CN100506921C - Method for preparing hydrophobic type nano silicon dioxide thruogh continuous surface treatment - Google Patents

Method for preparing hydrophobic type nano silicon dioxide thruogh continuous surface treatment Download PDF

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CN100506921C
CN100506921C CNB2005100337764A CN200510033776A CN100506921C CN 100506921 C CN100506921 C CN 100506921C CN B2005100337764 A CNB2005100337764 A CN B2005100337764A CN 200510033776 A CN200510033776 A CN 200510033776A CN 100506921 C CN100506921 C CN 100506921C
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surface treatment
dioxide
nano silicon
silicon
gas
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CN1687246A (en
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王跃林
刘莉
龙成坤
徐宁
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Guangzhou Hui Fu Research Institute Co.,Ltd.
Hubei HuiFu nano materials Co., Ltd
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GUANGZHOU JIBISHI SCI-TECH INDUSTRY Co Ltd
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Abstract

The method for preparing hydrophobic type nano silicon dioxide by utilizing continuous surface treatment process includes the following steps: continuously feeding hydrophilic type nano silicon dioxide into surface treatment furnace and making it react with continuously-supplied silane surfactant treatment agent, controlling type of surface treatment agent, reaction material matching ratio, reaction temperature and reaction time so as to obtain hydrophobic type nano silicon dioxide whose hydrophobic rate is 10-99.99%.

