CN103011840A - 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, particularly a kind of automobile honeycomb ceramic carrier is with the preparation method of ultra-fine molten silicon micro mist.
Background technology
Along with the high speed development of national economy, China's automobile pollution rapid growth.According to statistics, by in by the end of June, 2012, China's vehicle guaranteeding organic quantity is 2.33 hundred million.At present the source of atmospheric pollution of nearly all big and medium-sized cities maximum is all from the discharging of vehicle exhaust, and wherein the hydrocarbon polymer of 73.5% in the atmospheric polluting material, 63.4% carbon monoxide, 46% oxynitrides are 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, and people's health is caused great infringement.
Administering automobile exhaust pollution is a systems engineering, needs multiple technologies, multiple means to come integrated use.For example, improve fuel qualities, improvement engine technology, strict exhaust emissions and use novel energy etc., wherein the purification of tail gas is one of important measures of environmental contamination reduction.In the car tail-gas catalytic purifier, support of the catalyst is to realize a key factor of efficient tail-gas purifying.In the solid support material that adopts, mainly be divided into two kinds of ceramic monolith and metallic carriers, but what be used widely is honeycomb ceramic carrier.Ceramic honey comb is to be formed by various material, and main material has: the composite interstitial substances such as trichroite, mullite, aluminium titanates, zirconium white, silicon carbide and violet green grass or young crops-mullite, trichroite-aluminium titanates.Wherein trichroite (2MgO2AL2035Si02) ceramic honey comb is as principal crystalline phase take cordierite crystal, its moulding is as cellular a kind of porous ceramics, it has that intensity is large, low bulk, resistance to heat shocks is good, adsorptivity is strong, the advantage such as wear-resistant and become the most frequently used self-contained auto-exhaust catalyst carrier, can satisfy state III, the requirement of state IV exhaust emission standard.Automobile is abominable especially with the environment for use of honeycomb ceramic carrier, and it is again component in the rear discharge treating system simultaneously, therefore, also requires very high to its system coordination adaptability.Cleaning catalyst for tail gases of automobiles to the major requirement of its honeycomb ceramic carrier is: with catalyst component without chemical reaction, specific surface area that certain physical strength, thermostability and good thermal shock, thermal expansivity is little and higher etc.For satisfying above-mentioned performance requriements, adding functional silica filler has irreplaceable effect to honeycomb ceramic carrier towards aspect development such as high strength, high heat-resisting, low bulks.Aspect functional silica filler, the molten silicon micro mist has unique intrinsic advantage.The main component of molten silicon micro mist is sio2, belongs to the amorphous body structure, and particle is ultra-fine, and its surface-area is large, active high, and it is the desirable raw material of chemical building material still not, and is the mineralizer of silicate material solid state reaction and sintering.It can improve the intensity of honeycomb ceramic carrier as the mineralizer of the sintering of the solid state reaction of trichroite and idiosome, reduces the thermal expansivity of trichroite, strengthens its work-ing life.
In honeycomb ceramic carrier preparation, add ultra-fine melting powder filler, mainly contain following two purposes: the one, effectively reduce the thermal expansivity of honeycomb ceramic carrier, satisfy thermal shock resistance; The 2nd, reduce the foreign matter content in the cordierite honeycomb ceramic, improve purity and the performance of cordierite honeycomb ceramic.Therefore, add functional ultra-fine molten silicon micropowder filler honeycomb ceramic carrier is had irreplaceable effect towards aspect development such as high strength, high heat-resisting, low bulks.The 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 automobile honeycomb ceramic carrier and will capture the difficult problems such as a lot of technology, technique, equipment with ultra-fine molten silicon micro mist.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, provide a kind of method more reasonable, workable, product has the automobile honeycomb ceramic carrier of the high-performances such as high heat-resisting, low bulk, low impurity with the preparation method of ultra-fine molten silicon micro mist.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention be a kind of automobile honeycomb ceramic carrier with the preparation method of ultra-fine molten silicon micro mist, be characterized in that its step is as follows:
(1) chooses SiO
2Content is not less than 99.8% unformed fused quartz sandy plain material, and carries out proportioning by following raw material granularity distribution: the 5-10 order accounts for 15-25%, and the 15-40 order accounts for 40-60%, and the 50-100 order accounts for 25-35%;
(2) the above-mentioned raw material for preparing is carried out the magnetic separation impurity elimination, select the magnetic plant greater than 6000GS to carry out magnetic separation; Carry out extra-fine grinding with accurate Ball Mill System again, grind mill Jie who uses and be alumina balls, mill Jie diameter is respectively: diameter is the 40-48% that accounts for of 18-20 mm, and diameter is the 25-38% that accounts for of 30-35 mm, and diameter is the 23-27% that accounts for of 46-48mm;
(3) use grading machine to carry out fine grading after the extra-fine grinding, obtain the work in-process of particle diameter D50=2-3 μ m, D90≤9 μ m, D100≤13 μ m after the classification;
(4) work in-process are heated to 110-130 ℃ after, add the surface modification mixed solution that accounts for work in-process weight 0.5-1.5% in the work in-process, raw material is coated modification, be incubated again 60-100 minute after the discharging cooling, and get final product; Described surface modification mixed solution is made into by the raw material of following weight ratio: KH-560 silane coupling agent 80-85%; Organic radical modified polyorganosiloxane tensio-active agent 6-12%; High-molecular polyvinyl alcohol hyper-dispersant 5-10%;
(5) after the cooling gained silicon powder is carried out the secondary fine grading, obtain the finished product of particle diameter D10≤1.5 μ m, D50=2-3 μ m, D90≤9 μ m, D100≤13 μ m after the classification.
