CN104710167A - Ultra-fine cordierite powder and preparation method thereof - Google Patents
Ultra-fine cordierite powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to ultra-fine cordierite powder and a preparation method thereof. The technical scheme is as follows: the preparation method comprises the following steps: uniformly mixing an inorganic salt solution of magnesium, an inorganic salt solution of aluminum and silica sol at a molar ratio of Mg<2+>:Al<3+>:SiO2 being 1:(1.9-2.1):(2.4-2.6), preparing mixed liquor, adding the mixed liquor into an ammonia water solution while stirring, and performing standing and ageing to prepare precursor colloid; then performing washing separation to obtain wet precursor colloid; or adding absolute ethanol into the wet precursor colloid for washing for 2-3 times, adding an alcohol dispersion agent, performing stirring or grinding dispersion, and obtaining pretreated colloid; finally drying the wet precursor colloid or the pretreated colloid and then performing heat treatment at a temperature of 1,000-1,400 DEG C for 0.5-5.5 hours to obtain the ultra-fine cordierite powder. The preparation method has the characteristics of simple process, low cost, energy conservation, consumption reduction and easiness for industrialized production; the prepared ultra-fine cordierite powder is narrow in particle size distribution, uniform and controllable in size and regular in morphology.
Description
Technical field
The invention belongs to cordierite powder technical field.Be specifically related to a kind of ultra-fine cordierite powder and preparation method thereof.
Background technology
Cordierite ceramica material has that linear expansivity is low, good thermal shock, specific inductivity are low and the performance such as dielectric loss is little, the electron devices such as Chang Zuowei anti-thermal shock and high-frequency chip inductor and radio ceramics packaged material are widely used, as automobile exhaust gas purifying installation, support of the catalyst, refractory coating, heat exchange material, wave filter, multilayer chip inductor and multilayer ceramic electronic substrate etc.And prepare ultra-fine, chemical uniformity good and low temperature sintering cordierite powder is the key of preparation high-performance cordierite ceramica material.
Prepare cordierite ceramic powder at present and usually adopt high-temperature solid phase reaction method and liquid phase method, wherein high temperature solid state reaction is mainly with MgO or Mg (OH)
2or magnesium-containing mineral, Al
2o
3or Al (OH)
3or boehmite and quartz etc. are raw material, adopt high temperature process heat trichroite, then mechanical mill obtains cordierite powder (remaining water brightness, Liu Yanchun, Dai Yiyi, etc. the discussion [J] of Solid phase synthesis cordierite powder. Shandong pottery, 2014, (3): 7-10+15.).Though the method technique is simple, obtained powder granularity is comparatively large, and can produce pollution in mechanical grinding process, makes the powder purity that obtains relatively low.Liquid phase method mainly comprises sol-gel method, colloidal sol-coprecipitation method etc.Wherein sol-gel method utilizes the inorganic salt of tetraethoxy, magnalium and urea, ethanol etc. to be raw material, first obtained aqueous precursor gel, then through super-dry, the obtained cordierite ceramic powder (Xie Zhiyong of calcining, Liang Hui, Xu Mingxia, Deng. sol-gel method prepares the solid state reaction process of cordierite powder and the research [J] of coking property. Journal of Inorganic Materials, 2004,19 (4): 779-783).Though it is good that the method obtains powder fine size, narrow particle size distribution and chemical stability, the method complex process, and organic reagent is used in a large number in preparation process, cost is higher.
Summary of the invention
The present invention is intended to overcome prior art defect, object is to provide that a kind of technique is simple, cost is low, energy-saving and cost-reducing and be easy to the preparation method of ultra-fine cordierite powder of suitability for industrialized production, the controlled and regular appearance of the ultra-fine cordierite powder narrow particle size distribution prepared by the method, size uniform.
For achieving the above object, the technical solution used in the present invention is:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 0.3 ~ 1.5mol/L
3+concentration is the aqueous solution of 0.3 ~ 1.5mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 1.9 ~ 2.1 ︰ 2.4 ~ 2.6, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 10 ~ 40wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 5 ~ 25wt% to pH value be 10 ~ 14; Still aging 0.5 ~ 24 hour, obtained presoma colloid.
