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    • 1. 发明授权
    • Process for producing solvent-soluble reactive polysiloxanes
    • 制备溶剂可溶性活性聚硅氧烷的方法
    • US08952117B2
    • 2015-02-10
    • US13996828
    • 2011-12-14
    • Akinori KitamuraNaomasa FurutaHiroshi Suzuki
    • Akinori KitamuraNaomasa FurutaHiroshi Suzuki
    • C08G77/06C08G77/20C08K5/103
    • C08K5/103C08G77/06C08G77/20
    • The present invention is a method for producing solvent-soluble polysiloxanes which includes a condensation process of subjecting a raw material having siloxane-bond-forming groups to hydrolytic copolycondensation in the presence of a catalyst to synthesize a reactive polysiloxane represented by general formula (1), the raw material containing both an organosilicon compound (S1) having a (meth)acryloyl group and siloxane-bond-forming groups and at least one silicon compound (S2) selected from among tetraalkoxysilanes and tetrahalogenosilanes, wherein in the condensation process, the organosilicon compound (S1) and silicon compound (S2) are used at a (S2)/(S1) molar ratio of 1.8 or less, and the condensation process is conducted by adding gradually a mixture of the silicon compound (S2) and the catalyst to a raw material liquid containing the organosilicon compound (S1) and water, while keeping the molar ratio of the amount of the silicon compound (S2) to the amount of the organosilicon compound (S1) within the range of 0.001/min to 0.3/min.
    • 本发明是一种溶剂可溶性聚硅氧烷的制造方法,其包括在催化剂存在下使具有硅氧烷键形成基团的原料进行水解共缩聚的缩合方法,合成由通式(1)表示的反应性聚硅氧烷, ,含有具有(甲基)丙烯酰基的有机硅化合物(S1)和硅氧烷键形成基团的原料和选自四烷氧基硅烷和四卤代硅烷中的至少一种硅化合物(S2),其中在缩合过程中,将有机硅 化合物(S1)和硅化合物(S2)以(S2)/(S1)摩尔比为1.8以下使用,缩合工序通过将硅化合物(S2)和催化剂的混合物逐渐加入到 含有有机硅化合物(S1)和水的原料液体,同时保持硅化合物(S2)的量与有机硅的量 化合物(S1)在0.001 / min至0.3 / min的范围内。
    • 2. 发明申请
    • PROCESS FOR PRODUCING SOLVENT-SOLUBLE REACTIVE POLYSILOXANES
    • 生产溶剂型可溶性反应性聚硅氧烷的方法
    • US20130338282A1
    • 2013-12-19
    • US13996828
    • 2011-12-14
    • Akinori KitamuraNaomasa FurutaHiroshi Suzuki
    • Akinori KitamuraNaomasa FurutaHiroshi Suzuki
    • C08G77/20C08K5/103
    • C08K5/103C08G77/06C08G77/20
    • The present invention is a method for producing solvent-soluble polysiloxanes which includes a condensation process of subjecting a raw material having siloxane-bond-forming groups to hydrolytic copolycondesation in the presence of a catalyst to synthesize a reactive polysiloxane represented by general formula (1), the raw material containing both an organosilicon compound (S1) having a (meth)acryloyl group and siloxane-bond-forming groups and at least one silicon compound (S2) selected from among tetraalkoxysilanes and tetrahalogenosilanes, wherein in the condensation process, the organosilicon compound (S1) and silicon compound (S2) are used at a (S2)/(S1) molar ratio of 1.8 or less, and the condensation process is conducted by adding gradually a mixture of the silicon compound (S2) and the catalyst to a raw material liquid containing the organosilicon compound (S1) and water, while keeping the molar ratio of the amount of the silicon compound (S2) to the amount of the organosilicon compound (S1) within the range of 0.001/min to 0.3/min.
