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03
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302-312
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)
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A
BSTRACT
An analysis of the literature shows that natural phosphates are suitable for de-composition with nitric acid,
which does not contain significant amounts of cal-cium carbonate, magnesium carbonate and silicates, iron
and aluminium com-pounds, which are easily decomposable acids, and as a result, complicate the
processing of phosphates and degrade the quality of fertilizers. The best way to obtain phosphorus-
containing fertilizers is the phosphoric acid decomposition of phosphate raw materials.
K
EYWORDS
Phosphrite, acid, decomposition, phosphorus-containing fertilizer, chemical pro-cessing, roasting,
combined flow chart, phosphorite enrichment.
I
NTRODUCTION
Uzbekistan is an agro-industrial country. It has
more than 25 million 736 thousand hectares of
agricultural land, including over 3.73 million
hectares irrigated [1].
It is on irrigated lands that over 97% of all
agricultural products of the republic are obtained.
Uzbekistan ranks fifth in the world in cotton
production. It has ensured its grain independence
by collecting more than 6 million tons of cereal
Journal
Website:
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m/index.php/ijasr
Copyright:
Original
content from this work
may be used under the
terms of the creative
commons
attributes
4.0 licence.
Research Article
STUDY OF THE INFLUENCE OF NITRIC ACID ENRICHMENT OF
PHOSPHORITES OF THE CENTRAL KYZYLKUM ON THE
PROCESS OF OBTAINING PHOSPHORUS-CONTAINING
FERTILIZERS BASED ON THEM
Submission Date:
June 20, 2023,
Accepted Date:
June 25, 2023,
Published Date:
June 30, 2023
Crossref doi:
https://doi.org/10.37547/ijasr-03-06-50
Safie Ortikova
Associate Professor Of The Department Of Chemistry And Chemical Technology, Fergana Polytechnic
Institute, 100170, Fergana, Uzbekistan
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grain in recent years. The population of
Uzbekistan today is over 36 million people. The
annual growth is at the level of 2.5%. And
irrigated arable land is not increasing due to the
acute shortage of water resources. On a per capita
basis, it is even falling.
Thus, in 1970, 0.22 hectares of irrigated land per
person, and now this figure has decreased to 0.14
hectares [1].
Each ton of mineral fertilizers provides the
annual need for food for 5-6 people. The cost of
production and use of fertilizers is 2-3 times paid
off by the cost of additional agricultural products.
Thanks to the use of mineral fertilizers, an
average of 40-50% of the increase in crop yields
is provided. The effectiveness of the use of
mineral fertilizers and chemical plant protection
products is expressed not only in increasing
yields and preserving products but also in a
significant increase in labour productivity in
agriculture. This can be seen, for example, from
the following data. On the planet, in the period
from 1900 to 1940, labour productivity in
agriculture increased by 60%, and over the next
40 years by 1980, with the widespread use of
chemicals, it increased 11 times [2].
A large branch of the chemical industry has been
created in Uzbekistan, working in agriculture.
Three open joint-stock companies: Maksam-
Chirchik, NavoiAzot and FerganaAzot produce
nitrogen fertilizers, the range of which consists of
ammonium nitrate, urea and ammonium sulfate.
Three JSCs: AmmophosMaxam, Samarkand
chemical and Kokand superphosphate plants
produce phosphorus-containing fertilizers, the
range of which consists of amorphous, suprefos,
ammonium
sulfate
phosphate,
simple
ammoniated superphosphate and nitrocalcium
phosphate fertilizer. The Kyzylkum Phosphorite
Plant provides phosphate raw materials to our
factories that produce phosphorus-containing
fertilizers. The Navoi Joint-Stock Association
“Electrokhimzavod” produces various types of
chemical plant protection products.
As a result of large-scale research and
technological work, significant results have been
achieved in the production of ammophos,
suprephos-NS, ammonium sulfate phosphate, PS-
Agro, simple and enriched superphosphates,
nitrocalcium phosphate and phosphatized nitrate
based on the processing of both enriched and
unenriched phosphorites of the Central
Kyzylkum.