(2) preparation of presoma wet gel
By described presoma colloid by whizzer washing separation 3 ~ 5 times or by inorganic ceramic film washing separation 3 ~ 5 times, then carry out press filtration or whizzer separation, obtain presoma wet gel.
(3) pre-treatment of presoma wet gel
In described presoma wet gel, add dehydrated alcohol, washing 2 ~ 3, the add-on of dehydrated alcohol is 10 ~ 60wt% of described presoma wet gel; Then add alcohols dispersion agent, the add-on of alcohols dispersion agent is 0.5 ~ 10wt% of presoma wet gel, stirs or grinding distribution, obtains colloid after pre-treatment.
(4) preparation of presoma powder
Described presoma wet gel is dry under 110 ~ 200 DEG C of conditions, obtain micron order presoma powder;
Or colloid after described pre-treatment is dry under 110 ~ 200 DEG C of conditions, obtain nano level presoma powder.
(5) preparation of ultra-fine cordierite powder
By described micron order presoma powder or nano level presoma powder 1000 ~ 1400 DEG C of thermal treatments 0.5 ~ 5.5 hour, obtain ultra-fine cordierite powder.
The inorganic salt of described magnesium are the one in magnesium chloride, magnesium nitrate, magnesium chloride hydrate and magnesium nitrate hydrate.
The inorganic salt of described aluminium are the one in aluminum chloride, Tai-Ace S 150, aluminum nitrate, aluminum chloride hydrate, aluminum sulfate hydrate, aluminum nitrate hydrate.
Described alcohols dispersion agent is more than one in isopropylcarbinol, propyl carbinol, glycol ether, Virahol.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect:
1, the raw material that the present invention adopts is easy to get, cheap, has lower production cost.
2, the present invention dewaters and pre-treatment to presoma colloid, ensure that the dispersiveness of powder after drying and thermal treatment, effectively can reduce the cost of powder dispersion treatment.
3, the present invention is in the process of the ultra-fine cordierite powder of preparation, and each technique is carried out under all caning be controlled in lesser temps, is conducive to saving energy and reduce the cost in production process.
4, the ultra-fine cordierite powder method of the present invention's employing, technological process is relatively simple, and production process is easy to control, and production cost is lower, is convenient to large-scale industrial production.
5, ultra-fine cordierite powder epigranular, the regular appearance prepared of the present invention, diameter of particle controls by the adjustment of the process system such as temperature of reaction, reaction times.
Therefore, the present invention has that technique is simple, cost is low, energy-saving and cost-reducing and be easy to the feature of suitability for industrialized production, the controlled and regular appearance of the ultra-fine cordierite powder narrow particle size distribution of preparation, size uniform.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of a kind of ultra-fine cordierite powder prepared by the present invention;
Fig. 2 is the SEM photo of the ultra-fine cordierite powder shown in Fig. 1;
Fig. 3 is the XRD figure spectrum of the ultra-fine cordierite powder of another kind prepared by the present invention;
Fig. 4 is the SEM photo of the ultra-fine cordierite powder shown in Fig. 3.
Embodiment
For a better understanding of the present invention, set forth content of the present invention further below by drawings and Examples, but the present invention is not only confined to the following examples.
embodiment 1
A kind of ultra-fine cordierite powder and preparation method thereof.The concrete steps of described preparation method are:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 0.3 ~ 0.5mol/L
3+concentration is the aqueous solution of 0.3 ~ 0.5mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 1.9 ~ 2.0 ︰ 2.4 ~ 2.5, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 10 ~ 15wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 5 ~ 10wt% to pH value be 10 ~ 11; Still aging 0.5 ~ 2 hour, obtained presoma colloid.
(2) preparation of presoma wet gel
By described presoma colloid by whizzer washing separation 3 ~ 5 times, then carry out press filtration, obtain presoma wet gel.
(3) pre-treatment of presoma wet gel
In described presoma wet gel, add dehydrated alcohol, washing 2 ~ 3, the add-on of dehydrated alcohol is 10 ~ 20wt% of described presoma wet gel; Then add alcohols dispersion agent, the add-on of alcohols dispersion agent is 0.5 ~ 2wt% of presoma wet gel, dispersed with stirring, obtains colloid after pre-treatment.
(4) preparation of presoma powder
Colloid after described pre-treatment is dry under 110 ~ 200 DEG C of conditions, obtain nano level presoma powder.
