Sol-Gel法二氧化硅溶胶的制备及性能影响研究

以正硅酸乙酯为前驱体,硝酸为催化剂,制备了SiO2溶胶.研究了催化剂、水、乙醇的加入量对溶胶粘度和凝胶时间的影响。结果表明,在保持其它反应条件不变的情况下,随着EtOH/TEOS摩尔比的增大,溶胶粘度减小,凝胶时间变长;随着H2O/TEOS摩尔比的增大,溶胶粘度先增大后减小,凝胶时间先变短后变长,H2O/TEOS=9.6左右时粘度最大,凝胶时间最短;pH<2时,随着HNO3/TEOS摩尔比的增大,溶胶粘度增大,凝胶时间变短。     

SiO2溶胶的甲基化改性及其性能研究

采用溶胶-凝胶法,以甲基三乙氧基硅烷(MTES)为疏水性前驱物,对SiO2溶胶进行甲基化改性,制备MTES-SiO2溶胶,考察了MTES的加入对SiO2溶胶化学结构和性能的影响.结果表明,随着MTES加入量的增加,溶胶的粘度减小,凝胶时间延长,溶胶粒径略微增大.红外光谱分析表明,MTES-SiO2溶胶以Si -O - Si键为主,体系中已成功引入Si - CH3基团,所形成的SiO2分子具有线型结构.MTES-SiO2溶胶在陈化过程中,在粘度发生急剧改变前,溶胶的粘度、固含量变化不大,溶胶粒径略有增加.随着凝胶点的接近,溶胶分子逐渐由线型结构过度到三维网络结构.     

莫来石纤维增强SiO2气凝胶隔热材料的制备

以正硅酸乙酯（TEOS）为硅源,采用溶胶-凝胶及超临界干燥技术制备了莫来石纤维增强SiO2气凝胶隔热材料,并系统地研究了HF催化剂以及溶剂等制备因素对气凝胶品质的影响。结果表明：HF催化剂、H2O、乙醇和甲酰胺用量对TEOS的水解缩聚反应有较大影响,调节其配比可以制备具有不同密度的SiO2气凝胶隔热材料;添加甲酰胺可以调节凝胶内部网络结构,防止干燥时由于应力不均而开裂或破裂。     

HCl-NH3双组分催化正硅酸乙酯快速制备SiO2气凝胶

以正硅酸乙酯(TEOS)为原料,水和乙醇为溶剂,盐酸和氨水为催化剂,采用溶胶-凝胶法制备了SiO2气凝胶.研究了水和乙醇及催化剂对制备SiO2气凝胶反应速度、凝胶时间的影响.结果表明HCl和NH3·H2O作为催化剂大大加速了溶胶和凝胶反应速度,使凝胶时间减少至几分钟甚至更短,所制备的SiO2气凝胶具有纳米多孔结构(骨架颗粒为15～20nm,孔洞尺寸为10～30 nm).     

合成条件对常压干燥炭气凝胶电导率的影响

以间苯二酚/甲醛为反应物,采用常压干燥工艺制备了高电导率的炭气凝胶,并用XRD和四探针电导率测试仪对其进行了表征。结果表明：炭气凝胶具有典型的非晶态结构,且其结构中存在特殊的半石墨相微晶;凝胶陈化时间、催化剂种类和溶胶pH值对炭气凝胶电导率影响不大;炭气凝胶的电导率随催化剂摩尔比、溶质固含量、炭化终温和升温速率的增大而升高。以Na2CO3为催化剂,催化剂摩尔比为500、溶质固含量为60%,5℃/min升温至1050℃炭化制备的炭气凝胶电导率高达98.0S/cm。     

催化剂对正硅酸乙酯常压合成SiO2气凝胶的研究

以正硅酸乙酯为硅源,分别以 HF 和 HF/氨水为催化剂,通过溶胶-凝胶法常压制备 SiO2 气凝胶.研究表明以 HF 为催化剂能有效地加快反应的速度,当以 HF/氨水为催化剂时对产品的合成和性能产生更大的影响.用热重分析仪(TG-DTA)、比表面(BET)、XRD、傅里叶变换红外光谱仪、激光粒度仪等仪器对两种产品微结构测试结果表明:两种产品都是非晶纳米多孔结构,体积平均粒径小于 20μm,为介孔结构.     

