CN111073350A - Preparation method of submicron active silica micropowder - Google Patents

Preparation method of submicron active silica micropowder Download PDF

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CN111073350A
CN111073350A CN201911352715.2A CN201911352715A CN111073350A CN 111073350 A CN111073350 A CN 111073350A CN 201911352715 A CN201911352715 A CN 201911352715A CN 111073350 A CN111073350 A CN 111073350A
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quartz sand
powder
grinding
zirconia balls
sand particles
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彭寿
李佩悦
周新军
吴建新
张乾伟
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CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
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CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/12—Treatment with organosilicon compounds
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Abstract

The invention relates to a preparation method of submicron active silica powder, which is characterized by comprising the following steps: (1) putting quartz sand into a vertical mixer, grinding the quartz sand into zirconia balls, wherein the mass ratio of the quartz sand to the zirconia balls is 1: 8-15, and grinding for 20-40 min to obtain quartz sand particles with the particle size of-75 mu m; (2) adding a sand mill, adding 1-10% of ethylene glycol, grinding the zirconium oxide balls as an ore grinding medium, grinding the quartz sand particles for 60-120 min, wherein the mass ratio of the quartz sand particles to the zirconium oxide balls is 1: 3-5; (3) centrifuging, and drying the lower layer until the moisture content is less than 0.3%; (4) dispersing for 30-40min by using a vibration mill or a powder scattering machine; (5) feeding into an integrated device of jet milling and surface modification, adding 0.1-1.0% of modifier, crushing, depolymerizing and modifying the powder, and collecting the product. The invention has the advantages that: benefit toGrinding the raw materials to submicron grade with a sand mill efficiently; adopts the integrated equipment of air flow crushing and surface modification, improves the production efficiency, obtains good depolymerization and modification effects, and the silicon micropowder D50At 0.2 to 0.5 μm, D100Less than or equal to 2 microns and the activation index higher than 80 percent.

