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Publication numberCN104003406 A
Publication typeApplication
Application numberCN 201410235770
Publication date27 Aug 2014
Filing date30 May 2014
Priority date30 May 2014
Publication number201410235770.4, CN 104003406 A, CN 104003406A, CN 201410235770, CN-A-104003406, CN104003406 A, CN104003406A, CN201410235770, CN201410235770.4
Inventors陈伟, 劳里林, 水中和
Applicant武汉理工大学
Export CitationBiBTeX, EndNote, RefMan
External Links: SIPO, Espacenet
Preparation method and applications of super-hydrophobic SiO2 aerogel powder
CN 104003406 A
Abstract
The invention relates to a preparation method and applications of super-hydrophobic SiO2 aerogel powder. The method is implemented through the following steps: preparing a silicon source solution, an oil phase, a surfactant and a surfactant aid into a microemulsion; then, neutralizing the microemulsion until the pH value is 6-10 so as to form wet microgel particles; sequentially carrying out ageing, washing and solvent exchange on the wet microgel particles; finally, modifying the obtained product by using a silane modifier, and drying gel at normal pressure and temperature so as to obtain aerogel powder. The method is capable of preparing aerogel powder by using a microemulsion, the particle size of aerogel powder prepared by using the method is uniformly distributed, and prepared aerogel powder has the characteristics of controllable particle size distribution, short preparation period, and capability of being dried at normal pressure and temperature.
Claims(10)  translated from Chinese
1.一种超疏水性SiO2气凝胶粉体的制备方法,其特征在于:采用硅源溶液、油相、表面活性剂和助表面活性剂制备的微乳液来制备湿凝胶,经陈化、洗涤、溶剂替换、表面改性处理,常压常温下干燥后得到所述超疏水性SiO2气凝胶粉体。 A method for producing a super-hydrophobic SiO2 airgel powder, wherein: the silicon source solution, the oil phase, the microemulsion surfactant and co-surfactant prepared wet gel prepared by aging washing, solvent substitution, surface modification, normal temperature and pressure to get the super-hydrophobic SiO2 airgel powder was followed by drying.
2.根据权利要求1所述的制备方法,其特征在于,制备微乳液的步骤为:将硅源溶液、表面活性剂、助表面活性剂与油相混合液体在200~500r/min转速下搅拌而转变为稳定不分层的澄清透明微乳液,所述表面活性剂的质量为硅源溶液与油相总质量的5%~25%;所述助表面活性剂的质量为硅源溶液与油相总质量的15%~50%。 2. The production method according to claim 1, characterized in that the step of preparing a microemulsion of: silicon source solution, a surfactant, co-surfactant mixed with the oil phase liquid was stirred at 200 ~ 500r / min speed The non-stratified into stable clear and transparent microemulsion, the surfactant mass of 5% to 25% silica source solution with the total mass of the oil phase; quality of the co-surfactant is an oil solution of silicon source 15% to 50% relative to the total mass.
3.根据权利要求1所述的制备方法,其特征在于,所述硅源为水玻璃溶液或硅酸溶胶。 3. The production method according to claim 1, wherein said silicon source is waterglass solution or silica sol.
4.根据权利要求1所述的制备方法,其特征在于,所述油相为庚烷、辛烷或煤油。 4. The production method according to claim 1, characterized in that the oil phase is heptane, octane or kerosene.
5.根据权利要求1所述的制备方法,其特征在于,所述表面活性剂为十六烷基三甲基溴化铵或十二烷基硫酸钠;所述助表面活性剂为正丁醇或2,4-己二醇。 5. The production method according to claim 1, wherein said surfactant is cetyl trimethyl ammonium bromide or sodium lauryl sulfate; the co-surfactant is n-butanol or 2,4-hexanediol.
6.根据权利要求1所述的制备方法,其特征在于,改性处理后的湿凝胶粉体在15C~35 C及常压条件下干燥0.5~4h形成气凝胶粉体。 6. The production method according to claim 1, characterized in that, after the wet gel powder modification at 15 C ~ 35 C and the pressure 0.5 ~ 4h dried airgel powder is formed.
7.根据权利要求1所述的制备方法,其特征在于,制备湿凝胶的步骤是将前述得到的微乳液中和到pH为6~10即得到SiO2湿凝胶。 7. The production method according to claim 1, characterized in that the step of preparing the wet gel is obtained microemulsion aforementioned neutralized to a pH of 6 to 10 to obtain SiO2 wet gel.
8.根据权利要求1所述的制备方法,其特征在于,所述表面改性处理步骤是将溶剂替换后的湿凝胶用有机溶剂和表面改性剂混合浸泡,改性Ih~48h。 8. The production method according to claim 1, wherein said surface modification treatment step is to replace the solvent after the wet gel with an organic solvent and a surface modifier mixed soaking, modified Ih ~ 48h.
9.根据权利要求8所述的制备方法,其特征在于,所述表面改性剂为三甲基氯硅烷或六甲基二硅氮烷。 9. The production method according to claim 8, wherein said surface modifying agent is trimethyl chlorosilane or hexamethyl disilazane.
10.根据权利要求1所述的制备方法制备得到的超疏水性SiO2气凝胶粉体在超疏水涂层中的应用。 10. The super-hydrophobic SiO2 airgel powder preparation method according to claim prepared in Super hydrophobic coating.
Description  translated from Chinese

