CN113105877A - Modified natural cellulose fiber, preparation method thereof and water invasion resistant well cementation cement slurry - Google Patents

Modified natural cellulose fiber, preparation method thereof and water invasion resistant well cementation cement slurry Download PDF

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CN113105877A
CN113105877A CN202110401187.6A CN202110401187A CN113105877A CN 113105877 A CN113105877 A CN 113105877A CN 202110401187 A CN202110401187 A CN 202110401187A CN 113105877 A CN113105877 A CN 113105877A
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cellulose fibers
water
natural cellulose
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刘开强
马瑞瑞
曹权
李斌
刘强
付志
江川
田孝斌
张兴国
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Southwest Petroleum University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic

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Abstract

The invention discloses a modified natural cellulose fiber, a preparation method thereof and water invasion resistant well cementing cement slurry. A method of modifying natural cellulose fibers comprising: the method comprises the steps of pretreating natural cellulose fibers by using a sodium hydroxide solution, combining a planetary ball mill with a vertical corundum-alumina ball milling tank, and ball milling the pretreated natural cellulose fibers, wherein the natural cellulose fibers comprise 100 parts by mass of total high-sulfate-resistance G-grade oil well cement and an admixture, 1.0-5.0 parts by mass of a fluid loss additive, 0.2-2.0 parts by mass of a dispersing agent, 0-1.0 part by mass of a retarder, 0.1-0.5 part by mass of modified cellulose fibers, 0.05-0.1 part by mass of a defoaming agent and 40-50 parts by mass of water. The well cementation cement slurry system has the advantages of cleanness, environmental protection, low cost, no dispersion in water, good water invasion resistance, high early compressive strength, adjustable thickening time and the like.

Description

Modified natural cellulose fiber, preparation method thereof and water invasion resistant well cementation cement slurry
Technical Field
The invention belongs to the field of oil and gas well cementing materials, and particularly relates to a modified natural cellulose fiber, a preparation method thereof and water invasion resistant well cementing cement slurry.
Background
The old oil field in China enters the middle and later development stages successively, and due to long-term water injection development, the old oil field faces the outstanding problems of disordered landing layer pressure systems, high formation water content, low crude oil recovery rate and the like. In order to stabilize the yield of the old oil field, the current common and effective mode is to drill a new encryption adjusting well in the old oil field to optimize the injection-production mode of the old oil field. However, in well cementing engineering of a regulation well, due to geological characteristics such as disorder of a pressure system, high formation water content and the like and the weight loss behavior of the cementing slurry in the solidification process, formation water is easy to invade into the annular cement slurry, so that the performance of the cement slurry is deteriorated, and the cementing quality of a second interface between the cement slurry and formation rock is reduced. Therefore, in recent years, industry researchers have conducted a great deal of research on how to improve the water invasion resistance of the cement slurry system for well cementing.
