CN106242637A - A kind of preparation method of porous mullite corundum ceramic - Google Patents
A kind of preparation method of porous mullite corundum ceramic Download PDFInfo
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Abstract
The present invention relates to the preparation method of a kind of porous mullite corundum ceramic, with bauxite and kieselguhr as raw material, use wet milling, filter, dry, stir, and binding agent, dispersant, foam stabilizer and foaming agent, it is shaped again, dries and sintering prepares porous mullite corundum ceramic.The inventive method has the features such as technique simple, with short production cycle, efficiency is high, constant product quality, low cost, on-demand production can prepare porous mullite corundum ceramic material, have preferable industrial utilization prospect.
Description
Technical field
The present invention relates to the preparation method of a kind of porous mullite-corundum ceramic, be specifically related to a kind of with bauxite and silicon
Diatomaceous earth is the method that porous mullite-corundum ceramic prepared by raw material.
Background technology
Porous ceramics is a kind of Inorganic Non-metallic Materials containing increased number of stomata, has porosity height, permeability height, corrosion resistant
The excellent specific properties such as erosion, specific surface area is big, bulk density is little and thermal conductivity is low, be widely used in metallurgy, chemical industry, environmental protection, the energy,
The every field such as food, pharmacy, biology, as filtration, separation, gas distribution, sound-absorbing, heat insulation, chemical filler, bioceramic and catalysis
The materials'uses such as agent carrier, because of its new green environment protection, are increasingly paid close attention to by this field scientific research personnel.
At present, the method preparing porous ceramics mainly has three kinds, including chemical method, Polymeric sponge method and foam method.
Chemical method refers to add some materials that can be produced bubble by chemical reaction in blank, produces gas by means of chemical reaction,
Goods are made to obtain pore.Polymeric sponge method is to utilize to have cancellated foam impregnation in ceramic size, dry
Through sintering organics removal after dry, obtaining porous ceramics, preparation process includes preparing organic ink, selecting suitable organic bubble
The steps such as foam, the pretreatment of foam, dipping, hanging, sintering.Foaming is introducing foaming agent in slurry, passes through mechanical means
Process and produce bubble, then cure pastes, obtain porous body, finally re-sinter and obtain porous ceramics.Wherein, prepared by chemical method
Porous ceramic articles is swift in response, and its bubble generated is wayward;Polymeric sponge method technique is simple, is commonly used to preparation
High porosity and there is the porous ceramics of through-hole structure, but, during calcining, the heating rate at low-temperature space must be very slow, and
Organic formwork, when burning-off removes, is easily generated slag, causes environmental pollution, ceramic frame easily to ftracture, and can significantly reduce last pottery
The mechanical strength of ceramic products;And foaming has generation, and bubble is small, porosity is high, hole shape and size is controlled, production cost
The advantages such as low and technique is simple.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of method preparing porous mullite-corundum ceramic, the method
There is the features such as technique simple, with short production cycle, efficiency is high, constant product quality, low cost, on-demand can produce preparation porous not
Carry out stone-corundum ceramic material, there is preferable industrial utilization prospect.
For solving above technical problem, the present invention is achieved through the following technical solutions:
Design the preparation method of a kind of porous mullite-corundum ceramic, comprise the steps:
(1) according to mullite-corundum pottery to Al2O3、SiO2Component requirements, weigh a certain proportion of bauxite and kieselguhr,
Will the two mix after carry out continuous wet-grinding 6~12h, then carry out filtering, dry, grind, obtain mixed-powder;Wherein, described aluminum
Alumina and diatomaceous ratio are so that Al in mixed-powder2O3With SiO2Mol ratio reach 2.5~5:1 and be as the criterion;
(2) in described mixed-powder, add suitable quantity of water (1.0~1.5 times), after stirring 10~30min, add described mixed powder
The sodium carboxymethyl cellulose of the Triammonium citrate of starch, 0.4~0.6wt%, 0.05~0.20wt% at end 4~6wt% and 0.05~
The silicones polyethers emulsion (solid content 50~60wt%) of 0.20wt%, add after stirring described mixed-powder 0.5~
The sodium lauryl sulphate of 1.0wt%, stirs 2~6min, to obtaining casting after uniform and stable foamed slurry, then, and will
The foamed slurry of molding is incubated the demoulding after 10~60min under the conditions of being placed in 40~70 DEG C, obtains base substrate;
(3) it is incubated 6~24h under the conditions of described base substrate being placed in 110~140 DEG C, after natural cooling, then is placed in 1300~1400 DEG C
Lower sintering, obtains porous mullite-corundum ceramic;Sintering temperature increasing schedule is: room temperature to 600 DEG C, heating rate is 2~5 DEG C
min-1;600~1000 DEG C, heating rate is 5~8 DEG C of min-1, and at 1000 DEG C, it is incubated 30~60min;More than 1000 DEG C,
Heating rate is 3~5 DEG C of min-1, finally insulation 2~6h.
