CN104710167B - A kind of ultra-fine cordierite powder and preparation method thereof - Google Patents
A kind of ultra-fine cordierite powder and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of ultra-fine cordierite powder and preparation method thereof.Its technical scheme is：By Mg2+︰ Al3+︰ SiO2Mol ratio be the ︰ 2.4 ~ 2.6 of 1 ︰ 1.9 ~ 2.1, the inorganic salt solution of the inorganic salt solution of magnesium, aluminium is well mixed with Ludox, be made mixed liquor, mixed liquor is added in ammonia spirit under agitation, still aging obtained presoma colloid；Then scrubbed isolated presoma wet gel；Or add absolute ethyl alcohol in presoma wet gel and wash 2 ~ 3 times, add alcohols dispersant, stirring or grinding distribution, colloid after being pre-processed；It is heat-treated 0.5 ~ 5.5 hour under the conditions of 1000 ~ 1400 DEG C after finally being dried by the presoma wet gel or by colloid after the pretreatment, produces ultra-fine cordierite powder.The present invention has that technique is simple, cost is low, energy-saving and the characteristics of be easy to industrialized production, and ultra-fine cordierite powder narrow particle size distribution, the size uniform of preparation be controllable and regular appearance.
Description
Technical field
The invention belongs to cordierite powder technical field.More particularly to a kind of ultra-fine cordierite powder and preparation method thereof.
Background technology
Cordierite ceramica material has the property such as low linear expansion coefficient, good thermal shock, dielectric constant are low and dielectric loss is small
Can, it is widely used frequently as the electronic devices such as anti-thermal shock and high-frequency chip inductor and high-frequency ceramic encapsulating material, such as automobile
Exhaust gas cleaner, catalyst carrier, refractory coating, heat exchange material, wave filter, multilayer chip inductor and multilayer ceramic electronic
Substrate etc..And prepare that ultra-fine, chemical uniformity is good and low temperature sintering cordierite powder is to prepare high-performance cordierite ceramic
The key of material.
Prepare cordierite ceramic powder generally use high-temperature solid phase reaction method and liquid phase method, wherein high temperature solid state reaction at present
Mainly with MgO or Mg (OH)2Or magnesium-containing mineral, Al2O3Or Al (OH)3Or boehmite and quartz etc. are raw material, are consolidated using high temperature
Cordierite is combined to, cordierite powder is made in then mechanical lapping（Remaining water brightness, Liu Yanchun, Dai Yiyi, wait Solid phase synthesis violets
Discussion [J] the Shandong ceramics of green stone powder, 2014, (3): 7-10+15.）.Though this method technique is simple, obtained powder
Granularity is larger, and pollution can be produced in mechanical grinding process, makes obtained powder purity relatively low.Liquid phase method mainly includes
Sol-gel process, colloidal sol-coprecipitation etc..Wherein sol-gel process is to utilize tetraethyl orthosilicate, the inorganic salts and urine of magnalium
Element, ethanol etc. are raw material, and aqueous precursor gel is first made, and cordierite ceramic powder then is made by drying, calcining（Xie Zhiyong,
Liang Hui, Xu Mingxia, sol-gel processes are waited to prepare the solid phase reaction process of cordierite powder and research [J] of agglutinating property
Journal of Inorganic Materials, 2004,19 (4): 779-783）.It is steady that though powder fine size, narrow particle size distribution and chemistry is made in this method
It is qualitative good, but this method complex process, and organic reagent is largely used in preparation process, cost is higher.
The content of the invention
It is contemplated that overcome prior art defect, it is therefore an objective to provide that a kind of technique is simple, cost is low, energy-saving and easy
In the preparation method of the ultra-fine cordierite powder of industrialized production, the ultra-fine cordierite powder size distribution prepared with this method
Narrow, size uniform is controllable and regular appearance.
To achieve the above object, the technical solution adopted by the present invention is：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 0.3 ~ 1.5mol/L water
Solution and Al3+Concentration is the 0.3 ~ 1.5mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio for the ︰ 2.4 of 1 ︰ 1.9 ~ 2.1 ~
2.6, by described two aqueous solution and SiO2Content is that 10 ~ 40wt% Ludox is well mixed, and mixed liquor is made；Then stirring
Under the conditions of mixing, it is 10 ~ 14 mixed solution to be added in 5 ~ 25wt% ammonia spirit to pH value；Still aging 0.5 ~ 24 hour,
Presoma colloid is made.
