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 of760 catalyst which is 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: ##STR18## wherein A is ##STR19## x is an integer greater than 1; y is an integer from 0 to about 6; wherein when y is 0, A is ##STR20## 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 compound has the structure: ##STR21## wherein A is ##STR22## 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 and z is 0 when x is 1 and d is 0.

Claim 5

The process of claim 1 wherein the water is removed continuously during the reaction.

Claim 6

The process of claim 1 wherein the water is removed by drawing off a gaseous phase of water and reaction mixture by distillation.

Claim 7

The process of claim 5 wherein the water is separated from the reaction mixture to produce a relatively anhydrous reaction mixture which is recycled to the reaction.

Claim 8

The process of claim 6 wherein the water is separated from the reaction mixture by fractional or azeotropic distillation, or adsorption.

Claim 9

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 10

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

Claim 11

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 respectively.

Claim 12

The process of claim 10 wherein the relative proportion of alkylenediamine to difunctional hydroxy alkylene compound is from about 3:1 to 1:1 respectively.

Claim 13

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 14

The process of claim 12 wherein the alkylenediamine is ethylenediamine or piperazine.

Claim 15

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 16

The process of claims 13 or 14 wherein the difunctional hydroxy alkylene compound is ethylene glycol, monoethanolamine or diethanolamine.

Claim 17

The process of claim 1 wherein the phosphorus acid or acid derivative compound has the structure: ##STR23## 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 substituted 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.

Claim 18

The process of claim 16 wherein the phosphorus acid or acid derivative compound is phosphoric acid, phosphorous acid, boron phosphate, ferric phosphate, aluminum phosphate, hexaethylphosphorous triamide or hexamethylphosphorous triamide.

Claim 19

A process for producing predominantly linearly extended polyalkylene polyamines by reacting an alkylenediamine with a difunctional hydroxy alkylene compound selected from the group consisting of alkylene glycols and alkanolamines in the presence of a catalytically effective amount of catalyst which is a phosphorus acid or acid derivative compound wherein the improvement comprises removing water during the reaction.

Claim 20

A process for producing predominantly linearly extended polyalkylene polyamines by reacting an alkylenediamine with a difunctional hydroxy alkylene compound selected from the group consisting of alkylene glycols and alkanolamines in the presence of a catalytically effective amount of catalyst which is a phosphorus acid or acid derivative compound wherein the improvement comprises removing water during the reaction.

Claim 21

A process for producing predominantly linearly extended polyethylene polyamines by reacting ethylenediamine with at least one of ethylene glycol, monoethanolamine and diethanolamine in the presence of a catalytically effective amount of at least one of phosphoric acid, phosphorous acid, boron phosphate, ferric phosphate, aluminum phosphate, hexaethylphosphorous triamide and hexamethylphosphorous triamide, while removing water to increase reaction conversion rates to said linearly extended polyethylene polyamines.

Claim 22

A process for producing predominantly linearly extended polyethylene polyamines by reacting ethylenediamine with at least one of ethylene glycol, monoethanolamine and diethanolamine in the presence of a catalytically effective amount of at least one of phosphoric acid, phosphorous acid, boron phosphate, ferric phosphate, aluminum phosphate, hexaethylphosphorous triamide and hexamethylphosphorous triamide, while removing water to increase reaction conversion rates to said linearly extended polyethylene polyamines.