CN114874404B - Environment-friendly oil well cement drag reducer with carbon nano tube tree structure and preparation method thereof - Google Patents
Environment-friendly oil well cement drag reducer with carbon nano tube tree structure and preparation method thereof Download PDFInfo
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- CN114874404B CN114874404B CN202210548011.8A CN202210548011A CN114874404B CN 114874404 B CN114874404 B CN 114874404B CN 202210548011 A CN202210548011 A CN 202210548011A CN 114874404 B CN114874404 B CN 114874404B
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 97
- 239000004568 cement Substances 0.000 title claims abstract description 65
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- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 47
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- 239000003129 oil well Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 15
- SZHIIIPPJJXYRY-UHFFFAOYSA-M sodium;2-methylprop-2-ene-1-sulfonate Chemical compound [Na+].CC(=C)CS([O-])(=O)=O SZHIIIPPJJXYRY-UHFFFAOYSA-M 0.000 claims abstract description 15
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 14
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- 238000006116 polymerization reaction Methods 0.000 claims abstract 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
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- 239000003999 initiator Substances 0.000 claims description 10
- 239000000178 monomer Substances 0.000 claims description 10
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- DGTOAFBVEDTEBA-UHFFFAOYSA-N sodium;prop-1-ene Chemical compound [Na+].[CH2-]C=C DGTOAFBVEDTEBA-UHFFFAOYSA-N 0.000 claims 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims 1
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- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract description 2
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- 230000000996 additive effect Effects 0.000 description 5
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- RECUKUPTGUEGMW-UHFFFAOYSA-N carvacrol Chemical compound CC(C)C1=CC=C(C)C(O)=C1 RECUKUPTGUEGMW-UHFFFAOYSA-N 0.000 description 5
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- 230000000052 comparative effect Effects 0.000 description 5
- WYXXLXHHWYNKJF-UHFFFAOYSA-N isocarvacrol Natural products CC(C)C1=CC=C(O)C(C)=C1 WYXXLXHHWYNKJF-UHFFFAOYSA-N 0.000 description 5
- 238000006073 displacement reaction Methods 0.000 description 4
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- -1 aldehyde ketone Chemical class 0.000 description 1
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- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
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- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
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- 238000002347 injection Methods 0.000 description 1
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
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- 238000009991 scouring Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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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
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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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/28—Friction or drag reducing additives
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- 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
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- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention discloses an environment-friendly oil well cement drag reducer with a carbon nano tube tree structure, which is prepared by the polymerization reaction of a carbon nano tube, acrylic acid, sodium methallylsulfonate and methallyl polyoxyethylene ether. The in-situ graft polymerization is carried out on the carbon nano tube to form a tree-shaped three-dimensional drag reducer molecular structure, the temperature resistance of the drag reducer is improved by utilizing the stable structure of the carbon nano tube and the high-energy C-C sigma bond in-situ grafting long side chains, and the drag reduction effect is prevented from being influenced by thermal degradation and hydrolysis under the high-alkalinity and high-temperature stratum environments of cement paste; and the sulfonic group is introduced into the side chain, and the strong electronegativity of the sulfonic group is utilized to improve the charge repulsion force of the sulfonic group, so that the dispersion and drag reduction effects of the cement paste are improved, and the temperature and salt resistance performance is improved. The drag reducer can be used for conventional well cementation and can also be used for well cementation of deep wells, ultra-deep wells and high-temperature and high-salt-content formations, and the preparation process of the drag reducer avoids the use of toxic and environment-polluted raw materials such as concentrated sulfuric acid, formaldehyde, acetone, naphthalene and the like in the production of the traditional drag reducer, so that the drag reducer is economic and environment-friendly.
Description
Technical Field
The invention relates to the technical field of oil and gas well cementation, in particular to an environment-friendly oil well cement drag reducer with a carbon nano tube tree-shaped structure and a preparation method thereof.
Background
Well cementation is a key link in the well construction process of oil and gas wells, and mainly aims to pack formation fluid, support a well wall and a casing, prevent the casing from being corroded, build a controllable oil and gas flow production channel and provide basic conditions for subsequent oil and gas well production increasing, reservoir transformation, well repair and other projects.