The present invention has a following positive beneficial effect:
(1) present invention employs pore-creating with the new process combined that foams to prepare porous mullite-corundum ceramic: the party
On the one hand given full play to pore creating material prepares the porous ceramics of even pore distribution to method, and another has played the most again foaming
Prepare the feature that the porosity of pottery is high, make full use of diatomite material simultaneously and there is the characteristic of natural porous, so that preparation
The pottery gone out not only hole is evenly distributed, and has the advantages that the porosity is high.
(2) the inventive method is compared with existing chemical method, overcomes chemical method bore hole size and gas release is uppity
Defect;Compared with simple foaming, can the most effectively control to connect the quantity of pore;With Polymeric sponge method phase
Ratio, the pottery prepared has higher mechanical strength.It is to say, pottery prepared by the inventive method to have distribution of pores equal
Even, connection stomatal number amount is effectively controlled and improves the features such as Mechanical Property of Ceramics.
(3) raw material sources of the present invention are extensive, cheap;Designed process is simple to operation,
Safety, equipment is few, invests little, production of easily founding the factory;Products obtained therefrom is with short production cycle, purity is high, steady quality, and low cost can
On-demand production.
(4) porous mullite-corundum material that the inventive method is prepared have that creep rate is low, thermal coefficient of expansion is little, anti-
The advantages such as thermal shock resistance is good, prop up at melted metal filtering, gas purification separation, heat exchanger, heat-insulation and heat-preservation, catalyst carrier, film
The field tools such as support body are widely used.
Accompanying drawing explanation
Fig. 1~Fig. 4 is followed successively by the porous mullite-corundum ceramic of the different batches prepared with the embodiment of the present invention 1~4
XRD figure spectrum.
Detailed description of the invention
The present invention is expanded on further below in conjunction with specific embodiment.Test method in following embodiment, as without saying especially
Bright, it is conventional method.Test material used in following embodiment and reagent, if no special instructions, be purchased from conventional chemical
Reagent shop, kieselguhr used contains SiO2For 85wt%, bauxite contains Al2O3For 90wt%.
Embodiment 1
The preparation method of a kind of porous mullite-corundum ceramic, comprises the following steps:
Weigh 320 grams of bauxite (Al of 2.825 moles respectively2O3) and the kieselguhr (SiO of 1.132 moles of 80 grams2) put into
In grinding machine after continuous wet-grinding 12h, carrying out being filtrated to get filter cake by slip, filter cake grinds after being placed in 110 DEG C of baking ovens drying and obtains
Mixed-powder, is placed in mixed-powder in container (water is 1.2:1 with the weight ratio of powder) the stirring 30min that adds water, is subsequently added into
20g starch, 2.0g Triammonium citrate, 0.4g sodium carboxymethyl cellulose and 0.6g silicones polyethers emulsion (solid content 55wt%), stir
Add 4g sodium lauryl sulphate after mixing uniformly, stir 6min, obtain casting after uniform and stable foamed slurry, then
Being placed in baking oven by the foamed slurry of molding after 40 DEG C of insulation 60min, the demoulding obtains the foam base substrate of solidification and is placed in 110 DEG C of bakings
Being incubated 24h in case, natural cooling is placed in electric furnace at 1400 DEG C insulation 4h, and its sintering temperature increasing schedule is: room temperature to 600
DEG C, heating rate is 2 DEG C of min-1;600~1000 DEG C, heating rate is 5 DEG C of min-1, and at 1000 DEG C, it is incubated 60min;
1000~1400 DEG C, heating rate is 3 DEG C of min-1, temperature retention time is 4h;Then naturally cool to room temperature obtain porous and do not come
Stone-corundum ceramic.The XRD of gained porous mullite-corundum ceramic is shown in Fig. 1.
