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УДК 678.8
PHYSICAL STUDIES OF LIGHTWEIGHT TAMPONADE COMPOSITE MATERIAL
BASED ON MICROSILICA AND LOCAL ORGANOMINERAL INGREDIENTS
Panjiev Olimjon Khollievich
Doctoral student, State Unitary Enterprise "Fan va Tarakkiyot"
Uzbekistan, Tashkent.
Abstract:
The paper presents the results of selecting the composition of composite gypsum
materials using inorganic fillers - ash microspheres, which are formed during the combustion of
coal at thermal power plants.
Based on the laboratory studies, composite compositions have been developed for obtaining
thermal insulation building products with low bulk density. The rheological properties and
physical and mechanical properties of mortar mixtures have been studied and the optimal
compositions of composite gypsum mixtures for the production of thermal insulation materials
using aluminosilicate ash microspheres have been determined.
Key words:
mineral binders, filler, aluminosilicate microsphere, low bulk density, superplasticizer,
composite composition, density, thermal insulation materials.
This project considers the development of a composition of lightweight composite
cements aimed at improving the quality of well casing and sealing of their lining. Particular
attention is paid to fields with low hydraulic fracturing gradients, where the use of lightweight
cement slurries is required.
The most effective approach to solving these problems is the use of special composite
lightweight expanding cement materials. The main objective of this work was to study the role and
mechanisms of action of modifying additives (expanding, lightweight, reinforcing and others) in
the composition of cement cements, to conduct a set of studies and improve the formulations of
lightweight cement materials.
To achieve this goal, various fillers and modifying additives were studied that can
improve the properties of cement cements, including strength, density and resistance to aggressive
environments.
One of the key components that determine the properties of cement materials is clinker -
the main product of firing the raw mix used in the production of Portland cements. The
mineralogical composition of clinker has a significant impact on the rheological and physical-
mechanical properties of cement mixtures, which makes its study an important stage in the
development of lightweight cementing materials [1].
There is a classification of clinkers by mineralogical composition. If the mass fraction of
C₃S exceeds 60%, the clinker is called alite; with a mass fraction of C₂S over 37% - belite; with a
C₃A content over 13% - aluminate; and with a mass fraction of C₄AF over 5% - aluminoferrite.
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Combined types are also distinguished, such as alite-aluminate or belite-aluminate clinkers.
Clinkers whose composition is within the specified limits are classified as normal.
For the production of oil well cements, mainly alitic and normal clinkers are used.
However, for special conditions, special compositions can be developed that meet specific
requirements [2].
Inert mineral additives are additives of mineral origin, which under normal conditions
only slightly chemically interact with the main substance of Portland cement during the hardening
process. Limestone and quartz sand are most often used as inert mineral additives. If the hardening
conditions deviate significantly from normal, inert additives can become active. Quartz, crushed or
in the form of sand, becomes an active additive at temperatures above 60 °C [3].
To develop the compositions of composite lightweight oil well cements in this work,
Portland cement grade M400, produced by the Navoi Cement Plant, was used as the main binder,
and microsilica, a silica-containing technogenic waste from the production of JSC
Uzmedkombinat (Bekabad), was used as a microfiller.
Binding construction substances are powdered materials that, when mixed with water,
form a plastic, easy-to-process mass that hardens over time into a durable rock-like div. In this
paper, the hydraulic binder is Navoi Portland cement grade M400 D0, tested in accordance with
the requirements of GOST 10178-85. The chemical and mineralogical composition of Portland
cement is presented in Tables 1 and 2.
