CN113121128B - High-strength toughened cementing material and preparation method and application thereof - Google Patents
High-strength toughened cementing material and preparation method and application thereof Download PDFInfo
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- CN113121128B CN113121128B CN202110623702.5A CN202110623702A CN113121128B CN 113121128 B CN113121128 B CN 113121128B CN 202110623702 A CN202110623702 A CN 202110623702A CN 113121128 B CN113121128 B CN 113121128B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B7/14—Cements containing slag
- C04B7/147—Metallurgical slag
- C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
- C04B7/17—Mixtures thereof with other inorganic cementitious materials or other activators with calcium oxide containing activators
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
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- C04B7/38—Preparing or treating the raw materials individually or as batches, e.g. mixing with fuel
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Abstract
The invention discloses a high-strength toughened cementing material, a preparation method and application thereof, and relates to the field of hydraulic cementing materials. The high-strength toughened cementing material consists of 100 parts of limestone, 10 to 15 parts of red clay, 1~8 parts of baddeleyite, 2 to 10 parts of zircon, 1~5 parts of siliceous correction raw materials, 1~5 parts of basalt tailings, 2~6 parts of sulfuric acid residues, 2~5 parts of copper slag and 3~5 parts of dihydrate gypsum; the mineral content in the high-strength toughened cementing material comprises C 3 S、C 2 S、C 3 A、C 4 AF and ZrSiO 4 Wherein, C is more than or equal to 50 percent 3 S≤65%，15%≤C 2 S≤30%，1.0%≤C 3 A≤2.5%，14%≤C 4 AF≤18%，1%≤ZrSiO 4 Less than or equal to 10 percent; the specific surface area of the high-strength toughened well cementing material is 300 to 360 m 2 (iv) kg; according to the invention, the reasonable design of the mineral components and the theory of particle tight packing are combined, and on the premise of ensuring the high toughness of the low elastic modulus, the hardened body of the cementing material is endowed with early strength development, so that the defects of poor mechanical property, slow development of early strength and the like of the existing cementing material are overcome.
Description
Technical Field
The invention relates to the field of hydraulic cementing materials, in particular to a high-strength toughened well cementation cementing material as well as a preparation method and application thereof.
Background
Due to the brittleness characteristic of ordinary portland cement, the cement stone has generally poor tensile, shear and impact resistance, and during well cementation construction, a cement sheath can be subjected to large impact, vibration and mechanical deformation in the perforation and acid fracturing production increasing processes of a target layer, which can cause the cement sheath to crack and plastically deform, so that the packing capability of the cement sheath is lost. Due to the advantages of low Young modulus, high Poisson ratio, strong impact resistance and the like, the elastic and tough cement is widely applied to high-temperature and high-pressure ultra-deep gas wells in Xinjiang area, shale gas wells in southwest area and special working condition wells (such as gas storage circulating injection and production and the like).
At present, the research on elastic and tough cement slurry systems is more at home and abroad, the mechanical property of the set cement is mainly improved by two modes of 'endogenous type' and 'exogenous type', the exogenous type mainly improves the mechanical property of the set cement by adding elastic and tough materials into cement ash (for example: ding Zhiwei. A low-temperature high-toughness cement slurry and a preparation method and application thereof: CN 106986584A, jin Jianzhou. An expansion toughness well cementation cement slurry and a preparation method thereof: CN 104371678A, shi Zhong south: CN 107699216A and the like for a gas storage well), and the elastic and tough materials mainly comprise four types, namely: the material is characterized by comprising four materials, namely fiber, rubber particles, latex and resin, wherein each material has respective performance advantages, but the material cost is generally high, the temperature resistance is difficult to guarantee, the construction and debugging are complex, and the like, so that the material is not beneficial to field application.
Therefore, the research on the elastic and flexible cement slurry system tends to improve the flexibility and mechanical deformation capability of the set cement in an endogenous mode so as to further realize cost reduction and efficiency improvement, the endogenous mode mainly starts from a cement production link, changes the content of mineral components in the cement and utilizes the particle tight packing principle to achieve the purposes of reinforcing and toughening the set cement, and further highlights the commercial development value of the endogenous high-strength toughened well cementation cementing material.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention provides a high-strength toughened well cementing material, aims to solve the problems of poor mechanical property, slow development of early strength and the like of the existing cementing material, and endows a hardened body of the cementing material with early strength development by reasonable design of mineral components in the high-strength toughened well cementing material and combining with a particle tight packing theory on the premise of ensuring the high toughness of a low elastic modulus so as to make up the defects of poor mechanical property, slow development of early strength and the like of the existing cementing material.
In order to solve the problems in the prior art, the invention is realized by the following technical scheme:
a high-strength toughened cementing material comprises the following components in parts by weight:
100 parts of limestone, 10-15 parts of red clay, 3245 parts of baddeleyite, 3245 parts of zxft, 2-10 parts of zircon, 3732 parts of siliceous correction raw material, 3963 parts of basalt tailings, 3963 parts of sulfuric acid residue, 4325 parts of zxft, 3536 parts of copper slag and 3926 parts of dihydrate gypsum; the mineral content in the high-strength toughened cementing material comprises C 3 S、C 2 S、C 3 A、C 4 AF and ZrSiO 4 Wherein, C is more than or equal to 50 percent 3 S≤65%，15%≤C 2 S≤30%，1.0%≤C 3 A≤2.5%，14%≤C 4 AF≤18%，1%≤ZrSiO 4 Less than or equal to 10 percent; the specific surface area of the high-strength toughened well cementing material is 300 to 360 m 2 Per kg; in the high-strength toughened cementing material, the chemical component requirements are as follows: zrO 2% or less 2 Less than or equal to 8 percent and alkali content (Na) 2 O+0.658K 2 O）≤0.75%，SO 3 Less than or equal to 3.0 percent, less than or equal to 3.0 percent of Loss and less than or equal to 0.75 percent of insoluble substances.