For example, Zhangguo et al established a quantitative evaluation method of the water invasion resistance of well cementation cement slurry by a method of washing the cement slurry with water flow and testing the conductivity of the water flow (Zhangguo, Kingjinshan, Kingjinxing, etc.. evaluation device and method of the water invasion resistance of well cementation cement slurry in the process of waiting to set [ P ]. CN107167499A, 2017); ruhaichuan and the like prepare a water channeling preventing material for well cementation (ruhaichuan, liu courage, zhang weibin and the like) by mixing inorganic materials such as sepiolite and the like and copolymers such as styrene sulfonic acid-maleic anhydride and the like, a water channeling preventing material for well cementation and a preparation method [ P ]. CN106701048A, 2017); liu Jing Li et al, by using N, N dimethylacrylamide monomer, acrylamide monomer, 2-acrylamido-2-methylpropanesulfonic acid and acrylic acid monomer to prepare water invasion resisting regulator, and using the regulator to prepare a temperature-resistant water invasion resisting gel cement slurry system (Liu Jing Li Chang, Lily Chang, Liqiang, temperature-resistant water invasion resisting gel cement slurry [ P ]. CN107352862A, 2017); an oil well cement anti-dispersion flocculant is synthesized by Wangjian Yao and the like in a free radical polymerization way, and can meet the requirements that cement paste is not isolated and not dispersed under the action of water scouring at 80 ℃ (Wangjian Yao, formerly Jian, Sun Fu, and the like, an oil well cement anti-dispersion flocculant [ J ] a drilling fluid and a completion fluid, 2018,35(2): 90-93); licheng and the like synthesize a water-soluble hydrophobic association polymer for well cementing cement slurry by using 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, maleic anhydride and octadecyl acrylate as monomers, and the water-soluble hydrophobic association polymer can obviously improve the water invasion resistance of the well cementing cement slurry (Licheng, Zhaojian, Liuhuan. the synthesis and performance of a hydrophobic association polymer channeling inhibitor for dynamic pressure well cementing [ J ] synthetic chemistry 2020,28(8): 722) 727.). The comparative analysis of the research results shows that in the well cementation cement slurry, the anti-dispersion flocculant and the hydrophobic association polymer are adsorbed on the surfaces of cement particles to enable the cement slurry to form a flocculation structure, so that the water invasion resistance of the cement slurry is improved, but the introduction of the polymers can slow down the hydration rate of the well cementation cement, so that the early mechanical property of the well cementation cement is reduced; meanwhile, the synthesis process of the materials is complex, and the cost of the well cementation cement slurry is increased to a certain extent. Therefore, the development of a low-cost water invasion resistant treating agent which can enhance the water invasion resistance of well cementation cement slurry and improve the early mechanical property of the well cementation cement slurry is urgently needed to improve the cementing quality of a second interface of well cementation of an old oil field adjusting well and guarantee the packing quality of a cement ring layer and the development benefit of the oil field.
The natural cellulose fiber is universally existed in various plants, has the advantages of reproducibility, cleanness, low cost and the like, contains a large amount of hydroxyl in the molecular structure, and can enable the cellulose fiber and cement particles to generate adsorption action through modes of polyvalent metal ion bridging, hydrogen bonds and the like; meanwhile, the physical bridging effect of the fibers in the cement paste can promote the cement paste to form a flocculation structure, and the cement paste has great potential for improving the water invasion resistance of the well cementation cement paste. However, natural cellulose fibers tend to agglomerate in cement slurries and are not easily dispersed due to their large length and diameter. Therefore, the invention establishes a natural cellulose fiber modification method suitable for well cementation cement slurry, and prepares a water invasion resistant cement slurry system which is non-dispersible in water, strong in water invasion resistance and good in mechanical property based on the modified cellulose fiber.
Disclosure of Invention
The invention aims to prepare modified natural cellulose fiber suitable for oil-gas well cementing cement slurry by a modification method, and prepare a water-invasion-resistant well cementing cement slurry system with good water-invasion resistance and early mechanical property by using the agent.
The preparation method of the modified natural cellulose fiber comprises the following steps:
(1) preparing 0.1mol/L sodium hydroxide solution, heating the solution to 60 ℃, and adding a part of untreated natural cellulose fibers into the sodium hydroxide solution, wherein the mass ratio of the solution to the natural cellulose fibers is 20: 1. Stirring for 5 minutes at the rotating speed of 4000r/min by using a constant-speed stirrer manufactured by Shenyang aerospace university application technology research; utilizing a circulating water type multipurpose vacuum pump to be matched with quick filter paper, filtering the stirred natural cellulose fiber, soaking the natural cellulose fiber by utilizing distilled water, and performing vacuum filtration twice to obtain the pretreated natural cellulose fiber;
(2) placing the pretreated natural cellulose fibers in a beaker, adding a certain amount of distilled water, wherein the mass ratio of the distilled water to the pretreated natural cellulose fibers is 20:1, and stirring with a glass rod to completely disperse the pretreated natural cellulose fibers in the distilled water;
(3) pouring distilled water containing natural cellulose fibers into a vertical corundum-alumina ball milling tank, putting corundum milling balls into the ball milling tank, ball milling the pretreated natural cellulose fibers at a set rotating speed for a set time, and adjusting the rotating speed and the ball milling time of a planetary ball mill according to the size of the required cellulose fibers;
(4) pouring out the ball-milled natural cellulose fibers, separating the grinding balls from the natural cellulose fiber solution, filtering the matched medium-speed filter paper by using a water-circulating multi-purpose vacuum pump, filtering the ball-milled natural cellulose fibers, and collecting the filtered natural cellulose fibers to obtain the modified natural cellulose fibers.
