CN1508068A - Method for preparing nano silicon dioxide using diatomaceous earth - Google Patents
Method for preparing nano silicon dioxide using diatomaceous earth Download PDFInfo
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- CN1508068A CN1508068A CNA021567646A CN02156764A CN1508068A CN 1508068 A CN1508068 A CN 1508068A CN A021567646 A CNA021567646 A CN A021567646A CN 02156764 A CN02156764 A CN 02156764A CN 1508068 A CN1508068 A CN 1508068A
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- precipitation
- diatomite
- silicon dioxide
- nano silicon
- acid
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 28
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 18
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 16
- 239000005909 Kieselgur Substances 0.000 title 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- 238000001556 precipitation Methods 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000032683 aging Effects 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 5
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 13
- 238000003916 acid precipitation Methods 0.000 claims description 10
- 239000002981 blocking agent Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 4
- 230000020477 pH reduction Effects 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- -1 polysiloxane Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 125000000373 fatty alcohol group Chemical group 0.000 claims 1
- 239000004115 Sodium Silicate Substances 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052911 sodium silicate Inorganic materials 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract 3
- 238000003483 aging Methods 0.000 abstract 1
- 239000012754 barrier agent Substances 0.000 abstract 1
- 230000003750 conditioning effect Effects 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000012756 surface treatment agent Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- JCCZVLHHCNQSNM-UHFFFAOYSA-N [Na][Si] Chemical compound [Na][Si] JCCZVLHHCNQSNM-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The method for preparing nano silicon dioxide by utilizing diatomite includes the following steps: calcining diatomite powder at a certain temperature, making the calcined diatomite powder and sodium hydroxide implement reaction under the condition of heating to form sodium silicate, filtering reaction product to remove residue, adding sodium salt, adding water to proper concentration, then adding acid to make precipitation separation, in the course of precipitation separation or in the end point of precipitation separation adding barrier agent or surface conditioning agent to prevent the formed hydrated nano silicon dioxide particles from coacervating, making the precipitation separate product undergo the processes of ageing, filtering, washing and drying so as to obtain the invented product.
Description
The invention relates to a method for preparing nano silicon dioxide by using diatomite.
The nano silicon dioxide is an important inorganic nano functional powder material, is widely applied to the fields of coatings, plastics, leather, rubber, adhesives, sealants, chemical fibers, ceramics, medicines and the like, and has good market prospect.
The existing preparation methods of nano silicon dioxide mainly comprise a gas phase method, a sol-gel method and a reversed-phase micelle microemulsion method.
The gas phase method is prepared by hydrolyzing silicon tetrachloride in oxyhydrogen flame. The silica molecules produced by the hydrolysis agglomerate into particles. These particles collide with each other and fuse into one body to form a three-dimensional and branched chain aggregate. Once these aggregate temperatures are below the silica melting point, this further collides, causing mechanical entanglement of the bonds, creating agglomerates. This method has the advantage of producing less aggregation of particles and the disadvantage of high cost.
The sol-gel method is to prepare homogeneous sol of metal oxide or metal non-oxide by using metal alkoxide and inorganic salt as raw materials and utilizing the hydrolysis or precipitation reaction of metal alkoxide and inorganic salt. Then, the sol-gel conversion process is carried out to form an organic polymer network or an inorganic network. After gelation, aging, drying and heat treatment are carried out. The method has the advantages of mild reaction condition, high purity of silicon dioxide, large specific surface area and good activity. The disadvantage is that the material shrinks due to the volatilization of solvent and moisture in the gel drying process, and the nano particles can be obtained only by post-treatment.
The reversed-phase micelle microemulsionmethod is characterized in that an emulsion is formed by a surfactant, an auxiliary agent, oil and water firstly, a solvent with a small dosage is wrapped in a solvent with a large dosage to form microbubbles, the surfaces of the microbubbles are composed of the surfactant, and the size of the microbubbles ranges from 5 nm to 100 nm. The formation of a solid phase from microbubbles allows nucleation to occur, such as by condensation, agglomeration, etc., within a tiny spherical droplet, thereby forming a spherical particle. The nano particles prepared by the method have small particle size and good dispersibility, but the process is complex and the production cost is higher.
The invention aims at the defects of the three methods for preparing the nano silicon dioxide, provides a method for preparing the high-quality nano silicon dioxide by using natural mineral diatomite minerals as raw materials, and can simplify the process and reduce the energy consumption and the production cost.
