CN112374504B - Process for manufacturing nano silicon dioxide by physical method - Google Patents
Process for manufacturing nano silicon dioxide by physical method Download PDFInfo
- Publication number
- CN112374504B CN112374504B CN202011221681.6A CN202011221681A CN112374504B CN 112374504 B CN112374504 B CN 112374504B CN 202011221681 A CN202011221681 A CN 202011221681A CN 112374504 B CN112374504 B CN 112374504B
- Authority
- CN
- China
- Prior art keywords
- slurry
- grinding
- hours
- silicon dioxide
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a process for preparing nano silicon dioxide by a physical method, which comprises the steps of raw material pretreatment, raw material particle surface treatment, primary crushing, particle dispersion, secondary crushing, particle dispersion and homogenization. The crystalline state and the granularity of a product prepared by the process for manufacturing the nano silicon dioxide by the physical method can not be achieved by the prior process; on the basis that the product purity reaches more than 99.9 percent, the process can meet the requirements of different industries such as chemical industry, electronics, integrated circuit wafers, LED substrate materials CMP and the like, and presents physical and chemical characteristics different from products manufactured by a non-physical manufacturing process; the solid content of the aqueous slurry of the product prepared by the invention can reach 50.5%, and the dispersion time at normal temperature is more than 180 days. Compared with the existing products with the same purity in the market, the process cost of the invention is less than 50%, the process of the invention has no dangerous raw materials such as inflammable, explosive, toxic, strong acid, strong alkali and the like, and has no high-temperature and high-pressure process.
Description
Technical Field
The invention relates to the technical field of silicon dioxide production processes, in particular to a process for manufacturing nano silicon dioxide by a physical method.
Background
The existing nano silicon dioxide is prepared by a chemical method, and the preparation method comprises a gas phase method, a precipitation method, a kaolin or hard kaolin silicon source method and a coal gangue or fly ash silicon source method.
The vapor phase processes are mainly Chemical Vapor Deposition (CVD) processes, also known as pyrolysis, dry or combustion processes. The raw materials are silicon tetrachloride, oxygen (or air) and hydrogen which are reacted at high temperature. The reaction formula is as follows:
SiCl 4 + 2H 2 + O 2 —>SiO 2 +4HCl
air and hydrogen are respectively pressurized, separated, cooled and dehydrated, dried by silica gel, dedusted and filtered, and then are sent into a synthetic hydrolysis furnace. The silicon tetrachloride raw material is sent to a rectifying tower for rectification, then is heated and evaporated in an evaporator, and is sent to a synthetic hydrolysis furnace by taking dried and filtered air as a carrier. The silicon tetrachloride is gasified at high temperature (flame temperature is 1000 to 1800 ℃), and then is subjected to gas phase hydrolysis with a certain amount of hydrogen and oxygen (or air) at the high temperature of about 1800 ℃; the generated fumed silica particles are extremely fine and form aerosol with gas, so that the aerosol is difficult to trap, and the fumed silica particles are gathered into larger particles in a collector, then the larger particles are collected by a cyclone separator and sent into a deacidification furnace, and the fumed silica is blown by nitrogen-containing air until the pH value is 4-6, so that the finished product is obtained.
