CN103396102B - A kind of preparation method of the low-expansion coefficient cordierite honeycomb ceramic based on fluid additive - Google Patents
A kind of preparation method of the low-expansion coefficient cordierite honeycomb ceramic based on fluid additive Download PDFInfo
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Abstract
Based on a preparation method for the low-expansion coefficient cordierite honeycomb ceramic of fluid additive, comprise the following steps: (1) powder raw material is prepared; (2) liquid blender preparation; (3) pug preparation; (4) moulded pottery not yet put in a kiln to bake preparation; (5) extrusion moulding; (6) dryness finalization; (7) base substrate post-treatment; (8) product burns till.Advantage of the present invention: with the addition of dispersion agent in pug after, in pug, the viscosity of shaping assistant can reduce greatly, extrusion pressure during formed product can be reduced on the one hand, the degree of freedom of pug Raw particle flow and slippage can be promoted on the other hand greatly, thus promote raw material aligning in extrusion direction; With the addition of lubricant in pug after, all lubricated liquid in feed particles surface is wrapped in, and the friction resistance of feed particles when there is relative movement just reduces greatly, thus the flowing between pug Raw particle and slippage are all become than being easier to generation.
Description
Technical field
The present invention relates to the manufacture field of ceramic honey comb, be specially a kind of preparation method of the low-expansion coefficient cordierite honeycomb ceramic based on fluid additive.
Background technology
Automobile honeycomb ceramic carrier requires that product material possesses very low thermal expansivity, thus guarantees that product can stand the impact of rapid heat cycle frequently and not occur cracking.Substantially all adopt cordierite to produce honeycomb ceramic carrier on the market at present.The theoretical thermal expansivity of cordierite is 1.45*10
-6/ DEG C (room temperature ~ 800 DEG C average coefficient of linear expansion), the heat shock resistance temperature of the honeycomb ceramic carrier produced according to this coefficient of expansion can only about reach 550 DEG C.And the normal use temperature of automobile honeycomb ceramic carrier be 650 DEG C to room temperature, the thermal expansivity therefore adopting common process to produce is 1.45*10
-6/ DEG C about cordierite honeycomb ceramic carrier can not meet the demands.
There is patent Introduction in Corning Incorporated, and the thermal expansivity of cordierite crystal is three heterotropic, and its A axle thermal expansivity is 2.9*10
-6/ DEG C, B axle thermal expansivity is 2.9*10
-6/ DEG C, C axle thermal expansivity is-1.1*10
-6/ DEG C, as long as and introduce and can make trichroite C axle arrangement as much as possible on some directions in product, just can produce thermal expansivity and be less than 1.45*10
-6/ DEG C below the cordierite honeycomb ceramic product of thermal expansivity, and also successfully to produce thermal expansivity be 0.5 ~ 1.0*10
-6/ DEG C cordierite honeycomb ceramic carrier product.
Current honeycomb ceramic carrier production technique is divided into two classes substantially: the first kind be after directly adopting synthesis trichroite powder levigate again carry out producing who knows production technique, this technique is because the crystal of trichroite is in the powder course of processing, the structure major part of cordierite crystal hexagonal columnar is destroyed, therefore cordierite crystal C axle substantially can not be facilitated in production process to extrude on direction at product align, therefore also just cannot produce the honeycomb ceramic carrier of low thermal coefficient of expansion.Equations of The Second Kind adopts the raw material such as kaolin, talcum, aluminum oxide required for synthesis of dichroite to carry out the production technique of producing, although this technique has possessed cordierite crystal extrude the condition that direction aligns at product, but owing to wanting to make the C axle of cordierite crystal synthesized in product sintering process align in the generation on direction of extruding of product, just must when formed product, in raw material, the raw material such as kaolin, talcum flats crystal aligns according to certain rule extruding on direction of product.
The test of Equations of The Second Kind production technique shows that trichroite is in building-up process, the generation direction of C axle carries out generating according to the flat extension direction of kaolin crystal, therefore the C axle of cordierite crystal in product to be made to extrude generation on direction at product align, in formed product process, kaolin will be made to extrude generation as much as possible on direction according to the extension of flats crystal at product and to align.
During in order to promote that kaolin flats crystal product is shaping, extrude generation as much as possible on direction at ceramic honey comb to align, the present invention is by adding the organic liquid additive combination of dispersion agent in conjunction with lubricant in the feed, strengthen mobility and the slipping property of shaping pug Raw, thus impel the extension direction of the kaolin flats crystal in shaping pug to produce as much as possible aligning extruding on direction of product.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of the low-expansion coefficient cordierite honeycomb ceramic based on fluid additive, to solve the problem in background technology.