（2）The preparation of presoma wet gel
The presoma colloid is separated 3 ~ 5 times by centrifuge washing or separated 3 ~ 5 times by inorganic ceramic membrane washing,
Press filtration or centrifuge separation are carried out again, obtain presoma wet gel.
（3）The pretreatment of presoma wet gel
Absolute ethyl alcohol is added into the presoma wet gel, washing 2 ~ 3, the addition of absolute ethyl alcohol is the presoma
10 ~ 60wt% of wet gel；Then add alcohols dispersant, the addition of alcohols dispersant for presoma wet gel 0.5 ~
10wt%, stirring or grinding distribution, colloid after being pre-processed.
（4）The preparation of presoma powder
The presoma wet gel is dried under the conditions of 110 ~ 200 DEG C, obtains micron order presoma powder；
Or dry colloid after the pretreatment under the conditions of 110 ~ 200 DEG C, obtain nanoscale presoma powder.
（5）The preparation of ultra-fine cordierite powder
The micron order presoma powder or nanoscale presoma powder is small in 1000 ~ 1400 DEG C of heat treatments 0.5 ~ 5.5
When, produce ultra-fine cordierite powder.
The inorganic salts of the magnesium are one kind in magnesium chloride, magnesium nitrate, magnesium chloride hydrate and magnesium nitrate hydrate.
The inorganic salts of the aluminium are aluminium chloride, aluminum sulfate, aluminum nitrate, aluminum chloride hydrate, aluminum sulfate hydrate, aluminum nitrate
One kind in hydrate.
The alcohols dispersant is one or more of isobutanol, n-butanol, diglycol, isopropanol.
Due to there is following good effect compared with prior art using above-mentioned technical proposal, the present invention：
1st, the raw material that the present invention uses is easy to get, cheap, has relatively low production cost.
2nd, the present invention is dehydrated and pre-processed to presoma colloid, ensure that powder is scattered after drying and heat treatment
Property, it can effectively reduce the cost of powder decentralized processing.
3rd, during ultra-fine cordierite powder is prepared, each technique is controllable to be carried out the present invention at a lower temperature,
Be advantageous to energy-saving in production process.
4th, the ultra-fine cordierite powder method that the present invention uses, technical process is relatively easy, and production process is easily controllable, raw
It is relatively low to produce cost, is easy to large-scale industrial production.
5th, the ultra-fine cordierite powder epigranular, the regular appearance that prepare of the present invention, diameter of particle can by reaction temperature,
The adjustment of the process systems such as reaction time is controlled.
Therefore, the present invention has that technique is simple, cost is low, energy-saving and the characteristics of be easy to industrialized production, preparation
Ultra-fine cordierite powder narrow particle size distribution, size uniform be controllable and regular appearance.
Brief description of the drawings
Fig. 1 is a kind of XRD spectrum of ultra-fine cordierite powder prepared by the present invention；
Fig. 2 is the SEM photograph of the ultra-fine cordierite powder shown in Fig. 1；
Fig. 3 is the XRD spectrum of another ultra-fine cordierite powder prepared by the present invention；
Fig. 4 is the SEM photograph of the ultra-fine cordierite powder shown in Fig. 3.
Embodiment
In order to be better understood from the present invention, present disclosure, but this is expanded on further below by drawings and examples
Invention is not limited solely to the following examples.
Embodiment 1
A kind of ultra-fine cordierite powder and preparation method thereof.The preparation method comprises the concrete steps that：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 0.3 ~ 0.5mol/L water
Solution and Al3+Concentration is the 0.3 ~ 0.5mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio for the ︰ 2.4 of 1 ︰ 1.9 ~ 2.0 ~
2.5, by described two aqueous solution and SiO2Content is that 10 ~ 15wt% Ludox is well mixed, and mixed liquor is made；Then stirring
Under the conditions of mixing, it is 10 ~ 11 mixed solution to be added in 5 ~ 10wt% ammonia spirit to pH value；Still aging 0.5 ~ 2 hour,
Presoma colloid is made.
（2）The preparation of presoma wet gel
By the presoma colloid by centrifuge washing separation 3 ~ 5 times, then press filtration is carried out, obtain presoma wet gel.
（3）The pretreatment of presoma wet gel
Absolute ethyl alcohol is added into the presoma wet gel, washing 2 ~ 3, the addition of absolute ethyl alcohol is the presoma
10 ~ 20wt% of wet gel；Then add alcohols dispersant, the addition of alcohols dispersant for presoma wet gel 0.5 ~
2wt%, it is dispersed with stirring, colloid after being pre-processed.