一种超疏水性S i O2气凝胶粉体的制备方法及应用 A super-hydrophobic airgel S i O2 powder preparation method and application

技术领域 Technical Field

[0001] 本发明属于无机非金属材料的制备技术领域,特别涉及一种超疏水性SiO2气凝胶粉体的制备方法及应用。 Preparation invention belongs to the technical field of inorganic non-metallic materials [0001] This particularly relates to the preparation and application of a super-hydrophobic SiO2 airgel powders.

背景技术 Background

[0002] SiO2气凝胶是一种独特的由纳米级微粒高度交联聚集的具有多孔性的固体材料,具有连续的三维网络结构,它由90%以上的空气和不到10%的固体组成。 [0002] SiO2 airgel is a unique nano-particles are highly crosslinked by the aggregation of a solid material with a porous, with a continuous three-dimensional network structure, which consists of more than 90% of the air and less than 10% of solid composition . SiO2气凝胶的结构特性,使得它具有力学、热学、声学、光学、电学等方面的特殊性质,比如它具有超低的表观密度(0.03g/cm3左右)、超低的导热系数(0.03W/m*K以下)、高比表面积(600~1200m2/g)、低折射率、低声阻、强吸附性能等。 Structural characteristics of SiO2 aerogels, so that it has special properties mechanical, thermal, acoustic, optical, electrical and other aspects, such as its ultra-low apparent density (around 0.03g / cm3), ultra-low thermal conductivity (0.03 W / m * K or less), high specific surface area (600 ~ 1200m2 / g), a low refractive index, whispered resistance, strong absorption properties. S iO2气凝胶作为一种新材料,因其特殊性质,其必然会在隔热绝热、医药、环保、化学化工催化、建筑节能、航空航天等领域有着广阔的应用前景。 S iO2 airgel as a new material, because of their special nature, it is bound to the heat insulation, medicine, environmental protection, chemistry and chemical catalysis, energy saving, aerospace and other fields have broad application prospects.

[0003]目前,SiO2气凝胶粉末的制备一般是采用制备气凝胶块体再磨成粉末或采用喷雾法或乳液法。 [0003] Currently, the preparation of SiO2 airgel powder is generally prepared using airgel blocks and then ground to a powder or spray or emulsion. 常压干燥制备气凝胶块体制作周期长,容易出现改性不完全的情况,使得制备出来的气凝胶粉体品质不佳;喷雾法制备出来的气凝胶粉体则容易在喷雾的过程中液滴产生粘连团聚,从而出现粒径超过Imm的粉体;乳液法制备出来的气凝胶则由于乳液液滴大小不均一,制备出来的气凝胶粉体粒径分布范围宽。 DRYING pressure airgel blocks long production cycle, modified incomplete situation prone to such quality out of the poor preparation of airgel powders; prepare legal airgel powder spray out of the spray is easy droplets produced during blocking reunion, which appears more than Imm powder particle size; aerogels prepared by emulsion method out of the emulsion droplet size due to non-uniform, wide airgel powder particle size distribution prepared out of range.

