CN103011840B - Preparation method for ultrafine fused silica powder used in automobile honeycomb ceramic carrier - Google Patents
Preparation method for ultrafine fused silica powder used in automobile honeycomb ceramic carrier Download PDFInfo
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Abstract
The invention provides a preparation method for ultrafine fused silica powder used in an automobile honeycomb ceramic carrier. The method comprises the following steps: an amorphous fused quartz sand raw material with SiO2 content not less than 99.8% is selected, is magnetically separated for removing impurities after being proportioned by a certain particle size distribution, and is superfinely grinded by a precise ball mill system; the diameters of mesoporous aluminum oxide balls for grinding are proportioned; the precise grading is implemented by a classifier after the superfine grinding to obtain semi-finished products; and the secondary precise grading is implemented for the semi-finished products after modification to obtain finished products, wherein the particle size D10 of the finished products is not more than 1.5 microns, the particle size D50 is in a range of 2 to 3 microns, the particle size D90 is not more than 9 microns, and the particle size D100 is not more than 13 microns. The method can produce the ultrafine fused silica powder used in the automobile honeycomb ceramic carrier, can reduce the thermal expansion coefficient of the automobile honeycomb ceramic carrier, and can improve the heat resistant shock temperature; and the superfine fused silica powder has excellent properties, such as high heat resistance, low expansion, low impurity and the like.
Description
Technical field
The present invention relates to a kind of preparation method of molten silicon micro mist, the particularly a kind of automobile honeycomb ceramic carrier preparation method with ultra-fine molten silicon micro mist.
Background technology
Along with the high speed development of national economy, China's automobile pollution increases fast.According to statistics, by by the end of June, 2012, China's vehicle guaranteeding organic quantity is 2.33 hundred million.The maximum source of atmospheric pollution in big and medium-sized cities nearly all at present all from the discharge of vehicle exhaust, wherein 73.5% in atmosphere pollution hydrocarbon, 63.4% carbon monoxide, 46% oxynitrides all from vehicle exhaust.In addition, the test result of domestic and international big city air quality is shown: vehicle exhaust is big city air-polluting primary pollution source, causes great infringement to the health of people.
Administering automobile exhaust pollution is a system engineering, needs multiple technologies, multiple means carrys out integrated use.Such as, improve fuel qualities, improvement engine technology, strict exhaust emissions and application novel energy etc., wherein the purification of tail gas is one of important measures reducing environmental pollution.In car tail-gas catalytic purifier, catalyst carrier is the key factor realizing efficient tail-gas purifying.In adopted carrier material, be mainly divided into ceramic monolith and metallic carrier two kinds, but what be used widely is honeycomb ceramic carrier.Ceramic honey comb can be formed by various material, and main material has: the composite interstitial substances such as cordierite, mullite, aluminium titanates, zirconia, silicon carbide and violet green grass or young crops-mullite, cordierite-aluminium titanates.Wherein cordierite (2MgO2AL2035Si02) ceramic honey comb take cordierite crystal as principal crystalline phase, its moulding is as cellular a kind of porous ceramics, it has the advantages such as intensity is large, low bulk, resistance to heat shocks are good, adsorptivity is strong, wear-resistant and becomes the most frequently used self-contained auto-exhaust catalyst carrier, can meet state III, the requirement of state IV exhaust emission standard.The environment for use of automobile honeycomb ceramic carrier is severe especially, and it is again parts in rear discharge treating system simultaneously, therefore, also requires very high to its system coordination adaptability.The major requirement of cleaning catalyst for tail gases of automobiles to its honeycomb ceramic carrier is: with catalyst component without chemical reaction, certain mechanical strength, heat endurance and good thermal shock, specific area etc. that thermal coefficient of expansion is little and higher.For meeting above-mentioned performance requirement, adding functionalized silica filler has irreplaceable effect to honeycomb ceramic carrier towards aspect development such as high strength, high heat-resisting, low bulks.At functionalized silica surface side filler, molten silicon micro mist has unique intrinsic advantage.The main component of molten silicon micro mist is sio2, belongs to amorphous body structure, particles ultra fine, and its surface area is large, active high, the desirable raw material of its not still chemical building material, and is the mineralizer of silicate material solid phase reaction and sintering.It as the mineralizer of the sintering of the solid phase reaction of cordierite and idiosome, can improve the intensity of honeycomb ceramic carrier, reduces the thermal coefficient of expansion of cordierite, strengthens its service life.
