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Preparation method and applications of super-hydrophobic SiO2 aerogel powder

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CN104003406A
CN104003406A CN 201410235770 CN201410235770A CN104003406A CN 104003406 A CN104003406 A CN 104003406A CN 201410235770 CN201410235770 CN 201410235770 CN 201410235770 A CN201410235770 A CN 201410235770A CN 104003406 A CN104003406 A CN 104003406A
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aerogel
powder
method
microemulsion
preparation
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CN 201410235770
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Chinese (zh)
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陈伟
劳里林
水中和
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武汉理工大学
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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.

Description

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 Methods and Application

技术领域 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。 [0001] Technical Field The present invention pertains to the preparation of inorganic nonmetallic materials, and in particular relates to a method of preparation and application of a super hydrophobic SiO2 airgel powder.

背景技术 Background technique

[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 aerogels are a unique aggregated nanoscale particles with highly crosslinked porous solid material, having a continuous three-dimensional network structure composed of more than 90% of air and less than 10% solids 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。 SiO2 aerogels structural properties, such that it has specific properties of mechanical, thermal, acoustic, optical, electrical, etc., such that it has ultra-low apparent density (about 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, low acoustic impedance, adsorption performance. 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 its special nature, it is bound to have broad application prospects in thermal insulation, medicine, environmental protection, chemistry and chemical catalysis, energy saving, aerospace and other fields.

[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 airgel powders SiO2 airgel generally used block then pulverized or spray or emulsion method. 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。 Atmospheric dried airgel block long production cycle, the modified incomplete state prone to such poor quality airgel powder prepared therefrom; Preparation Method airgel powder sprayed out of the spray tends to blocking droplet generation during agglomeration, which appears in the powder particle diameter exceeding Imm; preparation of emulsion produced airgel out since the emulsion droplet size 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。 Monodispersion [0004] Microemulsions are thermodynamically stable, transparent water droplets in oil (W / 0) or oil in water (0 / W) is formed, the particle diameter of the microstructure of 5 ~ 70nm, a surfactant ordered assembly molecule at the oil / water interface is formed. 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。 Except microemulsions and emulsions microemulsion droplets are formed by the water phase in the oil phase surfactant and co-surfactant action 5 to IOnm uniform properties of the liquid, and the liquid is an emulsion particle diameter in μ m or more, the emulsion can be stratified by gravity or centrifugation, while microemulsions are capable of prolonged standing or centrifugal water phase 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 two immiscible continuous medium is divided into a surfactant amphiphiles minute space, the microreactor is formed, in particular W / ο microemulsion can be formed microreactor (Micro pool) used to prepare nano-materials so that the size can be controlled in the nanometer range to the micron level, the reaction was generated in the solid-phase particles in the reaction 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。 Microemulsions can be of the size and stability of nanomaterials regulation, restriction nanoparticle nucleation, growth, coalescence, agglomeration and other processes, to form a particle size may 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。 Thus, an urgent need to find a way to make the airgel and the powder particle size distribution can be prepared dried at ambient temperature and pressure.

发明内容 SUMMARY

[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 method for preparing a superhydrophobic SiO2 airgel powder and its application, which was prepared by microemulsion method, the airgel can be made uniform particle size distribution of the powder in the normal temperature and pressing it to 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 technical solution of 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 SiO2 airgel powder preparation, characterized in that: wet gel is prepared using silica source solution, the oil phase, a surfactant and a microemulsion prepared cosurfactant, by Chen of washing, solvent substitution, the surface modification treatment, followed by drying at normal temperature and pressure to give the superhydrophobic powders SiO2 airgel. [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 embodiment, the step of preparing the microemulsion are: silicon source solution, a surfactant, co-surfactant with the oil phase liquid was stirred and mixed into a clear stable without delamination at 200 ~ 500r / min speed transparent microemulsion, the surfactant mass of from 5% to 25% relative to the total mass of silica source solution with the oil; the co-surfactant mass of 15% to 50% relative to the total mass of silica source solution with the oil of . 硅源溶液与油相的体积比优选为1:20~1:1。 The volume of the silicon source with the oil phase solution 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] In the above embodiment, the silicon source is a silicic acid sol or water glass solution. 所述硅酸溶胶的质量分数优选为10%~50%。 The mass fraction of silica sol is preferably 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 sodium silicate modulus of 1.0 to 4.0 or a mixed solution of potassium water-glass solution and water.

