Method for the manufacture of concentrated phosphorus acid
View Patent ↗A method for the manufacture of concentrated phosphorous acid starting from pure P 4 O 6 is disclosed. The P 4 O 6 is hydrolyzed, preferably under stirring in water in the presence of a homogeneous Broensted acid catalyst while maintaining in the hydrolysis/reaction medium a pH below 5 whereby the free water level, at the completion of the hydrolysis, is in the range from 0 to 40%.
1. A method for manufacture of a concentrated phosphorous acid by mixing pure P 4 O 6 and a reaction medium containing water and a homogeneous Broensted acid, said reaction medium having a pH below 5 whereby, at the end of the P 4 O 6 hydrolysis, free water is present in an amount of from 0 to 40%, expressed in relation to the final reaction mixture, wherein the homogeneous Broensted acid is selected from the group consisting of sulfuric acid, sulfurous acid, trifluoroacetic acid, trifluoromethane sulfonic acid, HCl, HBr, HI, methane sulfonic acid, oxalic acid, p-toluene sulfonic acid, naphthalene sulfonic acid and mixtures thereof.
2. The method in accordance with claim 1 wherein the concentrated phosphorous acid is recovered.
3. The method in accordance with claim 1 wherein the pure P 4 O 6 is added, under stirring to the reaction medium.
4. The method in accordance with claim 1 wherein the free water is present in a level of from 0 to 30% by weight.
5. The method in accordance with claim 1 wherein the pH of the reaction medium is below 4.
6. The method in accordance with claim 1 wherein the pure P 4 O 6 contains at least 97% by weight of P 4 O 6 .
7. The method in accordance with claim 1 wherein the pure P 4 O 6 contains less than 1by weight of elemental phosphorus.
8. The method in accordance with claim 1 wherein the pH of the reaction medium is maintained below 2.
9. The method in accordance with claim 1 wherein the reaction is carried out at a temperature in the range of from 20° C. to 200° C. in a process by adding the P 4 O 6 to the water containing the homogeneous Broensted acid, said process being selected from the group consisting of:
(1) in a closed vessel batch arrangement under autogeneous pressure built up;
(2) in a vessel batch arrangement in the absence of pressure containment; and
(3) in a continuous process, possibly under autogeneous pressure built up, whereby the concentrated phosphorous acid is withdrawn on a continuous basis.
10. The method in accordance with claim 1 wherein the pure P 4 O 6 is prepared by reacting gaseous or liquid phosphorus with oxygen or a mixture of oxygen and an inert gas, in essentially stoichiometric amounts, in a reactor at an average temperature in the range from 1600 K to 2000 K by removing the heat created by the exothermic reaction of phosphorus and oxygen with a residence time from 0.5 to 60 seconds followed by quenching the concentrated phosphorous acid to a temperature below about 700° K.
11. The method in accordance with claim 10 wherein the residence time is from 5 to 30 seconds.
12. The method in accordance with claim 11 wherein the concentrated phosphorous acid reaction product is quenched to a temperature below about 350° K and wherein the residence time is from 8 to 30 seconds.