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7/24/2019 Phosphoric Acid Wet Process
1/40
WET PROCESS PHOSPHORIC ACID
The main reaction in the wet process phosphoric acid may be represented
by the following equation:
Cal0F2
(PO
4 ). + 101y
-7
4
+10nH
2
0 4.10
CaSO 4
n H
2
O + 6 H
3
PO4 + 2 HF
where N= 0, 1/2 or 2 depending on the hydrate form in which the calcium
sulfate crystallizes.
The reaction is the net result of two reactions take place simultaneously.
12 H
3
PO
4+ Cn
10
F
2
(p04
Ca (H2PO4 )2 + CaF2
CaF
2
+9 Ca (H
2
PO4 + 10 H2
SO
4
+ 10 H
2
O
aSO4 n H
2
O + 6 H
3
PO
4
+ 2 HF
Phosphate rock contains many impurities.
hese impurities participate in
numerous side reactions. The HF formed by the reaction reacts with silica
and other impurities (Na, K, Mg, and Al) to form
fluosilicates
and other
more complex compounds. A variable amount of the fluorine
is volatilized
as SiF
4
, HF, or both.
The heat of reaction calculated from heat of formation is 230 KCal/g-mole
of apatite which is equivalent to 228 KCa1/Kgm of apatite or about
505 KCa1/Kgm of
p205.
The heat required to raise the temperature of gypsum (C
p
= 0.265
Cal/gm C) and phosphoric acid (3 0 P
2 0
5
; C, = 0.703 Cal/gm C) from 25C
to 3 8C and 71C iespectively is calculated to be 122 KCal/Kgm of P
205fed.,
Thus, about 383 KCal/Kgm of P
2
0
5
remains to be dissipated. In practice, some
9
7/24/2019 Phosphoric Acid Wet Process
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of the heat is lost by convection and conduction. On the other hand,
some heat may be brought in by u se of heated wash water or, if the wash
water is not heated, some of the heat in the gypsum is transferred to
the recycled weak acid and thus returned to the reaction. Additional
heat will be generated by reaction of additional sulf uric acid with
impurities in the rock. Most phosphate rock contains 10 -20 more calcium
than that required to form pure fluorapatite with the phosphorus in the
rock, which may result from substitution of carbonate for phosphate in the
apatite or presence of calcite or both. Reaction of this amount of
calcium with sulfuric acid to form gypsum would increase the net heat of
reaction per kilogram of P
2
0
5
by about 11 -16 .
Hydrogen fluoride is shown as a product of reaction in the first
equation. It reacts with the silica present as an impurity in phosphate
rock
to form fluosilicic acid which, in turn, forms fluosilicates and other
compounds with impurities in the rock. The thermal effect of these reactions
is negligible.
The net heat of reaction is influenced to some extent by the con-
centration of the sulfuric acid used, as shown below:
Sulfuric Acid
Conc. % H SO
2 4
94.55
98
95.73
93
98.03
90
99.22
85
01.03
80
02.65
75
04.00
If the conditions are such that the calcium sulfate crystallizes in
the form of anhydrite or hemihydrate
rather
than gypsum, the excess heat to
Heat of formation of H2SO4
KCal/gm mole
1
0
7/24/2019 Phosphoric Acid Wet Process
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be dissipated is about 100 kcal/kg of P
2
0
5
less than the value given
above.
Commercial wet processes may be classified according to the hydrate
form in which the calcium sulf ate crystallizes:
Anhydrite
Hemihydrate
Dihydrate
CaSO4
CaSO 4
. 1/2H20
CaSO
4
2H20
The hydrate form is controlled mainly by temperature and concentration
of H
3
PO
4
and H
2
SO 4
in the liquid phase (diagram
page
38 ). At present
there is no commercial use of the anhydrite process, mainly because the re-
quired reaction temperature is high enough to cause severe corrosion difficulties.
Processes in commercial use follow:
Crystal Form (s)
Number of
Separation
Steps
Usual Conc.
of Product
Acid, P205
Usual Temp.,C
Reactor
Recrystallizer
Dihydrate
1
26-32
70-85
Hemihydrate
Hemihydrate-dihydrate
Hemihydrate-dihydrate
1
1
2
40-50
26-30
40-50
85-100
90-100
90-100
50-60
50-65
Dihydrate-hemihydrate
2
35-38
65-70
90-100
a. Filtration or centrifuging steps
At present, dihydrate processes are by far the most popular and, hence,
data pertaining to dihydrate plants are given below:
Plant P arameters based on
p
2
0
5
per day
ton of
Range
Avg.