The limestone component content requirement is as follows: caO is more than or equal to 50 percent, al 2 O 3 ≤1.0%，MgO＜2.5%。
The content of the red clay components is required to be: siO 2 2 ≥60%，Al 2 O 3 ≤12%。
The content of the baddeleyite components is required to be as follows: zrO (ZrO) 2 ≥90%。
ZrSiO in the zirconite 4 Is at least 95% pure.
The iron raw material comprises the following components in percentage by weight: fe 2 O 3 ≥60%。
The silicon correction raw material has the following component content requirements: siO 2 2 ≥80%。
The invention also provides a preparation method of the high-strength toughened well cementation cementing material, which comprises the following steps:
a raw material crushing step: respectively crushing limestone, red clay, baddeleyite, zirconite, a siliceous correction raw material, basalt tailings, sulfuric acid slag and copper slag by using an impact crusher, wherein the crushing ratio is controlled to be 50-60;
pre-homogenization treatment: conveying the crushed raw materials in the raw material crushing step to a pre-homogenizing warehouse for pre-homogenizing treatment;
the material preparation step: conveying the raw materials subjected to pre-homogenization treatment to a batching station, and proportioning according to the mixing ratio of 100 parts of limestone, 10-15 parts of red clay, 1~8 parts of baddeleyite, 2-10 parts of zircon, 1~5 parts of siliceous correction raw material, 1~5 parts of basalt tailings, 2~6 parts of sulfuric acid slag and 2~5 parts of copper slag;
grinding: conveying the mixed materials after proportioning into a ball mill, and grinding into cement raw materials, wherein the grinding ratio is controlled within 300-1000;
and (3) homogenization treatment: inputting the ground cement raw materials into a continuous cement raw material homogenizing warehouse to uniformly mix the cement raw materials;
and (3) calcining: feeding the uniformly mixed cement raw material from the uppermost stage preheater at the tail part of the rotary kiln, carrying out heat exchange with waste hot gas from the rotary kiln in the process of passing through C1-C4 preheaters, preheating, then feeding into a decomposing furnace, calcining until most of carbonate is decomposed, feeding into the rotary kiln through the last stage preheater, and calcining at high temperature in the rotary kiln to obtain cement clinker; the calcination temperature is controlled to be 1300-1500 ℃; after the calcined cement clinker is output to the rotary kiln, the cement clinker is rapidly cooled by a grate cooler to obtain the cement clinker;
and (3) finished product preparation: sending the prepared cement clinker and the crushed dihydrate gypsum into a batching station, proportioning according to the mixing ratio of 100 parts of the cement clinker and 3~5 parts of the dihydrate gypsum, conveying the materials into a ball mill after batching, grinding the materials into a cement finished product, and controlling the specific surface area within 300 to360 m 2 And/kg, finally storing the obtained cement finished product for a period of time and homogenizing to obtain the high-strength toughened well cementation cementing material.
The invention also provides the application of the high-strength toughened well cementation cementing material in an oil well cement slurry system.
The application of the high-strength toughened well cementation cementing material in an oil well cement slurry system is to apply the high-strength toughened well cementation cementing material to oil well cement slurry, wherein the oil well cement slurry comprises the following components in parts by weight:
100 parts of high-strength toughened well cementation cementing material, 0.5 to 4 parts of fluid loss additive, 0.3 to 4 parts of retarder, 0.1 to 2 parts of defoamer and 40 to 46 parts of distilled water.
The fluid loss agent is HX-12L, is colorless or slightly yellowish transparent viscous liquid, and the prepared cement slurry has low water loss, good rheological property, stable slurry, low free liquid, no influence on thickening time and certain dispersion effect.
The retarder is HX-36L, is light red transparent viscous liquid, has an obvious retarding effect on cement paste, the thickening time and the addition amount are in a linear relation, and the thickening curve is thickened at a right angle.
The defoaming agent is DF-A, is Sub>A light yellow homogeneous liquid, has quick defoaming, strong foam inhibition and better compatibility with other additives.
The preparation process of the oil well cement slurry system is as follows:
weighing 0.5 to 4 parts of fluid loss additive, 0.3 to 4 parts of retarder and 0.1 to 2 parts of defoaming agent, dissolving the components in 40 to 46 parts of distilled water to prepare an aqueous solution, filling the aqueous solution into a slurry cup on a high-speed stirrer, rotating the stirrer at a low speed of 4000 +/-200 revolutions per minute according to the GB/T10238-2015 pulping standard, uniformly adding 100 parts of high-strength toughening cementing material within 15 seconds, and stirring at a high speed of 12000 +/-500 revolutions per minute for 35 seconds to obtain the cement slurry oil well system.
