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    • 5. 发明授权
    • Method of making sulfur containing organosilicon compounds
    • 制备含硫有机硅化合物的方法
    • US06740767B1
    • 2004-05-25
    • US10293841
    • 2002-11-12
    • Chad Aaron BuesingJohn Michael Gohndrone
    • Chad Aaron BuesingJohn Michael Gohndrone
    • C07F708
    • C07F7/1892
    • A process for producing organosilicon compounds of the formula (RO)3-mRmSi—Alk—Sn—Alk—SiRm(OR)3-m in which R is a monovalent hydrocarbon having 1-12 carbon atoms, Alk is a divalent hydrocarbon having 1-18 carbon atoms, m is 0, 1 or 2, and n is 2-8, preferably 3-8. The process consists generally of the steps of (I) heating and reacting (A) a sulfide compound such as M2Sn or MHS where H is hydrogen, M is ammonium or an alkali metal, and n is 1-8; with (B) a silane compound of the formula (RO)3-mRmSi—Alk—X where X is Cl, Br or I, and m is 0, 1, or 2; and with (C) sulfur. Step (I) is carried out in the presence of a phase transfer catalyst, and an aqueous phase containing a buffer or a basic compound, to form a product mixture. In step (II), the product mixture is again heated to a temperature of 80-100° C., preferably a temperature of 85-95° C., and most preferably to a temperature of 87-92° C., for about 1-3 hours, and the desired organosilicon compound can be obtained by separating it from the resulting product mixture. The result is a composition with improved color.
    • 一种制备式(RO)3-mRmSi-Alk-Sn-Alk-SiRm(OR)3-m的有机硅化合物的方法,其中R是具有1-12个碳原子的一价烃,Alk是具有1 -18个碳原子,m为0,1或2,n为2-8,优选为3-8。 该方法通常包括以下步骤:(I)加热和(A)硫化物如M2Sn或MHS,其中H为氢,M为铵或碱金属,n为1-8; 与(B)式(RO)3-mRmSi-Alk-X的硅烷化合物,其中X为Cl,Br或I,m为0,1或2; 和(C)硫。 步骤(I)在相转移催化剂和含有缓冲液或碱性化合物的水相存在下进行,以形成产物混合物。 在步骤(II)中,将产物混合物再次加热至80-100℃,优选温度为85-95℃,最优选温度为87-92℃,约为 1-3小时,所需的有机硅化合物可以通过将其与所得产物混合物分离而获得。 结果是具有改进颜色的组合物。