Reactor Volume, gals.
270-625
4 10
Agitator HP
0.77-2.40 1.50
Recycle, GPM
3.7-17.1
11.1
Filter area, Sq.
t.
1.01-2.02
1.37
11
7/24/2019 Phosphoric Acid Wet Process
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Phosphate rock is a very complex raw material which effects the
phosphoric acid plant operation in many ways. The more common quality
factors
for wet-process phosphoric acid production and their eff ect
are:
Lower grade ( P
2
0
5
) means that more tonnage must be
brought, transported, handled and (usually) ground;
An increase in the Ca0 : P
2 0
weight ratio increases
the sulfuric acid
requiremen
t
(Any Ca0 present
as CaSO4 should be excluded in calculating this
ratio);
3.
agnesium oxide may form precipitates with fluorine
in the reactor which may blind the filter cloth; therefore,
high Mg0 content can be a problem. When phosphoric
acid is used to produce ammonium phosphates or poly-
phosphates, water-insoluble (but citrate-soluble) magnesium
ammonium phosphate compounds may be formed. These compounds
from troublesome impurities in liquid fertilizers;
Increases of the Fe 2 0 3+ Al
2
0 3
content
above 2 -3 decrease
the plant capacity, often decrease
the
P
2
0
5
recovery,
and cause post-precipitation problems (sludge). 'However,
up to about 5 may be tolerable in some cases;
It
is desirable to have enough reactive silica (802) to
form SiF
4
and/or fluosilicates so as to avoid formation of
free HF, which is corrosive. Excessive silica or other
acid-insoluble impurities may cause erosion of equipment and
possible accumulations in digestion vessels depending on
particle size, character, and plant design. Also, a high
percentage of silica in the rock would increase the required
filter area;
Chlorine contents above about 0.01 cause increased corrosion
of stainless steel. More expensive alloys may tolerate
a Cl content of 0.10 or perhaps higher;
High organic matter may increase foaming problems (by
stabilizing the foam), increase viscosity, and hinder
filtration. The effect depends on both the character
and quantity of organic matter. Some rocks must be calcined
12
7/24/2019 Phosphoric Acid Wet Process
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to remove organic matter to make them usable;
Carbon dioxide (CO
2
) contributes to foaming and
increases consumption of antifoam reagents;
All commercial phosphate rocks contain fluorine (F );
no special effect has been noted due to variations
in fluorine content within the range of experience.
Effects of fluorine on scaling, corrosion, and post-precipitation
are related to other elements that combine with fluorine, in-
cluding Na, K, Al, Mg, and Si;
Some rocks which contain sulfides release hydrogen sulfide
( H
2
S) upon acidulation. This gas is toxic. Also sulfides
tend to increase corrosion;
Many other less common impurities may be present in sufficient
quantity to require consideration (Ti0
2
, SrO, Ba0, Cd, etc.);
Hardness is a factor in that harder rocks require more
grinding capacity;
The particle size of the rock as received effects the amount
of crushing and grinding required. Very fine particle size
may lead to dust losses in handling;
Low reactivity of the rock may require finer grinding;
Filterability of the rock-acid slurry is one of the most
important characteristics of a phosphate rock for use in
phosphoric acid production. Factors influencing filterability
are complex and not completely understood. However, if
a plant
is to be designed to use a specific rock, an acceptable
filtration rate can usually be attained through experimental
and by adjusting operating conditions, addition of crystal
modifiers, or pretreatment of the rock.
P 2
0
5
losses in phosphoric acid plant. There are four types of
p
2
0
5
losses;
Citrate insoluble (C. I.) loss; due to unreacted phosphate
rock, about 1 of input P205.
Citrate soluble (C.S .) loss,
of
1 3
2
0
5
with gypsum through i
HPO4
or SO4' about 2 - 4
due to co-crystallization
somorphic substitution of
.5 of input p205.
