CN1546373A - Process for preparing size-controllable nano-silicon dioxide - Google Patents
Process for preparing size-controllable nano-silicon dioxide Download PDFInfo
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- CN1546373A CN1546373A CNA2003101125824A CN200310112582A CN1546373A CN 1546373 A CN1546373 A CN 1546373A CN A2003101125824 A CNA2003101125824 A CN A2003101125824A CN 200310112582 A CN200310112582 A CN 200310112582A CN 1546373 A CN1546373 A CN 1546373A
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Abstract
The invention provides a process for preparing dimension controllable nano silicon dioxide comprising continuously conveying organic halogensilane, hydrogen, and oxygen by a finite proportion into combustion nozzle then firing chamber, conducting hydrolytic reaction in 1000 deg. C to 2000deg. C flame, subjecting the reaction product to congregation, cyclone air-solid segregation and deacidification post-treatment, and vacuum-packing.
Description
Technical Field
The utility model relates to a preparation method of silicon dioxide.
Background
The nano silicon dioxide is widely applied to the fields of rubber, plastics, coatings, paint ink, adhesives, cosmetics, medicines, agriculture and the like due to the unique physical and chemical properties of the nano silicon dioxide, and has the functions of reinforcement, thickening, thixotropy, extinction, sedimentation prevention, sagging resistance, aging prevention and the like. At present, the method for preparing nano silicon dioxide can be divided into two methods, one method is a wet method, silicate solution (such as sodium silicate) is adopted for hydrolysis under the acidic or alkaline condition, and then silicon dioxide, also called precipitated silica, is obtained through a series of post-treatment processes. The other method is a dry method, which is to prepare silica aerogel by flame high-temperature hydrolysis of organic silicon halides (such as silicon tetrachloride, methyltrichlorosilane and the like), and then obtain silica by post-treatment processes such as aggregation, separation, deacidification and the like, and the silica is also called fumed silica or fumed silica. The performance of the silicon dioxide prepared by the two methods is different to a certain extent, the wet-method silicon dioxide product has low purity and high content of ionic impurities, the particle diameter ratio of the product is larger, the particle structure is low, and large non-redispersible hard aggregate is easy to form, so that the characteristics of the nano material are lost, and the reinforcing property, thickening property and thixotropy of the wet-method silicon dioxide are not as good as those of the dry-method silicon dioxide. The dry-method silicon dioxide product has high purity (the silicon dioxide content is more than 99.8 percent), the primary particle size of the product is between 7 and 40 nanometers, and the specific surface area is 100-2Has excellent reinforcing property, thickening property and thixotropic property.
Fumed silica was originally developed by Degussa corporation of germany in 1941, but currently only a few countries of germany, the united states, japan, ukraine, and china have mastered the commercial production technology of fumed silica in the world. The conventional production process of fumed silica is basically similar, and comprises the steps of mixing vaporized halosilane with hydrogen and oxygen, then burning in a combustion chamber (reaction chamber) to prepare silica aerogel, then gathering by a gathering device, separating solid products from reaction waste gas and unreacted gas by gas-solid separation (such as gravity settling, cyclone separation, centrifugal separator separation and impact separator separation), and then removing hydrogen halide gas adsorbed on the surface of silica by a deacidification process to obtain a finished product. Specific methods can be found in us patent 4108964, 3954945, 4048290, chinese patent CN1043633C, etc.
In the process for producing fumed silica, cooling of the combustion chamber is a critical process because the reaction temperature is substantially 1700 ℃ or higher (above the melting point of silica) during the production of silica, and it is necessary to lower the temperature in the reaction chamber to 800 ℃ or lower immediately after the reaction, otherwise the produced silica particles are liable to collide with each other and fuse into large particles, and if the cooling rate is too slow, crystalline silica is liable to be produced, which affects the properties of the product. The traditional method adopts air cooling, has poor cooling effect, and the temperature in the reaction chamber is not easy to control, so the primary particle size of the silicon dioxide is difficult to effectively control, the particle size distribution is wider, and the yield of the fumed silica is lower.