Compared with the prior art, the beneficial technical effects brought by the invention are as follows:
1. in the invention, zirconite and baddeleyite are added into the cement raw material, on one hand, zrSiO is utilized 4 The cement stone heat-resistant reinforcing agent has the advantages of high temperature resistance, high strength, corrosion resistance, strong inertia and the like, and can be used for reasonably grading cement particles to realize the function of reinforcing the temperature resistance of the cement stone. On the other hand, zrO 2 The crystal form can be converted into a tetragonal phase structure during high-temperature calcination, and the matrix of the cement clinker is opposite to the tetragonal phase ZrO 2 The binding force is large, and tetragonal-phase ZrO in the chemical components of the cement is generated in the process of cooling to room temperature 2 Can be stably retained, when the set cement is subjected to fracture stress, the set cement matrix at the tip of the fracture is opposite to tetragonal-phase ZrO in the fracture propagation process 2 The binding force is greatly weakened, and ZrO at this time 2 The tetragonal phase is converted into the monoclinic phase, and not only can volume expansion and compressive strain be generated in the phase change process of the crystal form, so that crack propagation at the tip of a crack is blocked, but also energy can be absorbed, and fracture energy can be improved, so that fracture toughness and impact resistance can be improved, and the toughening effect of the set cement can be realized.
2. By newly adding ZrSiO into the cement mineral 4 The mineral components and the mode of reasonably controlling the grain composition of the raw materials, and the like not only endow the hardened body of the hydraulic cementing material with more rapid strength development, but also keep good sedimentation stability of the prepared cement slurry system.
3. By adding a new ZrO in the cement 2 The chemical components are based on cement raw materials and a cement production process which is controlled finely, so that the cement stone is toughened and reduced in brittleness, the additive is not required to be additionally adjusted, the cost is low, the site construction is convenient, and the defects of low strength, high brittleness and the like of the common silicate cement stone are overcome.
Drawings
FIG. 1 is a graph of a three-axis stress-strain test of set cement provided in examples 1, 2 and 3 of the present invention;
FIG. 2 is a graph showing the results of a cement paste thickening curve test provided in example 3 of the present invention;
FIG. 3 is a graph of the results of a cement slurry thickening curve test with a retarder provided in example 6 of the present invention;
FIG. 4 is a graph of the cement slurry thickening curve test results with set retarder provided in example 7 of the present invention;
FIG. 5 is a graph of the cement slurry thickening curve test results with set retarder provided in example 8 of the present invention.
Detailed Description
The technical scheme of the invention is clearly and completely described below by combining the embodiment of the invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
As a preferred embodiment of the invention, the embodiment discloses a preparation method of a high-strength toughened well cementing material, and the proportions of the components in the high-strength toughened well cementing material are in parts by weight.
In this example, a dry cement production process was used: respectively crushing limestone, red clay, baddeleyite, zirconite, a siliceous correction raw material, basalt tailings, sulfuric acid slag and copper slag by using an impact crusher, wherein the crushing ratio is controlled to be 50-60; conveying the crushed raw materials to a pre-homogenizing warehouse for pre-homogenizing treatment;
conveying the pre-homogenized raw materials to a batching station, and proportioning according to the mixing ratio of 100 parts of limestone, 12 parts of red clay, 3 parts of baddeleyite, 4 parts of zircon, 2 parts of siliceous correcting raw materials, 3 parts of basalt tailings, 2 parts of sulfuric acid slag and 4 parts of copper slag;
conveying the mixed materials after proportioning into a ball mill, and grinding into cement raw materials, wherein the grinding ratio is controlled within 300-1000; inputting the ground cement raw materials into a continuous cement raw material homogenizing warehouse to uniformly mix the cement raw materials; feeding the uniformly mixed cement raw material from the uppermost stage preheater at the tail part of the rotary kiln, carrying out heat exchange with waste hot gas from the rotary kiln in the process of passing through C1-C4 preheaters, preheating, then feeding into a decomposing furnace, calcining until most of carbonate is decomposed, feeding into the rotary kiln through the last stage preheater, and calcining at high temperature in the rotary kiln to obtain cement clinker; the calcination temperature is controlled to be 1300-1500 ℃; after the calcined cement clinker is output to the rotary kiln, the cement clinker is rapidly cooled by a grate cooler to obtain the cement clinker;
and (3) finished product preparation: sending the prepared cement clinker and the crushed dihydrate gypsum into a batching station, proportioning according to the mixing ratio of 100 parts of the cement clinker and 4 parts of the dihydrate gypsum, conveying the materials into a ball mill after batching, grinding the materials into a finished cement product, and controlling the specific surface area to be 300-360 m 2 And/kg, and finally storing the obtained cement finished product for a period of time and homogenizing to obtain the high-strength toughened well cementing material.
The mineral content in the high-strength toughened cementing material comprises C 3 S、C 2 S、C 3 A、C 4 AF and ZrSiO 4 Wherein, C is more than or equal to 50 percent 3 S≤65%，15%≤C 2 S≤30%，1.0%≤C 3 A≤2.5%，14%≤C 4 AF≤18%，1%≤ZrSiO 4 Less than or equal to 10 percent; the specific surface area of the high-strength toughened well cementing material is 300 to 360 m 2 Per kg; in the high-strength toughened cementing material, the chemical component requirements are as follows: zrO 2% or less 2 Less than or equal to 8 percent and alkali content (Na) 2 O+0.658K 2 O）≤0.75%，SO 3 Less than or equal to 3.0 percent, less than or equal to 3.0 percent of Loss and less than or equal to 0.75 percent of insoluble substances.
