Fee Related CN105948789B (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
CN1513806A (en) * 2003-04-30 2004-07-21 东南大学 Calcium phosphorus kind ceramic bone structure engineering porous support material
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
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
CN1513806A (en) * 2003-04-30 2004-07-21 东南大学 Calcium phosphorus kind ceramic bone structure engineering porous support material
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
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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