US3879501A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for preparing phosphorus-containing polyols
Assignee: Naphtachimie SA
•
Filing: 1971-12-20
•
Granted: 1975-04-22
•
Expires: 1991-12-20
Abstract
Abstract This invention is addressed to phosphorus-containing polyols prepared by reacting a chloro-chloro-alkyl phosphate having an average of 0.5 to 2.5 chlorine atoms joined directly to a phosphorus atom with a primary or secondary amine having at least one function which is capable of reacting with an organic isocyanate in the presence of water and a hydrogen chloride acceptor whose reaction product with HCl is soluble in water, and the flame or fire resistant polyurethanes prepared by reaction of a phosphorus-containing polyol and an organic polyisocyanate.
Inventors
- 👤 Michel A Buisson
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 20:21
CPC Classifications
C; C07; C07F; C07F9/00; C07F9/02; C07F9/06; C07F9/22; C08; C08G; C08G18/00; C08G18/06; C08G18/28; C08G18/30; C08G18/38; C08G18/3878; C08G18/3889; C08G18/40; C08G18/48; C08G18/50; C08G18/5075; C08G18/509
Claims Analysis
Total Claims: 9
Claim 1
Independent Claim
158 words
A method for the preparation of phosphorus containing compounds comprising the steps of adding to a reaction mixture containing an amine selected from the group consisting of lower mono- and di-alkanol amines and primary and secondary lower alkylene diamines and water, a chloro-chloroalkyl phosphate containing an average of 0.5 to 2.5 chlorine atoms joined directly to a phosphorus atom prepared by reaction of a lower alkylene oxide with phosphorus oxychloride in two or more successive increments to liberate HCl to form a salt with unreacted amine, with each succeeding increment of the chloro-chloroalkyl phosphate containing decreasing amounts of the chloro-chlOroalkyl phosphate, adding to the reaction mixture after each increment of chloro-chloroalkyl phosphate an alkali metal hydroxide in an amount sufficient to displace the HCl from the salt, with the reaction being carried out at a temperature within the range of 30* to 100*C, and separating the aqueous phase to recover the phosphorus containing compound from the organic phase.
Claim 2
Independent Claim
158 words
A method for the preparation of phosphorus containing compounds comprising the steps of adding to a reaction mixture containing an amine selected from the group consisting of lower mono- and di-alkanol amines and primary and secondary lower alkylene diamines and water, a chloro-chloroalkyl phosphate containing an average of 0.5 to 2.5 chlorine atoms joined directly to a phosphorus atom prepared by reaction of a lower alkylene oxide with phosphorus oxychloride in two or more successive increments to liberate HCl to form a salt with unreacted amine, with each succeeding increment of the chloro-chloroalkyl phosphate containing decreasing amounts of the chloro-chlOroalkyl phosphate, adding to the reaction mixture after each increment of chloro-chloroalkyl phosphate an alkali metal hydroxide in an amount sufficient to displace the HCl from the salt, with the reaction being carried out at a temperature within the range of 30* to 100*C, and separating the aqueous phase to recover the phosphorus containing compound from the organic phase.
Claim 3
Independent Claim
157 words
A METHOD FOR THE PREPARATION OF PHOSPHORUS CONTAINING COMPOUNDS COMPRISING THE STEPS OF ADDING TO A REACTION MIXTURE CONTAINING AN AMINE SELECTED FROM THE GROUP CONSISTING OF LOWER MONO- AND DI-ALKANOL AMINES AND PRIMARY AND SECONDARY LOWER ALKYLENE DIAMINES AND WATER, A CHLORO-CHLOROALKYL PHOSPHATE CONTAINING AN AVERAGE OF 0.5 TO 2.5 CHLORINE ATOMS JOINED DIRECTLY TO A PHOSPHORUS ATOM PREPARED BY REACTION OF A LOWER ALKYLENE OXIDE WITH PHOSPHORUS OXYCHLORIDE IN TWO OR MORE SUCCESSIVE INCREMENTS TO LIBERATE HC1 TO FORM A SALT WITH UNREACTED AMINE, WITH EACH SUCCEEDING INCREMENT OF THE CHLORO-CHLOROALKYL PHOSPHATE, ADDING TO THE REACTION OF THE CHLORO-CHOLORALKYL PHOSPHATE, ADDING TO THE REACTION MIXTURE AFTER EACH INCREMENT OF CHLORO-CHLOROALKYL PHOSPHATE AN ALKALI METAL HYDROXIDE IN AN AMOUNT SUFFICIENT TO DISPLACE THE HC1 FROM THE SALT, WITH THE REACTION BEING CARRIED OUT AT A TEMPERATURE WITH THE RANGE OF 30*C, AND SEPARATING THE AQUEOUS PHASE TO RECOVER THE PHOSPHORUS CONTAINING COMPOUND FROM THE ORGANIC PHASE.
