CN106565383A - Composite particle, and preparation method and application thereof - Google Patents
Composite particle, and preparation method and application thereof Download PDFInfo
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- CN106565383A CN106565383A CN201510671409.0A CN201510671409A CN106565383A CN 106565383 A CN106565383 A CN 106565383A CN 201510671409 A CN201510671409 A CN 201510671409A CN 106565383 A CN106565383 A CN 106565383A
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Abstract
The invention relates to the technical field of oil gas well cementing, and especially relates to a composite particle, and a preparation method and an application thereof. The composite particle comprises a core which is an elastic particle and a shell layer which is a rigid particle and coats the external surface of the core. The preparation method of the composite particle is characterized in that airflow entrainment is used to drive the elastic particle and the rigid particle to move relative to each other in order to form the composite particle. The composite particle has high temperature resistance, improves the acid and alkali resistance of the elastic particle, has good stability, has good compatibility with cement mortar, has no floatation phenomenon, has no thickness increase phenomenon in the curing process, obviously reduces the elastic modulus of set cement, increases the deformation ability of the set cement, is spherical, and facilitates increase of the fluidity of the cement mortar.
Description
Technical field
The present invention relates to oil gas well cementing operation technical field, more particularly to a kind of composite particles, its preparation method and application.
Background technology
As gas well annular space phenomenon with pressure is more and more universal, the sealing quality of cement sheath and durability are increasingly subject in industry
Pay attention to.But traditional cements stone is a kind of fragile material, oil well long-term production or operation process cement sheath easily occur crackle or
Person's microannulus, causes wellheadpressure.Especially current shale oil gas, the application of fine and close Oil/gas Well staged fracturing technology, to water
Mudstone elastic deformability requires higher, it is desirable to which Behavior of Hardened Cement Paste can couple casing deformation.Therefore in order to effectively improve Behavior of Hardened Cement Paste
Long term seal ability, it is desirable to have effect improves the mechanical property of Behavior of Hardened Cement Paste, improves the deformability of Behavior of Hardened Cement Paste, effectively reduces cement
The elastic modelling quantity of stone, and ensure the enough intensity of Behavior of Hardened Cement Paste.The material for improving Behavior of Hardened Cement Paste elastic performance conventional at present mainly has：
The materials such as styrene-butadiene latex latex, styrene-acrylic latex, rubber grain and organic resin class, but latex and organic resin class material are because of valency
Lattice are high and limit widely using for they, rubber grain and resin material are affected due to temperature resistance ability and the defect of itself
Its application in oil gas well cementing operation.Wherein rubber grain becomes many elasticity water due to wide material sources, low price
The preferred material of mud system, but its surface hydrophobicity, and easily floating and temperature tolerance are poor, cause its application to receive larger
Restriction.
It is therefore desirable to developing a kind of novel elastic material based on nucleocapsid structure, the cement mortar to be formed is set to reduce
Behavior of Hardened Cement Paste elastic modelling quantity, reduces Behavior of Hardened Cement Paste fragility, increases Behavior of Hardened Cement Paste deformability, and rationally reduces cost.
The content of the invention
One of present invention provides a kind of composite particles, and the composite particles are by the elastic granule as kernel and are coated on described
The rigid particles as shell of kernel outer surface are constituted.
Additionally, by mechanical coating technology, realizing carries out the possibility of physical modification to elastic granule, by elastic granule
Surface physics coats such as rigid material such as SILICA FUME, flyash, particularly with the hydraulicity and/or alkali-activated carbonatite volcano grey matter
Material, realize non-porous cladding, the water-wet behavior of inner nuclear material can be effectively improved, further improve elastic granule and cement
Cementation between stone, improves the temperature resistant capability and stability of elastic granule, while Mechanical Behavior of Hardened Cement Paste can be improved, effectively
Behavior of Hardened Cement Paste elastic modelling quantity is reduced, increases Behavior of Hardened Cement Paste strain rate.Therefore, using the composite particles of nucleocapsid structure of the invention, energy
It is enough effectively to meet high temperature well cementing requirements.
