Process for preparing aliphatic diperoxydicarboxylic acids

Claim 2

A process for preparing a saturated C 6 -C 16 aliphatic diperoxydicarboxylic acid which comprises the steps of bringing together and reacting, a saturated C 6 -C 16 aliphatic dicarboxylic acid and hydrogen peroxide in a phosphoric acid reaction medium in a reaction zone, wherein the molecular ratio of said dicarboxylic acid and hydrogen peroxide is within the range of from about 1:2 to about 1:5, whereby there is formed a reaction slurry in said reaction zone, the amount of phosphoric acid employed being sufficient to provide an easily stirrable reaction mixture and to predissolve the dicarboxylic acid reactant at temperatures between about 60°-100° C.; maintaining the reaction slurry in an agitated condition; maintaining the temperature of the reaction slurry within the range of from about 20° to about 70° C. during the reaction period and thereafter separating the diperoxydicarboxylic acid from the reaction slurry.

Claim 3

Process of claim 1 wherein the hydrogen peroxide has a concentration within the range of from about 30 to about 90%.

Claim 4

Process of claim 2 wherein the hydrogen peroxide has a concentration of at least about 65%.

Claim 5

Process of claim 1 wherein the molecular ratio of dicarboxylic acid and hydrogen peroxide is within the range of from about 1:3 to 1:4.

Claim 6

Process of claim 1 wherein the phosphoric acid has a concentration within the range of from about 70 to about 100%.

Claim 7

Process of claim 5 wherein the phosphoric acid has a concentration within the range of from about 85 to about 95%.

Claim 8

Process of claim 1 wherein the molecular ratio of the dicarboxylic acid and phosphoric acid is within the range of from about 1:6 to about 1:15.

Claim 9

Process of claim 7 wherein the molecular ratio of the dicarboxylic acid and phosphoric acid is within the range of from about 1:8 to about 1:12.

Claim 10

Process of claim 1 wherein the dicarboxylic acid is dissolved in the phosphoric acid reaction medium prior to being brought together and reacted with the hydrogen peroxide.

Claim 11

Process of claim 1 wherein the dicarboxylic acid reactant is azelaic acid.

Claim 12

Process of claim 1 wherein the dicarboxylic acid reactant is dodecanedioic acid.

Claim 13

A process for preparing a saturated C 6 -C 16 aliphatic diperoxydicarboxylic acid which comprises the steps of bringing together and reacting, a saturated C 6 - 16 aliphatic dicarboxylic acid and hydrogen peroxide having a concentration within the range of from about 30% to about 90%, in a phosphoric acid reaction medium, in a reaction zone, wherein the molecular ratio of said dicarboxylic acid and hydrogen peroxide is within the range of from about 1:2 to about 1:5, the phosphoric acid having a concentration within the range of from about 70 to about 100%, the molecular ratio of dicarboxylic acid and phosphoric acid being within the range of from about 1:6 to about 1:15, whereby there is formed a reaction slurry in said reaction zone; maintaining the reaction slurry in an agitated condition; maintaining the temperature of the reaction slurry within the range of from about 20° to about 70° C. and thereafter separating the diperoxydicarboxylic acid from the reaction slurry.

Claim 14

A process for preparing a saturated C 6 -C 16 aliphatic diperoxydicarboxylic acid which comprises the steps of bringing together and reacting, a saturated C 6 - 16 aliphatic dicarboxylic acid and hydrogen peroxide having a concentration within the range of from about 30% to about 90%, in a phosphoric acid reaction medium, in a reaction zone, wherein the molecular ratio of said dicarboxylic acid and hydrogen peroxide is within the range of from about 1:2 to about 1:5, the phosphoric acid having a concentration within the range of from about 70 to about 100%, the molecular ratio of dicarboxylic acid and phosphoric acid being within the range of from about 1:6 to about 1:15, whereby there is formed a reaction slurry in said reaction zone; maintaining the reaction slurry in an agitated condition; maintaining the temperature of the reaction slurry within the range of from about 20° to about 70° C. and thereafter separating the diperoxydicarboxylic acid from the reaction slurry.

