CN105924217B - A kind of preparation method of light porous magnesium phosphate-aluminum phosphate Ceramic Balls - Google Patents
A kind of preparation method of light porous magnesium phosphate-aluminum phosphate Ceramic Balls Download PDFInfo
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Abstract
A kind of preparation method of light porous magnesium phosphate-aluminum phosphate Ceramic Balls, it is characterised in that using following steps：（1）Magnesium carbonate, biphosphate aluminium powder, frit powder carries out dry-mixed；（2）It is granulated, shaping, cylindric base substrate is made；（3）After 70 DEG C of dry base substrates 5 hours, base substrate is put into inner bottom part as in the spherical alumina crucible of semicircle, 150 DEG C are heated to 5 DEG C/min speed and be incubated 2 hours under air atmosphere, 380 DEG C are heated to 10 20 DEG C/min speed and be incubated 1 hour again, then 680 DEG C are heated to 1 DEG C/min speed and is incubated 2 hours, finally 1100 DEG C are heated to 5 DEG C/min speed and be incubated 2 hours, room temperature then is naturally cooled to, that is, light porous magnesium phosphate-aluminum phosphate Ceramic Balls are made.
Description
Technical field
The present invention is to provide a kind of preparation method of light porous magnesium phosphate-aluminum phosphate Ceramic Balls, belong to special cermacis
Technical field of material.
Background technology
Porous calcium phosphate magnesium（Mg3(PO4)2）- aluminum phosphate（AlPO4）The application of Ceramic Balls in the industrial production is very extensive,
Catalyst carrier, high-temperature filter, chemical filler, insulation and refractory material etc. can be used as.As carrier of photocatalyst and
Other liquid phase reactor catalyst carriers, and as in water during the adsorbent of noxious material, there is efficient catalysis in order to ensure
Effect and（Or）Adsorption efficiency, often require that porous ceramic ball is in suspended state in water, this just needs to prepare a kind of lightweight
Porous ceramic ball.At present, " core " of the spheroid as spherical base substrate made of the organic matter mainly lost both at home and abroad using easily burning, so
Spherical organic " core " is removed by burning till afterwards, so as to prepare a kind of suspensible porous ceramics hollow ball.The shortcomings that this method is：
Shaping is more difficult, and during organic matter burns and lost, is easily caused ceramics cracking or destroys, reduce the yield rate of product；In addition,
This technical process is more complicated, and cost is higher, deficiency in economic performance, easily pollutes environment.In order to overcome above-mentioned problem, the present invention carries
A kind of light porous aluminum phosphate-calcium silicates Ceramic Balls efficient, simple, safe and reliable, easily operated, cost is cheap are supplied
Preparation method.
The content of the invention
The technology of the present invention provides a kind of light porous phosphoric acid efficient, simple, safe and reliable, easily operated, cost is cheap
The preparation method of aluminium-magnesium phosphate Ceramic Balls, its technical scheme are：
A kind of preparation method of light porous magnesium phosphate-aluminum phosphate Ceramic Balls, it is characterised in that using following steps：（1）
Magnesium carbonate, biphosphate aluminium powder, frit powder is 1 according to mass ratio：1.25：0.03 ratio carries out dry-mixed；Wherein, melt
Composition in block is:The silica of 50 wt% lithias, 30 wt% sodium oxide molybdena and 20 wt%；（2）It is 8 to add concentration
For wt% poly-vinyl alcohol solution as binding agent, the addition of binding agent is the 5% of blank gross mass；Then it is granulated, is molded, is made
Cylindric base substrate；（3）After 70 DEG C of dry base substrates 5 hours, base substrate is put into inner bottom part as the spherical alumina crucible of semicircle
It is interior, heat to 150 DEG C with 5 DEG C/min speed under air atmosphere and be incubated 2 hours, then with 10-20 DEG C/min's
Speed heats to 380 DEG C and is incubated 1 hour, then heats to 680 DEG C and insulation 2 with 1 DEG C/min speed
Hour, finally heat to 1100 DEG C with 5 DEG C/min speed and be incubated 2 hours, then naturally cool to room temperature, i.e.,
Light porous magnesium phosphate-aluminum phosphate Ceramic Balls are made.
A kind of preparation method of described light porous magnesium phosphate-aluminum phosphate Ceramic Balls, it is characterised in that：Step（1）In
The average grain diameter of magnesium carbonate powder be 0.6 micron, aluminium dihydrogen phosphate powder average particle size is 0.5 micron, frit powder it is flat
Equal particle diameter is 0.7 micron.