The precipitation method is also called sodium silicate acidification method, and water glass solution is adopted to react with acid, and the nano silicon dioxide is obtained through precipitation, filtration, washing, drying and calcination. The reaction formula is as follows:
Na 2 SiO 3 + 2H + —> SiO 2 + 2Na + + H 2 O
the silicon source method of the kaolin or the hard kaolin comprises the following steps: firstly, kaolin or hard kaolin is crushed into 50 to 60 meshes, then the kaolin or hard kaolin is roasted for 2 hours at a high temperature of 500 to 600 ℃, and then the roasted soil and industrial hydrochloric acid with the concentration of 30 percent are mixed according to the weight ratio of 1:2.5 Proportioning, carrying out acid leaching for 7 hours at about 90 ℃, neutralizing, filtering, washing and drying to obtain nano silicon dioxide, wherein the product quality meets the GB10507-89 standard; and simultaneously obtaining the high-efficiency water purifying agent polyaluminium chloride. The roasting and acid leaching reaction formula is as follows:
roasting: al (aluminum) 2 O 3 •2SiO 2 •2H 2 O —> Al 2 O 3 •2SiO 2 + 2H 2 O
Acid leaching: al (aluminum) 2 O 3 •2SiO 2 + 6HCl + 9H 2 O—>2AlCl 3 •6H 2 O + 2SiO 2
The silicon source method of the coal gangue or the fly ash comprises the following steps: firstly, coal gangue or fly ash is crushed to the granularity of less than 120 meshes, and then the method comprises two steps:
the first step of sodium silicate production: mixing pulverized coal gangue or fly ash and soda ash according to the weight ratio of 1:50, evenly mixing, melting at high temperature (1400 to 1500 ℃,1 hour), extracting and dissolving in water (more than 100 ℃,4 to 5 hours), filtering to remove impurities, and concentrating the filtrate to 45 to 46 Baume degrees to obtain the sodium silicate.
The second step is to produce the nano silicon dioxide: firstly, sodium silicate is prepared into a water glass solution (the modulus is 2.4 to 3.6 2 The content is 4 to 10 percent), then the mixture is soaked in sulfuric acid with the concentration of 5 to 20 percent (the temperature is 28 to 32 ℃, and the time is 8 to 16 hours), the temperature is raised to 80 ℃, the mixture is stirred, the pH value is adjusted to be 5 to 7, the mixture is cured for 20 minutes, and then the nano silicon dioxide is obtained after filtration, washing, drying and sorting. The nanometer silicon dioxide is active and has high purity.
The existing nano silicon dioxide production technology has the following defects:
(1) Original sourceThe raw particles are amorphous and have great difference from crystalline particles in physical properties, and the prior art synthesizes SiO 2 There is no condition for the crystallization of the particles in the process.
(2) The primary particles have narrow strength distribution, which can not meet the requirements of most fields, and the prior art does not have the condition that the primary particles are beyond the size of 15-40 nm.
(3) The prior art has the problems of high energy consumption, large pollution, high safety risk, large environmental protection pressure and the like. According to the characteristics of the existing process, the process has the technical processes of using flammable, explosive, toxic, strong acid and other raw materials, and high temperature and high pressure.
(4) The existing high-purity product process has high cost (determined by process characteristics).
(5) The existing low-cost product has low purity (determined by process characteristics).
Disclosure of Invention
In view of the above technical problems in the related art, the present invention provides a process for producing nano-silica by physical method, which can overcome the above disadvantages in the prior art.
In order to achieve the technical purpose, the technical scheme of the invention is realized as follows:
a process for preparing nano silicon dioxide by a physical method comprises the following steps:
s1, raw material pretreatment: based on the weight portion, 1 portion of crystalline SiO 2 Adding the mixture into 0.8-1.5 parts of deionized water containing ammonium salt for primary dispersion to form slurry;
s2, surface treatment of raw material particles: adding a proper amount of surface treating agent into the slurry subjected to preliminary dispersion, and treating the slurry by using a dispersion machine;
s3, first-stage crushing and particle dispersing: conveying the dispersed slurry to a sand mill, and grinding for 1.5-3 hours by using zirconia microspheres with the diameter of 0.2-0.4mm as grinding media;
s4, secondary crushing and particle dispersing: continuously grinding for 6-11 hours, adjusting the particle size of the grinding medium to 0.5-2.5mm in the grinding process, adding an auxiliary agent with the mass of 0.5-4% of the powder, and adjusting the solid content by using deionized water;
s5, homogenization: and (3) conveying the continuously produced slurry to a stirring tank for stirring and homogenizing, and adding an auxiliary agent with the powder mass of 0.2-1.2% in the process.
