CN114525119A - Preparation method of inorganic fiber toughening agent for oil-gas well cementing cement slurry - Google Patents
Preparation method of inorganic fiber toughening agent for oil-gas well cementing cement slurry Download PDFInfo
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- CN114525119A CN114525119A CN202210156390.6A CN202210156390A CN114525119A CN 114525119 A CN114525119 A CN 114525119A CN 202210156390 A CN202210156390 A CN 202210156390A CN 114525119 A CN114525119 A CN 114525119A
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- 239000004568 cement Substances 0.000 title claims abstract description 90
- 239000002002 slurry Substances 0.000 title claims abstract description 42
- 239000012745 toughening agent Substances 0.000 title claims abstract description 41
- 239000012784 inorganic fiber Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000835 fiber Substances 0.000 claims abstract description 79
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000007788 roughening Methods 0.000 claims abstract description 8
- 238000001694 spray drying Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000003921 oil Substances 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 229920002748 Basalt fiber Polymers 0.000 claims description 15
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052599 brucite Inorganic materials 0.000 claims description 15
- 239000004917 carbon fiber Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 15
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 6
- 239000005543 nano-size silicon particle Substances 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 28
- 125000004122 cyclic group Chemical group 0.000 abstract description 7
- 230000004048 modification Effects 0.000 abstract description 6
- 238000012986 modification Methods 0.000 abstract description 6
- 238000007789 sealing Methods 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 2
- 238000005553 drilling Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000004575 stone Substances 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 239000002657 fibrous material Substances 0.000 description 7
- 239000003129 oil well Substances 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 230000008719 thickening Effects 0.000 description 6
- 230000009471 action Effects 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- IRLPACMLTUPBCL-KQYNXXCUSA-N 5'-adenylyl sulfate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OS(O)(=O)=O)[C@@H](O)[C@H]1O IRLPACMLTUPBCL-KQYNXXCUSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000008186 active pharmaceutical agent Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- -1 aldehyde ketone Chemical class 0.000 description 3
- 239000002518 antifoaming agent Substances 0.000 description 3
- 230000005465 channeling Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000013505 freshwater Substances 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 3
- 239000001095 magnesium carbonate Substances 0.000 description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000012744 reinforcing agent Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 239000012530 fluid Substances 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention provides a preparation method of an inorganic fiber toughening agent for oil and gas well cementing cement slurry, which relates to the technical field of unconventional oil and gas well drilling and completion and is prepared by the following steps: (1) a single fiber stirring-ultrasonic pretreatment process; (2) the mixing process of suspension-stirring of various fibers; (3) mechanical roughening process for the surface of various fibers; (4) fiber surface modification process; (5) a spray drying process; the inorganic fiber toughening agent for oil-gas well cementing cement slurry prepared by the invention can be well compatible with a cement slurry system, does not change the rheological property of the cement slurry, can effectively reduce the brittleness of the set cement, improve the mechanical flexibility of the set cement, enhance the cyclic load resistance of the set cement, and meet the sealing integrity of a cement ring in the production period of an oil-gas well.
Description
Technical Field
The invention belongs to the technical field of oil-gas drilling and completion engineering, and particularly relates to a preparation method of an inorganic fiber toughening agent for oil-gas well cementing cement slurry.
Background
Nowadays, unconventional oil and gas resources have taken an important position in the global energy structure. Horizontal well technology and large-scale staged hydraulic fracturing technology have become key technologies for shale gas yield increase. However, in staged hydraulic fracturing, the horizontal cement sheath will be subjected to cyclic loading caused by temperature and pressure changes in the wellbore. Therefore, the cement paste is required to have good elastic toughness and compressive strength, wherein the toughening agent plays a crucial role. The invention relates to a toughening channeling-preventing agent for cement and toughening cement (CN 104291733B) for shale gas horizontal well cementing, which are authorized in China, wherein styrene butadiene rubber and latex powder are compounded according to the mass ratio of 2:1, so that the elastic modulus of a set cement is reduced to 11.67GPa, the breaking strength is improved to 1.98MPa, and no fiber material is used; the invention 'a magnesium carbonate whisker flexibilizer (CN 105368411B) for reducing brittleness of oil and gas well set-stone' which is authorized in China uses magnesium carbonate whisker as a flexibilizer to greatly improve the breaking strength of the set-stone, but does not pay attention to the elastic modulus of the set-stone, and six-speed rotational viscosity data of cement paste shows that the thickening effect of the magnesium carbonate whisker is obvious. Said invention solves the problem of brittleness of cement stone to a certain extent, but does not relate to the property of cement stone resisting cyclic load.