Table 1 - Chemical composition of Portland cement of the Navoi Cement Plant
Oxide content, wt.%
SiO
2
А1
2
О
3
Fe
2
О
3
СаО
MgO
SO
3
R
2
O
ППП
Сумма
23,96
4,7
0,79
66,76
2,86
0,57
0,30
-
100,0
Table 2 - Mineralogical composition of cement from Navoi Cement Plant
Cement
Mineral content, mass, %
C
3
S
C
2
S
C
3
A
C
4
AF
Cement M400 D 0
56.51
26,08
11,24
2,40
Table 3 - Physical and mechanical characteristics of Portland cement of Navoi cement plant
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№
Name of parameters
The meaning of the parameters
of cement M400 DO
1
Degree of grinding: residue on sieve No. 008,%
6,4
2
Water/binder ratio
0,32
3
Setting time, hours-minutes
– beginning of setting
– end of setting
2-25
4-50
4
Compressive strength, at the age of 28 days, MPa
49,5
5
Bending strength, 28 days, MPa
6,7
Figure 1 - X-ray diffraction pattern of Portland cement from Navoi Cement Plant
In oil and gas regions with complex geological and technical conditions, problems with high-
quality layer isolation often arise. Analysis of literature data [4] shows that the number of wells
experiencing complications after cementing remains significant.
One of the main reasons for unsatisfactory well casing may be the use of standard oil well
cement. Portland cement without additives often proves ineffective in complex geological and
technical conditions and requires modification to ensure reliable isolation.
Table 4 - Physical characteristics of microsilica.
№ Name of indicators
The meaning of the indicators
1
Appearance
Ultrafine material of dark gray light
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2
Ultrafine material of dark gray light
3
3
Loss on ignition (LOI), % no more than
3
4
Mass fraction of silicon dioxide (SiO2) % not less
than
85
5
Mass fraction of sulfur dioxide (SО
3
) % no more
than
0,6
6
Mass fraction of magnesium oxide (MgO), no
more than
3
7
Bulk density, kg/m³, not less than
250
Note: bulk density in uncompacted state – 0.25 t/m³; in compacted state – up to 0.40-0.70
t/m³.
According to the results of studies conducted by an accredited laboratory, the chemical
composition of microsilica of Uzmedkombinat is presented in Table 5.
Table 5 - Chemical composition of microsilica of Uzmedkombinat
Oxide content, mass %
SiO
2
Al
2
O
3
Fe
2
O
3
МgO
СaO
Na
2
O
K
2
O
SО
3
C
П.п.п.
93,80
0,70
0,90
1,00
1,20
0,50
0,0
0,20
0,80 0,60
Figure 2 shows a diffraction pattern of microsilica, from which it is evident that the main
phase of the finely dispersed material is SiO
2
Figure 2 - Diffraction pattern of Uzmedkombinat microsilica
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In the diffraction pattern of Uzmedkombinat microsilica (Fig. 2), the main component of
the material is amorphous silica (SiO₂), which is confirmed by the characteristic wide diffuse peak
in the range of 2θ ≈ 20–30°. These characteristics indicate the amorphous state of the substance
and confirm the high pozzolanic activity of microsilica, which makes it an effective component for
use in composite plugging materials.
Microsilica is a by-product of ferroalloy production, consisting of spherical particles of
active silicon oxide. The average particle size of microsilica is 0.05-0.1 μm, which is
approximately 100 times smaller than the average particle size of cement. Due to its high
dispersion and amorphous state, microsilica has significant pozzolanic activity and acts as an
effective microfiller [6].
In concrete, microsilica exhibits two key effects: microfilling and pozzolanic. The
microfilling effect consists of filling the voids between cement grains with the smallest particles of
microsilica, as well as creating crystallization centers, which contributes to more uniform
hardening of the cement stone.
The pozzolanic effect is caused by the chemical interaction of microsilica with calcium
hydroxide, which is released during the hydration of cement. As a result of the interaction, strong
low-basic calcium hydrosilicates are formed, which significantly improves the properties of
cement stone. The use of microsilica helps to increase the volume of gel pores and reduce capillary
pores, increases the density, water resistance and frost resistance of concrete.
The use of microsilica is advisable in combination with water-reducing additives, such as
superplasticizers (SP). Due to its high dispersion, microsilica absorbs a significant amount of
water, which without the use of SP can minimize the positive effect of the active mineral additive,
and in some cases even reduce the strength characteristics of concrete.
The new generation superplasticizer "Polyplast SP-1", created on the basis of
polycarboxylate esters, ensures high mobility and cohesion of mortar mixtures of lightweight oil
well cement at low values of the water-cement ratio, and also preserves their properties for a
long time. For SP based on polycarboxylates, the presence of an anionic base and a hydrophobic
effect is characteristic, ensuring the repulsion of particles of the solid phase. The type and length
of the main chain, as well as the length and frequency of the side chains vary in different SP
molecules, which allows for effective control of their adsorption processes on binder grains.