A kind of preparation method of described light porous magnesium phosphate-aluminum phosphate Ceramic Balls, it is characterised in that：Step（2）In
Shaping refer to powder carry out dry-pressing formed, briquetting pressure 10-25MPa.
Fig. 1 is the photo that light porous magnesium phosphate-aluminum phosphate Ceramic Balls prepared by the technology of the present invention are floated in water；From
It can see in figure：Magnesium phosphate-aluminum phosphate Ceramic Balls are floated in water, illustrate that the volume of magnesium phosphate-aluminum phosphate Ceramic Balls 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：
Fusible at a lower temperature using aluminium dihydrogen phosphate is liquid, then at relatively high temperatures again solidifiable property
Can so that base substrate spontaneously formed in sintering process for spheroid, concrete principle it is as follows：Aluminium dihydrogen phosphate be heated to 150 DEG C,
After insulation 2 hours, aluminium dihydrogen phosphate is changed into as liquid, is then heated rapidly to 380 DEG C and is incubated 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 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
Spheroid.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 understands and carbonic acid reactive magnesium generation magnesium phosphate, and water
Steam and carbon dioxide etc. have the function that pore-forming, can thus prepare light porous magnesium phosphate-aluminum phosphate ceramics.
Embodiment
Embodiment 1
Magnesium carbonate powder, biphosphate aluminium powder, frit powder is 1 according to mass ratio：1.25：0.03 ratio is carried out
It is dry-mixed；Wherein, the silica containing 50 wt% lithias, 30 wt% sodium oxide molybdena and 20 wt% in frit；Control magnesium 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；For the poly-vinyl alcohol solution that addition concentration is 8 wt% as binding agent, the addition of binding agent is blank gross mass
5%；Then it is granulated, is dry-pressing formed with 10MPa pressure, cylindric base substrate is made；After 70 DEG C of dry base substrates 5 hours, base substrate
Inner bottom part is put into as in the spherical alumina crucible of semicircle, 150 are heated to 5 DEG C/min speed under air atmosphere
DEG C and be incubated 2 hours, then with 10 DEG C/min speed heat to 380 DEG C and be incubated 1 hour, then with 1 DEG C/min
Speed heat to 680 DEG C and be incubated 2 hours, finally heat to 1100 DEG C with 5 DEG C/min speed and be incubated
2 hours, room temperature is then naturally cooled to, that is, light porous magnesium phosphate-aluminum phosphate Ceramic Balls are made.Surveyed with Archimedes method
The bulk density for obtaining porous ceramic ball is 0.92 g/cm3, open pore rate is 36 %.The crystalline phase that Ceramic Balls are measured with XRD analysis is
Magnesium phosphate and aluminum phosphate.
Embodiment 2
Magnesium carbonate powder, biphosphate aluminium powder, frit powder is 1 according to mass ratio：1.25：0.03 ratio is carried out
It is dry-mixed；Wherein, the silica containing 50 wt% lithias, 30 wt% sodium oxide molybdena and 20 wt% in frit；Control magnesium 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；For the poly-vinyl alcohol solution that addition concentration is 8 wt% as binding agent, the addition of binding agent is blank gross mass
5%；Then it is granulated, is dry-pressing formed with 20MPa pressure, cylindric base substrate is made；After 70 DEG C of dry base substrates 5 hours, base substrate
Inner bottom part is put into as in the spherical alumina crucible of semicircle, 150 are heated to 5 DEG C/min speed under air atmosphere
DEG C and be incubated 2 hours, then with 15 DEG C/min speed heat to 380 DEG C and be incubated 1 hour, then with 1 DEG C/min
Speed heat to 680 DEG C and be incubated 2 hours, finally heat to 1100 DEG C with 5 DEG C/min speed and be incubated
2 hours, room temperature is then naturally cooled to, that is, light porous magnesium phosphate-aluminum phosphate Ceramic Balls are made.Surveyed with Archimedes method
The bulk density for obtaining porous ceramic ball is 0.93 g/cm3, open pore rate is 33 %.The crystalline phase that Ceramic Balls are measured with XRD analysis is
Magnesium phosphate and aluminum phosphate.