The invention firstly calcines the diatomite ore powder, then reacts with caustic soda, and prepares the nano silicon dioxide by adopting the processes of acid precipitation, particle blocking (anti-agglomeration), aging, washing and dehydration after the reaction product is filtered to remove residues.
The process comprises the following steps:
(1) calcining the diatomite powder at a certain temperature to remove organic matters and oxidize ferrous iron into high-valence iron;
(2) the calcined diatomite powder and caustic soda are reacted under the heating condition to generate a sodium silicate aqueous solution, and the reaction formula is as follows:
(3) filtering the reaction product, removing solid residues, adding sodium salt, adding water to adjust to proper concentration, and precipitating with acid; and adding a particle blocking agent or a surface treatment agent in the acid precipitation process or at the end point of the acid precipitation. The acid precipitation chemical reaction formula is as follows:
m in the reaction formula (2) is SiO in sodium silicate2With Na2The ratio of O (sodium-silicon ratio) to SiO in the calcined diatomaceous earth powder2The content is related to the feeding ratio of caustic soda.
The diatomite is natural mineral and has SiO as main chemical component2·nH2O，SiO2The content is 70-95%.
When acid is used for precipitation in the step (3), sulfuric acid or hydrochloric acid can be used.
In the step (3), the sodium salt added before the acid precipitation is sodium sulfate or sodium chloride or the mother liquor obtained after the filtration of the product of the previous precipitation, and the using amount is 20-60% of the mass of the calcined diatomite.
The particle blocking agent or surface treatment agent used in step (3) is a chemical substance capable of generating adsorption with the surface of the nano-silica particles, such as fatty alcohol, silane, polysiloxane, fatty amine, and the like.
The formula and the process conditions of the invention are as follows:
(1) the calcining temperature of the diatomite is 500-850 ℃; the calcination time is 20-75 min.
(2) The mass ratio of the materials for the reaction of the calcined diatomite and the caustic soda is as follows: calcined diatomite powder, caustic soda and water are 1 (0.3-0.8) to 3.0-6.0 respectively; the reaction temperature of the calcined diatomite and the caustic soda is 80-120 ℃;
the reaction time of the calcined diatomite and the caustic soda is 0.5-4.0 hr.
(3) The acid dosage of the precipitation operation is 40-80% of the weight of the calcined diatomite; the pH value of the acidification end point is 3-5; the concentration of the acid precipitation solution is 10-20 Baume degrees (10 degrees Be 'to 24 degrees Be');
the precipitation temperature is 30-80 ℃; the settling time is 50-120 min.
(4) The dosage of the particle blocking agent in precipitation is 2-8% of the mass of the nano silicon dioxide.
The process flow of the invention is shown in figure 1.
Compared with the prior art, the method has the advantages of cheap and easily available raw materials, simple process, small product particle size, high specific surface area, good particle dispersibility and low production cost.
Example 1
Jilin Linjiang grade II diatomite (SiO)283.2% content, particle size passing 200 mesh) 1175g, calcined in a tube furnace at 700 ℃ for 35 min. The weight of the calcined diatomaceous earth was 1000 g. The calcined diatomaceous earth was added with 500g of solid industrial caustic soda and 4500g of water, and stirred in a reaction vessel to react for 90 gmin (reaction temperature 100 ℃); filtering the reaction product to remove residues, adding 200g of industrial sodium sulfate, adding water to dilute the solution to 18-degree Baume degrees, adding 550g of sulfuric acid to precipitate (the precipitation temperature is 35 ℃, the time is 100min, and the end-point pH value is about 3.5), and adding 45 g of butanol serving as a particle blocking agent in the precipitation process; aging the precipitation product for 30min, filtering, washing and drying to obtain the nano silicon dioxide product.
Example 2
Jilin Linjiang grade II diatomite (SiO)283.2% content, particle size passing 200 mesh) 1175g, calcined in a tube furnace at 600 ℃ for 40 min. The weight of the calcined diatomaceous earth was 1000 g. Adding the calcined diatomite to 550g of solid industrial caustic soda and 4500g of water are stirred in a reaction kettle to react for 120min (the reaction temperature is 100 ℃); filtering the reaction product to remove residues, adding 200g of industrial sodium sulfate, adding water to dilute the solution to 16-degree Baume, adding 600g of sulfuric acid to precipitate (the precipitation temperature is 45 ℃, the time is 90min, and the end-point pH value is about 3.5), and adding 40 g of particle blocking agent glycerol in the precipitation process; aging the precipitation product for 30min, filtering, washing and drying to obtain the nano silicon dioxide product.