（4）The preparation of presoma powder
Colloid after the pretreatment is dried under the conditions of 110 ~ 200 DEG C, obtains nanoscale presoma powder.
（5）The preparation of ultra-fine cordierite powder
The nanoscale presoma powder is heat-treated 0.5 ~ 2 hour at 1000 ~ 1100 DEG C, produces ultra-fine cordierite powder
Body.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride；The inorganic salts of the aluminium are aluminium chloride；The dispersant is
Isobutanol.
Embodiment 2
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 1.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride；The inorganic salts of the aluminium are aluminum nitrate hydrate；Described point
Powder is the mixture of isobutanol, n-butanol and isopropanol.
Embodiment 3
A kind of ultra-fine cordierite powder and preparation method thereof.The preparation method comprises the concrete steps that：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 0.5 ~ 0.8mol/L water
Solution and Al3+Concentration is the 0.5 ~ 0.8mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio for the ︰ 2.5 of 1 ︰ 2.0 ~ 2.1 ~
2.6, by described two aqueous solution and SiO2Content is that 15 ~ 20wt% Ludox is well mixed, and mixed liquor is made；Then stirring
Under the conditions of mixing, it is 11 ~ 12 mixed solution to be added in 10 ~ 15wt% ammonia spirit to pH value；Still aging 2 ~ 8 hours, system
Obtain presoma colloid；
（2）The preparation of presoma wet gel
By the presoma colloid by inorganic ceramic membrane washing separation 3 ~ 5 times, then centrifuge separation is carried out, obtain forerunner
Body wet gel.
（3）The pretreatment of presoma wet gel
Absolute ethyl alcohol is added into the presoma wet gel, washing 2 ~ 3, the addition of absolute ethyl alcohol is the presoma
20 ~ 30wt% of wet gel；Then alcohols dispersant is added, the addition of alcohols dispersant is 2 ~ 4wt% of presoma wet gel,
Grinding distribution, colloid after being pre-processed.
（4）The preparation of presoma powder
Colloid after the pretreatment is dried under the conditions of 110 ~ 200 DEG C, obtains nanoscale presoma powder.
（5）The preparation of ultra-fine cordierite powder
The nanoscale presoma powder is heat-treated 1.5 ~ 3.5 hours at 1100 ~ 1200 DEG C, produces ultra-fine cordierite powder
Body.
In the present embodiment：The inorganic salts of the magnesium are magnesium nitrate；The inorganic salts of the aluminium are aluminum sulfate；The dispersant is
N-butanol.
Embodiment 4
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 3.
In the present embodiment：The inorganic salts of the magnesium are magnesium nitrate；The inorganic salts of the aluminium are aluminum sulfate；The dispersant is
The mixture of diglycol and isopropanol.
Embodiment 5
A kind of ultra-fine cordierite powder and preparation method thereof.The preparation method comprises the concrete steps that：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 0.8 ~ 1.2mol/L water
Solution and Al3+Concentration is the 0.8 ~ 1.2mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio for the ︰ 2.4 of 1 ︰ 2.0 ~ 2.1 ~
2.5, by described two aqueous solution and SiO2Content is that 20 ~ 30wt% Ludox is well mixed, and mixed liquor is made；Then stirring
Under the conditions of mixing, it is 12 ~ 13 mixed solution to be added in 15 ~ 20wt% ammonia spirit to pH value；Still aging 8 ~ 12 hours,
Presoma colloid is made.
（2）The preparation of presoma wet gel
By the presoma colloid by centrifuge washing separation 3 ~ 5 times, then centrifuge separation is carried out, it is wet to obtain presoma
Gel.
（3）The pretreatment of presoma wet gel
Absolute ethyl alcohol is added into the presoma wet gel, washing 2 ~ 3, the addition of absolute ethyl alcohol is the presoma
30 ~ 40wt% of wet gel；Then alcohols dispersant is added, the addition of alcohols dispersant is 4 ~ 6wt% of presoma wet gel,
It is dispersed with stirring, colloid after being pre-processed.
（4）The preparation of presoma powder
Colloid after the pretreatment is dried under the conditions of 110 ~ 200 DEG C, obtains nanoscale presoma powder.
