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RESEARCH ON THE ELIMINATION OF FOAMING IN THE PROCESS OF EXTRACTION
OF PHOSPHORIC ACID FROM HIGH-CARBONATE PHOSPHORITE RAW MATERIALS
Yuzboyev Shukhrat Toshmuradovich
Deputy Production Director of "Ammofos-Maxam" JSC
mail:
Sadikov Bakhodir Bagirovich
Production director of "Ammofos-Maksam" JSC, candidate of technical sciences
mail:
Daddy Yassir
Independent researcher of the Tashkent Institute of Chemical Technology
Mirzakulov Kholtura Choriyevich
Director of Network center "Retraining and professional development of teaching staff" under
the Tashkent Institute of Chemical Technology, Ph.D., professor
mail:
Yorboboyev Ruslan Choriyevich
Senior teacher (PhD) at Tashkent Institute of Chemical Technology
mail:
Annotation:
The process of decomposing carbonated phosphorite raw materials from the
Tashkura mine with sulfuric acid and extracting phosphoric acid, and the foaming frequency of
the resulting phosphate slurry and its elimination methods were studied. The height and density
of the foam formed in the process of decomposition of light carbonate phosphorite raw materials
in the presence of phosphoric and sulfuric acids under optimal conditions were determined, and
the methods and optimal conditions for reducing the foam density using "PAA-gel" and "Struktol
SB-2195" as defoaming reagents were investigated.
Key words:
Tashkura mine carbonate phosphorite raw materials, phosphoric acid slurry,
foaming rate, PAA-gel, "Struktol SB-2195" EFK, decomposition.
Annotatsiya:
Tashkura koni yoqri korbonatli fosforit xomashyosini sulfat kislotasi bilan
parchalash va ekstraktsion fosfor kislotasi olish jarayoni va unda hosil boʼladigan fosfatkislotali
boʼtqaning koʼpiklanish karraligi va uni bartaraf etish usullari oʼrganildi. Yoqri korbonatli
fosforit xomashyosini maqbul sharoitda fosfat va sulfat kislotalari ishtirokida parchalash
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jarayonida hosil boʼladigan koʼpik balandligi va karraligi aniqlandi hamda koʼpiklanishni
bartaraf etuvchi reagentlar sifatida “PАА-gel” va “Struktol SB-2195” ishtirokida koʼpik
karraligini kamaytirish usullari va maqbul sharoitlari tadqiq qilindi.
Kalit soʼzlar:
Tashkura koni yoqri korbonatli fosforit xomashyosini, fosforkislotali boʼtqa,
koʼpiklanish karraligi, PАА-gelь, “Struktol SB-2195”’ EFK, parchalash.
Аннотация:
Изучен процесс разложения серной кислотой высококарбонатного
фосфоритного сырья месторождения Ташкура и получения экстракционной фосфорной
кислоты, кратность пены образующейся в ней фосфорнокислотной пульпы и способы ее
устранения. Определены высота и кратность пены, образующейся при разложении
высококарбонатного фосфоритного сырья в присутствии фосфорной и серной кислот в
оптимальных условиях, а также исследованы методы и оптимальные условия снижения
кратности пены в присутствии "ПАА-гель" и "Структол СБ-2195" в качестве
пеногасителей.
Ключевые слова:
Высококарбонатное фосфоритовое сырье месторождения Ташкура,
фосфорнокислый пульпы, пенообразователь, ПАА-гель, «Structol SB-2195» ЭФК,
разложения.
Literature review.
"Kyzilkum Phosphorite Complex" LLC of Central Kyzylkum (MK)
in Navoi region produces 3 types: washed-burnt phosphorite (YuKFK), washed-dried
phosphorite (YuQF) and high-carbonate phosphorite raw materials (YuKFX). In our republic,
only "Ammofos-Maxam" JSC produces EFC from YuKFK by the dihydrate method [1, 2].
"Kyzilkum Phosphorite Complex" LLC has an annual production capacity of 716,000 tons (~
26.2% P
2
O
5
), but produces 450,000 tons of UFK per year on average. [3, 4].