[0004] 微乳液是热力学稳定、透明的水滴在油中(W/0)或油滴在水中(0/W)形成的单分散体系,其微结构的粒径为5~70nm,是表面活性剂分子在油/水界面形成的有序组合体。 Monodisperse system [0004] Microemulsions are thermodynamically stable, transparent water droplets in oil (W / 0) or oil in water (0 / W) is formed, the particle size of its micro structure 5 ~ 70nm, the surface-active Ordered assembly molecules at the oil / water interface formation. 微乳液和乳液的不同之处在于微乳液是由水相油相在表面活性剂和助表面活性剂的作用下形成的液滴在5~IOnm的性质均一的液体,而乳液则是液体粒径在μ m以上,所以乳液能在重力或者离心的作用下分层,而微乳液则能在长时间静置或离心下水相油相不分层。 The difference is that the microemulsion and microemulsion is an emulsion droplets under oil phase in the aqueous phase by the surfactant and co-surfactant role in the formation of the 5 to the nature of liquid IOnm uniform, while the emulsion is a liquid particle In μ m or more, the emulsion can be under the influence of gravity or centrifugal stratification, and the microemulsion is capable of long standing or centrifugal water phase of the oil phase is not hierarchical.

[0005] 在微乳液体系中,两种互不相溶的连续介质被表面活性剂双亲分子分割成微小空间,形成微型反应器,特别是W/ο型微乳液,可以形成微反应器(微水池)从而用来制备纳米材料,其大小可控制在纳米级范围到微米级,反应物在体系中反应生成固相粒子。 [0005] In the microemulsion system, the continuous medium is divided into two mutually insoluble amphiphilic surfactant molecules into tiny space, forming the microreactor, especially W / ο microemulsion can form micro-reactor (micro Pool) thereby to nanomaterials, the size can be controlled in the nanometer range to the micron level, the reaction was the reaction of solid-phase particles in the system. 微乳液能对纳米材料的粒径和稳定性进行调控,限制纳米粒子的成核、生长、聚结、团聚等过程,从而形成的颗粒粒径可调控。 Microemulsion capable of particle size and stability of nanomaterials regulate, restrict nanoparticle nucleation, growth, coalescence, agglomeration and other processes, particle size and thus formed can be regulated. 因此,急需寻找一种能够使气凝胶粉体颗粒粒径分布均匀且在常温常压下即可干燥的制备方法。 Hence, the urgent need to find a way to make airgel powder particle size distribution and can be dried at ambient temperature and pressure preparation.

发明内容 DISCLOSURE

[0006] 本发明的目的在于提供一种超疏水性SiO2气凝胶粉体的制备方法及应用,该方法采用微乳液法制备,能够使气凝胶粉体颗粒粒径分布均匀且在常温常压下即可干燥。 [0006] The object of the present invention is to provide a super-hydrophobic SiO2 airgel powder preparation and application of the method were prepared by microemulsion method, it is possible to make airgel powder particle size and uniform distribution of the normal temperature pressure can be dry.