Claim 15

Process of claim 12 wherein the hydrogen peroxide has a concentration of at least about 65%.

Claim 16

Process of claim 12 wherein the phosphoric acid has a concentration within the range of from about 85 to about 95%.

Claim 17

Process of claim 12 wherein the molecular ratio of dicarboxylic acid to phosphoric acid is within the range of from about 1:8 to about 1:12.

Claim 18

Process of claim 12 wherein the dicarboxylic acid is dissolved in the phosphoric acid reaction medium prior to being brought together and reacted with the hydrogen peroxide.

Claim 19

Process of claim 12 wherein the dicarboxylic acid reactant is azelaic acid.

Claim 20

Process of claim 12 wherein the dicarboxylic acid reactant is dodecanedioic acid.

Claim 21

A process for preparing a saturated C 12 -C 16 aliphatic diperoxydicarboxylic acid which comprises the steps of bringing together and reacting, a saturated C 12 -C 16 aliphatic dicarboxylic acid and hydrogen peroxide in a phosphoric acid reaction medium containing up to about 5% by weight of the phosphoric acid of a stronger acid selected from the group consisting of sulfuric acid, methanesulfonic acid, trifluromethanesulfonic acid and toluenesulfonic acid, in a reaction zone wherein the molecular ratio of said dicarboxylic acid and hydrogen peroxide is within the range of from 1:2 to about 1:5, whereby there is formed a reaction slurry in said reaction zone, the amount of phosphoric acid employed being sufficient to provide an easily stirrable reaction mixture and to predissolve the dicarboxylic acid reactant at temperatures between about 60°-100° C.; maintaining the reaction slurry in an agitated condition; maintaining the temperature of the reaction slurry within the range of from about 20° to about 70° C. during the reaction period and thereafter separating the diperoxydicarboxylic acid from the reaction slurry.

Claim 22

A process for preparing a saturated C 12 -C 16 aliphatic diperoxydicarboxylic acid which comprises the steps of bringing together and reacting, a saturated C 12 -C 16 aliphatic dicarboxylic acid and hydrogen peroxide in a phosphoric acid reaction medium containing up to about 5% by weight of the phosphoric acid of a stronger acid selected from the group consisting of sulfuric acid, methanesulfonic acid, trifluromethanesulfonic acid and toluenesulfonic acid, in a reaction zone wherein the molecular ratio of said dicarboxylic acid and hydrogen peroxide is within the range of from 1:2 to about 1:5, whereby there is formed a reaction slurry in said reaction zone, the amount of phosphoric acid employed being sufficient to provide an easily stirrable reaction mixture and to predissolve the dicarboxylic acid reactant at temperatures between about 60°-100° C.; maintaining the reaction slurry in an agitated condition; maintaining the temperature of the reaction slurry within the range of from about 20° to about 70° C. during the reaction period and thereafter separating the diperoxydicarboxylic acid from the reaction slurry.

Claim 23

Process of claim 19 wherein the stronger acid is sulfuric acid.

Claim 24

Process of claim 19 wherein the stronger acid is methanesulfonic acid.

Claim 25

Process of claim 19 wherein the stronger acid is trifluoromethanesulfonic acid.

Claim 26

Process of claim 19 wherein the stronger acid is toluenesulfonic acid.

Claim 27

Process of claim 19 wherein the hydrogen peroxide concentration is within the range of from about 30 to about 90%.

Claim 28

Process of claim 24 wherein the hydrogen peroxide has a concentration of at least about 65%.

Claim 29

Process of claim 19 wherein the molecular ratio of dicarboxylic acid and hydrogen peroxide is within the range of from about 1:3 to about 1:4.

Claim 30

Process of claim 19 wherein the phosphoric acid concentration is within the range of from about 70 to about 100%.

Claim 31

Process of claim 27 wherein the phosphoric acid has a concentration within the range of from about 85 to about 95%.

