Preparation of polyalkylene polyamines

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 acid or acid derivative compound; b) removing water during the reaction; and c) recovering the polyalkylene polyamines.

Claim 3

The process of claim 1 wherein the- alkylenediamine has the structure: wherein A is or x is an integer greater tnan 1; y is an integer from 0 to about 6; wherein when y is 0, A is 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 or 2 wherein the difunctional hydroxy alkylene compound has the structure : wherein A is or each R, Rl, R2 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 to 3 wherein the water is removed continuously during the reaction.

Claim 6

The process of claim 1 to 3 wherein the water is removed by drawing off a gaseous phase of water and reaction mixture by distillation or is separated from tne reaction mixture to produce a relatively anhydrous reaction mixture which is recycled to the reaction or is separated from the reaction mixture by fractional or azeotropic distillation, or adsorption.

Claim 7

The process of claim 1 to 5 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 8

The process of claim 6 wherein said pressure is from about 13,8 200 to 172,5 bar 2500 psig, and said time period is from 10 minutes to 20 hours.

Claim 9

The process of claim 1 to 7 wherein the relative proportion of alkylenediamine to difunctional hydroxy alkylene compound in mole equivalents is from about 6:1 to about 1:1 respectively, preferably from about 3:1 to 1:1 respectively.

Claim 10

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 and is preferably ethylenediamine or piperazine.

Claim 11

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. 13440 11. The process of claims 9 or 10 wherein the difunctional hydroxy alkylene compound is ethylene glycol, monoethanolamine or diethanolamine. 12. The process of claim 1 to 11 wherein the phosphorus acid or acid derivative compound has the structure: wherein Y is an oxygen or sulfur atom; m is 0 or 1; X is hydroxy, alkoxy, aryloxy, or the thioanalogs of the foregoing, alkyl or aryl substitutea amino, halo, or the salts or phosphorus anhydrides or thioanhydrides of the foregoing when X is hydroxy or mercapto; R' and R" are hydrogen, alkyl, aryl or one of the groups previously defined by X and is preferably phosphoric acid, phosphorous acid, boron phosphate, ferric phosphate, aluminum phosphate, hexaethylphosphorous triamide or hexamethylphosphorous triamide.