The content requirement of limestone components is as follows: caO is more than or equal to 50 percent, al 2 O 3 Less than or equal to 1.0 percent and MgO less than 2.5 percent. The red clay has the following component content requirements: siO 2 2 ≥60%，Al 2 O 3 Less than or equal to 12 percent. The content of the baddeleyite components is required to be as follows: zrO (ZrO) 2 Not less than 90 percent. ZrSiO in the zircon 4 Is at least 95% pure. The iron raw material comprises the following components in percentage by weight: fe 2 O 3 Not less than 60 percent. The silicon correction raw material has the following component content requirements: siO 2 2 ≥80%。
Weighing 44 parts of distilled water, filling the distilled water into a slurry cup of a high-speed stirrer, rotating the stirrer at a low speed (4000 +/-200 revolutions per minute) according to the GB/T10238-2015 pulping standard, uniformly adding 100 parts of the prepared high-strength toughening well cementation cementing material within 15 seconds, and then stirring at a high speed (12000 +/-500 revolutions per minute) for 35 seconds to obtain the high-strength toughening well cementation cement slurry system.
Example 2
As another preferred embodiment of the present invention, the present embodiment relates to a high strength toughened well cementation cement slurry system, which comprises the following specific steps:
in this example, a dry cement production process was used: respectively crushing limestone, red clay, baddeleyite, zirconite, a siliceous correction raw material, basalt tailings, sulfuric acid slag and copper slag by using an impact crusher, wherein the crushing ratio is controlled to be 50-60; conveying the crushed raw materials to a pre-homogenizing warehouse for pre-homogenizing treatment;
conveying the pre-homogenized raw materials to a batching station, and proportioning according to the mixing ratio of 100 parts of limestone, 12 parts of red clay, 5 parts of baddeleyite, 6 parts of zircon, 2 parts of siliceous correcting raw materials, 3 parts of basalt tailings, 2 parts of sulfuric acid slag and 2 parts of copper slag;
conveying the mixed materials after proportioning into a ball mill, and grinding into cement raw materials, wherein the grinding ratio is controlled within 300-1000; inputting the ground cement raw materials into a continuous cement raw material homogenizing warehouse to uniformly mix the cement raw materials; feeding the uniformly mixed cement raw material from the uppermost stage preheater at the tail part of the rotary kiln, carrying out heat exchange with waste hot gas from the rotary kiln in the process of passing through C1-C4 preheaters, preheating, then feeding into a decomposing furnace, calcining until most of carbonate is decomposed, feeding into the rotary kiln through the last stage preheater, and calcining at high temperature in the rotary kiln to obtain cement clinker; the calcination temperature is controlled to be 1300-1500 ℃; after the calcined cement clinker is output to the rotary kiln, the cement clinker is rapidly cooled by a grate cooler to obtain the cement clinker;
and (3) finished product preparation: sending the prepared cement clinker and the crushed dihydrate gypsum into a batching station, proportioning according to the mixing ratio of 100 parts of the cement clinker and 4 parts of the dihydrate gypsum, conveying the materials into a ball mill after batching, grinding the materials into a finished cement product, and controlling the specific surface area to be 300-360 m 2 And/kg, and finally storing the obtained cement finished product for a period of time and homogenizing to obtain the high-strength toughened well cementing material.
The above high strengthThe mineral content in the cement material for tough well cementation comprises C 3 S、C 2 S、C 3 A、C 4 AF and ZrSiO 4 Wherein, C is more than or equal to 50 percent 3 S≤65%，15%≤C 2 S≤30%，1.0%≤C 3 A≤2.5%，14%≤C 4 AF≤18%，1%≤ZrSiO 4 Less than or equal to 10 percent; the specific surface area of the high-strength toughened well cementing material is 300 to 360 m 2 Per kg; in the high-strength toughened well cementation cementing material, the chemical component requirements are as follows: zrO 2% or less 2 Less than or equal to 8 percent and alkali content (Na) 2 O+0.658K 2 O）≤0.75%，SO 3 Less than or equal to 3.0 percent, less than or equal to 3.0 percent of Loss and less than or equal to 0.75 percent of insoluble substances.
The content requirement of limestone components is as follows: caO is more than or equal to 50 percent, al 2 O 3 Less than or equal to 1.0 percent and MgO less than 2.5 percent. The red clay has the following component content requirements: siO 2 2 ≥60%，Al 2 O 3 Less than or equal to 12 percent. The content of the baddeleyite components is required to be as follows: zrO (ZrO) 2 Not less than 90 percent. ZrSiO in the zirconite 4 Is at least 95% pure. The iron raw material comprises the following components in percentage by weight: fe 2 O 3 Not less than 60 percent. The silicon correction raw material has the following component content requirements: siO 2 2 ≥80%。
Weighing 44 parts of distilled water, filling the distilled water into a slurry cup of a high-speed stirrer, rotating the stirrer at a low speed (4000 +/-200 revolutions per minute) according to the GB/T10238-2015 pulping standard, uniformly adding 100 parts of the prepared high-strength toughening well cementation cementing material within 15 seconds, and then stirring at a high speed (12000 +/-500 revolutions per minute) for 35 seconds to obtain the high-strength toughening well cementation cement slurry system.