Technical problem solved by the invention realizes by the following technical solutions:
Based on a preparation method for the low-expansion coefficient cordierite honeycomb ceramic of fluid additive, comprise the following steps:
(1) powder raw material preparation: take the high-purity lamellar kaolin powder of 35 ~ 45wt%, the high-purity platy talc powder of 35 ~ 45wt%, 10 ~ 30wt% aluminum oxide powder, take the binding agent of above-mentioned raw materials gross weight 3 ~ 8wt% as shaping assistant simultaneously, above-mentioned raw materials, binding agent are added in powder mixer and fully stirs, until mix, obtain powder raw material;
(2) liquid blender preparation: take the powder raw material gross weight 20 ~ 35wt% water, 0.1 ~ 1.5wt% dispersion agent, the 0.5 ~ 2.5wt% lubricant that obtain in step (1), above-mentioned dispersion agent and lubricant are slowly added to the water and stir, until dispersion agent and lubricant are dissolved in water, obtain liquid blender;
(3) pug preparation: the powder raw material that step (1) mixes is put into kneader and rubs, spray into the liquid blender that step (2) obtains, powder raw material becomes clod gradually simultaneously, namely completes pug preparation after the plasticity-of clod is stable;
(4) moulded pottery not yet put in a kiln to bake preparation: the pug that step (3) obtains is put into vacuum pugmill and carries out vacuum mud refining, vacuum tightness≤-0.09MPa in mud refining process, obtain the moulded pottery not yet put in a kiln to bake supporting with forming machine barrel specification; If moulded pottery not yet put in a kiln to bake has demixing phenomenon, can adopt repeatedly repetition mud refining mode that moulded pottery not yet put in a kiln to bake is met the demands;
(5) extrusion moulding: the moulded pottery not yet put in a kiln to bake that step (4) obtains is put into vacuum-extruder, extrudes out the ceramic honey comb biscuit of desired size by mould;
(6) dryness finalization: the ceramic honey comb biscuit that step (5) obtains is put into microwave oven and carries out heat drying, until drying completes water ratio≤2% in base substrate, take out from microwave oven, base substrate is fixed to the ceramic honey comb work in-process of required specification;
(7) base substrate post-treatment: after the ceramic honey comb work in-process after step (6) being shaped put chi according to the ratio of burning till contraction, two ends redundance is cut away;
(8) product burns till: the ceramic honey comb work in-process processed according to dimensional requirement in step (7) are put into kiln and burns till, firing period is 25 ~ 120 hours, firing temperature is 1360 DEG C ~ 1450 DEG C, soaking time is 4 ~ 8 hours, obtains required low-expansion coefficient cordierite honeycomb ceramic.
As the one optimization of above technical scheme; Binding agent in step (1) is Mierocrystalline cellulose, not containing Ash residue after calcining, has oilness, film-forming properties, water-soluble simultaneously.
As the one optimization of above technical scheme; Described Mierocrystalline cellulose be molecular weight 4000 ~ 20000 Vltra tears (HPMC).
As the one optimization of above technical scheme; Dispersion agent in step (2) adds to prevent the kaolin in raw material and the excessive gelling of Mierocrystalline cellulose, and dispersion agent is polyether glycol.
As the one optimization of above technical scheme; Lubricant in step (2) is to make liquid blender form integument on powder raw material surface, thus make powder raw material have better slipping property, mobility thus reduce pug forming pressure, promote pug Raw particle better orientation movement, lubricant is water miscible organic high molecular compound.
As the one optimization of above technical scheme; Described water miscible organic high molecular compound is the one or more combination in oleic acid ester, oleate soap, lauroleate, polyvinyl alcohol.
Liquid blender in the present invention comprises dispersion agent and the large family macromolecule organic compound of lubricant two.Because honeycomb ceramic carrier forming requirements pug has quite high plasticity-, the plasticity-depending inorganic raw material self alone cannot meet the shaping requirement of carrier at all, generally for the plasticity-increasing carrier, under the prerequisite of inorganic raw material not changing product, the shaping assistant of Mierocrystalline cellulose as carrier is added in capital in the feed, in order to increase the plasticity-of pug, thus pug plasticity-is made to meet the shaping requirement of carrier.Because Mierocrystalline cellulose has very strong viscosity, the inorganic raw material after adding in pug will be adhered to firmly, is difficult to flowing and slippage occur, is also just difficult to produce when carrier is shaping align.With the addition of dispersion agent in pug after, ensureing that under the shaping required plastic prerequisite of carrier, in pug, cellulosic viscosity can reduce greatly, thus making the feed particles in pug possess the degree of freedom of well flowing and slippage.
