US4243553A
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US
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Production of improved molybdenum disulfide catalysts
Assignee: Katalistiks International Inc
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Filing: 1979-06-11
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Granted: 1981-01-06
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Expires: 1999-06-11
Abstract
Abstract High surface area molybdenum disulfide, MoS2, is produced by the thermal decomposition of selected substituted ammonium thiomolybdate salts at temperatures of about 300 DEG -800 DEG C., with said salts being heated to decomposition temperature slowly, in an essentially oxygen-free atmosphere, through the temperature interval in which the substantial portion of the particular substituted ammonium thiomolybdate salts decompose. The product molybdenum disulfide has superior catalytic properties for the water gas shift and methanation reactions compared with conventional MoS2. The stability of the catalyst is enhanced by decomposing the thiomolybdate salt in admixture with an inert, preformed particulate diluent or by bulk doping said salt with tungsten or vanadium prior to decomposition of the salt. The molybdenum disulfide of the invention also has desirable properties for use in catalyzed hydrogenation and hydrotreating reactions, i.e., hydrodenitrogenation and hydrodesulfurization reactions, particularly when employed in nickel or cobalt-promoted form.
Inventors
- 👤 Alfred W. Naumann
- 👤 Albert S. Behan
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 17:02
CPC Classifications
C; C07; C07C; C07C1/00; C07C1/02; C07C1/04; C07C1/0425; C07C1/0445; B; B01; B01J; B01J27/00; B01J27/02; B01J27/04; B01J27/047; B01J27/051; C01; C01B; C01B3/00; C01B3/02; C01B3/06; C01B3/12; C01B3/16; C01G; C01G39/00; C01G39/06; C10; C10G; C10G45/00; C10G45/02; C10G45/04; C07C2527/00; C07C2527/02; C07C2527/04; C07C2527/047; C07C2527/051; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/52
Claims Analysis
Total Claims: 32
Claim 1
Independent Claim
131 words
A process for the production of improved, sulfur resistant catalysts comprising thermally decomposing a thiomolybdate salt having the formula B 2 [MoO x S 4-x ], where B is a substituted aliphatic ammonium or a cyclic amine containing one or more basic N atoms, and x is 0, 1 or 2, at a decomposition temperature of from about 300° C. to about 800° C., said substituted ammonium thiomolybdate salt being heated to said decomposition temperature slowly, in an essentially oxygen-free atmosphere, through the temperature interval in which a substantial portion of said substituted ammonium thiomolybdate salt decomposes, said salt decomposing to form a molybdenum disulfide, MoS 2 , product having desirable properties for use as a catalyst for water gas shift and methanation reactions and for catalyzed hydrogenation or hydrotreating reactions.
Claim 2
Dependent Claim
131 words
A process for the production of improved, sulfur resistant catalysts comprising thermally decomposing a thiomolybdate salt having the formula B 2 [MoO x S 4-x ], where B is a substituted aliphatic ammonium or a cyclic amine containing one or more basic N atoms, and x is 0, 1 or 2, at a decomposition temperature of from about 300° C. to about 800° C., said substituted ammonium thiomolybdate salt being heated to said decomposition temperature slowly, in an essentially oxygen-free atmosphere, through the temperature interval in which a substantial portion of said substituted ammonium thiomolybdate salt decomposes, said salt decomposing to form a molybdenum disulfide, MoS 2 , product having desirable properties for use as a catalyst for water gas shift and methanation reactions and for catalyzed hydrogenation or hydrotreating reactions.
Claim 3
Dependent Claim
23 words
The process of claim 1 in which said salt is decomposed at a temperature of from about 400° C. to about 500° C.
Claim 4
Dependent Claim
24 words
The process of claim 1 in which said molybdenum disulfide has a surface area of from about 25 to about 150 m 2 /gm.
Claim 5
Dependent Claim
46 words
The process of claim 1 in which said ammonium thiomolybdate salt is heated to said decomposition temperature slowly, at a rate of about 0.5° to about 2° C./min., under vacuum, through said temperature interval in which a substantial portion of the substituted ammonium thiomolybdate salt decomposes.
Claim 6
Dependent Claim
12 words
The process of claim 1 in which B is the piperazinium cation.
Claim 7
Dependent Claim
12 words
The process of claim 1 in which B is the hexamethylenetetramonium cation.
Claim 8
Dependent Claim
17 words
The process of claim 1 in which B is n-C 4 H 9 NH 3 + .
Claim 9
Dependent Claim
20 words
The process of claim 1 in which said B is (C 2 H 5 ) 2 NH 2 + .
Claim 10
Dependent Claim
17 words
The process of claim 1 in which said B is (CH 3 ) 4 N + .
Claim 11
Dependent Claim
13 words
The process of claim 1 in which said B is the piperidinium cation.