Example 3
As another preferred embodiment of the present invention, the present embodiment relates to a high strength and toughness reinforced well cementing cement slurry system, which comprises the following specific components:
in this example, a dry cement production process was used: respectively crushing limestone, red clay, baddeleyite, zirconite, a siliceous correction raw material, basalt tailings, sulfuric acid slag and copper slag by using an impact crusher, wherein the crushing ratio is controlled to be 50-60; conveying the crushed raw materials to a pre-homogenizing warehouse for pre-homogenizing treatment;
conveying the pre-homogenized raw materials to a batching station, and proportioning according to the mixing ratio of 100 parts of limestone, 12 parts of red clay, 7 parts of baddeleyite, 8 parts of zircon, 2 parts of siliceous correcting raw materials, 3 parts of basalt tailings, 2 parts of sulfuric acid slag and 2 parts of copper slag;
conveying the mixed materials after proportioning into a ball mill, and grinding into cement raw materials, wherein the grinding ratio is controlled to be 300-1000; inputting the ground cement raw materials into a continuous cement raw material homogenizing warehouse to uniformly mix the cement raw materials; feeding the uniformly mixed cement raw material from the uppermost stage preheater at the tail part of the rotary kiln, carrying out heat exchange with waste hot gas from the rotary kiln in the process of passing through C1-C4 preheaters, preheating, then feeding into a decomposing furnace, calcining until most of carbonate is decomposed, feeding into the rotary kiln through the last stage preheater, and calcining at high temperature in the rotary kiln to obtain cement clinker; the calcination temperature is controlled to be 1300-1500 ℃; after the calcined cement clinker is output to the rotary kiln, the cement clinker is rapidly cooled by a grate cooler to obtain the cement clinker;
and (3) finished product preparation: sending the prepared cement clinker and the crushed dihydrate gypsum into a batching station, proportioning according to the mixing ratio of 100 parts of the cement clinker and 4 parts of the dihydrate gypsum, conveying the materials into a ball mill after batching, grinding the materials into a finished cement product, and controlling the specific surface area to be 300-360 m 2 And/kg, and finally storing the obtained cement finished product for a period of time and homogenizing to obtain the high-strength toughened well cementing material.
The mineral content in the high-strength toughened cementing material comprises C 3 S、C 2 S、C 3 A、C 4 AF and ZrSiO 4 Wherein, C is more than or equal to 50 percent 3 S≤65%，15%≤C 2 S≤30%，1.0%≤C 3 A≤2.5%，14%≤C 4 AF≤18%，1%≤ZrSiO 4 Less than or equal to 10 percent; the specific surface area of the high-strength toughened well cementing material is 300 to 360 m 2 Per kg; in the high-strength toughened well cementation cementing material, the chemical component requirements are as follows: zrO 2% or less 2 Less than or equal to 8 percent and alkali content (Na) 2 O+0.658K 2 O）≤0.75%，SO 3 Less than or equal to 3.0 percent, less than or equal to 3.0 percent of Loss and less than or equal to 0.75 percent of insoluble substances.
The content requirement of limestone components is as follows: caO is more than or equal to 50 percent, al 2 O 3 ≤10% and MgO less than 2.5%. The red clay has the following component content requirements: siO 2 2 ≥60%，Al 2 O 3 Less than or equal to 12 percent. The content of the baddeleyite components is required to be as follows: zrO (ZrO) 2 Not less than 90 percent. ZrSiO in the zirconite 4 Is at least 95% pure. The iron raw material comprises the following components in percentage by weight: fe 2 O 3 Not less than 60 percent. The silicon correction raw material has the following component content requirements: siO 2 2 ≥80%。
Weighing 44 parts of distilled water, filling the distilled water into a slurry cup of a high-speed stirrer, rotating the stirrer at a low speed (4000 +/-200 revolutions per minute) according to the GB/T10238-2015 pulping standard, uniformly adding 100 parts of the prepared high-strength toughening well cementation cementing material within 15 seconds, and then stirring at a high speed (12000 +/-500 revolutions per minute) for 35 seconds to obtain the high-strength toughening well cementation cement slurry system.
Mechanical property experiments are carried out on the set cements obtained after the cement slurry is hardened in the embodiments 1 to 3, wherein the mechanical property experiments comprise a compression strength test, a breaking strength test and an elastic modulus test under a triaxial stress condition, and the test contents are strictly carried out according to the GB/T19139 oil well cement experiment method. The results of the performance tests are shown in table 1 below.
TABLE 1 Cement stone mechanical property test structure
| Examples | Curing temperature (. Degree.C.) | Age (d) | Compressive strength (MPa) | Flexural strength (MPa) | Triaxial elastic modulus GPa (confining |
| Example 1 | 60 | 2 | 30.8 | 4.3 | 8.9 |
| Example 2 | 60 | 2 | 34.5 | 6.1 | 7.8 |
| Example 3 | 60 | 2 | 37.2 | 8.5 | 5.6 |
As can be seen from the test results in table 1 and the test curves in fig. 1: within a reasonable regulation range, along with the increase of the content of zircon and baddeleyite, under the same condition, the compression strength of the set cement is obviously increased, the breaking strength is obviously improved (the impact resistance is improved, the toughness is stronger), and the elastic modulus of the set cement is obviously reduced (which indicates that the mechanical deformation capability of the set cement is improved, and the micro-annular space formation can be better inhibited).