The modified natural cellulose fiber obtained above is used to prepare water invasion resistant well cementation cement slurry, which comprises the following components in parts by weight: 100 parts of high sulfate-resistant G-grade oil well cement and admixture, 1.0-5.0 parts of fluid loss additive, 0.2-2.0 parts of dispersant, 0-1.0 part of retarder, 0.1-0.5 part of modified cellulose fiber, 0.05-0.1 part of defoaming agent and 40-50 parts of water.
Further, the admixture is one or a mixture of any two of slag, fly ash, micro-silicon, quartz sand, silicon powder and glass beads.
Further, the fluid loss agent is a copolymer of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide and acrylic acid, and is purchased from Weiliang chemical Co., Ltd;
further, the dispersant is an acetone-formaldehyde polycondensate purchased from Weihui chemical Co., Ltd;
further, the retarder is a blend of polyhydroxycarboxylic acid and sulfonate;
further, the defoaming agent is tributyl phosphate, purchased from urban Congon chemical Co., Ltd;
the preparation method of the water invasion resistant well cementation cement slurry comprises the following steps:
weighing 100 parts by weight of high sulfate-resistant G-grade oil well cement and an admixture, 1.0-5.0 parts by weight of a fluid loss agent, 0.2-2.0 parts by weight of a dispersant, 0-1.0 part by weight of a retarder and 0.1-0.5 part by weight of modified cellulose fibers, and dry-mixing the solid powder into a dry mixture;
weighing 0.05-0.1 part by weight of defoaming agent, mixing the defoaming agent with 40-50 parts by weight of water, pouring the aqueous solution into a constant speed stirrer (provided by Shenyang aerospace university application and technology research institute), stirring at the rotating speed of 4000 +/-200 r/min, and pouring the dry mixture into the constant speed stirrer within 15 seconds; and then the rotating speed of the constant speed stirrer is increased to 12000 +/-500 r/min, and stirring is continued for 35 seconds, so that the water-invasion-resistant cement paste system is obtained.
The technical scheme provided by the invention is that from the viewpoint of oil well cement paste, in order to improve the water invasion resistance of a high-water-content stratum well cementation cement paste system, the water invasion resistance well cementation cement paste is developed by modifying natural renewable cellulose fibers, and has the advantages of environmental friendliness, low cost, no dispersion in water, strong water invasion resistance, excellent mechanical properties, capability of adjusting the cement paste thickening time according to construction requirements and the like.
Drawings
FIG. 1 shows the water dispersion state of a control cement slurry system;
FIG. 2 example 1 aqueous dispersion of a cement slurry system containing 1.2g of modified cellulose fibers;
FIG. 3 example 2 the water dispersion of a cement slurry system containing 1.2g of modified cellulose fibers.
Detailed Description
The technical solution of the present invention is described in detail below with reference to examples.
Control group
A cement paste system: 540G of high sulfate-resistant G-grade oil well cement, 60G of micro-silicon, 12G of fluid loss additive, 3G of dispersing agent, 0.5G of defoaming agent and 264G of water.
TABLE 1 comparative group Cement mortar System Performance test results
Figure BDA0003020360060000031
FIG. 1 shows the water dispersion state of the cement slurry system of the control group.
At normal temperature, 5mL of newly-prepared control group cement slurry is injected into a beaker containing 150mL of clear water by using an injector, the cement slurry is dispersed in the beaker water, and the beaker is turbid by using the clear water.