13
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Water soluble (W.S. ) loss, due to incomplete washing of
gypsum cake, about 0.5 - 1 of input P205.
Mechanical losses due to spillage, leakage, f ilter and
pipe washing, evaporator carry-over and losses as sludge.
This loss could be up to 4 .5 - 5 P
2 0 5 input.
The aim of designers and operators of reaction systems is to minimize
above losses. A high concentration of free sulfuric acid, in phosphoric
acid plant reactor slurry, will result in coating the phosphate rock with
calcium sulfate, thus blocking further reaction. O n the other hand, a low
concentration of free sulfuric acid will increase the amount of phosphate
co-crystallize with the gypsum. The optimum concentration of free sulfuric
acid varies with rock composition. The liquid phase of the reactor slurry
consists of phosphoric acid (3 0 P
2 0
5
) with about 1.5 - 2.5 free sulfuric
acid. The solid phase is mainly gypsum which is about 35-4 5 .
Calculation of sulfuric acid required per ton P
2 0 5
recovered
Assuming 94 overall P
2 0 5
recovery, P
2
0
5
fed,
2000
= 2127.6 lbs
0.94
If rock contains 3 3 P 2
05,
rock required,
2127.6
= 6447.3 lbs
. 3 3
Ca0 in the rock at 51 ,
644 7.3 x 0.51
3288.1 lbs
Ca0 equivalent to SO
3
(assuming 1 SO
3
in the rock)
6447.3 x 0.01 x 56
45.1
bs
80
Ca0 combined with
P
2
0
5
in filter cake (this P
2 0
5
is about
3.3 of input P 2 0
5
and assuming CaO/P2
0 5o
f 1)
14
7/24/2019 Phosphoric Acid Wet Process
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2127.6 x 0.03 3
70.2 lbs.
Ca0 combined with fluorine (assuming 15 of the fluorine combines
with Ca0 to form CaF
2
6447.3 x 0.15 x 0.037
6
52.7
2 x 19
Total Ca0 unreactive with sulfuric acid
45.1 + 70.2 + 52.7
168.0 lbs.
Net Ca0 for reaction with H
2
SO
4
3 288.1 - 168.0
3120.1 lbs
H 2
SO
4
required to form Ca SO4
3120.1
8
=5460.2 lbs
56
Excess H
2
SO
4
(assume 2 in reactor slurry, containing 30
P20
- 5
acid)
2
2000
30
= 133.3 lbs
Total H
2
SO
4
required
5593.5 lbs
H
2
SO
4
/P
2
0
5
2.8
In the following tabulation the sulf uric acid requirement for median-
grade rock is based on rock of typical impurity content and typical
operating conditions, and requirements for rocks of other Ca : P
2
0
5ratios
re estimated in proportion to that ratio.
High
Median
1.50
2.78
Low
Ca0 : P
2
0
5
ratio in rock
H
2
SO
4
requirement, tons/ton of P205
1.70
3.15
1.35
2.50
Normally, 4.9-5.3 ton
produced.
gypsum
is produced per ton P
2
0
5
15
7/24/2019 Phosphoric Acid Wet Process
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In
Out
Prod+ tct acid
ypsum
e/o
b.
0
b.
Phosphate
rock
lb.
Sulfuric acid
lb.
Water,
otal,
lb.
b.
Vapor,
otal,
lb.
b.
Loss
or
error,
lb.
Wet-Process Phosphoric Acid Over-All Chemical .11t,terinl Balance'
P 2
0,
34.42
106.64
106.64
31.80
100.00
1.09
0.59
106.59
0.05
Si%
5.08
15.74 15.74
0.16 0.50 2.26
13.67 1.57e
15.74
CaO
49.44
153.18
153.18
0.98 3.08
24.64
149.08 152.16 1.02
Fe20,
0.76
2.35
0.14 0.39
2.74
0.81
2.55
0.17 1.03
3.58
-.84
A1103
0.74
2.29
0.04
0.11
2.40
0.07
0.22
0.39 2.35
2.57
-- .17
Na2O
0.35
1.08
1.08
0.27
0.84
0.11
0.67 1.51
-.43
SO 2
0.76
2.35
72.70
204.29
200.64
0.98 3.08
33.33
201.60
204.74
1.90
F
3.52
10.90
10.90
0.96
3.02
0.79 4.77
3.11` 10.90
CO :
3.41
10.56
10.56
10.56'
10.56
Other'
0.84
2.60
2.60
0.53 1.67
0.25
1.51
3.18
- .58
A nhy.
t o t a l
99.32
307,69 72.88
204.79
512.48
36.56
114.96
03.03
381.33
15.24 511.53
0.95
-1.48
-4.59
-4.59
-0.40
-1.26
-0.33
-2.00
--1.29 -4.55
Corr.
total
97.84
303.10
72.88
204,79
507.89
36.16
113.70 62,70 379.33 13.95
506.98
Comb.
