CN1422805A - High-dispersion nano silicon dioxide preparation method - Google Patents
High-dispersion nano silicon dioxide preparation method Download PDFInfo
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- CN1422805A CN1422805A CN 02149782 CN02149782A CN1422805A CN 1422805 A CN1422805 A CN 1422805A CN 02149782 CN02149782 CN 02149782 CN 02149782 A CN02149782 A CN 02149782A CN 1422805 A CN1422805 A CN 1422805A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 28
- 239000006185 dispersion Substances 0.000 title claims description 10
- 239000005543 nano-size silicon particle Substances 0.000 title claims description 8
- 238000002360 preparation method Methods 0.000 title claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 52
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 239000007789 gas Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000000926 separation method Methods 0.000 claims abstract description 26
- 230000008569 process Effects 0.000 claims abstract description 17
- 230000001681 protective effect Effects 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 7
- 150000002367 halogens Chemical class 0.000 claims abstract description 7
- 229910000077 silane Inorganic materials 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 5
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 4
- 238000006482 condensation reaction Methods 0.000 claims abstract description 4
- 239000011261 inert gas Substances 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims description 19
- 238000002485 combustion reaction Methods 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000000428 dust Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 238000004220 aggregation Methods 0.000 claims description 3
- 230000002776 aggregation Effects 0.000 claims description 3
- 239000003570 air Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000009461 vacuum packaging Methods 0.000 claims description 3
- 239000002737 fuel gas Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 229910004721 HSiCl3 Inorganic materials 0.000 claims 1
- 229910003910 SiCl4 Inorganic materials 0.000 claims 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims 1
- 229910052794 bromium Inorganic materials 0.000 claims 1
- 238000001354 calcination Methods 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims 1
- 229910052731 fluorine Inorganic materials 0.000 claims 1
- 239000011737 fluorine Substances 0.000 claims 1
- 125000001153 fluoro group Chemical group F* 0.000 claims 1
- 125000005843 halogen group Chemical group 0.000 claims 1
- 229910052740 iodine Inorganic materials 0.000 claims 1
- 239000011630 iodine Substances 0.000 claims 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical group Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims 1
- 239000011164 primary particle Substances 0.000 abstract description 6
- 229910052681 coesite Inorganic materials 0.000 abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract 2
- 229910052682 stishovite Inorganic materials 0.000 abstract 2
- 229910052905 tridymite Inorganic materials 0.000 abstract 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- 229910021485 fumed silica Inorganic materials 0.000 description 6
- 239000005055 methyl trichlorosilane Substances 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- 239000004965 Silica aerogel Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- -1 coatings Substances 0.000 description 3
- 230000008719 thickening Effects 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- 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 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910000039 hydrogen halide Inorganic materials 0.000 description 1
- 239000012433 hydrogen halide Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Abstract
The invention discloses a method to prepare high-disperse nano SiO2, imputting O2-H2 organic halogen silane in a certain proportion into reaction room to make burning reaction, at the same time inputting a protective gas, vapor and inert gases, adopting the produced water and heat to make high-temperature hydrolytic condensation reaction and making the late process such as aggregative gas-solid separation deacidification on the reaction product to obtain it, primary particle dimaeter 7-40 nm, ratio surface area 100-400 m2/g, pH value 3.8-4.5, SiO2 receiving rate >99%.
Description
Technical Field
The invention relates to a preparation method of high-dispersion nano silicon dioxide.
Background
The high-dispersion nano-silica is widely applied to the fields of rubber, plastics, coatings, paint and ink, adhesives, cosmetics, medicines, agriculture and the like due to the unique physical and chemical properties of the high-dispersion nano-silica, and has the effects of reinforcement, thickening, thixotropy, extinction, sedimentation prevention, sagging resistance, aging prevention and the like. The existing methods for preparing high-dispersion nano-silica can be divided into two methods, one method is a wet method, a silicate solution (such as sodium silicate) is hydrolyzed under acidic or alkaline conditions, then silica is obtained through a series of post-treatment processes, and is also called precipitated silica, the other method is a dry method, silicon dioxide aerogel is prepared through flame high-temperature hydrolysis by adopting organic silicon halides (such as silicon tetrachloride, methyl trichlorosilane and the like), then silica is obtained through post-treatment processes of aggregation, separation, deacidification and the like, and is also called fumed silica or fumed silica, the performances of the silica prepared by the two methods are different to a certain extent, the wet-method silica has low purity, high ionic impurity content, larger grain diameter ratio of the product, low particle structure, and easy formation of large non-redispersible hard aggregate, whichcauses loss of the characteristics of nano-materials, therefore, the reinforcing property, thickening property and thixotropy of the wet-process silicon dioxide are not as good as those of the dry-process silicon dioxide, the purity of the dry-process silicon dioxide product is high (the content of the silicon dioxide is more than 99.8 percent), the primary particle size of the product is 7-40 nanometers, and the specific surface area is 100-400 m2Has excellent reinforcing property, thickening property and thixotropic property.