Example 1
Modification of natural cellulose fiber:
preparing 800ml of 0.1mol/L sodium hydroxide solution, heating to 60 ℃, weighing 40g of natural cellulose fibers, placing the natural cellulose fibers in the sodium hydroxide solution, and stirring for 5 minutes at the rotating speed of 4000r/min by using a constant-speed stirrer; fast filter paper is matched with a water-circulating type multipurpose vacuum pump to filter a sodium hydroxide solution; and soaking and cleaning the natural cellulose fibers twice by using distilled water, and then putting the pretreated natural cellulose fibers into the distilled water (the mass ratio of the distilled water to the natural cellulose fibers is 20: 1). Then, a planetary ball mill is matched with a vertical corundum ball milling tank, and the pretreated natural cellulose fiber solution is ball milled for 60 minutes at the rotating speed of 300 r/min; and then filtering the ball-milled natural cellulose fiber by using a circulating water type multipurpose vacuum pump matched with medium-speed filter paper to obtain the modified natural cellulose fiber.
Water intrusion resistant cement slurry system 1:
540G of high-sulfate-resistance G-grade oil well cement, 60G of micro-silicon, 12G of fluid loss additive, 3G of dispersing agent, 0.5G of defoaming agent and 264G of water, wherein the mass is the modified natural cellulose fiber in the table 2.
Table 2 example 1 performance test results for water intrusion resistant cement slurry system 1
Figure BDA0003020360060000041
FIG. 2 is a graph of the water dispersion of example 2 with a modified cellulose fiber cement slurry system containing 1.2 g.
At normal temperature, 5mL of a newly-prepared water-invasion-resistant cement paste system 1 (containing 1.2g of modified natural cellulose fibers) is injected into a beaker containing 150mL of clear water by using an injector, the water-invasion-resistant cement paste system 1 (containing 1.2g of modified natural cellulose fibers) has no obvious dispersion phenomenon in the water, and the clear water in the beaker is transparent.
Example 2
Modification of natural cellulose fiber:
preparing 800ml of 0.1mol/L sodium hydroxide solution, heating to 60 ℃, weighing 40g of natural cellulose fibers, placing the natural cellulose fibers in the sodium hydroxide solution, and stirring for 5 minutes at the rotating speed of 4000r/min by using a constant-speed stirrer; fast filter paper is matched with a water-circulating type multipurpose vacuum pump to filter a sodium hydroxide solution; and soaking and cleaning the natural cellulose fibers twice by using distilled water, and then putting the pretreated natural cellulose fibers into the distilled water (the mass ratio of the distilled water to the natural cellulose fibers is 20: 1). Then, a planetary ball mill is matched with a vertical corundum ball milling tank, and the pretreated natural cellulose fiber solution is ball milled for 60 minutes at the rotating speed of 400 r/min; and then filtering the ball-milled natural cellulose fiber by using a circulating water type multipurpose vacuum pump matched with medium-speed filter paper to obtain the modified natural cellulose fiber.
Water intrusion resistant cement slurry system 2:
540G of high-sulfate-resistance G-grade oil well cement, 60G of micro-silicon, 12G of fluid loss additive, 3G of dispersing agent, 0.5G of defoaming agent and 264G of water, wherein the mass is the modified natural cellulose fiber in the table 3.
Table 3 example 2 water intrusion resistant cement slurry system 2 performance test results
Figure BDA0003020360060000051
FIG. 3 is a graph of the water dispersion of example 2 with a modified cellulose fiber cement slurry system containing 1.2 g.
At normal temperature, 5mL of a newly-prepared water-invasion-resistant cement paste system 2 (containing 1.2g of modified natural cellulose fibers) is injected into a beaker containing 150mL of clear water by using an injector, the water-invasion-resistant cement paste system 2 (containing 1.2g of modified natural cellulose fibers) has no obvious dispersion phenomenon in the water, and the clear water in the beaker is transparent. Therefore, the natural cellulose fiber can better inhibit the dispersion phenomenon of cement slurry in water after ball milling modification, and the water invasion resistance of the well cementation cement slurry can be improved by utilizing the modified natural cellulose fiber.