Example 3
Jilin Linjiang grade II diatomite (SiO)2Content 83.2%, particle size passing 200 mesh) 23kg, calcined in a tube furnace at 600 ℃ for 45 min. The weight of the calcined diatomaceous earth was 20 kg. Adding 11kg of solid industrial caustic soda and 90kg of water into the calcined diatomite, and stirring and reacting for 120min (reaction temperature is 100 ℃) in a reaction pot; filtering the reaction product to remove residues, adding 4kg of industrial sodium sulfate, adding water to dilute the reaction product to 16-degree Baume degrees, adding 12kg of sulfuric acid to perform precipitation (the precipitation temperature is 42 ℃, the time is 90min, and the end-point pH value is about 3.5), and adding 820 g of a particleblocking agent glycerol in the precipitation process; aging the precipitation product for 30min, filtering, washing and drying to obtain the nano silicon dioxide product.
The results of the detection and analysis of the nano-silica of each example are shown in Table 1.
Table 1 results of the detection and analysis of nanosilica products of the examples
| Item | Example 1 | Example 2 | Example 3 |
| Silicon dioxide content% | 98.65 | 98.87 | 98.79 |
| Particle size, nm | 15～40 | 15～40 | 15～40 |
| Reduced on ignition,% | 2.21 | 2.16 | 2.20 |
| PH | 5.7 | 5.8 | 5.6 |
| Specific surface area, m2/g | 526 | 509 | 498 |
| Pore volume, ml/g | 0.62 | 0.67 | 0.65 |
| Bulk Density, g/ml | 0.10 | 0.11 | 0.11 |
| Oil absorption, ml/100g | 216 | 208 | 210 |
Claims (5)
1. A method for preparing nano silicon dioxide by using diatomite is characterized by comprising the following steps:
(1) calcining the diatomite ore powder;
(2) reacting calcined diatomite powder with caustic soda under heating;
(3) filtering the reaction product to remove residues, adding sodium salt, adding water to adjust to a proper concentration, adding acid to precipitate, and adding a particle blocking agent;
(4) and (4) aging, filtering, washing and drying the precipitation product.
2. The method for calcining the diatomite ore powder is characterized in that the calcining temperature is 500-850 ℃; the calcination time is 20-75 min.
3. The calcined diatomite of claim 1 is reacted with caustic soda under heating, wherein: the mass ratio of the materials is as follows: calcined diatomite powder, caustic soda and water are 1 to (0.3-0.8) to (3.0-6.0); the reaction temperature is 80-120 ℃; the reaction time is 0.5-4.0 hr.
4. The acid precipitation according to claim 1, wherein the amount of acid is 40-80% of the mass of calcined diatomite; the pH value of the acidification end point is 3-5; the concentration of the acid precipitation solution was: 10-20 Baume degrees (10 DEG Be 'to 24 DEG Be'); the amount of the sodium salt before acid precipitation is 20-60% of the weight of the calcined diatomite; the acidification temperature is 30-80 ℃; the acid precipitation time is 50-120 min.
