US4670575A
Expired / Lapsed
US
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Process for purification of phosphoric mono esters
Assignee: Kao Corp
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Filing: 1985-05-24
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Granted: 1987-06-02
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Expires: 2005-05-24
Abstract
Abstract A novel process for producing a phosphoric monoester which comprises reacting per 1 mole of a linear or branched, saturated or non-saturated aliphatic alcohol having from 8 to 36 carbon atoms, from 2 to 10 moles of a polyphosphoric acid at 100 to 116% concetration converted as orthophosphoric acid in (a) one or more solvents selected from the group consisting of linear or branched saturated aliphatic hydrocarbons having from 4 to 8 carbon atoms and saturated cycloaliphatic hydrocarbons having from 5 to 7 carbon atoms, then adding (b) a lower alcohol having from 1 to 4 carbon atoms and water to the reaction mixture, transferring the orthophosphoric acid to the lower alcohol-aqueous phase to separate it from the phosphoric monoester, and concentrating the thus recovered orthophosphoric acid for reuse. The process reaction proceeds smoothly, separation and purification can be carried out readily and very effectively and the recovered phosphoric acid can be re-used.
Inventors
- 👤 Tomihiro Kurosaki
- 👤 Junya Wakatsuki
- 👤 Hisakazu Furugaki
- 👤 Katsutoshi Kojima
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 10:37
CPC Classifications
C; C07; C07F; C07F9/00; C07F9/02; C07F9/06; C07F9/08; C07F9/09; C07F9/025
Claims Analysis
Total Claims: 8
Claim 1
Independent Claim
92 words
A process for purifying a monoalkyl phosphoric ester having 8-32 C atoms from a mixture comprising said monoalkyl phosphoric ester and orthophosphoric acid, which comprises: adding, as a solvent, (a) one or more materials selected from the group consisting of linear or branched saturated aliphatic hydrocarbons having from 4 to 8 carbon atoms and saturated cycloaliphatic hydrocarbons having from 5 to 7 carbon atoms and (b) a lower alcohol having from 1 to 4 carbon atoms and water to said mixture thereby isolating and separating the phosphoric ester in the hydrocarbon phase.
Claim 2
Dependent Claim
92 words
A process for purifying a monoalkyl phosphoric ester having 8-32 C atoms from a mixture comprising said monoalkyl phosphoric ester and orthophosphoric acid, which comprises: adding, as a solvent, (a) one or more materials selected from the group consisting of linear or branched saturated aliphatic hydrocarbons having from 4 to 8 carbon atoms and saturated cycloaliphatic hydrocarbons having from 5 to 7 carbon atoms and (b) a lower alcohol having from 1 to 4 carbon atoms and water to said mixture thereby isolating and separating the phosphoric ester in the hydrocarbon phase.
Claim 3
Dependent Claim
43 words
The purification process as defined in claim 1, wherein the phosphoric ester mainly consists of a compound represented by the following general formula (I): ##STR3## where R represents a linear or branched alkyl or alkenyl group having from 8 to 36 carbon atoms.
Claim 4
Dependent Claim
14 words
The purification process as defined in claim 1, wherein the lower alcohol is isopropanol.
Claim 5
Dependent Claim
102 words
A process for purifying a phosphoric ester, which comprises adding to a mixture containing a phosphoric ester and orthophosphoric acid, (a) at least one material selected from the group consisting of linear or branched saturated aliphatic hydrocarbons having from 4 to 8 carbon atoms and saturated cycloaliphatic hydrocarbons having from 5 to 7 carbon atoms and (b) a lower alcohol having from 1 to 4 carbon atoms and water, isolating the phosphoric ester into the hydrocarbon phase, removing the lower alcohol and water incorporated into the hydrocarbon phase through azeotropic distillation to produce a residue and then recrystallizing or topping the residue.
Claim 6
Dependent Claim
102 words
A process for purifying a phosphoric ester, which comprises adding to a mixture containing a phosphoric ester and orthophosphoric acid, (a) at least one material selected from the group consisting of linear or branched saturated aliphatic hydrocarbons having from 4 to 8 carbon atoms and saturated cycloaliphatic hydrocarbons having from 5 to 7 carbon atoms and (b) a lower alcohol having from 1 to 4 carbon atoms and water, isolating the phosphoric ester into the hydrocarbon phase, removing the lower alcohol and water incorporated into the hydrocarbon phase through azeotropic distillation to produce a residue and then recrystallizing or topping the residue.
Claim 7
Dependent Claim
33 words
The process of claim 1, wherein said phosphoric ester is monooctyl phosphate, monodecyl phosphate, monooctadecyl phosphate, monotetracosyl phosphate, monooctacosyl phosphate, monooctenyl phosphate, monooctadecenyl phosphate, monotetracosenyl phosphate, mon-2-hexyldecyl phosphate, mono-2-octylundecyl phosphate or mono-2-tetradecyloctadecyl phosphate.
Claim 8
Dependent Claim
33 words
The process of claim 4, wherein said phosphoric ester is monooctyl phosphate, monodecyl phosphate, monooctadecyl phosphate, monotetracosyl phosphate, monooctacosyl phosphate, monooctenyl phosphate, monooctadecenyl phosphate, monotetracosenyl phosphate, mono-2-hexyldecyl phosphate, mono-2-octylundecyl phosphate or mono-2-tetradecyloctadecyl phosphate.
References Cited (Backward Citations)
US2658909A
Cited
US4410466A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1990-06-01 | 1990-12-01 | 1991-06-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1994-06-01 | 1994-12-01 | 1995-06-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1998-06-01 | 1998-12-01 | 1999-06-02 | $7700.00 | Window Closed / Lapsed |