Disclosure of Invention
The invention aims to provide a preparation method of size-controllable nano silicon dioxide, which can effectively control the primary particle size of silicon dioxide particles, improve the yield and save a large amount of energy.
The invention provides a preparation method of size-controllable nano silicon dioxide, which comprises the steps of continuously conveying organohalosilane, hydrogen and oxygen to a combustion nozzle according to the standard volume ratio of 1: 1.1-3: 1-8, then feeding the mixture into a combustion chamber, carrying out hydrolysis reaction in flame at the temperature of 1000-2000 ℃, cooling the space between the combustion nozzle and the combustion chamber in an open manner, cooling the combustion chamber in a jacket water-filling cooling method, carrying out aggregation, cyclone gas-solid separation and deacidification post-treatment on reaction products, and finally carrying out vacuum packaging on the reaction products to obtain finished products.
In the above scheme, the halogen atom in the organohalosilane is fluorine, chlorine, bromine or iodine, preferably chlorine such as SiCl4，CH3SiCl3，(CH3)2SiCl2，(CH3)3SiCl，HSiCl3And mixtures thereof; the oxygen is pure oxygen, mixed gas of oxygen and inert gas or air; the flame temperature is preferably 1200-1700 ℃; the cyclone gas-solid separation process adopts three cyclone separators for separation, products subjectedto primary separation directly enter a primary 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 a tail gas treatment system; the deacidification process adopts a sectional deacidification method, the temperature in the deacidification furnace is kept at 450-750 ℃, auxiliary gas is introduced into the deacidification furnace, the product subjected to primary deacidification is conveyed to a secondary deacidification furnace for secondary deacidification, and tail gas subjected to secondary deacidification enters a tail gas treatment system.
The reaction mechanism of the present invention is as follows:
(1)
(2)
the particle size of the silicon dioxide product is controlled by controlling the proportion between halosilane and combustion gas and adopting an effective cooling method, wherein the proportion of organohalosilane, hydrogen and oxygen is 1: 1.1-3: 1-8; the combustion nozzle and the combustion chamber are in an open mode, outside air can enter the combustion chamber through negative pressure in the combustion chamber to play a cooling role, meanwhile, a combustion chamber jacket adopts a water cooling method to replace the traditional air cooling, the cooling efficiency is improved, the temperature of the combustion chamber can be instantly reduced to be below 800 ℃ from 1700 ℃ above, the particle size of primary particles can be effectively prevented from being increased due to mutual collision and sintering of the silicon dioxide particles at high temperature, the primary particle size of the silicon dioxide particles can be controlled to be below 40 nanometers, and the particle size distribution is narrow. The invention adopts a three-stage cyclone separation method to separate the silicon dioxide particles from the combustion waste gas, which can ensure that the yield of the silicon dioxide is more than 99 percent, and the application of the product is seriously influenced because the surface of the silicon dioxide after the combustion waste gas is separated also adsorbs hydrogen chloride without deacidification treatment, and the invention adopts a two-stage deacidification process, which can ensure that the pH of the product is more than 3.8.
The primary particle size of the nano silicon dioxide prepared by the method is 7-40 nm, and the specific surface area is 100-400m2Between/g. Compared with the traditional production process of fumed silica, the method can effectively control the primary particle size of the silica particles, improve the yield and save a large amount of energy.
The invention will be further explained with reference to the drawings.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a schematic view of the structure of the combustion nozzle and combustion chamber of the present invention.
Detailed Description
As shown in fig. 1, premixed and uniformly mixed halosilane, hydrogen and oxygen continuously enter a combustion nozzle 1, and undergo a combustion reaction in a reaction chamber 3, and the halosilane undergoes a high-temperature hydrolysis condensation reaction by using water generated by combustion and generated heat, thereby generating silica aerogel with a particle size of 7-40 nm. The silicon dioxide aerogel enters the collector 4 and forms a silicon dioxide aggregate with the diameter of about 1 micron after being collected. Then the silicon dioxide aggregate and the reaction waste gas enter a cyclone separator 5 together, the silicon dioxide aggregate and the reaction waste gas are separated, the silicon dioxide flows downwards and enters a deacidification furnace 6, the reaction waste gas and part of the silicon dioxide flow upwards and enter a next-stage cyclone separator for secondary separation, the tail gas of the secondary separation enters a third-stage separation, the silicon dioxide obtained by the second-stage separation and the third-stage separation returns to the first-stage separation, and the tail gas of the third-stage separation enters a tail gas treatment system, so that the yield of the silicon dioxide is more than 99 percent.