Embodiment 2
The preparation method of a kind of porous mullite-corundum ceramic, comprises the following steps:
Weigh 332 grams of bauxite (Al of 2.930 moles respectively2O3) and the kieselguhr (SiO of 0.976 mole of 69 grams2) put into
In grinding machine after continuous wet-grinding 6h, carrying out being filtrated to get filter cake by slip, filter cake grinds after being placed in 110 DEG C of baking ovens drying and is mixed
Close powder, mixed-powder is placed in container (water is 1.2:1 with the weight ratio of powder) the stirring 10min that adds water, is subsequently added into 20g
Starch, 2.0g Triammonium citrate, 0.2g sodium carboxymethyl cellulose and 0.8g silicones polyethers emulsion (solid content 55wt%), stirring
Add 4.0g sodium lauryl sulphate after uniformly, stir 4min, obtain casting after uniform and stable foamed slurry, then will
After the foamed slurry of molding is placed in baking oven in 70 DEG C insulation 10min, the demoulding obtains the foam base substrate of solidification and is placed in 140 DEG C of bakings
Being incubated 6h in case, natural cooling is placed in electric furnace at 1400 DEG C insulation 2h, and its sintering temperature increasing schedule is: room temperature to 600 DEG C,
Heating rate is 5 DEG C of min-1;600~1000 DEG C, heating rate is 8 DEG C of min-1, and at 1000 DEG C, it is incubated 30min;1000
~1400 DEG C, heating rate is 5 DEG C of min-1, temperature retention time is 2h;Then naturally cool to room temperature and obtain porous mullite-just
Beautiful pottery.The XRD of gained porous mullite-corundum ceramic is shown in Fig. 2.
Embodiment 3
The preparation method of a kind of porous mullite-corundum ceramic, comprises the following steps:
Weigh 259 grams of bauxite (Al of 2.286 moles respectively2O3) and the kieselguhr (SiO of 0.573 mole of 40.5 grams2) put
Entering in grinding machine after continuous wet-grinding 11h, carry out being filtrated to get filter cake by slip, filter cake grinds after being placed in 110 DEG C of baking ovens drying
To mixed-powder, mixed-powder is placed in container (water is 1.3:1 with the weight ratio of powder) the stirring 30min that adds water, then adds
Enter 15g starch, 1.5g Triammonium citrate, 0.6g sodium carboxymethyl cellulose and 0.2g silicones polyethers emulsion (solid content 55wt%),
It is stirring evenly and then adding into 2.5g sodium lauryl sulphate, stirs 5min, obtain casting after uniform and stable foamed slurry, so
After the foamed slurry of molding is placed in baking oven in 40 DEG C insulation 50min after, the demoulding obtains the foam base substrate of solidification and is placed in 110
Being incubated 20h in DEG C baking oven, natural cooling is placed in electric furnace at 1400 DEG C insulation 2h, and its sintering temperature increasing schedule is: room temperature is extremely
600 DEG C, heating rate is 4 DEG C of min-1;600~1000 DEG C, heating rate is 6 DEG C of min-1, and be incubated at 1000 DEG C
50min;1000~1400 DEG C, heating rate is 4 DEG C of min-1, temperature retention time is 2h;Then, after naturally cooling to room temperature, obtain
Porous mullite-corundum ceramic.The XRD of gained porous mullite-corundum ceramic is shown in Fig. 3.