In above-mentioned pug, increase lubricant, better can promote the slippage between pug Raw particle, the mobility of raw material when enhancing carrier is shaping.Thus promote that further the extension direction of kaolin flats crystal is extruded on direction at carrier and produce aligning of a large amount of rules.Lubricant of the present invention is water miscible organic high molecular compound, because pug needs to use water as blender in layoutprocedure, adopt water-insoluble lipid lubricant not only can affect the uniformity coefficient of pug, the difficulty of also can increase carrier drying, burning till, thus reduce conforming product rate.
Compared with prior art, tool of the present invention has the following advantages:
(1) after with the addition of dispersion agent in pug, ensureing under the shaping required plastic prerequisite of carrier, in pug, the viscosity of shaping assistant can reduce greatly, extrusion pressure during formed product can be reduced on the one hand, the degree of freedom of pug Raw particle flow and slippage can be promoted on the other hand greatly, thus promote raw material aligning in extrusion direction;
(2) after with the addition of lubricant in pug, feed particles surface is all wrapped in by one deck lubricating fluid, therefore the friction resistance of feed particles when there is relative movement just reduces greatly, thus makes the flowing between pug Raw particle and slippage all become than being easier to generation;
Embodiment
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with specific embodiment, setting forth the present invention further.
Embodiment 1
Based on a preparation method for the low-expansion coefficient cordierite honeycomb ceramic of fluid additive, comprise the following steps:
(1) powder raw material preparation: take the high-purity lamellar kaolin powder of 35wt%, the high-purity platy talc powder of 45wt%, 20wt% aluminum oxide powder, take the binding agent of above-mentioned raw materials gross weight 3wt% as shaping assistant simultaneously, above-mentioned raw materials, binding agent are added in powder mixer and fully stirs, until mix, obtain powder raw material;
(2) liquid blender preparation: take the powder raw material gross weight 26wt% water, 0.5wt% dispersion agent, the 1.5wt% lubricant that obtain in step (1), above-mentioned dispersion agent and lubricant are slowly added to the water and stir, until dispersion agent and lubricant are dissolved in water, obtain liquid blender;
(3) pug preparation: the powder raw material that step (1) mixes is put into kneader and rubs, spray into the liquid blender that step (2) obtains, powder raw material becomes clod gradually simultaneously, namely completes pug preparation after the plasticity-of clod is stable;
(4) moulded pottery not yet put in a kiln to bake preparation: the pug that step (3) obtains is put into vacuum pugmill and carries out twice vacuum mud refining, in mud refining process, vacuum tightness is-0.09MPa, obtains the moulded pottery not yet put in a kiln to bake supporting with forming machine barrel specification;
(5) extrusion moulding: the moulded pottery not yet put in a kiln to bake that step (4) obtains is put into vacuum-extruder is under the condition of 10MPa at extrusion pressure, is extruded into the plasticity-ceramic honey comb biscuit of desired size by mould;
(6) dryness finalization: the ceramic honey comb biscuit that step (5) obtains is put into microwave oven and carry out the drying of inside and outside homogeneous heating, until the water ratio in base substrate is 2%, take out from microwave oven, base substrate is fixed to the ceramic honey comb work in-process of required specification;
(7) base substrate post-treatment: after the ceramic honey comb work in-process after step (6) being shaped put chi according to the ratio of burning till contraction, two ends redundance is cut away;
(8) product burns till: the base substrate processed in step (7) is put into kiln and burns till, and firing period is 36 hours, and firing temperature is 1360 DEG C DEG C, and soaking time is 4 hours, obtains required low-expansion coefficient cordierite honeycomb ceramic.