The foaming produced in the processes of obtaining double superphosphate,
monodicalcium phosphate, precipitate [5, 6] by decomposing BFX in the presence of different
standards of EFK, phosphorsulfurcalcium RS-agro and enriched superphosphate SPF-26, SPF-23
[7, 8] in the presence of sulfuric and phosphoric acids, nitrophos fertilizers [9] by decomposing
them in the presence of nitric acid, and various technological and technical methods. studies
have been conducted on elimination using However, chemical reagents were not used in the
research to reduce foaming during the decomposition of BFX with mineral acids.
Research methods.
In carrying out research work, MQ YuKFX (OzDSt 2825:2018,
produced at "Kyzilkum Phosphorite Kombinati" LLC), EFK (TSh 6.6-21:2018, produced at
"Ammofos-Maxam" JSC) and sulfuric acid (GOST 2184-2013) and PAA-gel (Ts 00203849-64-
2016, produced at "Navoiyazot" JSC) and "Struktol SB-2195" (Struktol SB-2195,
Schell+Seilacher GmbH, Germany) reagents were used.
Discussion and results:
The chemical composition of YuKFX used in research works is
as follows, heavy. %:
Р
2
О
5
- 21.8; CaO - 49.8; MgO - 1.20;
Al
2
О
3
- 0.31;
Fe
2
О
3
- 0.65;
СО
2
-
12.10;
Cl
-
- 0.24;
СаО/Р
2
О
5
- 2.285; insoluble residue - 4.5; H
2
O - 1.2; organic carbons - 2.0
was determined on the basis of chemical and physico-chemical analysis.
In the research work carried out in the experimental device, the effects of the duration of
the process and the amount of "PAA-gel" and "Struktol SB-2195" substances on the foaming
process (foam height, foam density (Kk), foam "living" period) during phosphate and sulfuric
acid decomposition of YuKFX from the Tashkura mine were studied. The formed Kk and the
period of existence - "living" time were taken as the factors characterizing the foaming process.
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The height of the foam was measured according to the values specified in the
dimensions, and the "living" time of the foam was measured with a stopwatch. Kk was defined
as the ratio of foam volume Vk to the liquid volume Vs used for its formation [10, 11].
Kk = Vk /Vs = Vg + Vs / Vs, where Vg is the gas volume in the foam.
The "living" time (U) of the foam is determined by the amount of liquid released at time
t (sec) or the rate of liquid release from the foam, i.e. U = Vs / t [12].
The extraction process of EFK was carried out at H2SO4 rate - 104%, Q:S = 1:3.0,
decomposition process temperature - 80 ℃ and duration - 90 minutes. In this case, the
extraction process of EFK was carried out in two stages. In the first stage, the foam height and
Kk were determined in the 12% EFK circulation solution for 20 minutes, and in the 93% sulfuric
acid digestion process for 90 minutes. At the initial stage, YuKFX was added to a circulating
solution of 12% P
2
O
5
EFK and 93% H
2
SO
4
to the obtained slurry at the same rate for 10 minutes,
and the height of foam and precipitate was measured.
The effects of PAA-gel and Struktol SB 2195 substances and their concentration and
quantity on the foaming process during the sulfuric acid decomposition of high-carbon
phosphorite of the Tashkura mine in the experimental model device in laboratory conditions
were determined. The results of the scientific research are presented in Figures 1, 2 and 3 below.
In these pictures, the effects of initial and surface passive substances ("PAA-gel" and "Struktol
SB 2195") on the process of foam formation (foam height, foam density, foam residence time,
etc.) during the decomposition of YuKFX from the "Tashkura" mine with 93% H
2
SO
4
in an
experimental model device in laboratory conditions were studied. In this case, the phosphorite
decomposition process was carried out in two stages, and the foam height and frequency were
studied in the first stage for 20 minutes in a 12% EFK circulating solution and for 70 minutes in
93% sulfuric acid decomposition processes. The rate of sulfuric acid was -104%, the Q:S phases
were in the ratio of 1:3, the duration of the process was -90 minutes, and at the initial stage,
phosphorite was added to the circulating solution of 12% P
2
O
5
EFK, and 93% H
2
SO
4
was added
to the obtained slurry at the same rate for 10 minutes. 10 in relation to the amount of
phosphorite; Graphs of the effect of surfactants "Struktol SB 2195" and "PAA-gel" on the foam
density up to 25 and 50 g/t are presented. When breaking up without surfactants and in the
presence of them, the foam density was 2.50-1.00 and in the second stage 3.35-1.05, surface
passive agent "Struktol SB 2195" and 10 of "PAA-gel"; The effect of 25 and 50 g/t on foam
density is 1.60-1.03 in the first stage, respectively; 1.47-1.00; 1.31-1.00 and 1.32-1.03; 1.28-
1.02; 1.24-1.00 and in the second stage 2.16-1.06; 2.05-1.00; 1.80-1.00 and 1.85-1.12; 1.67-
1.07; It was found to decrease to 1.58-1.01.
