Synthesis and application of water resistance and endurance silane coupling agents

耐水耐久硅烷偶联剂的合成及应用

• 批准号: 13470406
• 负责人: TERANAKA Toshio
• 金额: $ 9.34万
• 依托单位: Kanagawa Dental College
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (B)
• 财政年份: 2001
• 资助国家: 日本
• 起止时间: 2001 至 2003
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-13470406/
• 关键词: surface modification; silane coupling agent; coupling-layer; hydrolysis; adhesion; water resistance; resin composite; ceramics

The cause of deterioration of the mechanical properties of composites is attributed to the hydrolysis of the silane-coupling layer between the inorganic silica filler, and the organic base resin. In order to improve the endurance of dental composites against hydrolysis, we have synthesized and studied silane coupling agents.Seven experimental composites were prepared, containing fillers, which were modified with either 3-methacryloyloxypropyltrimethoxysilane (3-MPS) or a mixture of 3-MPS and the hydrophobic fluoroalkyltrimethoxysilanes. They were subjected to water immersion for 1,800 days and the Thermal Cycling Test for 30,000 cycles. The composite specimen containing filler modified with a mixture of 3-MPS and methacryloyloxypropyltrimethoxysilane showed no significant on tensile strength. In contrast -MPS modified filler containing composite demonstrated significant decrease after water immersion period and thermal stress.To improve further water resistance of the polysiloxane laye … More r at the silica/resin interface, a mixture of 3-MPS and novel silane coupling agents (MAnbF, n=5,7,9,1) with a hydrophobic fluoroalkyl and methaclyloyl group (i. e. 3{[1'-(perfluoro-5-mathylhexy) methyl-2'-(methacryloyloxy9] ethoxy }propil-trimethoxysilane (MA7bF))were synthesized. The concentration of each silane solution was adjusted with ethanol at 2 mass%, at various weight ratios of MAnbF 10, 20, 30, 50, 70 and 100% to 3-MPS. The tensile bond strength of the resin composites were measured, as well the contact angles of resin monomer mixture to glass plates modified with each silane. MA5bF formed a coupling layer with high bond strength and high water resistance at the silica/resin interface in all concentrations studied. MA7bF, MA9bF and MA11bF formed these layers at concentrations within 10-30%.From the results obtained in this study, it was suggested that the surface modification of the silica with a MA5bF or a mixture of 3-MPS and nonafluorohexyltrimethoxysilane increase the water endurance of resin composite. Less

复合材料力学性能恶化的原因是无机硅填料与有机基树脂之间的硅烷偶联层的水解。为了提高牙科复合材料的抗水解能力，我们合成并研究了硅烷偶联剂。用3-甲基丙烯酰氧基丙基三甲氧基硅烷（3-MPS）或3-MPS与疏水性氟烷基三甲氧基硅烷的混合物进行改性，制备了七种实验复合材料。他们接受了1800天的水浸泡和30000次的热循环测试。用3-MPS和甲基丙烯酰氧基丙基三甲氧基硅烷混合改性的填料对复合试样的拉伸强度无显著影响。相比之下，含有复合材料的-MPS改性填料在浸水时间和热应力后表现出明显的降低。为了进一步提高聚硅氧烷层在硅树脂界面上的耐水性，合成了3- mps和新型硅烷偶联剂（MAnbF, n=5,7,9,1）与疏水性氟烷基和甲基酰基(即3{[1'-（全氟-5-mathylhexy）甲基-2'-（甲基丙烯酰氧基9]乙氧基}丙烯-三甲氧基硅烷（MA7bF））的混合物。以2质量%的乙醇调节硅烷溶液的浓度，MAnbF的质量比分别为10、20、30、50、70和100%。测定了树脂复合材料的拉伸结合强度，以及树脂单体混合物与各硅烷改性玻璃板的接触角。MA5bF在所有浓度下均在硅胶/树脂界面形成了高结合强度和高耐水性的耦合层。MA7bF、MA9bF和MA11bF的浓度在10 ~ 30%之间。本研究结果表明，用MA5bF或3-MPS与非氟己基三甲氧基硅烷的混合物对二氧化硅进行表面改性可以提高树脂复合材料的耐水性。少

项目成果

二瓶 智太郎: "コンポジットレジンの耐水耐久性向上に関する研究-ポリフルオロアルキルシラン混合シラン処理剤の効果-"神奈川歯学. 38. 154-166 (2003)

二平知太郎：“提高复合树脂的耐水性和耐久性的研究-聚氟烷基硅烷混合硅烷处理剂的效果-”《神奈川牙科科学》38. 154-166 (2003)。

Nihei T, Kurata S, Kondo Y, Umemoto K, Yoshino K, Teranaka T: "Effect of silane coupling agents with a fluoroalkyl and a methacryloyl groups in a molecule. -Treatment of silane mixture of silane/ 3-methacryloyloxypropyl-trimethoxy-silane-"J Jpn Soc Dent M

Nihei T、Kurata S、Kondo Y、Umemoto K、Yoshino K、Teranaka T：“分子中含有氟烷基和甲基丙烯酰基的硅烷偶联剂的效果。-硅烷/3-甲基丙烯酰氧基丙基三甲氧基硅烷的硅烷混合物的处理

Nihei T, Kurata S, Kondo Y, Umemoto K, Yoshino N, Teranaka T: "Enhanced hydrolytic stability of dental composites by use of fluoroalkyltrimethoxysilanes"J Dent Res. 81(7). 482-486 (1995)

Nihei T、Kurata S、Kondo Y、Umemoto K、Yoshino N、Teranaka T：“通过使用氟烷基三甲氧基硅烷增强牙科复合材料的水解稳定性”J Dent Res。

Nihei T: "Study on the improvement of water endurance of resin composite"J Kanagawa Odont Soc. 38(4). 154-166 (2003)

Nihei T：“提高树脂复合材料耐水性的研究”J Kanakawa Odont Soc。

Naohiro Omoto: "Modification of enamel surface by novel phosphate type hybrid surfactant"Transaction of the fourth international congress on dental materials. 16. 222 (2002)

Naohiro Omoto：“新型磷酸盐型杂化表面活性剂对牙釉质表面的改性”第四届国际牙科材料大会论文集。