CN106565383B - A kind of composite particles, preparation method and application - Google Patents
A kind of composite particles, preparation method and application Download PDFInfo
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Abstract
The present invention relates to oil gas well cementing operation technical field, in particular to a kind of composite particles, preparation method and application.The composite particles are made of the kernel of elastic granule and the shell for the rigid particles for being coated on the kernel outer surface.The preparation method of composite particles comprising following steps: the elastic granule is carried secretly using air-flow and the rigid particles do relative motion, to form the composite particles.Composite particles of the invention have the characteristics that temperature tolerance is high, while improving the acidproof alkali ability of elastic granule；Its stability is good；Can be good with cement slurry compatibility, the increase consistency phenomenon of no floating and maintenance processes；And it can be substantially reduced Behavior of Hardened Cement Paste elasticity modulus, increase the deformability of Behavior of Hardened Cement Paste；In addition, composite particles of the invention are spherical shape, be conducive to the mobility for increasing cement slurry.
Description
Technical field
The present invention relates to oil gas well cementing operation technical field, in particular to a kind of composite particles, preparation method and application.
Background technique
As gas well annular space phenomenon with pressure is more and more common, the sealing quality and durability of cement sheath are increasingly by industry
Interior attention.But traditional cements stone is a kind of fragile material, is easy to appear and splits in oil well long-term production or operation process cement sheath
Line or microannulus, lead to wellheadpressure.The application of especially current shale oil gas, fine and close oil/gas well staged fracturing technology, it is right
Behavior of Hardened Cement Paste elastic deformation energy force request is higher, it is desirable that Behavior of Hardened Cement Paste can couple casing deformation.Therefore in order to effectively improve Behavior of Hardened Cement Paste
Long term seal ability, need to be effectively improved the mechanical property of Behavior of Hardened Cement Paste, improve the deformability of Behavior of Hardened Cement Paste, cement is effectively reduced
The elasticity modulus of stone, and guarantee the enough intensity of Behavior of Hardened Cement Paste.The currently used material for improving Behavior of Hardened Cement Paste elastic property mainly has:
The substances such as styrene-butadiene latex latex, styrene-acrylic latex, rubber grain and organic resin class, but latex and organic resin substance are because of price
High and limit being widely used for they, rubber grain and resin material are affected due to temperature resistance ability difference and the defect of itself
Its application in oil gas well cementing operation.Wherein rubber grain becomes many elastic cements slurries due to from a wealth of sources, cheap
The preferred material of system, but its surface hydrophobicity, and easily floating and temperature tolerance are poor, its application is caused to receive biggish limit
System.
It is therefore desirable to develop a kind of novel elastic material based on core-shell structure, enable the cement slurry to be formed
Behavior of Hardened Cement Paste elasticity modulus is reduced, Behavior of Hardened Cement Paste brittleness is reduced, increases Behavior of Hardened Cement Paste deformability, and rationally reduce cost.
Summary 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
The rigid particles as shell of the kernel outer surface form.
In addition, the possibility for carrying out physical modification to elastic granule is realized by mechanical coating technology, by elasticity
The material of grain surface physics cladding rigidity such as SILICA FUME, flyash, especially has the hydraulicity and/or alkali-activated carbonatite volcanic ash
The material of matter realizes non-porous cladding, can be effectively improved the water-wet behavior of inner nuclear material, further improves elastic granule and cement
Cementation between stone, improves the temperature resistant capability and stability of elastic granule, while can improve Mechanical Behavior of Hardened Cement Paste, effectively drops
Low Behavior of Hardened Cement Paste elasticity modulus increases Behavior of Hardened Cement Paste strain rate.Therefore, using the composite particles of core-shell structure of the invention, Neng Gouyou
Effect ground meets high temperature well cementing requirements.
It should be pointed out that the kernel of composite particles of the invention only has an elastic granule, and the number of the particle of shell
Amount is far above one, but to reach the quantity of non-porous cladding and/or continuous cladding elastic granule.Wherein non-porous cladding refers to packet
After being covered with the non-porous experimental test of the embodiment 7 of the composite particles of shell of the invention through the invention, fail to find diesel oil group
The cladding divided；It is continuous to coat the non-porous examination for referring to the embodiment 7 of the composite particles for being coated with shell of the invention through the invention
After test 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 by shell, prevent core water-swellable, while can reduce the ratio of mud in cement slurry, improve water
Mudstone mechanical property.