Example 4
As still another preferred embodiment of the present invention, in the present embodiment, in order to prepare the high strength toughened well cementation cementing material, the components of the high strength toughened well cementation cementing material are limestone, red clay, baddeleyite, zirconite, siliceous correction raw material, basalt tailings, sulfuric acid slag, copper slag and dihydrate gypsum. When selecting raw materials, the raw materials should be selectedNote that the limestone component content requirement: caO is more than or equal to 50 percent, al 2 O 3 Less than or equal to 1.0 percent and MgO less than 2.5 percent. The content requirement of the red clay components is as follows: siO 2 2 ≥60%，Al 2 O 3 Less than or equal to 12 percent. The content requirement of the baddeleyite components is as follows: zrO (zirconium oxide) 2 More than or equal to 90 percent. ZrSiO in zircon 4 Is at least 95% pure. The iron raw material comprises the following components in percentage by weight: fe 2 O 3 Not less than 60 percent. The silicon correction raw material has the following component content requirements: siO 2 2 More than or equal to 80 percent; then preparing raw materials according to the following mixture ratio: 100 parts of limestone, 10 parts of red clay, 1 part of baddeleyite, 2 parts of zircon, 1 part of siliceous correcting raw material, 1 part of basalt tailings, 4 parts of sulfuric acid residue, 3 parts of copper slag and 3 parts of dihydrate gypsum; and then, generating cement raw materials from limestone, red clay, baddeleyite, zirconite, siliceous correction raw materials, basalt tailings, sulfuric acid slag and copper slag according to a dry cement production method, mixing 100 parts of the produced cement raw materials with 3 parts of dihydrate gypsum, calcining to obtain cement clinker, storing the powder for a period of time, and homogenizing to obtain the high-strength toughened well cementation cementing material.
Example 5
As still another preferred embodiment of the present invention, in the present embodiment, in order to prepare the high strength toughened well cementation cementing material, the components of the high strength toughened well cementation cementing material are limestone, red clay, baddeleyite, zirconite, siliceous correction raw material, basalt tailings, sulfuric acid slag, copper slag and dihydrate gypsum. When raw material selection is carried out, the following requirements on the content of limestone components are required: caO is more than or equal to 50 percent, al 2 O 3 Less than or equal to 1.0 percent and MgO less than 2.5 percent. The content requirement of the red clay components is as follows: siO 2 2 ≥60%，Al 2 O 3 Less than or equal to 12 percent. The content requirement of the baddeleyite components is as follows: zrO (ZrO) 2 Not less than 90 percent. ZrSiO in zircon 4 Is at least 95% pure. The iron raw material comprises the following components in percentage by weight: fe 2 O 3 Not less than 60 percent. The silicon correction raw material has the following component content requirements: siO 2 2 More than or equal to 80 percent; then preparing raw materials according to the following mixture ratio: 100 parts of limestone, 15 parts of red clay, 8 parts of baddeleyite, 10 parts of zirconite, 5 parts of siliceous correcting raw material, 5 parts of basalt tailings, 6 parts of sulfuric acid slag, 5 parts of copper slag and 5 parts of dihydrate gypsum; then the original material is mixedThe materials limestone, red clay, baddeleyite, zirconite, siliceous correction raw material, basalt tailings, sulfuric acid slag and copper slag are produced into cement raw material according to the dry cement production method, then 100 parts of the produced cement raw material is mixed with 5 parts of dihydrate gypsum to be calcined to obtain cement clinker, and the cement clinker is stored for a period of time to be homogenized to obtain the high-strength toughened well cementation cementing material.
The mineral content of the high-strength toughened well cementation cementing material prepared according to the specific raw materials selected in the above examples 4 and 5 and the method comprises C 3 S、C 2 S、C 3 A、C 4 AF and ZrSiO 4 Wherein, C is more than or equal to 50 percent 3 S≤65%，15%≤C 2 S≤30%，1.0%≤C 3 A≤2.5%，14%≤C 4 AF≤18%，1%≤ZrSiO 4 Less than or equal to 10 percent; the specific surface area of the high-strength toughened well cementing material is 300 to 360 m 2 Per kg; in the high-strength toughened cementing material, the chemical component requirements are as follows: zrO 2% or less 2 Less than or equal to 8 percent and alkali content (Na) 2 O+0.658K 2 O）≤0.75%，SO 3 Less than or equal to 3.0 percent, less than or equal to 3.0 percent of Loss and less than or equal to 0.75 percent of insoluble substances.
Example 6
The embodiment provides a preparation method of a high-strength toughened well cementing cement slurry system (the following components are in parts by weight) convenient for construction, and the high-strength toughened well cementing material is prepared by adopting the production method of the embodiment 3.
Weighing 2 parts of fluid loss agent HX-12L, 0.3 part of retarder HX-36L and 0.2 part of defoamer DF-A, dissolving the components in 44 parts of distilled water to prepare an aqueous solution, filling the aqueous solution into Sub>A slurry cup on Sub>A high-speed stirrer, rotating the stirrer at Sub>A low speed (4000 +/-200 revolutions per minute) according to the GB/T10238-2015 pulping standard, uniformly adding 100 parts of high-strength toughening well cementing materials within 15 seconds, and then stirring at Sub>A high speed (12000 +/-500 revolutions per minute) for 35 seconds to obtain the high-strength toughening well cementing slurry system.