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 HCl adsorbed on the surface of the silicon dioxide must be removed through deacidification treatment. The invention adopts a two-stage deacidification method, as shown in figure 1, the silicon dioxide separated from a primary cyclone separator 5 directly enters a primary deacidification furnace 6, and simultaneously deacidification auxiliary gas is introduced from the bottom of the deacidification furnace, wherein the auxiliary gas can be nitrogen or mixed gas of nitrogen and water vapor. At the entrance that auxiliary gas got into the deacidification stove, there is a heater 7 to auxiliary gas heating, and the temperature before guaranteeing auxiliary gas to get into the deacidification stove is between 150 ~ 250 ℃, preferredly 200 ~ 220 ℃. In the deacidification furnace, heating is carried out through heating pipes which are arranged in a staggeredmode, so that the temperature in the deacidification furnace is guaranteed to be 450-750 ℃, and 550-650 ℃ is preferred. By calcining the silica at high temperature, HCl is desorbed from the silica surface and carried away by the assist gas. An outlet is arranged at the upper end of the deacidification furnace, silicon dioxide after primary deacidification is discharged from the outlet and enters a secondary deacidification furnace 8 for secondary deacidification, tail gas returns to the primary cyclone separator 5, the silicon dioxide discharged from the secondary deacidification furnace enters a storage tank 10, the tail gas enters a tail gas treatment system, and after secondary deacidification, the pH value of 4% aqueous suspension of a product is more than 3.8, so that the use requirements of most fields can be met.
The silica product in the storage tank has very small apparent density (20-60 g/L), so that the silica product is difficult to be ideally packaged by using a traditional packaging method. 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.
The technical scheme for controlling the primary particle size of the product comprises the following steps: the primary particle size of the silica can be controlled by controlling the ratio between raw materials and the amount of raw material supply, while controlling the temperature in the combustion chamber. If a product with high specific surface area and small particle size needs to be produced, the supply amount of the organohalosilane can be reduced, the amount of air is increased, the cooling effect is improved, the probability of mutual collision among primary particles generated by reaction is reduced, and the purpose of controlling the particle size is achieved.
The cooling of the combustion chamber is realized by adopting an open mode between the combustion nozzle 1 and the combustion chamber 3, so that outside air can enter the reaction chamber from the combustion chamber opening 2 through negative pressure in the combustion chamber to play a role of cooling, the cooling mode of a combustion chamber jacket adopts water cooling to replace the traditional air cooling, cooling water enters from inlets 11 and 13 and flows out from outlets 12 and 14, and the cooling water is cooled and then returns for recycling, the method improves the cooling efficiency, can instantly reduce the temperature in the reaction chamber from more than 1400 ℃ to less than 800 ℃, can effectively control the particle size and the particle size distribution of products, and can also improve the yield of the device.