The primary purpose of well cementation is to pack formation fluid, in the well cementation engineering, cement slurry is injected into an annular space formed by a borehole and a casing, and the packing of the formation fluid is realized by utilizing the characteristics of dense solidification and interface cementation of the cement slurry. In well cementation, a cementing surface (called as a first cementing surface in engineering) formed by cement slurry and the outer wall of a metal casing and a cementing surface (called as a second cementing surface in engineering) formed by the cement slurry and a stratum (well wall) are formed, and the well cementation engineering requires that both interfaces have good cementing property and packing capacity. Good packing capacity is achieved by good cementation provided that the cementation interface is clean and the cementing material is in sufficient contact with the interface. Before cementing, the mud adheres to the outer wall of the casing already during running into the casing of the wellbore, and a mud filter cake is already formed on the wall of the wellbore during drilling. Mud and mud filter cake are materials without cementation, and the residue of the mud and the mud filter cake on two interfaces seriously influences the cementation capability of the cement slurry and the two interfaces, thereby influencing the well cementation quality, the service life of an oil well and the development benefit of the oil field.
The main means for ensuring the packing property of a cement slurry solidified body to a stratum and the well cementation quality is to improve the replacement efficiency of the cement slurry to the slurry and a slurry filter cake in the well cementation and water injection process. According to the theory of rheology, the fluid has three flow states of plug flow, laminar flow and turbulent flow. Wherein, the energy of turbulent flow state is high, the scouring energy is strong, the displacement efficiency is high. The cement slurry is a high-concentration solid (cement particle) suspension dispersion system, has higher viscosity and shear force, and makes the cement slurry difficult to realize turbulent flow displacement in well cementation. The oil well cement drag reducer is an additive which is added into a well cementing cement slurry system to reduce the viscosity and the shearing force of the cement slurry. The drag reducer is added into the oil well cement slurry system, which is beneficial to realizing turbulent flow displacement under lower discharge capacity or having higher turbulent flow degree under the same discharge capacity in engineering, thereby improving the displacement efficiency and the well cementation quality.
On the one hand, with the reduction of shallow oil and gas resources and the development of oil and gas exploration and development technologies, the oil and gas exploration and development technologies develop towards deep high-temperature strata, the temperature of the strata encountered by drilling is higher and higher, and the situations of the stratum encountered by drilling in special strata such as a salt-gypsum layer, a brine layer and the like are more and more. On the other hand, the environmental protection requirements in the construction engineering process are higher and higher. Therefore, the oil well cement drag reducer is required to have environment-friendly characteristics in addition to high drag reduction capability and high temperature and salt resistance capability. The development of the environment-friendly oil well cement drag reducer with excellent performance is an urgent need in the field of oil and gas field development.
Disclosure of Invention
The invention aims to provide an environment-friendly oil well cement drag reducer with a carbon nano tube tree structure, which can be applied to the well cementation of deep wells, ultra-deep wells and high-temperature and high-salt-content stratums.
The invention provides an environment-friendly oil well cement drag reducer which is a drag reducer with a tree-shaped three-dimensional structure formed by in-situ graft polymerization on a carbon nano tube. The molecular structural formula of the drag reducer is as follows:
in the formula, the structure of the graft polymer chain is as follows:
the preparation method of the environment-friendly oil well cement drag reducer with the carbon nano tube tree structure comprises the following steps:
(1) The weight percentage is as follows: 0.100 to 0.150 percent of carbon nano tube, 12.0 percent of Acrylic Acid (AA), 5.0 percent of sodium Methallylsulfonate (MAS) and 82.9 percent of methallyl polyoxyethylene ether (TPEG, the molecular weight is 1200 to 2400), and all the raw materials are weighed; the water is obtained according to the total mass of the four raw materials and the water = 40: 60.
