US4085053A
Expired / Lapsed
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Metal dithiophosphate process and/composition
Assignee: Ethyl Corp
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Filing: 1977-05-23
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Granted: 1978-04-18
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Expires: 1997-05-23
Abstract
Abstract Disclosed are a process for manufacturing metal dithiophospates, and metal dithiophosphate compositions. The process for manufacturing zinc, barium, cadmium, magnesium or nickel dithiophosphates comprises reacting phosphorus pentasulfide with one or more alcohols to form a dithiophosphoric acid; neutralizing said dithiophosphoric acid with zinc, barium, cadmium, magnesium or nickel base in the presence of an acidic promoter; and reacting a substantial portion of the excess acidic promoter with a weak base. The metal dithiophosphates and lubricating oils containing said dithiophosphates are also disclosed.
Inventors
- 👤 Gunter Caspari
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 21:32
CPC Classifications
C; C10; C10M; C10M137/00; C10M137/02; C10M137/04; C10M137/10; C07; C07F; C07F9/00; C07F9/02; C07F9/06; C07F9/16; C07F9/165; C10M2207/00; C10M2207/40; C10M2207/402; C10M2207/404; C10M2223/00; C10M2223/02; C10M2223/04; C10M2223/045; C10N; C10N2010/00; C10N2010/04; C10N2010/14; C10N2010/16
Claims Analysis
Total Claims: 44
Claim 1
Independent Claim
70 words
A lubricating oil composition comprising a major proportion of a lubricating oil and an effective amount of an oil soluble antiwear additive, said additive comprising a zinc, barium, cadmium, magnesium or nickel dithiophosphate, said dithiophosphate made by neutralization of dithiophosphoric acid with zinc, barium, cadmium, magnesium or nickel base in the presence of an acidic promoter followed by reacting a substantial portion of excess acidic promoter with a weak base.
Claim 2
Dependent Claim
70 words
A lubricating oil composition comprising a major proportion of a lubricating oil and an effective amount of an oil soluble antiwear additive, said additive comprising a zinc, barium, cadmium, magnesium or nickel dithiophosphate, said dithiophosphate made by neutralization of dithiophosphoric acid with zinc, barium, cadmium, magnesium or nickel base in the presence of an acidic promoter followed by reacting a substantial portion of excess acidic promoter with a weak base.
Claim 3
Dependent Claim
12 words
The composition of claim 1 wherein the dithiophoshphate is a zinc dithiophosphate.
Claim 4
Dependent Claim
12 words
The composition of claim 2 wherein the dithiophosphate is a zinc dialkyldithiophosphate.
Claim 5
Dependent Claim
12 words
The composition of claim 2 wherein the dithiophosphate is a zinc diaryldithiophosphate.
Claim 6
Dependent Claim
13 words
The composition of claim 2 wherein dithiophosphoric acid is neutralized with zinc oxide.
Claim 7
Dependent Claim
12 words
The composition of claim 1 wherein the acidic promoter is nitric acid.
Claim 8
Dependent Claim
18 words
The composition of claim 1 wherein the molar ratio of weak base to acidic promoter is about 0.5-10:1.
Claim 9
Dependent Claim
18 words
The composition of claim 7 wherein the molar ratio of weak base to acidic promoter is about 1-3:1.
Claim 10
Dependent Claim
30 words
The composition of claim 1 wherein the weak base forms a salt with the acidic promoter and does not replace the zinc, barium, cadmium, magnesium or nickel in the dithiophosphate.
Claim 11
Dependent Claim
11 words
The composition of claim 9 wherein the weak base contains nitrogen.
Claim 12
Dependent Claim
12 words
The composition of claim 10 wherein the base comprises ammonia or urea.
Claim 13
Dependent Claim
21 words
The composition of claim 1 wherein the additive is present at a concentration of about 0.05 to about 5 weight percent.
Claim 14
Dependent Claim
21 words
The composition of claim 12 wherein the additive is present at a concentration of about 0.1 to about 3 weight percent.
Claim 15
Dependent Claim
30 words
The composition of claim 1 wherein the lubricating oil has a viscosity from about 40 Saybolt Universal seconds at 100° F. to about 200 Saybolt Universal seconds at 210° F.
Claim 16
Dependent Claim
60 words
A process for the manufacture of zinc, barium, cadmium, magnesium or nickel dithiophosphate comprising reacting phosphorus pentasulfide with one or more alcohols to form a dithiophosphoric acid; neutralizing said dithiophosphoric acid with zinc, barium, cadmium, magnesium or nickel base in the presence of an acidic promoter; and reacting a substantial portion of the excess acidic promoter with a weak base.
Claim 17
Dependent Claim
60 words
A process for the manufacture of zinc, barium, cadmium, magnesium or nickel dithiophosphate comprising reacting phosphorus pentasulfide with one or more alcohols to form a dithiophosphoric acid; neutralizing said dithiophosphoric acid with zinc, barium, cadmium, magnesium or nickel base in the presence of an acidic promoter; and reacting a substantial portion of the excess acidic promoter with a weak base.
Claim 18
Dependent Claim
11 words
The process of claim 15 for the manufacture of zinc dithiophosphate.