[0007] 为实现上述目的,本发明的技术方案是: [0007] To achieve the above object, the present invention is:

[0008] 一种超疏水性SiO2气凝胶粉体的制备方法,其特征在于:采用硅源溶液、油相、表面活性剂和助表面活性剂制备的微乳液来制备湿凝胶,经陈化、洗涤、溶剂替换、表面改性处理,常压常温下干燥后得到所述超疏水性SiO2气凝胶粉体。 [0008] A superhydrophobic powder prepared SiO2 airgel, characterized in that: to prepare the wet gel silicon source solution, the oil phase, surfactant and cosurfactant microemulsion prepared by Chen of washing, solvent substitution, surface modification, normal temperature and pressure to get the super-hydrophobic SiO2 airgel powder was followed by drying. [0009] 上述方案中,制备微乳液的步骤为:将硅源溶液、表面活性剂、助表面活性剂与油相混合液体在200~500r/min转速下搅拌而转变为稳定不分层的澄清透明微乳液,所述表面活性剂的质量为硅源溶液与油相总质量的5%~25% ;所述助表面活性剂的质量为硅源溶液与油相总质量的15%~50%。 [0009] In the above, the step of preparing a microemulsion of: silicon source solution, surface active agents, surfactants and oil are mixed into a stable liquid stirring clarification is not hierarchical at 200 ~ 500r / min speed transparent microemulsion, the surfactant mass of 5% to 25% silica source solution with the total mass of the oil phase; quality of the co-surfactant is 15% to 50% silica source solution with the total mass of the oil phase . 硅源溶液与油相的体积比优选为1:20~1:1。 The volume of the silicon source solution with the oil phase is preferably from 1:20 to 1: 1.

[0010] 上述方案中,所述硅源为水玻璃溶液或硅酸溶胶。 [0010] the above-described embodiment, the silicon source is waterglass solution or silica sol. 所述硅酸溶胶的质量分数优选为10%~50%。 The mass fraction of silica sol is preferably from 10% to 50%. 所述水玻璃溶液为模数为1.0~4.0的钠水玻璃或钾水玻璃溶液与水的混合溶液。 The sodium silicate solution is a modulus of sodium water glass or a mixed solution of 1.0 to 4.0 of potassium silicate solution with water was.

[0011 ] 上述方案中,所述油相为庚烷、辛烷或煤油。 [0011] the above-described embodiment, the oil phase as heptane, octane or kerosene.

[0012] 上述方案中,所述表面活性剂为十六烷基三甲基溴化铵(CTAB)或十二烷基硫酸钠(SDS)。 [0012] The above-described embodiment, the surfactant is cetyl trimethyl ammonium bromide (CTAB) or sodium dodecyl sulfate (SDS).

[0013] 上述方案中,所述助表面活性剂为正丁醇或2,4-己二醇。 [0013] The above-described embodiment, the co-surfactant is n-butanol or 2,4-hexanediol.

[0014] 上述方案中,改性处理后的湿凝胶粉体在15 C~35 C及常压条件下干燥0.5~4h形成气凝胶粉体。 [0014] In the above scheme, the wet gel powder after modification at 15 C ~ 35 C and the pressure 0.5 ~ 4h dried airgel powder is formed. 温度优选为室温25C下。 The temperature is preferably room temperature of 25 C.

[0015] 上述方案中,制备湿凝胶的步骤是将前述得到的微乳液中和到pH为6~10即得到SiOjM凝胶。 [0015] the above, the step of preparing a wet gel is obtained in the aforementioned microemulsion neutralized to pH 6 to 10 to obtain SiOjM gel. 中和微乳液所用的酸溶液为硫酸、盐酸、或硝酸的水溶液;酸溶液浓度为 In acid solution and microemulsion used is an aqueous solution of sulfuric acid, hydrochloric acid or nitric acid; the acid solution at a concentration of

0.5~2.5mol/L ;碱溶液为氨水、氢氧化钠、或氢氧化钾的水溶液,其浓度为0.5~5mol/L。 0.5 ~ 2.5mol / L; alkali solution of ammonia, sodium hydroxide, potassium hydroxide, or an aqueous solution of a concentration of 0.5 ~ 5mol / L. 当硅源为水玻璃溶液时,采用酸溶液中和微乳液;当硅源为硅酸溶胶时,采用碱溶液中和微乳液,硅酸溶胶可使用市售硅酸溶胶或用离子交换树脂除去水玻璃中的阳离子制得。 When the silicon source is sodium silicate solution with an acid solution and microemulsion; when the silicon source is silica sol, alkali solution, microemulsion, use a commercially available silica sol sol or silicic acid ion exchange resin to remove and water glass cation system.