Description

A kind of method by continuous surface Processing of Preparation hydrophobic nano silicon-dioxide
Technical field
The present invention relates to a kind of method for preparing hydrophobic nano silicon-dioxide.
Background technology
Nano silicon plays effects such as reinforcement, thickening, thixotroping, delustring, anti-settling, anti-sag and anti-aging owing to its unique physicochemical property are widely used in fields such as rubber, plastics, coating, paint, printing ink, tackiness agent, makeup, medicine, agricultural.Nano silicon adopts organosilicon halogenide (as silicon tetrachloride, METHYL TRICHLORO SILANE etc.) to make aerosil by the flame pyrohydrolysis, through aftertreatment technologys such as overbunching, separation and depicklings and obtain silicon-dioxide, be also referred to as thermal silica or aerosil then.The silica product purity height (dioxide-containing silica is greater than 99.8%) of this method gained, the primary particle diameter of product are between 7~40nm, and specific surface area is 100~400m 2/ g has excellent reinforcement, thickening and thixotropic property.But because product surface contains a large amount of silicon hydroxyls (Si-OH), form hydrogen bond easily and make product have wetting ability, influence the homodisperse of aerosil in organic polymer, can't satisfy the special requirement of some industry, greatly suppressed the Application Areas of product.For improving wetting property, dispersiveness, the interface bond strength between nano fumed silica particle and the organic molecule, improve the over-all properties of matrix material, widen the Application Areas of product, need product is carried out surface treatment, to remove the silicon hydroxyl of product surface.
The aerosil production technology is to be succeeded in developing in nineteen forty-one by German Degussa company the earliest, has only a few countries such as Germany, the U.S., Japan, Ukraine and China to grasp the suitability for industrialized production technology of aerosil in the world at present.Especially the continuous surface treatment technology of aerosil concentrates in the hand of Germany, the U.S. and major company of Japanese a few family especially, specifically can be referring to U.S. Pat 4503092 and US5458916.Ukraine and China all adopt surface treatment mode intermittently at present.Because of the equipment of this treatment process and simple to operate, control easily.Serialization produces that then process and equipment are complicated, operation control difficulty, but quality is relatively stable, the product that most importantly both can prepare different hydrophobic rate according to different technological processs, improve the production potential and the utilization ratio of device, also can directly be connected, realize online surface treatment with the aerosil production equipment.The development trend of aerosil process for treating surface is the serialization treatment process at present.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing hydrophobic nano silicon-dioxide, this method can effectively be controlled the hydrophobic rate of product and improve its dispersion effect and quality of stability, also can improve the production potential and the utilization ratio of device.
A kind of method provided by the invention by continuous surface Processing of Preparation hydrophobic nano silicon-dioxide, it is characterized in that hydrophilic nano-silicon dioxide is input into surface treatment stove and silicane surface treatment agent without interruption continuously in the surface treatment reaction in furnace, the mole proportioning of control reaction mass is a hydrophilic nano-silicon dioxide: silicane surface treatment agent=(2.5~20): (1~2), flow velocity is 2~20mm/s, it is 5~50min with the time that temperature is 200~500 ℃, make hydrophobic rate and be 10~99.99% hydrophobic nano silicon-dioxide, and remove the waste gas that is mingled with by Analytic Tower.
The nano silicon that adopts vapor phase process to produce, the surface has highly active silicon hydroxyl, and they mainly exist in three kinds of modes.The one, isolated free hydroxyl, with certain spacing " connection " on the particulate surface; The 2nd, association hydroxyl adhesion, that form hydrogen bond; The 3rd, twin hydroxyl, two hydroxyls are connected on the Siliciumatom.Surface treatment to fumed silica is exactly by certain technology and equipment, select the suitable surface treatment agent and the hydroxyl reaction of silica sphere, unify a little organic groups at silica sphere with chemical bonded refractory, make the aerosil surface have in various degree hydrophobicity.Generally can all can be used as surface treatment agent with the material of surface hydroxyl generation chemical reaction.The present invention mainly adopts organic halosilanes as (CH 3) 2SiCl 2(CH 3) 3SiCl, silazane are as (CH 3Si) 2NH and (CH 3Si) 2NC 2H 3, siloxanes such as D 4And D 3As surface treatment agent.
The present invention adopts the successive mode that hydrophilic nano-silicon dioxide is carried out surface treatment, silicon-dioxide is input in the processing stove by the controlled charging valve of speed of rotation continuously from the top of surface treatment stove, above the processing stove, be provided with an atomisation unit, below atomisation unit, be provided with a carrier gas inlet, carrier gas enters body of heater with tangential direction, makes to enter body of heater through the nano silicon after the atomisation unit effect with the vaporific spiral of gas phase.The bottom of handling stove is provided with the inlet of surface treatment agent and auxiliary agent, surface treatment agent and auxiliary agent upwards flow from handling furnace bottom, contact with the nano silicon of screw current downflow, react under the high temperature action in stove and realize that gas separates with solid, the surface treatment stove can adopt the method for infrared or microwave heating.