(2) Adding 65.0% of the water weighed in the step (1) into a reaction kettle, slowly adding the carbon nano tubes weighed in the step (1) into the reaction kettle under high-speed stirring, and stirring for 30min to fully disperse the carbon nano tubes;
(3) Adding the MAS and TPEG monomers weighed in the step (1) into the reaction kettle in the step (2) under medium-speed stirring, stirring for 10-15 min, and fully dissolving;
(4) Adding 25.0% of water weighed in the step (1) into a feeding tank (I), adding the monomer AA weighed in the step (1) into the feeding tank (I), stirring for 10min, and fully dissolving for later use;
(5) Adding the remaining 10.0% of the water weighed in the step (1) into a feeding tank (II), weighing initiator ammonium persulfate according to 2.0-2.5% of the mass of the three monomers weighed in the step (1), adding into the feeding tank (II), stirring for 10min, and fully dissolving for later use;
(6) Heating the reaction kettle and the raw materials in the step (3) to 50 +/-2 ℃ under stirring;
(7) Dropwise adding the raw materials prepared in the steps (4) and (5) into the reaction kettle from two different feed inlets respectively, wherein the dropwise adding speed is 55-60 min; keeping the temperature at 50 +/-2 ℃ in the dropping process;
(8) After the step (7) is finished, the reaction kettle is heated to 60-65 ℃ for reaction for 4 hours;
(9) Adding 40% of naoh solution to the reaction kettle, adjusting the solution pH = 7.0-8.0;
(10) Cooling to below 30 deg.C, and discharging to obtain the product solution.
The reaction principle for preparing the drag reducer is as follows:
compared with the prior art, the invention has the advantages that:
(1) The drag reducer has a tree-like three-dimensional structure, improves the temperature resistance of the drag reducer by utilizing the stable structure of the carbon nano tube and the in-situ grafting of the high-energy C-C sigma bond long side chain, and avoids the influence of thermal degradation and hydrolysis on the drag reduction effect under the high-alkalinity and high-temperature stratum environments of cement paste. The sulfonic group is introduced into the side chain, the strong electronegativity of the sulfonic group is utilized to improve the charge repulsion force of the sulfonic group so as to improve the dispersion and drag reduction effects of the cement paste, and the adsorptivity of the sulfonic group is improved to enhance the temperature and salt resistance of the drag reducer. The drag reducer has wide temperature range, can be suitable for medium and low temperature well cementing cement slurry systems, and can also be suitable for high temperature and ultrahigh temperature deep well cementing cement slurry systems. Meanwhile, the cement slurry has good salt resistance, and can be suitable for well cementing cement slurry systems with high salinity and saturated salt water.
(2) On the basis of reducing the viscosity and the shearing force of cement particles by dispersing the cement particles by the repulsion of negative charge groups, the drag reduction effect of the drag reducer is further improved by utilizing the steric hindrance effect of the long branched chain with the tree structure. Has high-efficiency drag reduction effect on pure cement slurry systems and cement slurry systems with various engineering formulas.
(3) Acrylic Acid (AA) with low toxicity, sodium Methallylsulfonate (MAS), methallyl polyoxyethylene ether and nontoxic carbon nanotubes are used as main raw materials, so that toxic and environment-pollution-large raw materials such as concentrated sulfuric acid, formaldehyde, acetone, naphthalene and the like used in the production of the traditional drag reducer are avoided, and the environmental friendliness in the production is ensured; polyether long chains with low biotoxicity and good degradability in the environment are used as dendritic branched chain monomers to meet the requirement of environmental protection; the product has no toxic substance residue, and has no influence on human health in use.
(4) The drag reducer product has good compatibility with other common oil field cement additives, and has no adverse effect on the performances of the cement paste system required by well cementation engineering, such as stability, thickening time, strength and the like.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
Fig. 1 is an infrared spectrum of the oil well cement drag reducer of example 1.
Fig. 2 shows a raman spectrum of the drag reducer of example 1.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1
Producing 1000kg drag reducer comprising the steps of:
(1) Weighing: carbon nanotubes (MWNTs), 0.400kg; sodium Methallylsulfonate (MAS), 20.0kg; methallyl polyoxyethylene ether (TPEG, molecular weight 2400), 332.0kg; acrylic Acid (AA), 48.0kg; 600.0kg of pure water;
(2) 390.0kg of water weighed in the step (1) is added into a reaction kettle, the carbon nano tube weighed in the step (1) is slowly added into the reaction kettle under high-speed stirring, and the mixture is stirred for 30min to be fully dispersed;
(3) Adding 20.0kg of MAS, 332.0kg of TPEG monomer raw materials and 400kg of water weighed in the step (1) into the reaction kettle in the step (2) under medium-speed stirring, and stirring for 10-15 min for full dissolution;
(4) Adding 150.0kg of water weighed in the step (1) into a feeding tank (I), adding 48.0kg of AA raw material weighed in the step (1) into the feeding tank (I), stirring for 10min, and fully dissolving for later use;
(5) Adding 60kg of water weighed in the step (1) into a feeding tank (II); weighing 8.00kg of initiator ammonium persulfate, adding into a feeding tank (II), stirring for 10min, and fully dissolving for later use;
(6) Heating the raw materials in the reaction kettle in the step (3) to 50 +/-2 ℃ under stirring;
(7) Respectively dripping the raw materials prepared in the steps (4) and (5) into the reaction kettle in the step (6) from two different feed inlets, wherein the dripping speed is controlled to be 55-60 min; keeping the temperature at 50 +/-2 ℃ in the dropping process;
(8) After the step (7) is finished, the reaction kettle is heated to 60-65 ℃ for reaction for 4 hours;
(9) Adding 40% of naoh solution to the reaction kettle, adjusting the solution pH = 7.0-8.0;
(10) Cooling to below 30 deg.C, and discharging to obtain the product solution.
