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US3725381A
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US
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Process for preparation of over-based sulfurized phenates
Assignee: Cosmo Oil Co Ltd
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Filing: 1970-06-19
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Granted: 1973-04-03
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Expires: 1990-06-19
Abstract
Abstract A process for the preparation of an over-based sulfurized phenate which comprises the steps of heating a mixture of a phenolic compound, elementary sulfur, an alkaline earth metal reagent such as an oxide of a hydroxide of an alkaline earth metal, and a dihydric alcohol at a temperature of from 110* to 200*C in the presence of a higher alcohol as solvent, wherein the weight ratio of the higher alcohol to the phenolic compound is at least 0.5, preferably at least 3.0, to thereby effect sulfurization and metal addition in parallel, distilling the reaction mixture at a temperature below 200* C to remove water formed in the reactions together with a major portion of any unreacted dihydric alcohol, and heating the reaction product contained in the distillation residue together with carbon dioxide at a temperature of from 70* to 200* C in the presence of the higher alcohol, wherein the weight ratio of the higher alcohol to the phenolic compound is at least 10.5, is disclosed.
Inventors
- 👤 Y Sakai
- 👤 T Hori
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 21:19
CPC Classifications
C; C10; C10M; C10M159/00; C10M159/12; C10M159/20; C10M159/22; C10M2219/00; C10M2219/02; C10M2219/022; C10N; C10N2040/00; C10N2040/25; C10N2040/252; C10N2040/253; C10N2070/00; C10N2070/02
Claims Analysis
Total Claims: 26
Claim 1
Independent Claim
12 words
The process of claim 1, wherein the alkaline earth metal is calcium.
Claim 2
Dependent Claim
12 words
The process of claim 1, wherein the dihydric alcohol is ethylene glycol.
Claim 3
Dependent Claim
92 words
The process of claim 1, wherein the sulfurization and metal addition reactions are carried out in the presence of a higher alcohol having from 9 to 24 carbon atoms, wherein the weight ratio of said higher alcohol to the phenolic compound used is from 0.5 to 10.5, and the reaction mixture is combined before removal of water and dihydric alcohol, with said higher alcohol in an amount such that the total amount of the higher alcohol in the product mixture is at least 10.5 times the weight of said phenolic compound used.
Claim 4
Dependent Claim
90 words
The process of claim 1, wherein the sulfurization and metal addition reactions are carried out in the presence of a higher alcohol having from 9 to 24 carbon atoms, wherein the weight ratio of said higher alcohol to the phenolic compound used is from 0.5 to 10.5, and the distillation residue is combined, before the carbon dioxide treatment, with said higher alcohol in an amount such that the total amount of said higher alcohol in the product mixture is at least 10.5 times the weight of said phenolic compound used.
Claim 5
Dependent Claim
45 words
The process of claim 1, wherein the sulfurization And metal addition reactions are carried out n the presence of a higher alcohol having from 9 to 24 carbon atoms, wherein the weight ratio of said higher alcohol to the phenolic compound is at least 10.5.
Claim 6
Dependent Claim
25 words
The process of claim 1, wherein the sulfurization and metal addition reactions are carried out in the presence of a lubricating oil as a diluent.
Claim 7
Dependent Claim
22 words
The process of claim 1, wherein a lubricating oil is added to the reaction mixture before removing the water and dihydric alcohol.
Claim 8
Dependent Claim
28 words
The process of claim 1, wherein the sulfurization and metal addition reactions are carried out under reduced pressure while removing the water formed and dihydric alcohol by distilling.
Claim 9
Dependent Claim
44 words
The process of claim 1, wherein a portion of the alkaline earth metal reagent used is added at the beginning of the sulfurization and metal addition reactions, and the remainder of the alkaline earth metal reagent is added after completion of the sulfurization reaction.
Claim 10
Dependent Claim
45 words
The process of claim 1, wherein a portion of the dihydric alcohol to be used for the reactions is added at the beginning of the sulfurization and metal addition reactions and the remainder of the dihydric alcohol is added after completion of the sulfurization reaction.