Further, the process for manufacturing the nano silicon dioxide by the physical method comprises the following steps: s6, drying: drying the slurry to obtain powder nano SiO 2 。
Further, after the solid content is adjusted by deionized water in the step S4, the mixture is continuously ground for 0.1 to 5 hours, and an auxiliary agent with the powder mass of 0.2 to 3 percent is added in the grinding process.
Further, the concentration of the ammonium salt in the deionized water in the step S1 is 0.5-3wt%.
Further, the time for the treatment with the disperser in step S2 is 0.5 to 1.5 hours.
Further, 0.1-1.5wt% of ammonium salt is added during the grinding process of step S3.
The invention has the beneficial effects that: the indexes of the grain crystalline state and the grain size range of the product prepared by the process for preparing the nano silicon dioxide by the physical method are not reached by the prior process technology; on the basis that the product purity reaches more than 99.9 percent, the process can meet the requirements of different industries such as chemical industry, electronics, integrated circuit wafers, LED substrate material CMP (chemical mechanical polishing) and the like, and presents different physical and chemical characteristics from products manufactured by a non-physical manufacturing process; the solid content of the aqueous slurry of the product prepared by the invention can reach 50.5%, and the dispersion time at normal temperature is more than 180 days. Compared with the existing products with the same purity in the market (except the difference between the crystal form and the primary granularity and the process), the process cost for preparing the nano silicon dioxide by the physical method is less than 50 percent, mainly reducing the raw materials and the energy consumption and realizing the process conditions; the process disclosed by the invention has no dangerous raw materials such as inflammable, explosive, toxic, strong acid, strong alkali and the like, has no high-temperature and high-pressure process, and reduces the production cost and the risks of safety and environmental protection.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 shows a powder of nano SiO in accordance with an embodiment of the present invention 2 Electron micrograph of the product.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
Example 1
S1, the purity of the crystalline SiO is more than or equal to 99.95 percent, D50=1um, D100 is less than or equal to 10um 2 1kg of the aqueous dispersion solution was added to 0.8kg of deionized water containing 0.5wt% of ammonium salt in batches to carry out preliminary dispersion to form a slurry;
s2, adding 1wt% of 8030 surface treating agent into the slurry subjected to primary dispersion, and treating for 1.5 hours by using a dispersion machine;
s3, primary crushing and particle dispersing: conveying the dispersed slurry to a sand mill (a polyurethane material is adopted by a sand mill impeller, a silicon carbide material is adopted by an inner cylinder, and the vertical type sand mill impeller is vertical), grinding a medium by using zirconia micro-beads with the diameter of 0.2mm at the rotating speed of 700 r/min for 1.5 hours, and adding 0.1wt% of ammonium salt in the middle;
s4, secondary crushing and particle dispersing: continuing to continue the step S for 3 hours, adjusting the grain diameter of the grinding medium to 0.5mm in the process, rotating at 650 r/min, adding 9002 auxiliary agent with the mass of 0.5wt% of the powder, and adjusting the solid content to the required index by using deionized water;
s5, particle size fraction, particle size distribution adjustment and particle dispersion steps: continuing to continue the step S4.1 hours, and adding 9006 auxiliary agents with the powder mass of 0.2wt% in the process;
s6, a homogenization step: the slurry produced continuously is conveyed to a stirring tank (the inner wall of the stirring tank is lined with polyethylene) for stirring and homogenization, the rotating speed of a stirring blade in the stirring tank is 5 r/min, and the slurry is added in the processAdding 9009 auxiliary agent with the mass of 0.2wt% of powder to the nano SiO 2 After the slurry is prepared, the slurry can be filled and hermetically stored, and the storage temperature is between 0 and 35 ℃;
s7, a drying step: drying the slurry by a spray dryer to obtain powder nano SiO 2 The water content is adjusted according to the requirement, and the obtained powder nano SiO 2 The product is shown in figure 1.