（5）The preparation of ultra-fine cordierite powder
The nanoscale presoma powder is heat-treated 3 ~ 5 hours at 1200 ~ 1300 DEG C, produces ultra-fine cordierite powder.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum nitrate；Described point
Powder is diglycol.
Embodiment 6
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 5.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum nitrate；Described point
Powder is the mixture of isobutanol and isopropanol.
Embodiment 7
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 5.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum nitrate；Described point
Powder is the mixture of isobutanol, n-butanol, diglycol and isopropanol.
Embodiment 8
A kind of ultra-fine cordierite powder and preparation method thereof.The preparation method comprises the concrete steps that：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 1.2 ~ 1.5mol/L water
Solution and Al3+Concentration is the 1.2 ~ 1.5mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio for the ︰ 2.5 of 1 ︰ 1.9 ~ 2.0 ~
2.6, by described two aqueous solution and SiO2Content is that 30 ~ 40wt% Ludox is well mixed, and mixed liquor is made；Then stirring
Under the conditions of mixing, it is 13 ~ 14 mixed solution to be added in 20 ~ 25wt% ammonia spirit to pH value；Still aging 10 ~ 20 hours,
Presoma colloid is made.
（2）The preparation of presoma wet gel
By the presoma colloid by inorganic ceramic membrane washing separation 3 ~ 5 times, then centrifuge separation is carried out, obtain forerunner
Body wet gel.
（3）The pretreatment of presoma wet gel
Absolute ethyl alcohol is added into the presoma wet gel, washing 2 ~ 3, the addition of absolute ethyl alcohol is the presoma
40 ~ 50wt% of wet gel；Then alcohols dispersant is added, the addition of alcohols dispersant is 6 ~ 8wt% of presoma wet gel,
It is dispersed with stirring, colloid after being pre-processed.
（4）The preparation of presoma powder
Colloid after the pretreatment is dried under the conditions of 110 ~ 200 DEG C, obtains nanoscale presoma powder.
（5）The preparation of ultra-fine cordierite powder
The nanoscale presoma powder is heat-treated 4 ~ 5.5 hours at 1300 ~ 1400 DEG C, produces ultra-fine cordierite powder
Body.
In the present embodiment：The inorganic salts of the magnesium are magnesium nitrate hydrate；The inorganic salts of the aluminium are aluminum chloride hydrate；
The dispersant is isopropanol.
Embodiment 9
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 8.
In the present embodiment：The inorganic salts of the magnesium are magnesium nitrate hydrate；The inorganic salts of the aluminium are aluminum chloride hydrate；
The dispersant is the mixture of n-butanol and diglycol.
Embodiment 10
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 8.
In the present embodiment：The inorganic salts of the magnesium are magnesium nitrate hydrate；The inorganic salts of the aluminium are aluminum chloride hydrate；
The dispersant is the mixture of isobutanol, diglycol and isopropanol.
Embodiment 11
A kind of ultra-fine cordierite powder and preparation method thereof.The preparation method comprises the concrete steps that：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 0.6 ~ 0.9mol/L water
Solution and Al3+Concentration is the 0.6 ~ 0.9mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio be the ︰ of 1 ︰ 1.95 ~ 2.05
2.45 ~ 2.55, by described two aqueous solution and SiO2Content is that 25 ~ 35wt% Ludox is well mixed, and mixed liquor is made；So
Afterwards under agitation, it is 10.5 ~ 12 mixed solution to be added in 12 ~ 18wt% ammonia spirit to pH value；Still aging 15
~ 24 hours, presoma colloid is made.
（2）The preparation of presoma wet gel
By the presoma colloid by centrifuge washing separation 3 ~ 5 times, then press filtration separation is carried out, it is wet solidifying to obtain presoma
Glue.
（3）The pretreatment of presoma wet gel
Absolute ethyl alcohol is added into the presoma wet gel, washing 2 ~ 3, the addition of absolute ethyl alcohol is the presoma
50 ~ 60wt% of wet gel；Then add alcohols dispersant, the addition of alcohols dispersant for presoma wet gel 8 ~
10wt%, grinding distribution, colloid after being pre-processed.
（4）The preparation of presoma powder
Colloid after the pretreatment is dried under the conditions of 110 ~ 200 DEG C, obtains nanoscale presoma powder.
（5）The preparation of ultra-fine cordierite powder
The nanoscale presoma powder is heat-treated 1 ~ 3 hour at 1250 ~ 1350 DEG C, produces ultra-fine cordierite powder.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum sulfate hydrate；
The dispersant is the mixture of n-butanol and isopropanol.