莫来石纤维增强SiO_2气凝胶隔热材料的制备工艺研究

以正硅酸乙酯(TEOS)为硅源,氢氟酸(HF)为催化剂,采用溶胶-凝胶法及超临界干燥技术制备了莫来石纤维增强S iO2气凝胶隔热材料,研究了HF催化剂、溶剂等制备因素对溶胶-凝胶过程的影响。结果表明,加入HF可以大大加快凝胶化过程,使凝胶时间从几小时缩短至几分钟;溶剂EtOH对凝胶化过程有明显的抑制作用,凝胶时间随其用量的增加而增加;H2O对凝胶化过程的影响比较复杂,凝胶时间随其用量的增加先减后增,转折点处水硅摩尔比为5∶1;气凝胶制备过程中加入甲酰胺可以调节凝胶内部网络结构,防止干燥时由于应力不均而开裂或破裂;适宜的原料配比(摩尔比)为:TEOS∶H2O∶HF∶EtOH∶甲酰胺=1∶(4~6)∶(0.05~0.1)∶(3~6)∶(0.3~0.5)。     

纳米固载杂多酸催化合成癸酸异戊酯

采用溶胶-凝胶法制备纳米固载杂多酸催化剂H4SiW12O40/SiO2。以癸酸和异戊醇为原料,催化合成癸酸异戊酯。考察了影响酯化率的各种因素,确定了适宜的工艺条件：酸醇物质的量比为1∶1.6,催化剂用量为反应物料总质量的3%,环己烷用量为8 mL,反应时间为60 min,酯化率可达96.70%。     

乙醇对溶胶-凝胶法制备SiO_2溶胶性能的影响

以HNO3为催化剂,用正硅酸乙酯(TEOS)溶胶-凝胶工艺制备纳米多孔二氧化硅薄膜。较详细地研究了工艺参数乙醇/TEOS摩尔比对溶胶性能的影响.结果表明,随着乙醇/TEOS摩尔比的增大,溶胶粘度减小,凝胶时间变长,胶体粒径有变小趋势。     

溶胶-凝胶法制备纳米二氧化硅

本文通过溶胶一凝胶法制备纳米SiO2。考察了不同温度、pH值、催化剂对制备纳米SiO2的影响。并运用了TEN表征了纳米SiO2的粒径大小、分散度以及粒子性状，得出了制备纳米SiO2较好的工艺条件。     

大颗粒超高纯度硅溶胶的制备及其表征(英文)

采用新工艺路线制备四乙氧基硅烷（tetraethoxysilane,TEOS）,以TEOS为原料制备超纯度大颗粒硅溶胶。TEOS是烷氧基硅烷法制备甲硅烷的副产物,经过精馏提纯以后,加入盐酸或氨水催化剂,采用溶胶-凝胶法制备硅溶胶。结果表明：TEOS和硅溶胶金属杂质离子总含量都低于0.3mg/L。用盐酸催化TEOS水解制备溶胶,胶粒直径达到129nm;用氨水催化,胶粒直径达272nm。当物质的量比n（C2H5OH）/n（TEOS）=6,n（H2O）/n（TEOS）=5,搅拌速度为250 r/min,制备的硅溶胶胶粒均匀度最好。加水不搅拌,胶粒很容易发生团聚,但是,当搅拌速率高于500 r/min时,胶粒出现团聚现象。     

纳米二氧化硅溶胶粒子的制备研究

以TEOS为前驱体,氨水作为催化剂,制备了单分散纳米二氧化硅溶胶,并且探讨了反应条件对二氧化硅溶胶粒径的影响。结果表明:在保持其它条件不变的情况下,随着NH4OH/TEOS摩尔比的增大,二氧化硅溶胶的粒径也增大;随着H2O/TEOS摩尔比的逐渐增大,二氧化硅溶胶的粒径先增大后基本不变;随着EtOH/TEOS摩尔比的增大,二氧化硅溶胶的粒径减小;随着反应温度的升高,二氧化硅溶胶的粒径显著减小。     

SiO_2改性三聚氰胺氰尿酸盐无卤阻燃剂的制备

在三聚氰胺(MA)与氰尿酸(CA)反应合成三聚氰胺氰尿酸盐(MCA)过程中加入SiO2溶胶,通过调控工艺参数,制备了改性MCA复合阻燃剂。研究发现:当反应体系pH为4.0,在MA和CA反应体系的粘度为5×104mPa.s时加入SiO2溶胶,反应时间为1h,所制备的改性MCA粒径较小,产率最高,实现了SiO2和MCA的有效复合和对MCA粒径的超细控制。     

