Patent US4143059A successfully refreshed from Google Patents.
US4143059A
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Process for preparing aluminum ethyl phosphite
Assignee: Bayer CropScience SA
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Filing: 1977-11-15
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Granted: 1979-03-06
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Expires: 1997-11-15
Abstract
Abstract Aluminum ethyl phosphite, useful as a plant fungicide, is made in an industrial process in high yield and good quality by reacting an excess of a ternary mixture of diethyl phosphite, monoethyl phosphite and phosphoric acid, with alumina at 20-200° C. under subatmospheric pressure, while eliminating water formed during the reaction.
Inventors
- 👤 Jean Abblard
- 👤 Michel Ghazarian
- 👤 Rene Viricel
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 17:29
CPC Classifications
C; C07; C07F; C07F9/00; C07F9/02; C07F9/06; C07F9/08; C07F9/141; C07F9/142
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
62 words
A process for manufacturing aluminum ethyl phosphite which comprises reacting an excess of a ternary mixture in equilibrium of, in mols: 23 to 93% diethyl phosphite, 59 to 7% monoethyl phosphite, 18 to 0.1% phosphoric acid with alumina at a temperature between 20° and 100° C., at subatmospheric pressure, the water resulting from the reaction being simultaneously eliminated as it is formed.
Claim 2
Dependent Claim
62 words
A process for manufacturing aluminum ethyl phosphite which comprises reacting an excess of a ternary mixture in equilibrium of, in mols: 23 to 93% diethyl phosphite, 59 to 7% monoethyl phosphite, 18 to 0.1% phosphoric acid with alumina at a temperature between 20° and 100° C., at subatmospheric pressure, the water resulting from the reaction being simultaneously eliminated as it is formed.
Claim 3
Dependent Claim
29 words
A process according to claim 1, wherein the starting ternary mixture comprises, in mols: 35 to 78% diethyl phosphite, 54 to 20% monoethyl phosphite, 11 to 1% phosphoric acid.
Claim 4
Dependent Claim
12 words
A process according to claim 1, wherein the alumina is a hydrargillite.
Claim 5
Dependent Claim
16 words
A process according to claim 1, wherein said alumina is in the hydrated or gel form.
Claim 6
Dependent Claim
24 words
A process according to claim 1, wherein the ternary mixture is present in a 50 to 200% (in mols) excess with respect to stoichiometry.
Claim 7
Dependent Claim
26 words
A process according to claim 5, wherein said ternary mixture comprises: 35 to 78% diethyl phosphite, 54 to 20% monoethyl phosphite, 11 to 1% phosphoric acid.
Claim 8
Dependent Claim
18 words
A process according to claim 1, wherein the temperature during said reaction is between 40° and 70° C.
Claim 9
Dependent Claim
39 words
A process according to claim 1, wherein when the temperature reaches 100° C., the reactor is reset to atmospheric pressure, and heated to 150° C., then kept at this latter temperature for a few minutes to complete the reaction.
Claim 10
Dependent Claim
28 words
A process according to claim 1, further comprising, after said reaction, cooling the mixture to ambient temperature, recovering precipitated aluminum ethyl phosphite, and spin-drying and washing said precipitate.
Claim 11
Dependent Claim
48 words
A process according to claim 1, further comprising, after said reaction, recovering aluminum ethyl phosphite and mother liquor, cooling and recycling the mother liquor, topping up the phosphite mixture in the mother liquor to the starting molar quantity, adding a stoichiometric quantity of alumina and repeating the reaction.
Claim 12
Dependent Claim
41 words
A process according to claim 1, wherein the ternary mixture is prepared from a mixture of (in mols) 55 to 98% diethyl phosphite, and 45 to 2% phosphoric acid, which is heated to 150° C. for 15 minutes to 1 hour.
Claim 13
Dependent Claim
24 words
A process according to claim 11, wherein the starting mixture comprises (in mols): 64 to 90% diethyl phosphite, and 36 to 10% phosphoric acid.
Claim 14
Dependent Claim
27 words
A process according to claim 1, wherein the ternary mixture is prepared by the action of phosphorus trichloride on an ethanol-water mixture according to the reaction: ##STR2##
Claim 15
Dependent Claim
34 words
A process according to claim 13, wherein said phosphorus trichloride is poured on said ethanol-water mixture at a temperature between 0° and 20° C. and the hydrochloric acid is eliminated as it is formed.
Claim 16
Dependent Claim
20 words
A process according to claim 3, wherein the hydrargillite has a specific surface of 5 to 30 m 2 /g.
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) | 1982-03-05 | 1982-09-04 | 1983-03-06 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-03-05 | 1986-09-04 | 1987-03-06 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-03-05 | 1990-09-04 | 1991-03-06 | $7700.00 | Window Closed / Lapsed |