Claim 12
Dependent Claim
13 words
The process of claim 1 in which said B is the pyrrolidinium cation.
Claim 13
Dependent Claim
29 words
The process of claim 1 and including decomposing said thiomolybdate in admixture with an inert, preformed particulate diluent, the stability of the resulting MoS 2 product being improved thereby.
Claim 14
Dependent Claim
41 words
The process of claim 4 in which said salt is decomposed at a temperature of from about 400° C. to about 500° C., the resulting molybdenum disulfide has a surface area of from about 25 to about 150 m 2 /gm.
Claim 15
Dependent Claim
15 words
The process of claim 5 in which x is 0, said salt being piperazinium thiomolybdate.
Claim 16
Dependent Claim
14 words
The process of claim 5 in which x is 1, said salt being oxythiomolybdate.
Claim 17
Dependent Claim
23 words
The process of claim 14 in which said salt is decomposed at a temperature of from about 400° C. to about 500° C.
Claim 18
Dependent Claim
23 words
The process of claim 15 in which said salt is decomposed at a temperature of from about 400° C. to about 500° C.
Claim 19
Dependent Claim
124 words
An improved, sulfur resistant catalyst produced by the process comprising thermally decomposing a thiomolybdate salt having the formula B 2 [MoO x S 4-x ], where B is a substituted aliphatic ammonium ion or a cyclic amine containing one or more basic N atoms, and x is 0, 1 or 2, at a decomposition temperature of from about 300° C. to about 800° C., said substituted ammonium thiomolybdate salt being heated to the decomposition temperature slowly, in an essentially oxygen-free atmosphere, through the temperature interval in which molybdate salt decomposes, said salt decomposing to form a molybdenum disulfide, MoS 2 , product having desirable properties for use as a catalyst for water gas shift and methanation reactions and for catalyzed hydrogenation or hydrotreating reactions.
Claim 20
Dependent Claim
124 words
An improved, sulfur resistant catalyst produced by the process comprising thermally decomposing a thiomolybdate salt having the formula B 2 [MoO x S 4-x ], where B is a substituted aliphatic ammonium ion or a cyclic amine containing one or more basic N atoms, and x is 0, 1 or 2, at a decomposition temperature of from about 300° C. to about 800° C., said substituted ammonium thiomolybdate salt being heated to the decomposition temperature slowly, in an essentially oxygen-free atmosphere, through the temperature interval in which molybdate salt decomposes, said salt decomposing to form a molybdenum disulfide, MoS 2 , product having desirable properties for use as a catalyst for water gas shift and methanation reactions and for catalyzed hydrogenation or hydrotreating reactions.
Claim 21
Dependent Claim
37 words
The catalyst of claim 18 in which said decomposition temperature is from about 400° C. to about 500° C., said product molybdenum disulfide having a surface area of from about 25 to about 150 m 2 /gm.
Claim 22
Dependent Claim
39 words
The catalyst of claim 18 in which said salt is heated slowly, at a rate of from about 0.5 to about 2° C./min., under vacuum, through said temperature interval in which the substantial portion of said substituted salt decomposes.
Claim 23
Dependent Claim
12 words
The catalyst of claim 18 in which B is the piperazinium cation.
Claim 24
Dependent Claim
12 words
The catalyst of claim 18 in which B is the hexamethylenetetramonium cation.
Claim 25
Dependent Claim
18 words
The catalyst of claim 18 in which said B is n-C 4 H 9 NH 3 + .
Claim 26
Dependent Claim
20 words
The catalyst of claim 18 in which said B is (C 2 H 5 ) 2 NH 2 + .
Claim 27
Dependent Claim
17 words
The catalyst of claim 18 in which said B is (CH 3 ) 4 N + .
Claim 28
Dependent Claim
13 words
The catalyst of claim 18 in which said B is the piperidinium cation.
Claim 29
Dependent Claim
13 words
The catalyst of claim 18 in which said B is the pyrrolidinium cation.
Claim 30
Dependent Claim
39 words
The catalyst of claim 19 in which said salt is heated slowly, at a rate of from about 0.5° to about 2° C./min., under vacuum, through said temperature interval in which the substantial portion of said substituted salt decomposes.
Claim 31
Dependent Claim
15 words
The catalyst of claim 21 in which x is 0, said salt being piperazinium thiomolybdate.
Claim 32
Dependent Claim
15 words
The catalyst of claim 21 in which x is 1, said salt being piperazinium oxythiomolybdate.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-01-06 | 1984-07-07 | 1985-01-06 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-01-06 | 1988-07-07 | 1989-01-06 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-01-06 | 1992-07-07 | 1993-01-06 | $7700.00 | Window Closed / Lapsed |