    • 本发明是一种溶剂可溶性聚硅氧烷的制造方法,其包括在催化剂存在下使具有硅氧烷键形成基团的原料进行水解共解聚的缩合方法,合成由通式(1)表示的反应性聚硅氧烷, ,含有具有(甲基)丙烯酰基的有机硅化合物(S1)和硅氧烷键形成基团的原料和选自四烷氧基硅烷和四卤代硅烷中的至少一种硅化合物(S2),其中在缩合过程中,将有机硅 化合物(S1)和硅化合物(S2)以(S2)/(S1)摩尔比为1.8以下使用,缩合工序通过将硅化合物(S2)和催化剂的混合物逐渐加入到 含有有机硅化合物(S1)和水的原料液体,同时保持硅化合物(S2)的量与有机硅的量 化合物(S1)在0.001 / min至0.3 / min的范围内。
    • 3. 发明申请
    • THERMAL-SHOCK-RESISTANT CURED PRODUCT AND METHOD FOR PRODUCING SAME
    • 耐热固化产品及其生产方法
    • US20140323677A1
    • 2014-10-30
    • US14241565
    • 2012-08-29
    • Akinori KitamuraNaomasa Furuta
    • Akinori KitamuraNaomasa Furuta
    • C08G77/20
    • C08G77/20C08F299/08C08G77/16C08K5/0025C08K5/07C09D183/06C08L83/04
    • The present invention is a method for producing a thermal-shock-resistant cured product, the method involving: a condensation step of preparing a cured-product precursor by subjecting monomers represented by general formulae (1) to (5) to copolycondensation at a specific rate in the presence of an acid catalyst; and a curing step of curing the cured-product precursor by polymerizing at least a portion of ethylenically unsaturated bonds in the cured-product precursor. Also, the present invention is a cured product prepared by said method. (In formulae (1) to (5): (X) is a siloxane bond producing group; R1, R2, and R4 are each a group selected from among a hydrogen atom, an alkyl group, an aralkyl group, a cycloalkyl group, a cycloaralkyl group, an aryl group, and a group having an ethylenically unsaturated bond; R3 and R5 are each a group selected from among a hydrogen atom, an alkyl group, an aralkyl group, a cycloalkyl group, a cycloaralkyl group, and an aryl group; and at least one of R1, R2, and R4 is a group having an ethylenically unsaturated bond.)
    • 本发明是一种耐热冲击性固化物的制造方法,其特征在于,具有以下工序:将通式(1)〜(5)表示的单体进行共聚缩聚而制备固化物前体的缩合工序 在酸催化剂存在下的速率; 以及通过在固化产物前体中聚合至少一部分烯键式不饱和键来固化固化产物前体的固化步骤。 此外,本发明是通过所述方法制备的固化产物。 (式(1)〜(5)中,(X)为硅氧烷键的生成基团; R1,R2,R4分别为选自氢原子,烷基,芳烷基,环烷基, 环烷基,芳基和具有烯键式不饱和键的基团; R3和R5分别为选自氢原子,烷基,芳烷基,环烷基,环烷基和芳基中的基团 并且R 1,R 2和R 4中的至少一个是具有烯属不饱和键的基团。
    • 4. 发明授权
    • Method for manufacturing reactive polysiloxane solution
    • 反应性聚硅氧烷溶液的制备方法
    • US08940852B2
    • 2015-01-27
    • US13996760
    • 2011-12-14
    • Naomasa FurutaAkinori Kitamura
    • Naomasa FurutaAkinori Kitamura
    • C08G77/20C08K5/05C08G77/14C08G77/34
    • C08K5/05C08G77/06C08G77/14C08G77/20C08G77/34
    • The present invention is a method for manufacturing a reactive polysiloxane solution, the method comprising: a condensation process for hydrolyzing and copolycondensing a starting compound containing an organosilicon compound having a reactive functional group selected from a (meth)acryloyl group and an oxetanyl group, and also having a siloxane bond-forming group to synthetize a reactive polysiloxane represented by general formula (1); a dissolution process for dissolving the obtained reactive polysiloxane in an organic solvent for water washing; and a washing process for bringing the obtained organic solution and water in contact with each other to remove the water layer from the mixed liquid. The organic solvent for water washing that is used is a compound (e.g., propylene glycol mono butyl ether, 1-pentanol) including a hydroxyl group, having a boiling point at 1 atm of 110° C.-200° C., and a solubility of 10 g or less in 100 g of water at 20° C.
