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US4002698A
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Methylation of toluene in the presence of a phosphorus-modified activated crystalline aluminosilicate catalyst
Assignee: Mobil Oil AS
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Filing: 1975-08-19
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Granted: 1977-01-11
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Expires: 1995-08-19
Abstract
Abstract Process for the methylation of toluene to selectively yield para-xylene by reacting toluene with a methylating agent, such as methanol, in the presence of a catalyst comprising a crystalline aluminosilicate zeolite, which zeolite has a silica/alumina ratio of at least about 12 and a constraint index, as hereinafter defined, within the approximate range of 1 to 12, the catalyst having been modified by the addition thereto of phosphorus in an amount of at least 0.5 percent by weight and activated by vapor phase treatment at a temperature between about 400 DEG C. and about 650 DEG C. for at least about 1 hour with a methanol/water mixture.
Inventors
- 👤 Warren W. Kaeding
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 02:03
CPC Classifications
C; C10; C10G; C10G35/00; C10G35/04; C10G35/06; C10G35/095; B; B01; B01J; B01J29/00; B01J29/04; B01J29/06; B01J29/40; B01J37/00; B01J37/28; C07; C07C; C07C2/00; C07C2/02; C07C2/04; C07C2/06; C07C2/08; C07C2/12; C07C2/54; C07C2/64; C07C2/66; C07C2/86; C07C2/861; C07C2/862; C07C2/864; C07C2/865; C07C2/868; C07C4/00; C07C4/02; C07C4/06; B01J2229/00; B01J2229/10; B01J2229/26; B01J2229/30; B01J2229/36; B01J2229/42; C07C2529/00; C07C2529/04; C07C2529/06; C07C2529/40; C07C2529/65; C07C2529/70; C10G2400/00; C10G2400/20; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/52; Y10; Y10S; Y10S585/00; Y10S585/8995; Y10S585/906
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
111 words
A process for the methylation of toluene to selectively yield para-xylene which comprises contacting toluene with a methylating agent under methylation conditions in the presence of a catalyst comprising a crystalline aluminosilicate zeolite, said zeolite having a silica to alumina ratio of at least about 12, a constraint index within the approximate range of 1 to 12, said catalyst having been modified by the addition thereto of phosphorus in an amount of at least 0.5 percent by weight and activated by vapor phase treatment with a mixture of methanol and water at a temperature between about 400° C. and about 650° C. for a period of at least about 1 hour.
Claim 2
Dependent Claim
111 words
A process for the methylation of toluene to selectively yield para-xylene which comprises contacting toluene with a methylating agent under methylation conditions in the presence of a catalyst comprising a crystalline aluminosilicate zeolite, said zeolite having a silica to alumina ratio of at least about 12, a constraint index within the approximate range of 1 to 12, said catalyst having been modified by the addition thereto of phosphorus in an amount of at least 0.5 percent by weight and activated by vapor phase treatment with a mixture of methanol and water at a temperature between about 400° C. and about 650° C. for a period of at least about 1 hour.
Claim 3
Dependent Claim
18 words
The process of claim 1 wherein said methylating agent is methanol, methyl chloride, methyl bromide, dimethylether or dimethylsulfate.
Claim 4
Dependent Claim
20 words
The process of claim 1 wherein said crystalline aluminosilicate zeolite is characterized by a silica/alumina ratio in excess of 30.
Claim 5
Dependent Claim
11 words
The process of claim 1 wherein said crystalline aluminosilicate is ZSM-5.
Claim 6
Dependent Claim
11 words
The process of claim 1 wherein said methylating agent is methanol.
Claim 7
Dependent Claim
22 words
The process of claim 1 wherein said phosphorus is present in an amount of between about 0.5 and about 25 weight percent.
Claim 8
Dependent Claim
21 words
The process of claim 1 wherein said mixture of methanol and water comprises a methanol/water volume ratio of 2/1 to 1/2.
Claim 9
Dependent Claim
22 words
The process of claim 1 wherein said mixture of methanol and water comprises an approximately equal volume mixture of methanol and water.
Claim 10
Dependent Claim
17 words
The process of claim 1 wherein said temperature is between about 500° C. and about 650° C.
Claim 11
Dependent Claim
16 words
The process of claim 1 wherein said period is between about 5 and about 30 hours.
Claim 12
Independent Claim
92 words
A method of activating a catalyst comprising a crystalline aluminosilicate zeolite, said zeolite having a silica to alumina ratio of at least about 12, a constraint index within the approximate range of 1 to 12, said catalyst having been modified by the addition thereto of phosphorus in an amount of at least 0.5 percent by weight which comprises subjecting said catalyst to vapor phase treatment with a mixture of methanol and water at a temperature between about 400° C. and about 650° C. for a period of at least about 1 hour.
Claim 13
Independent Claim
92 words
A method of activating a catalyst comprising a crystalline aluminosilicate zeolite, said zeolite having a silica to alumina ratio of at least about 12, a constraint index within the approximate range of 1 to 12, said catalyst having been modified by the addition thereto of phosphorus in an amount of at least 0.5 percent by weight which comprises subjecting said catalyst to vapor phase treatment with a mixture of methanol and water at a temperature between about 400° C. and about 650° C. for a period of at least about 1 hour.
Claim 14
Dependent Claim
20 words
The method of claim 11 wherein said crystalline aluminosilicate zeolite is characterized by a silica/alumina ratio in excess of 30.
Claim 15
Dependent Claim
11 words
The method of claim 11 wherein said crystalline aluminosilicate is ZSM-5.
Claim 16
Dependent Claim
22 words
The method of claim 11 wherein said phosphorus is present in an amount of between about 0.5 and about 25 weight percent.
Claim 17
Dependent Claim
21 words
The method of claim 11 wherein said mixture of methanol and water comprises a methanol/water volume ratio of 2/1 to 1/2.
Claim 18
Dependent Claim
22 words
The method of claim 11 wherein said mixture of methanol and water comprises an approximately equal volume mixture of methanol and water.
Claim 19
Dependent Claim
17 words
The method of claim 11 wherein said temperature is between about 400° C. and about 650° C.
Claim 20
Dependent Claim
16 words
The method of claim 11 wherein said period is between about 5 and about 30 hours.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-01-11 | 1980-07-12 | 1981-01-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-01-11 | 1984-07-12 | 1985-01-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-01-11 | 1988-07-12 | 1989-01-11 | $7700.00 | Window Closed / Lapsed |