The process for producing fumed silica was originally developed by Degussa corporation of germany in 1941, but only a few countries such as germany, usa, japan, ukraine, and china, etc. in the world currently hold industrial production techniques of fumed silica, and the conventional process for producing fumed silica is basically similar in that vaporized halosilane is mixed with hydrogen and oxygen, then burned in a combustion chamber (reaction chamber) to produce silica aerogel, which is then aggregated by a collector, and solid products are separated from reaction exhaust gas and unreacted gas by gas-solid separation (e.g., gravity settling, cyclone separation, centrifugal separator separation, impact separator separation), and hydrogen halide gas adsorbed on the surface of silica is removed by a deacidification process to obtain a finished product, as described in us patents 418964, 3954945 and 4048290 and chinese patent CN 1043633C, etc. however, in the conventional process, the fumed silica particles are easy to deposit on the wall of the reaction chamber, and the size of the reaction chamber is reduced by the deposited silica particles with the time, so that the geometric size and the shape of the reaction flame are influenced, the uniformity and the quality of a product are finally influenced, and sometimes the mechanical cleaning of the reaction chamber is required to be stopped in the production process, so thatthe production continuity is influenced.
Disclosure of Invention
The invention aims to provide a preparation method of high-dispersion nano silicon dioxide, which can effectively improve the continuity of production, the stability of products and the yield of the products.
The invention provides a preparation method of high-dispersion nano silicon dioxide, which comprises the steps of continuously conveying oxygen, hydrogen and organic halogen silane into a combustion nozzle according to the proportion (standard volume) of 1: 1.2-2: 0.3-1 for combustion reaction in a reaction chamber, simultaneously conveying protective gas into the reaction chamber, carrying out high-temperature hydrolysis condensation reaction on the halogen silane at 1000-1700 ℃ by using water generated by combustion and heat generated by combustion, carrying out post-treatment processes of aggregation gas-solid separation, deacidification and the like on reaction products, and finally carrying out vacuum packaging on the reaction products to obtain the finished products.
The reaction mechanism of the present invention is as follows:
(1)
(2)
the nano silicon dioxide prepared by the method has the primary particle size of 7-40 nm and the specific surface area of 100-400 m2The burning nozzle and the reaction chamber prevent the deposition of nano silicon dioxide on the wall of the reaction chamber in the production process, improve the production continuity and the product stabilityThe pH value of the silica gel is 3.8-4.5, a closed system is formed in the whole production process, no dust pollution is caused, and the yield of the silica is more than 99%.
The invention is further described with reference to the following drawings and detailed description.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a schematic view of the structure of a combustion furnace and a reaction chamber in the present invention.
Detailed Description
FIG. 1 is a process flow diagram of the present invention, in which premixed and uniformly mixed halosilane, hydrogen and oxygen continuously enter a combustion nozzle 1, a combustion reaction is performed in a reaction chamber 3, halosilane performs a high-temperature hydrolysis condensation reaction by using water generated by combustion and heat generated to generate silica aerogel with a particle size of 7-40 nm, the silica aerogel enters a collector 4, silica aggregates with a particle size of 0.5-1.5 μm are formed after the silica aerogel is collected, the silica aggregates and reaction waste gas enter a cyclone separator 5 together to separate the silica aggregates from the reaction waste gas, the silica flows downward and enters a deacidification furnace 6, the reaction waste gas and a part of the silica flow upward and enter a next-stage cyclone separator to perform a second-stage separation, tail gas from the second-stage separation enters a third-stage separation, and silica obtained from the second-stage separation and the third-stage separation returns to the first, the tail gas of tertiary separation gets into dust collecting equipment 8, and the silica that dust collecting equipment filtered out returns the deacidification stove, and tail gas gets into tail gas processing apparatus, can guarantee like this that separation efficiency is greater than 99%.