Embodiment 2
Based on a preparation method for the low-expansion coefficient cordierite honeycomb ceramic of fluid additive, comprise the following steps:
(1) powder raw material preparation: take the high-purity lamellar kaolin powder of 45wt%, the high-purity platy talc powder of 35wt%, 20wt% aluminum oxide powder, take the binding agent of above-mentioned raw materials gross weight 5wt% as shaping assistant simultaneously, above-mentioned raw materials, binding agent are added in powder mixer and fully stirs, until mix, obtain powder raw material;
(2) liquid blender preparation: take the powder raw material gross weight 26wt% water, 0.8wt% dispersion agent, the 1.5wt% lubricant that obtain in step (1), above-mentioned dispersion agent and lubricant are slowly added to the water and stir, until dispersion agent and lubricant are dissolved in water, obtain liquid blender;
(3) pug preparation: the powder raw material that step (1) mixes is put into kneader and rubs, spray into the liquid blender that step (2) obtains, powder raw material becomes clod gradually simultaneously, namely completes pug preparation after the plasticity-of clod is stable;
(4) moulded pottery not yet put in a kiln to bake preparation: the pug that step (3) obtains is put into vacuum pugmill and carries out twice vacuum mud refining, in mud refining process, vacuum tightness is-0.093MPa, obtains the moulded pottery not yet put in a kiln to bake supporting with forming machine barrel specification;
(5) extrusion moulding: the moulded pottery not yet put in a kiln to bake that step (4) obtains is put into vacuum-extruder is under the condition of 10MPa at extrusion pressure, is extruded into the plasticity-ceramic honey comb biscuit of desired size by mould;
(6) dryness finalization: the ceramic honey comb biscuit that step (5) obtains is put into microwave oven and carry out the drying of inside and outside homogeneous heating, until the water ratio in base substrate is 1.5%, take out from microwave oven, base substrate is fixed to the ceramic honey comb work in-process of required specification;
(7) base substrate post-treatment: after the ceramic honey comb work in-process after step (6) being shaped put chi according to the ratio of burning till contraction, two ends redundance is cut away;
(8) product burns till: the base substrate processed in step (7) is put into kiln and burns till, and firing period is 72 hours, and firing temperature is 1450 DEG C, and soaking time is 8 hours, obtains required low-expansion coefficient cordierite honeycomb ceramic.
Embodiment 3
Based on a preparation method for the low-expansion coefficient cordierite honeycomb ceramic of fluid additive, comprise the following steps:
(1) powder raw material preparation: take the high-purity lamellar kaolin powder of 40wt%, the high-purity platy talc powder of 43wt%, 17wt% aluminum oxide powder, take the binding agent of above-mentioned raw materials gross weight 5wt% as shaping assistant simultaneously, above-mentioned raw materials, binding agent are added in powder mixer and fully stirs, until mix, obtain powder raw material;
(2) liquid blender preparation: take the powder raw material gross weight 25.5wt% water, 1wt% dispersion agent, the 2wt% lubricant that obtain in step (1), above-mentioned dispersion agent and lubricant are slowly added to the water and stir, until dispersion agent and lubricant are dissolved in water, obtain liquid blender;
(3) pug preparation: the powder raw material that step (1) mixes is put into kneader and rubs, spray into the liquid blender that step (2) obtains, powder raw material becomes clod gradually simultaneously, namely completes pug preparation after the plasticity-of clod is stable;
(4) moulded pottery not yet put in a kiln to bake preparation: the pug that step (3) obtains is put into vacuum pugmill and carries out twice vacuum mud refining, in mud refining process, vacuum tightness is-0.093MPa, obtains the moulded pottery not yet put in a kiln to bake supporting with forming machine barrel specification;
(5) extrusion moulding: the moulded pottery not yet put in a kiln to bake that step (4) obtains is put into vacuum-extruder is under the condition of 10MPa at extrusion pressure, is extruded into the plasticity-ceramic honey comb biscuit of desired size by mould;
(6) dryness finalization: the ceramic honey comb biscuit that step (5) obtains is put into microwave oven and carry out the drying of inside and outside homogeneous heating, until the water ratio in base substrate is 1%, take out from microwave oven, base substrate is fixed to the ceramic honey comb work in-process of required specification;
(7) base substrate post-treatment: after the ceramic honey comb work in-process after step (6) being shaped put chi according to the ratio of burning till contraction, two ends redundance is cut away;
(8) product burns till: the base substrate processed in step (7) is put into kiln and burns till, and firing period is 48 hours, and firing temperature is 1430 DEG C, and soaking time is 5 hours, obtains required low-expansion coefficient cordierite honeycomb ceramic.