Embodiment 12
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 11.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum sulfate hydrate；
The dispersant is the mixture of n-butanol, diglycol and isopropanol.
Embodiment 13
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 11.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum sulfate hydrate；
The dispersant is the mixture of isobutanol and n-butanol.
Embodiment 14
A kind of ultra-fine cordierite powder and preparation method thereof.The preparation method comprises the concrete steps that：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 0.3 ~ 0.5mol/L water
Solution and Al3+Concentration is the 0.3 ~ 0.5mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio for the ︰ 2.4 of 1 ︰ 1.9 ~ 2.0 ~
2.5, by described two aqueous solution and SiO2Content is that 10 ~ 15wt% Ludox is well mixed, and mixed liquor is made；Then stirring
Under the conditions of mixing, it is 10 ~ 11 mixed solution to be added in 5 ~ 10wt% ammonia spirit to pH value；Still aging 0.5 ~ 2 hour,
Presoma colloid is made.
（2）The preparation of presoma wet gel
By the presoma colloid by centrifuge washing separation 3 ~ 5 times, then press filtration is carried out, obtain presoma wet gel.
（3）The preparation of presoma powder
The presoma wet gel is dried under the conditions of 110 ~ 200 DEG C, obtains micron order presoma powder.
（4）The preparation of ultra-fine cordierite powder
The micron order presoma powder is heat-treated 0.5 ~ 2 hour at 1000 ~ 1100 DEG C, produces ultra-fine cordierite powder
Body.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride；The inorganic salts of the aluminium are aluminium chloride；The dispersant is
Isobutanol.
Embodiment 15
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 14.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride；The inorganic salts of the aluminium are aluminum nitrate hydrate；Described point
Powder is the mixture of isobutanol, n-butanol and isopropanol.
Embodiment 16
A kind of ultra-fine cordierite powder and preparation method thereof.The preparation method comprises the concrete steps that：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 0.5 ~ 0.8mol/L water
Solution and Al3+Concentration is the 0.5 ~ 0.8mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio for the ︰ 2.5 of 1 ︰ 2.0 ~ 2.1 ~
2.6, by described two aqueous solution and SiO2Content is that 15 ~ 20wt% Ludox is well mixed, and mixed liquor is made；Then stirring
Under the conditions of mixing, it is 11 ~ 12 mixed solution to be added in 10 ~ 15wt% ammonia spirit to pH value；Still aging 2 ~ 8 hours, system
Obtain presoma colloid.
（2）The preparation of presoma wet gel
By the presoma colloid by inorganic ceramic membrane washing separation 3 ~ 5 times, then centrifuge separation is carried out, obtain forerunner
Body wet gel.
（3）The preparation of presoma powder
The presoma wet gel is dried under the conditions of 110 ~ 200 DEG C, obtains micron order presoma powder.
（4）The preparation of ultra-fine cordierite powder
The micron order presoma powder is heat-treated 1.5 ~ 3.5 hours at 1100 ~ 1200 DEG C, produces ultra-fine cordierite powder
Body.
In the present embodiment：The inorganic salts of the magnesium are magnesium nitrate；The inorganic salts of the aluminium are aluminum sulfate；The dispersant is
N-butanol.
Embodiment 17
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 16.
In the present embodiment：The inorganic salts of the magnesium are magnesium nitrate；The inorganic salts of the aluminium are aluminum sulfate；The dispersant is
The mixture of diglycol and isopropanol.
Embodiment 18
A kind of ultra-fine cordierite powder and preparation method thereof.The preparation method comprises the concrete steps that：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 0.8 ~ 1.2mol/L water
Solution and Al3+Concentration is the 0.8 ~ 1.2mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio for the ︰ 2.4 of 1 ︰ 2.0 ~ 2.1 ~
2.5, by described two aqueous solution and SiO2Content is that 20 ~ 30wt% Ludox is well mixed, and mixed liquor is made；Then stirring
Under the conditions of mixing, it is 12 ~ 13 mixed solution to be added in 15 ~ 20wt% ammonia spirit to pH value；Still aging 8 ~ 12 hours,
Presoma colloid is made.
（2）The preparation of presoma wet gel
By the presoma colloid by centrifuge washing separation 3 ~ 5 times, then centrifuge separation is carried out, it is wet to obtain presoma
Gel.
