有机硅烷共缩合制备抗紫外超疏水减反射涂层

具有超疏水自洁功能的减反射涂层对太阳能光热组件在室外长期使用上有重要的意义,可以减少减反射涂层的清洗成本,延长减反射涂层的使用寿命。利用含有甲基和乙基等疏水基团的有机硅氧烷制备具有一定孔隙率的涂层,有望实现减反射和超疏水双重性能。本研究采用四甲氧基硅烷（TMOS）和甲基三乙氧基硅烷（MTES）共缩合,并利用甲氧基三甲基硅烷（MMS）进行羟基封端,制备了可以稳定两个月以上的均一溶胶。通过控制MTES和TMOS的水解工艺条件,采用浸渍提拉法制备了在400～800nm可见光波段平均透光率为97.06%、最高透光率为98.27%、水接触角为165°的超疏水减反射涂层,提出了MTES/TMOS/MMS溶胶的共缩合反应机理。涂层经过紫外耐久测试1080h后,涂层仍具有良好的减反射性能、疏水性和抗刻划强度,表现出良好的紫外耐久性。     

超疏水超亲油玻璃纤维过滤膜的制备及其乳化水分离效率

通过溶胶-凝胶法,以MTES(甲基三乙氧基硅烷)为前驱体,在玻璃纤维(玻纤)过滤膜表面直接进行水解缩合反应,制备具有高效油水分离功能的玻纤过滤膜材料。通过扫描电子显微镜和红外光谱分析MTES处理前后玻纤过滤膜的微观形貌与表面组成的变化,并通过接触角仪测试玻纤过滤膜的接触角,采用Karl Fischer水分仪测试玻纤过滤膜的油水分离效率。结果表明:经过MTES处理后,玻纤过滤膜的微观孔隙结构不变,而纤维表面布满疏水亲油的–CH3基团和纳米凸起结构,处理后的玻纤过滤膜有超疏水超亲油性能,玻纤过滤膜对乳化水的油水分离效率可以达到96.09%。     

水分散有机硅-聚氨酯嵌段共聚物的制备与性能研究

以端羟基聚二甲基硅氧烷（PDMS）和氨烃基硅烷偶联剂（DB-912）为原料,合成了端氨烃基聚二甲基硅氧烷低聚物（NS）,并以此作为扩链剂,制备了水分散有机硅-聚氨酯嵌段共聚物（WPSUR）。考察了NS的摩尔质量与扩链剂类型对乳胶粒粒径、薄膜疏水性与耐热稳定性的影响。结果发现,随着NS摩尔质量的增加,乳液粒径增大;扩链剂类型对乳液及薄膜性能影响较大,采用NS为扩链剂制备的WPSUR,乳液呈现较高的表现黏度,薄膜吸水率较低、对水的表面接触角达103°,疏水性较好;与引入小分子硅烷偶联剂的体系相比,体系中有机硅链段含量大大增加,耐热稳定性良好;水分散液均呈现良好的离心稳定性,乳液具有良好的耐高温性能与冰冻-解冻稳定性。     

氟改性硅溶胶的制备及性能

[目的]具有特殊润湿性的透明疏水材料在自清洁、金属防腐、微流体运输、防结冰、油水分离等领域具有广阔的应用前景。[方法]以正硅酸乙酯(TEOS)作为前驱体,十七氟硅烷偶联剂(FAS)和环氧硅烷偶联剂(KH560)为改性剂,采用两步法制备了氟改性硅溶胶,并将其涂覆在载玻片和聚丙烯(PP)纤维织物表面,制成了疏水材料。采用接触角测量仪、傅里叶变换红外光谱仪和扫描电镜对其进行表征,考察了改性剂的用量、水解时乙醇的比例及稀释倍数对材料疏水性能的影响。[结果]在乙醇与水的质量比为3∶2,偶联剂总用量为3%(质量分数),FAS与KH560的质量比为1∶1的条件下制备的硅溶胶稀释10倍后可以在载玻片和织物表面形成致密的涂层,它们对水的接触角分别达到了112°和153°,且具有优异的自清洁性能。[结论]通过溶胶-凝胶法,利用TEOS与FAS共水解的方式,可以获得性能优异的疏水材料。     