When elastic material is in reasonable dosage proportional region, can guarantee Behavior of Hardened Cement Paste, elastic deformation amount exists under compression
Between 0.1-0.5%, it at this moment can be effectively prevent the destruction of the factors to Behavior of Hardened Cement Paste such as staged fracturing and thermal expansion, to guarantee solid
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, have at one
In body embodiment, the ratio of the thickness of the average grain 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 the latex powder that elasticity modulus is less than 1.5GPa, preferably institute
Stating elastic granule includes acrylonitrile-butadiene rubber powder and/or styrene butadiene rubber powder.
In a specific embodiment, the average grain diameter of the elastic granule is 100-180 microns, partial size d50=110-
165 microns；It is preferred that 120-140 microns of the average grain diameter of the elastic granule, partial size d50=125-145 microns.
In a specific embodiment, the shore hardness of the elastic granule is 60-100, and in mass, phosphorus content is less than
Or it is 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,
It is preferred that the material includes at least one of silicon ash, flyash and metakaolin.
In a specific embodiment, the flat average grain diameter of the rigid particles is 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 described above comprising following steps:
Air-flow carries the elastic granule secretly and the rigid particles do relative motion in confined conditions, thus described in being formed
Composite particles.
In a specific embodiment, the mass ratio of the elastic granule and the rigid particles is 100:(10-50),
Preferably 100:(20-30).
In a specific embodiment, the system revolving speed for controlling the air-flow is 1500-3000rpm；It is preferred that the system
Revolving speed is 2000-2500rpm.
In a specific embodiment, the elastic granule is carried secretly using air-flow and the rigid particles do relative motion
Time is 20-30 minutes.
The three of the present invention provide a kind of application of composite particles as described above in oil gas well cementing operation.
Compared with prior art, the beneficial effects of the present invention are:
(1) composite particles temperature tolerance of the invention is high, improves the acidproof alkali ability of elastic granule；
(2) composite particles stability of the invention is good；
(3) composite particles of the invention are good with cement slurry compatibility, and in cement slurry maintenance processes, composite particles do not occur
Hydro-planing, while there is not thickening behavior in cement slurry, so that cement slurry property be made to be greatly improved；
(4) composite particles of the invention can be substantially reduced Behavior of Hardened Cement Paste elasticity modulus, increase the deformability of Behavior of Hardened Cement Paste；
(5) composite particles of the invention are spherical shape, are conducive to the mobility for increasing cement slurry.
Detailed description of the invention
The structural schematic diagram of core-shell structure composite particles is shown in Fig. 1, and wherein inner core is elastic granule, and outside is rigid
Property particles coat kernel formed shell.
The forming process schematic diagram of composite particles is shown in Fig. 2, can carry out ball to elastic material first as needed
Shape, then with spheroidization treated rigid particles, such as silicon ash is after mixing, impacts composite algorithm shape using dry type later
At the particle of continuous and/or non-porous cladding.
PCS-1 system flow chart is shown in Fig. 3；Wherein, 1 is loading hopper, and 2 be sample injector, and 3 be processing system, and 4 be cold
But system, 5 be control system.
Microstructure of the composite particles under scanning electron microscope is shown in Fig. 4, as can be seen from the figure the ball of composite particles
Shape degree is very high.
Specific embodiment
In the present invention, using compound particle hybrid system (Tsinghua University, PCS-1), composite algorithm, benefit are impacted using dry type
Carried under one's arms particle with the high-speed flow that equipment rotation generates and done high speed relative motion, by impact make elastic granule and rigid particles with
Van der Waals force and electrostatic force generation are compound, form the elastic particle of core-shell structure.By adjusting system revolving speed in 1500-
3000r/min, control system put into raw material, open row's powder switch by control cabinet again after running 20-30min, arrange powder 15-
20min forms final products.
In the present invention, elasticity modulus, accepted standard GB/T are measured using instrument ToniPrax (Germany)
23561.8.Poisson's ratio is measured using instrument ToniPrax (Germany), accepted standard is GB/T 50081-2002).Using beauty
State instrument Instron2450-200 measures compression strength and tensile strength, and accepted standard is GB/T 50081-2002, wherein
Compression strength and tensile strength use same device measuring).
Embodiment 1
By 100 parts by weight, average grain diameter is 120 microns, partial size d50=123 microns, elasticity modulus 0.6GPa, shore is hard
Degree is 70, and (average grain diameter is 1.45 micro- in the silicon ash after 30 parts of the nitrile rubber particle addition ball-types that phosphorus content is 0.5wt%
Rice, partial size d50It=1.40 microns, stirs evenly, and adjusts compound particle hybrid system (Tsinghua University, PCS-1) revolving speed 2500
Rev/min, it controls charging rate 5kg/ minutes, coats the time 30 minutes, collecting average grain diameter is 180 microns, partial size d50=175
The composite particles of micron.