(5) preparation of ultra-fine cordierite powder
By described nano level presoma powder 1000 ~ 1100 DEG C of thermal treatments 0.5 ~ 2 hour, obtain ultra-fine cordierite powder.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride; The inorganic salt of described aluminium are aluminum chloride; Described dispersion agent is isopropylcarbinol.
embodiment 2
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 1.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride; The inorganic salt of described aluminium are aluminum nitrate hydrate; Described dispersion agent is the mixture of isopropylcarbinol, propyl carbinol and Virahol.
embodiment 3
A kind of ultra-fine cordierite powder and preparation method thereof.The concrete steps of described preparation method are:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 0.5 ~ 0.8mol/L
3+concentration is the aqueous solution of 0.5 ~ 0.8mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 2.0 ~ 2.1 ︰ 2.5 ~ 2.6, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 15 ~ 20wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 10 ~ 15wt% to pH value be 11 ~ 12; Still aging 2 ~ 8 hours, obtained presoma colloid;
(2) preparation of presoma wet gel
By described presoma colloid by inorganic ceramic film washing separation 3 ~ 5 times, then carry out whizzer separation, obtain presoma wet gel.
(3) pre-treatment of presoma wet gel
In described presoma wet gel, add dehydrated alcohol, washing 2 ~ 3, the add-on of dehydrated alcohol is 20 ~ 30wt% of described presoma wet gel; Then add alcohols dispersion agent, the add-on of alcohols dispersion agent is 2 ~ 4wt% of presoma wet gel, grinding distribution, obtains colloid after pre-treatment.
(4) preparation of presoma powder
Colloid after described pre-treatment is dry under 110 ~ 200 DEG C of conditions, obtain nano level presoma powder.
(5) preparation of ultra-fine cordierite powder
By described nano level presoma powder 1100 ~ 1200 DEG C of thermal treatments 1.5 ~ 3.5 hours, obtain ultra-fine cordierite powder.
In the present embodiment: the inorganic salt of described magnesium are magnesium nitrate; The inorganic salt of described aluminium are Tai-Ace S 150; Described dispersion agent is propyl carbinol.
embodiment 4
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 3.
In the present embodiment: the inorganic salt of described magnesium are magnesium nitrate; The inorganic salt of described aluminium are Tai-Ace S 150; Described dispersion agent is the mixture of glycol ether and Virahol.
embodiment 5
A kind of ultra-fine cordierite powder and preparation method thereof.The concrete steps of described preparation method are:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 0.8 ~ 1.2mol/L
3+concentration is the aqueous solution of 0.8 ~ 1.2mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 2.0 ~ 2.1 ︰ 2.4 ~ 2.5, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 20 ~ 30wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 15 ~ 20wt% to pH value be 12 ~ 13; Still aging 8 ~ 12 hours, obtained presoma colloid.
(2) preparation of presoma wet gel
By described presoma colloid by whizzer washing separation 3 ~ 5 times, then carry out whizzer separation, obtain presoma wet gel.
(3) pre-treatment of presoma wet gel
In described presoma wet gel, add dehydrated alcohol, washing 2 ~ 3, the add-on of dehydrated alcohol is 30 ~ 40wt% of described presoma wet gel; Then add alcohols dispersion agent, the add-on of alcohols dispersion agent is 4 ~ 6wt% of presoma wet gel, dispersed with stirring, obtains colloid after pre-treatment.
(4) preparation of presoma powder
Colloid after described pre-treatment is dry under 110 ~ 200 DEG C of conditions, obtain nano level presoma powder.
(5) preparation of ultra-fine cordierite powder
By described nano level presoma powder 1200 ~ 1300 DEG C of thermal treatments 3 ~ 5 hours, obtain ultra-fine cordierite powder.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum nitrate; Described dispersion agent is glycol ether.
embodiment 6
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 5.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum nitrate; Described dispersion agent is the mixture of isopropylcarbinol and Virahol.
embodiment 7
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 5.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum nitrate; Described dispersion agent is the mixture of isopropylcarbinol, propyl carbinol, glycol ether and Virahol.
embodiment 8
A kind of ultra-fine cordierite powder and preparation method thereof.The concrete steps of described preparation method are:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 1.2 ~ 1.5mol/L
3+concentration is the aqueous solution of 1.2 ~ 1.5mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 1.9 ~ 2.0 ︰ 2.5 ~ 2.6, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 30 ~ 40wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 20 ~ 25wt% to pH value be 13 ~ 14; Still aging 10 ~ 20 hours, obtained presoma colloid.