ITO
1.29
3.99 16.37
46.00
49.91)
11.15
35.06
15.81
95.83
130.89
Dry
total 99.13
307.09 89.25 250.79
557.88 47.31
148.76
78.54 475.10
13.05
637.87
Free
1120
0.87
2.70 10.75
:30.21
441.08
474.59
52.69 165.67 21.46
129.84
99.09 4 394.60
Total 100.00
309.79 100.00 281.00
441,68
1032.47
100.00
314.43
100.00
605.00
113.04 1032.47
Basis: 100.0 lb. P
2 0
6
produced.
6
By difference
in column.
C
13y difference in
line. d
Maximum calculated for evaporative
cooling. ' "Other" includes Mg() and K
2
0 plus difference for 100% corrected anhydrous total.
is the oxygen equiv-
alent of fluoride subtracted to correct for use of analyses given as oxides.
7/24/2019 Phosphoric Acid Wet Process
9/40
TYPICAL ANALYSES OF DI-HYDRATE PROCESS ACIDS
FLORIDA ROCK, WT.
NOMINAL P
2
0
5
3 0
45 5 4
P
2
0
5
28.85
45.12
54.16
Mg0
0.43
0.71
0.76
1.17
1.83
M.2 0
3
0.80
1.02
1.18
H
2
SO 4
(total)
1.85
3.23
2.92
Solids
0.25
2.31
2.34
F
2.18
1.38
1.18
Ca0
0.35
0.39
0.26
H
2
O
53.39
29.53 20.20
Sp. Gr.
at 25C)
1.340
1.565
1.740
7/24/2019 Phosphoric Acid Wet Process
10/40
7
0
70
0
lD
60
50
40
30
2
10
0
2
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1.61
3.45
5.27
7.06
8.82
1.80
3.64
5.45
7.24
9.00
1.98
3.82
5.63
7.41
9.17
2.17
4.00
5_81
7.56
0.35
0.184
0.183
0.181
0.178
0.176
1.05
1.06
1.07
1.08
1.09
9.52
11.25
12.95
14.62
16.27
9.70
11.42
13.12
14.70
16.14
0.87
11.59
13.20
14.96
m.no
10.04
11.76
13.45
15.12
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11.93
13.62
15.28
16.92
10.30
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13.79
15.45
17.09
10.56
12.27
13.90
15.62
17.25
10.74
12.44
14.12
1.5.78
17.41
10.91
12.61
14.29
15.94
17.57
11.08
12.78
14.46
16.11
17.73
0.179
0.170
0.167
0.165
0.102
1.10
1.11
1.12
1.13
1.14
17.90
19.50
21.07
22.62
24.15
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19.65
21.22
22.78
24.30
18.22
19.81
21.38
22.93
24.45
18.38
19.97
21.54
23.08
24.61
18.54
20.13
21.69
23.24
24.74
18.70
20.28
21.85
23.39
24.91
18.86
20.44
22.00
23.54
25.06
19.02
20.60
22.16
23.69
25.21
19.18
20.76
22.31
23.85
25.34
19.34
20.91
22.47
24.00
25.51
0.100
0.158
0.155
0.153
0.151
1.15
1.16
1.17
1.18
1.19
25.66
27.14
28.6/
30.06
31.48
25.81
27.29
28.76
30.20
31.02
25.90
27.44
28.90
30.34
31.70
26.11
27.59
20.04
30.48
31.00
26.24
27.73
29.10
30.43
32.05
26.40
27.88
29.33
30.77
32.19
26.55
28.03
29.48
30.91
32.33
20.70
28.17
29.62
31.06
32.47
26.8.5
28.32
29.77
31.20
32.61
27.00
28.46
29.91
31.34
:12.75
0.149
0.147
9.145
0.143
0.141
1.20
1.21
1.22
1.23
1.24
32.89
34.28
35.65
37.00
38.34
33.03
34.42
35.78
37.14
38.47
33.17
34.55
35.02
37.27
38.60
33.31
34.69
30.06
37.40
38.73
33.45
34.83
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37.54
38.86
33.58
34.96
3)1.33
37.67
39.00
33.72
35.10
34.46
37.80
30.13
33.86
35.24
36.60
37.94
39.26
34.00
35.38
36.73
38.07
39.39
34.14
35.51
36.87
38.20
39.52
0.139
0.137
0.135
0.133