[0011 ] 上述方案中,所述油相为庚烷、辛烷或煤油。 [0011] In the above embodiment, the oil phase is 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] In the above 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] In the above 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 embodiment, the wet gel was dried powder after reforming treatment airgel powder form 0.5 ~ 4h at 15 ° C ~ 35 ° C and atmospheric pressure. 温度优选为室温25°C下。 At room temperature is preferably 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] In the above embodiment, the step of preparing the wet gel is obtained the aforementioned microemulsion neutralized to a pH of 6 to 10 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 Neutralizing the acid solution used in the microemulsion is aqueous sulfuric acid, hydrochloric acid, or nitric acid; the acid concentration of the solution

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, at 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 and microemulsions, may be used a commercially available silica sol, or silica sol with an ion exchange resin to remove cationic water glass prepared.

[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] In the above embodiment, the surface modification treatment after the step of replacing the solvent mixture with an organic solvent wet gel and soaked surface modifier, 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] In the above embodiment, the surface modifying agent is trimethylchlorosilane (of TMCS) or hexamethyl disilazane (HMDS).

[0018] 上述方案中,所述陈化步骤为在15~80°C下陈化I~48h。 [0018] In the above embodiment, the aging step at 15 ~ 80 ° C 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] In the above embodiment, the step of washing with absolute ethanol and deionized water rinse alternating wet gel after aging 2 to 15, wherein the oil phase was removed and the 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15~80°C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] In the above embodiment, the step of replacing the solvent with low surface tension organic solvent at 15 ~ 80 ° C to replace the wet gel after washing water out and replaced with 2 to 4 fractional organic solvents, replace the number is 2 to 5 times, each time replacing 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。 20Hz ~ 30Hz ultrasonic ultrasonic dispersing IOmin ~ Ih or dispersed by stirring with a number of 500r / min when the revolution frequency of each replacement.

[0021]本发明的有益效果是: [0021] Advantageous 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 powders can effectively control the particle size distribution of the powder, but also to obtain dried airgel powder prepared at ambient temperature and pressure, energy consumption is reduced. 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 in comparison 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 controllable particle size distribution characteristics, short preparation period, it can be dried at normal temperature and pressure.

[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) Method airgel powder prepared by the particle size distribution, small particle diameter, narrow particle size distribution can be well attached to the surface of the base material to produce a layer of gas condensate superhydrophobic body powder coating can be achieved 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 an SEM view of an embodiment of the powder prepared SiO2 airgel. [0025] 图2为实施例1所制备SiO2气凝胶粉体的XRD图。 [0025] FIG. 2 is a XRD pattern of Example 1 SiO2 airgel powder prepared embodiment.

[0026] 图3为实施例1所制备SiO2气凝胶粉体的FT-1R图。 [0026] FIG. 3 is a FT-1R FIG SiO2 airgel powder prepared in Example.

[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] Example 4 is an SiO2 airgel powder prepared embodiment of the contact angle of the test results of 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 SEM embodiment of FIG.

[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] Example 2 FIG 6 is a powder prepared SiO2 airgel embodiment the contact angle of the 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 in Example 3 Preparation of Powder SiO2 airgel embodiment.

[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 a diagram of the effect of four airgel powder prepared superhydrophobic coatings 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 better understanding of the present invention, the following embodiment is further illustrated in conjunction with the present invention and the accompanying drawings, but the present invention is not limited to the following embodiments.

[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 silicic acid sol as a raw material, and the kerosene was added 2ml IOml silicic acid sol in a container, and added 0.8g of cetyl trimethyl ammonium bromide (CTAB) and a co-surfactant 2.8g agent 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 stirring using a magnetic stirrer, until the liquid from the vessel the emulsion becomes clear and transparent milky 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。 Aqueous ammonia was added dropwise with stirring to a solution of PH ~ 12 until the microemulsion viscosity, the reaction was complete, the vessel is formed wet gel fine 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。 Deionized container 7K, soaked and washed with aging 6h absolute ethanol, filtered off with suction, and kerosene to remove excess 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 were dispersed for 2 hours and each replacement lh at an ultrasonic frequency of 25Hz with alcohol and n-hexane as a solvent. 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 (of TMCS) ratio of 2: 1 solution of hydrophobically modified, until completion of the reaction of TMCS was washed with n-hexane unreacted, 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。 FIG FIG 1 is a SEM airgel powder obtained can be seen from FIG 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。 FIG 2 is a XRD pattern of the obtained airgel powders, such description is for monolithic airgel powder composition. 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 a FT-1R FIG superhydrophobic powders of the obtained airgel, FIG wave number is 119 701 284 601 ^ 871 ^ (^ 1 vibration -S1-CH3 absorption peak group described gas condensate prepared powder body having hydrophobic properties. FIG. 4 is a superhydrophobic powders aerogels in slide contact angle of the surface coating, the contact angle reaches 161.5 °, this airgel powder is described superhydrophobic powders .

