CN101760054B - Preparation method of pyrophyllite-based nanometer composite powder - Google Patents
Preparation method of pyrophyllite-based nanometer composite powder Download PDFInfo
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- CN101760054B CN101760054B CN 200810163819 CN200810163819A CN101760054B CN 101760054 B CN101760054 B CN 101760054B CN 200810163819 CN200810163819 CN 200810163819 CN 200810163819 A CN200810163819 A CN 200810163819A CN 101760054 B CN101760054 B CN 101760054B
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Abstract
The invention relates to a preparation method of pyrophyllite-based nanometer composite powder, which uses low-aluminum-content pyrophyllite, kaolin and superfine silicon dioxide powder as solid raw materials and uses silane coupling agents and titanate coupling agents as surface modifiers. The Al2O3 content in the pyrophyllite powder is smaller than 20 percent, the Al2O3 carries out the calcination at the temperature between 500 and 700 DEG C, the kaolin is powder between 200 and 300 meshes and is calcined at the temperature between 500 and 700 DEG C, the average grain diameter of the superfine silicon dioxide powder is smaller than 0.5 mum, and the superfine silicon dioxide powder are dried at the temperature between 100 and 200 DEG C. The coupling agents are silane coupling agents or titanium ester coupling agents or compounds of the silane coupling agents and the titanium ester coupling agents. The invention has a formulation consisting of the following ingredients in percentage by weight: 50 to 90 of pyrophyllite powder, 0 to 20 of kaolin, 10 to 30 of superfine silicon dioxide powder and 0.5 to 2.0 of coupling agents. The coupling agents are respectively added by two times, 10 to 50 percent of the total amount of the coupling agents are added during wet method grinding, and 50 to 90 percent of the total amount of the coupling agents are added during dry method grinding. The composite powder has the average grain diameter smaller than 2 mum.
Description
Technical field
The present invention relates to a kind of preparation method of pyrophyllite-based nanometer composite powder, belong to novel material and mineral exploration and exploitation and Application Areas.
Background technology
Agalmatolite [Al
2(OH)
2(Si
2O
5)
2]
2Be a kind of of clay mineral, mainly be comprised of quartz, kaolinite, sericite, belong to 2: 1 type stratiforms of crystalline texture hydrous alumino silicates mineral, the structural unit layer is by two " silicon-oxygen tetrahedron ", and one " oxyhydrogen aluminum stone layer " forms.The theoretical chemistry component is: Al
2O
328.3%, SiO
266.7%, H
2O 5.0%, contains in addition Fe, Mg, Ca, K, a small amount of impurity such as Na.
The agalmatolite single crystal (oblique system) of natural output is rare, often is foliated lamellar, flakey, radial, fibrous or column aggregate, tool pearliness or wax-like gloss.That mineral have is white, pale yellow, light green, brick red and grey brown isochrome, little translucent.The fine and smooth tool soapy feeling of agalmatolite quality, hardness low (1-2), proportion 2.65-2.90g/cm
3, refractoriness＞1700 ℃, heat conduction, electric conductivity are low, good insulation preformance, stable chemical performance only has at high temperature and could be decomposed by sulfuric acid.
China is Pyrophyllite Resource big country, and the gross annual output amount accounts for about 40% of world's gross annual output amount, but in recovery process, the wasting of resources is very serious, adopt richness and abandon poorly, the rate of recovery is low to be to be quotidian in mining, and the development and use that therefore strengthen low aluminium pyrophyllite are significant.
The 1999.09.22 of Patent Office of the People's Republic of China day disclosed " preparation method of dispersible silico-aluminate " (publication number: 1229056), relate to a kind of preparation method who is dispersed in the high purity silicon aluminate in water and/or the acid solution medium, it is realized by hydrolysis and the thermal treatment of aluminum compound and silicate compound.
The 2005.11.02 of Patent Office of the People's Republic of China day disclosed " a kind of manufacture method of nanometer silicon-aluminium composite material " (publication number: CN 1689971A), relate to a kind of pyrophyllite nano-dispersed emulsion that is scattered in the etoh solvent, it is take pyrophyllite as raw material, by the water soaking pyrophyllite in powder, add silane coupling agent through hydrophobic treatment, process with tensio-active agent parcel again, be scattered in and make the nano-dispersed emulsion in the coordinative solvent.