Example 2
S1, preparing crystalline SiO with the purity of more than or equal to 99.95 percent, D50=3um and D100 of less than or equal to 15um 2 1kg of deionized water containing 3wt% of ammonium salt pairs is added into 1.5kg of the mixture in batches for primary dispersion to form slurry;
s2, adding 3.5wt% of 8030 surface treating agent into the slurry subjected to primary dispersion, and treating for 0.5 hour by using a dispersion machine;
s3, primary crushing and particle dispersing: conveying the dispersed slurry to a sand mill (a polyurethane material is adopted by a sand mill impeller, a silicon carbide material is adopted by an inner cylinder, and the vertical type sand mill impeller is vertical), grinding a medium by using zirconia micro-beads with the diameter of 0.4mm at the rotating speed of 950 rpm for 3 hours, and adding 1.5wt% of ammonium salt in the middle;
s4, secondary crushing and particle dispersing: continuing to continue the step S3 for 11 hours, adjusting the grain diameter of the grinding medium to 2.5mm in the process, rotating at 950 rpm, adding 9002 auxiliary agent with the mass of 4wt% of the powder, and adjusting the solid content to the required index by using deionized water;
s5, particle size fraction, particle size distribution adjustment and particle dispersion steps: continuing to continue the step S for 4 hours, and adding 9006 auxiliary agents accounting for 3wt% of the powder in the process;
s6, a homogenization step: continuously produced slurry is conveyed to a stirring tank (polyethylene is lined on the inner wall of the stirring tank) for stirring and homogenization, the rotating speed of a stirring blade in the stirring tank is 20 r/min, and 9009 auxiliary agent with the powder mass of 1.2wt% is added in the process, so that the nano SiO 2 After the slurry is prepared, the slurry can be canned and hermetically stored, and the storage temperature is between 0 and 35 ℃;
s7, a drying step: drying the slurry by a spray dryer to obtain powder nano SiO 2 The moisture is adjusted as required.
Example 3
S1, the purity of the crystalline SiO is more than or equal to 99.95 percent, D50=2um, D100 is less than or equal to 12um 2 1kg of deionized water containing 1wt% of ammonium salt pairs is added into 1kg of the mixture in batches for primary dispersion to form slurry;
s2, adding 2wt% of 8030 surface treating agent into the slurry subjected to primary dispersion, and treating for 1 hour by using a dispersion machine;
s3, primary crushing and particle dispersing: conveying the dispersed slurry to a sand mill (the impeller of the sand mill is made of polyurethane material, the inner cylinder is made of silicon carbide material, and the sand mill is vertical), grinding a medium which is zirconia micro-beads with the diameter of 0.3mm at the rotating speed of 800 r/min for 2 hours, and adding 1wt% of ammonium salt in the middle;
s4, secondary crushing and particle dispersing: continuing to continue the step S3 for 8 hours, adjusting the grain diameter of the grinding medium to 1mm in the process, rotating at 700 r/min, adding 9002 percent of auxiliary agent with the mass of 2 weight percent of powder, and adjusting the solid content to the required index by deionized water;
s5, a homogenization step: continuously produced slurry is conveyed to a stirring tank (polyethylene is lined on the inner wall of the stirring tank) for stirring and homogenization, the rotating speed of a stirring blade in the stirring tank is 10 r/min, and 9009 auxiliary agent with the powder mass of 0.6 percent is added in the process, so that the nano SiO 2 After the slurry is prepared, the slurry can be filled and hermetically stored, and the storage temperature is between 0 and 35 ℃;
s6, a drying step: drying the slurry by a spray dryer to obtain powder nano SiO 2 The moisture is adjusted as required.
The temperature of all the raw materials is between 5 and 29 ℃.
Powder of Nano SiO obtained in examples 1 to 3 2 The crystal form and particle size of the product are shown in table 1.