Claim 4
Independent Claim
157 words
A METHOD FOR THE PREPARATION OF PHOSPHORUS CONTAINING COMPOUNDS COMPRISING THE STEPS OF ADDING TO A REACTION MIXTURE CONTAINING AN AMINE SELECTED FROM THE GROUP CONSISTING OF LOWER MONO- AND DI-ALKANOL AMINES AND PRIMARY AND SECONDARY LOWER ALKYLENE DIAMINES AND WATER, A CHLORO-CHLOROALKYL PHOSPHATE CONTAINING AN AVERAGE OF 0.5 TO 2.5 CHLORINE ATOMS JOINED DIRECTLY TO A PHOSPHORUS ATOM PREPARED BY REACTION OF A LOWER ALKYLENE OXIDE WITH PHOSPHORUS OXYCHLORIDE IN TWO OR MORE SUCCESSIVE INCREMENTS TO LIBERATE HC1 TO FORM A SALT WITH UNREACTED AMINE, WITH EACH SUCCEEDING INCREMENT OF THE CHLORO-CHLOROALKYL PHOSPHATE, ADDING TO THE REACTION OF THE CHLORO-CHOLORALKYL PHOSPHATE, ADDING TO THE REACTION MIXTURE AFTER EACH INCREMENT OF CHLORO-CHLOROALKYL PHOSPHATE AN ALKALI METAL HYDROXIDE IN AN AMOUNT SUFFICIENT TO DISPLACE THE HC1 FROM THE SALT, WITH THE REACTION BEING CARRIED OUT AT A TEMPERATURE WITH THE RANGE OF 30*C, AND SEPARATING THE AQUEOUS PHASE TO RECOVER THE PHOSPHORUS CONTAINING COMPOUND FROM THE ORGANIC PHASE.
Claim 5
Dependent Claim
45 words
A method as defined in claim 1 wherein the chloro-chloroalkyl phosphate is prepared by reacting phosphorus oxychloride with an alkylene oxide at a temperature of 0* to 100*C. in a mole ratio of 0.5 to 2.5 moles of alkylene oxide per mole of phosphorus oxychloride.
Claim 6
Dependent Claim
25 words
A method as defined in claim 2 wherein the alkylene oxide is selected from the group consisting of ethylene oxide, propylene oxide and mixtures thereof.
Claim 7
Dependent Claim
38 words
A method as defined in claim 1 wherein the chloro-chloroalkyl phosphate and the amine are reacted in a ratio of about 1 mole of amine per chlorine atom joined directly to a phosphorus atom in the chloro-chloroalkyl phosphate.
Claim 8
Dependent Claim
27 words
A method as defined in claim 1 wherein the reaction mixture contains sufficient water to completely dissolve the reaction product of the hydrogen chloride acceptor with HCl.
Claim 9
Dependent Claim
38 words
A method as defined in claim 1 wherein the reaction mixture contains an amount of water ranging up to 1.5 times the quantity of water necessary to dissolve the reaction product of the hydrogen chloride acceptor and HCl.
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) | 1978-04-21 | 1978-10-21 | 1979-04-22 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-04-21 | 1982-10-21 | 1983-04-22 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-04-21 | 1986-10-21 | 1987-04-22 | $7700.00 | Window Closed / Lapsed |