0.132
1.25
1.26
1.27
1.28
1.29
39.65
40.05
42.23
43.50
44.74
39.78
41.08
42.30
43.62
44.87
39.91
41.21
42.49
43.75
44.99
40.04
41.34
42.01
43.87
45.12
40.17
41.46
42.74
44.00
45.24
40.30
41.59
42.87
44.12
45.36
40.43
41.72
42.09
44.25
45.49
40.56
41.85
43.12
44.37
45.61
40.69
41.98
43.24
44.50
45.73
40.82
42.10
43.37
44.62
45.86
0.130
0.128
0.127
0.125
0.124
1.30
1.31
1.32
1.33
1.34
45.98
47.20
48.40
49.60
50.78
46.10
47.32
48.52
40.71
50.89
40.22
47.44
48.64
49.83
51.01
46.35
47.56
48.76
49.95
51.13
46.47
47.68
48.88
50.07
51.24
40.50
47.80
49.00
50.19
51.30
46.71
47.02
49.12
50.30
51.48
46,84
4804
49.24
50.42
51.59
40.90
48.17
49.36
50.54
51.71
47.08
48.29
49.48
50.66
51.83
0.122
0.120
0.119
0.118
0.117
1.35
1.36
1.37
1.38
1.39
51.94
53.10
54.24
55.3G
56.48
52.00
53,21
54.35
55,48
56.59
52.17
53.32
54.46
55.59
56.70
52.29
53.44
54.58
55.70
56.81
52_40
53.55
54.69
55.81
56.92
52.52
53.67
54.80
55.02
57.03
52.44
53.78
54.02
54.04
57.11
52.75
53.90
55.03
50.15
57.26
52.87
54.01
.5.514
54.26
57.36
52.98
54.12
55.25
54.37
57.47
0.115
0.114
0.113
0.112
0.110
1.40
1.41
1.42
1.43
1.44
57.58
58.08
59.76
60.83
61.88
57,69
58.79
59.84
00.93
61.99
57.80
58.89
59.97
61.04
62.10
57.91
50.00
60.08
61.15
62.20
58.02
59.11
60.19
61.25
62.30
58.13
59.22
60.29
61.36
62.41
58.24
59.33
60.40
61.40
62.51
58.35
59.43
60.51
61.57
62.62
58.46
59.54
60.61
61.07
62.72
58.57
59.65
60.72
61.78
62.83
0.100
0.108
0.107
0.106
0.105
1.45
1.40
1.47
1.48
1.49
62.93
63.97
05.00
60.01
47.02
03.04
04.07
45.10
60.11
07.12
63.14
04.18
65.20
66.21
67.22
63.24
64.28
65.30
64.31
67.32
63.35
64.38
65.40
60.41
07.42
63.45
64.48
05.50
611.52
67.52
63.56
64.59
65.61
66.02
67.62
63.00
64.69
115.71
60.72
67.72
63.76
64.79
65.81
66.82
67.82
63.86
64.89
65.91
66.92
67.92
0.104
0.103
0.102
0.101
0.100
1.50
1.51
1.52
1.53
1.54
68.01
69.00
69.98
70.95
71.91
68.11
69.10
70.08
71.05
72.01
68,21
69.20
70.18
71.14
72_10
68,31
60.30
70.27
71.24
72.20
68.41
69.30
70.37
71.34
72.30
68.51
69.49
70.47
71.43
72.39
68.61
69.59
70.56
71.53
72.49
68.71
69.69
70.66
71.62
72.58
08.80
69.78
70.76
71.72
72.68
68.90
60.88
70.85
71.82
72.77
0.090
0.098
0.097
0.096
0.095
1.55
1.56
1.57
1.58
1.59
72.87
73.81
74.75
75.68
76.61
72.96
73.01
74.84
75.78
70.70
73.06
74.00
74.94
75.87
76.79
73.15
74.10
75.03
75.96
76.88
73.25
74.19
75.12
76.05
70.97
73.34
74.28
75.22
70.14
77.06
73.44
74,38
75.31
76.21
77.16
73.53
74.47
75.40
76.33
77.25
73.62
74.56
75.50
76.42
77.34
73.72
74.64
75.59
76.51
77,43
0.095
0.004
0.093
0.092
0.092
1.60
1.61
1 .62
1 .63
1.64
77.52
78.43
79.33
80.23
81.12
77.61
78.52
70.42
80.32
81.26
77.70
78.41
79.51
80.41
81,29
77.80
78.70
79.60
80.50
81.38
77.89
78.79
79.69
80.58
81.47
77.98
78.88
79.78
80.07
81.40
78.07
78.07
70.87
80.76
81.65
78.16
79.06
79.90
80.85
81.74
78.25
79.15
80.05
80.94
81.82
78.34
79,24
80.14
81.03
81.01
0.001
0.090
-0.090
0.080
0.088
1.65
1.60
1.67