" a kind of method of producing the silicon-aluminium compound stopping composition with the agalmatolite manufacturing " (patent No.: ZL 2,004 1 0066103.4) of authorizing the 2007.05.02 of Patent Office of the People's Republic of China day, relate to a kind of method of producing the silicon-aluminium compound stopping composition take agalmatolite as the raw material manufacturing, it is agalmatolite to be pulverized obtain the agalmatolite breeze, then the agalmatolite breeze is carried out the techniques such as pickling, flotation, drying after calcining and makes product.
By the domestic and foreign literature data analysis of present grasp, scientific worker both domestic and external has done a large amount of research and developments for modification and the application of mineral material.At present research mainly still concentrates on the modification application of the Mineral resources such as kaolin, calcium carbonate, for the applied research work of agalmatolite relatively also seldom, use low aluminium pyrophyllite and kaolin, superfine silicon dioxide and be raw material calcine, composite, prepare powder through two subsurface coupling modified techniques, can be applied to reinforcing rubber again, the research and development of the industrialization pyrophyllite product that performance can compare favourably with high wear-resistant carbon black are report not also.
Summary of the invention
The technical problem that quasi-solution of the present invention is determined provides a kind of preparation method of pyrophyllite-based nanometer composite powder.This powder can replace in certain proportion that high wear-resistant carbon black is applied to the styrene-butadiene rubber(SBR) product and the Main Mechanical that do not reduce rubber product.
For achieving the above object, the present invention by the following technical solutions: with low aluminium pyrophyllite, kaolin, nanometer SiO
2Powder is main raw material, utilizes silane and titanate coupling agent to be surface-modifying agent, by techniques such as high-temperature calcination, surperficial coupling processing, prepares styrene-butadiene rubber(SBR) reinforcement pyrophyllite-based nanometer composite powder.
The present invention is a kind of preparation method of pyrophyllite-based nanometer composite powder, it is characterized in that having following technological process and step:
1. described pyrophyllite is the low aluminium pyrophyllite in powder of 200-300 order, the Al of pyrophyllite in powder
2O
3Content is less than 20%, and through 500-700 ℃ of calcining, packing, for subsequent use.
2. described kaolin is 200-300 order kaolin, through 500-700 ℃ of calcining, packing, for subsequent use.
3. described silicon-dioxide powdery is superfine powder, and median size is less than 0.5 μ m, through 100-200 ℃ of oven dry, packing, for subsequent use.
4. described coupling agent is silane coupling agent or titanate coupling agent or the compound of the two, and the adding total amount of coupling agent is the 0.5-2% of solid base.Silane coupling agent comprises 3-aminopropyl triethoxysilane, 3-glycidyl ether oxygen base propyl trimethoxy silicane, 3-methacryloxypropyl trimethoxy silane, two-(3-(triethoxyl silane)-propyl group)-tetrasulfide, and titanate coupling agent comprises sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester, tetra isopropyl two (dioctyl phosphorous acid acyloxy) titanic acid ester.
5. batch mixing, grinding, filtration, drying: the raw material for subsequent use in 1,2,3 is mixed in proportion, grinds after adding suitable quantity of water and part coupling agent, be ground to median size and stop to grind less than 2 μ m, filter, drying.
6. coupling processing: gained powder in 5 in the coupling machine, is carried out surface modification and namely obtains product of the present invention under 100-120 ℃ of temperature.
7. the prescription of powder of the present invention following (wt%): base-material: pyrophyllite in powder 50-90, kaolin 0-20, silicon-dioxide powdery 10-30.Coupling agent: 0.5-2.0
Embodiment
Embodiment 1:
Starting in the stirred pot of stirring in the 50kg deionized water, add successively Al
2O
3Content is 8% pyrophyllite in powder 10kg, kaolin 2kg, silicon-dioxide powdery 2kg, rear adding 0.07kg 3-aminopropyl triethoxysilane stirs, continue to stir 1 hour, then grind, be ground to median size and begin to filter, dry, pulverize less than 2 μ m.Powder after the pulverizing carries out the coupling modification at the coupling machine with 0.1kg 3-aminopropyl triethoxysilane, namely makes pyrophyllite-based nanometer composite powder.