Example 2
1000kg of drag reducer was produced by the same procedure as in example 1, except that the initiator, ammonium persulfate, was used in an amount of 10.0kg.
Example 3
1000kg of drag reducer was produced by the same procedure as in example 1, except that the molecular weight of methallyl polyoxyethylene ether TPEG was 1200 and the amount of ammonium persulfate used as the initiator was 10.0kg.
Example 4
1000kg of drag reducer was produced by the same procedure as in example 1, except that the amount of carbon nanotubes (MWNTs) was 0.600kg.
Example 5
1000kg of drag reducer is produced, and the preparation method has the same steps as example 1, except that the amount of carbon nanotubes (MWNTs) is 0.600kg; the molecular weight of the methallyl polyoxyethylene ether TPEG is 1200; the initiator ammonium persulfate dosage is 10.0kg.
Example 6
1000kg of drag reducer is produced, and the preparation method has the same steps as example 1, except that the amount of carbon nanotubes (MWNTs) is 0.600kg; the molecular weight of the methallyl polyoxyethylene ether TPEG is 1200.
And (3) performance testing:
1. characterization of infrared spectrum structure of drag reducer
The drag reducer prepared in example 1 of the present invention was dried and ground, and its molecular structure was characterized by using a WQF-520 fourier transform infrared spectrometer using a KBr tabletting method, and the results are shown in fig. 1. In the figure, 3450cm -1 The broad peak mainly adsorbs the stretching vibration peak of water molecules O-H; 2931cm -1 Is a polyether chain C-H stretching vibration peak; 1713cm -1 C = O stretching vibration peak in carbonyl; 1643cm -1 C = C of the carbon nanotube stretching peak; 1460cm -1 Is a vibration peak of stretching of COO oxygen atoms, 1413cm -1 is-CH 2 Peak of flexural vibration of-1192 cm -1 Is a oscillation peak of the COO oxygen atom of 1122cm -1 Is the C-O-C ether bond shock peak, 1046cm -1 And 664cm -1 Peak of stretching vibration of-S-O-, 832cm -1 Out-of-plane vibration absorption peaks for the carboxylic acid hydroxyl groups; 720cm -1 The absorption peak at (A) is mainly the in-plane vibration of the-CH-of the carbon nanotube. Infrared spectrum analysis shows that: characteristic infrared spectrum peaks of four raw materials of MWNTs, AA, MAS and TPEG all appear in a sample, and the sample is an in-situ graft copolymer of a carbon nano tube and three monomers.
2. Drag reducer raman spectral characterization
The raman spectrum of a carbon nanotube mainly has two spectral bands: g belt (1500-1605 cm) -1 ) And D belt (1250-1450 cm) -1 ) The G band represents the C = C tangential stretching vibration in the carbon nanotube, and the D band and sp in the hexagonal framework of the carbon nanotube 3 Scattering of the hybridized carbon is relevant. After the grafting reaction, the C = C structure in the carbon nano tube is converted into a C-C structure, namely sp of carbon 2 Hybridization to carbon sp 3 Hybridization, therefore, the intensity ratio of the D band and the G band (I) D /I G ) The value is an important index of the in-situ grafting degree of the carbon nano tube. The raman spectral characterization of the drag reducer of example 1 of the present invention is shown in fig. 2. As can be seen from the figure: i of pure carbon nanotubes (MWNTs) D /I G About 2.40, and I of a carbon nanotube graft polymer (biopolymer) D /I G About 2.46. D band decrease, G band increase, sp 2 Reduction of the relative amount of hybridized carbon, sp 3 The increase in the relative amount of hybridized carbon further illustrates the in situ graft polymerization of the monomers on the carbon nanotubes via covalent bonds.