Disclosure of Invention
The invention aims to provide a preparation method of an inorganic fiber toughening agent for oil-gas well cementing cement slurry, and the prepared toughening agent can be well compatible with cement slurry additives, does not change the basic performance of the cement slurry, improves the flexural strength and compressive strength of cement stone, reduces the elastic modulus, and ensures the mechanical integrity of a cement sheath under the action of cyclic load.
In order to achieve the purpose, the invention provides a preparation method of an inorganic fiber toughening agent for oil and gas well cementing cement slurry, which comprises the following steps:
respectively placing basalt fibers, carbon fibers, brucite fibers and silicon carbide fibers in high-speed stirrers filled with deionized water, wherein the amount of the corresponding fibers added in each high-speed stirrer is 5-15% of the mass of the deionized water;
carrying out secondary dispersion treatment on the fibers in the deionized water for 30 minutes by using ultrasonic waves;
filtering, washing and drying for later use;
(2) adding one or more of the pretreated basalt fiber, carbon fiber, brucite fiber and silicon carbide fiber into deionized water according to a preset proportion, stirring for 120 plus 240 minutes by using a constant-speed stirrer under the conditions of 2000 plus 4000 revolutions per minute, and carrying out mixing treatment;
filtering, washing with water, and drying;
(3) placing the composite fiber obtained in the step (2) in a grinding machine to improve the surface roughness of the fiber;
(4) transferring the fiber mixture subjected to roughening treatment in the step (3) into a warm water bath, adding a neutral nano silicon dioxide solution into deionized water, stirring for 20-30 minutes, then aging for 3-4 hours, and then filtering the fiber mixture;
(5) and (4) placing the fiber mixture modified by the nano silicon dioxide in the step (4) into spray drying equipment to obtain the inorganic fiber toughening agent for oil and gas well cementing.
In the scheme, the length of the inorganic fiber of the basalt fiber, the carbon fiber, the brucite fiber and the silicon carbide fiber is 0.5-3 mm.
In the scheme, in the step (1), the stirring is carried out for 15-30 minutes under the condition of more than 10000 revolutions per minute.
In the above scheme, the drying in step (5) is carried out at 120-150 ℃ for 120 minutes.
In the scheme, the step (3) is carried out for 5-8 minutes by using a mechanical grinding method.
Compared with the prior art, the preparation method of the inorganic fiber toughening agent for the oil-gas well cementing cement slurry provided by the invention has the following advantages and characteristics: the inorganic non-metal fiber material is used as a toughening agent, the surface of the fiber material is modified, hydrophilic groups are added, and the bonding strength between the fiber material and a cement paste hydration product is enhanced, so that the cement stone has good compressive strength and bending strength and lower elastic modulus, the mechanical damage of a cement ring under the action of alternating load is prevented and controlled, and the sealing integrity of the cement ring is ensured.
Drawings
FIG. 1 is an SEM schematic diagram of a toughening agent prepared by the preparation method of the inorganic fiber toughening agent for oil and gas well cementing cement slurry provided by the invention in set cement.
FIG. 2 is a schematic diagram of a thickening curve of a well cementation cement slurry system (1.88g/cm3, 90 ℃ 56MPa 50min) in the preparation method of the inorganic fiber toughening agent for the well cementation cement slurry of the oil and gas well provided by the invention.
FIG. 3 is a schematic diagram of a triaxial compression curve of a cement sample of a well cementing cement slurry system in the preparation method of the inorganic fiber toughening agent for well cementing cement slurry of an oil and gas well provided by the invention.