It is known that one ton of raw cotton removes
from the soil annually 45 kg of nitrogen, 15 kg of
P
2
O
5
and 45 kg of K
2
O. One ton of wheat removes
from the soil annually 35 kg of nitrogen, 10 kg of
P
2
O
5
and 24 kg of K
2
O. With a gross harvest of 3
million tons of raw cotton and 6.1 million tons of
wheat, only these two crops are annually carried
away from the soil with a yield of 348.5 thousand
tons of nitrogen, 106 thousand tons of
phosphorus and 281.4 thousand tons of
potassium. But other crops also take out a large
amount of nutrients from the soil. They need to be
replenished into the soil. We should not forget
about the low utilization rate of nutrients from
mineral fertilizers by plants. From nitrogen and
potash fertilizers, on average, 60-70% of nitrogen
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and potassium are used, and from phosphorus
fertilizers in the year of application - only about
20-25% and for 2-3 subsequent years about 40%
of phosphorus. The weak use of phosphorus
fertilizers in the year of application is caused by
the fact that phosphorus compounds are in the
soil in an immobile or extremely inactive state
and therefore cannot be completely absorbed by
the roots of plants. Therefore, phosphorus
fertilizers must be applied in an amount that is 4-
5 times higher than the phosphorus removal by
the increase in yield (of a particular crop) that
they want to receive [4].
All this suggests that in Uzbekistan it is necessary
to increase the production of mineral fertilizers,
especially
phosphorus-containing
ones.
Questions arise about how this should be done
and what brand of phosphorus-containing
fertilizer is necessary for agriculture in the first
place.
Naturally, to increase the production of
phosphorus-containing fertilizers, it is necessary
to increase the capacity of the Kyzylkum
phosphorite plant. And at the same time, it is
necessary to develop an acceptable, with good
technical and economic indicators, technology for
processing phosphorites of the Central Kyzylkum.
Objects and methods of research
The normal and stable operation of phosphate
fertilizer plants depends primarily on the quality
of phosphate raw materials. The world's best
phosphate raw material is apatite concentrate
from the Kola Peninsula in Russia. Its composition
(wt%): 39.4 P
2
O
5
; 52.0 CaO; CaO: P
2
O
5
= 1.32; 3.0
(Fe
2
O
3
+Al
2
O
3
); 0.3 MgO; 0.9 (K
2
O+Na
2
O); 3.0F; no
CO
2
; 1.5 SiO
2
; 2.0 insoluble residue.
Currently, only for it, there are technologies for
processing almost any phosphorus-containing
fertilizers with good technical and economic
indicators. The transition to the processing of
poor phosphorites significantly worsens the
technical and economic indicators of the
production of phosphorus-containing fertilizers.
For example, the production of 1t P
2
O
5
in
extractive phosphoric acid from Karatau
phosphorites with a content of 24.5% P
2
O
5
costs
almost 2 times more than from Khibiny apatite
concentrate [5].
In the Republic of Uzbekistan, phosphorites of the
Central Kyzylkum are used as phosphate raw
materials. These phosphorites are phosphorus-
poor phosphate raw materials containing, in
addition, several undesirable impurities. The
average sample of phosphorite from the Jerooy-
Sardara deposit contains (wt.%): 16.2 P
2
O
5
; 46.2
CaO; CaO: P
2
O
5
= 2.85; 17.7 CO
2
; 0.6 MgO; 2.9
(Fe
2
O
3
+Al
2
O
3
); 1.5 (K
2
O+Na
2
O); 2.65 SO
3
; 1.94 F;
7.8 insoluble residue. The low content of
phosphorus, the high value of calcium module
(2.85), the high content of carbonates (17.7%
CO
2
), presence of chlorine (0.1%) make
phosphorite flour of the Central Kyzylkum
practically unsuitable for acid processing in order
to obtain concentrated phosphorus-containing
fertilizers. A high calcium modulus causes a large
overrun of the acidic reagent.
Intensive exploitation of deposits of rich raw
materials naturally leads to their depletion. It is
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becoming more and more difficult and expensive
to extract phosphate raw materials and process
them. Therefore, all over the world, there is a
search for ways to reduce the cost of processes for
obtaining phosphorus-containing fertilizers and
to involve poor phosphate raw materials in
production. Such work is being carried out in
Uzbekistan. Promising in this regard are the
methods
of
chemical,
mechanical,
mechanochemical, thermal, and microbiological
activation of phosphate raw materials, which
convert the indigestible form of P
2
O
5
in the raw
material into a plant-assimilable form at the
lowest cost [6
–
8].