[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) dilution of sodium silicate modulus of 3.0, and stirred to obtain a uniform water glass 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 milky emulsion of the liquid from the vessel 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 wet gel particles formed in the container. 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+。 Deionized water was added to the container, soaked 8 hours and aging with absolute ethanol and deionized water alternately washed, suction 8 times to remove excess SDS and kerosene 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 is filtered off with suction, with the respective alcohol as solvent replacement and octane for 12 hours. 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 hydrophobically modified, until after completion of the reaction gel powder obtained by suction filtration, and dried at room temperature to give airgel powders 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。 FIG 5 is a particle size analysis of the powder obtained airgel, can be seen from the embodiment of FIG SiO2 airgel powder particles prepared in Example 2 was 24 μ m, 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。 FIG 6 is a superhydrophobic powders airgel slide contact angle on the surface of the coating, the contact angle reaches 154 °, this airgel powder is described 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 of sodium silicate modulus of 3.2 and stirred uniformly, diluted sodium water glass 732 by a styrene type strongly acidic ion exchange resin to remove Na +, silicic acid to give 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 4ml heptane and silica sol, was added 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。 Stirred with a magnetic stirrer, until the liquid from the vessel the emulsion becomes clear and transparent milky 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 to be sticky, the reaction was complete, the vessel is formed wet gel fine 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, partition with alcohol and heptane for 4 hours and replaced each dispersed frequency 25KHz ultrasonic 30min as solvent. 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 bis (trimethylsilyl) amine (of HMDZ) ratio of 1: 1 mixed solution of hydrophobically modified particles wet gel, until completion of the reaction was washed with heptane unreacted hexamethyl disilazane (HMDZ), and dried at room temperature to obtain a 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 FIG 7 is a particle size analysis of prepared FIG airgel powders, granules embodiment SiO2 airgel powder prepared in Example 3 36 μ m, 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] Due to the small diameter of the airgel particles prepared by the present invention, a narrow particle size distribution, is easily adsorbed on the base material, so that the superhydrophobic powders prepared aerogels of the present invention can be applied superhydrophobic coating field. 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 in Example 3 as an example, by airgel powder: acetone ratio (0.3g: 5ml) airgel powder dispersion, and brushing it on the concrete surface, after boil-off gas acetone gel powder adsorbed on the concrete surface superhydrophobic coating. 图8为超疏水涂层的超疏水效果。 FIG 8 is a superhydrophobic effect superhydrophobic coating.

Claims (10)

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。 1. A method for preparing superhydrophobic powders SiO2 aerogels, wherein: silicon source solution, the oil phase of the microemulsion prepared surfactants and co-surfactants is prepared wet gel by aging , washing, solvent substitution, the surface modification treatment, followed by drying at normal temperature and pressure to give the superhydrophobic powders SiO2 airgel.
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, wherein 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 and non-stratified into stable clear and transparent microemulsion, the surfactant mass of from 5% to 25% relative to the total mass of the silicon source solution with the oil; mass of the co-surfactant is a silicon source and a solution of the oil 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, wherein 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。 The production method according to claim 1, wherein the surfactant is cetyltrimethylammonium 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15°C~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 the wet gel modified powder treated at 15 ° C ~ 35 ° C and the pressure 0.5 ~ 4h was dried airgel powder form.
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, wherein the step of preparing the wet gel is obtained the aforementioned microemulsion neutralized to a pH of 6 to 10 to obtain a wet gel SiO2.
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 the surface modification treatment after the step of replacing the solvent soaking wet gel mixed with an organic solvent and a surface modifier, a 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. A method of preparation according to claim 8, wherein said surface modifying agent is trimethylchlorosilane 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. Application of the superhydrophobic coating superhydrophobic SiO2 airgel powder prepared according to the method of claim 1 prepared.
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