Process for producing a thiometallate or a selenometallate material
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C01B-017/00
C01B-025/14
C01D-005/08
C01G-039/06
B01J-027/04
B01J-027/047
B01J-027/049
B01J-027/051
B01J-035/02
B01J-035/10
B01J-037/03
C01B-017/20
C01B-019/00
C01G-039/00
C01G-041/00
C01G-049/00
C01G-051/00
C01G-053/00
C10G-047/02
B82Y-030/00
출원번호
US-0010885
(2011-01-21)
등록번호
US-8956585
(2015-02-17)
발명자
/ 주소
Reynolds, Michael Anthony
출원인 / 주소
Shell Oil Company
인용정보
피인용 횟수 :
0인용 특허 :
50
초록▼
A method for producing a thiometallate or selenometallate material is provided in which a first salt containing an anionic component selected from the group consisting of MoS42−, MoSe42−, WS42−, WSe42−, VS43−, and VSe43− and a second salt containing a cationic component comprising a metal in any non
A method for producing a thiometallate or selenometallate material is provided in which a first salt containing an anionic component selected from the group consisting of MoS42−, MoSe42−, WS42−, WSe42−, VS43−, and VSe43− and a second salt containing a cationic component comprising a metal in any non-zero oxidation state selected from the group consisting of Cu, Fe, Ag, Co, Mn, Re, Ru, Rh, Pd, Ir, Pt, B, Al, Ce, La, Pr, Sm, Eu, Yb, Lu, Dy, Ni, Zn, Bi, Sn are mixed under anaerobic conditions in an aqueous mixture at a temperature of from 50° C. to 150° C.
대표청구항▼
1. A method for producing a thiometallate or selenometallate material, comprising: mixing a first salt and a second salt in an aqueous mixture under anaerobic conditions, where, during mixing the aqueous mixture has a temperature of from 50° C. to 150° C., and wherein the first salt comprises a cati
1. A method for producing a thiometallate or selenometallate material, comprising: mixing a first salt and a second salt in an aqueous mixture under anaerobic conditions, where, during mixing the aqueous mixture has a temperature of from 50° C. to 150° C., and wherein the first salt comprises a cationic component and an anionic component containing a first metal selected from the group consisting of Mo, W, and V, where the anionic component is selected from the group consisting of MoS42−, MoSe42−, WS42−, WSe42−, VS43−, and VSe43− and mixtures thereof, and wherein the second salt comprises a cationic component comprising a second metal in any non-zero oxidation state selected from the group consisting of Cu, Fe, Ag, Co, Mn, Re, Ru, Rh, Pd, Ir, Pt, B, Al, Ce, La, Pr, Sm, Eu, Yb, Lu, Dy, Ni, Zn, Bi, Sn, and mixtures thereof, where the first and second salts are soluble in the aqueous mixture; andseparating a solid material from the aqueous mixture comprising a) the first metal; and b) the second metal, wherein at least a portion of the solid material separated from the aqueous mixture has a structure according to a formula selected from the group consisting of formula (I), formula (II), formula (III), and formula (IV): where M is either the first metal or the second metal; at least one M is the first metal and at least one M is the second metal; and Q is either sulfur or selenium; where M is either the first metal or the second metal, and at least one M is the first metal and at least one M is the second metal, Q is either sulfur or selenium, and X is selected from the group consisting of SO4, PO4, oxalate (C2O4), acetylacetonate, acetate, citrate, tartrate, Cl, Br, I, ClO4, and NO3; where M is either the first metal or the second metal, and at least one M is the first metal and at least one M is the second metal, Q is either sulfur or selenium, and X is selected from the group consisting of SO4, PO4, oxalate (C2O4), acetylacetonate, acetate, citrate, tartrate, Cl, Br, I, ClO4, and NO3; where M is either the first metal or the second metal, and at least one M is the first metal and at least one M is the second metal, Q is either sulfur or selenium, and X is selected from the group consisting of SO4, PO4, oxalate (C2O4), acetylacetonate, acetate, citrate, tartrate, Cl, Br, I, ClO4, and NO3; wherein the solid material separated from the aqueous mixture contains at most 0.5 wt.% of the cationic component of the first salt and contains less than 0.5 wt.% of ligands other than sulfur-containing ligands. 2. The method of claim 1 wherein the amount of the first salt and the amount of the second salt mixed in the aqueous mixture are selected to provide an atomic ratio of the second metal to the first metal of greater than 1.6:1. 3. The method of claim 1 wherein the solid material separated from the aqueous mixture comprises at most 0.1 wt. % oxygen. 