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Picture 1.
The dependence of the foaming rate on the duration of the process in the
presence of initial and surface passive substances in the decomposition of YuKFX with 12%
P
2
O
5
EFK circulating solution and H
2
SO
4
.
PAA-gel and "Struktol SB 2195"-10 g/t;
Decomposition with 12% P
2
O
5
circulating solution (1; 2; 3) and H
2
SO
4
(1”; 2”; 3”): 1; 1"-
without the participation of SPM; 2; 2"-"Struktol SB 2195"; 3; 3"-PAA-gel. (H
2
SO
4
rate is
104% and Q:S=1:3.0).
Picture 2.
The dependence of the foaming rate on the duration of the process in the
presence of initial and surface passive substances in the decomposition of YuKFX with 12%
P
2
O
5
EFK circulating solution and H
2
SO
4
.
PAA-gel and "Struktol SB 2195"-25 g/t;
Decomposition with 12% P
2
O
5
EFK circulating solution (1; 2; 3) and H
2
SO
4
(1”; 2”; 3”): 1; 1"-
without the participation of SPM; 2; 2"-"Struktol SB 2195"; 3; 3"-PAA-gel. (H
2
SO
4
rate is
104% and Q:S=1:3.0).
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In the process of decomposition of phosphorite in the presence of 12% P
2
O
5
EFK
circulating solution, the value of the foam multiplier was initially 2.5 (without the participation
of a surfactant), 10 from the surfactants "Struktol SB 2195" and "PAA-gel"; When added in
amounts of 25 and 50 g/t, the foaming ratio is 2.4, respectively; 2.09; 1.77 and 1.87; 1.80; was
1.72, i.e. 1.04; 1.19; 1.41 and 1.31; 1.36; It decreased by 1.42 times.
Picture 3.
The dependence of the foaming rate on the duration of the process in the
presence of initial and surface passive substances in the decomposition of YuKFX with 12%
P
2
O
5
EFK circulating solution and H
2
SO
4
. Decomposition with PAA-gel and "Struktol SB
2195"-50 g/t; 12% P
2
O
5
EFK circulating solution (1; 2; 3) and H
2
SO
4
(1; 2; 3"): 1; 1"-without
the participation of SPM; 2; 2"-"Struktol SB 2195"; 3; 3"-PAA-gel. (H
2
SO
4
rate is 104% and
Q:S=1:3.0).
In the first stage, 10 of the surfactants "Struktol SB 2195" and "PAA-gel"; The value of
the foam factor when breaking down the slag with 93% H
2
SO
4
when added in amounts of 25 and
50 g/t (the foam factor was 3.45 without the addition of a surfactant) is 2.16, respectively; 2.05;
1.80 and 1.85; 1.67; was 1.58, i.e. 1.59; 1.68; 1.91 and 1.86; 2.06; decreased by 2.18 times.
Also, the extraction process of phosphoric acid was studied based on processing of
Toshkura mine YuKFX with sulfuric acid. The process of extraction of MQ YuKFX and
phosphoconcentrates under the influence of sulfuric acid depends on the temperature and acid
concentration in the system, and it was found that calcium sulfate crystals in the obtained
product are formed in different states.
It was observed that plate-like crystals of size (80-140)x(20-60) μm are formed from
thermoconcentrate porridge, and needle-like, fan-shaped or star-shaped gypsum crystals are
formed from the decomposition of high carbonate phosphorites.