Example 1
The methyltrichlorosilane is added at a ratio of 7.5m3H, hydrogen gas at 12m3H, air at 105m3The supply amount/h is continuously fed into premixer for premixing (the volume is standard volume), preheated to 120 deg.C, and fed into combustion furnace nozzle, and the specific process is shown in figure 1, the temperature in reaction chamber is 720 deg.C, the temperature in primary deacidification furnace is 600 deg.C, the temperature in secondary deacidification furnace is 550 deg.C, and deacidification auxiliary gas is water vapor and nitrogen gas, and its temperature is 230 deg.CThe quality indexes of the prepared silicon dioxide are as follows:
silica content (%) (hydrofluoric acid process) 99.85
Average particle diameter (nm) of primary particles (Electron microscopy) 30
Specific surface area (m)2/g) (BET method) 153
pH (4% aqueous suspension) 3.95
Carbon content (%) 0.01
Example 2
The methyltrichlorosilane of example 1 was replaced by silicon tetrachloride, which was 7m3H, hydrogen gas at 15m3H, air at 130m3The supply amount and the process are the same as those in example 1, the temperature in the reaction chamber is 640 ℃, and other steps are the same as those in example 1, and the quality indexes of the prepared silicon dioxide are as follows:
silica content (%) (hydrofluoric acid process) 99.85
Average particle diameter (nm) of primary particles (Electron microscopy) 12
Specific surface area (m)2/g) (BET method) 283
pH (4% aqueous suspension) 4.05
Carbon content (%) not measured
Example 3
The methyltrichlorosilane from example 1 was replaced by 60% methyltrichlorosilane and 40% silicon tetrachloride and was supplied in an amount of 8.5m3H, hydrogen is 16m3H, air 125m3The temperature in the reaction chamber is 690 ℃, other process parameters are the same as those in example 1, and the quality indexes of the prepared silicon dioxide are as follows:
silica content (%) (hydrofluoric acid process) 99.82
Average particle diameter (nm) of primary particles (Electron microscopy) 15
Specific surface area (m)2/g) (BET method) 208
pH (4% aqueous suspension) 4.23
Carbon content (%) 0.01
Claims (9)
1. A preparation method of nano silicon dioxide with controllable size is characterized by comprising the following steps: continuously conveying organohalosilane, hydrogen and oxygen to a combustion nozzle according to the standard volume ratio of 1: 1.1-3: 1-8, then feeding the mixture into a combustion chamber, carrying out hydrolysis reaction in flame at the temperature of 1000-2000 ℃, wherein the space between the combustion nozzle and the combustion chamber is cooled in an open mode, the combustion chamber adopts a jacket water-filling cooling method, reaction products are subjected to processes of aggregation, cyclone gas-solid separation and deacidification post-treatment, and finally vacuum packaging is carried out to obtain the finished product.
2. The method of claim 1, wherein: the halogen atom in the organic halogen silane is fluorine, chlorine, bromine or iodine.
3. The method of claim 2, wherein: the organic halogen silane is SiCl4，CH3SiCl3，(CH3)2SiCl2，(CH3)3SiCl，HSiCl3Or a mixture thereof.
4. The method of claim 1, wherein: the oxygen is pure oxygen, mixed gas of oxygen and inert gas or air.
5. The method of claim 1, wherein: the flame temperature is 1200-1700 ℃.
6. The method of claim 1, wherein: the cyclone gas-solid separation process adopts three cyclone separators for separation, products subjected to primary separation directly enter a primary 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 a tail gas treatment system.
7. The method of claim 1, wherein: the deacidification process adopts a sectional deacidification method, the temperature in the deacidification furnace is kept at 450-750 ℃, auxiliary gas is introduced into the deacidification furnace, the product subjected to primary deacidification is conveyed to a secondary deacidification furnace for secondary deacidification, and tail gas subjected to secondary deacidification enters a tail gas treatment system.