Example 7
The embodiment provides a preparation method of a high-strength toughened well cementing cement slurry system convenient for construction (the following components are in parts by weight), and the production method of the embodiment 3 is adopted to prepare the high-strength toughened well cementing material.
Weighing 2 parts of filtrate reducer HX-12L, 0.6 part of retarder HX-36L and 0.2 part of defoamer DF-A, dissolving the filtrate reducer in 44 parts of distilled water to prepare an aqueous solution, filling the aqueous solution into Sub>A slurry cup on Sub>A high-speed stirrer, rotating the stirrer at Sub>A low speed (4000 +/-200 revolutions per minute) according to the GB/T10238-2015 slurry standard, uniformly adding 100 parts of high-strength toughened well cementing material within 15 seconds, and then stirring at Sub>A high speed (12000 +/-500 revolutions per minute) for 35 seconds to obtain the high-strength toughened well cementing system cement slurry.
Example 8
The embodiment provides a preparation method of a high-strength toughened well cementing cement slurry system (the following components are in parts by weight) convenient for construction, and the production method of the embodiment 3 is adopted to prepare the high-strength toughened well cementing material.
Weighing 2 parts of filtrate reducer HX-12L, 0.9 part of retarder HX-36L and 0.2 part of defoamer DF-A, dissolving the filtrate reducer in 44 parts of distilled water to prepare an aqueous solution, filling the aqueous solution into Sub>A slurry cup on Sub>A high-speed stirrer, rotating the stirrer at Sub>A low speed (4000 +/-200 revolutions per minute) according to the GB/T10238-2015 slurry standard, uniformly adding 100 parts of high-strength toughened well cementing material within 15 seconds, and then stirring at Sub>A high speed (12000 +/-500 revolutions per minute) for 35 seconds to obtain the high-strength toughened well cementing system cement slurry.
The grouts of examples 3, 6, 7 and 8 were subjected to engineering performance testing experiments which included: the method comprises the following steps of density testing, fluidity testing, API water loss testing, free liquid testing and thickening time testing, wherein the content of the testing is strictly carried out according to the GB/T19139 oil well cement testing method. The results of the performance tests are shown in table 2 below.
TABLE 2 Cement mortar engineering Performance test
As can be seen from the test results in Table 2, the high-strength toughened well cementation cement slurry system prepared by the invention has the advantages of good fluidity, low water loss, zero free liquid and the like, and the test curves shown in a combined graph of figures 2 to 5 show that: the cement slurry thickening time has good adjustability, can effectively improve the field adaptability of the cement slurry system, and provides favorable guarantee for the safety of well cementation construction and the quality of well cementation.
Example 9
The embodiment provides a preparation method of a high-strength toughened well cementing cement slurry system convenient for construction (the following components are in parts by weight), and the production method of the embodiment 3 is adopted to prepare the high-strength toughened well cementing material.
Weighing 4 parts of fluid loss agent HX-12L, 2 parts of retarder HX-36L and 0.1 part of defoamer DF-A, dissolving the components in 40 parts of distilled water to prepare an aqueous solution, filling the aqueous solution into Sub>A slurry cup on Sub>A high-speed stirrer, rotating the stirrer at Sub>A low speed (4000 +/-200 revolutions per minute) according to the GB/T10238-2015 slurry standard, uniformly adding 100 parts of high-strength toughening well cementation cementing material within 15 seconds, and then stirring at Sub>A high speed (12000 +/-500 revolutions per minute) for 35 seconds to obtain the high-strength toughening well cementation cement slurry system.
Example 10
The embodiment provides a preparation method of a high-strength toughened well cementing cement slurry system convenient for construction (the following components are in parts by weight), and the production method of the embodiment 3 is adopted to prepare the high-strength toughened well cementing material.
Weighing 4 parts of filtrate reducer HX-12L, 4 parts of retarder HX-36L and 2 parts of defoamer DF-A, dissolving the filtrate reducer in 46 parts of distilled water to prepare an aqueous solution, filling the aqueous solution into Sub>A slurry cup on Sub>A high-speed stirrer, rotating the stirrer at Sub>A low speed (4000 +/-200 revolutions per minute) according to GB/T10238-2015 pulping standard, uniformly adding 100 parts of high-strength and toughened well cementing material within 15 seconds, and then stirring at Sub>A high speed (12000 +/-500 revolutions per minute) for 35 seconds to obtain the high-strength and toughened well cementing slurry system.
Claims (10)
1. A high-strength toughened cementing material comprises the following components in parts by weight:
100 parts of limestone, 10-15 parts of red clay, 3245 parts of baddeleyite, 3245 parts of zxft, 2-10 parts of zircon, 3732 parts of siliceous correction raw material, 3963 parts of basalt tailings, 3963 parts of sulfuric acid residue, 4325 parts of zxft, 3536 parts of copper slag and 3926 parts of dihydrate gypsum; the high-strength toughened well cementing adhesiveThe mineral content of the coagulated material includes C 3 S、C 2 S、C 3 A、C 4 AF and ZrSiO 4 Wherein, C is more than or equal to 50 percent 3 S≤65%，15%≤C 2 S≤30%，1.0%≤C 3 A≤2.5%，14%≤C 4 AF≤18%，1%≤ZrSiO 4 Less than or equal to 10 percent; the specific surface area of the high-strength toughened well cementing material is 300 to 360 m 2 (iv) kg; in the high-strength toughened cementing material, the chemical component requirements are as follows: zrO 2% or less 2 Less than or equal to 8 percent and alkali content (Na) 2 O+0.658K 2 O）≤0.75%，SO 3 Less than or equal to 3.0 percent, less than or equal to 3.0 percent of Loss and less than or equal to 0.75 percent of insoluble substances.
