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双语推荐：四甲氧基硅烷

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以3-（2，3-环氧丙氧）丙基三甲氧基硅烷（KH-560）为单体，在异丙醇为溶剂、四甲基氢氧化铵（TMAH）为催化剂的体系中一步水解缩合制备出笼型缩水甘油基倍半硅氧烷（G-POSS）。采用傅立叶变换红外光谱、核磁共振波谱及基质辅助激光解吸飞行时间质谱等手段对产物进行了分析和表征。结果表明，成功地合成了高纯度的笼型十缩水甘油基倍半硅氧烷（T10）。
Cage glydidyl polyhedral oligomeric silsesquioxanes(G-POSS) was prepared by one-step hydrolytic condensation from 3-(2,3-epoxypropoxy) propytrimethoxysilane(KH-560) in the system of isopropyl alcohol and tetramethylammonium hydroxide (TMAH). G-POSS was characterized using FTIR,1H-NMR and MALDI-TOF-MS. The results show that highly purified cage decaglycidyl polyhedral oligomeric silsesquioxanes is successfully prepared.

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采用1,1,3,3-四甲基二硅氧烷和烯丙基缩水甘油醚为原料,以氯铂酸为催化剂,以四氢呋喃为溶剂,在温和条件下经硅氢加成合成了1,3-二[3-(环氧乙基甲氧基)丙基]-1,1,3,3-四甲基二硅氧烷。产物经红外光谱、核磁共振氢谱和质谱表征。考查了催化剂用量、反应温度、溶剂、原料摩尔比和反应时间等因素对反应转化率的影响。当1,1,3,3-四甲基二硅氧烷和烯丙基缩水甘油醚的摩尔比为1:3,催化剂用量为1,1,3,3-四甲基二硅氧烷质量的0.016%,在0-10℃下于四氢呋喃溶剂中搅拌反应12 h,产物摩尔转化率可达89.5%。
1,3-bis-(3-oxiranylmethoxy-propyl)-1,1,3,3-tetramethyl-disiloxane was synthesized in mild condition via hydrosilylation reaction between 1,1,3,3-tetramethyl-disiloxane and allyl glycidyl ether. Tetrahydrofuran was used as solvent and chloroplatinic acid as catalyst. The products was characterized by IR, 1H NMR and the mass spectrometry. The effects of the reaction conditions including the catalyst dosage, the reaction temperature, the solvent, the molar ratio of reactants and the reaction time on conversion rates were investigated. The molar conversion rate could reach 89.5%when the reaction conditions were as followings:the molar ratio of 1,1,3,3-tetramethyl-disiloxan to allyl glycidyl ether was 1:3, the amount of the catalyst was 0.016%based on the weight of 1,1,3,3-tetramethyl-disiloxan, and the reaction was stirred at 0-10℃ for 12 h in tetrahydrofuran.

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以甲基苯基二甲氧基硅烷为原料,在盐酸催化下,在过量水中进行水解缩聚反应,得到端羟基聚甲基苯基硅氧烷。采用红外光谱、核磁共振谱和飞行时间质谱对产物进行了表征,并探讨了水解缩聚机理。结果表明,产物是以四聚体为主的端羟基聚甲基苯基硅氧烷,平均相对分子质量为862。
Hydroxyl terminated polymethylphenylsiloxane was prepared via hydrolysis /condensation of di-methoxymethylphenylsilane in water with hydrochloric acid as a catalyst .The structure of the product was characterized by FTIR、 NMR and MADLI-TOF/TOF MS, and the behavior of hydrolysis and condensation was proposed .Result shows that the product consists of linear hydroxyl terminated polymethylphenylsiloxane oligomers with an average molecular weight of 862 and tetramer is the major component .