The effect of SiO_2 particle size on iron based F–T synthesis catalysts

The effect of particle size of silica, as catalyst binder, on the chemical and mechanical properties of iron based FT catalyst was studied in this work. The samples were characterized using XRD, BET, TEM, FT-IR, and H2-TPR, respectively. The attrition resistance and the FT activity were tested. Si-8–Si-15 catalysts prepared with 8–15 nm silica sol show good attrition resistance(attrition loss b 4%), especially Si-13 with an attrition loss of 1.89%. Hematite appeared in XRD patterns when silica sol above 15 nm is used. TEM micrographs show that no obvious Si O_2 particles appear when silica sol particle with size less than 8 nm was used, but Si O_2 particles coated with small ferrihydrite particles appear when silica sol above 8 nm was used. Si–O–Si vibration peak in FT-IR spectra increases with increasing silica sol size. Samples prepared with silica sol show good stability of FT reactions, and the average molecular weight of FT products increases with the increase of Si O_2 particle.     

Preparation and characterization of waterborne epoxy latexes and epoxy/(silica sol) composites

A series of waterborne epoxy latexes was synthesized, and epoxy/(silica sol) composite latexes were prepared. The effects of functional monomer methacrylic acid (MAA) and silica sol on the latex particle size, morphology, and stability were investigated. With increasing amounts of MAA, the conversion rate increased, the particle size reduced, and the viscosity of the epoxy latexes increased. The epoxy latexes had storage stability and could be stored at room temperature for more than 6 months with a solid content variation of less than 1%. For the (silica sol)‐modified waterborne epoxy latexes, the effects of preparation techniques and silica sol content on the latexes and latex films were investigated. When the silica sol content increased, the particle size of the composite latexes decreased. The morphology investigation showed that when the silica sol content increased, the uneven surface level of the latex films was increased. The increase of elemental silica on the surface was in accord with the improvement of the water resistance of the composite latex films. The heat resistance of these films was improved as well, and their overall performance was better than that of the epoxy latex films. J. VINYL ADDIT. TECHNOL., 20:57–64, 2014. © 2014 Society of Plastics Engineers     

A Novel Preparation Method for Foamed Silica Ceramics by Sol-Gel Reaction and Mechanical Foaming

A simple method for obtaining silica foam has been developed by combining sol-gel reaction and mechanical foaming without added organic pore formers, in order to reduce generation of CO₂ and harmful gases by decomposition of the organic compounds. The silica foam was prepared by mechanically foaming the silica sol and controlling the viscosity change and gelling. The gelation time of the silica sol can be varied from 10 minutes to 3 hours by changing the pH, temperature and concentration of the surfactant added as a foam stabilizer. The dried silica gel foam was calcined at 600°C then fired at 1000°C to obtain sintered silica foam. The porosity and average pore size of the silica foam was 84% and 140 m, respectively. The bending strength and gas permeability of the sintered silica foam was 2.4 MPa and 9.4 × 10^–11 m², respectively.     

Enhanced esterification of carboxylic acids with ethanol using propylsulfonic acid-functionalized natural rubber/hexagonal mesoporous silica nanocomposites

Propylsulfonic acid-functionalized natural rubber (NR)/hexagonal mesoporous silica (HMS) nanocomposites (NR/HMS-SO₃H) with different acid contents were prepared via an in situ sol–gel process, and then applied as heterogeneous acid catalysts in the esterification of model carboxylic acids and palm fatty acid distillate (PFAD) with ethanol. The NR/HMS-SO₃H composites exhibited a wormhole-like framework with enhanced wall thickness, high mesoporosity, and enhanced hydrophobicity. The NR/HMS-SO₃H composites exhibited a superior catalytic performance compared to a commercial Nafion/silica composite solid acid catalyst (SAC-13) and conventional propylsulfonic acid-functionalized HMS (HMS-SO₃H). The NR/HMS-SO₃H catalyst can be regenerated and reused in the esterification.     

芳香驱蚊微胶囊剂的制备

以脲醛树脂为壁材,使用原位聚合法制备芳香驱蚊微胶囊。考察了微胶囊结构、包埋率、粒径及其分布等影响因素。优化的缩聚反应条件是:以十二烷基硫酸钠为表面活性剂,以盐酸为酸性催化剂,催化剂分批加入,终点pH值2.0,酸化4 h,固化温度70℃,固化时间2 h,搅拌速度800 r/min,可以得到包封率为91.3%、缓释效果良好、粒径分布均匀且粒径1~10μm的流动性球型固体微胶囊。