2. The high-strength toughened well cementation cement material as claimed in claim 1, wherein: the limestone component content requirement is as follows: caO is more than or equal to 50 percent, al 2 O 3 ≤1.0%，MgO＜2.5%。
3. The high-strength toughened well cementation cement material as claimed in claim 1, wherein: the red clay has the following component content requirements: siO 2 2 ≥60%，Al 2 O 3 ≤12%。
4. The high-strength toughened well cementation cement material as claimed in claim 1, wherein: the content of the baddeleyite components is required to be as follows: zrO (ZrO) 2 More than or equal to 90 percent; zrSiO in the zirconite 4 Is at least 95% pure.
5. The high-strength toughened well cementation cement material as claimed in claim 1, wherein: the iron raw material comprises the following components in percentage by weight: fe 2 O 3 ≥60%。
6. The high-strength toughened well cementation cement material as claimed in claim 1, wherein: the silicon correction raw material has the following component content requirements: siO 2 2 ≥80%。
7. The method for preparing the high-strength toughened cementing material according to any one of the claims 1 to 6, which is characterized in that: the method comprises the following steps:
a raw material crushing step: respectively crushing limestone, red clay, baddeleyite, zirconite, a siliceous correction raw material, basalt tailings, sulfuric acid slag and copper slag by using an impact crusher, wherein the crushing ratio is controlled to be 50-60;
pre-homogenization treatment: conveying the crushed raw materials in the raw material crushing step to a pre-homogenizing warehouse for pre-homogenizing treatment;
the material preparation step: conveying the raw materials subjected to pre-homogenization treatment to a batching station, and proportioning according to the mixing ratio of 100 parts of limestone, 10-15 parts of red clay, 1~8 parts of baddeleyite, 2-10 parts of zircon, 1~5 parts of siliceous correction raw material, 1~5 parts of basalt tailings, 2~6 parts of sulfuric acid slag and 2~5 parts of copper slag;
grinding: conveying the mixed materials after proportioning into a ball mill, and grinding into cement raw materials, wherein the grinding ratio is controlled within 300-1000;
and (3) homogenization treatment: inputting the ground cement raw materials into a continuous cement raw material homogenizing warehouse to uniformly mix the cement raw materials;
and (3) calcining: feeding the uniformly mixed cement raw material from the uppermost stage preheater at the tail part of the rotary kiln, carrying out heat exchange with waste hot gas from the rotary kiln in the process of passing through C1-C4 preheaters, preheating, then feeding into a decomposing furnace, calcining until most of carbonate is decomposed, feeding into the rotary kiln through the last stage preheater, and calcining at high temperature in the rotary kiln to obtain cement clinker; the calcination temperature is controlled to be 1300-1500 ℃; after the calcined cement clinker is output to the rotary kiln, the cement clinker is rapidly cooled by a grate cooler to obtain the cement clinker;
and (3) finished product preparation: sending the prepared cement clinker and the crushed dihydrate gypsum into a batching station, proportioning according to the mixing ratio of 100 parts of the cement clinker and 3~5 parts of the dihydrate gypsum, conveying the materials into a ball mill after batching, grinding the materials into a cement finished product, and controlling the specific surface area within 300-360 m 2 And/kg, and finally storing the obtained cement finished product for a period of time and homogenizing to obtain the high-strength toughened well cementing material.
8. The use of a strong and toughened cementing cement material as claimed in any one of claims 1 to 6 in oil well cement slurry systems, wherein: the high-strength toughened well cementation cementing material is applied to oil well cement slurry, and the oil well cement slurry comprises the following components in parts by weight:
100 parts of high-strength toughened well cementing material, 0.5 to 4 parts of fluid loss agent, 0.3 to 4 parts of retarder, 0.1 to 2 parts of defoaming agent and 40 to 46 parts of distilled water.
9. The use of a strong toughened cementing cement material as claimed in claim 8 in an oil well cement slurry system, wherein: the fluid loss agent is HX-12L, the retarder is HX-36L, and the defoaming agent is DF-A.
10. The use of a strong toughened cementing cement material as claimed in claim 8 in an oil well cement slurry system, wherein: the preparation process of the oil well cement slurry system is as follows:
weighing 0.5 to 4 parts of fluid loss additive, 0.3 to 4 parts of retarder and 0.1 to 2 parts of defoaming agent, dissolving the materials in 40 to 46 parts of distilled water to prepare an aqueous solution, filling the aqueous solution into a slurry cup on a high-speed stirrer, rotating the stirrer at a low speed of 4000 +/-200 revolutions per minute according to GB/T10238-2015 pulping standard, uniformly adding 100 parts of high-strength toughened well cementation cementing material within 15 seconds, and stirring at a high speed of 12000 +/-500 revolutions per minute for 35 seconds to obtain the oil well cement slurry system.
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