1.68
1.69
82.00
82.88
83.75
84.61
85.47
82.09
82.90
83.84
84.70
85 54
82.17
83.05
83.92
84.79
85.64
82.26
83.14
84.01
84.87
85.73
82.35
83.22
84.10
84.911
85.82
82.44
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85.90
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84.27
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82.61
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82.70
83.57
84.44
85.30
86.10
82.79
83.60
84.53
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86.24
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0.087
0.087
0.0811
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1.71
1.72
1 . 7 3
1.74
80.33
87.18
88.02
88.85
89.08
86.41
87.26
88.10
88.93
89.76
86.50
87.34
88.18
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89.84
86.58
87.43
88.27
89.10
89.93
86.67
87.51
88.35
89.18
90.01
86.75
87.60
88.43
89.26
90.09
86.84
87 .418
88 52
89.35
90.17
84.92
87.76
88.60
89.43
90.25
87.01
87.85
88.08
89.51
90.34
87.09
87.93
88.77
89.60
90.42
0.085
0.084
0.083
3 .083
0.082
1.75
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90.50
91.32
00.58
91.40
90.66
91.48
90.74
91 . 50
90.82
90.91
90,90
91.07
01 . 15
91 .23
0.082
0.081
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7/24/2019 Phosphoric Acid Wet Process
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Viscosity, density, and pH of saturated solutions in the system
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Com position of solution
Viscosity
Density.
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pH
Weight percent
Mole
N 1 1 1
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Centipoises
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1.43
1.44
1.36
1.63
1.77
2.26
2.49
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3.24
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30.73
32.13
32.59
33.85
36.31
38.66
41.86
44.02
47.32
50.91
50.84
49.5.5
47.01
41.68
39.02
36.34
30.8,5
2.060
2.047
2.020
1.931
1.843
1.752
1.68.5
1.633
1.568
1.498
1.499
1.467
1.426
1.313
1.248
1.192
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4.02
4.37
4.60
4.69
5.45
6.30
7.84
9.02
11.73
15.88
15.79
12.61
9.10
4.89
3.68
2.94
1.87
5.01
5.49
5 .30
5.94
7.00
8.20
10.36
12.06
15.99
22.08
22.00
17.34
12.30
6.37
4.70
3 .68
2.24
1.246
1.257
1.260
1.268
1.285
1 . 300
1.322
1 .337
1.363
1.390
1.393
1 .375
1 .352
1.303
1.277
1.25.3
1.201
8.66
8.51
8.42
7.70
7.12
6.86
6.49
6.30
6.09
5.84
5.81
5.70
5 .59
5 .30
5.07
4.84
3.69
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12.73
2.58
2.72
2.96
3.30
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3.70
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4.72.
4.51
3.91
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35.84
35 .57
38.59
41.06
43.66
46.06
48.87
51.65
54.30
55.83
55.64
54.34
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