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    • 10. 发明授权
    • Method for making molybdenum and sulfur containing compounds
    • 制备含钼和硫的化合物的方法
    • US5300274A
    • 1994-04-05
    • US603064
    • 1990-10-25
    • Liwen WeiCatherine L. CoyleThomas R. HalbertEdward I. Stiefel
    • Liwen WeiCatherine L. CoyleThomas R. HalbertEdward I. Stiefel
    • C01G39/00C07F11/00C01G39/06
    • C07F11/005C01G39/006C01P2006/60C01P2006/80C01P2006/82Y10S423/14
    • A method for preparing molybdenum and sulfur containing compounds of the general formula X.sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O, where X is a cation selected from the group consisting of Na.sup.+, K.sup.+, R.sub.4 N.sup.+, R.sub.3 NH.sup.+, R.sub.2 NH.sub.2.sup.+, RNH.sub.3.sup.+, NH.sub.4.sup.+, R.sub.4 P.sup.+, R.sub.4 As.sup.+,(R.sub.3 P).sub.2 N.sup.+, R is a C.sub.1 -C.sub.30 alkyl, C.sub.6 -C.sub.30 aryl, C.sub.7 -C.sub.30 aralkyl or C.sub.2 -C.sub.30 alkoxyalkyl group and mixtures thereof, and y is from 0 to 2. The method comprises preparing a sulfide solution that contains from about 9 wt. % to about 13 wt. % sulfide sulfur; contacting the solution with elemental sulfur and a hydroxide; adding a molybdenum compound for a time and at a temperature sufficient to form a reaction mixture and a precipitate; separating the precipitate; and contacting the remaining reaction mixture with additional sulfide solution to form (NH.sub.4 ).sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O. When compounds containing cations other than NH.sub.4.sup.+ are to be produced, the (NH.sub.4).sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O is contacted with a cation exchange compound containing a desired substitute cation selected from above and an anion selected from the group consisting of Cl.sup.-, Br.sup.-, F.sup.-, I.sup.-, BF.sub.4.sup.-, PF.sub.6.sup.-, OH.sup.-, BR.sub.4.sup.- where R is a C.sub.1 -C.sub.30 alkyl, C.sub.6 -C.sub.30 aryl, C.sub.7 -C.sub.30 aralkyl or C.sub.2 -C.sub.30 alkoxyalkyl group, and mixtures thereof, in the presence of a solvent and for a time and at a temperature sufficient to form X.sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O, where X is other than NH.sub.4.sup.+.
    • 一种制备通式为X2Mo2S12.yH2O的含钼和硫化合物的方法,其中X是选自Na +,K +,R4N +,R3NH +,R2NH2 +,RNH3 +,NH4 +,R4P +,R4As +,(R3P)2N + R为C1-C30烷基,C6-C30芳基,C7-C30芳烷基或C2-C30烷氧基烷基及其混合物,y为0至2.该方法包括制备含有约9wt。 %至约13重量% 硫化硫% 使溶液与元素硫和氢氧化物接触; 在足以形成反应混合物和沉淀物的温度下加入钼化合物; 分离沉淀物; 并将剩余的反应混合物与另外的硫化物溶液接触以形成(NH 4)2 Mo 2 S 12·yH 2 O。 当要生产含有除NH4 +之外的阳离子的化合物时,(NH 4)2 Mo 2 S 12·yH 2 O与含有选自上述的所需取代阳离子的阳离子交换化合物和选自Cl-,Br-,F - ,I - ,BF4-,PF6-,OH-,BR4-,其中R是C1-C30烷基,C6-C30芳基,C7-C30芳烷基或C2-C30烷氧基烷基,及其混合物, 溶剂并在足以形成X2Mo2S12.yH2O的温度下进行,其中X不是NH 4 +。