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以四甲氧基硅烷、氯苯、溴苯、镁粉为原料,在四氢呋喃与甲苯组成的混合溶液中进行格氏反应,得到二苯基二甲氧基硅烷。研究了反应溶剂种类及其配比、氯苯与溴苯的配比对产品收率的影响。结果表明,较佳反应条件为,甲苯与四氢呋喃的质量比为4∶1,氯苯与溴苯的量之比为95∶5,此时得到的产品收率84%,纯度98%,氯的质量分数小于10×10-6,未检出多氯联苯。
Diphenyl dimethoxy silane was prepared with tetramethoxysilane,chlorobenzene,bromo-benzene,and magnesium as the raw materials,in mixed solution of THF and toluene by Grignard reaction. The effect of kinds and the ratio of the solvents,the ratio of chlorobenzene and bromobenzene on the product yield was studied.Results show that when the mass ratio of toluene to tetrahydrofuran was 4∶1 ,ratio of chloro-benzene and bromobenzene was 95∶5 ,the obtained product was with yield of 84%and purity of 98%,and the mass fraction of chlorine was less than 10 ×10 -6 .No PCBs were detected.

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以苯基三甲氧基硅烷(Phenyltrimethoxysilane,PTMS)、1,1,3,3-四甲基二硅氧烷(1,1,3,3-Tetramethyldisiloxane,HTMS)和六甲基二硅氧烷(Hexamethyldisiloxane,HMDSO)为主要原料,酸性阳离子交换树脂为催化剂,采用水解缩聚的方法制备了苯基含氢硅树脂(Hydrogen containing phenyl silicone resin,PHMT树脂),采用傅里叶转换红外线光谱(Fourier Transform Infrared Spectroscopy,FTIS)和核磁共振氢谱(1H Nuclear Magnetic Resonance Spectroscopy,1HNMR)对其结构进行了表征,并对其制备工艺、固化性能进行了研究.结果表明,甲氧基的水解程度达99.9%,但羟基缩聚不完全,其残留量约为质量分数0.57%.采用含氢量为体积分数0.37%,黏度为722 mPa·s的苯基含氢硅树脂为交联剂,其固化物机械性能较好.
Hydrogen containing phenyl silicone resin was prepared through hydrolysis polycondensation process , by using phenyltrimethoxyl silane , tetramethyldisiloxane and hexamethyl disiloxane as start ma-terial , and acidic cation exchange resin as catlyst .The structure of the polymer was characterized through Fourier Transform Infrared Spectroscopy ( FTIS ) and 1H Nuclear Magnetic Resonance Spectroscopy (1HNMR), and the preparation process and the curing properties were also studied .The results showed that the hydrolysis extent of the methoxyl reached 99.9%, but the polycondensation of Si-OH was not complete, and the residue was about 0.57%.The cured polymer had better mechnical performance when used the silicone resin with moderate hydrogen content , 0.37%, and with moderate viscosity , 722 mPa· s.

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苯基三甲氧基硅烷在四甲基氢氧化铵催化下经有限水解-缩聚-重排制备笼形八苯基硅倍半氧烷,反应时间短,产率高.采用透射电镜(TEM)、傅立叶红外光谱(FT-IR)、29Si核磁共振光谱(29Si NMR)、1H核磁共振光谱(1H NMR)、13C核磁共振光谱(13C NMR)、元素分析和热分析(TGA)等对笼形八苯基硅倍半氧烷的形貌、结构和热性能进行研究.结果表明:笼形八苯基硅倍半氧烷是不规则长方体纳米颗粒,粒径小于400 nm,热稳定性高,在N2和空气中的初始分解温度(失重5%)均大于450℃.同时,对中间产物进行红外表征以推测反应机理.
Octaphenylsilesquioxane (OPS) with high yield was synthesized via limited-hydrolytic-polycon-densation-rearrangement of phenyltrimethoxysilane (PTMS) using tetramethylammonium as the catalyst in short reaction time. The morphology, structure and thermal properties of the products were characterized by TEM, FT-IR, 29Si NMR, 1H NMR, 13C NMR, elemental analysis and TGA. The results showed that octaphenyl-silesquioxane was regular rectangular nanoparticle with size less than 400 nm and high thermal stability, whose thermal decomposition temperature (weight loss at 5%) was more than 450 ℃ in both N2 and air. The intermediate product was also determined by FT-IR in order to infer the synthesis mechanism.