Embodiment 2
By 100 parts by weight, average grain diameter is 180 microns, partial size d50=165 microns, elasticity modulus 0.8GPa, shore is hard
Degree is 85, and 20 parts by weight after ball-type are added in the butadiene-styrene rubber particle that phosphorus content is 0.5%, and average grain diameter is 5.6 microns, grain
Diameter d50=5.4 microns, phosphorus content is controlled to stir evenly, and adjust 2000 revs/min of PCS-1 revolving speed in 0.5% flyash
It charging rate 5kg/ minutes processed, coats the time 20 minutes, collects 250 microns of product average grain diameter, partial size d50=240 microns answer
Close particle.
Embodiment 3
By 100 parts by weight, average grain diameter is 120 microns, partial size d50=125 microns, elasticity modulus 0.5GPa, shore is hard
Degree is 60, and 10 parts by weight after ball-type are added in the butadiene-styrene rubber particle that phosphorus content is 0.5%, and average grain diameter is 1.6 microns, grain
Diameter d50It in=1.2 microns of metakaolin, stirs evenly, and adjusts 1000 revs/min of PCS-1 revolving speed, control charging rate
It 5kg/ minutes, coats the time 20 minutes, collects 215 microns of product average grain diameter, partial size d50=220 microns of composite particles.
Embodiment 4
By 100 parts by weight, average grain diameter is 100 microns, partial size d50=110 microns, elasticity modulus 1GPa, shore hardness
It is 90,50 parts by weight after ball-type are added in the butadiene-styrene rubber particle that phosphorus content is 0.5%, and average grain diameter is 1.0 microns, partial size
d50=1.35 microns, phosphorus content controls to stir evenly, and adjust 3000 revs/min of PCS-1 revolving speed in 0.5% flyash
It charging rate 5kg/ minutes, coats the time 20 minutes, collects 200 microns of product average grain diameter, partial size d50=189 microns compound
Particle.
Embodiment 5
By 100 parts by weight, average grain diameter is 120 microns, and particle diameter distribution index is d50=125 microns, elasticity modulus is
25 parts by weight after ball-type, average grain is added in 1.5GPa, shore hardness 100, the butadiene-styrene rubber particle that phosphorus content is 0.5%
Diameter is 1.3 microns, partial size d50=1.35 microns, phosphorus content be 0.5% flyash in, stir evenly, and adjust PCS-1 revolving speed
It 2000 revs/min, controls charging rate 5kg/ minutes, coats the time 20 minutes, collect 233 microns of product average grain diameter, partial size
d50=240 microns of composite particles.
Embodiment 6
By 100 parts by weight, average grain diameter is 141 microns, partial size d50=145 microns, elasticity modulus 0.7GPa, shore is hard
Degree is 80, and 40 parts by weight after ball-type are added in the butadiene-styrene rubber particle that phosphorus content is 1.0%, and average grain diameter is 10.0 microns,
Partial size d50=8.5 microns, phosphorus content be 0.5% flyash in, stir evenly, and adjust 2000 revs/min of PCS-1 revolving speed,
Control charging rate 5kg/ minutes coats the time 20 minutes, collects 215 microns of product average grain diameter, partial size d50=210 microns
Composite particles.
Embodiment 7
30 sample of composite particles grab sample that will be prepared in embodiment 1, divides 3 groups, every group of 10 samples impregnate diesel oil respectively
In 24 hours, room temperature is air-dried 2 hours using air-dry machine, destroy core-shell structure, take core carry out spectrofluorimetry, first group 9
9 sample, second group of 10 sample, third group samples, do not find diesel component, illustrate to realize 90% or more non-porous cladding.
Also, other embodiments also play similar effect.
Comparative example 1
For the improvement for comparing addition composite particles with being not added with compound particle Mechanical Behavior of Hardened Cement Paste, make first
Ordinary water mudstone test sample, that is, be not added with compound particle, using 100 parts of cement (good G grades of China, Dezhou continental shelf company), drop filter
It loses 5 parts of agent (DZJ-Y, Dezhou continental shelf company), 1.2 parts of dispersing agent (DZS, Dezhou continental shelf company), retarder (DZH-2, moral
State continental shelf company) 1.5 parts, 40 parts of water, 0.2 part of defoaming agent (DZX, Dezhou continental shelf company) configures the water of traditional performance
Mud system, density 1.9g/cm3, conserve 72 hours under 80 DEG C and 20MPa environment, measurement elasticity modulus, Poisson's ratio, resistance to compression
Intensity and tensile strength.It the results are shown in Table 1.