TABLE 1 powder Nano SiO 2 Crystal form and particle size of product
| Serial number | Crystal form | D50（nm） | D97（nm） | D100（nm） |
| 1 | Crystallization of | 73 | 115 | 177 |
| 2 | Crystallization of | 82 | 131 | 196 |
| 3 | Crystallization of | 88 | 164 | 220 |
In summary, by means of the above technical scheme of the present invention, the indexes of the grain crystalline state and the grain size range of the product produced by the process of the present invention are not reached by the existing process technology; the process can greatly improve the product purity and meet the requirements of different industries; compared with the existing products with the same purity in the market (except the difference between the crystal form and the primary granularity and the process), the process for preparing the nano silicon dioxide by the physical method has the advantages that the process cost is less than 50 percent, and mainly the reduction of raw materials and energy consumption and the realization of process conditions are realized; the process disclosed by the invention has no dangerous raw materials such as inflammable, explosive, toxic, strong acid, strong alkali and the like, has no high-temperature and high-pressure process, and reduces the production cost and the risks of safety and environmental protection.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (1)
1. A process for manufacturing nano silicon dioxide by a physical method is characterized by comprising the following steps:
s1, pretreatment of raw materials: based on the weight portion, 1 portion of crystalline SiO 2 Adding the mixture into 0.8-1.5 parts of deionized water containing ammonium salt for primary dispersion to form slurry, wherein the concentration of the ammonium salt in the deionized water in the step S1 is 0.5-3wt%;
s2, surface treatment of raw material particles: adding a proper amount of surface treating agent into the slurry subjected to preliminary dispersion, and treating the slurry by using a dispersion machine, wherein the treatment time of the dispersion machine in the step S2 is 0.5-1.5 hours;
s3, first-stage crushing and particle dispersing: conveying the dispersed slurry to a sand mill, grinding for 1.5-3 hours by using zirconia microbeads with the diameter of 0.2-0.4mm as grinding media, wherein an impeller of the sand mill is made of a polyurethane material, an inner cylinder of the sand mill is made of a silicon carbide material, and 0.1-1.5wt% of ammonium salt is added in the grinding process in the step S3;
s4, secondary crushing and particle dispersing: continuously grinding for 6-11 hours, adjusting the particle size of the grinding medium to 0.5-2.5mm in the grinding process, adding an auxiliary agent with the mass of 0.5-4% of the powder, continuously grinding for 0.1-5 hours after adjusting the solid content by deionized water, and adding the auxiliary agent with the mass of 0.2-3% of the powder in the grinding process;
s5, homogenization: conveying the continuously produced slurry to a stirring tank for stirring and homogenizing, and adding an auxiliary agent with the mass of 0.2-1.2% of the powder in the process;
s6, drying: drying the slurry to obtain powder nano SiO 2 。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011221681.6A CN112374504B (en) | 2020-11-05 | 2020-11-05 | Process for manufacturing nano silicon dioxide by physical method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011221681.6A CN112374504B (en) | 2020-11-05 | 2020-11-05 | Process for manufacturing nano silicon dioxide by physical method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112374504A CN112374504A (en) | 2021-02-19 |
| CN112374504B true CN112374504B (en) | 2023-01-24 |
Family
ID=74578783
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011221681.6A Active CN112374504B (en) | 2020-11-05 | 2020-11-05 | Process for manufacturing nano silicon dioxide by physical method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112374504B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103101919A (en) * | 2013-02-27 | 2013-05-15 | 东华大学 | Method for preparing ultrafine crystalline silica by using quartz tailings |