A lot of HCl gas is also adsorbed in the separated silicon dioxide, so that the pH value of the product is too low, the application of the product is limited, and the HCl adsorbed on the surface of the silicon dioxide is removed through deacidification treatment, as shown in figure 1, the separated silicon dioxide enters a deacidification furnace from the lower part, meanwhile, water vapor, preferably mixed gas of water vapor and nitrogen is introduced from the bottom of the deacidification furnace, a heater 7 is arranged at an inlet of the deacidification furnace for heating the water vapor, and the temperature of the water vapor before entering the deacidification furnace is 150-250 ℃, preferably 200-220 ℃. Heating in a deacidification furnace by heating pipes which are arranged in a staggered way to ensure that the temperature in the furnace is between 450 and 750 ℃, preferably between 550 and 650 ℃, the silica is calcined at high temperature to desorb HCl from the surface of the silica, and the water vapor promotes the desorption of HCl through hydrogen bond interaction with HCl, an outlet is arranged at the upper end of the deacidification furnace, the silicon dioxide after HCl removal is discharged from the outlet and enters a storage tank 9, the tail gas returns to the dust removal device 8 for filtration, the filtered silicon dioxide returns to the deacidification furnace for deacidification recovery, thus ensuring that the yield of the product is more than 99 percent, dust removing equipment can be not used in the implementation process, because the cyclone efficiency can reach 99 percent through three-stage separation as long as the cyclone separation parameters are well controlled, and the tail gas from the deacidification furnace returns to the primary cyclone separator, so that the yield of the product can be completely ensured to reach more than 99 percent.
Silica products in tanks are difficult to package ideally with conventional packaging methods due to the very low apparent density. The invention adopts a vacuum packaging machine, the valve port packaging bag is vacuumized, the silicon dioxide is sucked into the packaging bag by utilizing pressure difference and is compressed, the packaging of the silicon dioxide without dust pollution is realized, and the packaging weight is 10 +/-0.1 Kg per bag.
FIG. 2 is a schematic view of a furnace and a reaction chamber of the present invention. The reaction mixture gas enters the reaction chamber 3 from the combustion nozzle 1, a jacket 2 is arranged on the nozzle, the position of the jacket can be adjusted up and down, so that the reaction gas is convenient to ignite and clean the reaction chamber, the jacket is adjusted to be the lowest in the reaction process, the nozzle and the reaction chamber 3 form a closed whole, and the influence of air entering the reaction chamber from the inlet 13 of the reaction chamber on the stability of the reaction is avoided. At the upper end of the reaction chamber, a protective gas inlet 14 is connected with protective gas, a protective gas outlet 10 is a tapered slit, so that the protective gas can enter the reaction chamber at an inclined angle, the protective gas 11 flows along the inner wall of the reaction chamber and surrounds the reaction flame 12, the contact between silicon dioxide particles generated by reaction and the inner wall of the reaction chamber is reduced, the silicon dioxide is prevented from being deposited on the upper surface, the silicon dioxide is deposited on the inner wall of the reaction chamber, the production is very harmful, the unobstructed performance of the system is very important for the whole production process, if the silicon dioxide is deposited on the inner wall of the reaction chamber and accumulated to a certain degree, the geometric shape of the reaction chamber can be changed, the shape and the stability of the reaction flame are changed, the quality of products is influenced, the unobstructed performance of the system is influenced when the deposition is serious, and equipment is blocked, so that the production is. The protective gas used in the present invention may be fuel gas, air, oxygen, hydrogen, inert gas, etc., and preferably a combustible mixed gas, so that sufficient heat can be provided for the reaction, and the product quality is not uneven due to uneven heat.
Example 1
The methyltrichlorosilane is added at a ratio of 7.5m3H, hydrogen gas at 8m3H, air 85m3The supply of the amount/h is continuously conveyed into a premixer for premixing (the volume is a standard volume), the premixed silica enters a nozzle of a combustion furnace after being preheated to 120 ℃, the specific process is shown in figure 1, the protective gas is air, the temperature in a deacidification furnace is 550 ℃, the temperature of water vapor and nitrogen is 200 ℃, and the quality indexes of the prepared silica are as follows: silica content (%) 99.80 Primary particle average particle diameter (nm) 20 specific surface area (m)2/g) 153pH 3.95 carbon content (%) 0.01
Example 2
The methyltrichlorosilane of example 1 was replaced by silicon tetrachloride, which was 7m3H, hydrogen at 8.5m3H, air at 72m3The supply amount of the catalyst/h is supplied, other process parameters are the same as those of the example 1, and the quality indexes of the prepared silicon dioxide are as follows: silica content (%) 99.85 Primary particle average particle diameter (nm) 16 specific surface area (m)2/g) 197pH value4.05 carbon content (%) not measured
Example 3
The methyltrichlorosilane of example 1 was substituted with 60% methyltrichlorosilane and 40% silicon tetrachlorideInstead, the supply amount is 10m3H, hydrogen 12m3H, air 96m3The other process parameters are the same as in example 1, and the quality indexes of the prepared silicon dioxide are as follows: silica content (%) 99.82 Primary particle average particle diameter (nm) 15 specific surface area (m)2/g) 208pH 4.03 carbon content (%) 0.01
The above examples are merely illustrative of the present invention and the scope of the present invention is not limited thereto. In addition, the method of the invention can be used to prepare other nano-metal oxides such as TiO with high dispersion by using hydrolyzable volatile metal halide as raw material2，ZrO2，Al2O3And the like.