Embodiment 2:
Starting in the stirred pot of stirring in the 50kg deionized water, add successively Al
2O
3Content is 15% pyrophyllite in powder 10kg, kaolin 2kg, silicon-dioxide powdery 2kg, rear adding 0.07kg 3-glycidyl ether oxygen base propyl trimethoxy silicane stirs, continue to stir 1 hour, then grind, be ground to median size and begin to filter, dry, pulverize less than 2 μ m.Powder after the pulverizing carries out the coupling modification at the coupling machine with 0.1kg 3-glycidyl ether oxygen base propyl trimethoxy silicane, namely makes pyrophyllite-based nanometer composite powder.
Embodiment 3:
Starting in the stirred pot of stirring in the 50kg deionized water, add successively Al
2O
3Content is 18% pyrophyllite in powder 10kg, kaolin 2kg, silicon-dioxide powdery 2kg, rear adding 0.07kg 3-methacryloxypropyl trimethoxy silane stirs, continue to stir 1 hour, then grind, be ground to median size and begin to filter, dry, pulverize less than 2 μ m.Powder after the pulverizing carries out the coupling modification at the coupling machine with 0.1kg 3-methacryloxypropyl trimethoxy silane, namely makes pyrophyllite-based nanometer composite powder.
Embodiment 4:
Starting in the stirred pot of stirring in the 60kg deionized water, add successively Al
2O
3Content is 15% pyrophyllite in powder 15kg, kaolin 3kg, silicon-dioxide powdery 2kg, rear adding 0.1kg 3-aminopropyl triethoxysilane stirs, continue to stir 1 hour, then grind, be ground to median size and begin to filter, dry, pulverize less than 2 μ m.Powder after the pulverizing carries out the coupling modification at the coupling machine with 0.15kg 3-aminopropyl triethoxysilane, namely makes pyrophyllite-based nanometer composite powder.
Embodiment 5:
Starting in the stirred pot of stirring in the 50kg deionized water, add successively Al
2O
3Content is 18% pyrophyllite in powder 10kg, kaolin 3kg, silicon-dioxide powdery 2kg, rear adding 0.1kg 3-methacryloxypropyl trimethoxy silane stirs, continue to stir 1 hour, then grind, be ground to median size and begin to filter, dry, pulverize less than 2 μ m.Powder after the pulverizing carries out the coupling modification at the coupling machine with 0.15kg 3-methacryloxypropyl trimethoxy silane, namely makes pyrophyllite-based nanometer composite powder.
Embodiment 6:
Starting in the stirred pot of stirring in the 50kg deionized water, add successively Al
2O
3Content is 18% pyrophyllite in powder 12kg, kaolin 3kg, silicon-dioxide powdery 2kg, rear adding 0.1kg 3-methacryloxypropyl trimethoxy silane stirs, continue to stir 1 hour, then grind, be ground to median size and begin to filter, dry, pulverize less than 2 μ m.Powder after the pulverizing carries out the coupling modification at the coupling machine with 0.12kg sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester, namely makes pyrophyllite-based nanometer composite powder.
Embodiment 7:
Starting in the stirred pot of stirring in the 50kg deionized water, add successively Al
2O
3Content is 18% pyrophyllite in powder 12kg, kaolin 3kg, silicon-dioxide powdery 2kg, rear adding 0.1kg pair-(3-(triethoxyl silane)-propyl group)-tetrasulfide stirs, continue to stir 1 hour, then grind, be ground to median size and begin to filter, dry, pulverize less than 2 μ m.Powder after the pulverizing carries out the coupling modification, namely makes pyrophyllite-based nanometer composite powder with 0.15kg pair-(3-(triethoxyl silane)-propyl group)-tetrasulfide at the coupling machine.
Embodiment 8:
Starting in the stirred pot of stirring in the 50kg deionized water, add successively Al
2O
3Content is 10% pyrophyllite in powder 12kg, kaolin 3kg, silicon-dioxide powdery 2kg, rear adding 0.1kg pair-(3-(triethoxyl silane)-propyl group)-tetrasulfide stirs, continue to stir 1 hour, then grind, be ground to median size and begin to filter, dry, pulverize less than 2 μ m.Powder after the pulverizing carries out the coupling modification at the coupling machine with 0.15kg tetra isopropyl two (dioctyl phosphorous acid acyloxy) titanic acid ester, namely makes pyrophyllite-based nanometer composite powder.
Product section of the present invention is replaced high wear-resistant carbon black use as strengthening agent, obtained desirable effect.