    • 本发明是一种制造反应性聚硅氧烷溶液的方法,该方法包括:使含有选自(甲基)丙烯酰基和氧杂环丁烷基的反应性官能团的有机硅化合物的起始化合物水解和共缩聚的缩合方法,以及 还具有硅氧烷键形成基团以合成由通式(1)表示的反应性聚硅氧烷; 将获得的反应性聚硅氧烷溶解在水洗有机溶剂中的溶解方法; 以及使得到的有机溶液和水彼此接触以从混合液中除去水层的洗涤方法。 使用的水洗有机溶剂是沸点为1atm,沸点为110℃-2200℃的包含羟基的化合物(例如丙二醇单丁基醚,1-戊醇)和 在20℃下在100g水中的溶解度为10g或更低
    • 5. 发明授权
    • Organosilicon compounds which have oxetanyl groups, and a method for the production and curable compositions of the same
    • 具有氧杂环丁烷基的有机硅化合物及其制备方法及其固化组合物
    • US08329774B2
    • 2012-12-11
    • US12812808
    • 2009-01-09
    • Sayaka OoikeHiroshi SuzukiAkinori Kitamura
    • Sayaka OoikeHiroshi SuzukiAkinori Kitamura
    • C08J3/28C07F7/02C08G77/00B05D3/02
    • C08G77/14C08G77/045C08L83/06
    • The object of the present invention is to provide an organosilicon compound having an oxetanyl group, which has a high proportion of an inorganic part in the structure, which, after production thereof, is stable with no gelling, and which has excellent storage stability when it is formed into a composition, and a production method thereof and a curable composition. The organosilicon compound is a compound having an oxetanyl group obtained by a method including a process in which a silicon compound A represented by the formula (1) and a silicon compound B having four siloxane bond-forming groups are subjected to hydrolysis and condensation at a ratio of 0.3 to 2.8 mol of silicon compound B based on 1 mol of silicon compound A. [In the formula, R0 is an organic group having an oxetanyl group, R1 is an alkyl group having 1 to 6 carbon atoms, an aralkyl group having 7 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms, or an organic group having an oxetanyl group, X is a hydrolyzable group, and n is 0 or 1.]
    • 本发明的目的是提供一种具有氧杂环丁烷基的有机硅化合物,其结构中无机部分的比例高,其生产稳定而没有胶化,并且当其具有优异的储存稳定性 形成组合物及其制备方法和可固化组合物。 有机硅化合物是通过包括以下方法获得的具有氧杂环丁烷基的化合物,其中将由式(1)表示的硅化合物A和具有四个硅氧烷键形成基团的硅化合物B在其中进行水解和缩合 比例为0.3〜2.8摩尔的硅化合物B,基于1摩尔的硅化合物A. [式中,R 0为具有氧杂环丁烷基的有机基团,R 1为碳原子数1〜6的烷基,具有 碳原子数为7〜10,碳原子数6〜10的芳基或氧杂环丁烷基的有机基团,X为水解性基团,n为0或1。
    • 7. 发明申请
    • CURABLE COMPOSITION AND PROCESS FOR PRODUCTION OF ORGANOSILICON COMPOUND
    • 可固化组合物和生产有机硅化合物的方法
    • US20110071255A1
    • 2011-03-24
    • US12989331
    • 2009-04-14
    • Sayaka OoikeAkinori KitamuraHiroshi Suzuki
    • Sayaka OoikeAkinori KitamuraHiroshi Suzuki
    • C09D183/07C08G77/20
    • C08G77/14C08G77/18C08G77/20C09D183/04
    • The present curable composition comprises an organosilicon compound produced by hydrolysis copolycondensation of (A) a silicon compound R0Si(R1)nX13-n [wherein R0 represents a (meth)acryloyl group; and X1 represents a hydrolyzable group] and (B) a silicon compound SiY14 [wherein Y1 represents a siloxane-bond forming group] under an alkaline condition at a ratio of compound (A) to compound (B) of 1:(0.3 to 1.8) by mol. The present process for producing an organosilicon compound comprises a reaction process of conducting alcohol exchange reaction of a silicon compound. SiY24 [wherein Y2 represents a siloxane-bond forming group] in 1-propanol to produce a composition; and a condensation process of adding a silicon compound R0Si(R1)nX23-n [wherein R0 represents a (meth)acryloyl group; and X2 represents a hydrolyzable group] to the composition to perform the hydrolysis copolycondensation of the silicon compounds under alkaline conditions.