有机硅接枝三聚氰胺树脂的合成与表面性能

以三聚氰胺和多聚甲醛为原料、羟基封端聚二甲基硅氧烷（PDMS-OH）为改性剂，制得一系列改性三聚氰胺树脂（MF-PDMS）。研究了反应介质、PDMS-OH用量对MF-PDMS树脂性能的影响，以及与树脂固化后的MF-PDMS材料性能的关系。采用红外光谱（FT-IR）、固体核磁共振氢谱（1H NMR）、X射线光电子能谱（XPS）、扫描电镜-能谱（SEM-EDS）表征了MF-PDMS材料的结构、表面化学组成，采用接触角测定仪、浸泡法分别测试了材料的接触角、吸水性，采用热重（TG）测试了对材料的热稳定性。结果表明：在二甲基乙酰胺（DMAc）反应介质中，PDMS-OH与三聚氰胺、甲醛可一步合成MF-PDMS树脂，接枝共聚的PDMS-OH可高效的提高MF-PDMS材料的疏水性能和热稳定性，当PDMS-OH的摩尔分数为1.0%（以三聚氰胺物质的量计）时材料的水接触角为91.81°、表面自由能降至28.1 mN/m、吸水质量分数降至2.83%、400 ℃时的残留率为58.03%、700 ℃时的残留率为16.60%。     

超疏水PET织物的制备及其抗菌性能

纺织物表面的超疏水特性将赋予其优异的自清洁性能。以PET无纺布为基材,探索了利用溶胶-凝胶法在预处理后的PET织物表面构筑具有微纳结构的超疏水涂层的方法;并利用扫描电镜（SEM）、接触角测量仪表征了改性PET织物表面的微观结构和润湿性。进一步地,分别以大肠杆菌和金黄色葡萄球菌为试验菌株,通过细菌转移法和抑菌圈法评价与分析了改性PET织物表面的抗菌性能。研究表明：利用改进的Stöber溶胶-凝胶过程能够在经碱减量法预处理的PET表面原位形成SiO₂纳米粒子;再用含疏水性长链的十二烷基硅烷对这一表面进行改性,并经过表面热处理,就能够成功地在PET织物表面构筑多层次的微/纳结构,从而制得表面具有超疏水特性的PET织物,其接触角可达到163°。这一超疏水PET织物能够抑制细菌在其表面的生长繁殖,表现出了明显的抗菌特性。     

有机–无机杂化超疏水涂层的制备

采用溶胶-凝胶法,以正硅酸乙酯(TEOS)和甲基三乙氧基硅烷(MTES)为前驱体、硅丙树脂为成膜物质,制备了有机-无机杂化超疏水材料.在对用该材料获得超疏水涂层的研究中,考察了硅丙树脂的含量,比值n(MTES)/n(TEOS)、n(C_2H_5OH)/n(TEOS)和n(NH_3·H_2O)/n(TEOS)对涂层性能的影响.测试结果表明,当硅丙树脂加入量占总物料量的25%(质量分数),摩尔比n(TEOS)∶n(MTES)∶n(C_2H_5OH)∶n(NH_3·H_2O)为1∶4∶30∶10时,涂层具有良好的疏水性和均匀的外观结构,涂层静态水接触角可达156°.     

基于不锈钢网超疏水涂层的制备及其油水分离应用研究

通过凝胶-溶胶法制备纳米二氧化硅粒子,并使用二甲基二乙氧基硅烷进行疏水改性。采用直接浸泡法在100目不锈钢网表面成功构造出了纳米级粗糙结构。并研究了浸泡次数和老化时间对样品表面润湿性的影响,同时用自制的油水分离装置进行油水分离实验。结果表明:样品对水的接触角达155°,油水分离效率达92%。     

聚硅氧烷包覆改性聚磷酸铵及其阻燃聚乙烯性能的研究

分别以二甲基二乙氧基硅烷（DMDES）、甲基三乙氧基硅烷（MTES）、苯基三甲氧基硅烷（PTMS）3种硅氧烷与正硅酸四乙酯（TEOS）共同作为前驱体,采用溶胶-凝胶工艺对聚磷酸铵（APP）进行微胶囊化包覆改性,分别制备得到改性聚磷酸铵APP/DMDES、APP/MTES和APP/PTMS,以改善其阻燃性、热稳定性和疏水性。通过傅里叶红外光谱、水接触角、扫描电子显微镜、能谱仪以及热失重分析等测试与表征手段,对3种不同聚硅氧烷包覆改性聚磷酸铵（MAPP）进行了对比研究,并研究了MAPP对低密度聚乙烯（PE-LD）阻燃性能、力学性能和热性能的影响。结果表明,在合适的工艺条件下,均可以制备得到聚硅氧烷包覆改性聚磷酸铵;较改性前的APP,改性聚磷酸铵的疏水性和热稳定性均显著提高;在PE-LD/APP/PTMS/季戊四醇（PER）/三聚氰胺（MEL）的质量比为65/18.7/11.7/4.6时,PELD复合材料的综合性能最好,极限氧指数为26.6%,高于包覆前APP的23.3%,达到UL 94 V-0级别,且拉伸性能最高,为12.84 MPa。     