Performance Detection: the product after step embodiment 1, embodiment 2, embodiment 3 being burnt till carries out thermal expansivity and thermal-shock resistance detects, above-described embodiment 1, embodiment 2, embodiment 3 are obtained product and carry out thermal expansivity, thermal-shock resistance detection, and detected result is as shown in table 1 below:
More than show and describe ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (6)
1., based on a preparation method for the low-expansion coefficient cordierite honeycomb ceramic of fluid additive, it is characterized in that: comprise the following steps:
(1) powder raw material preparation: take the high-purity lamellar kaolin powder of 35 ~ 45wt%, the high-purity platy talc powder of 35 ~ 45wt%, 10 ~ 30wt% aluminum oxide powder, take the binding agent of above-mentioned raw materials gross weight 3 ~ 8wt% as shaping assistant simultaneously, above-mentioned raw materials, binding agent are added in powder mixer and fully stirs, until mix, obtain powder raw material;
(2) liquid blender preparation: take the powder raw material gross weight 20 ~ 35wt% water, 0.1 ~ 1.5wt% dispersion agent, the 0.5 ~ 2.5wt% lubricant that obtain in step (1), above-mentioned dispersion agent and lubricant are slowly added to the water and stir, until dispersion agent and lubricant are dissolved in water, obtain liquid blender;
(3) pug preparation: the powder raw material that step (1) mixes is put into kneader and rubs, spray into the liquid blender that step (2) obtains, powder raw material becomes clod gradually simultaneously, namely completes pug preparation after the plasticity-of clod is stable;
(4) moulded pottery not yet put in a kiln to bake preparation: the pug that step (3) obtains is put into vacuum pugmill and carries out vacuum mud refining, vacuum tightness≤-0.09MPa in mud refining process, obtain the moulded pottery not yet put in a kiln to bake supporting with forming machine barrel specification; If moulded pottery not yet put in a kiln to bake has demixing phenomenon, can adopt repeatedly repetition mud refining mode that moulded pottery not yet put in a kiln to bake is met the demands;
(5) extrusion moulding: the moulded pottery not yet put in a kiln to bake that step (4) obtains is put into vacuum-extruder, extrudes out the ceramic honey comb biscuit of desired size by mould;
(6) dryness finalization: the ceramic honey comb biscuit that step (5) obtains is put into microwave oven and carries out heat drying, until drying completes water ratio≤2% in base substrate, take out from microwave oven, base substrate is fixed to the ceramic honey comb work in-process of required specification;
(7) base substrate post-treatment: after the ceramic honey comb work in-process after step (6) being shaped put chi according to the ratio of burning till contraction, two ends redundance is cut away;
(8) product burns till: the ceramic honey comb work in-process processed according to dimensional requirement in step (7) are put into kiln and burns till, firing period is 25 ~ 120 hours, firing temperature is 1360 DEG C ~ 1450 DEG C, soaking time is 4 ~ 8 hours, obtains required low-expansion coefficient cordierite honeycomb ceramic.
2. the preparation method of a kind of low-expansion coefficient cordierite honeycomb ceramic based on fluid additive according to claim 1, is characterized in that: the binding agent in step (1) is Mierocrystalline cellulose, not containing Ash residue after calcining.
3. the preparation method of a kind of low-expansion coefficient cordierite honeycomb ceramic based on fluid additive according to claim 2, is characterized in that: described Mierocrystalline cellulose be molecular weight 4000 ~ 20000 Vltra tears.
4. the preparation method of a kind of low-expansion coefficient cordierite honeycomb ceramic based on fluid additive according to claim 1, is characterized in that: the dispersion agent in step (2) is polyether glycol.
5. the preparation method of a kind of low-expansion coefficient cordierite honeycomb ceramic based on fluid additive according to claim 1, is characterized in that: the lubricant in step (2) is water miscible organic high molecular compound.
6. the preparation method of a kind of low-expansion coefficient cordierite honeycomb ceramic based on fluid additive according to claim 5, is characterized in that: described water miscible organic high molecular compound is the one or more combination in oleic acid ester, oleate soap, lauroleate, polyvinyl alcohol.
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| CN104671741B (en) * | 2015-01-14 | 2017-07-25 | 凯龙蓝烽新材料科技有限公司 | A kind of preparation method of the big specification honeycomb ceramic carrier of use for diesel engine |
| CN106732819A (en) * | 2016-12-07 | 2017-05-31 | 山东大学 | A kind of preparation method of porous ceramic catalyst carrier material |
| CN111018544A (en) * | 2019-10-25 | 2020-04-17 | 界首市伟盛古窑彩陶制作发展有限公司 | Preparation process of extrusion molding ceramic pug |
| CN111377723B (en) * | 2020-03-24 | 2020-11-03 | 洛阳中超新材料股份有限公司 | Low-cost environment-friendly corundum-mullite honeycomb ceramic heat accumulator and preparation method thereof |
| CN114057474B (en) * | 2021-11-16 | 2023-02-07 | 重庆奥福精细陶瓷有限公司 | Large-size ultrathin-wall honeycomb ceramic catalyst carrier and preparation method and application thereof |
| CN116063093B (en) * | 2023-01-05 | 2023-12-26 | 武汉理工大学 | DPF honeycomb ceramic based on flaked kaolin and preparation method thereof |
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