Also be provided with a material outlet in the bottom of handling stove, after coming out, material outlet enters an Analytic Tower through the nano silicon after the surface treatment, the bottom of Analytic Tower is provided with gas and steam-in, gas and steam upwards flow from the bottom, but the byproduct gas that produces in unreacted surface treatment agent of effective elimination and the reaction process is further carried out gas and is separated with solid.The temperature of Analytic Tower is controlled at 200~300 ℃, regulates Analytic Tower tail gas outlet valve and makes the pressure of surface treatment stove and Analytic Tower be lower than 10mmH 2O is to remove the waste gas that is mingled with.The nano silicon that process is resolved delivers into " wind cabinet " separator from the bottom of Analytic Tower by high-pressure air, product is separated, the product that does not meet size-grade distribution is separated, finally obtain the dewatering nano silica product of even particle size distribution.
Utilizing the present invention can prepare hydrophobic rate is 10~99.99% hydrophobic nano silicon-dioxide, to be applicable to different Application Areass, improves the quality of nano silicon.
The present invention is further illustrated below in conjunction with the drawings and the specific embodiments.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
As shown in Figure 1, the hydrophilic nano-silicon dioxide gas-solid mixture of coming by gas delivery from former feed bin, enter surface treatment stove 2 by rotation charging valve 1, under the effect of pressure reduction and weight, the solid silica powder enters in the body of heater, and the gas that has the part SiO 2 powder is back to the feed bin top through return line 10 once more, realizes material circulation conveying.Under the excessive prerequisite of the silicon-dioxide of pipe-line transportation,, can guarantee that powder measures to deliver into body of heater steadily, exactly by the pressure reduction between control carrier pipe and the surface treatment stove 2 and the rotating speed of rotation charging valve.
Enter the SiO 2 powder of surface treatment stove 2, at first enter and place the atomisation unit 3 of handling furnace roof portion.The powder film is under action of gravity, and the sedimentation of slowly floating downwards forms vaporific.Be provided with a carrier gas inlet 4 below atomisation unit 3, employed carrier gas can be rare gas element such as N 2Gas, carrier gas enters in the body of heater with tangential direction, and mist silicon-dioxide enters the shaft of surface treatment stove 2 in a spiral manner under the blowing of carrier gas, and the gas after separating transfers out with tail gas.
Enter the vaporific silicon-dioxide of shaft, continue to float in a spiral manner sedimentation downwards, under the high temperature action of electric heating, contact with surface treatment auxiliary agent 6 with the surface treatment agent mixing steam 5 that slowly upwards sprays from the bottom and to carry out surface chemical reaction, and finally realize gas solid separation.Reacted tail gas upwards enters the expanding reach of handling stove 2 and separates, and enter exhaust treatment system through offgas duct 9, and surface treated SiO 2 powder continues downward sedimentation.The carrier gas that enters through the bottom purges separation, and coarse particles is deposited on furnace bottom, and adjusting Analytic Tower 8 valves are controlled its pressure makes product be transported to Analytic Tower 8 through bypass 7.Bottom at pyritous desorption tower 8 feeds nitrogen, also can be aided with steam in case of necessity silicon-dioxide is purged, and further carries out gas solid separation, removes the small molecular by product in unreacted surface treatment agent and the reaction process.The gas that removes enters exhaust treatment system through offgas duct 9, and the silicon-dioxide after handling utilizes high-pressure air to be transported to " wind cabinet " separator 12 by the handling machinery 11 of bottom, can control the material level of Analytic Tower 8 by the air consumption of regulating handling machinery 11, so that smooth production process is carried out.Enter the gas-solid mixture of separator 12, because density variation, under the effect of gravity and air-flow, coarse particles is at first separated, and gas is directly transferred out, and product is promptly separated and the handling machinery 13 by the bottom transfers out smoothly like this.The coarse particles that is mingled with product is separated once more by the air that the bottom enters, and real coarse particles is sunken to the separator bottom, discharges by slag-drip opening 14.
In the above-mentioned technology, the mole proportioning of control reaction mass is a hydrophilic nano-silicon dioxide: silicane surface treatment agent=(2.5~20): (1~2), reaction flow velocity are that 2~20mm/s, temperature of reaction are that 200~500 ℃ and reaction times are 5~50min; The silicane surface treatment agent can adopt halosilanes, silazane or type siloxane surface treatment agent; The surface treatment stove can adopt infrared or microwave heating obtains the required high temperature of surface treatment reaction; The temperature of Analytic Tower is controlled at 200~300 ℃, regulates Analytic Tower tail gas outlet valve and makes the pressure of surface treatment stove and Analytic Tower be lower than 10mmH 2O is to remove the waste gas that is mingled with.
Now enumerate 3 embodiment by above-mentioned technology, the proportioning of various materials and have related parameter as shown in table 1, adopt hexamethyldisilazane (HMDS) and octamethylcyclotetrasiloxane (D4) respectively three kinds of nano silicons to be carried out surface treatment, obtained the hydrophobic type silicon-dioxide of three kinds of different hydrophobic rate for treatment agent.
Table 1
Figure C200510033776D00061