[0016] 上述方案中,所述表面改性处理步骤是将溶剂替换后的湿凝胶用有机溶剂和表面改性剂混合浸泡,改性Ih~48h。 [0016] the above-described embodiment, the surface modification step is to replace the solvent after the wet gel mixed with an organic solvent and a surface modifier soaking, modified Ih ~ 48h. 所述有机溶剂为正己烷、环己烷、庚烷或辛烷。 The organic solvent is n-hexane, cyclohexane, heptane or octane.

[0017] 上述方案中,所述表面改性剂为三甲基氯硅烷(TMCS)或六甲基二硅氮烷(HMDS)。 [0017] The above-described embodiment, the surface modifying agent is trimethylchlorosilane (TMCS) or hexamethyl disilazane (HMDS).

[0018] 上述方案中,所述陈化步骤为在15~80C下陈化I~48h。 [0018] The above scheme, the aging step at 15 ~ 80 C under aging I ~ 48h.

[0019] 上述方案中,所述洗涤步骤是用无水乙醇和去离子水交替冲洗陈化后的湿凝胶2~15次,除去其中的油相以及多余的Na+等杂质离子。 [0019] of the above, the washing step with ethanol and deionized water rinse alternately wet gel after aging from 2 to 15 times, the oil phase and remove excess impurities such as Na + ions.

[0020] 上述方案中,所述溶剂替换步骤是用低表面张力的有机溶剂在15~80C将洗涤后的湿凝胶中的水分替换出来,用2~4种有机溶剂分步替换,替换次数为2~5次,每次替换时间为2~12h。 [0020] The above-described embodiment, the step of replacing the solvent is an organic solvent with a low surface tension at 15 ~ 80 C wet gel after washing in the water replace it with two to four kinds of organic solvent fractional replacement, Replace number from 2 to 5 times, each time was replaced with 2 ~ 12h. 每次替换时用频率为20Hz~30Hz的超声波进行超声分散IOmin~Ih或用500r/min转数搅拌分散。 Each time replaced with a frequency of 20Hz ~ 30Hz ultrasonic ultrasonic dispersing IOmin ~ Ih stirring dispersing or 500r / min rotation speed.

[0021]本发明的有益效果是: [0021] The beneficial effects of the present invention are:

[0022] I)采用微乳液法制备气凝胶粉体,可以有效的控制粉体的粒径分布,还能在常温常压下干燥制备得气凝胶粉体,减小了生产能耗。 [0022] I) was prepared by microemulsion method airgel powder, can effectively control the particle size distribution of the powder, but also in the preparation was dried at ambient temperature and pressure airgel powder, reduced energy consumption. 微乳液法与传统的制备方法相比,具有明显的优势和先进性。 Microemulsion method compared with the conventional production method has obvious advantages and advanced. 同时具有粒径分布可调控、制备周期短、在常温常压下即可干燥的特点。 While having a particle size distribution can be regulated, short preparation period, can be dried at ambient temperature and pressure characteristics.

[0023] 2)该法制备的气凝胶粉体颗粒粒径分布均匀,其颗粒粒径小,粒径分布窄,可以在基底材料表面上较好地附着从而产生一层超疏水性气凝胶粉体涂层,可以达到超疏水、自清洁的效果。 [0023] 2) Preparation of airgel powder particle size distribution of the rule of law, its small particle size, narrow particle size distribution can be better adhered to produce super-hydrophobic airgel layer on the substrate surface body powder coating, can achieve superhydrophobic, self-cleaning effect.

附图说明 Brief Description

[0024] 图1为实施例1所制备SiO2气凝胶粉体的SEM图。 [0024] FIG. 1 is prepared in Example 1 SiO2 airgel powders SEM embodiment. [0025] 图2为实施例1所制备SiO2气凝胶粉体的XRD图。 [0025] FIG. 2 as an example a prepared SiO2 airgel powder XRD pattern implemented.