3. Application properties of drag reducers
The performance of the drag reducers of examples 1 to 6 was evaluated according to SY/T5504.3-2008 "evaluation method for oil well Cement admixtures" (section 3: drag reducer). The compatibility of the drag reducer and the performance of other cement paste systems are tested by referring to GB/T19139-2012 oil well cement test method.
(1) Drag reducing Properties of the drag reducer products of examples 1-6
The formula of the cement paste is as follows: 792.0G jiahua (HSR) grade G well cement +11.88G (40% solution) drag reducer (product of examples 1-6) + water (W/C = 0.44). The rheological properties were measured at 85 ℃ under atmospheric thickening for 20min and the results are given in Table 1.
Results of performance tests on drag reducers prepared in examples 1 to 6 in Table 1
The experimental results in Table 1 show that the drag reducing agent of the invention has drag reducing effect satisfying SY/T5504.3-2008 stipulated that n is more than 0.5, K is less than 0.7 Pa.n s The requirements of (1).
(2) Drag reduction performance of drag reducer of example 1 at medium and low temperature
The formula of the cement paste is as follows: 792.0G carvacrol (HSR) grade G well cement +11.88G (40% solution) drag reducer (product of example 1) + water (W/C = 0.44). The rheological properties were measured at different experimental temperatures for 20min at atmospheric thickening time and the results are given in table 2.
TABLE 2 Performance test results of drag reducers at different temperatures
The experimental results in Table 2 show that the drag reducing agent of the invention has drag reducing effect satisfying SY/T5504.3-2008 stipulated that n is more than 0.5, K is less than 0.7 Pa.n s The requirements of (1).
(3) Drag reduction performance of drag reducer of example 1 under high temperature conditions
Thickening the cement paste for 20min at different experimental temperatures by using high temperature and high pressure, and then cooling to 90 ℃ to measure the rheological property of the cement paste.
The experimental formula at 120 ℃ is as follows: 792.0G jiahua (HSR) grade G well cement +11.88G (40% solution) drag reducer (example 1 product) +2.40G retarder BS200R + water (W/C = 0.44).
The experimental formula at 150 ℃ is as follows: 792.0G carvacrol (HSR) grade G well cement +11.88G (40% solution) drag reducer (example 1 product) +11.88G retarder BS200R + water (W/C = 0.44).
The experimental formula at 180 ℃ is as follows: 792.0G carvacrol (HSR) grade G well cement +11.88G (40% solution) drag reducer (example 1 product) +39.60G retarder BS200R + water (W/C = 0.44).
The test results are shown in Table 3.
TABLE 3 drag reducer Performance test data sheet at different temperatures (high temperatures)
The experimental results of table 3 show that: the drag reducer has excellent drag reduction effect in a high temperature range of 120-180 ℃, and meets the requirements specified in SY/T5504.3-2008.
Comparative example: a drag reducer was prepared as a comparative sample by removing the addition of carbon nanotubes on the basis of example 1 and the other steps were identical. The drag reduction performance of the comparative samples was tested at high temperature in the same manner as described above. The test results are shown in Table 4.
TABLE 4 TABLE of experimental data of drag reducer performance at different temperatures (high temperature) for drag reducer of comparative example
Comparing table 3 and table 4, it can be seen that when the drag reducer in the comparative example (without the carbon nanotube) is in the high temperature range of 120 ℃ to 180 ℃, although n meets the standard requirement, the value of n is significantly reduced compared to scheme 1; the K value can meet the standard requirement under the condition of 120, but the K value is greatly increased, and the K value can not meet the standard requirement under the conditions of 150 ℃ and 180 ℃; the high bond energy grafting of the carbon nano tube and the three-dimensional structure of the drag reducer are proved to have obvious improvement effect on the temperature resistance and drag reduction performance of the product.