超疏水防紫外双功能水性织物涂层的制备及性能研究

利用乳液缩聚法制备芯材为氟硅烷（ FAS13）壁材接枝紫外吸收剂的二氧化硅微胶囊,将其与有机硅树脂乳液共混,涂覆于棉织物表面形成超疏水防紫外织物涂层。通过扫描电镜和透射电镜观察微胶囊的形态和粒径,并对涂层的水接触角和防紫外性能进行了测试,同时测试了涂层的耐老化、耐磨损、耐高温以及耐酸碱性。结果表明：织物涂层中微胶囊最佳含量为 45%（其中内含 6%紫外吸收剂）,由此制备的涂层表面水接触角可达到 150°以上,并且具有较好的耐老化、耐高温、耐酸碱腐蚀、耐磨损等性能;同时该织物涂层具有优异的防紫外性,紫外线防护系数（UPF）可以达到 111.2。     

Facile fabrication of robust superhydrophobic cotton fabrics modified by polysiloxane nanowires for oil/water separation

The removal of oil and organic pollutants from water is highly desired due to increasing industrial oil-contaminated wastewater, as well as frequent oil spill accidents. In this paper, superhydrophobic and superoleophilic fabrics were facilely fabricated for oil/water separation application via in situ growth of polysiloxane nanowires on cotton fabrics. The polysiloxane nanowires were immobilized on the cotton fabrics through a self-assembly process of alkylsilane on the microfibers of fabrics. The combination of the hierarchical structure and the low-surface-energy polysiloxane nanowires greatly contributed to the superhydrophobicity of the fabrics. Furthermore, the superhydrophobicity remained even after they were exposed to different chemicals for 72 h and strong ultraviolet irradiation and repeated abrasion, indicating excellent stability. More importantly, the as-prepared cotton fabrics were successfully used for separating various oil/water mixtures by a solely gravity-driven process with high separation efficiency and desirable durability. The cotton fabrics are commercially available, low-cost, and environmentally friendly materials, and thus such superhydrophobic and superoleophilic cotton fabrics could be very attractive for oil/water separation and oil spill cleanup when high flexibility, strength, and chemical resistance are taken into account.     

Encapsulation of flexible organic light emitting diodes by UV-cure epoxy siloxane

In this research, a silicon additive was synthesized by reaction of the hydroxyl terminated poly-dimethyl siloxane (PDMS-OH) with 3-glycidoxy propyl tri-methoxy silane (TMS-epoxy). The synthesized silicon additive characterized and evaluated to use as a curing agent for preparing high-performance and impermeable epoxy resin for encapsulation of flexible optoelectronic devices such as thin film photovoltaics and polymer light-emitting diodes to protect them against water penetration and increase their lifespan. The synthesized additive was characterized by FTIR, NMR, and elemental analysis. Thermal properties of the UV curable resin were investigated by using DSC and DMTA. The prepared UV cure epoxy resin exhibited an appropriate melting temperature (56.19 °C). Contact angle test, SEM, and calcium test was used to investigate the properties of UV-cured coating resin. The water contact angle of the cured prepared resin film showed good hydrophobicity. The SEM results confirmed the uniformity of cured film and UV cure resin dispersion. Transparency and flexibility of the cured film to encapsulate the flexible light emitting diodes are acceptable. The permeability of cured film to water vapor was evaluated by calcium test, which shows the cured film suitability to encapsulate the FOLED. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 48033.     