Claim 11
Dependent Claim
57 words
The process of claim 1, wherein a portion of the alkaline earth metal reagent and a portion of the dihydric alcohol are added at the beginning of the sulfurization and metal addition reactions, and the remainder of the alkaline earth metal reagent and the remainder of the dihydric alcohol are added after completion of the sulfurization reaction.
Claim 12
Dependent Claim
58 words
The process of claim 1, wherein the sulfurization and metal addition reactions are carried out at from 110* to 150*C, the removal of water and dihydric alcohol is carried out by distillation at a temperature below 150*C and the carbon dioxide treatment is first carried out at from 70* to 150*C and then at from 120* to 200*C.
Claim 13
Dependent Claim
20 words
The process of claim 1, wherein the sulfurization and metal addition reactions are carried at at from 155* to 200*C.
Claim 14
Dependent Claim
35 words
A process for preparing an over-based sulfurized phenate according to claim 1, which further comprises, after the carbon dioxide treatment removing any precipitate and a portion of the higher alcohol from the carbon dioxide-treated mixture.
Claim 15
Dependent Claim
45 words
A process for preparing an over-based sulfurized phenate according to claim 1, which further comprises adding a lubricating oil, after the carbon dioxide treatment, to the carbon dioxide-treated mixture, and removing any precipitate and at least a portion of the higher alcohol from said mixture.
Claim 16
Dependent Claim
107 words
A process for the preparation of an over-based sulfurized phenate according to claim 1, which further comprises adding to the carbon dioxide-treated mixture, after the carbon dioxide treatment, an alkaline earth metal reagent selected from the group consisting of an oxide or a hydroxide of an alkaline earth metal and a dihydric alcohol having from 2 to 6 carbon atoms, heating the mixture at from 20* to 200*C, distilling off at a temperature below 200*C substantially all of the water formed in the reaction and a major portion of the unreacted dihydric alcohol, and heating the distillation residue at from 70* to 200*C together with carbon dioxide.
Claim 17
Dependent Claim
37 words
The process of claim 1, wherein the temperature of the reaction mixture after the completion of the sulfurization reaction at from 110* to 200*C is kept at from 20* to 200*C to complete the metal addition reaction.
Claim 18
Dependent Claim
36 words
The process according to claim 1 wherein the weight ratio of the higher alcohol to the phenolic compound when said resultant mixture is heated at a temperature of from 110* to 200*C is at least 3.0.
Claim 19
Dependent Claim
36 words
The process according to claim 1 wherein the weight ratio of the higher alcohol to the phenolic compoUnd when said resultant mixture is heated at a temperature of from 110* to 200*C is at least 10.5.
Claim 20
Dependent Claim
19 words
The process according to claim 1 wherein R is an alkyl group having from 1 to 50 carbon atoms.
Claim 21
Dependent Claim
38 words
The process according too claim 1 wherein said phenolic compound is selected from the group consisting of phenol, butylphenol, amylphenol, octylphenol, dioctylphenol, nonylphenol, dinonylphenol, dodecylphenol, cetylphenol, higher alkyl phenols having groups derived from olefin polymers, and mixtures thereof.
Claim 22
Dependent Claim
17 words
The process according to claim 22 wherein said olefin polymer contains from 9 to 125 carbon atoms.
Claim 23
Dependent Claim
18 words
The process according to claim 22 wherein said olefin polymer contains from about 3,500 to 7,000 carbon atoms.
Claim 24
Dependent Claim
29 words
The process according to claim 1 wherein said elementary sulfur is used in an amount at a level of from 1.0-3.5 g atoms per mole of said phenolic compound.
Claim 25
Dependent Claim
17 words
The process according to claim 1 wherein said higher alcohol has from 9 to 18 carbon atoms.
Claim 26
Dependent Claim
20 words
The process according to claim 1 wherein said resultant mixture is heated at a temperature of from 120* to 190*C.
References Cited (Backward Citations)
US3437595A
Cited
US3464970A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1976-04-02 | 1976-10-02 | 1977-04-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1980-04-02 | 1980-10-02 | 1981-04-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1984-04-02 | 1984-10-02 | 1985-04-03 | $7700.00 | Window Closed / Lapsed |