Compared with prior art, the inventive method has following technique effect: the inventive method is by selecting the proportioning raw materials of the most suitable granularity, mill Jie proportioning of grinding plant is carried out parameter control, 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 high-performances such as height is heat-resisting, low bulk, low impurity with ultra-fine molten silicon micro mist, can reduce automobile honeycomb ceramic carrier thermal expansivity, improves the heat shock resistance temperature.
Embodiment
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 consist of its Copyright law.
Embodiment 1, and a kind of automobile honeycomb ceramic carrier is characterized in that with the preparation method of ultra-fine molten silicon micro mist its step is as follows:
(1) chooses SiO
2Content is not less than 99.8% unformed fused quartz sandy plain material, and distributes by following raw material granularity and to carry out proportioning: the 5-10 order accounts for 15%, 15-40 order and accounts for 60%, 50-100 order and account for 25%;
(2) the above-mentioned raw material for preparing is carried out the magnetic separation impurity elimination, select the magnetic plant greater than 6000GS to carry out magnetic separation; Carry out extra-fine grinding with accurate Ball Mill System again, grind the mill uses and be situated between and be alumina balls, grind Jie's diameter and be respectively: diameter be 18-20 mm account for 40%, diameter is the 25-38% that accounts for of 35 mm, diameter be 46-48mm account for 25%;
(3) use grading machine to carry out fine grading after the extra-fine grinding, obtain the work in-process of particle diameter D50=2-3 μ m, D90≤9 μ m, D100≤13 μ m after the classification;
(4) work in-process are heated to 110 ℃ after, add the surface modification mixed solution that accounts for work in-process weight 0.5% in the work in-process, raw material is coated modification, be incubated again 60 minutes after the discharging cooling, and get final product; Described surface modification mixed solution is made into by the raw material of following weight ratio: KH-560 silane coupling agent 80%; Organic radical modified polyorganosiloxane tensio-active agent 10%; High-molecular polyvinyl alcohol hyper-dispersant 10%;
(5) after the cooling gained silicon powder is carried out the secondary fine grading, obtain the finished product of particle diameter D10≤1.5 μ m, D50=2-3 μ m, D90≤9 μ m, D100≤13 μ m after the classification.
Embodiment 2, and a kind of automobile honeycomb ceramic carrier is characterized in that with the preparation method of ultra-fine molten silicon micro mist its step is as follows:
(1) chooses SiO
2Content is not less than 99.8% unformed fused quartz sandy plain material, and distributes by following raw material granularity and to carry out proportioning: the 15-10 order accounts for 25%, 15-40 order and accounts for 40%, 50-100 order and account for 35%;
(2) the above-mentioned raw material for preparing is carried out the magnetic separation impurity elimination, select the magnetic plant greater than 6000GS to carry out magnetic separation; Carry out extra-fine grinding with accurate Ball Mill System again, grind the mill uses and be situated between and be alumina balls, grind Jie's diameter and be 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 grading machine to carry out fine grading after the extra-fine grinding, obtain the work in-process of particle diameter D50=2-3 μ m, D90≤9 μ m, D100≤13 μ m after the classification;
(4) work in-process are heated to 120 ℃ after, add the surface modification mixed solution that accounts for work in-process weight 1.5% in the work in-process, raw material is coated modification, be incubated again 100 minutes after the discharging cooling, and get final product; Described surface modification mixed solution is made into by the raw material of following weight ratio: KH-560 silane coupling agent 85%; Organic radical modified polyorganosiloxane tensio-active agent 10%; High-molecular polyvinyl alcohol hyper-dispersant 5%;
(5) after the cooling gained silicon powder is carried out the secondary fine grading, obtain the finished product of particle diameter D10≤1.5 μ m, D50=2-3 μ m, D90≤9 μ m, D100≤13 μ m after the classification.