4. The method of claim 1 wherein the amount of the first salt and the total volume of the aqueous mixture are selected to provide at most 0.2 moles of the anionic component from the first salt per liter of the total volume of the aqueous mixture, and where the amount of the second salt and the total volume of the aqueous mixture are selected to provide at most 1 mole of the cationic component of the second salt per liter of the total volume of the aqueous mixture. 5. The method of claim 1 wherein the first salt is contained in a first aqueous solution and the second salt is contained in a second aqueous solution, and the first salt and the second salt are mixed in the aqueous mixture by mixing the first aqueous solution and the second aqueous solution. 6. The method of claim 5 wherein the first aqueous solution containing the first salt and the second aqueous solution containing the second salt are added to a third aqueous solution to form the aqueous mixture. 7. The method of claim 6 wherein the volume ratio of the third aqueous solution to the first aqueous solution is from 0.5:1 to 50:1 where the first aqueous solution contains at most 0.8 moles per liter of the first salt and the volume ratio of the third aqueous solution to the second aqueous solution is from 0.5:1 to 50:1 where the second aqueous solution contains at most 3 moles per liter of the second salt. 8. The method of claim 6 wherein the first aqueous solution and the second aqueous solution are added to the third aqueous solution and mixed in the third aqueous solution such that the instantaneous concentration of the first salt in the aqueous mixture is at most 0.05 moles per liter and such that the instantaneous concentration of the second salt in the aqueous mixture is at most 0.05 moles per liter. 9. The method of claim 1 wherein the solid material separated from the aqueous mixture is particulate and has a particle size distribution, where the mean particle size or the median particle size of the particle size distribution of the solid material is from 50 nm to 10 μm. 10. The method of claim 1 wherein the solid material separated from the aqueous mixture is particulate where the particles have an average BET surface area of from 50 m2/g to 500 m2/g. 11. The method of claim 1 wherein the solid material separated from the aqueous mixture is at least 20% crystalline. 12. The method of claim 1 wherein the aqueous mixture contains more than 0 vol. % but less than 50 vol. % of an organic solvent containing from 1 to 5 carbons and selected from the group consisting of an alcohol, a diol, an aldehyde, a ketone, an amine, an amide, a furan, an ether, acetonitrile, and mixtures thereof where the first salt and the second salt are soluble in the aqueous mixture. 13. The method of claim 1 wherein the solid material separated from the aqueous mixture comprises alternating MIS4 and MIIS4 tetrahedral formations, where each tetrahedral formation shares at least two sulfur atoms with an adjacent tetrahedral formation, and where MI is the first metal and MII is the second metal. 14. The method of claim 1 wherein the solid material separated from the aqueous mixture is comprised of alternating atoms of the metal of the anionic component of the first salt and the metal of the cationic component of the second salt bonded to and linked by two sulfur atoms or two selenium atoms. 15. The method of claim 1 wherein the solid material separated from the aqueous mixture is comprised of at least three linked chain elements, the chain elements being comprised of a first chain element including the first metal having a structure according to formula (V) and a second chain element including the second metal having a structure according to formula (VI) where M1 is the first metal, where M2 is the second metal, and where Q is either sulfur or selenium; where the solid material contains at least one first chain element and at least one second chain element, and where at least a portion of the chain elements in the solid material are linked by bonds between two sulfur atoms or two selenium atoms of a chain element and the metal of an adjacent chain element. 16. The method of claim 1 wherein the solid material separated from the aqueous mixture is comprised of monomeric units that repeat in the solid material so that the solid material is a polymer formed of the repeating monomeric units, where a monomeric unit is comprised of the first metal and the second metal having the structure of formula (IV): where M1 is the metal of the cationic component from the second metal salt, M2 is the metal of the anionic component of the first salt, Q is either sulfur or selenium, and x is at least 2.
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