R
ESULTS AND DISCUSSION
Phosphorites of the Central Kyzylkum have
become the main phosphate raw material for
factories in Uzbekistan that produce phosphorus-
containing mineral fertilizers. Phosphorite
manifestations are found in many regions of
Uzbekistan. These are Fergana, Surkhandarya,
Tashkent, Navoi (Pendtikent), Central Kyzylkum,
Bukharo-Khiva and Karakalpak regions. But the
most promising in terms of industrial
development was the Central Kyzylkum [9].
The Kyzylkum phosphorite-bearing basin covers
an area of 65 thousand km2. If we assume that the
industrial phosphorite content covers only 5% of
this area, then the forecast reserves of
phosphorites with an average total thickness of
their layers of 2.5 m will be 16.25 billion tons or
1.95 billion tons of P
2
O
5
(with an average content
of P
2
O
5
of 12%). Marly granular phosphorite ores
have been discovered and studied in the Kyzyl
Kum by exploration work on an area of 3000 km2.
The estimated resources of phosphorites to a
depth of 300 m are 10 billion tons, approximately
2 billion tons of P
2
O
5
, including depths available
for open mining (up to 60 m). 1-1.2 billion tons of
ore, 200-
240 million tons of Р
2
О
5
[9].
The Jerooy-Sardarinskoye deposit, whose
predicted resources are estimated at 2.9-3.0
billion tons of ore (550 million tons of P
2
O
5
), is the
most studied.
A characteristic feature of granular phosphorites
is the stability of the mineral composition. At all
deposits, phosphorites have a three-component
composition. The main mineral composing
phosphate grains is fluoro carbonate apatite
(francolite) with unit cell parameters а0=9.33Ǻ,
с0=6.89 Ǻ, containing 33% Р
2
О
5
, 3.5-
4.0% СО
2
and up to 3% SO
3
, isomorphically included in its
crystal structure. The second important mineral -
calcite forms cement, and is also part of the
granular material of phosphorite ores. Together
with francolite, they make up from 75-80 to 93-
95% of the mass of the ore. A distinctive feature
of the Kyzylkum phosphorites is the presence of
three carbonates in them: relics of calcite,
preserved from replacement by phosphate inside
phosphatized shells - "endocalcite"; cement
calcite
-
"exocalcite";
carbonate group,
isomorphically included in the crystal lattice of
the phosphate mineral The relationship between
calcite and francolite largely determines the
technological properties of ores. The third,
quantitatively, the mineral component of
phosphorite ores - clay substance - is usually
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included in the composition of cement. Its content
is 5-25%. The predominant mineral in the clay
substance is hydromica (21-87% fraction),
montmorillonite (0-86%) and kaolinite (2-15%)
are associated with it. Partial separation of them
from phosphorite ores can be carried out by
washing or dry scrubbing before firing. In
addition to these main minerals, gypsum and
hydro goethite are always present as an
admixture in oxidized phosphorite ores, and
organic matter (up to 4%) and pyrite (up to 1%)
are always present in unoxidized ores. Of
minerals - impurities, the content of which does
not exceed tenths and hundredths of a per cent,
zeolites (clinoptilolite), palygorskite, silty quartz,
and others are noted. The ores of the Jerooy-
Sardara deposit have the following average
mineral composition, %: francolite 56.0; calcite
26.5; quartz 7.5-8.0; hydromicaceous minerals
and feldspars 4.0-4.5; gypsum 3.5; goethite 1.0;
zeolite less than 1; organic matter is about 0.5
[10].
An average sample of phosphorite from the
Jerooy-Sardara deposit contains (wt%): 16.2
Р
2
О
5
; 46.2 CaO; CaO: P
2
O
5
=2.85; 17.7 CO
2
; 0.6
MgO; 2.9 (Fe
2
O
3
+Al
2
O
3
), 1.5 (K
2
O+Na
2
O); 2.65
SO
3
; 1.94 F; 0.1 Cl; 7.8 insoluble residues. This raw
material is poor in phosphorus, complicated for
processing by the presence of a large amount of
undesirable impurities. Such raw materials are
unsuitable
for
obtaining
concentrated
phosphorus-containing fertilizers from it. On the
world market of phosphate raw materials,
phosphorus concentrates with a content of at
least 33% Р
2
О
5
are in demand
Poor raw materials must be enriched. First of all,
you need to get rid of excessive amounts of
carbonates. The most common enrichment
method is flotation. But Kyzylkum phosphorites,
along with a high degree of carbonization, are
characterized by the fine intergrowth of
phosphate minerals with calcite, so attempts to
enrich them using flotation did not lead to
positive results [9].
