IPC분류정보
국가/구분 |
United States(US) Patent
등록
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국제특허분류(IPC7판) |
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출원번호 |
US-0275482
(2011-10-18)
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등록번호 |
US-8658558
(2014-02-25)
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발명자
/ 주소 |
- Maesen, Theodorus
- Kuperman, Alexander E.
- Dykstra, Dennis
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출원인 / 주소 |
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인용정보 |
피인용 횟수 :
1 인용 특허 :
64 |
초록
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In a process for forming a bulk hydroprocessing catalyst by sulfiding a catalyst precursor made in a co-precipitation reaction, up to 60% of the metal precursor feeds do not react to form catalyst precursor and end up in the supernatant. In the present disclosure, the metals can be recovered in an e
In a process for forming a bulk hydroprocessing catalyst by sulfiding a catalyst precursor made in a co-precipitation reaction, up to 60% of the metal precursor feeds do not react to form catalyst precursor and end up in the supernatant. In the present disclosure, the metals can be recovered in an electro-coagulation reactor, wherein portion of the metal residuals in the supernatant reacts with the electrodes to form a slurry containing insoluble metal compounds. The insoluble metal compounds are isolated and recovered, forming an effluent stream. The insoluble metal compounds and/or the effluent stream can be further treated to form at least a metal precursor feed which can be used in the co-precipitation reaction.
대표청구항
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1. A process for forming a bulk hydroprocessing catalyst, the method comprises: co-precipitating at reaction conditions at least a Group VIB metal precursor feed and at least a Promoter metal precursor feed selected from Group VIII, Group IIB, Group IIA, Group IVA and combinations thereof, to form a
1. A process for forming a bulk hydroprocessing catalyst, the method comprises: co-precipitating at reaction conditions at least a Group VIB metal precursor feed and at least a Promoter metal precursor feed selected from Group VIII, Group IIB, Group IIA, Group IVA and combinations thereof, to form a mixture comprising a catalyst precursor;isolating the catalyst precursor from the mixture, forming a supernatant containing at least a Promoter metal residual and at least a Group VIB metal residual in a total amount of at least 10 mole % of the metal precursor feeds;supplying the supernatant to a reactor vessel having a plurality of electrodes having a positive or a negative charge provided by a power supply, wherein the electrodes dissolve in water generating an electrode dissolution product;reacting the electrode dissolution product with at least one of the metal residuals, forming a slurry containing insoluble metal compounds;isolating the insoluble metal compounds from the slurry, forming a first effluent stream containing less than 50 mole % of metal ions in the metal residuals;treating the first effluent stream to recover at least 80 mol % of the metal ions to form at least a metal precursor feed;recycling the metal precursor feed to the co-precipitating step; andsulfiding the catalyst precursor forming the bulk catalyst. 2. The process of claim 1, wherein the recovering of 80 mole % of at least one of the metal residuals from the first effluent stream comprises treating the first effluent stream by chemical precipitation, forming a second effluent stream contains less than 2000 ppm of at least one of the metal residuals. 3. The process of claim 1, wherein the electrodes are substantial parallel electrolytic plates. 4. The process of claim 1, wherein the electrodes are aluminum. 5. The process of claim 4, wherein the electrodes sacrifice aluminum ions into the supernatant forming at least an aluminum complex with at least one of the Promoter metal residual. 6. The process of claim 5, wherein the Promoter metal residual comprises at least a nickel compound and the insoluble metal compounds comprise NiAlO4. 7. The process of claim 1, wherein the first effluent stream contains less than 20 mole % of the Promoter metal residual. 8. The process of claim 7, wherein the first effluent stream contains less than 50 ppm of the Promoter metal residual. 9. The process of claim 1, wherein the Group VIB metal residual comprises at least a Mo compound and a W compound. 10. The process of claim 2, wherein the treatment of the first effluent stream comprises adding at least an additive selected from the group of a base, an acid, a sulfide-containing compound, and mixtures thereof under mixing conditions for a sufficient amount of time to precipitate at least a portion of at least one of the metal residuals at a first pre-selected pH. 11. The process of claim 10, wherein the additive is selected from the group of nitric acid and sulphuric acid and the first pre-selected pH is less than 3. 12. The process of claim 10, further comprising isolating and recovering the precipitate forming a second effluent stream comprising less than 25 mole % of at least one of the metal residuals. 13. The process of claim 12, further comprising acidifying the second effluent stream to a pH of less than 6.5. 14. The process of claim 13, further comprising adding at least a calcium compound to the second effluent stream under mixing conditions forming a slurry containing at least a calcium salt, wherein the molar ratio of added calcium compound to Group VIB metal residual is 2/1 to 50/1. 15. The process of claim 14, wherein the calcium salt comprises at least one of CaMoO4 and CaWO4. 16. The process of claim 14, further comprising isolating and recovering the calcium salt, forming an effluent stream containing less than 500 ppm metals. 17. The process of claim 1, further comprising calcining the catalyst precursor at a temperature of at least 300° C. before the sulfidation step. 18. The process of claim 17, wherein the calcination is at a temperature of at least 325° C. for the catalyst precursor to have the formula (X)b(Mo)c(W)dOz; wherein X is Ni or Co, the molar ratio of b:(c+d) is 0.5/1 to 3/1, the molar ratio of c:d is >0.01/1, and z=[2b+6(c+d)]/2. 19. The process of claim 1, further comprising drying the catalyst precursor at a temperature of 200° C. or less before the sulfidation step, wherein the catalyst precursor has the formula Av[(MP)(OH)x(L)ny]z(MVIBO4), wherein A is at least one of an alkali metal cation, an ammonium, an organic ammonium and a phosphonium cation,MP is selected from the group of Group VIII, Group IIB, Group IIA, Group IVA and combinations thereof, P is oxidation state with MP having an oxidation state of either +2 or +4 depending on the selection of MP,L is at least a ligating agent L having an charge n<=0;MVIB is at least a Group VIB metal having an oxidation state of +6,MP:MVIB has an atomic ratio of 100:1 to 1:100;v−2+P*z−x*z+n*y*z=0; and0
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