Claims (9)
1. A preparation method of high-dispersion nano silicon dioxide is characterized by comprising the following steps: continuously conveying oxygen, hydrogen and organic halogen silane into a combustion nozzle according to the proportion (standard volume) of 1: 1.2-2: 0.3-1 for combustion reaction in a reaction chamber, simultaneously conveying a protective gas into the reaction chamber, carrying out high-temperature hydrolysis condensation reaction on the halogen silane at 1000-1700 ℃ by using water generated by combustion and generated heat, carrying out post-treatment processes of aggregation, gas-solid separation, deacidification and the like on reaction products, and finally carrying out vacuum packaging to obtain the finished product.
2. The method for preparing highly dispersed nano-silica according to claim 1, characterized in that: the halogen atom in the organic halogen silane is fluorine, chlorine, bromine or iodine.
3. Highly dispersed nanosilica as claimed in claim 2The preparation method is characterized by comprising the following steps: the organic halogen silane is SiCl4，CH3SiCl3，(CH3)2SiCl2，(CH3)3SiCl，HSiCl3Or a mixture thereof.
4. The method for preparing highly dispersed nano-silica according to claim 1, characterized in that: the oxygen can be pure oxygen, a mixed gas of oxygen and other inert gases or air.
5. The method for preparing highly dispersed nano-silica according to claim 1, characterized in that: the protective gas is one or a mixture of fuel gas, air, oxygen, hydrogen and inert gas.
6. The method for preparing highly dispersed nano-silica according to claim 1, characterized in that: the combustion nozzle is positioned at the upper end of the inlet of the reaction chamber, and a jacket capable of adjusting the position of the combustion nozzle up and down is arranged on the combustion nozzle; the upper end of the reaction chamber is provided with a protective gas inlet, the protective gas outlet is a tapered slit, and the protective gas enters the reaction chamber from the protective gas inlet at an inclined angle.
7. The method for preparing highly dispersed nano-silica according to claim 1, characterized in that: the gas-solid separation treatment process adopts three cyclone separators for separation, products subjected to primary separation directly enter a deacidification furnace, tail gas enters secondary separation, tail gas generated by the secondary separation enters tertiary separation, products subjected to the secondary and tertiary separation return to the primary separation, and tail gas subjected to the tertiary separation enters dust removal equipment.
8. The method for preparing highly dispersed nano-silica according to claim 1, characterized in that: the deacidification treatment process comprises the steps of calcining and deacidifying in a deacidification furnace, heating in the deacidification furnace through heating pipes arranged in a crossed mode, keeping the temperature in the deacidification furnace at 450-750 ℃, meanwhile, introducing auxiliary gas into the deacidification furnace, and heating the auxiliary gas by a heater at an inlet of the auxiliary gas entering the deacidification furnace, wherein the heater is used for heating the auxiliary gas to enable the temperature of the auxiliary gas to be 150-250 ℃.
9. The method for preparing highly dispersed nano-silica according to claim 8, characterized in that: the auxiliary gas is water vapor and nitrogen.
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| CN 02149782 CN1222472C (en) | 2002-12-30 | 2002-12-30 | High-dispersion nano silicon dioxide preparation method |
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| CN 02149782 CN1222472C (en) | 2002-12-30 | 2002-12-30 | High-dispersion nano silicon dioxide preparation method |
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| WO2012075669A1 (en) * | 2010-12-10 | 2012-06-14 | 中国科学院过程工程研究所 | Process for synthesizing hydrophobic silicon dioxide nanoparticles by combustion |
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| CN103466636A (en) * | 2013-08-27 | 2013-12-25 | 浙江合盛硅业有限公司 | System for producing fumed silica with methyl trichlorosilane |
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2002
- 2002-12-30 CN CN 02149782 patent/CN1222472C/en not_active Expired - Lifetime
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