Chemical processing of natural phosphates is
carried out in three main ways. The most common
method is the decomposition of phosphates with
acids - sulfuric, nitric, phosphoric and
hydrochloric.
In [11, 12], an attempt was made to enrich the
ores of Jerooy-Sardara by a chemical method
using a nitric acid solution of calcium and
magnesium nitrates containing 12% Ca(NO
3
)2,
10% Mg(NO
3
)
2
and 4.06% HNO
3
. The degree of
extraction of carbon dioxide was 63-65%, and the
transition of P
2
O
5
to the liquid phase was 0.14-
0.78%.
Using 15% nitric acid, selective decomposition of
the carbonate part of phosphorite (more than
80%) with the smallest losses of P
2
O
5
with a
solution (10-11%) can be achieved at an acid rate
of 80% for the CO
2
content in phosphorite, a
temperature of 30-35
℃
and processing time 30-
40 min.
When using nitric acid with a concentration of 9%
in an amount of 30% of the stoichiometry and
maintaining the treatment process for 50
minutes. It is possible to reduce the CO
2
content
in the ore from 17% to 8.2%. The loss of P2O5
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with the liquid phase does not exceed 1%. When
using sulfuric acid (3-9%), it is not possible to
achieve the required degree of CO
2
removal, since
a significant amount of P
2
O
5
passes into the liquid
phase (up to 18.34% of the initial one) [13].
In [14], for chemical enrichment of phosphorites
of the Central Kyzylkum, a nitric acid extract of
phosphate raw materials was used. It is shown
that under optimal conditions of the process, the
content of P
2
O
5
phosphorite increases from 18.5
to 31.3%. The maximum content of P
2
O
5
, the
minimum content of CO
2
(2.8%) and CaO (40.7%)
in the concentrate is achieved at an H
3
PO
4
concentration of 6.0%, a nitric acid extract rate of
100% and a temperature of 15
℃
; interaction
time (60-90 min.) does not play a significant role.
The yield of P
2
O
5
in the filtrate (12.3%) reaches a
minimum at an H
3
PO
4
concentration of 6.0%, an
extraction rate of 80%, and a temperature of 15
℃
. The disadvantages of chemical enrichment
methods are:
1) the formation of a large amount of dilute salt
solutions that cannot be drained into the sewer,
but must be disposed of somehow;
2) loss of P
2
O
5
with these solutions, since 100%
selectivity in the extraction of carbonates cannot
be achieved.
With a high content of carbonates in phosphate
raw materials, as is the case in Kyzylkum
phosphorites (17.7% CO
2
), the best method of
enrichment of such raw materials is thermal.
Therefore, roasting was included in the combined
technological scheme for the enrichment of
phosphorites,
which
has
already
been
implemented at the Kyzylkum phosphorite plant.
This scheme also provides for the washing of raw
materials from chlorides bringing the chlorine
content in washed, dried and washed, calcined
phosphorus concentrates to an acceptable rate of
0.04% [15].
Promising in the issue of enrichment of low-grade
phosphorites is phosphoric acid decomposition,
to obtain both unilateral and complex fertilizers.
The decomposition of minerals contained in
natural phosphates with phosphoric acid occurs
according to the following main reactions:
(
)
(
)
5
4
3
4
2
2
4
2
3
2
7
5
5
Ca F
PO
H PO
H O
Ca H PO
H O
HF
+
+
=
+
(
)
(
)
(
)
3
3
4
2
4
2
2
4
2
2
2
2
2
4
2
MgCa CO
H PO
Ca H PO
H O
Mg H PO
H O
CO
+
=
+
+
2
3
3
4
2
4.
2
2
2
2
R O
H PO
H O
RPO
H O
+
+
=
Phosphoric acid decomposition of phosphate raw
materials underlies the production of a single
phosphorus fertilizer - double superphosphate,
both by the in-line and by the chamber method.
This type of fertilizer is one of the cheapest
concentrated phosphate fertilizers, suitable for
use on any soil and for all crops [16].