Example 3
Water intrusion resistant cement slurry system 3: to verify the effect of the retarder on the water invasion resistant cement slurry system, the following experiments were performed.
540G of high-sulfate-resistance G-grade oil well cement, 60G of micro-silicon, 12G of fluid loss additive, 3G of dispersing agent, 1.2G (300r/min) of modified natural cellulose fiber, 0.5G of retarder, 0.5G of defoaming agent and 264G of water, wherein the mass is shown in the table 4.
Table 4 example 3 water intrusion resistant cement slurry system 3 performance test results
Figure BDA0003020360060000052
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (9)

1. The preparation method of the modified natural cellulose fiber is characterized by comprising the following steps:
1) preparing 0.1mol/L sodium hydroxide solution, heating the solution to 60 ℃, adding a part of untreated natural cellulose fibers into the sodium hydroxide solution, wherein the mass ratio of the solution to the natural cellulose fibers is 20: 1; stirring for 5 minutes at the rotating speed of 4000 r/minute by using a constant-speed stirrer; utilizing a circulating water type multipurpose vacuum pump to be matched with quick filter paper, filtering the stirred cellulose fibers, soaking the cellulose fibers in distilled water, and performing vacuum filtration twice to obtain pretreated natural cellulose fibers;
2) placing the pretreated natural cellulose fibers in a container, adding distilled water, stirring the distilled water and the fibers at a mass ratio of 20:1, and completely dispersing the treated natural cellulose fibers in the distilled water;
3) pouring the dispersion liquid into a vertical corundum alumina ball milling tank, putting corundum milling balls into the ball milling tank, and carrying out ball milling on pretreated cellulose fibers;
4) pouring out the ball-milled natural cellulose fiber solution, separating the grinding ball and the cellulose fibers, filtering the ball-milled natural cellulose fibers by using a circulating water type multipurpose vacuum pump matched with medium-speed filter paper, and collecting the cellulose fibers to obtain the modified natural cellulose fibers.
2. A modified natural cellulose fiber obtained by the production method according to claim 1.
3. The water invasion resistant well cementation cement slurry is characterized by comprising the following components in parts by weight: 100 parts of high sulfate-resistant G-grade oil well cement and admixture, 1.0-5.0 parts of fluid loss additive, 0.2-2.0 parts of dispersant, 0-1.0 part of retarder, 0.1-0.5 part of modified cellulose fiber according to claim 2, 0.05-0.1 part of defoamer and 40-50 parts of water.
4. The cement slurry for resisting water invasion and cementing according to claim 3, wherein the admixture is one or more of slag, fly ash, micro-silicon, quartz sand, silicon powder and glass beads.
5. The cement slurry for resisting water invasion according to claim 3, wherein the fluid loss agent is one or more of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide and acrylic acid copolymer.
6. The cement slurry for resisting water invasion and cementing according to claim 3, wherein the dispersant is acetone-formaldehyde polycondensate.
7. The cement slurry for resisting water invasion according to claim 3, wherein the retarder is a blend of polyhydroxy carboxylic acid and sulfonate.
8. The cement slurry for resisting water invasion and cementing according to claim 3, wherein the defoaming agent is tributyl phosphate.
9. The method for preparing a cement slurry for cementing wells resistant to water invasion as claimed in any one of claims 3 to 8, comprising the following steps:
weighing high sulfate-resistant G-grade oil well cement, an admixture, a fluid loss agent, 0.2-2.0 parts by weight of a dispersant, a retarder and modified cellulose fibers according to parts by weight, and dry-mixing the solid powder into a dry mixture;
then mixing the defoaming agent into water, pouring the aqueous solution into a constant speed stirrer, stirring at the rotating speed of 4000 +/-200 r/min, and pouring the dry mixture into the constant speed stirrer within 15 seconds; and then the rotating speed of the constant speed stirrer is increased to 12000 +/-500 r/min for continuously stirring for 35 seconds, and the water invasion resistant well cementation cement slurry is obtained.
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