It is pointed out that the kernel of the composite particles of the present invention only has an elastic granule, and the quantity of the granule of shell is remote
More than one, but to reach the quantity of non-porous cladding and/or continuous cladding elastic granule.Wherein non-porous cladding is referred to and is coated with
The composite particles of the shell of the present invention fail to find diesel component after the non-porous experimental test of embodiments of the invention 7
Cladding；Continuous cladding refers to that the composite particles of the shell for being coated with the present invention are surveyed by the non-porous test of embodiments of the invention 7
After examination, the cladding of diesel component can be found.
In a specific embodiment, the shell is coated on the outer layer of the kernel in non-porous form.Using non-porous cladding
Can effectively prevent water from penetrating into by shell, prevent core water-swellable, while the ratio of mud in cement mortar can be reduced, improve cement
Stone mechanical property.
When elastomeric material is in reasonable dosage proportion, under compression elastic deformation amount exists to can guarantee that Behavior of Hardened Cement Paste
Between 0.1-0.5%, destruction of the factors such as staged fracturing and thermal expansion to Behavior of Hardened Cement Paste at this moment can be effectively prevented, it is solid so as to ensure
The long term seal ability of Behavior of Hardened Cement Paste after well, improves safety in production time and the Inter-zonal packing effect of Oil/gas Well.Therefore, at one
In specific embodiment, the ratio of the thickness of the mean diameter of the kernel and the shell is 2:1-8:1, preferably 2:1-5:1.
In a specific embodiment, the elastic granule includes latex powder of the elastic modelling quantity less than 1.5GPa, the preferably bullet
Property granule include acrylonitrile-butadiene rubber powder and/or styrene butadiene rubber powder.
In a specific embodiment, the mean diameter of the elastic granule be 100-180 microns, particle diameter d50=110-165
Micron；It is preferred that the mean diameter 120-140 micron of the elastic granule, particle diameter d50=125-145 microns.
In a specific embodiment, the shore hardness of the elastic granule be 60-100, in mass, phosphorus content be less than or
Equal to 1.0%；It is preferred that the shore hardness of the elastic granule is 70-85, phosphorus content is less than or equal to 0.5%.
In a specific embodiment, the rigid particles are the material with the hydraulicity and/or alkali-activated carbonatite volcano grey matter, preferably
The material includes at least one in silicon ash, flyash and metakaolin.
In a specific embodiment, the flat mean diameter of the rigid particles be 1.0-10.0 microns, particle diameter distribution
d50=1.35-8.5 microns；Preferably 1.3-5.6 microns, particle diameter distribution d50=1.35-5.4 microns.
The two of the present invention provide a kind of method for preparing composite particles as above, and it comprises the steps：
Air-flow carries the elastic granule secretly and the rigid particles do relative motion in confined conditions, described compound so as to be formed
Granule.
In a specific embodiment, the mass ratio of the elastic granule and the rigid particles is 100:(10-50) it is, excellent
Elect 100 as:(20-30).
In a specific embodiment, the system rotating speed for controlling the air-flow is 1500-3000rpm；It is preferred that the system rotating speed
For 2000-2500rpm.
In a specific embodiment, the time that the elastic granule and the rigid particles do relative motion is carried secretly using air-flow
For 20-30 minutes.
The three of the present invention provide a kind of application of composite particles as above in oil gas well cementing operation.
Compared with prior art, the invention has the beneficial effects as follows：
(1) composite particles temperature tolerance of the invention is high, improves the acidproof alkali ability of elastic granule；
(2) composite particles good stability of the invention；
(3) composite particles of the invention are good with the cement mortar compatibility, and in cement mortar maintenance processes, composite particles occur without drift
Emerge as while cement mortar occurs without thickening behavior, so that cement slurry property is greatly improved；
(4) composite particles of the invention can substantially reduce Behavior of Hardened Cement Paste elastic modelling quantity, increase the deformability of Behavior of Hardened Cement Paste；
(5) composite particles of the invention are spherical, are conducive to increasing the mobility of cement mortar.