(2) preparation of presoma wet gel
By described presoma colloid by inorganic ceramic film washing separation 3 ~ 5 times, then carry out whizzer separation, obtain presoma wet gel.
(3) pre-treatment of presoma wet gel
In described presoma wet gel, add dehydrated alcohol, washing 2 ~ 3, the add-on of dehydrated alcohol is 40 ~ 50wt% of described presoma wet gel; Then add alcohols dispersion agent, the add-on of alcohols dispersion agent is 6 ~ 8wt% of presoma wet gel, dispersed with stirring, obtains colloid after pre-treatment.
(4) preparation of presoma powder
Colloid after described pre-treatment is dry under 110 ~ 200 DEG C of conditions, obtain nano level presoma powder.
(5) preparation of ultra-fine cordierite powder
By described nano level presoma powder 1300 ~ 1400 DEG C of thermal treatments 4 ~ 5.5 hours, obtain ultra-fine cordierite powder.
In the present embodiment: the inorganic salt of described magnesium are magnesium nitrate hydrate; The inorganic salt of described aluminium are aluminum chloride hydrate; Described dispersion agent is Virahol.
embodiment 9
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 8.
In the present embodiment: the inorganic salt of described magnesium are magnesium nitrate hydrate; The inorganic salt of described aluminium are aluminum chloride hydrate; Described dispersion agent is the mixture of propyl carbinol and glycol ether.
embodiment 10
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 8.
In the present embodiment: the inorganic salt of described magnesium are magnesium nitrate hydrate; The inorganic salt of described aluminium are aluminum chloride hydrate; Described dispersion agent is the mixture of isopropylcarbinol, glycol ether and Virahol.
embodiment 11
A kind of ultra-fine cordierite powder and preparation method thereof.The concrete steps of described preparation method are:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 0.6 ~ 0.9mol/L
3+concentration is the aqueous solution of 0.6 ~ 0.9mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 1.95 ~ 2.05 ︰ 2.45 ~ 2.55, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 25 ~ 35wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 12 ~ 18wt% to pH value be 10.5 ~ 12; Still aging 15 ~ 24 hours, obtained presoma colloid.
(2) preparation of presoma wet gel
By described presoma colloid by whizzer washing separation 3 ~ 5 times, then carry out press filtration separation, obtain presoma wet gel.
(3) pre-treatment of presoma wet gel
In described presoma wet gel, add dehydrated alcohol, washing 2 ~ 3, the add-on of dehydrated alcohol is 50 ~ 60wt% of described presoma wet gel; Then add alcohols dispersion agent, the add-on of alcohols dispersion agent is 8 ~ 10wt% of presoma wet gel, grinding distribution, obtains colloid after pre-treatment.
(4) preparation of presoma powder
Colloid after described pre-treatment is dry under 110 ~ 200 DEG C of conditions, obtain nano level presoma powder.
(5) preparation of ultra-fine cordierite powder
By described nano level presoma powder 1250 ~ 1350 DEG C of thermal treatments 1 ~ 3 hour, obtain ultra-fine cordierite powder.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum sulfate hydrate; Described dispersion agent is the mixture of propyl carbinol and Virahol.
embodiment 12
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 11.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum sulfate hydrate; Described dispersion agent is the mixture of propyl carbinol, glycol ether and Virahol.
embodiment 13
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 11.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum sulfate hydrate; Described dispersion agent is the mixture of isopropylcarbinol and propyl carbinol.
embodiment 14
A kind of ultra-fine cordierite powder and preparation method thereof.The concrete steps of described preparation method are:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 0.3 ~ 0.5mol/L
3+concentration is the aqueous solution of 0.3 ~ 0.5mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 1.9 ~ 2.0 ︰ 2.4 ~ 2.5, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 10 ~ 15wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 5 ~ 10wt% to pH value be 10 ~ 11; Still aging 0.5 ~ 2 hour, obtained presoma colloid.