Embodiment 3
Magnesium carbonate powder, biphosphate aluminium powder, frit powder is 1 according to mass ratio：1.25：0.03 ratio is carried out
It is dry-mixed；Wherein, the silica containing 50 wt% lithias, 30 wt% sodium oxide molybdena and 20 wt% in frit；Control magnesium 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；For the poly-vinyl alcohol solution that addition concentration is 8 wt% as binding agent, the addition of binding agent is blank gross mass
5%；Then it is granulated, is dry-pressing formed with 25 MPa pressure, cylindric base substrate is made；After 70 DEG C of dry base substrates 5 hours, base substrate
Inner bottom part is put into as in the spherical alumina crucible of semicircle, 150 are heated to 5 DEG C/min speed under air atmosphere
DEG C and be incubated 2 hours, then with 20 DEG C/min speed heat to 380 DEG C and be incubated 1 hour, then with 1 DEG C/min
Speed heat to 680 DEG C and be incubated 2 hours, finally heat to 1100 DEG C with 5 DEG C/min speed and be incubated
2 hours, room temperature is then naturally cooled to, that is, light porous magnesium phosphate-aluminum phosphate Ceramic Balls are made.Surveyed with Archimedes method
The bulk density for obtaining porous ceramic ball is 0.93g/cm3, open pore rate is 32 %.The crystalline phase that Ceramic Balls are measured with XRD analysis is
Magnesium phosphate and aluminum phosphate.
Claims (2)
1. a kind of preparation method of light porous magnesium phosphate-aluminum phosphate Ceramic Balls, it is characterised in that using following steps：（1）
Magnesium carbonate, biphosphate aluminium powder, frit powder are 1 according to mass ratio：1.25：0.03 ratio carries out dry-mixed；Wherein, frit
In composition be:The silica of 50 wt% lithias, 30 wt% sodium oxide molybdena and 20 wt%；Control the flat of magnesium carbonate powder
Equal particle diameter 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）For the poly-vinyl alcohol solution that addition concentration is 8 wt% as binding agent, the addition of binding agent is the 5% of blank gross mass；So
It is granulated, is molded afterwards, cylindric base substrate is made；（3）After 70 DEG C of dry base substrates 5 hours, it is semi-round ball that base substrate, which is put into inner bottom part,
In the alumina crucible of shape, heat to 150 DEG C with 5 DEG C/min speed under air atmosphere and be incubated 2 hours, then with
10-20 DEG C/min speed heats to 380 DEG C and is incubated 1 hour, then with 1 DEG C/min speed heat temperature raising
To 680 DEG C and 2 hours are incubated, finally 1100 DEG C is heated to 5 DEG C/min speed and is incubated 2 hours, then certainly
Room temperature so is cooled to, that is, light porous magnesium phosphate-aluminum phosphate Ceramic Balls are made.
A kind of 2. preparation method of light porous magnesium phosphate-aluminum phosphate Ceramic Balls as claimed in claim 1, it is characterised in that：
Step（2）In shaping refer to powder carry out dry-pressing formed, briquetting pressure 10-25MPa.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1502588A (en) * | 2002-11-26 | 2004-06-09 | 张福长 | Porous inorganic material and mfg mehtod thereof |
| CN101343193A (en) * | 2008-08-15 | 2009-01-14 | 昆明理工大学 | High-temperature oxidation resistant porous ceramic paint and manufacture method thereof |
| CN101671197A (en) * | 2009-09-23 | 2010-03-17 | 北京航空航天大学 | Preparation method of carbon foam heat insulation material added with hollow ceramic balls |
| CN104291850A (en) * | 2014-09-19 | 2015-01-21 | 深圳大学 | Phosphate-base light-weight porous material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20060147364A1 (en) * | 2004-12-30 | 2006-07-06 | Council Of Scientific And Industrial Research | Process for synthesising porous crystalline aluminophosphate molecular sieves |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1502588A (en) * | 2002-11-26 | 2004-06-09 | 张福长 | Porous inorganic material and mfg mehtod thereof |
| CN101343193A (en) * | 2008-08-15 | 2009-01-14 | 昆明理工大学 | High-temperature oxidation resistant porous ceramic paint and manufacture method thereof |
| CN101671197A (en) * | 2009-09-23 | 2010-03-17 | 北京航空航天大学 | Preparation method of carbon foam heat insulation material added with hollow ceramic balls |
| CN104291850A (en) * | 2014-09-19 | 2015-01-21 | 深圳大学 | Phosphate-base light-weight porous material and preparation method thereof |
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