Claim 19
Dependent Claim
61 words
The process of claim 15 wherein the phosphorus pentasulfide is reacted with alcohol at a temperature from about 100° F. to about 250° F., the dithiophosphoric acid is neutralized at a temperature from about 100° F. to about 250° F., and the acidic promoter is reacted with a weak base at a temperature from about 100° F. to about 250° F.
Claim 20
Dependent Claim
52 words
The process of claim 15 wherein the molar ratio of phosphorus pentasulfide to alcohol is about 1 to 4, the molar ratio of dithiophosphoric acid to zinc, barium, cadmium, magnesium or nickel base is about 1 to 0.6, and the molar ratio of weak base to acidic promoter is 1.5 to 1.
Claim 21
Dependent Claim
11 words
The process of claim 15 wherein the alcohol comprises alkyl alcohols.
Claim 22
Dependent Claim
16 words
The process of claim 19 wherein the alcohol contains about 3 to about 20 carbon atoms.
Claim 23
Dependent Claim
11 words
The process of claim 15 wherein the alcohol comprises aryl alcohols.
Claim 24
Dependent Claim
16 words
The process of claim 21 wherein the alcohol contains about 6 to about 30 carbon atoms.
Claim 25
Dependent Claim
16 words
The process of claim 15 wherein the dithiophosphoric acid is neutralized with zinc oxide or carbonate.
Claim 26
Dependent Claim
11 words
The process of claim 15 wherein the promoter is nitric acid.
Claim 27
Dependent Claim
21 words
The process of claim 15 wherein about 0.001 to about 0.5 moles of promoter are used per mole of dithiophosphoric acid.
Claim 28
Dependent Claim
29 words
The process of claim 15 wherein the weak base forms a salt with the acidic promoter and does not replace zinc, barium, cadmium, magnesium or nickel in the dithiophosphate.
Claim 29
Dependent Claim
10 words
The process of claim 26 wherein the base contains nitrogen.
Claim 30
Dependent Claim
12 words
The process of claim 27 wherein the base comprises ammonia or urea.
Claim 31
Dependent Claim
74 words
A process for the manufacture of zinc, barium, cadmium, magnesium or nickel dithiophosphates comprising reacting one mole phosphorus pentasulfide with about four moles of alcohol to form a dithiophosphoric acid; combining said dithiophosphoric acid with zinc, barium, cadmium, magnesium or nickel base in the presence of an acidic promoter to form a neutralization mixture and neutralizing said dithiophosphoric acid; and adding a weak base to the neutralization mixture after the neutralization is essentially complete.
Claim 32
Dependent Claim
74 words
A process for the manufacture of zinc, barium, cadmium, magnesium or nickel dithiophosphates comprising reacting one mole phosphorus pentasulfide with about four moles of alcohol to form a dithiophosphoric acid; combining said dithiophosphoric acid with zinc, barium, cadmium, magnesium or nickel base in the presence of an acidic promoter to form a neutralization mixture and neutralizing said dithiophosphoric acid; and adding a weak base to the neutralization mixture after the neutralization is essentially complete.
Claim 33
Dependent Claim
47 words
A composition comprising zinc, barium, cadmium, magnesium or nickel dithiophosphate, said dithiophosphate made by neutralization of dithiophosphoric acid with zinc, barium, cadmium, magnesium or nickel base in the presence of an acidic promoter followed by reacting a substantial portion of excess acidic promoter with a weak base.
Claim 34
Dependent Claim
47 words
A composition comprising zinc, barium, cadmium, magnesium or nickel dithiophosphate, said dithiophosphate made by neutralization of dithiophosphoric acid with zinc, barium, cadmium, magnesium or nickel base in the presence of an acidic promoter followed by reacting a substantial portion of excess acidic promoter with a weak base.
Claim 35
Dependent Claim
12 words
The composition of claim 30 wherein the dithiophosphate is a zinc dithiophosphate.
Claim 36
Dependent Claim
12 words
The composition of claim 30 wherein the dithiophosphate is a zinc dialkyldithiophosphate.
Claim 37
Dependent Claim
12 words
The composition of claim 31 wherein the dithiophosphate is a zinc diaryldithiophosphate.
Claim 38
Dependent Claim
13 words
The composition of claim 31 wherein dithiophoric acid is neutralized with zinc oxide.
Claim 39
Dependent Claim
12 words
The composition of claim 30 wherein the acidic promoter is nitric acid.
Claim 40
Dependent Claim
18 words
The composition of claim 30 wherein the molar ratio of weak base to acidic promoter is about 0.5-10:1.
Claim 41
Dependent Claim
18 words
The composition of claim 36 wherein the molar ratio of weak base to acidic promoter is about 1-3:1.
Claim 42
Dependent Claim
30 words
The composition of claim 30 wherein the weak base forms a salt with the acidic promoter and does not replace the zinc, barium, cadmium, magnesium or nickel in the dithiophosphate.
Claim 43
Dependent Claim
11 words
The composition of claim 38 wherein the weak base contains nitrogen.
Claim 44
Dependent Claim
12 words
The composition of claim 39 wherein the base comprises ammonia or urea.
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) | 1981-04-17 | 1981-10-17 | 1982-04-18 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-04-17 | 1985-10-17 | 1986-04-18 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-04-17 | 1989-10-17 | 1990-04-18 | $7700.00 | Window Closed / Lapsed |