(2) preparation of presoma wet gel
By described presoma colloid by whizzer washing separation 3 ~ 5 times, then carry out press filtration, obtain presoma wet gel.
(3) preparation of presoma powder
Described presoma wet gel is dry under 110 ~ 200 DEG C of conditions, obtain micron order presoma powder.
(4) preparation of ultra-fine cordierite powder
By described micron order presoma powder 1000 ~ 1100 DEG C of thermal treatments 0.5 ~ 2 hour, obtain ultra-fine cordierite powder.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride; The inorganic salt of described aluminium are aluminum chloride; Described dispersion agent is isopropylcarbinol.
embodiment 15
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 14.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride; The inorganic salt of described aluminium are aluminum nitrate hydrate; Described dispersion agent is the mixture of isopropylcarbinol, propyl carbinol and Virahol.
embodiment 16
A kind of ultra-fine cordierite powder and preparation method thereof.The concrete steps of described preparation method are:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 0.5 ~ 0.8mol/L
3+concentration is the aqueous solution of 0.5 ~ 0.8mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 2.0 ~ 2.1 ︰ 2.5 ~ 2.6, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 15 ~ 20wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 10 ~ 15wt% to pH value be 11 ~ 12; Still aging 2 ~ 8 hours, obtained presoma colloid.
(2) preparation of presoma wet gel
By described presoma colloid by inorganic ceramic film washing separation 3 ~ 5 times, then carry out whizzer separation, obtain presoma wet gel.
(3) preparation of presoma powder
Described presoma wet gel is dry under 110 ~ 200 DEG C of conditions, obtain micron order presoma powder.
(4) preparation of ultra-fine cordierite powder
By described micron order presoma powder 1100 ~ 1200 DEG C of thermal treatments 1.5 ~ 3.5 hours, obtain ultra-fine cordierite powder.
In the present embodiment: the inorganic salt of described magnesium are magnesium nitrate; The inorganic salt of described aluminium are Tai-Ace S 150; Described dispersion agent is propyl carbinol.
embodiment 17
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 16.
In the present embodiment: the inorganic salt of described magnesium are magnesium nitrate; The inorganic salt of described aluminium are Tai-Ace S 150; Described dispersion agent is the mixture of glycol ether and Virahol.
embodiment 18
A kind of ultra-fine cordierite powder and preparation method thereof.The concrete steps of described preparation method are:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 0.8 ~ 1.2mol/L
3+concentration is the aqueous solution of 0.8 ~ 1.2mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 2.0 ~ 2.1 ︰ 2.4 ~ 2.5, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 20 ~ 30wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 15 ~ 20wt% to pH value be 12 ~ 13; Still aging 8 ~ 12 hours, obtained presoma colloid.
(2) preparation of presoma wet gel
By described presoma colloid by whizzer washing separation 3 ~ 5 times, then carry out whizzer separation, obtain presoma wet gel.
(3) preparation of presoma powder
Described presoma wet gel is dry under 110 ~ 200 DEG C of conditions, obtain micron order presoma powder.
(4) preparation of ultra-fine cordierite powder
By described micron order presoma powder 1200 ~ 1300 DEG C of thermal treatments 3 ~ 5 hours, obtain ultra-fine cordierite powder.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum nitrate; Described dispersion agent is glycol ether.
embodiment 19
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 18.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum nitrate; Described dispersion agent is the mixture of isopropylcarbinol and Virahol.
embodiment 20
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 18.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum nitrate; Described dispersion agent is the mixture of isopropylcarbinol, propyl carbinol, glycol ether and Virahol.
embodiment 21
A kind of ultra-fine cordierite powder and preparation method thereof.The concrete steps of described preparation method are:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 1.2 ~ 1.5mol/L
3+concentration is the aqueous solution of 1.2 ~ 1.5mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 1.9 ~ 2.0 ︰ 2.5 ~ 2.6, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 30 ~ 40wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 20 ~ 25wt% to pH value be 13 ~ 14; Still aging 10 ~ 20 hours, obtained presoma colloid.
(2) preparation of presoma wet gel
By described presoma colloid by inorganic ceramic film washing separation 3 ~ 5 times, then carry out whizzer separation, obtain presoma wet gel.