The present invention compares with background technology, uses low aluminium pyrophyllite and composite kaolin and superfine silicon dioxide, so that raw material sources are more extensive, exploitation has realistic meaning for lean ore.Add surperficial coupling properties-correcting agent so that powder granularity is easily controlled by process of lapping, without pickling, also need not be dispersed in and make slip in the organic solvent, optimized technique, three-waste free pollution has been realized green chemical industry technique.Product cost is lower simultaneously, is easy to industry and applies.
Claims (1)
1. the preparation method of a pyrophyllite-based nanometer composite powder is characterized in that, with low aluminium pyrophyllite, kaolin, nanometer SiO
2Powder is main raw material, utilizes silane and titanate coupling agent to be surface-modifying agent, by high-temperature calcination, surperficial coupling processing technique, prepares styrene-butadiene rubber(SBR) reinforcement pyrophyllite-based nanometer composite powder, has following technological process and step:
(1) described pyrophyllite is the low aluminium pyrophyllite in powder of 200-300 order, the Al of pyrophyllite in powder
2O
3Content is less than 20%, and through 500-700 ℃ of calcining, packing, for subsequent use;
(2) described kaolin is 200-300 order kaolin, through 500-700 ℃ of calcining, packing, for subsequent use;
(3) described silicon-dioxide powdery is superfine powder, and median size is less than 0.5 μ m, through 100-200 ℃ of oven dry, packing, for subsequent use;
(4) described coupling agent is silane coupling agent or titanate coupling agent or the compound of the two, the adding total amount of coupling agent is the 0.5-2% of solid base, silane coupling agent is selected from 3-aminopropyl triethoxysilane, 3-glycidyl ether oxygen base propyl trimethoxy silicane, 3-methacryloxypropyl trimethoxy silane, two-(3-(triethoxyl silane)-propyl group)-tetrasulfide, and titanate coupling agent is selected from sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester, tetra isopropyl two (dioctyl phosphorous acid acyloxy) titanic acid ester;
(5) batch mixing, grinding, filtration, drying: the raw material for subsequent use in (1), (2), (3) is mixed in proportion, grind after adding suitable quantity of water and part coupling agent, be ground to median size and stop to grind less than 2 μ m, filter, drying;
(6) coupling processing: gained powder in (5) is carried out surface modification and namely obtains product in the coupling machine under 100-120 ℃ of temperature.
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| CN103333527B (en) * | 2013-06-04 | 2015-08-12 | 广东新会美达锦纶股份有限公司 | A kind of manufacture method of polyamide fibre chemical fibre surface modification matting agent |
| CN105017812A (en) * | 2014-11-26 | 2015-11-04 | 安徽池州博源非金属矿研发中心有限公司 | Composite titanium dioxide |
| CN105038327A (en) * | 2014-11-26 | 2015-11-11 | 安徽池州博源非金属矿研发中心有限公司 | Preparation method of dolomite composite titanium dioxide |
| CN105001679A (en) * | 2014-11-26 | 2015-10-28 | 安徽池州博源非金属矿研发中心有限公司 | Composite titanium dioxide |
| RU2676060C2 (en) * | 2017-03-03 | 2018-12-25 | Дмитрий Николаевич Задорин | Smooth scaled pyrophyllite-based substrate and method for production thereof |
| CN106883458A (en) * | 2017-03-09 | 2017-06-23 | 浙江皓翔矿业有限公司 | A kind of preparation method of modified pyrophyllite powder |
| CN109135346A (en) * | 2018-09-05 | 2019-01-04 | 中建材蚌埠玻璃工业设计研究院有限公司 | Modified silicon powder of a kind of high pure and ultra-fine and preparation method thereof |
| CN111437793A (en) * | 2020-03-27 | 2020-07-24 | 浙江工业大学 | Pyrophyllite-carbon composite adsorption material and liquid phase preparation method thereof |
| CN114854188B (en) * | 2022-04-28 | 2023-02-24 | 福州大学 | Pyrophyllite/polyurethane composite film and preparation method and application thereof |
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| CN101058646A (en) * | 2007-05-30 | 2007-10-24 | 中南大学 | Method of preparing inorganic composition particles for polymer composite material |
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| CN101058646A (en) * | 2007-05-30 | 2007-10-24 | 中南大学 | Method of preparing inorganic composition particles for polymer composite material |
Non-Patent Citations (3)
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|---|
| JP特开平8－48910A 1996.02.20 |
| 王志远等."偶联剂KH-550改性煅烧高岭土对NBR胶料性能的影响".《橡胶工业》.2007,第54卷(第4期),第228－2231页. |
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