5. The added particle blocking agent as set forth in claim 1, wherein:
(1) the particle blocking agent is fatty alcohol, silane, polysiloxane and fatty amine;
(2) the particle blocking agent can be added in the precipitation process, or can be added at the precipitation end point or before aging, and the dosage of the particle blocking agent is 2-8% of the mass of the nano silicon dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02156764 CN1212267C (en) | 2002-12-18 | 2002-12-18 | Method for preparing nano silicon dioxide using diatomaceous earth |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02156764 CN1212267C (en) | 2002-12-18 | 2002-12-18 | Method for preparing nano silicon dioxide using diatomaceous earth |
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| Publication Number | Publication Date |
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| CN1508068A true CN1508068A (en) | 2004-06-30 |
| CN1212267C CN1212267C (en) | 2005-07-27 |
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| CN 02156764 Expired - Fee Related CN1212267C (en) | 2002-12-18 | 2002-12-18 | Method for preparing nano silicon dioxide using diatomaceous earth |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913595A (en) * | 2010-08-04 | 2010-12-15 | 中国科学院广州地球化学研究所 | Method for preparing porous carbon and white carbon black by using diatomite |
| CN101962188A (en) * | 2010-11-15 | 2011-02-02 | 西藏大为建筑环保工程有限责任公司 | Method for preparing ultrafine high-purity SiO2 from volcanic ash |
| CN101985357A (en) * | 2010-10-13 | 2011-03-16 | 蒋珂 | Preparation method of white carbon black |
| CN102491351A (en) * | 2011-12-13 | 2012-06-13 | 沈阳化工大学 | Method for preparing white carbon black through natural clinoptilolite |
| CN103193236A (en) * | 2013-03-05 | 2013-07-10 | 浙江工业大学 | Method of preparing silica by using diatomite |
| CN104192851A (en) * | 2014-08-28 | 2014-12-10 | 确成硅化学股份有限公司 | Method for preparing nano silicon dioxide |
| CN104556073A (en) * | 2015-01-16 | 2015-04-29 | 陈旭 | Process for purifying inorganic nonmetallic minerals |
| CN107324350A (en) * | 2017-08-22 | 2017-11-07 | 北京依依星科技有限公司 | A kind of method for preparing nanoprecipitation silica using low-grade diatomite |
| CN111807392A (en) * | 2020-06-28 | 2020-10-23 | 山东泰星新材料股份有限公司 | Preparation method of submicron-grade superfine aluminum hydroxide, product and application thereof |
| CN112639026A (en) * | 2018-08-29 | 2021-04-09 | 日东电工株式会社 | Method for producing structure containing ionic liquid, and structure containing ionic liquid |
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| RU2740995C1 (en) * | 2020-05-22 | 2021-01-22 | Федеральное государственное бюджетное образовательное учреждение высшего образования «Национальный исследовательский Мордовский государственный университет им. Н.П. Огарёва» | Method of producing microsilica from natural diatomite by precipitation of nitric acid solution |
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2002
- 2002-12-18 CN CN 02156764 patent/CN1212267C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913595A (en) * | 2010-08-04 | 2010-12-15 | 中国科学院广州地球化学研究所 | Method for preparing porous carbon and white carbon black by using diatomite |
| CN101985357A (en) * | 2010-10-13 | 2011-03-16 | 蒋珂 | Preparation method of white carbon black |
| CN101985357B (en) * | 2010-10-13 | 2013-01-02 | 常州福思特医药化工研究所有限公司 | Preparation method of white carbon black |
| CN101962188A (en) * | 2010-11-15 | 2011-02-02 | 西藏大为建筑环保工程有限责任公司 | Method for preparing ultrafine high-purity SiO2 from volcanic ash |
| CN102491351A (en) * | 2011-12-13 | 2012-06-13 | 沈阳化工大学 | Method for preparing white carbon black through natural clinoptilolite |
| CN103193236A (en) * | 2013-03-05 | 2013-07-10 | 浙江工业大学 | Method of preparing silica by using diatomite |
| CN104192851A (en) * | 2014-08-28 | 2014-12-10 | 确成硅化学股份有限公司 | Method for preparing nano silicon dioxide |
| CN104556073A (en) * | 2015-01-16 | 2015-04-29 | 陈旭 | Process for purifying inorganic nonmetallic minerals |
| CN107324350A (en) * | 2017-08-22 | 2017-11-07 | 北京依依星科技有限公司 | A kind of method for preparing nanoprecipitation silica using low-grade diatomite |
| CN107324350B (en) * | 2017-08-22 | 2020-03-13 | 北京依依星科技有限公司 | Method for preparing nano precipitated silica by using low-grade diatomite |
| CN112639026A (en) * | 2018-08-29 | 2021-04-09 | 日东电工株式会社 | Method for producing structure containing ionic liquid, and structure containing ionic liquid |
| CN112639026B (en) * | 2018-08-29 | 2023-11-10 | 日东电工株式会社 | Method for producing structure containing ionic liquid, and structure containing ionic liquid |
| CN111807392A (en) * | 2020-06-28 | 2020-10-23 | 山东泰星新材料股份有限公司 | Preparation method of submicron-grade superfine aluminum hydroxide, product and application thereof |
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| Publication number | Publication date |
|---|---|
| CN1212267C (en) | 2005-07-27 |
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