Embodiment 4
The preparation method of a kind of porous mullite-corundum ceramic, comprises the following steps:
Weigh 178 grams of bauxite (Al of 1.571 moles respectively2O3) and the kieselguhr (SiO of 0.314 mole of 22.2 grams2) put into
In grinding machine after continuous wet-grinding 10h, carrying out being filtrated to get filter cake by slip, filter cake grinds after being placed in 110 DEG C of baking ovens drying and obtains
Mixed-powder, is placed in mixed-powder in container (water is 1.5:1 with the weight ratio of powder) the stirring 10min that adds water, is subsequently added into
10g starch, 1.0g Triammonium citrate, 0.1g sodium carboxymethyl cellulose and 0.4g silicones polyethers emulsion (solid content 55wt%), stir
Add 1.5g sodium lauryl sulphate after mixing uniformly, stir 4min, obtain casting after uniform and stable foamed slurry, then
After the foamed slurry of molding is placed in baking oven in 60 DEG C insulation 20min, the demoulding obtains the foam base substrate of solidification and is placed in 120 DEG C
Being incubated 12h in baking oven, natural cooling is placed in electric furnace at 1300 DEG C insulation 3h, and its sintering temperature increasing schedule is: room temperature to 600
DEG C, heating rate is 4 DEG C of min-1;600~1000 DEG C, heating rate is 5 DEG C of min-1, and at 1000 DEG C, it is incubated 40min;
1000~1300 DEG C, heating rate is 3 DEG C of min-1, temperature retention time is 3h;After naturally cooling to room temperature, obtain porous mullite-
Corundum ceramic.The XRD of gained porous mullite-corundum ceramic is shown in Fig. 4.
Although, the present invention is described in detail the most with a general description of the specific embodiments, but
On the basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (6)
1. the preparation method of porous mullite-corundum ceramic, it is characterised in that comprise the steps:
(1) according to mullite-corundum pottery to Al2O3、SiO2Component requirements, weigh a certain proportion of bauxite and kieselguhr,
Continuous wet-grinding 6~12h after the two is mixed, then carry out filtering, dry, grind, obtain mixed-powder;
(2) in described mixed-powder, add suitable quantity of water, after stirring 10~30min, add described mixed-powder 4~6wt%
The sodium carboxymethyl cellulose of the Triammonium citrate of starch, 0.4~0.6wt%, 0.05~0.20wt% and the silicon of 0.05~0.20wt%
Resin polyethers emulsion, adds the sodium lauryl sulphate of described mixed-powder 0.5~1.0wt% after stirring, stirring 2~
6min, to obtaining casting after uniform and stable foamed slurry, then, is placed in 40~70 DEG C of conditions by the foamed slurry of molding
The demoulding after lower insulation 10~60min, obtains base substrate;
(3) it is incubated 6~24h under the conditions of described base substrate being placed in 110~140 DEG C, after natural cooling, then is placed in 1300~1400 DEG C
Lower sintering, obtains porous mullite-corundum ceramic.
The preparation method of porous mullite-corundum ceramic the most according to claim 1, it is characterised in that: step (1) described aluminum
Alumina and diatomaceous ratio are so that Al in mixed-powder2O3With SiO2Mol ratio reach 2.5~5:1 and be as the criterion.
The preparation method of porous mullite-corundum ceramic the most according to claim 1, it is characterised in that: described in step (2)
Starch, Triammonium citrate addition are followed successively by 5wt%, 0.5wt% of described mixed-powder.
The preparation method of porous mullite-corundum ceramic the most according to claim 1, it is characterised in that: described in step (2)
The consumption of water is 1.0~1.5 times of described mixed-powder weight.
The preparation method of porous mullite-corundum ceramic the most according to claim 1, it is characterised in that: described in step (2)
The solid content of silicones polyethers emulsion is 50~60wt%.
The preparation method of porous mullite-corundum ceramic the most according to claim 1, it is characterised in that: described in step (3)
The temperature increasing schedule of sintering is: room temperature to 600 DEG C, heating rate is 2~5 DEG C of min-1;600~1000 DEG C, heating rate is 5~8
℃•min-1, and at 1000 DEG C, it is incubated 30~60min;More than 1000 DEG C, heating rate is 3~5 DEG C of min-1, finally it is incubated 2
~6h.
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Cited By (2)
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CN108610088A (en) * | 2018-06-04 | 2018-10-02 | 武汉科技大学 | A kind of alumina-mullite porous heat-insulating ceramics and preparation method thereof |
CN110981458A (en) * | 2019-12-27 | 2020-04-10 | 中国天辰工程有限公司 | Device for containing silicon-aluminum-phosphorus molecular sieve and preparation method thereof |
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