Fabrication of durable superhydrophobic and superoleophilic cotton fabric with fluorinated silica sol via sol–gel process

Superhydrophobic and superoleophilic cotton fabric was successfully prepared with fluorinated silica sol via a facile sol–gel method. A fluorinated polymeric sol–gel precursor (PHFBMA-MTS) was synthesized via free-radical polymerization by using hexafluorobutyl methacrylate (HFBMA) in the presence of (3-mercaptopropyl)trimethoxysilane (MTS) as the chain transfer agent, which led to the formation of fluoropolymer with alkoxysilane end groups. Then the fluorinated silica sol was prepared by introducing PHFBMA-MTS as the co-precursor of tetraethylorthosilicate (TEOS) in the sol–gel process with ammonium hydroxide as the catalyst, which was then used to fabricate superhydrophobic and superoleophilic fabric coatings through a simple dip-coating method. The coated fabrics showed superhydrophobic property with a high water contact angle of 154.1° and superoleophilic property with an oil contact angle of 0°. Moreover, the coated fabrics still kept superhydrophobicity even after ultrasonic treatment, as well as for organic solutions, acidic solutions. Thus, the coated fabrics were successfully applied to separate oil–water mixture with separation efficiency up to 99.8%. More importantly, the separation efficiency had no significant change after 20 cycles of oil–water separation. These present a simple, low-cost, and durable approach to achieve industrialized application of coated fabrics in oil–water separation. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47005.     

Preparation and oil–water separation evaluations of polypropylene/low‐melt‐point polyester composites reinforced by thermal bonding and one‐step solution immersion

Nonwoven fabrics have been fabricated for oil–water separation, but simplifying the manufacturing processes is still a challenge. In this work, a facile and easily scaled up approach based on thermal bonding and one‐step solution immersion has been successfully developed to prepare nonwoven fabrics with high separation efficiency and flux of oil. Here, polypropylene (PP) and low‐melt‐point polyester (LPET) fibers with a unique sheath–core structure are employed to form PP/LPET nonwoven fabrics. Thermal bonding by hot press and hydrophobic treatment with 1H,1H,2H,2H‐perfluorodecyl‐1‐thiol (PFDT) are used to manufacture oil–water separation nonwoven fabrics. Effects of the ratio of LPET fibers and the concentration of PFDT are discussed in terms of mechanical properties, morphology, surface chemical composition, water contact angle and performance of oil–water separation and flux of the nonwoven fabrics. The results show that the strength of the nonwoven fabrics gradually increases with increasing ratio of LPET fibers. After immersion in PFDT, the nonwoven fabrics show high hydrophobicity with a water contact angle of 143°. They can be used to separate oil–water mixtures. The separation efficiency is 97–99% and the oil flux is 62 364.92 L m^?2 h^?1. This study provides a new prospect for simple introduction of a hydrophobic agent on a nonwoven fabric to achieve various functional oil–water separation materials. © 2020 Society of Chemical Industry     

耐腐蚀超疏水超亲油不锈钢网的制备及其在油水分离过程中的应用

以不锈钢网为基底,通过化学刻蚀法制备微米级粗糙表面,通过一步浸泡法将st9ber法制得的疏水亲油纳米Si O2颗粒沉积到粗糙的不锈钢网表面,制备了具有微纳二级粗糙结构的超疏水超亲油不锈钢网。利用扫描电子显微镜(SEM)、傅里叶变换红外光谱仪(FT-IR)和接触角测量仪(CA)表征了超疏水超亲油不锈钢网的表面形貌、化学组成和润湿性能,并将其用于油水分离过程中。结果表明,疏水亲油纳米Si O2颗粒成功的沉积到不锈钢网表面;水滴在超疏水超亲油不锈钢网上的接触角最大为151°,煤油的接触角为0°;制备的超疏水超亲油不锈钢网不仅能高效的分离不同种类油和水的混合物,还能高效的分离油和腐蚀性液体(强酸或强碱水溶液)的混合物,其耐腐蚀特性可满足复杂环境下的油水分离要求。     

羟基硅油改性HTPB型聚氨酯的合成与性能

以端羟基聚丁二烯(HTPB)为软段、异佛尔酮二异氰酸酯(IPDI)和3,3′-二氯-4,4′-二苯基甲烷二胺(MOCA)为硬段、羟基硅油(PDMS-OH)为改性剂和硅烷偶联剂(DB-550)为交联剂,合成了硅氧烷封端的HTPB型聚氨酯(PU)。采用L9(34)正交试验法优选出最佳工艺条件,探讨了PDMS-OH用量对改性PU的力学性能、耐水性能的影响,并对改性PU的耐老化性能进行了测定。结果表明:加入DB-550后,可以降低相分离程度;当R=2.5、w(HO-PDMS)=9%和n(MOCA):n(DB-550)=9:1时,采用直接法合成的改性PU具有优异的力学性能,并且其吸水率较低、耐老化性能较好。     