Description of the drawings
Fig. 1 is shown the structural representation of nucleocapsid structure composite particles, and wherein inner core is elastic granule, and outside is rigidity
The shell that particles coat kernel is formed.
Fig. 2 is shown the forming process schematic diagram of composite particles, can carry out spheroidization to elastomeric material first as needed,
Then the rigid particles after processing with spheroidization, such as after silicon ash mix homogeneously, formed using dry type impact composite algorithm connect afterwards
The granule of continuous and/or non-porous cladding.
Fig. 3 is shown PCS-1 system flow charts；Wherein, 1 is loading hopper, and 2 is injector, and 3 is processing system, 4
For cooling system, 5 is control system.
Fig. 4 is shown microstructure of the composite particles under scanning electron microscope, as can be seen from the figure the sphericity of composite particles
It is very high.
Specific embodiment
In the present invention, using compound particle hybrid system (Tsing-Hua University, PCS-1), using dry type composite algorithm, profit are impacted
The high velocity air particle of carrying under one's arms for producing is rotated with equipment and does high speed relative motion, by impact make elastic granule and rigid particles with
There is compound, the elastic particle of formation nucleocapsid structure with electrostatic force in Van der Waals force.Existed by adjusting system rotating speed
1500-3000r/min, control system input raw material is opened row's powder and is switched by switch board again after operation 20-30min, arranges powder
15-20min, forms final products.
In the present invention, elastic modelling quantity is measured using instrument ToniPrax (Germany), accepted standard is GB/T 23561.8.
Poisson's ratio is measured using instrument ToniPrax (Germany), accepted standard is GB/T 50081-2002).Using U.S.'s instrument
Instron2450-200 measures comprcssive strength and tensile strength, and accepted standard is GB/T 50081-2002, wherein, resistance to compression
Intensity and tensile strength use same device measuring).
Embodiment 1
By 100 weight portions, mean diameter is 120 microns, particle diameter d50=123 microns, elastic modelling quantity is 0.6GPa, shore
Hardness is 70, and phosphorus content is for (mean diameter is 1.45 in 30 parts of silicon ashes added after ball-type of nitrile rubber granule of 0.5wt%
Micron, particle diameter d50=1.40 microns, stir, and adjust compound particle hybrid system (Tsing-Hua University, PCS-1) and turn
2500 revs/min of speed, controls charging rate 5kg/ minute, coats 30 minutes time, and it is 180 microns to collect mean diameter,
Particle diameter d50=175 microns of composite particles.
Embodiment 2
By 100 weight portions, mean diameter is 180 microns, particle diameter d50=165 microns, elastic modelling quantity is 0.8GPa, shore
Hardness is 85, and phosphorus content is that 0.5% butadiene-styrene rubber granule adds 20 weight portions after ball-type, and mean diameter is 5.6 micro-
Rice, particle diameter d50=5.4 microns, phosphorus content is in 0.5% flyash, to stir, and adjusts PCS-1 rotating speeds 2000
Rev/min, charging rate 5kg/ minute is controlled, 20 minutes time is coated, collect 250 microns of product mean diameter, particle diameter
d50=240 microns of composite particles.
Embodiment 3
By 100 weight portions, mean diameter is 120 microns, particle diameter d50=125 microns, elastic modelling quantity is 0.5GPa, shore
Hardness is 60, and phosphorus content is that 0.5% butadiene-styrene rubber granule adds 10 weight portions after ball-type, and mean diameter is 1.6 micro-
Rice, particle diameter d50In=1.2 microns of metakaolin, stir, and adjust 1000 revs/min of PCS-1 rotating speeds, control into
Material speed 5kg/ minute, 20 minutes time is coated, collect 215 microns of product mean diameter, particle diameter d50=220 microns answer
Close granule.
