Reduced ternary molybdenum and tungsten sulfides and hydroprocessing catalysis therewith
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
B01J-027/51
C01B-017/32
출원번호
US-0694907
(1996-08-09)
발명자
/ 주소
Hilsenbeck Shane J.
McCarley Robert E.
Schrader Glenn L.
Xie Xiaobing
출원인 / 주소
The United States of America as represented by the United States Department of Energy
대리인 / 주소
LaMarre
인용정보
피인용 횟수 :
26인용 특허 :
0
초록▼
New amorphous molybdenum/tungsten sulfides with the general formula M.sup.n+.sub.2x/n (L.sub.6 S.sub.8)S.sub.x, where L is molybdenum or tungsten and M is a ternary metal, has been developed. Characterization of these amorphous materials by chemical and spectroscopic methods (IR, Raman, PES) shows t
New amorphous molybdenum/tungsten sulfides with the general formula M.sup.n+.sub.2x/n (L.sub.6 S.sub.8)S.sub.x, where L is molybdenum or tungsten and M is a ternary metal, has been developed. Characterization of these amorphous materials by chemical and spectroscopic methods (IR, Raman, PES) shows that the (M.sub.6 S.sub.8).sup.0 cluster units are present. Vacuum thermolysis of the amorphous Na.sub.2x (Mo.sub.6 S.sub.8)S.sub.x .multidot.yMeOH first produces poorly crystalline NaMo.sub.6 S.sub.8 by disproportionation at 800.degree. C. and well-crystallized NaMo.sub.6 S.sub.8 at .gtoreq. 900.degree. C. Ion-exchange of the sodium material in methanol with soluble M.sup.2+ and M.sup.3+ salts (M=Sn, Co, Ni, Pb, La, Ho) produces the M.sup.n+.sub.2x/n (Mo.sub.6 S.sub.8)S.sub.x .multidot.yMeOH compounds. Additionally, the new reduced ternary molybdenum sulfides with the general formula M.sup.n+.sub.2x/n Mo.sub.6 S.sub.8+x (MeOH).sub.y [MMOS] (M=Sn, Co, Ni) is an effective hydrodesulfurization (HDS) catalyst both as-prepared and after a variety of pretreatment conditions. Under specified pretreatment conditions with flowing hydrogen gas, the SnMoS type catalyst can be stabilized, and while still amorphous, can be considered as "Chevrel phase-like" in that both contain Mo.sub.6 S.sub.8 cluster units. Furthermore, the small cation NiMoS and CoMoS type pretreated catalyst showed to be very active HDS catalysts with rates that exceeded the model unpromoted and cobalt-promoted MoS.sub.2 catalysts.
대표청구항▼
[ We claim:] [1.] Chemical compositions comprising:M.sup.n+.sub.2x/n (L.sub.6 S.sub.8)S.sub.xwhere L is molybdenum or tungsten and M is ternary metal selected from the group consisting of lithium, sodium, potassium, rubidium, cesium, magnesium, calcium, strontium, barium, titanium, vanadium, chromiu
[ We claim:] [1.] Chemical compositions comprising:M.sup.n+.sub.2x/n (L.sub.6 S.sub.8)S.sub.xwhere L is molybdenum or tungsten and M is ternary metal selected from the group consisting of lithium, sodium, potassium, rubidium, cesium, magnesium, calcium, strontium, barium, titanium, vanadium, chromium, manganese, iron, ruthenium, osmium, cobalt, iridium, nickel, palladium, platinum, copper, zinc, silver, gold, cadmium, mercury, gallium, indium, thallium, tin, lead, bismuth, scandium, lanthanum, yttrium, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, erbium thulium, holmium, ytterbium, and lutetium; wherein n is 1, 2, or 3; and x is from 0.5 to 1.5; and wherein the chemical structure is amorphous. [8.] A method for making an amorphous chemical composition having the formula:M.sup.n+.sub.2x/n (L.sub.6 S.sub.8)S.sub.xwhere L is molybdenum or tungsten; M is selected from the group consisting of sodium, tin, cobalt, nickel, lead, lanthanum, and holmium; n is 1, 2, or 3; and x is from 1 to 1.5, comprising the following steps:reacting L.sub.6 Cl.sub.12 and an alkali metal sulfide in a solvent to produce a first reaction product and an alkali metal chloride;filtering the first reaction product to separate the first reaction product from the solvent;extracting the first reaction product with a second solvent to remove the alkali metal chloride to form a second reaction product;reacting the second reaction product with a M metal salt to form a third reaction product;extracting the third reaction product with a solvent to remove metal salts and unreacted M metal salts to form a fourth reaction product;heating the fourth reaction product to form the amorphous chemical composition having the formula M.sup.n+.sub.2x/n (L.sub.6 S.sub.8)S.sub.x.
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