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EXAMPLE 3 10
3.465 tons sulfuric acid (100%)
A rock phosphate from Iran having the following 5.080 tons calcium sulfate.
analysis was processed according to the present inven
tion. EXAMPLE 5
Rock phosphate from Florida was made into a slurry
P20S 15.90 % .112 moles per 100 g
15 having the following composition:
CaO 28.64 % .511 moles per 100 g
MgO 2.64 % .065 moles per 100 g
A120, 1.27 % .012 moles per 100 g Rock
FeZOJ 10.64 % .066 moles per 100 g % X030
K20 .13 % .001 moles per 100 g
NaZO .12 % .002 moles per 100 g 20 P205 32.80 9.84
510; 30.30 % CaO 46.60 13.98
MgO .80 .24
A120, .80 .24
In order to obtain 1 ton of P205 as the ?nal product, F8203 .60 .18
20 .11 .03
the following initial quantities of materials were used Na 0 .10 .03
and the amount of the various materials recovered at 25 sad, 7.40 2.22
the different stages of the process are indicated:
1.0417 tons P205 rock (96% recovery) In order to obtain 1 ton of P205 as the ?nal product,
6.552 tons rock phosphate the following initial contents of P205 and materials were
10.920 tons slurry rock phosphate (60% solid con utilized and the amounts of the various materials ob
tent) 30 tained during the stages of the process are as follows:
6.347 tons P205 (100%) recycled 1.041 tons P205 from rock
11.754 tons P205 (54%) recycled concentration of 3.173 tons solids content (42.5%)
P205 in the slurry 32.40% 7.468 tons slurry
5.432 tons oxalic acid added 1.043 tons P20, (100%)
6.217 tons oxalate salts recovered 35 3.261 tons P205 phosphoric acid (32% P205")
4.225 tons sulfuric acid (100%) used 0.285 tons silica separated
7.415 tons calcium sulfate recovered. 2.50 tons oxalic acid crystallized added
EXAMPLE 4 2.90 tons oxalate salts
1.94 tons sulfuric acid (100%)
A mixture of rock phosphate from Florida and slimes 40 2.80 tons calcium sulphate
were made into a slurry having the following composi
tiOn: ~ What is claimed is:
l. A method for the manufacture of phosphoric acid
Rock Slimes Mixter rock 30% from phosphate rock comprising
% X0.30 % ><0.70 slurry 70% 45 (a) mixing crushed phosphate rock with a stoichio
P205 32.80 9.84 12.20 8.54 18.38 .129 Mel/100g metric excess of phosphoric acid in the presence of
CaO 46.60 13.98 16.70 11.69 25.67 .458 water to form a slurry and heating the slurry at a
MgO .80 .24 2.90 2.03 2.27 .056 temperature and for a period of time suf?cient to
A1203 .80 .24 11.90 8.33 8.57 .084
R220, .60 .18 3.50 2.45 2.64 .016 convert the rock into a calcium monophosphate;
K20 .11 .03 .80 .56 .59 .006 50 (b) adding oxalic acid to the heated slurry to form a
Na2O .10 .03 .30 .21 .24 .004
SD; 7.40 2.22 - 35.80 25.06 27.28. slurry of precipitated calcium oxalate therein; and
metals .624 (c) recovering the phosphoric acid from the slurry
P205 added 0.624-0.l29 = .495
resulting from step (b).
2. The method of claim 1 wherein the calcium oxalate
In order to obtain 1 ton of P205 as the ?nal product, 55 precipitate is separated from the slurry resulting from
the following initial contents of P205 and materials were step (b) and the phosphoric acid is recovered from the
utilized and the amounts of the various materials ob liquid obtained from such separation step.
tained during the stages of the process are as follows: 3. The method of claim 1 wherein the phosphoric
1.041 tons P205 from rock + slimes phosphate (96%) acid is recovered from the slurry resulting from step (b)
5.668 tons solids content (42.5%) 60 by extraction of the slurry with solvents which are
13.335 tons slurry selective for phosphoric acid.
7.378 tons P205 (54% P205) theoretical 4. The method of claim 1 wherein the separated cal
9.223 tons P205 -phosphoric acid (54% P205") excess cium oxalate is treated with a stoichiometric amount of
25% sulfuric acid to regenerate the oxalic acid and produce
concentration of P205 in the slurry 22.09% 65 calcium sulphate.
silica separated 1.546 tons 5. The method of claim 1 wherein the phosphoric
4.456 tons oxalic acid crystallized added acid recovery step is carried out by multiple effect dis
5.163 tons oxalate salts tillation.
9
4,108,957
10
6. The method of claim 1 wherein the phosphate rock 11. The method of claim 1 wherein the phosphoric
is crushed to a particle size of less than about 1 micron. acid added has a concentration in the range from about
5 to 54% P205 by weight.
7. The method of claim 1 wherein the heating is car 12. The method of claim 1 wherein the oxalic acid is
ried out for a time period from about 0.3 to 3 hours at a added in a step-wise manner so as to separately precipi
temperature from about 70 to 90 C. tate the various metal values in the phosphate rock.
13. The method of claim 12 wherein uranium is sepa
8. The method of claim 2 wherein the calcium oxalate rately recovered from the phosphate rock.
is separated by ?ltration or cycloning. 14. The method of claim 1 wherein the amount of
9. The method of claim 1 wherein the amount of 10 oxalic acid used is from about 60 to 150% of the stoi
100% phosphoric acid added in step (a) is in the range chiometric amount based on the metals to be removed
from the mixture.
from about 1.00 to 3.00 tons per ton of phosphate rock. 15. The method of claim 1 wherein the amount of
10. The method of claim 1 wherein the amount of oxalic acid used is about 70% of the stoichiometric
oxalic acid added is in the range from about 0.8 to 2.0 amount based on the metals to be removed from the
mixture.
tons per ton of phosphate rock. t * ? * $
25
30
35
45
50
55
65