Claim 32

Process of claim 19 wherein the molecular ratio of dicarboxylic acid and phosphoric acid is within the range of from about 1:6 to about 1:15.

Claim 33

Process of claim 29 wherein the molecular ratio of the dicarboxylic acid and phosphoric acid is within the range of from about 1:8 to about 1:12.

Claim 34

Process of claim 19 wherein the dicarboxylic acid is dissolved in the phosphoric acid reaction medium prior to being brought together and reacted with the hydrogen peroxide.

Claim 35

Process of claim 19 wherein the dicarboxylic acid reactant is azelaic acid.

Claim 36

Process of claim 19 wherein the dicarboxylic acid reactant is dodecanedioic acid.

Claim 37

A process for preparing a saturated C 12 -C 16 aliphatic diperoxydicarboxylic acid which comprises the steps of bringing together and reacting, a saturated C 12 -C 16 aliphatic dicarboxylic acid and hydrogen peroxide having a concentration within the range of from about 30 to about 90%, in a phosphoric acid reaction medium containing up to about 5% by weight of the phosphoric acid selected from the group consisting of sulfuric acid, methanesulfonic acid, trifluromethanesulfonic acid and toluenesulfonic acid of a stronger acid, in a reaction zone, wherein the molecular ratio of said dicarboxylic acid and hydrogen peroxide is within the range of from about 1:2 to about 1:5, the phosphoric acid having a concentration within the range of from about 70 to about 100%, the molecular ratio of dicarboxylic acid and phosphoric acid being within the range of from about 1:6 to about 1:15, whereby there is formed a reaction slurry in said reaction zone; maintaining the reaction slurry in an agitated condition; maintaining the temperature of the reaction slurry within the range of from about 20° to about 70° C. and thereafter separating the diperoxydicarboxylic acid from the reaction slurry.

Claim 38

A process for preparing a saturated C 12 -C 16 aliphatic diperoxydicarboxylic acid which comprises the steps of bringing together and reacting, a saturated C 12 -C 16 aliphatic dicarboxylic acid and hydrogen peroxide having a concentration within the range of from about 30 to about 90%, in a phosphoric acid reaction medium containing up to about 5% by weight of the phosphoric acid selected from the group consisting of sulfuric acid, methanesulfonic acid, trifluromethanesulfonic acid and toluenesulfonic acid of a stronger acid, in a reaction zone, wherein the molecular ratio of said dicarboxylic acid and hydrogen peroxide is within the range of from about 1:2 to about 1:5, the phosphoric acid having a concentration within the range of from about 70 to about 100%, the molecular ratio of dicarboxylic acid and phosphoric acid being within the range of from about 1:6 to about 1:15, whereby there is formed a reaction slurry in said reaction zone; maintaining the reaction slurry in an agitated condition; maintaining the temperature of the reaction slurry within the range of from about 20° to about 70° C. and thereafter separating the diperoxydicarboxylic acid from the reaction slurry.

Claim 39

Process of claim 34 wherein the stronger acid is sulfuric acid.

Claim 40

Process of claim 34 wherein the stronger acid is methanesulfonic acid.

Claim 41

Process of claim 34 wherein the stronger acid is trifluoromethanesulfonic acid.

Claim 42

Process of claim 34 wherein the stronger acid is toluenesulfonic acid.

Claim 43

Process of claim 34 wherein the hydrogen peroxide has a concentration of at least about 65%.

Claim 44

Process of claim 34 wherein the phosphoric acid has a concentration within the range of from about 85 to about 95%.

Claim 45

Process of claim 34 wherein the molecular ratio of dicarboxylic acid to phosphoric acid is within the range of from about 1:8 to about 1:12.

Claim 46

Process of claim 34 wherein the dicarboxylic acid is dissolved in the phosphoric acid reaction medium prior to being brought together and reacted with the hydrogen peroxide.

Claim 47

Process of claim 34 wherein the dicarboxylic acid reactant is azelaic acid.

Claim 48

Process of claim 34 wherein the dicarboxylic acid reactant is dodecanedioic acid.