(4) Salt resistance of drag reducer of example 1
The formula of the cement paste comprises: 792.0G jiahua (HSR) grade G well cement +11.88G (40% solution) drag reducer (product of example 1) + NaCl + water (W/C = 0.44). The rheological properties were measured at 85 ℃ for a period of 20min at atmospheric thickening and the results are given in Table 5.
TABLE 5 Performance test results for drag reducers at different salt loadings
The experimental results of table 5 show that: the drag reducer has excellent salt resistance, can adapt to a saturated saline water cement slurry system, and meets the requirements specified in SY/T5504.3-2008.
(5) Engineering properties of drag reducers
(1) Compatibility of the drag reducer with fluid loss additives of example 1
Selecting a biological glue type fluid loss agent BS100, a cellulose fluid loss agent SZ1-2 and a synthetic polymer type fluid loss agent BS100L-G. The engineering formula of the cement paste is as follows: 792.0G carvacrol (HSR) grade G oil well cement +11.88G (40% solution) drag reducer (product of example 1) + fluid loss additive +3.96G retarder BS200R + water (W/C = 0.44). The rheological property and the water loss property of the product are measured at 85 ℃ under normal pressure thickening time of 20min, and the experimental results are shown in Table 6.
TABLE 6 Experimental data on the effect of different types of fluid loss additives on the performance of drag reducers
Experimental results show that the drag reducer has excellent drag reduction effect in an engineering formula and meets the requirements of standards on drag reduction performance; the drag reducer has excellent adaptability with the common fluid loss additive in the engineering formula, and has no adverse effect on the performance of the fluid loss additive.
(2) Compatibility of drag reducer with retarder of example 1
The engineering formula of the cement paste is formed by selecting compound organic phosphate retarder BS200, compound polyhydroxy carboxylic acid retarder BS200R and compound polymer retarder SN-3: 792.0G carvacrol (HSR) grade G oil well cement +11.88G (40% solution) drag reducer (product of example 1) +39.6G fluid loss additive BS100L-G + retarder + water (W/C = 0.44). The rheological properties were measured at 85 ℃ for 20min of thickening time at atmospheric pressure and at 120 ℃ for the thickening time, the results of the experiments being given in Table 7.
TABLE 7 Experimental data sheet for the effect of different types of retarders on the performance of drag reducers
The experimental results in table 7 show that the drag reducer of the present invention has excellent drag reduction effect in the engineering formulation, and meets the requirements of the standards on drag reduction performance; the drag reducer has excellent adaptability with common retarder in engineering formula.
(6) Toxicity test of drag reducer
A third-party detection mechanism (Shanghai chemical institute detection and validation Co.) was entrusted to perform an experiment on the toxicity of the drag reducer prepared in the embodiments 1 to 6 of the present invention, and the experimental results show that the drag reducer of the present invention: acute oral toxicity LD 50 Values > 2000mg/kg (white mice). It is low-toxic or non-toxic.
(7) Experiment of degradability of drag reducer
A third party organization (environmental laboratory of chemical industry institute of chemical and chemical university, southwest) was entrusted to measure the chemical oxygen demand and the biological oxygen demand of the drag reducer of example 1, and the experimental results are shown in tables 8 and 9.
TABLE 8 reference evaluation chart for biodegradability of wastewater
| BOD 5 COD value | ＞0.45 | 0.30-0.45 | 0.20-0.30 | ＜0.20 |
| Biodegradability assessment | Good taste | Is better | Is difficult to | It is not suitable for |
TABLE 9 Biochemical evaluation test result table for drag reducer sample
The experimental results show that: compared with the commonly used sulfonated aldehyde ketone condensate drag reducer, the oil well cement drag reducer of the invention has better biodegradability.
Although the present invention has been described with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the present invention.
Claims (7)
1. An environment-friendly oil well cement drag reducer with a carbon nano tube tree structure is characterized in that the molecular structural formula of the drag reducer is as follows:
wherein the grafted polymer chain has the following structural formula:
the drag reducer is prepared by the polymerization reaction of carbon nano tubes, acrylic acid, sodium methallylsulfonate and methallyl polyoxyethylene ether; the mass percentage of each raw material component is as follows:
0.100% of carbon nano tube, 12.0% of acrylic acid, 5.00% of sodium methallyl sulfonate, 82.9% of methallyl polyoxyethylene ether, and the total mass percentage of the four raw materials is 100%.