Embodiment 4
By 100 weight portions, mean diameter is 100 microns, particle diameter d50=110 microns, elastic modelling quantity is 1GPa, and shore is hard
Spend for 90, phosphorus content is that 0.5% butadiene-styrene rubber granule adds 50 weight portions after ball-type, and mean diameter is 1.0 microns,
Particle diameter d50=1.35 microns, phosphorus content is in 0.5% flyash, to stir, and adjust 3000 turns of PCS-1 rotating speeds/
Minute, charging rate 5kg/ minute is controlled, 20 minutes time is coated, collect 200 microns of product mean diameter, particle diameter d50=189
The composite particles of micron.
Embodiment 5
By 100 weight portions, mean diameter is 120 microns, and particle diameter distribution index is d50=125 microns, elastic modelling quantity is
1.5GPa, shore hardness is 100, and phosphorus content is that 0.5% butadiene-styrene rubber granule adds 25 weight portions after ball-type, is put down
Particle diameter is 1.3 microns, particle diameter d50=1.35 microns, phosphorus content is in 0.5% flyash, to stir, and adjusts PCS-1
2000 revs/min of rotating speed, controls charging rate 5kg/ minute, coats 20 minutes time, collects product mean diameter 233 micro-
Rice, particle diameter d50=240 microns of composite particles.
Embodiment 6
By 100 weight portions, mean diameter is 141 microns, particle diameter d50=145 microns, elastic modelling quantity is 0.7GPa, shore
Hardness is 80, and phosphorus content is that 1.0% butadiene-styrene rubber granule adds 40 weight portions after ball-type, and mean diameter is 10.0 micro-
Rice, particle diameter d50=8.5 microns, phosphorus content is in 0.5% flyash, to stir, and adjusts PCS-1 rotating speeds 2000
Rev/min, charging rate 5kg/ minute is controlled, 20 minutes time is coated, collect 215 microns of product mean diameter, particle diameter
d50=210 microns of composite particles.
Embodiment 7
By the sample of composite particles randomization 30 prepared in embodiment 1, divide 3 groups, per group of 10 samples soak respectively bavin
24 hours in oil, room temperature is air-dried 2 hours using air-dry machine, destroys nucleocapsid structure, is taken core and is carried out spectrofluorimetry,
First group of 9 samples, second group of 10 samples, the 3rd group of 9 samples, do not find diesel component, illustrate to realize more than 90%
Non-porous cladding.
Also, other embodiment also plays similar effect.
Comparative example 1
In order to contrast addition composite particles and the improvement for being not added with compound particle Mechanical Behavior of Hardened Cement Paste, ordinary water is made first
Mudstone test sample, that is, be not added with compound particle, using 100 parts of cement (good China G levels, Dezhou continental shelf company), drops
5 parts of fluid loss agents (DZJ-Y, Dezhou continental shelf company), 1.2 parts of dispersant (DZS, Dezhou continental shelf company), slow setting
1.5 parts of agent (DZH-2, Dezhou continental shelf company), 40 parts of water, defoamer (DZX, Dezhou continental shelf company) 0.2
Part, the mortar architecture of traditional performance is configured, density is 1.9g/cm3, conserve 72 hours under 80 DEG C and 20MPa environment,
Measurement elastic modelling quantity, Poisson's ratio, comprcssive strength and tensile strength.The results are shown in Table 1.
Embodiment 8
Using 100 parts of cement (good China G levels, Dezhou continental shelf company), fluid loss additive (DZJ-Y, Dezhou continental shelf public affairs
Department) 5 parts, 1.2 parts of dispersant (DZS, Dezhou continental shelf company), retarder (DZH-2, Dezhou continental shelf company)
1.5 parts, 40 parts of water, 6 parts of the composite particles prepared in embodiment 1- embodiment 7,0.2 part of defoamer configures density
For 1.9g/cm3, conserve 72 hours under 80 DEG C and 20MPa environment, measurement elastic modelling quantity, Poisson's ratio, comprcssive strength and anti-
Tensile strength.The results are shown in Table 1.
Compared with comparative example 1, adding Behavior of Hardened Cement Paste elastic modelling quantity after the composite particles in embodiment 1- embodiment 7 substantially reduces,
Deformability is most strong.