Description

Preparation method of submicron active silica micropowder
Technical Field
The invention belongs to the technical field of deep processing of nonmetallic minerals, and particularly relates to a preparation method of submicron active silicon micro powder.
Background
The silicon micropowder has the physical and chemical characteristics of high temperature resistance, acid and alkali resistance, excellent dielectric property, low thermal expansion coefficient, good filling and reinforcing properties and the like, and is widely applied to the chemical industries of coatings, rubber, plastics, high-grade ceramics and the like and the industries of semiconductor chips, optical fibers, high-voltage electrical appliance materials and the like. In recent years, the development of domestic silica products gradually changes from extensive to fine, especially the popularization of micro-nano technology and the development of optical electronic products, and the development of silica micro powder products in the superfine direction is accelerated.
The preparation of the superfine silicon powder is a mechanical pulverization process, and microscopically, the mechanical force promotes the coalescence of material particles while causing the particle size of the material particles to be reduced and the specific surface area to be increased, thereby increasing the apparent particle size and reducing the specific surface area. The strength relationship between the pulverization and the polymerization determines the efficiency of the powder preparation to a certain extent. When the silicon micropowder is ground to the particle size of about 5 μm by a dry method, the polymerization of the particles seriously reduces the grinding efficiency; the silicon micropowder has strong dispersion in liquid, the efficiency of wet grinding is higher than that of dry grinding, and nano-scale powder can be prepared, but the wet grinding has the defects that serious quartz particle polymerization can occur in the slurry drying process, and the depolymerization of the silicon micropowder becomes a technological problem. Since the last 90 years, the technology of preparing ultrafine powder by using a jet milling process has made a great breakthrough, but the silicon-oxygen covalent bond in silicon dioxide is a firm three-dimensional network structure, so that the silicon dioxide is difficult to break, the particle hardness is high, the single jet milling efficiency is not high, the energy consumption is high, and the difficulty in preparing submicron-grade silicon micropowder is high.
Disclosure of Invention
The invention aims to solve the problem that the submicron active silica powder is difficult to stably produce at present and provides a preparation method of the submicron active silica powder.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of submicron active silica powder is characterized by comprising the following steps:
(1) coarse grinding: putting quartz sand into a vertical mixer, wherein an ore grinding medium is zirconia balls, controlling the mass ratio of the quartz sand to the zirconia balls to be 1: 8-15, and grinding for 20-40 min to obtain quartz sand particles with the particle size of less than 75 mu m;
(2) fine grinding: adding the quartz sand particles obtained in the step (1) into a sand mill, adding ethylene glycol accounting for 1-10% of the weight of the quartz sand particles as a dispersing agent, taking zirconia balls as an ore milling medium, wherein the mass ratio of the quartz sand particles to the zirconia balls is 1: 3-5, and the ore milling time is 60-120 min to obtain the granularity D50≤0.2μm，D100Ore pulp with the particle size less than or equal to 1 mu m;
(3) dewatering and drying: centrifuging the ore pulp obtained in the step (2), removing the upper clear water, and drying the lower precipitate at 100-130 ℃ until the moisture content is less than 0.3%, thus obtaining plate powder;
(4) dispersing: dispersing the hardened powder obtained in the step (3) for 30-40min by adopting a vibration mill or a powder scattering machine to obtain powder;
(5) airflow crushing modification: and (3) conveying the powder obtained in the step (4) into airflow crushing-surface modification integrated equipment (equipment disclosed in CN 101433876A), adding a modifier accounting for 0.1-1.0% of the weight of the powder, colliding and rubbing material particles in a crushing chamber under the action of supersonic airflow, crushing, depolymerizing and modifying the powder, and collecting qualified products through a dust collector to obtain the submicron active silicon micro powder.
Furthermore, the vertical stirrer is internally provided with a polyurethane or alumina lining, the sand mill is internally provided with a polyurethane lining, and the vibration mill or the powder scattering machine is internally provided with an alumina lining.
Further, the modifier in the step (5) is a mixed solution of a silane coupling agent and ethanol, and the mass ratio of the silane coupling agent to the ethanol is 1: 3-6
Further, the submicron active silica powder D50At 0.2~0.5μm，D100Less than or equal to 2 microns and the activation index higher than 80 percent.
The invention has the advantages that: the front-end wet grinding process utilizes a sand mill to efficiently grind the raw materials to submicron level; the rear end adopts jet milling-surface modification integrated equipment, the mechanical force in the jet milling process is utilized to provide the depolymerization effect, the production efficiency of the jet milling equipment is improved, meanwhile, the adsorption effect of the modifier on the particle surface is enhanced due to the large amount of new high-activity surfaces of the particles, so that good depolymerization and particle modification effects are obtained, the silica micropowder D50 is 0.2-0.5 mu m, the D100 is less than or equal to 2 mu m, and the activation index is higher than 80%.
Drawings
Fig. 1 is a preparation process diagram of submicron active silica powder.
Detailed Description
A preparation method of submicron active silica micropowder comprises the following specific implementation steps:
the method is characterized in that quartz sand obtained by mineral separation and purification of a place in Taihu lake of Anhui province is used as a silicon micro powder raw material, and the silica micro powder comprises the following chemical components: SiO 22≥99.5%，Fe2O3Less than or equal to 0.0060 percent and the granularity less than 0.71 mm.
(1) Adding quartz sand into a vertical stirring ball mill, grinding the inner lining of a grinding cavity by polyurethane, grinding an ore grinding medium by zirconia balls, grinding the quartz sand and the zirconia balls for 30min under the condition that the mass ratio of the quartz sand to the zirconia balls is 1:10 and 350 r/min, and screening to remove quartz sand particles with the particle size of more than 74 mu m;
(2) adding the quartz sand particles with the particle size of less than 74 mu m obtained in the step (1) into a sand mill for superfine grinding, adding ethylene glycol accounting for 5 percent of the weight of the quartz sand particles as a dispersing agent, adopting a polyurethane lining in the sand mill, taking zirconia balls as grinding media, grinding the quartz sand particles and the zirconia balls for 60min at the rotating speed of 2000 r/min to obtain the quartz sand particles with the particle size of D50=0.18μm，D100Ore pulp of =0.89 μm;
(3) conveying the ore pulp obtained in the step (2) into a centrifuge for high-speed centrifugation, operating for 5min at 4000 revolutions per minute, removing supernatant, and drying lower-layer precipitates at 120 ℃ until the water content is less than or equal to 0.3%, thus obtaining plate caking powder;
(4) adding the hardened powder obtained in the step (3) into a vibration mill, wherein the vibration mill is an alumina lining, the grinding medium is zirconia balls, the mass ratio of the hardened powder to the zirconia balls is 1:8, and grinding for 30min to obtain powder;
(5) sending the powder obtained in the step (4) into an integrated device of jet milling and surface modification (the device is disclosed in the patent publication No. CN 101433876A), and respectively adding a silane coupling agent accounting for 0.2 percent of the weight of the powder and ethanol accounting for 0.6 percent of the weight of the powder; spraying modifier solution (ethanol solution of silane coupling agent) into the pulverizing chamber via nozzle by using quantitative adding device, simultaneously opening supersonic pulverizing nozzle, pulverizing silica particles in the pulverizing chamber with high-pressure air to achieve the purpose of surface modification treatment while pulverizing, and collecting qualified product via dust collector to obtain D50At 0.2 to 0.5 μm, D100Silicon micropowder with the particle size less than or equal to 2 mu m.
The main technical indexes of the prepared submicron active silica powder are as the following table 1:
Figure 263958DEST_PATH_IMAGE001

Claims (4)