Embodiment 8
Using 100 parts of cement (good G grades of China, Dezhou continental shelf company), fluid loss additive (DZJ-Y, Dezhou continental shelf company) 5
Part, 1.2 parts of dispersing agent (DZS, Dezhou continental shelf company), 1.5 parts of retarder (DZH-2, Dezhou continental shelf company), 40 parts of water,
6 parts of the composite particles prepared in embodiment 1- embodiment 7,0.2 part of defoaming agent, configuring density is 1.9g/cm3, 80 DEG C and
It is conserved 72 hours under 20MPa environment, measurement elasticity modulus, Poisson's ratio, compression strength and tensile strength.It the results are shown in Table 1.
Compared with comparative example 1, Behavior of Hardened Cement Paste elasticity modulus obviously drops after adding the composite particles in embodiment 1- embodiment 7
Low, deformability is most strong.
The present embodiment the results show that composite particles can effectively improve the temperature tolerance of original elastic granule, stability with
And it is cementing with cement, while Behavior of Hardened Cement Paste elasticity modulus is greatly reduced.The effective hard crisp characteristic for improving Behavior of Hardened Cement Paste, improves cement
The durability of stone is conducive to the long-term sealing ability for improving gas well Behavior of Hardened Cement Paste, and meets the segmentation of the unconventional oil and gas such as shale gas
Demand of the pressure break to Behavior of Hardened Cement Paste.
Table 1
| Embodiment | Behavior of Hardened Cement Paste elasticity modulus | Poisson's ratio | Compression 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 (19)
1. a kind of composite particles, the composite particles are by the elastic granule as kernel and are coated on the work of the kernel outer surface
It is formed for the rigid particles of shell, the rigid particles are the material with the hydraulicity and/or alkali-activated carbonatite volcano grey matter.
2. composite particles according to claim 1, which is characterized in that the shell is coated in described in non-porous form
The outer layer of core.
3. composite particles according to claim 1 or 2, which is characterized in that the average grain diameter of the kernel and the shell
Thickness ratio be 2:1-8:1.
4. composite particles according to claim 3, which is characterized in that the thickness of the average grain diameter of the kernel and the shell
The ratio of degree is 2:1-5:1.
5. composite particles according to claim 1 or 2, which is characterized in that the elastic granule includes that elasticity modulus is less than
The latex powder of 1GPa.
6. composite particles according to claim 5, which is characterized in that the elastic granule include acrylonitrile-butadiene rubber powder and/or
Styrene butadiene rubber powder.
7. composite particles according to claim 1 or 2, which is characterized in that the average grain diameter of the elastic granule is 100-
180 microns, partial size d50=110-165 microns.
8. composite particles according to claim 7, which is characterized in that the average grain diameter 120-140 of the elastic granule is micro-
Rice, partial size d50=125-145 microns.
9. composite particles according to claim 1 or 2, which is characterized in that the shore hardness of the elastic granule is 60-
100, in mass, phosphorus content is less than or equal to 1.0%.
10. composite particles according to claim 9, which is characterized in that the shore hardness of the elastic granule is 70-85,
In mass, phosphorus content is less than or equal to 0.5%.
11. composite particles according to claim 1 or 2, which is characterized in that the rigid particles include silicon ash, flyash
At least one of with metakaolin.
12. composite particles according to claim 1 or 2, which is characterized in that the average grain diameter of the rigid particles is 1.0-
10.0 microns, particle diameter distribution d50=1.35-8.5 microns.
13. composite particles according to claim 12, which is characterized in that the average grain diameter of the rigid particles is 1.3-
5.6 microns, particle diameter distribution d50=1.35-5.4 microns.
14. a kind of method for preparing the composite particles as described in any one of claim 1-13 comprising following steps:
Air-flow carries the elastic granule secretly and the rigid particles do relative motion in confined conditions, to be formed described compound
Particle.
15. according to the method for claim 14, which is characterized in that the mass ratio of the elastic granule and the rigid particles
Example is 100:(10-50).
16. according to the method for claim 15, which is characterized in that the mass ratio of the elastic granule and the rigid particles
Example is 100:(20-30).
17. the method according to any one of right 14-16, which is characterized in that the system revolving speed for controlling the air-flow is
1500-3000rpm。
18. according to method described in right 17, which is characterized in that the system revolving speed for controlling the air-flow is 2000-2500rpm.
19. application of the composite particles as described in any one of claim 1-13 in oil gas well cementing operation.
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