阳离子氟代聚丙烯酸酯乳液的制备及应用

以(NH4)2S2O8作引发剂,阳、非离子表面活性剂作乳化剂,将甲基丙烯酸十二氟庚酯(RfAA)、丙烯酸丁酯(BA)、甲基丙烯酸二甲氨乙酯(DM)以及丙烯酸羟丙酯(HPAA)进行乳液聚合,制得了一种稳定的阳离子氟代聚丙烯酸酯乳液(PCFBA)。用红外光谱(IR)、核磁共振氢谱(1HNMR)对PCFBA主组分的结构进行了表征。用扫描电镜SEM、接触角测量仪、电脑测控柔软度仪等研究了PCFBA在棉纤维织物表面的成膜性及应用性能。结果表明,PCFBA可在纤维表面形成相对均匀的疏水膜,该膜附着在纤维表面,能使整理后棉织物与水的接触角达到134.5°、静态吸水时间超过6 h;当PCFBA用量从0.3 g/100 mL H2O增大到1 g/100 mL H2O时,水在其整理的棉纤维织物表面的接触角从128.2°增大到134.5°,而棉织物的白度则由85.44°略降至84.40°。     

Covalent surface functionalization of nonwoven fabrics with controlled hydrophobicity,water absorption,and pH regulation properties

A modular method for functionalization of nonwoven fabrics was developed using a two-step process. In the first step, the fabrics were grafted with a linker molecule, 10-undecenoyl chloride, via esterification, followed by attachment of a functional material under UV irradiation. Perfluorodecanethiol and 3-mercaptopropionic acid (MPA) were connected to the linker-modified fabrics using thiol-ene click chemistry. Perfluorodecanethiol modified fabrics exhibited hydrophobicity with water contact angle of about 140° while MPA-modified fabrics were able to lower the pH of a solution by about 1.6. We additionally demonstrated the possibility to connect functional polymers to the linker-modified fabrics by radical graft polymerization of acrylic acid; this produced a thin layer of the polymer on the surface of the fabric. Fabrics modified with poly(acrylic acid) exhibited increased hydrophilicity with water contact angle of 0° for both cotton and viscose-polyester fabrics, while the water absorption capability for polypropylene fabrics increased from about 50 to 1200%.     

Microwave‐assisted synthesis of silver nanoparticles on cotton fabric modified with 3‐aminopropyltrimethoxysilane

In this study, silver nanoparticles were synthesized on cotton fabric modified with 3‐aminopropyltrimethoxysilane (APTMS) using sodium citrate as a reducing/stabilizing agent by microwave‐assisted process. The presence of a highly oriented amino‐terminated self‐assembled monolayer and formation of APTMS was demonstrated by an X‐ray photoelectron spectroscopy (XPS) analysis. The silver‐coated cotton fabrics were examined by scanning electron microscopy (SEM) and energy dispersive X‐ray (EDX). UV protection, antistatic, and hydrophobic properties were also evaluated. The results show that silver‐coated fabric modified with APTMS possesses excellent antistatic, UV protection with ultraviolet protection factor (UPF) of 396.5 and superhydrophobic properties with contact angle of 153.2°. APTMS pretreatment improves the adhesive strength between silver coatings and cotton fabric. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 130: 3862–3868, 2013     

Synthesis and characterization of poly(methyl methacrylate)/polysiloxane composites and their coating properties

A series of poly(methyl methacrylate) (PMMA)/polysiloxane composites and their coatings were prepared as designed. A copolymer (PMMAVTEOS) containing methyl methacrylate (MMA) and vinyltriethoxysilane (VTEOS) was prepared by free radical polymerization and then condensed with methyl triethoxysilane (MTES) to fabricate PMMA/polysiloxane composites; their corresponding coatings were obtained via a curing process in an oven (at 75 °C). The polymers were characterized by gel permeation chromatography and Fourier transform infrared spectroscopy. The surface property, hardness, water contact angle, thermal stability, and optical property of the coatings were investigated by scanning electron microscopy, pencil hardness testing, water contact angle testing, thermogravimetric analysis, and ultraviolet–visible spectroscopy, respectively. The results showed that, after addition of MMA, the pencil hardness of the coatings was reduced from 6H to 2H and the thermal stability decreased from 365 to 314 °C. However, it increased the flexibility and adhesion properties (the water contact angle increased from 94.7° to 102.1°). The transparent PMMA/polysiloxane coatings showed excellent scratch resistance, a smooth surface, high thermal stability, and a strong adhesion property. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46358.