In honeycomb ceramic carrier preparation, add ultra-fine melting powder filler, mainly contain following two objects: one is the thermal coefficient of expansion effectively reducing honeycomb ceramic carrier, meets thermal shock resistance; Two is reduce the impurity content in cordierite honeycomb ceramic, improves purity and the performance of cordierite honeycomb ceramic.Therefore, add functional ultra-fine molten silicon micropowder filler and have irreplaceable effect to honeycomb ceramic carrier towards aspect development such as high strength, high heat-resisting, low bulks.Automobile honeycomb ceramic carrier is high with the production technology content of ultra-fine molten silicon micro mist, is a direction of silicon powder technical development.Accomplish that consecutive production goes out the ultra-fine molten silicon micro mist of automobile honeycomb ceramic carrier and will capture the difficult problems such as a lot of technology, technique, equipment.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, there is provided a kind of method more reasonable, workable, product has the preparation method of the ultra-fine molten silicon micro mist of automobile honeycomb ceramic carrier of the superior functions such as height is heat-resisting, low bulk, low impurity.
Technical problem to be solved by this invention is realized by following technical scheme.The present invention is the preparation method of a kind of automobile honeycomb ceramic carrier with ultra-fine molten silicon micro mist, and be characterized in, its step is as follows:
(1) SiO is chosen
2content is not less than the unformed vitreous silica sandy plain material of 99.8%, and carries out proportioning by following raw material granularity distribution: 5-10 order accounts for 15-25%, and 15-40 order accounts for 40-60%, and 50-100 order accounts for 25-35%;
(2) magnetic separation impurity elimination is carried out to the above-mentioned raw material prepared, select the magnetic plant being greater than 6000GS to carry out magnetic separation; Carry out extra-fine grinding with precision ball grinder system again, it is alumina balls that the mill that grinding uses is situated between, and mill Jie diameter is respectively: diameter be 18-20 mm account for 40-48%, diameter be 30-35 mm account for 25-38%, diameter be 46-48mm account for 23-27%;
(3) use grader to carry out fine grading after extra-fine grinding, obtain after classification particle diameter D50=2-3 μm, D90≤9 μm, D100≤13 μm semi-finished product;
(4), after semi-finished product being heated to 110-130 DEG C, in semi-finished product, adding the surface modification mixed liquor accounting for semi-finished product weight 0.5-1.5%, coating modification is carried out to raw material, then discharging cooling after being incubated 60-100 minute, to obtain final product; Described surface modification mixed liquor is made into by the raw material of following weight ratio: KH-560 silane coupler 80-85%; Organo-modified polysiloxane surfactant 6-12%; High-molecular polyvinyl alcohol hyper-dispersant 5-10%;
(5) after cooling, secondary fine grading is carried out to gained silicon powder, after classification, obtain the finished product of particle diameter D10≤1.5 μm, D50=2-3 μm, D90≤9 μm, D100≤13 μm.
Compared with prior art, the inventive method has following technique effect: the inventive method is by selecting the pulp furnish of appropriate particle size the most, state modulator is carried out to mill Jie proportioning of milling apparatus, control dioxide-containing silica and Control of Impurities technology, and carry out surface modification, the automobile honeycomb ceramic carrier that production is obtained has the superior functions such as height is heat-resisting, low bulk, low impurity with ultra-fine molten silicon micro mist, can reduce automobile honeycomb ceramic carrier thermal coefficient of expansion, improve heat shock resistance temperature.
Detailed description of the invention
Below further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not form the restriction to its right.