FIG. 4 is a schematic view of a circulation load resistance curve of a cement sample of a well cementation cement slurry system in the preparation method of the inorganic fiber toughening agent for the well cementation cement slurry of the oil and gas well provided by the invention.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
As shown in fig. 1; the invention provides a preparation method of an inorganic fiber toughening agent for oil-gas well cementing cement slurry, which comprises the following steps:
(1) single fiber 'stirring-ultrasonic' pretreatment process
Respectively placing basalt fibers, carbon fibers, brucite fibers and silicon carbide fibers in high-speed stirrers filled with deionized water, wherein the amount of the corresponding fibers added in each high-speed stirrer is 5-15% of the mass of the deionized water;
stirring for 15-30 minutes under the condition of more than 10000 revolutions per minute;
carrying out secondary dispersion treatment on the fibers in the deionized water for 30 minutes by using ultrasonic waves;
filtering, washing and drying for later use;
(2) suspension-stirring mixing process for multiple fibers
Adding one or more of the pretreated basalt fiber, carbon fiber, brucite fiber and silicon carbide fiber into deionized water according to a preset proportion, stirring for 120 plus 240 minutes by using a constant-speed stirrer under the conditions of 2000 plus 4000 revolutions per minute, and carrying out mixing treatment;
filtering, washing with water, and drying;
(3) mechanical roughening process for surfaces of various fibers
Placing the composite fiber obtained in the step (2) in a grinding machine, and treating for 5-8 minutes by using a mechanical grinding method to improve the surface roughness of the fiber;
(4) fiber surface modification process
Transferring the fiber mixture subjected to roughening treatment in the step (3) into a warm water bath, adding a neutral nano silicon dioxide solution into deionized water, stirring for 20-30 minutes, then aging for 3-4 hours, and then filtering the fiber mixture;
(5) spray drying process
And (4) placing the fiber mixture modified by the nano silicon dioxide in the step (4) into spray drying equipment, and drying at the temperature of 120-150 ℃ for 120 minutes to obtain the inorganic fiber toughening agent for oil and gas well cementing.
Wherein the inorganic fibers of the basalt fibers, the carbon fibers, the brucite fibers and the silicon carbide fibers have the length of 0.5-3 mm.
Example 1:
the preparation method of the inorganic fiber toughening agent for the oil-gas well cementing cement slurry comprises the following relevant process parameters:
(1) single fiber 'stirring-ultrasonic' pretreatment process
The mass ratio of the pretreated fiber to the deionized water is as follows: 5 percent.
The pretreatment rotating speed is as follows: 10000 rpm.
Stirring time: for 20 minutes.
Ultrasonic treatment time: for 30 minutes.
(2) Suspension-stirring mixing process for multiple fibers
The mass ratio of the basalt fibers, the carbon fibers, the brucite fibers and the silicon carbide fibers is 3:3:1: 1.
Stirring speed: 3000 rpm.
Stirring time: for 150 minutes.
(3) Mechanical roughening process for surfaces of various fibers
Grinding time: for 5 minutes.
(4) Fiber surface modification process
Water bath temperature: at 75 ℃.
Concentration of the nano-silica solution: 30 percent of mass fraction.
Stirring speed: 2000 rpm.
Stirring time: for 25 minutes.
Aging time: for 3 hours.
(5) Spray drying process
Drying temperature: 120 ℃ is adopted.
Drying time: 120 minutes.
(6) Preparation of cement paste
Adding the prepared inorganic fiber toughening agent into oil well cement to prepare toughening cement slurry for oil and gas wells (all components are in parts by weight): 100 parts of G-grade oil well cement, 46 parts of fresh water, 2 parts of AMPS polymer fluid loss additive, 0.5 part of micro-silicon reinforcing agent, 1 part of magnesium oxide expanding agent, 0-1.25 parts of inorganic fiber toughening agent, 1.2 parts of elastic colloidal particle gas channeling preventing agent, 0.3 part of aldehyde ketone polymer dispersing agent, 0.04 part of polycarboxylic acid retarder and 0.02 part of organic silicon defoaming agent. The inorganic toughening agent is a modified mixed fiber with the mass ratio of basalt fiber, carbon fiber, brucite fiber and silicon carbide fiber being 3:3:1: 1. And (3) uniformly mixing and stirring the raw materials according to the API 10B standard to obtain the toughening cement slurry for the oil-gas well. The thickening time test conditions were: 90 ℃ X56 MPa X50 m 55. The strength maintenance conditions of the set cement are as follows: 45 ℃ at 90 ℃ under normal pressure for 48 hours. The cement paste correlation properties were determined and the results are shown in tables 1 and 2. The microscopic morphology of the fibers in the set cement is shown in FIG. 1.
Table 1 associated properties of the toughened cement slurry for oil and gas wells prepared in example 1
Table 2 mechanical strength properties of the toughened cement slurry for oil and gas wells prepared in example 1
Example 2:
the preparation method of the inorganic fiber toughening agent for the oil-gas well cementing cement slurry comprises the following relevant process parameters:
(1) single fiber 'stirring-ultrasonic' pretreatment process
The mass ratio of the pretreated fiber to the deionized water is as follows: 10 percent.