(3) preparation of presoma powder
Described presoma wet gel is dry under 110 ~ 200 DEG C of conditions, obtain micron order presoma powder.
(4) preparation of ultra-fine cordierite powder
By described micron order presoma powder 1300 ~ 1400 DEG C of thermal treatments 4 ~ 5.5 hours, obtain ultra-fine cordierite powder.
In the present embodiment: the inorganic salt of described magnesium are magnesium nitrate hydrate; The inorganic salt of described aluminium are aluminum chloride hydrate; Described dispersion agent is Virahol.
embodiment 22
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 21.
In the present embodiment: the inorganic salt of described magnesium are magnesium nitrate hydrate; The inorganic salt of described aluminium are aluminum chloride hydrate; Described dispersion agent is the mixture of propyl carbinol and glycol ether.
embodiment 23
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 21.
In the present embodiment: the inorganic salt of described magnesium are magnesium nitrate hydrate; The inorganic salt of described aluminium are aluminum chloride hydrate; Described dispersion agent is the mixture of isopropylcarbinol, glycol ether and Virahol.
embodiment 24
A kind of ultra-fine cordierite powder and preparation method thereof.The concrete steps of described preparation method are:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 0.6 ~ 0.9mol/L
3+concentration is the aqueous solution of 0.6 ~ 0.9mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 1.95 ~ 2.05 ︰ 2.45 ~ 2.55, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 25 ~ 35wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 12 ~ 18wt% to pH value be 10.5 ~ 12; Still aging 15 ~ 24 hours, obtained presoma colloid.
(2) preparation of presoma wet gel
By described presoma colloid by whizzer washing separation 3 ~ 5 times, then carry out press filtration separation, obtain presoma wet gel.
(3) preparation of presoma powder
Described presoma wet gel is dry under 110 ~ 200 DEG C of conditions, obtain micron order presoma powder.
(4) preparation of ultra-fine cordierite powder
By described micron order presoma powder 1250 ~ 1350 DEG C of thermal treatments 1 ~ 3 hour, obtain ultra-fine cordierite powder.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum sulfate hydrate; Described dispersion agent is the mixture of propyl carbinol and Virahol.
embodiment 25
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 24.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum sulfate hydrate; Described dispersion agent is the mixture of propyl carbinol, glycol ether and Virahol.
embodiment 26
A kind of ultra-fine cordierite powder and preparation method thereof.Except following material, all the other are with embodiment 24.
In the present embodiment: the inorganic salt of described magnesium are magnesium chloride hydrate; The inorganic salt of described aluminium are aluminum sulfate hydrate; Described dispersion agent is the mixture of isopropylcarbinol and propyl carbinol.
This embodiment compared with prior art has following positively effect:
1, the raw material that the present invention adopts is easy to get, cheap, has lower production cost.
2, the present invention dewaters and pre-treatment to presoma colloid, ensure that the dispersiveness of powder after drying and thermal treatment, effectively can reduce the cost of powder dispersion treatment.
3, the present invention is in the process preparing trichroite superfine powder, and each technique is carried out under all caning be controlled in lesser temps, is conducive to saving energy and reduce the cost in production process.
What 4, the present invention adopted prepares trichroite superfine powder method, and technological process is relatively simple, and production process is easy to control, and production cost is lower, is convenient to large-scale industrial production.
5, cordierite powder epigranular, the regular appearance prepared of the present invention, diameter of particle controls by the adjustment of the process system such as temperature of reaction, reaction times.As shown in drawings, Fig. 1 is the XRD figure spectrum of a kind of ultra-fine cordierite powder prepared by embodiment 20; Fig. 2 is the SEM photo of the ultra-fine cordierite powder shown in Fig. 1.As can be seen from Fig. 1, Fig. 2, prepared powder is the trichroite of pure phase, and the median size of cordierite powder is 20 ~ 40 μm, and size-grade distribution is comparatively even.Fig. 3 is the XRD figure spectrum of a kind of ultra-fine cordierite powder prepared by embodiment 3; Fig. 4 is the SEM photo of the ultra-fine cordierite powder shown in Fig. 3.As can be seen from Fig. 3, Fig. 4, prepared powder is the trichroite of pure phase, and the median size of cordierite powder is 100 ~ 500nm, even particle size distribution.