[0026] 图3为实施例1所制备SiO2气凝胶粉体的FT-1R图。 [0026] FIG. 3 as an example an SiO2 airgel powder prepared FT-1R embodiment.

[0027] 图4为实施例1所制备SiO2气凝胶粉体的接触角测试结果图。 [0027] FIG. 4 as an example a powder compact prepared SiO2 airgel contact angle test results shown in Fig.

[0028] 图5为实施例2所制备SiO2气凝胶粉体的SEM图。 [0028] FIG. 5 is prepared in Example 2 SiO2 airgel powder compact SEM image.

[0029] 图6为实施例2所制备SiO2气凝胶粉体的接触角测试结果图。 [0029] FIG. 6 is prepared in Example 2 SiO2 airgel powder compact contact angle of test results in Fig.

[0030] 图7为实施例3所制备SiO2气凝胶粉体的粒径分布图。 [0030] FIG. 7 is a particle size distribution of SiO2 airgel prepared in Example 3 Powders implemented.

[0031] 图8为实施例4所制备超疏水性气凝胶粉体涂层的效果图。 [0031] FIG. 8 is prepared in Example 4 superhydrophobic effect of airgel powder coating embodiment.

具体实施方式 DETAILED DESCRIPTION

[0032] 为更好的理解本发明,下面结合实施例和附图进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。 [0032] For a better understanding of the present invention is further illustrated below in connection with the contents of the present invention and the accompanying drawings, but the present invention is not limited to the following examples.

[0033] 实施例1 [0033] Example 1

[0034] 以20%质量分数的硅酸溶胶为原料,在容器中加入IOml煤油和2ml硅酸溶胶,并加入0.8g十六烷基三甲基溴化铵(CTAB)和2.8g助表面活性剂正丁醇。 [0034] 20% by mass of silica sol as raw material, adding IOml kerosene and 2ml silica sol in the container, and add 0.8g of cetyl trimethyl ammonium bromide (CTAB) and 2.8g co-surfactants agent n-butanol. 使用250rpm磁力搅拌机搅拌,待容器中液体从乳白色的乳液变为澄清透明的微乳液。 250rpm using a magnetic stirrer stirring until the liquid from the container into a clear and transparent milky white emulsion of microemulsion. 边搅拌边滴加PH~12的氨水溶液,待微乳液黏稠,反应完成,容器中形成细微的湿凝胶颗粒。 Was added dropwise with stirring ammonia solution PH ~ 12 until microemulsion viscosity, the reaction was complete, the container is formed fine wet gel particles. 容器中加入去离子7K,浸泡6h陈化和用无水乙醇洗涤、抽滤,以除去煤油和多余的CTAB。 Container deionized 7K, soak 6h aging and washed with ethanol, suction to remove excess kerosene and CTAB. 抽滤之后的湿凝胶,分别用酒精和正己烷作溶剂各替换2小时并在25Hz频率的超声波下分散lh。 After the wet gel filtration, respectively with alcohol and n-hexane as a solvent to replace two hours each and 25Hz frequency of the ultrasonic dispersed lh. 用正己烷与三甲基氯硅烷(TMCS)比例为2:1的溶液进行疏水改性,待反应完全后用正己烷洗涤未反应的TMCS,室温干燥Ih即可得到二氧化硅气凝胶粉体。 N-hexane and trimethylchlorosilane (TMCS) ratio of 2: 1 solution of hydrophobically modified, until completion of the reaction was washed with n-hexane unreacted TMCS, and dried at room temperature to obtain a silica airgel powder Ih body. 图1是得到的气凝胶粉体的SEM图,从图中可以看出SiO2气凝胶粉体颗粒比较均匀,从I μ m~3 μ m之间。 Figure 1 is a powder obtained airgel SEM image, it can be seen from the figure SiO2 airgel powder particles are relatively evenly between the I μ m ~ 3 μ m. 图2为所得到的气凝胶粉体的XRD图,说明这种气凝胶粉体是一种不定形物。 Figure 2 is the resultant airgel powder XRD pattern shows that airgel powder is an amorphous substance. 图3为所得到的超疏水性气凝胶粉体的FT-1R图,图中波数为284601^119701^871(^1为-S1-CH3基团的振动吸收峰,说明所制备的气凝胶粉体为具有疏水性质。图4为超疏水性气凝胶粉体在载玻片表面涂层的接触角测试,接触角达到161.5,说明此气凝胶粉体为超疏水性粉体。 Figure 3 is the resulting airgel superhydrophobic powder FT-1R, FIG wave number is 284 601 119 701 ^ 871 ^ (^ 1 -S1-CH3 groups vibration absorption peak, indicating gas condensate prepared powder body having hydrophobic properties. Figure 4 is a super-hydrophobic airgel powder surface of the slide in the contact angle of the coating, the contact angle reaches 161.5 , the description for this airgel powder is superhydrophobic powder .