2. The preparation method of the environment-friendly oil well cement drag reducer with the carbon nanotube tree structure as defined in claim 1, wherein the drag reducer is prepared by polymerization reaction of carbon nanotubes, acrylic acid, sodium methallylsulfonate and methallyl polyoxyethylene ether; the preparation steps are as follows:
s1, dispersing a carbon nano tube in water, and then adding sodium methallylsulfonate and methallyl polyoxyethylene ether to obtain a solution A;
s2, dropwise adding an acrylic acid aqueous solution and an initiator aqueous solution into the solution A at a speed of 55-60 min; and (3) keeping the temperature at 50 +/-2 ℃ in the dripping process, heating to 60-65 ℃ after dripping is finished, reacting for 4 hours, adding a sodium hydroxide solution after the reaction is finished, adjusting the pH to be 7.0-8.0, and cooling to obtain the drag reducer.
3. The method for preparing the carbon nanotube tree-structured environment-friendly oil well cement drag reducer as claimed in claim 2, wherein the ratio of the total mass of the four raw materials to the total amount of water is 4: 6.
4. The method for preparing the carbon nanotube tree-structured environment-friendly oil well cement drag reducer according to claim 3, wherein the step S1 comprises the following steps:
adding water with the total water amount of 65.0 percent into a reaction kettle, slowly adding the carbon nano tube into the reaction kettle under high-speed stirring, and stirring for 30min to fully disperse the carbon nano tube; then adding the methyl allyl sodium sulfonate and the methyl allyl polyoxyethylene ether monomer into the reaction kettle under the condition of medium-speed stirring, stirring for 10-15 min, and fully dissolving to obtain a solution A.
5. The method for preparing the carbon nanotube tree-structured environment-friendly oil well cement drag reducer according to claim 4, wherein the step S2 is as follows:
taking water with the total water amount of 25.0%, adding an acrylic acid monomer, and stirring to fully dissolve to obtain an acrylic acid aqueous solution; adding initiator ammonium persulfate into the rest 10.0 percent of water, and stirring to fully dissolve to obtain initiator aqueous solution;
respectively dripping an acrylic acid aqueous solution and an initiator aqueous solution into the solution A from two feed inlets of the reaction kettle at the same time, wherein the dripping speed is controlled to be 55-60 min; and (3) keeping the temperature at 50 +/-2 ℃ in the dripping process, heating to 60-65 ℃ after dripping is finished, reacting for 4 hours, adding a sodium hydroxide solution after the reaction is finished, adjusting the pH to be 7.0-8.0, and cooling to obtain the drag reducer.
6. The method for preparing the carbon nanotube tree-structured environment-friendly oil well cement drag reducer as defined in claim 5, wherein the amount of the initiator is 2.0-2.5% of the total mass of the three monomers of acrylic acid, sodium methallylsulfonate and methallyl polyoxyethylene ether.
7. The method for preparing the carbon nanotube tree-structured environment-friendly oil well cement drag reducer according to claim 6, wherein the molecular weight of the methallyl polyoxyethylene ether is 1200 to 2400.
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| CN111218263A (en) * | 2020-02-27 | 2020-06-02 | 成都欧美克石油科技股份有限公司 | Novel drag reducer for oil well cement and preparation method thereof |
| CN113024747A (en) * | 2021-03-30 | 2021-06-25 | 西南石油大学 | Hyperbranched polymer based on carbon nano tube and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108794696A (en) * | 2017-04-27 | 2018-11-13 | 中国石油天然气集团公司 | A kind of drag reducer, preparation method and applications |
| CN108794697A (en) * | 2017-04-27 | 2018-11-13 | 中国石油天然气集团公司 | A kind of drag reducer, preparation method and applications |
| CN110003409A (en) * | 2019-04-29 | 2019-07-12 | 西南石油大学 | A kind of carbon nano-tube hybridization Heat Resistant and Salt Tolerant Polymer and preparation method thereof |
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| CN111218263A (en) * | 2020-02-27 | 2020-06-02 | 成都欧美克石油科技股份有限公司 | Novel drag reducer for oil well cement and preparation method thereof |
| CN113024747A (en) * | 2021-03-30 | 2021-06-25 | 西南石油大学 | Hyperbranched polymer based on carbon nano tube and preparation method thereof |
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