1. a preparation method of submicron active silica powder is characterized by comprising the following steps:
(1) coarse grinding: putting quartz sand into a vertical mixer, wherein an ore grinding medium is zirconia balls, controlling the mass ratio of the quartz sand to the zirconia balls to be 1: 8-15, and grinding for 20-40 min to obtain quartz sand particles with the particle size of less than 75 mu m;
(2) fine grinding: adding the quartz sand particles obtained in the step (1) into a sand mill, adding ethylene glycol accounting for 1-10% of the weight of the quartz sand particles as a dispersing agent, grinding the quartz sand particles into zirconia balls, grinding the quartz sand particles into the zirconia balls for 60-120 min to obtain D, wherein the mass ratio of the quartz sand particles to the zirconia balls is 1: 3-550≤0.2μm，D100Ore pulp with the particle size less than or equal to 1 mu m;
(3) dewatering and drying: centrifuging the ore pulp obtained in the step (2), removing the upper clear water, and drying the lower precipitate at 100-130 ℃ until the moisture content is less than 0.3%, thus obtaining plate powder;
(4) dispersing: dispersing the hardened powder obtained in the step (3) for 30-40min by adopting a vibration mill or a powder scattering machine to obtain powder;
(5) airflow crushing modification: and (3) conveying the powder obtained in the step (4) into airflow crushing-surface modification integrated equipment, adding a modifier accounting for 0.1-1.0% of the weight of the powder, colliding and rubbing material particles in a crushing chamber under the action of supersonic airflow, crushing, depolymerizing and modifying the powder, and collecting qualified products through a dust collector to obtain the submicron active silicon micro powder.
2. The method for preparing submicron active silica powder according to claim 1, characterized in that: the vertical stirrer is internally provided with a polyurethane or alumina lining, the sand mill is internally provided with a polyurethane lining, and the vibration mill or the powder scattering machine is internally provided with an alumina lining.
3. The method for preparing submicron active silica powder according to claim 1, characterized in that: the modifier in the step (5) is a mixed solution of a silane coupling agent and ethanol, and the mass ratio of the silane coupling agent to the ethanol is 1: 3-6.
4. The method for preparing submicron active silica powder according to claim 1, characterized in that: the submicron active silica powder D50At 0.2 to 0.5 μm, D100Less than or equal to 2 microns and the activation index higher than 80 percent.
CN201911352715.2A 2019-12-25 2019-12-25 Preparation method of submicron active silica micropowder Pending CN111073350A (en)

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Publication number Priority date Publication date Assignee Title
CN101024732A (en) * 2006-02-24 2007-08-29 阮建军 Dry production process for producing epoxy moulding plastic super fine silicone micropowder
CN101433876A (en) * 2008-12-02 2009-05-20 北京航空航天大学 Integrated device for airflow pulverization and surface modification and technique thereof for preparing ultrafine grain
CN102093758A (en) * 2009-12-10 2011-06-15 湖南金马硅业有限公司 Artificial composite pigment and preparation method thereof
CN102120581A (en) * 2010-01-08 2011-07-13 湖南金马硅业有限公司 High-purity ultra-fine torispherical silicon micro-powder prepared from natural powder quartz ore and preparation method of silicon micro-powder
CN103627215A (en) * 2013-11-27 2014-03-12 连云港东海硅微粉有限责任公司 Preparation method of submicron silica powder
CN105936509A (en) * 2016-06-01 2016-09-14 安徽晶晶石英科技有限公司 Purifying method of ultralow-metal element highly pure quartz
CN108003382A (en) * 2017-12-28 2018-05-08 江苏联瑞新材料股份有限公司 A kind of preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order
CN108751204A (en) * 2018-05-14 2018-11-06 江苏联瑞新材料股份有限公司 A kind of preparation method of submicron silicon dioxide dispersion liquid
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
CN109320998A (en) * 2018-10-10 2019-02-12 江苏联瑞新材料股份有限公司 A kind of method that sub-micron silicon micropowder surface is modified

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101024732A (en) * 2006-02-24 2007-08-29 阮建军 Dry production process for producing epoxy moulding plastic super fine silicone micropowder
CN101433876A (en) * 2008-12-02 2009-05-20 北京航空航天大学 Integrated device for airflow pulverization and surface modification and technique thereof for preparing ultrafine grain
CN102093758A (en) * 2009-12-10 2011-06-15 湖南金马硅业有限公司 Artificial composite pigment and preparation method thereof
CN102120581A (en) * 2010-01-08 2011-07-13 湖南金马硅业有限公司 High-purity ultra-fine torispherical silicon micro-powder prepared from natural powder quartz ore and preparation method of silicon micro-powder
CN103627215A (en) * 2013-11-27 2014-03-12 连云港东海硅微粉有限责任公司 Preparation method of submicron silica powder
CN105936509A (en) * 2016-06-01 2016-09-14 安徽晶晶石英科技有限公司 Purifying method of ultralow-metal element highly pure quartz
CN108003382A (en) * 2017-12-28 2018-05-08 江苏联瑞新材料股份有限公司 A kind of preparation method of the spherical crystallization silicon powder of high-power total incapsulation transistor micron order
CN108751204A (en) * 2018-05-14 2018-11-06 江苏联瑞新材料股份有限公司 A kind of preparation method of submicron silicon dioxide dispersion liquid
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
CN109320998A (en) * 2018-10-10 2019-02-12 江苏联瑞新材料股份有限公司 A kind of method that sub-micron silicon micropowder surface is modified

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