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通过溶胶-凝胶法以四甲氧基硅烷(TMOS)和甲基三甲氧基硅烷(MTMS)作为混合的前体,聚乙二醇(PEG)为致孔剂,制备了具有贯通孔道结构的双孔硅胶整体柱,采用3-巯基丙基三甲氧基硅烷(MTPMS)对硅胶整体柱表面进行巯基化修饰后,分别将金、银纳米粒子组装在整体柱材料表面。利用透射电子显微镜(TEM)、紫外-可见吸收光谱(UV-Vis)、扫描电子显微镜(SEM)对金、银纳米粒子形貌、吸收光谱及组装金、银纳米粒子前后整体柱的形貌进行了表征。以对巯基苯胺(PATP)为探针分子,分别采用波长为633和532nm的激发光作为激发光源,研究金和银纳米粒子修饰的硅胶整体柱的在柱表面增强拉曼光谱(SERS)性能。结果表明,该基底呈现出很强的SERS活性,结合整体柱的分离富集优势将在食品/环境领域现场痕量检测方面具有广泛的应用前景。
A novel silica monolith modified with Ag/Au nanoparticles was prepared for the on-column surface enhanced Raman spectroscopy (SERS ) . The bare monolithic silica column was prepared from in-situ co-condensation of tetraethoxysilane (TMOS)andmethyltrimethoxysilane(MTMS)inthepresenceofpolyethyleneglycol(PEG)viaasol-gelprocessinthecapil-lary ,and was chemically modified with (3-mercaptopropyl) trimethoxysilane (MTPMS) ,followed by immobilization of Ag/Au nanoparticles .Transmission electron microscopy (TEM) and UV-Vis spectrometer were used to collect the TEM images and the extinction spectra of the nanoparticles colloid ,respectively .Scanning electron microscope (SEM ) was utilized to record the mor-phology of the silica monolith .The authros used p-aminothiophenol (PATP) as a probing molecule ,and the SERS effect was in-vestigated on Au/Ag nanoparticle-modified silica monolith under the excitation line of 633 and 532 nm ,respectively .It is conclu-ded that nanoparticle-modified silica

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利用溶胶-凝胶技术，以正硅酸四乙酯、3-叠氮丙基三乙氧基硅烷为前驱体，氨水为催化剂制备光固化二氧化硅溶胶，以十六烷基三甲氧基硅烷为拒水剂对棉织物进行拒水整理。先浸轧光固化二氧化硅溶胶，再浸渍烷烃硅氧烷，无需焙烘，通过紫外光照直接赋予织物拒水性能。采用扫描电镜、X射线光电子能谱仪对整理后的棉织物进行测试。结果表明，光固化二氧化硅溶胶沉积在织物表面，提高了棉织物的粗糙度。接触角测试表明，棉织物对水接触角(5μL)达到155°；整理后的棉织物经30次皂洗后，与水的接触角仍大于135°。
The light curing silica sol was prepared by sol- gel technology using tetraethylorthosilicate (TEOS) and 3- azidopropyltriethoxysilane as precursor, ammonia as catalyst, which was applied in water repel?lence on cotton fabrics with hydrophobic additives hexadecyltrimethoxysilane (HDTMS) as additive. The water repel ence property of fabric was endowed by dip- padding the light curing silica sol, then dipping into alkane siloxane, and then was exposed to UV light without curing. The treated cotton fabrics were characterized by scanning electron microscopy (SEM) and X- ray photoelectron spectroscopy (XPS). The results showed that the light curing silica sol nanoparticles were coated on the cotton fiber surface and increased the surface roughness. Contact angle results demonstrated that the water contact angle of the treated cotton fabric was 155° for 5μL and was stil greater than 135° after 30 times soaping.