Therefore, the present invention has that technique is simple, cost is low, energy-saving and cost-reducing and be easy to the feature of suitability for industrialized production, the controlled and regular appearance of the ultra-fine cordierite powder narrow particle size distribution of preparation, size uniform.
Claims (5)
1. a preparation method for ultra-fine cordierite powder, is characterized in that the step of described preparation method is:
(1) preparation of presoma colloid
The inorganic salt of magnesium and the inorganic salt of aluminium are dissolved in the water respectively, obtained Mg
2+concentration is the aqueous solution and the Al of 0.3 ~ 1.5mol/L
3+concentration is the aqueous solution of 0.3 ~ 1.5mol/L, then presses Mg
2+︰ Al
3+︰ SiO
2mol ratio be 1 ︰ 1.9 ~ 2.1 ︰ 2.4 ~ 2.6, by described two kinds of aqueous solution and SiO
2content is that the silicon sol of 10 ~ 40wt% mixes, obtained mixed solution; Then under agitation, mixing solutions is joined in the ammonia soln of 5 ~ 25wt% to pH value be 10 ~ 14; Still aging 0.5 ~ 24 hour, obtained presoma colloid;
(2) preparation of presoma wet gel
By described presoma colloid by whizzer washing separation 3 ~ 5 times or by inorganic ceramic film washing separation 3 ~ 5 times, then carry out press filtration or whizzer separation, obtain presoma wet gel;
(3) pre-treatment of presoma wet gel
In described presoma wet gel, add dehydrated alcohol, washing 2 ~ 3, the add-on of dehydrated alcohol is 10 ~ 60wt% of described presoma wet gel; Then add alcohols dispersion agent, the add-on of alcohols dispersion agent is 0.5 ~ 10wt% of presoma wet gel, stirs or grinding distribution, obtains colloid after pre-treatment;
(4) preparation of presoma powder
Described presoma wet gel is dry under 110 ~ 200 DEG C of conditions, obtain micron order presoma powder;
Or colloid after described pre-treatment is dry under 110 ~ 200 DEG C of conditions, obtain nano level presoma powder;
(5) preparation of ultra-fine cordierite powder
By described micron order presoma powder or nano level presoma powder 1000 ~ 1400 DEG C of thermal treatments 0.5 ~ 5.5 hour, obtain ultra-fine cordierite powder.
2. the preparation method of ultra-fine cordierite powder according to claim 1, is characterised in that the inorganic salt of described magnesium are the one in magnesium chloride, magnesium nitrate, magnesium chloride hydrate and magnesium nitrate hydrate.
3. the preparation method of ultra-fine cordierite powder according to claim 1, is characterised in that the inorganic salt of described aluminium are the one in aluminum chloride, Tai-Ace S 150, aluminum nitrate, aluminum chloride hydrate, aluminum sulfate hydrate, aluminum nitrate hydrate.
4. the preparation method of ultra-fine cordierite powder according to claim 1, is characterised in that described alcohols dispersion agent is more than one in isopropylcarbinol, propyl carbinol, glycol ether, Virahol.
5. a ultra-fine cordierite powder, is characterized in that described ultra-fine cordierite powder is the ultra-fine cordierite powder prepared described in the preparation method of ultra-fine cordierite powder according to any one of claim 1 ~ 4.
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| CN105254282A (en) * | 2015-11-12 | 2016-01-20 | 季红军 | Preparation method of architectural ceramic material |
| CN108752011A (en) * | 2018-05-30 | 2018-11-06 | 安徽理工大学 | A method of using anhydrous magnesium chloride as fused salt base CORDIERITE SYNTHESIZED AT LOW TEMPERATURE powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105254282A (en) * | 2015-11-12 | 2016-01-20 | 季红军 | Preparation method of architectural ceramic material |
| CN108752011A (en) * | 2018-05-30 | 2018-11-06 | 安徽理工大学 | A method of using anhydrous magnesium chloride as fused salt base CORDIERITE SYNTHESIZED AT LOW TEMPERATURE powder |
| CN108752011B (en) * | 2018-05-30 | 2021-05-18 | 安徽理工大学 | Method for synthesizing cordierite powder at low temperature by taking anhydrous magnesium chloride as molten salt base |
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