（3）The preparation of presoma powder
The presoma wet gel is dried under the conditions of 110 ~ 200 DEG C, obtains micron order presoma powder.
（4）The preparation of ultra-fine cordierite powder
The micron order presoma powder is heat-treated 3 ~ 5 hours at 1200 ~ 1300 DEG C, produces ultra-fine cordierite powder.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum nitrate；Described point
Powder is diglycol.
Embodiment 19
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 18.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum nitrate；Described point
Powder is the mixture of isobutanol and isopropanol.
Embodiment 20
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 18.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum nitrate；Described point
Powder is the mixture of isobutanol, n-butanol, diglycol and isopropanol.
Embodiment 21
A kind of ultra-fine cordierite powder and preparation method thereof.The preparation method comprises the concrete steps that：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 1.2 ~ 1.5mol/L water
Solution and Al3+Concentration is the 1.2 ~ 1.5mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio for the ︰ 2.5 of 1 ︰ 1.9 ~ 2.0 ~
2.6, by described two aqueous solution and SiO2Content is that 30 ~ 40wt% Ludox is well mixed, and mixed liquor is made；Then stirring
Under the conditions of mixing, it is 13 ~ 14 mixed solution to be added in 20 ~ 25wt% ammonia spirit to pH value；Still aging 10 ~ 20 hours,
Presoma colloid is made.
（2）The preparation of presoma wet gel
By the presoma colloid by inorganic ceramic membrane washing separation 3 ~ 5 times, then centrifuge separation is carried out, obtain forerunner
Body wet gel.
（3）The preparation of presoma powder
The presoma wet gel is dried under the conditions of 110 ~ 200 DEG C, obtains micron order presoma powder.
（4）The preparation of ultra-fine cordierite powder
The micron order presoma powder is heat-treated 4 ~ 5.5 hours at 1300 ~ 1400 DEG C, produces ultra-fine cordierite powder
Body.
In the present embodiment：The inorganic salts of the magnesium are magnesium nitrate hydrate；The inorganic salts of the aluminium are aluminum chloride hydrate；
The dispersant is isopropanol.
Embodiment 22
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 21.
In the present embodiment：The inorganic salts of the magnesium are magnesium nitrate hydrate；The inorganic salts of the aluminium are aluminum chloride hydrate；
The dispersant is the mixture of n-butanol and diglycol.
Embodiment 23
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 21.
In the present embodiment：The inorganic salts of the magnesium are magnesium nitrate hydrate；The inorganic salts of the aluminium are aluminum chloride hydrate；
The dispersant is the mixture of isobutanol, diglycol and isopropanol.
Embodiment 24
A kind of ultra-fine cordierite powder and preparation method thereof.The preparation method comprises the concrete steps that：
（1）The preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is 0.6 ~ 0.9mol/L water
Solution and Al3+Concentration is the 0.6 ~ 0.9mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio be the ︰ of 1 ︰ 1.95 ~ 2.05
2.45 ~ 2.55, by described two aqueous solution and SiO2Content is that 25 ~ 35wt% Ludox is well mixed, and mixed liquor is made；So
Afterwards under agitation, it is 10.5 ~ 12 mixed solution to be added in 12 ~ 18wt% ammonia spirit to pH value；Still aging 15
~ 24 hours, presoma colloid is made.
（2）The preparation of presoma wet gel
By the presoma colloid by centrifuge washing separation 3 ~ 5 times, then press filtration separation is carried out, it is wet solidifying to obtain presoma
Glue.
（3）The preparation of presoma powder
The presoma wet gel is dried under the conditions of 110 ~ 200 DEG C, obtains micron order presoma powder.
（4）The preparation of ultra-fine cordierite powder
The micron order presoma powder is heat-treated 1 ~ 3 hour at 1250 ~ 1350 DEG C, produces ultra-fine cordierite powder.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum sulfate hydrate；
The dispersant is the mixture of n-butanol and isopropanol.
Embodiment 25
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 24.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum sulfate hydrate；
The dispersant is the mixture of n-butanol, diglycol and isopropanol.
Embodiment 26
A kind of ultra-fine cordierite powder and preparation method thereof.In addition to following materials, remaining is the same as embodiment 24.
In the present embodiment：The inorganic salts of the magnesium are magnesium chloride hydrate；The inorganic salts of the aluminium are aluminum sulfate hydrate；
The dispersant is the mixture of isobutanol and n-butanol.