[0035] 实施例2 [0035] Example 2

[0036] 按水:水玻璃体积比(3:1)稀释模数为3.0的钠水玻璃,并搅拌均匀过滤得到水玻璃溶液,在容器中加入IOml煤油和4ml水玻璃溶液,加入4g十二烷基硫酸钠(SDS)和 [0036] by water: water glass volume ratio (3: 1) was diluted modulus of 3.0 sodium water glass, sodium silicate and stir the solution was filtered, and the kerosene was added 4ml IOml waterglass solution in the vessel, was added 4g twelve alkyl sulfate (SDS) and

3.5g助表面活性剂2,4-己二醇。 3.5g cosurfactant 2,4-hexanediol. 在200rpm转数搅拌下容器中液体从乳白色的乳液变为澄清透明的微乳液。 The number of revolutions 200rpm stirring vessel from the milky liquid emulsion becomes clear and transparent microemulsion. 边搅拌边滴加2mol/L的硫酸溶液,待微乳液黏稠,反应完成,容器中形成湿凝胶颗粒。 Was added dropwise with stirring 2mol / L sulfuric acid solution, microemulsion viscosity until the reaction is complete, the vessel form a wet gel particles. 容器中加入去离子水,浸泡8小时陈化和用无水乙醇和去离子水交替洗涤、抽滤8次,以除去煤油和多余的SDS和Na+。 Vessel was charged with deionized water, soak 8 hours aging and with ethanol and deionized water alternating washing, leaching 8 times to remove excess kerosene and SDS and Na +. 抽滤之后的湿凝胶,用酒精和辛烷作溶剂各替换12小时。 After the wet gel filtration, as a solvent with alcohol and replace octane 12 hours each. 用辛烷:TMCS(1:2)比例的溶液进行溶剂替换和疏水改性,待反应完全后抽滤得到凝胶粉体,室温干燥3h得到气凝胶粉体。 With octane: TMCS (1: 2) was subjected to solvent replacement ratio and hydrophobic modification, pending completion of the reaction gel powder obtained after filtration, dried at room temperature to give airgel powder 3h. 图5是得到的气凝胶粉体的粒径分析图,从图中可以看出实施例2所制备的SiO2气凝胶粉体颗粒为24 μ m,粒径分布为9 μ m~69 μ m。 Figure 5 is a particle size analysis chart airgel powder obtained from the figure can be seen to implement SiO2 airgel powder particles prepared in Example 2 was 24 μ m, the particle size distribution of 9 μ m ~ 69 μ m. 图6为超疏水性气凝胶粉体在载玻片表面涂层的接触角测试,接触角达到154,说明此气凝胶粉体为超疏水性粉体。 Figure 6 is a super-hydrophobic airgel powder contact angle of the surface coating on a glass slide, the contact angle reaches 154 , the description for this airgel powder is superhydrophobic powders. [0037] 实施例3 [0037] Example 3