Embodiment 1, a kind of automobile honeycomb ceramic carrier preparation method of ultra-fine molten silicon micro mist, it is characterized in that, its step is as follows:
(1) SiO is chosen
2content is not less than the unformed vitreous silica sandy plain material of 99.8%, and carries out proportioning by the distribution of following raw material granularity: 5-10 order accounts for 15%, 15-40 order and accounts for 60%, 50-100 order and account for 25%;
(2) magnetic separation impurity elimination is carried out to the above-mentioned raw material prepared, select the magnetic plant being greater than 6000GS to carry out magnetic separation; Carry out extra-fine grinding with precision ball grinder system again, it is alumina balls that the mill that grinding uses is situated between, and mill Jie diameter is respectively: diameter be 18-20 mm account for 40%, diameter be 35 mm account for 25-38%, diameter be 46-48mm account for 25%;
(3) use grader to carry out fine grading after extra-fine grinding, obtain after classification particle diameter D50=2-3 μm, D90≤9 μm, D100≤13 μm semi-finished product;
(4), after semi-finished product being heated to 110 DEG C, in semi-finished product, adding the surface modification mixed liquor accounting for semi-finished product weight 0.5%, coating modification is carried out to raw material, then discharging cooling after being incubated 60 minutes, to obtain final product; Described surface modification mixed liquor is made into by the raw material of following weight ratio: KH-560 silane coupler 80%; Organo-modified polysiloxane surfactant 10%; High-molecular polyvinyl alcohol hyper-dispersant 10%;
(5) after cooling, secondary fine grading is carried out to gained silicon powder, after classification, obtain the finished product of particle diameter D10≤1.5 μm, D50=2-3 μm, D90≤9 μm, D100≤13 μm.
Embodiment 2, a kind of automobile honeycomb ceramic carrier preparation method of ultra-fine molten silicon micro mist, it is characterized in that, its step is as follows:
(1) SiO is chosen
2content is not less than the unformed vitreous silica sandy plain material of 99.8%, and carries out proportioning by the distribution of following raw material granularity: 15-10 order accounts for 25%, 15-40 order and accounts for 40%, 50-100 order and account for 35%;
(2) magnetic separation impurity elimination is carried out to the above-mentioned raw material prepared, select the magnetic plant being greater than 6000GS to carry out magnetic separation; Carry out extra-fine grinding with precision ball grinder system again, it is alumina balls that the mill that grinding uses is situated between, and mill Jie diameter is respectively: diameter be 18-20 mm account for 47%, diameter be 30-35 mm account for 30%, diameter be 46-48mm account for 23%;
(3) use grader to carry out fine grading after extra-fine grinding, obtain after classification particle diameter D50=2-3 μm, D90≤9 μm, D100≤13 μm semi-finished product;
(4), after semi-finished product being heated to 120 DEG C, in semi-finished product, adding the surface modification mixed liquor accounting for semi-finished product weight 1.5%, coating modification is carried out to raw material, then discharging cooling after being incubated 100 minutes, to obtain final product; Described surface modification mixed liquor is made into by the raw material of following weight ratio: KH-560 silane coupler 85%; Organo-modified polysiloxane surfactant 10%; High-molecular polyvinyl alcohol hyper-dispersant 5%;
(5) after cooling, secondary fine grading is carried out to gained silicon powder, after classification, obtain the finished product of particle diameter D10≤1.5 μm, D50=2-3 μm, D90≤9 μm, D100≤13 μm.
Embodiment 3, a kind of automobile honeycomb ceramic carrier preparation method of ultra-fine molten silicon micro mist, it is characterized in that, its step is as follows:
(1) SiO is chosen
2content is not less than the unformed vitreous silica sandy plain material of 99.8%, and carries out proportioning by the distribution of following raw material granularity: 5-10 order accounts for 20%, 15-40 order and accounts for 50%, 50-100 order and account for 30%;
(2) magnetic separation impurity elimination is carried out to the above-mentioned raw material prepared, select the magnetic plant being greater than 6000GS to carry out magnetic separation; Carry out extra-fine grinding with precision ball grinder system again, it is alumina balls that the mill that grinding uses is situated between, and mill Jie diameter is respectively: diameter be 18-20 mm account for 45%, diameter be 30-35 mm account for 28%, diameter be 46-48mm account for 27%;
(3) use grader to carry out fine grading after extra-fine grinding, obtain after classification particle diameter D50=2-3 μm, D90≤9 μm, D100≤13 μm semi-finished product;
(4), after semi-finished product being heated to 130 DEG C, in semi-finished product, adding the surface modification mixed liquor accounting for semi-finished product weight 0.8%, coating modification is carried out to raw material, then discharging cooling after being incubated 80 minutes, to obtain final product; Described surface modification mixed liquor is made into by the raw material of following weight ratio: KH-560 silane coupler 84%; Organo-modified polysiloxane surfactant 6%; High-molecular polyvinyl alcohol hyper-dispersant 10%;
(5) after cooling, secondary fine grading is carried out to gained silicon powder, after classification, obtain the finished product of particle diameter D10≤1.5 μm, D50=2-3 μm, D90≤9 μm, D100≤13 μm.