Present embodiment has following good effect compared with prior art：
1st, the raw material that the present invention uses is easy to get, cheap, has relatively low production cost.
2nd, the present invention is dehydrated and pre-processed to presoma colloid, ensure that powder is scattered after drying and heat treatment
Property, it can effectively reduce the cost of powder decentralized processing.
3rd, during cordierite superfine powder is prepared, each technique is controllable to be carried out the present invention at a lower temperature,
Be advantageous to energy-saving in production process.
What the 4th, the present invention used prepares cordierite superfine powder method, and technical process is relatively easy, and production process is easy to control
System, production cost is relatively low, is easy to large-scale industrial production.
5th, cordierite powder epigranular, regular appearance prepared by the present invention, diameter of particle can pass through reaction temperature, reaction
The adjustment of the process systems such as time is controlled.As shown in drawings, Fig. 1 is a kind of ultra-fine cordierite powder prepared by embodiment 20
The XRD spectrum of body；Fig. 2 is the SEM photograph of the ultra-fine cordierite powder shown in Fig. 1.It is from Fig. 1, Fig. 2 as can be seen that prepared
Powder be pure phase cordierite, the average grain diameter of cordierite powder is 20 ~ 40 μm, and size distribution is more uniform.Fig. 3 is implementation
A kind of XRD spectrum of ultra-fine cordierite powder prepared by example 3；Fig. 4 is the SEM photograph of the ultra-fine cordierite powder shown in Fig. 3.From
As can be seen that prepared powder is the cordierite of pure phase in Fig. 3, Fig. 4, the average grain diameter 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 the characteristics of be easy to industrialized production, preparation
Ultra-fine cordierite powder narrow particle size distribution, size uniform be controllable and regular appearance.
Claims (4)
1. a kind of preparation method of ultra-fine cordierite powder, it is characterised in that be the step of the preparation method：
(1) preparation of presoma colloid
The inorganic salts of the inorganic salts of magnesium and aluminium are dissolved in water, Mg is made2+Concentration is the 0.3~1.5mol/L aqueous solution
And Al3+Concentration is the 0.3~1.5mol/L aqueous solution, then by Mg2+︰ Al3+︰ SiO2Mol ratio for the ︰ 2.4 of 1 ︰ 1.9~2.1~
2.6, by described two aqueous solution and SiO2Content is that 10~40wt% Ludox is well mixed, and mixed liquor is made；Then exist
Under stirring condition, it is 10~14 mixed solution to be added in 5~25wt% ammonia spirit to pH value；Still aging 0.5~
24 hours, presoma colloid is made；
(2) preparation of presoma wet gel
The presoma colloid is separated 3~5 times by centrifuge washing or by inorganic ceramic membrane washing separation 3~5 times, then
Press filtration or centrifuge separation are carried out, obtains presoma wet gel；
(3) pretreatment of presoma wet gel
Absolute ethyl alcohol is added into the presoma wet gel, is washed 2~3 times, the addition of absolute ethyl alcohol is the presoma
10~60wt% of wet gel；Then add alcohols dispersant, the addition of alcohols dispersant for presoma wet gel 0.5~
10wt%, stirring or grinding distribution, colloid after being pre-processed；
(4) preparation of presoma powder
The presoma wet gel is dried under the conditions of 110~200 DEG C, obtains micron order presoma powder；
Or dry colloid after the pretreatment under the conditions of 110~200 DEG C, obtain nanoscale presoma powder；
(5) preparation of ultra-fine cordierite powder
The micron order presoma powder or nanoscale presoma powder are heat-treated 0.5~5.5 hour at 1000~1400 DEG C,
Produce ultra-fine cordierite powder.
2. the preparation method of ultra-fine cordierite powder according to claim 1, the inorganic salts for being characterised by the magnesium are chlorine
Change one kind in magnesium, magnesium nitrate, magnesium chloride hydrate and magnesium nitrate hydrate.
3. the preparation method of ultra-fine cordierite powder according to claim 1, the inorganic salts for being characterised by the aluminium are chlorine
Change one kind in aluminium, aluminum sulfate, aluminum nitrate, aluminum chloride hydrate, aluminum sulfate hydrate, aluminum nitrate hydrate.
4. the preparation method of ultra-fine cordierite powder according to claim 1, it is different to be characterised by the alcohols dispersant
One or more of butanol, n-butanol, diglycol, isopropanol.
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