8. The method of claim 7, wherein: the temperature in the deacidification furnace is kept at 550-650 ℃.
9. The method of claim 7, wherein: the auxiliary gas is nitrogen or a mixed gas of nitrogen and water vapor.
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Cited By (12)
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| CN100369811C (en) * | 2006-04-29 | 2008-02-20 | 广州吉必时科技实业有限公司 | Comprehensive utilization method of by-product for poycrystalline silicon production process |
| CN101830469B (en) * | 2009-12-30 | 2011-12-14 | 邓兵国 | Adjustable super-high pressure pulse static silica micropowder purifying machine |
| 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 |
| WO2013078802A1 (en) * | 2011-11-30 | 2013-06-06 | 广州吉必盛科技实业有限公司 | Deacidification process and apparatus thereof |
| CN103235359A (en) * | 2012-07-26 | 2013-08-07 | 上海拜安实业有限公司 | Single-mode fiber connector wire on basis of adhesive-free vitrification technology, related nanometer-sized silicon dioxide and manufacturing method |
| 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 |
| CN103626191A (en) * | 2013-12-20 | 2014-03-12 | 贵州万方铝化科技开发有限公司 | Preparation method of nano-scale silicon dioxide |
| CN107120641A (en) * | 2017-06-27 | 2017-09-01 | 哈尔滨工业大学 | A kind of three CFBBs that nano silicon is prepared for combusting rice hull |
| CN107777693A (en) * | 2017-11-14 | 2018-03-09 | 宜昌汇富硅材料有限公司 | The production technology and device of a kind of nano fumed silica |
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| CN100369811C (en) * | 2006-04-29 | 2008-02-20 | 广州吉必时科技实业有限公司 | Comprehensive utilization method of by-product for poycrystalline silicon production process |
| CN101830469B (en) * | 2009-12-30 | 2011-12-14 | 邓兵国 | Adjustable super-high pressure pulse static silica micropowder purifying machine |
| 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 |
| WO2013078802A1 (en) * | 2011-11-30 | 2013-06-06 | 广州吉必盛科技实业有限公司 | Deacidification process and apparatus thereof |
| US9273905B2 (en) | 2011-11-30 | 2016-03-01 | Guangzhou Gbs High-Tech & Industry Co., Ltd. | Deacidification process and apparatus thereof |
| CN103235359A (en) * | 2012-07-26 | 2013-08-07 | 上海拜安实业有限公司 | Single-mode fiber connector wire on basis of adhesive-free vitrification technology, related nanometer-sized silicon dioxide and manufacturing method |
| 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 |
| CN103466636B (en) * | 2013-08-27 | 2016-08-17 | 合盛硅业股份有限公司 | A kind of system utilizing methyl trichlorosilane to produce fume colloidal silica |
| CN104925817B (en) * | 2013-12-20 | 2018-03-20 | 贵州万方铝化科技开发有限公司 | The preparation method of nanometer grade silica |
| CN103626191A (en) * | 2013-12-20 | 2014-03-12 | 贵州万方铝化科技开发有限公司 | Preparation method of nano-scale silicon dioxide |
| CN104925817A (en) * | 2013-12-20 | 2015-09-23 | 贵州万方铝化科技开发有限公司 | Nanometer silica preparation method |
| CN107120641A (en) * | 2017-06-27 | 2017-09-01 | 哈尔滨工业大学 | A kind of three CFBBs that nano silicon is prepared for combusting rice hull |
| CN107120641B (en) * | 2017-06-27 | 2023-06-06 | 哈尔滨工大华实环保科技有限公司 | Three-circulation fluidized bed boiler for preparing nano silicon dioxide by rice hull combustion |
| CN107777693A (en) * | 2017-11-14 | 2018-03-09 | 宜昌汇富硅材料有限公司 | The production technology and device of a kind of nano fumed silica |
| CN107777693B (en) * | 2017-11-14 | 2021-01-22 | 湖北汇富纳米材料股份有限公司 | Production process and device of nano fumed silica |
| CN108394910A (en) * | 2018-05-15 | 2018-08-14 | 湖北兴瑞硅材料有限公司 | The method of gas-phase silica raw materials for production mixture |
| CN108394910B (en) * | 2018-05-15 | 2020-02-14 | 湖北兴瑞硅材料有限公司 | Method for mixing raw materials for producing fumed silica |
| CN111484023A (en) * | 2019-12-23 | 2020-08-04 | 浙江精功新材料技术有限公司 | Horizontal deacidification furnace for producing high-temperature steam based on hydrogen combustion method |
| CN111484023B (en) * | 2019-12-23 | 2022-10-11 | 浙江精功新材料技术有限公司 | Horizontal deacidification furnace for producing high-temperature steam based on hydrogen combustion method |
| CN113401912A (en) * | 2021-07-06 | 2021-09-17 | 苏州大学 | Device and method for regulating and controlling size of silica particles synthesized by flame method |
| WO2023279427A1 (en) * | 2021-07-06 | 2023-01-12 | 苏州大学 | Device and method for regulating and controlling size of silicon dioxide particles synthesized by flame process |
| CN113401912B (en) * | 2021-07-06 | 2023-03-07 | 苏州大学 | Device and method for regulating and controlling size of silica particles synthesized by flame method |
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