Embodiment 3, and a kind of automobile honeycomb ceramic carrier is characterized in that with the preparation method of ultra-fine molten silicon micro mist its step is as follows:
(1) chooses SiO
2Content is not less than 99.8% unformed fused quartz sandy plain material, and distributes by following raw material granularity and to carry out proportioning: the 5-10 order accounts for 20%, 15-40 order and accounts for 50%, 50-100 order and account for 30%;
(2) the above-mentioned raw material for preparing is carried out the magnetic separation impurity elimination, select the magnetic plant greater than 6000GS to carry out magnetic separation; Carry out extra-fine grinding with accurate Ball Mill System again, grind the mill uses and be situated between and be alumina balls, grind Jie's diameter and be 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 grading machine to carry out fine grading after the extra-fine grinding, obtain the work in-process of particle diameter D50=2-3 μ m, D90≤9 μ m, D100≤13 μ m after the classification;
(4) work in-process are heated to 130 ℃ after, add the surface modification mixed solution that accounts for work in-process weight 0.8% in the work in-process, raw material is coated modification, be incubated again 80 minutes after the discharging cooling, and get final product; Described surface modification mixed solution is made into by the raw material of following weight ratio: KH-560 silane coupling agent 84%; Organic radical modified polyorganosiloxane tensio-active agent 6%; High-molecular polyvinyl alcohol hyper-dispersant 10%;
(5) after the cooling gained silicon powder is carried out the secondary fine grading, obtain the finished product of particle diameter D10≤1.5 μ m, D50=2-3 μ m, D90≤9 μ m, D100≤13 μ m after the classification.
Claims (1)
1. an automobile honeycomb ceramic carrier is characterized in that its step is as follows with the preparation method of ultra-fine molten silicon micro mist:
(1) chooses SiO
2Content is not less than 99.8% unformed fused quartz sandy plain material, and carries out proportioning by following raw material granularity distribution: the 5-10 order accounts for 15-25%, and the 15-40 order accounts for 40-60%, and the 50-100 order accounts for 25-35%;
(2) the above-mentioned raw material for preparing is carried out the magnetic separation impurity elimination, select the magnetic plant greater than 6000GS to carry out magnetic separation; Carry out extra-fine grinding with accurate Ball Mill System again, grind mill Jie who uses and be alumina balls, mill Jie diameter is respectively: diameter is the 40-48% that accounts for of 18-20 mm, and diameter is the 25-38% that accounts for of 30-35 mm, and diameter is the 23-27% that accounts for of 46-48mm;
(3) use grading machine to carry out fine grading after the extra-fine grinding, obtain the work in-process of particle diameter D50=2-3 μ m, D90≤9 μ m, D100≤13 μ m after the classification;
(4) work in-process are heated to 110-130 ℃ after, add the surface modification mixed solution that accounts for work in-process weight 0.5-1.5% in the work in-process, raw material is coated modification, be incubated again 60-100 minute after the discharging cooling, and get final product; Described surface modification mixed solution is made into by the raw material of following weight ratio: KH-560 silane coupling agent 80-85%; Organic radical modified polyorganosiloxane tensio-active agent 6-12%; High-molecular polyvinyl alcohol hyper-dispersant 5-10%;
(5) after the cooling gained silicon powder is carried out the secondary fine grading, obtain the finished product of particle diameter D10≤1.5 μ m, D50=2-3 μ m, D90≤9 μ m, D100≤13 μ m after the classification.
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Cited By (10)
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| CN103937294A (en) * | 2014-05-08 | 2014-07-23 | 连云港华威硅微粉有限公司 | Preparation method of silicon micropowder for high-density integrated circuit packaging |
| CN104163430A (en) * | 2014-09-09 | 2014-11-26 | 江苏联瑞新材料股份有限公司 | Method for preparing high-purity transparent silica micro powder for pouring sealant |
| CN104194274A (en) * | 2014-09-09 | 2014-12-10 | 江苏联瑞新材料股份有限公司 | Method for preparing silica powder for full-encapsulated epoxy molding compound |
| CN106255315A (en) * | 2016-07-28 | 2016-12-21 | 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 |
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| 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 |
| US20220162080A1 (en) * | 2019-01-30 | 2022-05-26 | Quarzwerke Gmbh | Sequestering of crystalline silicon dioxide |
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| CN103937294A (en) * | 2014-05-08 | 2014-07-23 | 连云港华威硅微粉有限公司 | Preparation method of silicon micropowder for high-density integrated circuit packaging |
| CN104163430A (en) * | 2014-09-09 | 2014-11-26 | 江苏联瑞新材料股份有限公司 | Method for preparing high-purity transparent silica micro powder for pouring sealant |
| CN104194274A (en) * | 2014-09-09 | 2014-12-10 | 江苏联瑞新材料股份有限公司 | Method for preparing silica powder for full-encapsulated epoxy molding compound |
| 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 |
| CN106255315A (en) * | 2016-07-28 | 2016-12-21 | 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 |
| 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 |
| US20220162080A1 (en) * | 2019-01-30 | 2022-05-26 | Quarzwerke Gmbh | Sequestering of crystalline silicon dioxide |
| 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 |
| CN111892058A (en) * | 2020-07-04 | 2020-11-06 | 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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