Claims (6)

1, a kind of method by continuous surface Processing of Preparation hydrophobic nano silicon-dioxide, it is characterized in that: hydrophilic nano-silicon dioxide is input into surface treatment stove and silicane surface treatment agent without interruption continuously in the surface treatment reaction in furnace, the mole proportioning of control reaction mass is a hydrophilic nano-silicon dioxide: silicane surface treatment agent=(2.5~20): (1~2), flow velocity is 2~20mm/s, it is 5~50min with the time that temperature is 200~500 ℃, make hydrophobic rate and be 10~99.99% hydrophobic nano silicon-dioxide, and remove the waste gas that is mingled with by Analytic Tower, the top of wherein said surface treatment stove is provided with an atomisation unit, below atomisation unit, be provided with a carrier gas inlet, carrier gas enters body of heater with tangential direction, hydrophilic nano-silicon dioxide carries out metered charge from the surface treatment furnace upper end by the rotation charging valve, the atomisation unit at body of heater top and below under the effect of the carrier gas that enters of tangential direction, hydrophilic nano-silicon dioxide enters the pyritous body of heater with the vaporific spiral way of gas phase, and carries out the successive surface chemical reaction and realize gas solid separation with the silicane surface treatment agent mixing steam that upwards sprays from the bottom continuous countercurrent.
2, the method by continuous surface Processing of Preparation hydrophobic nano silicon-dioxide according to claim 1, it is characterized in that: described carrier gas is a rare gas element.
3, the method by continuous surface Processing of Preparation hydrophobic nano silicon-dioxide according to claim 1 is characterized in that: described surface treatment stove adopts infrared or microwave heating obtains the required high temperature of surface treatment reaction.
4, the method by continuous surface Processing of Preparation hydrophobic nano silicon-dioxide according to claim 1, it is characterized in that: described silicane surface treatment agent is halosilanes, silazane or type siloxane surface treatment agent.
5, the method by continuous surface Processing of Preparation hydrophobic nano silicon-dioxide according to claim 1, it is characterized in that: the temperature of described Analytic Tower is controlled at 200~300 ℃, regulates Analytic Tower tail gas outlet valve and makes the pressure of surface treatment stove and Analytic Tower be lower than 10mmH 2O is to remove the waste gas that is mingled with.
6, the method by continuous surface Processing of Preparation hydrophobic nano silicon-dioxide according to claim 1 is characterized in that: prepared hydrophobic nano silicon-dioxide utilizes " wind cabinet " separator to realize the separation of thickness particle.
CNB2005100337764A 2005-03-28 2005-03-28 Method for preparing hydrophobic type nano silicon dioxide thruogh continuous surface treatment Active CN100506921C (en)

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CN101723317B (en) * 2009-12-09 2013-02-27 广州吉必盛科技实业有限公司 Method and device for on-line continuous surface treatment of hydrophilic nano-silicon dioxide
CN102513031B (en) 2011-11-30 2014-04-16 广州吉必盛科技实业有限公司 Deacidification process and equipment thereof
CN103073927A (en) * 2013-01-31 2013-05-01 沈阳化工股份有限公司 Surface-modified fumed silica capable of improving tearing strength of silicone rubber and production method of silicon dioxide
CN105399103B (en) * 2015-12-24 2017-12-05 江西黑猫炭黑股份有限公司 A kind of aerosil flatting silica and preparation method thereof
CN106000290A (en) * 2016-07-12 2016-10-12 常州大学 Silica gel hydrophobic modification method achieved under action of microwaves
CN108441026A (en) * 2018-04-25 2018-08-24 福建远翔新材料股份有限公司 A kind of dewatering nano hydrated SiO 2 and its preparation method and application
CN111392735B (en) * 2020-02-20 2021-08-06 广州汇富研究院有限公司 Surface modification combined treatment method of fumed silica
CN111286215B (en) * 2020-02-21 2021-07-06 广州汇富研究院有限公司 Continuous process for modifying surface of fumed silica

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3873337A (en) * 1972-08-14 1975-03-25 Degussa Process for the hydrophobization of higher dispersed oxides
US4503092A (en) * 1982-03-27 1985-03-05 Degussa Aktiengesellschaft Process for the hydrophobization of pyrogenically produced silica
US5057151A (en) * 1988-11-25 1991-10-15 Wacker-Chemie Gmbh Process for preparing hydrophobic particulate solids containing si-oh groups and a process for using the same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3873337A (en) * 1972-08-14 1975-03-25 Degussa Process for the hydrophobization of higher dispersed oxides
US4503092A (en) * 1982-03-27 1985-03-05 Degussa Aktiengesellschaft Process for the hydrophobization of pyrogenically produced silica
US5057151A (en) * 1988-11-25 1991-10-15 Wacker-Chemie Gmbh Process for preparing hydrophobic particulate solids containing si-oh groups and a process for using the same

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