    • 本固化性组合物包含通过(A)硅化合物R0Si(R1)nX13-n [其中R0表示(甲基)丙烯酰基的水解共缩聚而制备的有机硅化合物; X表示可水解基团]和(B)在化合物(A)与化合物(B)的比例为1:(0.3〜1.8)的条件下,在碱性条件下,硅化合物SiY14 [其中Y1表示硅氧烷键形成基团] )。 本发明的有机硅化合物的制造方法包括进行硅化合物的醇交换反应的反应方法。 SiY24 [其中Y2表示硅氧烷键形成基]在1-丙醇中以产生组合物; 和加入硅化合物R0Si(R1)nX23-n [其中R0表示(甲基)丙烯酰基的缩合方法; X2表示水解性基团],在碱性条件下进行硅化合物的水解共缩聚。
    • 9. 发明申请
    • PROCESS FOR PRODUCING SILICON COMPOUND HAVING OXETANYL GROUP
    • 生产含氧化合物的方法
    • US20110245448A1
    • 2011-10-06
    • US13128308
    • 2009-12-14
    • Sayaka OikeAkinori KitamuraHiroshi Suzuki
    • Sayaka OikeAkinori KitamuraHiroshi Suzuki
    • C08G77/18
    • C07F7/0874
    • Provided is a method for efficiently producing a cationically curable condensed silicon compound. There was an unsolved problem that, in a condensation reaction, an oxetanyl group is subjected to ring-opening under an acidic condition, while gelation is easily caused under an alkaline condition. It was found that a silicon compound (C) having an oxetanyl group can be obtained without causing gelation even at a high concentration by the present method including a first step of separately subjecting a silicon compound (A) having four siloxane bond-forming groups and a silicon compound (B) having an oxetanyl group to alcohol exchange reaction with 1-propanol and a second step of subjecting silicon compounds (AP) and (BP) undergone the first step to hydrolytic copolycondensation under an alkaline condition at a specific ratio.
    • 提供一种有效地制造阳离子固化型浓缩硅化合物的方法。 没有解决的问题是,在缩合反应中,氧杂环丁烷基在酸性条件下开环,而在碱性条件下容易引起凝胶化。 发现通过本方法可以获得具有氧杂环丁烷基的硅化合物(C),而不引起高浓度的凝胶化,该方法包括:分别对具有四个硅氧烷键形成基团的硅化合物(A)和 具有氧杂环丁烷基的硅化合物(B)与1-丙醇进行醇交换反应,第二步是在碱性条件下以特定比例进行第一步的硅化合物(AP)和(BP)的水解共缩聚。
    • 10. 发明授权
    • Curable composition and process for production of organosilicon compound
    • 有机硅化合物的固化组合物及其制备方法
    • US08829142B2
    • 2014-09-09
    • US12989331
    • 2009-04-14
    • Sayaka OoikeAkinori KitamuraHiroshi Suzuki
    • Sayaka OoikeAkinori KitamuraHiroshi Suzuki
    • C08G77/08C08G77/14C09D183/04C08G77/18C08G77/20
    • C08G77/14C08G77/18C08G77/20C09D183/04
    • The present curable composition comprises an organosilicon compound produced by hydrolysis copolycondensation of (A) a silicon compound R0Si(R1)nX13-n [wherein R0 represents a (meth)acryloyl group; and X1 represents a hydrolyzable group] and (B) a silicon compound SiY14 [wherein Y1 represents a siloxane-bond forming group] under an alkaline condition at a ratio of compound (A) to compound (B) of 1:(0.3 to 1.8) by mol. The present process for producing an organosilicon compound comprises a reaction process of conducting alcohol exchange reaction of a silicon compound. SiY24 [wherein Y2 represents a siloxane-bond forming group] in 1-propanol to produce a composition; and a condensation process of adding a silicon compound R0Si(R1)nX23-n [wherein R0 represents a (meth)acryloyl group; and X2 represents a hydrolyzable group] to the composition to perform the hydrolysis copolycondensation of the silicon compounds under alkaline conditions.
    • 本固化性组合物包含通过(A)硅化合物R0Si(R1)nX13-n [其中R0表示(甲基)丙烯酰基的水解共缩聚而制备的有机硅化合物; X表示可水解基团]和(B)在化合物(A)与化合物(B)的比例为1:(0.3〜1.8)的条件下,在碱性条件下,硅化合物SiY14 [其中Y1表示硅氧烷键形成基团] )。 本发明的有机硅化合物的制造方法包括进行硅化合物的醇交换反应的反应方法。 SiY24 [其中Y2表示硅氧烷键形成基]在1-丙醇中以产生组合物; 和加入硅化合物R0Si(R1)nX23-n [其中R0表示(甲基)丙烯酰基的缩合方法; X2表示水解性基团],在碱性条件下进行硅化合物的水解共缩聚。