Claims (1)
1. an automobile honeycomb ceramic carrier preparation method for ultra-fine molten silicon micro mist, it is characterized in that, its step is as follows:
(1) SiO is chosen
2content is not less than the unformed vitreous silica sandy plain material of 99.8%, and carries out proportioning by the distribution of following raw material granularity: 5-10 order accounts for 20%, 15-40 order and accounts for 50%, 50-100 order and account for 30%;
(2) magnetic separation impurity elimination is carried out to the above-mentioned raw material prepared, select the magnetic plant being greater than 6000GS to carry out magnetic separation; Carry out extra-fine grinding with precision ball grinder system again, it is alumina balls that the mill that grinding uses is situated between, and mill Jie diameter is respectively: diameter be 18-20mm account for 45%, diameter be 30-35mm account for 28%, diameter be 46-48mm account for 27%;
(3) use grader to carry out fine grading after extra-fine grinding, obtain after classification particle diameter D50=2-3 μm, D90≤9 μm, D100≤13 μm semi-finished product;
(4), after semi-finished product being heated to 130 DEG C, in semi-finished product, adding the surface modification mixed liquor accounting for semi-finished product weight 0.8%, coating modification is carried out to raw material, then discharging cooling after being incubated 80 minutes, to obtain final product; Described surface modification mixed liquor is made into by the raw material of following weight ratio: KH-560 silane coupler 84%; Organo-modified polysiloxane surfactant 6%; High-molecular polyvinyl alcohol hyper-dispersant 10%;
(5) after cooling, secondary fine grading is carried out to gained silicon powder, after classification, obtain the finished product of particle diameter D10≤1.5 μm, D50=2-3 μm, D90≤9 μm, D100≤13 μm.
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| CN103937294B (en) * | 2014-05-08 | 2017-02-01 | 连云港华威硅微粉有限公司 | Preparation method of silicon micropowder for high-density integrated circuit packaging |
| CN104163430B (en) * | 2014-09-09 | 2016-08-24 | 江苏联瑞新材料股份有限公司 | Preparation method for the high-purity transparent fine silica powder of casting glue |
| CN104194274B (en) * | 2014-09-09 | 2016-09-07 | 江苏联瑞新材料股份有限公司 | The preparation method of the epoxy molding plastic silicon powder of total incapsulation |
| CN106255315B (en) * | 2016-07-28 | 2019-04-16 | 江苏联瑞新材料股份有限公司 | A kind of preparation method of ic substrate electron level superfine composite silicon powder |
| CN106278207A (en) * | 2016-07-29 | 2017-01-04 | 江苏联瑞新材料股份有限公司 | A kind of honeycomb ceramic carrier preparation method of functional silicon powder for automobile exhaust purifier |
| CN110510619A (en) * | 2019-09-11 | 2019-11-29 | 江苏凯达石英股份有限公司 | The preparation method of active superfine vitreous silica SILICA FUME |
| CN111892058B (en) * | 2020-07-04 | 2022-05-17 | 江苏联瑞新材料股份有限公司 | Superfine silicon powder for surface mount discrete device and preparation method thereof |
| CN111974527A (en) * | 2020-07-07 | 2020-11-24 | 江苏联瑞新材料股份有限公司 | Preparation method of high-purity fused silica micropowder for IC packaging |
| CN114479518A (en) * | 2022-01-17 | 2022-05-13 | 安徽科技学院 | Superfine electronic grade composite quartz powder with low expansion rate and high thermal conductivity and production method thereof |
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