[0038] 按水:水玻璃体积比(4:1)稀释模数为3.2的钠水玻璃并搅拌均匀,将稀释水玻璃通过732钠型强酸型苯乙烯离子交换树脂以去除Na+,得到硅酸溶胶。 [0038] by water: water glass volume ratio (4: 1) dilution modulus of 3.2 sodium water glass and stir evenly, the diluted water glass by 732 to remove Na Na strong acid ion exchange resin + styrene, silicic acid sol. 取20ml庚烷及4ml硅酸溶胶,并加入1.6g十六烷基三甲基溴化铵(CTAB)和3.0g助表面活性剂正丁醇。 Take 20ml of heptane and 4ml silicic acid sol, and adding 1.6g of cetyl trimethyl ammonium bromide (CTAB) and 3.0g of n-butanol co-surfactant. 使用磁力搅拌机搅拌,待容器中液体从乳白色的乳液变为澄清透明的微乳液。 Using a magnetic stirrer stirring until the liquid from the container into a clear and transparent milky white emulsion of microemulsion. 边搅拌边滴加2mol/L的氢氧化钠溶液,待微乳液黏稠,反应完成,容器中形成细微的湿凝胶颗粒。 Was added dropwise with stirring 2mol / L sodium hydroxide solution, microemulsion viscosity until the reaction was complete, the container is formed fine wet gel particles. 用去离子水浸泡陈化8h之后,使用去离子水洗涤以除去CTAB。 After immersion in deionized water aging 8h, washed with deionized water to remove CTAB. 抽滤之后的湿凝胶,分用酒精和庚烷作溶剂各替换4小时并在25KHz频率的超声波下分散30min。 After the wet gel filtration, sub alcohol used as a solvent and heptane replace four hours each and 25KHz frequency ultrasonic dispersed 30min. 用庚烷与六甲基二硅氮烷(HMDZ)比例为1:1的混合溶液对湿凝胶颗粒进行疏水改性,待反应完全后用庚烷洗涤未反应的六甲基二硅氮烷(HMDZ),室温干燥0.5h即可得到二氧化硅气凝胶粉体。 With heptane and hexamethyl disilazane (HMDZ) ratio of 1: 1 mixed solution of hydrophobically modified wet gel particles, hexamethyldisilazane After completion of the reaction was washed with heptane unreacted silazane (HMDZ), dried at room temperature to obtain the silica airgel powder 0.5h. 图7是制备得到气凝胶粉体的粒径分析图,实施例3所制备的SiO2气凝胶粉体颗粒36 μ m,粒径分布为15 μ m ~91 μ m0 Figure 7 is a particle size analysis chart prepared airgel powders, powder particles embodiment SiO2 airgel prepared in Example 3 36 μ m, a particle size distribution of 15 μ m ~ 91 μ m0

[0039] 实施例4 [0039] Example 4

[0040] 由于本发明制备出的气凝胶颗粒粒径小,粒径分布范围窄,容易吸附在基底材料上,故本发明制备的超疏水性气凝胶粉体可应用在超疏水涂层领域。 [0040] The present invention due to the small particle size aerogels prepared, narrow particle size distribution, easily adsorbed on the substrate material, so super-hydrophobic airgel powder prepared by the present invention can be applied superhydrophobic coating fields. 以实施例3制备的气凝胶粉体为例,按气凝胶粉体:丙酮比例为(0.3g:5ml)分散气凝胶粉体,并将其涂刷于混凝土表面,丙酮挥发之后气凝胶粉体吸附于混凝土表面形成超疏水涂层。 Airgel powder prepared as in Example 3, for example, by airgel powder: ratio of acetone (0.3g: 5ml) airgel powder dispersion, and brushing the concrete surface, after the acetone volatile gas gel powder adsorbed on the surface of the concrete form superhydrophobic coatings. 图8为超疏水涂层的超疏水效果。 Figure 8 is a super-hydrophobic effect superhydrophobic coating.

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International ClassificationC04B41/50, C09C3/12, C09C3/08, C09D1/00, C09C1/28, C01B33/14, C01B33/158, C01B33/159
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