In the oil and gas industry of the republic, an urgent task is the development,
implementation and application of lightweight oil well cement compositions using finely dispersed
industrial waste as active mineral additives. Such additives, in combination with various chemical
modifiers, help to increase the reactivity of oil well cement slurries.
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Figure 3 - Change in the normal density of composite binders for the production of thermal
insulation materials from the content of microsilica
It is known that the setting time of cements depends on the normal density, fineness of
grinding and various additives. In this regard, studies were conducted to study the effect of the
content of microsilica on the setting time of composite binders intended for the production of
thermal insulation materials.
To determine the setting time of the developed composite binders, the Vika device was
used. The results are shown in Figure 4. The studies have shown that with an increase in the
content of microsilica, both the beginning and end of the setting of the mortar mixture increase.
It was found that the increased water demand of composite binders, caused by an
increase in the content of microsilica, slows down the hydration process, which leads to an
extension of the setting time of the composite mortar mixture. To study the effect of microsilica
on the strength characteristics of the developed composite binders, standard samples measuring
4×4×16 cm were prepared from normal-density dough.
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(Н.С. - beginning of setting, К.С. - end of setting.)
Figure 4 - Effect of microsilica on the setting of composite binders
The results of the studies showed that the addition of microsilica even in the amount of 2-
5% helps to compact the structure of the transition zone by filling the free spaces. This leads to a
decrease in the size of the crystals and strengthening of the weak zone of the hardened mortar
mixture, and also increases the adhesion of the cement matrix.
In addition, the pozzolanic reactions of finely dispersed microsilica have a chemical effect,
contributing to a further increase in the strength and durability of lightweight oil well cement.
A study of the hardening process of lightweight oil well cement showed that during the
first 7 days of hardening of composite oil well cements, microsilica has a noticeable effect on the
strength properties. Its interaction with the hydration products of cement monominerals begins in
the early stages of hardening of mortar mixtures based on composite binders and is completed by
the 28th day.
Based on the conducted research, it was established that the introduction of microsilica
into the composition of the cement mixture and the creation of composite binders has a positive
effect on the rheological properties of the cement paste, as well as on the bulk density of products
made on their basis.
It was found that the spherical shape of finely dispersed microsilica particles promotes the
formation of a porous structure during interaction with a gas-forming reagent in molded products.
Finely dispersed microsilica particles fill the volume between coarsely dispersed particles of
hydrated cement compounds, which significantly reduces water separation from the composite
mortar mixture.
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The use of cement-microsilica compositions in the production of thermal insulation
materials allows obtaining products with a bulk density of 300-500 kg / m³, with a low thermal
conductivity coefficient and improved thermal insulation characteristics.
In order to reduce water consumption and increase the fluidity of the cement-microsilica
mortar mixture, the study used the superplasticizer of the "Polyplast SP-1" brand. The results of the
studies showed that an increase in the microsilica content in the mixture leads to an increase in
spreadability, while the addition of a superplasticizer helps to reduce the normal density of the
mortar mixture.
Figure 5 - Effect of superplasticizer content on the normal density of cement-microsilica
composite mortar mix
without superplasticizer; 2- 0.75% superplasticizer SP-1
From Figure 5 it is evident that with an increase in the microsilica content in the composition,
the normal density of the mortar mix without superplasticizer (curve 1) increases significantly,
reaching more than 200% with a content of 20% microsilica. Adding 0.75% superplasticizer SP-1
(curve 2) allows to significantly reduce the normal density: with the same microsilica content, the
indicators decrease to 150%, which improves the processability and workability of the mix.
A study of the hardening process of lightweight oil-well cements showed that microsilica has
a positive effect on the strength characteristics at all stages of hardening. The interaction of
microsilica with hydration products begins at the early stages of hardening and continues up to 28
days, providing a significant improvement in mechanical properties. Laboratory studies have
shown that the developed compositions of the cement-microsilica composition have low density
and high strength characteristics, which meets the requirements for materials used in the oil and
gas industry for cementing casing columns.
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