The result of the present embodiment shows, composite particles can effectively improve the temperature tolerance of original elastic granule, stability and with
Cement it is cementing, while Behavior of Hardened Cement Paste elastic modelling quantity is greatly reduced.Effectively improve the hard crisp characteristic of Behavior of Hardened Cement Paste, improve Behavior of Hardened Cement Paste
Durability, be conducive to improve gas well Behavior of Hardened Cement Paste long-term sealing ability, and meet the unconventionaloil pools such as shale gas segmentation pressure
Split the demand to Behavior of Hardened Cement Paste.
Table 1
| Embodiment | Behavior of Hardened Cement Paste elastic modelling quantity | Poisson's ratio | Comprcssive strength | Tensile strength |
| Embodiment 1 | 3.2GPa | 0.20 | 14.5MPa | 2.0MPa |
| Embodiment 2 | 3.0GPa | 0.21 | 10.5MPa | 1.7MPa |
| Embodiment 3 | 2.8GPa | 0.22 | 8.4MPa | 1.45MPa |
| Embodiment 4 | 3.8GPa | 0.20 | 16.2MPa | 2.1MPa |
| Embodiment 5 | 3.2GPa | 0.20 | 15.4MPa | 2.1MPa |
| Embodiment 6 | 2.8GPa | 0.21 | 8.2MPa | 1.7MPa |
| Comparative example 1 | 11.5GPa | 0.19 | 28.5MPa | 2.4MPa |
Claims (12)
1. a kind of composite particles, the composite particles are by the elastic granule as kernel and the work for being coated on the kernel outer surface
Rigid particles for shell are constituted.
2. composite particles according to claim 1, it is characterised in that the shell is coated on described in non-porous form
The outer layer of kernel.
3. composite particles according to claim 1 and 2, it is characterised in that the mean diameter of the kernel and the shell
The ratio of the thickness of layer is 2:1-8:1, preferably 2:1-5:1.
4. composite particles according to any one in claim 1-3, it is characterised in that the elastic granule includes bullet
Property latex powder of the modulus less than 1GPa, the preferably elastic granule includes acrylonitrile-butadiene rubber powder and/or styrene butadiene rubber powder.
5. composite particles according to any one in claim 1-4, it is characterised in that the elastic granule it is average
Particle diameter be 100-180 microns, particle diameter d50=110-165 microns；It is preferred that the mean diameter 120-140 micron of the elastic granule,
Particle diameter d50=125-145 microns.
6. composite particles according to any one in claim 1-5, it is characterised in that the shore of the elastic granule
Hardness is 60-100, and in mass, phosphorus content is less than or equal to 1.0%；It is preferred that the shore hardness of the elastic granule is 70-85,
Phosphorus content is less than or equal to 0.5%.
7. composite particles according to any one in claim 1-6, it is characterised in that the rigid particles be with
The material of the hydraulicity and/or alkali-activated carbonatite volcano grey matter, the preferably material are included in silicon ash, flyash and metakaolin at least
It is a kind of.
8. composite particles according to any one in claim 1-7, it is characterised in that the rigid particles it is average
Particle diameter be 1.0-10.0 microns, particle diameter distribution d50=1.35-8.5 microns；Preferably 1.3-5.6 microns, particle diameter distribution d50=1.35-5.4
Micron.
9. a kind of method of the composite particles prepared as described in any one in claim 1-8, it comprises the steps：
Air-flow carries the elastic granule secretly and the rigid particles do relative motion in confined conditions, described compound so as to be formed
Granule.
10. method according to claim 9, it is characterised in that the quality of the elastic granule and the rigid particles
Ratio is 100:(10-50), preferably 100:(20-30).
11. methods according to claim 9 or 10, it is characterised in that the system rotating speed for controlling the air-flow is
1500-3000rpm；It is preferred that the system rotating speed is 2000-2500rpm.
Application of 12. composite particles as described in any one in claim 1-8 in oil gas well cementing operation.
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| CN106565383B (en) | 2019-09-20 |
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