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分别以衣康酸（ITA）、马来酸酐（MAH）和甲基丙烯酸缩水甘油酯（GMA）为功能单体，采用预乳化半连续工艺通过种子乳液聚合方法成功合成了表层功能化的聚二甲基硅氧烷/聚甲基丙烯酸甲酯（PDMS/PMMA）核壳乳胶粒子（~320 nm）。PDMS核乳胶粒子以八甲基环四硅氧烷（D 4）和四甲基四乙烯基环四硅氧烷（VD 4）为单体、甲基三乙氧基硅烷（MTES）为交联剂构建而成，实验研究了反应时间、乳化剂和催化剂用量、单体D 4与VD 4比例对聚合体系的影响，并确定了PDMS核乳胶粒子合成最佳工艺。通过激光粒度分析仪、傅里叶变换红外光谱仪、透射电子显微镜等分析表明：当反应时间为10 h、乳化剂用量为核单体总量的5.3%、催化剂用量为核单体总量的5.3%、核单体比D 4∶VD 4=4∶1时，核单体转化率接近85%，PDMS核乳胶粒子尺寸在290 nm左右。
In this paper, the polydimethyl siloxane/polymethyl methacrylate(PDMS/PMMA)core-shell latex particles (-320 nm)respectively with itaconic acid(ITA),maleic anhydride(MAH)and glycidyl methacrylate(GMA) as functional monomer in surface layer were successfully synthesized employing pre-emulsification semi-continuous process by seeded emulsion polymerization method. Octamethyl cyclotetrasiloxane(D 4 )and Tetravinyl tetramethyl cyelotetrasiloxane as the main monomer were compounded to form PDMS core latex particles with methyl triethoxysilane(MTES)as cross-linking agent. The effects of the reaction time, surfactant and catalyst concentration, and the ratio of D 4 and VD 4 on the polymerization system were studied, and the optimal synthesizing process of PDMS core latex particles was defined.By laser particle size analyzer, Fourier transform infrared spectrometer and transmission electron microscopy analysis showed that the core monomer conversion was nearly 85%and PDMS latex particle size wa

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以钛酸四正丁酯、甲基三乙氧基硅烷、二甲基二乙氧基硅烷、甲基苯基二甲氧基硅烷为原料,乙酰丙酮(acac)为螯合剂、盐酸为催化剂、乙醇为溶剂,利用溶胶-凝胶法、控制n(Ti)∶n(Si)=0.1~0.5,50℃水解温度下制备了含钛硅树脂,钛的引入使得杂化硅树脂在不使用催化剂和室温固化剂的情况下,140℃3d实现固化。通过涂层外观分析、光学显微镜、扫描电镜、紫外-可见吸收光谱、傅里叶变换红外光谱、变温傅里叶变换红外光谱、热重进行了表征。结果表明成功合成了含Si—O—Ti共价键的杂化硅树脂;当n(acac)/n(Ti)=0.3时,含钛硅树脂预聚物的储存稳定性较好;R/(Si+Ti)≥1.36时,能制备表面光滑的硅树脂;含钛杂化硅树脂具有较好的耐热性且其热性能随钛含量的增大而提高。
In this paper,a kind of titanium-containing hydrid silicone resin was prepared by the hydrolysis-con-densation of tetra-n-butyltitanate,methyltriethoxysilane,dimethyldiethoxylsilane and methylphenyldimethox-ysilane through sol-gel method in ethanol system,using hydrochloric acid as catalyst,acetylacetone as comple-xing agent,hydrolysis temperature 50 ℃,and n (Ti)∶n (Si)=0.1-0.5.The curing condition was 140 ℃ for 3 d. The appearance and structure of titanium-containing hybrid silicone resin was characterized by optical micro-scope,scanning electron microscope (SEM),energy dispersive spectroscopy (EDS),ultraviolet and visible spectroscopy (UV-Vis),Fourier transform infrared spectroscopy (FT-IR )and thermal gravimetric analysis (TGA).The results indicate that,titanium-containing hybrid silicone resin consists of Ti—O—Si covalent bond,when n (acac)/n (Ti)=0.3,the storage stability was well,and when R/(Si+Ti)≥1.36,the resin had a smooth surface without cracks.The introductio

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