| CN107428544A (en) * | 2015-03-31 | 2017-12-01 | 日挥触媒化成株式会社 | Silica-based composite particles dispersion liquid, its manufacture method and the polishing slurry for including silica-based composite particles dispersion liquid |
| 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 |
| US20190106328A1 (en) * | 2015-07-10 | 2019-04-11 | Wolfgang Lortz | SiO2 Containing Dispersion With High Salt Stability |
| CN111180719A (en) * | 2020-01-07 | 2020-05-19 | 马鞍山科达普锐能源科技有限公司 | Method for preparing nano silicon by three-stage grinding |
| CN111196899A (en) * | 2018-11-20 | 2020-05-26 | 江苏金石研磨有限公司 | Superfine grinding preparation process for nano silicon oxide |
-
2020
- 2020-11-05 CN CN202011221681.6A patent/CN112374504B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103101919A (en) * | 2013-02-27 | 2013-05-15 | 东华大学 | Method for preparing ultrafine crystalline silica by using quartz tailings |
| CN107428544A (en) * | 2015-03-31 | 2017-12-01 | 日挥触媒化成株式会社 | Silica-based composite particles dispersion liquid, its manufacture method and the polishing slurry for including silica-based composite particles dispersion liquid |
| US20190106328A1 (en) * | 2015-07-10 | 2019-04-11 | Wolfgang Lortz | SiO2 Containing Dispersion With High Salt Stability |
| 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 |
| CN111196899A (en) * | 2018-11-20 | 2020-05-26 | 江苏金石研磨有限公司 | Superfine grinding preparation process for nano silicon oxide |
| CN111180719A (en) * | 2020-01-07 | 2020-05-19 | 马鞍山科达普锐能源科技有限公司 | Method for preparing nano silicon by three-stage grinding |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112374504A (en) | 2021-02-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2407055C (en) | Precipitated silicas, silica gels with and free of deposited carbon from caustic biomass ash solutions and processes | |
| WO2004073600A2 (en) | A novel process and appratus for the manufacture of precipitated silica from rice husk ash | |
| CN111547730B (en) | Preparation method of ultrafine precipitated silica anticaking agent for powder coating | |
| US4940571A (en) | Method of making large particle size, high purity dense silica | |
| CN105819484B (en) | A kind of Nano-meter CaCO33/SiO2The preparation method and dispersing method of compound particle | |
| CN114956101A (en) | High-dispersion micron-size silicon dioxide microsphere and preparation method thereof | |
| CN112374504B (en) | Process for manufacturing nano silicon dioxide by physical method | |
| CN1032585C (en) | Preparation for super fine powder of titanium dioxide | |
| CN111646480B (en) | Crystalline nano silicon dioxide and preparation method thereof | |
| RU2394764C1 (en) | Method of producing silicon dioxide | |
| CN108675310A (en) | The method for preparing ultrapure quartz sand as raw material using fluosilicic acid | |
| CN101172610B (en) | Method of producing high-temperature silica powder | |
| CN102491350A (en) | Method for directly preparing high-dispersion silicon dioxide microspheres from rice hulls | |
| CN107601536B (en) | Method for extracting aluminum oxide from high-alumina fly ash | |
| CN102198941B (en) | Method for preparing white carbon black by hydrolyzing silicon tetrachloride | |
| CN108821294A (en) | The method for preparing ultrapure quartz sand as raw material using common quartz sand | |
| CN111410197B (en) | Method for producing polyhedral silicon crystal | |
| Ishihara et al. | Synthesis of silicon carbide powders from fumed silica powder and phenolic resin | |
| CN102398908A (en) | Method for eliminating agglomeration produced in preparation of high-purity spherical nanometer amorphous silicon micropowder | |
| CN107200334A (en) | A kind of rice husk prepares the Efficient utilization method of white carbon | |
| CN110255569B (en) | Method for directly producing and preparing white carbon black from quartz mineral powder | |
| CN113929101A (en) | Method for co-producing white carbon black and fluosilicate by utilizing silicon tetrafluoride tail gas | |
| CN113321221A (en) | Method for preparing white carbon black by using iron tailings | |
| CN108570248B (en) | Preparation method of core-shell titanium dioxide coated silicon dioxide | |
| CN114804130B (en) | Method for preparing water glass and white carbon black by using serpentine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |