Preparation of polyalkylene polyamines using phosphorus amide catalyst

Claim 2

A process for producing predominantly linearly extended polyalkylene polyamines comprising: (a) contacting (i) an alkylenediamine with (ii) a difunctional hydroxy alkylene compound selected from the group consisting of alkylene glycols and alkanolamines; (iii) in the presence of a catalytically effective amount of a phosphorus amide compound having at least one phosphorus-nitrogen bond; and (b) recovering the polyalkylene polyamines.

Claim 3

The process of claim 1 wherein the alkylenediamine reactant has the structure: ##STR30## wherein A is ##STR31## x is an integer greater than 1; y is an integer from 0 to about 6, wherein when y is 0, A is ##STR32## and each R, R 1 , R 2 , R 3 , R 4 and R 5 is a hydrogen or lower alkyl.

Claim 4

The process of claim 1 wherein the difunctional hydroxy alkylene reactant has the structure: ##STR33## wherein A is ##STR34## each R, R 1 , R 2 R 3 , R 4 , and R 5 is hydrogen or lower alkyl; each a, b and c is any integer greater than 1; d is 0 or an integer greater than 1; each x and z is 0 or 1; each w and y is any integer from 0 to about 6; provided that d, w and y are 0 and z is 1 when x is 0; and z is 0 when x is 1 and d is 0.

Claim 5

The process of claim 1 wherein the phosphorus amide compound has at least one phosphorus-nitrogen bond.

Claim 6

The process of claim 1 wherein the phosphorus amide compound has at least one --P--N--C-- or --P--N--H bond.

Claim 7

The process of claim 1 wherein the phosphorus amide compound is a phosphoramidous, phosphordiamidous, phosphoramidic, phosphordiamidic, phosphonamidous, or phosphonamidic acid, ester, half-ester, anhydride, or metal salt, a triamino phosphine or triaminophosphine oxide, a phosphonic or phosphonous diamide, a phosphinic amide, or a phosphonic amide.

Claim 8

The process of claim 1 wherein the phosphorus amide compound is hexyethyl phosphorous triamide or hexamethyl phosphorous triamide.

Claim 9

The process of claim 1 wherein the phosphorus amide compound is a phosphorous or phosphoric alkyleneamide.

Claim 10

The process of claim 8 wherein said phosphorous or phosphoric alkyleneamide is formed by reacting phosphorous or phosphoric acid, or a derivative thereof, with the alkyleneamine reactant of step (a) prior to or during the reaction of step (a) but before contacting with the difunctional hydroxy alkylene compound.

Claim 11

The process according to claim 8 wherein said phosphorous or phosphoric alkyleneamide is a phosphorus amide of ethylenediamine or diethylenetriamine.

Claim 12

The process according to claim 1 wherein the phosphorus amide compound contains a phosphorus atom having an oxidation level of three.

Claim 13

The process of claim 1 wherein the reaction is conducted at temperatures of from above about 250° to about 350° C., at a pressure sufficient to provide a reaction mixture in a liquid phase, for a time period sufficient to provide a total reaction conversion of from about 10% to about 80%.

Claim 14

The process of claim 12 wherein said temperature is from about 275° C., said pressure is from about 200 to 2500 psig, and said time period is from 10 minutes to 20 hours.

Claim 15

The process of claim 1 wherein the relative proportion of alkylenediamine to difunctional hydroxy alkylene compound in mole equivalents is from about 6:1 to about 1:1.

Claim 16

The process of claim 14 wherein the relative proportion of alkylenediamine to difunctional hydroxy alkylene compound is from about 3:1 to 1:1.

Claim 17

The process of claim 2 wherein the alkylenediamine has a structure wherein x is from 2 to about 6; y is from 0 to about 2; and all R groups are hydrogen.

Claim 18

The process of claim 16 wherein the alkylenediamine is ethylenediamine or piperazine.

Claim 19

The process of claim 3 wherein the difunctional hydroxy alkylene compound has a structure wherein a is from 2 to about 6; w is from 0 to about 2; y is 0; and all R groups are hydrogen.

Claim 20

The process of claim 17 or 18 wherein the hydroxy containing compound is ethylene glycol, monoethanolamine or diethanolamine.

Claim 21

A process for producing predominantly linearly extended polyalkylene polyamines comprising reacting an alkylenediamine with a difunctional hydroxy alkylene compound selected from the group consisting of alkylene glycols or alkanolamines, wherein the improvement comprises providing a phosphorus amide catalyst having at least one phosphorus-nitrogen bond.

Claim 22

A process for producing predominantly linearly extended polyalkylene polyamines comprising reacting an alkylenediamine with a difunctional hydroxy alkylene compound selected from the group consisting of alkylene glycols or alkanolamines, wherein the improvement comprises providing a phosphorus amide catalyst having at least one phosphorus-nitrogen bond.

Claim 23

A process for producing predominantly linearly extended polyalkylene polyamines consisting essentially of: (a) contacting (i) an alkylenediamine with (ii) a difunctional hydroxy lower alkylene compound selected from the group consisting of alkylene glycols and alkanolamines; (iii) in the presence of a catalytically effective amount of a phosphorus amide compound having at least one phosphorus-nitrogen bond, said phosphorus amide compound being formed prior to being contacted with said difunctional hydroxy lower alkylene compound; and (b) recovering the polyalkylene polyamines.

Claim 24

A process for producing predominantly linearly extended polyalkylene polyamines consisting essentially of: (a) contacting (i) an alkylenediamine with (ii) a difunctional hydroxy lower alkylene compound selected from the group consisting of alkylene glycols and alkanolamines; (iii) in the presence of a catalytically effective amount of a phosphorus amide compound having at least one phosphorus-nitrogen bond, said phosphorus amide compound being formed prior to being contacted with said difunctional hydroxy lower alkylene compound; and (b) recovering the polyalkylene polyamines.

Claim 25

The process of claim 21 wherein the alkylenediamine reactant has the structure: ##STR35## wherein A is ##STR36## x is an integer from 2 to about 6; y is an integer from 0 to about 6, wherein when Y is 0, A is ##STR37## and each R, R 1 , R 2 , R 3 , R 4 and R 5 is a hydrogen or lower alkyl.