The pretreatment rotating speed is as follows: 12000 rpm.
Stirring time: for 25 minutes.
Ultrasonic treatment time: for 30 minutes.
(2) Suspension-stirring mixing process for multiple fibers
The mass ratio of the basalt fibers, the carbon fibers, the brucite fibers and the silicon carbide fibers is 2:4:1: 1.
Stirring speed: 3000 rpm.
Stirring time: 180 minutes.
(3) Mechanical roughening process for surfaces of various fibers
Grinding time: for 6 minutes.
(4) Fiber surface modification process
Water bath temperature: at 75 ℃.
Concentration of the nano-silica solution: 35 percent of mass fraction.
Stirring speed: 2200 rpm.
Stirring time: for 30 minutes.
Aging time: for 4 hours.
(5) Spray drying process
Drying temperature: 135 ℃ is adopted.
Drying time: 120 minutes.
(6) Preparation of cement paste
Adding the prepared inorganic fiber toughening agent into oil well cement to prepare toughening cement slurry for oil and gas wells (all components are in parts by weight): 100 parts of G-grade oil well cement, 46 parts of fresh water, 2.5 parts of AMPS polymer fluid loss additive, 0.5 part of micro-silicon reinforcing agent, 0.5 part of lattice expanding agent, 0-1.25 parts of inorganic fiber toughening agent, 1.2 parts of elastic colloidal particle gas channeling preventing agent, 0.3 part of aldehyde ketone polymer dispersing agent, 0.04 part of polycarboxylic acid retarder and 0.02 part of organic silicon defoaming agent. The inorganic toughening agent is a mixed fiber with the mass ratio of basalt fiber, carbon fiber, brucite fiber and silicon carbide fiber being 2:4:1: 1. And (3) uniformly mixing and stirring the raw materials according to the API 10B standard to obtain the toughening cement slurry for the oil-gas well. The thickening time test conditions were: 90 ℃ X56 MPa X50 m 55. The strength maintenance conditions of the set cement are as follows: 45 ℃ at 90 ℃ under normal pressure for 48 hours. The cement paste correlation properties were determined and the results are shown in tables 3 and 4. The thickening curve of the 1% toughener with cement slurry added is shown in figure 2.
Table 3 associated properties of the toughened cement slurry for oil and gas wells prepared in example 2
Table 4 mechanical strength properties of the toughened cement slurry for oil and gas wells prepared in example 2
Example 3:
the preparation method of the inorganic fiber toughening agent for the oil-gas well cementing cement slurry comprises the following relevant process parameters:
(1) single fiber 'stirring-ultrasonic' pretreatment process
The mass ratio of the pretreated fiber to the deionized water is as follows: 15 percent.
The pretreatment rotating speed is as follows: 12000 rpm.
Stirring time: for 20 minutes.
Ultrasonic treatment time: for 30 minutes.
(2) Suspension-stirring mixing process for multiple fibers
The mass ratio of the basalt fibers, the carbon fibers, the brucite fibers and the silicon carbide fibers is 4:2:1: 1.
Stirring speed: 3500 rpm.
Stirring time: for 240 minutes.
(3) Mechanical roughening process for surfaces of various fibers
Grinding time: for 8 minutes.
(4) Fiber surface modification process
Water bath temperature: at 75 ℃.
Concentration of the nano-silica solution: 40 percent of mass fraction.
Stirring speed: 2000 rpm.
Stirring time: for 30 minutes.
Aging time: for 4 hours.
(5) Spray drying process
Drying temperature: at 150 ℃.
Drying time: 120 minutes.