In the dihydrate method of obtaining extractive phosphoric acid (EFK), the process of
sulfuric acid decomposition of new unenriched phosphorite raw materials from Toshkura mine
was carried out at a temperature of 80-90 ℃, with 104% sulfuric acid in a ratio of 1:3, with a
circulating solution (EFK) containing 10-16% P
2
O
5
and 96% sulfuric acid for 4 hours.
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In this case, the chemical composition of the slurry obtained from the Toshkura mine
YuKFX, circulating solution containing 10-16% P
2
O
5
and 96% sulfuric acid was studied on the
basis of laboratory analysis. Data obtained on the basis of chemical laboratory analyzes are
presented in table 1.
Table 1.
The chemical composition of the porridge obtained on the basis of sulfuric acid
decomposition of Toshkura mine YuKFX
№ H
2
SO
4
standard
Circulating
Solution:
Amount of P
2
O
5
in EFK, %
Chemical composition of porridge, mass. %
P
2
O
5
CaO
MgO
SO
3
F
1
104
10
10,34
9,95
0,45
0,78
1,19
2
12
11,56
9,95
0,45
0,78
1,19
3
14
12,78
9,95
0,45
0,78
1,19
4
16
14,00
9,95
0,45
0,78
1,19
In this case, it was found that the chemical composition of the porridge obtained from the
decomposition of the solid and liquid phases (Q:S) in the ratio of 1:3 for 4 hours with a sulfuric
acid standard of 104%, the amount of P
2
O
5
in the circulating solution increased by 10.4 - 14.0%
when the acid standard and the concentration of the circulating solution increased. Also, It was
found that CaO is 9.95%, MgO is 0.45%, SO
3
is 0.78%, and F is 1.19%.
Table 2
Chemical composition of EFK obtained on the basis of sulfuric acid decomposition
of Toshkura mine new YuKFX
№
Amount of P
2
O
5
in
circulating
EFK
Chemical composition of EFK, mass.
According
to
P
2
O
5
K
parch.
P
2
O
5
CaO
MgO
SO
3
F
1
10
15,07
0,31
0,42
3,15
0,84
96,5
2
12
16,71
0,35
0,39
2,80
0,70
97,4
3
14
18,37
0,39
0,37
2,54
0,56
98,3
4
16
20,22
0,43
0,34
1,92
0,42
98,7
The amount of P
2
O
5
in the dihydrate method of extractive phosphoric acid (EFK)
production depends on the composition of phosphate raw materials and the concentration of the
circulating solution. The process of decomposition of phosphate raw materials takes place at a
temperature of 80-90 ℃, and the concentration of P
2
O
5
in the liquid phase of the obtained
porridge depends on the concentration of the circulating solution, the amount of sulfate ions in it
is 1.0-1.5%, the ratio of S:Q phases is 3:1, the extraction time is 3.5-4.5 hours, and the average
duration of 4 hours is the optimal conditions for the technological processes of EFK production.
In this case, when the P
2
O
5
concentration of the circulating solution changes from 10 to 16%, the
phosphorite decomposition coefficient increases from 96.5 to 98.7%, and the P
2
O
5
concentration
in the obtained EFK also increases from 15.07 to 20.22%. The results of the study are presented
in Table 2.
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Conclusion.
Thus, the conclusion from the obtained results is that in the technological
factors carried out above, it was found that the substance "PAA-gel" eliminates more foaming
than the surface passive substance "Struktol SB 2195" (1.01-1.14 times under optimal conditions
in the first stage, and 1.17-1.22 times in the second stage) and the optimal amount of surfactants
"PAA-gel" and "Struktol SB 2195" is 25-40 is g/t. In the research work, it would be appropriate
to study the ratio of liquid and solid phases, the rate of acids, the concentration of the circulating
solution, the duration of the process, temperature and other technological factors in a relatively
wide range, and then draw a conclusion based on the analysis of the results.
The processing of Toshkura mine YuKFX was studied in two stages, in the first stage
with circulating solution (EFK), and in the second stage with 93% sulfuric acid decomposition
process research was studied. The effects of P
2
O
5
content in the circulating solution up to 10-
16% for obtaining high-concentration EFK were studied. From the obtained results, it was found
that the higher the concentration of the circulating solution, the higher the concentration of the
obtained EFK.
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