The paper [17] studied the physical and
mechanical properties and chemical composition
of off-balance phosphorus-containing raw
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materials - mineralized mass, in order to process
it into one-sided phosphorus [18-23], as well as
complex phosphorus-containing fertilizers [24-
32].
The rheological parameters, as well as the water-
insoluble part, were studied [33]. Mineralized
mass was used as raw material (composition, wt.
%: 14.33 P
2
O
5
; 43.66 CaO; 1.19 MgO; 1.38 Fe
2
O
3
;
1.18 Al
2
O
3
; 2.22 SO
3
; 14.70 CO
2
; 1. 75 F; 13.23 n.o.)
- waste from the production of washed calcined
phosphorus
concentrate
and
extraction
phosphoric acid (EPA) of Almalyk JSC
"Ammophos-Maxam" composition (wt.%): 18.43
Р
2
О
5
; 0.21 CaO; 0.30 MgO; 0.44 Fe
2
O
3
; 0.79 Al
2
O
3
;
1.71F; 1.47 SO
3
. The number of initial
components was taken based on the mass ratios
of EPA: FS from 100:15 to 100:30.
Samples of ammophosphate that meet the
requirements of agriculture were obtained, and
their rheological properties were also studied
[24]
In order to study the water-insoluble part of
ammophosphate fertilizers, namely its chemical
composition, because the difference between the
total and water-soluble forms of P
2
O
5
in the
products was a significant achievement of the
goal after the interaction of the extraction of
phosphoric acid with the mineralized mass under
the conditions [24], the pulp was quickly filtered
under a vacuum of 550- 600 mmHg Art. on a
Buchner funnel using one layer of filter paper. The
precipitate remaining on the filter was washed
with hot water until neutral according to the
indicator paper. The washed precipitate was
dried with filter paper in an oven at 105
℃
. The
dried precipitate was weighed and analyzed for
the content of total, digestible, and water-soluble
forms of P
2
O
5
. The results are shown in Table 1.
Table 1. Composition of the water-insoluble part of ammophosphate fertilizers
Mass ratio
EPA: FS
Mass
of dry
sedim
ent,
gr.
P
2
O
5
content, wt. %
,
in 2% lim.
acid, %
by 0.2 M
tril. B, %
Р
2
О
5
tot
.
Р2О5usv.
in 2% lim.
Kis-te
Р
2
О
5
usv.
by 0.2 M
tril. B
Р
2
О
5
a
q.
100:15
8.6
16.70
8.99
7.42
0.32
53.83
44.43
100:20
11.4
17.89
8.27
6.96
0.28
46.23
38.90
100:25
15.8
21.49
8.96
7.49
0.10
41.69
34.85
100:30
22.2
22.11
8.94
6.96
-
40.43
31.48
From the data in the table, one can observe the
presence of trace amounts of water-soluble P2O5,
but this indicates insufficient washing of the
precipitate. The main result of the study is that in
the water-insoluble part of the fertilizer, 40-54%
of phosphorus is in the form digestible for plants
общ
усв
О
Р
О
Р
5
2
5
2
,
5
2
5
2
общ
усв
О
Р
О
Р
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in relation to its total content. This suggests that
when phosphoric acid interacts with the
mineralized mass, the phosphate mineral is
activated. Activation is facilitated by the intensive
release of CO2 from the phosphate mineral, which
destroys its structure. Upon activation, unreacted
phosphates differ significantly in structure from
the original ones. Their grains are etched with
acid, have a porous structure and are 15-30 times
smaller than the original ones. Therefore,
although they are water insoluble, their P2O5 is
available to plants. That is why ammophosphates
belong to the so-called
C
ONCLUSION
Suitable for nitric acid decomposition are natural
phosphates that do not contain significant
amounts of calcium carbonate, magnesium
carbonate and silicates, iron and aluminium
compounds. All these impurities hinder the
processing of phosphates and degrade the quality
of fertilizers. Particularly harmful are impurities
of iron-containing minerals that are easily
decomposed by acids, such as glauconite, and
limonite, for example. Promising in this matter is
the enrichment of low-grade phosphorites with
phosphoric acid. Fertilizers obtained as a result of
phosphoric acid decomposition have a high
concentration of the nutrient component, as well
as positive physical and mechanical properties.
R
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Горный
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Минеев, В. Г., & Бычкова, Л. А. (2003).
Состояние и перспективы применения
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земледелии.
Агрохимия, (8), 5
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