(6) Preparation of cement paste
Adding the prepared inorganic fiber toughening agent into oil well cement to prepare toughening cement slurry for oil and gas wells (all components are in parts by weight): 100 parts of G-grade oil well cement, 46 parts of fresh water, 2 parts of AMPS polymer fluid loss additive, 0.5 part of micro-silicon reinforcing agent, 1 part of magnesium oxide expanding agent, 0-1.25 parts of inorganic fiber toughening agent, 1.2 parts of elastic colloidal particle gas channeling preventing agent, 0.3 part of aldehyde ketone polymer dispersing agent, 0.04 part of polycarboxylic acid retarder and 0.02 part of organic silicon defoaming agent. The inorganic toughening agent is a mixed fiber with the mass ratio of basalt fiber, carbon fiber, brucite fiber and silicon carbide fiber being 4:2:1: 1. And (3) uniformly mixing and stirring the raw materials according to the API 10B standard to obtain the toughening cement slurry for the oil-gas well. The thickening time test conditions were: 90 ℃ X56 MPa X50 m 55. The strength maintenance conditions of the set cement are as follows: 45 ℃ at 90 ℃ under normal pressure for 48 hours. The cement paste correlation properties were measured and the results are shown in tables 5 and 6. The results of the triaxial compression strength test of the set cement with 1% of the toughening agent are shown in figure 3, and the results of the cyclic load resistance test are shown in figure 4.
The set cement maintained mechanical integrity under 70 cyclic loads.
TABLE 5 associated Properties of the toughened cement slurry for oil and gas wells prepared in example 3
Table 6 mechanical strength properties of the toughened cement slurry for oil and gas wells prepared in example 3
The inorganic fibers are inert in the fluid state of the cement paste, so that the hydration reaction speed of the cement paste cannot be influenced before the cement paste is thickened. If the short fibers with the diameter of micron order are adopted, the micro-cracks can be well prevented from developing, the bridging effect is achieved, the cracks are prevented from further extending, the mechanical property of the set cement under the action of cyclic load is improved, the radial cracks are prevented from developing, and the sealing integrity of the cement sheath is improved.
The invention provides a preparation method of an inorganic fiber toughening agent for oil-gas well cementing cement slurry, which has the following advantages compared with the prior art: the inorganic non-metal fiber material is used as a toughening agent, the surface of the fiber material is modified, hydrophilic groups are added, and the bonding strength between the fiber material and a cement paste hydration product is enhanced, so that the cement stone has good compressive strength and bending strength and lower elastic modulus, the mechanical damage of a cement ring under the action of alternating load is prevented and controlled, and the sealing integrity of the cement ring is ensured.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. A preparation method of an inorganic fiber toughening agent for well cementing cement slurry of an oil and gas well is characterized by comprising the following steps:
(1) respectively placing basalt fibers, carbon fibers, brucite fibers and silicon carbide fibers in high-speed stirrers filled with deionized water, wherein the amount of the corresponding fibers added in each high-speed stirrer is 5-15% of the mass of the deionized water;
carrying out secondary dispersion treatment on the fibers in the deionized water for 30 minutes by using ultrasonic waves;
filtering, washing and drying for later use;
(2) adding one or more of the pretreated basalt fiber, carbon fiber, brucite fiber and silicon carbide fiber into deionized water according to a preset proportion, stirring for 120 plus 240 minutes by using a constant-speed stirrer under the conditions of 2000 plus 4000 revolutions per minute, and carrying out mixing treatment;
filtering, washing with water, and drying;
(3) placing the composite fiber obtained in the step (2) in a grinding machine to improve the surface roughness of the fiber;
(4) transferring the fiber mixture subjected to roughening treatment in the step (3) into a warm water bath, adding a neutral nano silicon dioxide solution into deionized water, stirring for 20-30 minutes, then aging for 3-4 hours, and then filtering the fiber mixture;
(5) and (5) placing the fiber mixture modified by the nano silicon dioxide in the step (4) into spray drying equipment to obtain the inorganic fiber toughening agent for oil and gas well cementing.
2. The preparation method of the inorganic fiber toughening agent for the oil-gas well cementing cement slurry, according to claim 1, is characterized in that the inorganic fiber length of the basalt fiber, the carbon fiber, the brucite fiber and the silicon carbide fiber is 0.5-3 mm.
3. The preparation method of the inorganic fiber toughening agent for the oil-gas well cementing cement slurry according to claim 1, wherein the stirring is carried out for 15-30 minutes under the condition of more than 10000 revolutions per minute in the step (1).
4. The method for preparing the inorganic fiber toughening agent for the oil-gas well cementing cement slurry as claimed in claim 1, wherein the drying in the step (5) is carried out at the temperature of 120-150 ℃ for 120 minutes.
5. The preparation method of the inorganic fiber toughening agent for the oil-gas well cementing cement slurry according to claim 1, wherein the step (3) is carried out for 5-8 minutes by using a mechanical grinding method.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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