CN104927799A - Carbon nano-tube complex thickener and preparation method thereof - Google Patents
Carbon nano-tube complex thickener and preparation method thereof Download PDFInfo
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
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Abstract
The invention discloses a carbon nano-tube complex thickener and a preparation method thereof. The carbon nano-tube complex thickener comprises the following substances in percentage by mass: 1-5% of a viscoelastic surfactant, 0.05-0.4% of modified carbon nano-tube particles, 0-8% of a countra-ion salt, 0-3% of an additive, and the balance of water, wherein the total proportion is 100%. According to the preparation method, the carbon nano-tube complex thickener can be prepared by uniformly mixing and stirring such components. The carbon nano-tube complex thickener has the advantages of being low in carbon nano-tube and surfactant consumption, relatively high in viscoelasticity and temperature resistance, shearing resistance and leak-off resistance properties, and simple in preparation method, and can be applied to the fields of acidizing fluids, fracturing fluids, drilling fluids and sand control fluids for oil-gas field development as well as water shut-off and profile control.
Description
Technical field
The present invention relates to oil-gas field development technical field, particularly a kind of carbon nanotube complex thickener and preparation method thereof.
Background technology
Gelled fluid is applied very extensive in oil-gas field development, and can be used for the aspects such as drilling well, completion, pressure break, acidifying, sand control and water plugging and profile controlling, is a kind of important oilfield working fluids.Tradition gelled fluid common polymer thickening material is formulated, but because it is containing residue residue, formation permeability injury is comparatively large, has higher friction pressure in addition, limits the further application of polymer gelled fluid.In recent years, viscoelastic surfactant fluids system receives much attention due to the thickening character of its uniqueness, is widely used in frscturing working fluid.It forms vermiform by special surface active agent and is wound around reticulated structure in water, compares general polymer and has better solid particulate suspension property.This system as small molecules associating system, also have anti-shearing, without residue, the formation injury excellent properties such as little.But, in conventional viscoelastic surfactant fluids system, dosage of surfactant is larger, general chemical agent cost is higher than traditional polymeric system, in addition its temperature tolerance poor and in middle and high infiltration reservoir the shortcomings such as filter loss is large, limit its application at the scene.
In order to solve the problem that conventional viscoelastic surfactant gelled fluid system temperature tolerance is poor, consumption is large, general adopt developed recruit more in the past, as long-chain or double type tensio-active agent, but there is composition principle and preparation technology is comparatively complicated, and price is higher, product universality is poor and have impact on applying in oil field.
People have developed again nanometer plan crosslinking technological in recent years, by nano material and the composite obtained gelled fluid of viscoelastic surfactant, the surface properties utilizing nano particle special and high surface, formed the plan cross-linked structure of two dimension by adsorption and electrostatic interaction and tensio-active agent vermiculate glues, be conducive to viscoelastic property and the heat resistance of improvement system.This system can form pseudo-filter cake on Reservoir rocks surface simultaneously, reduces the filter loss of liquid, and the filter cake formed easily broken glue return row, can not stratum be injured.In numerous nano material, carbon nanotube (CNT) and derivative thereof, owing to having high specific surface area, excellent electrical properties and unusual mechanical property, more and more receive the concern of people.Exactly because these advantages make carbon nanotube have great application in special material and oil-gas field development etc.Existing result of study display Chinese patent CN201410355821.7 discloses a kind of fracturing liquid containing CNT (carbon nano-tube) and viscoelastic anionic tensio-active agent, CNT (carbon nano-tube) and viscoelastic anionic tensio-active agent compound is adopted in patent, can significantly improve of the fracturing fluid viscoelastic property and heat resistance, make of the fracturing fluid filter loss obviously reduce simultaneously.
Obviously, this novel nano-material of carbon nanotube has the advantage of uniqueness for negatively charged ion viscoelastic surfactant class viscosifying agent improved performance aspect, but find in application process the carbon nanotube that uses at present due to dispersiveness poor, effective concentration is low, in addition function of surface functional group kind is single, can not the excellent properties of abundant carbon nanotube, cause carbon nanotube large usage quantity, add viscosifying agent cost.In addition, due to the negatively charged ion viscoelastic surfactant viscosifying agent limitednumber that market is applied, how to utilize carbon nanotube to improve positively charged ion, both sexes class viscoelastic surfactant multiviscosisty performance, expanding the range of application of such viscosifying agent, is also a problem urgently to be resolved hurrily at present.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, the object of the present invention is to provide a kind of carbon nanotube complex thickener and preparation method thereof, this carbon nanotube complex thickener adopts modified carbon nano tube tube material, effectively can play the improvement effect to viscoelastic surfactant fluids performance of carbon nanotube, be characterized in carbon nanotube and dosage of surfactant is low, preparation is simple, excellent performance.
In order to achieve the above object, technical scheme of the present invention is as follows:
A kind of carbon nanotube complex thickener, it is as follows that raw material composition presses mass percent:
Described modified multiwalled carbon nanotube be technical grade carbon nanotube in the NaOH solution of 2mol/L, 90-110 DEG C of reflux 2h, is cooled to room temperature, and filtration washing is to neutral, and at 100 DEG C, dry 2h obtains pretreated carbon nanotube product; Gained pre-treatment product again through volume ratio be the concentrated nitric acid of 3:1 and the vitriol oil in 50-70 DEG C of reflux 0.5h, be cooled to room temperature, filtration washing is to neutral, and at 100 DEG C, dry 2h obtains modified multiwalled carbon nanotube product.This modified multiwalled carbon nanotube material diameter is less than 5nm, and length is less than 2 μm, and finishing has great amount of hydroxy group, carboxylated hydrophilic functional group, favorable dispersity in water, and can keep stable 20h, in surfactant soln, steady time is longer.
Described tensio-active agent is: cats product alkyl quaternary ammonium salts, alkyl carbon chain lengths 16-22; Or anion surfactant fatty acid acyl amido sulfonate sodium, Sulfonated Fatty Acid Methyl Ester, fatty acid chain length is 18-22; Or amphoterics alkyl betaine, alkylamide propyl-betaine, alkyl carbon chain lengths is 18-22.
Described gegenion salt is the one in sodium salicylate, sodium-chlor, Repone K, ammonium chloride.
Described auxiliary agent is the one in lauryl alcohol, sodium lauryl sulphate.
The preparation method of above-mentioned carbon nanotube complex thickener is as follows:
Be configured to the aqueous solution by the stirring that to be added to the water by tensio-active agent of following mass percent proportioning under normal temperature, then add carbon nanotube particulate, gegenion salt and auxiliary agent successively, stir, carbon nanotube complex thickener can be obtained:
Modified multiwalled carbon nanotube 0.05-0.4%; Tensio-active agent 1-5%; Gegenion salt 0-8%;
Auxiliary agent 0-3%; Water surplus.
The know-why of institute of the present invention foundation:
The present invention adopt tensio-active agent can form vermiculate glues winding arrangement in water, after adding modified carbon nano tube tube particle, carbon nanotube particle and vermiculate glues generation crosslinked action, can the netted micellar structure of formative dynamics as Fig. 1 model, improve the mechanical property of compound system; The function functional group such as hydroxyl, carboxyl that modified carbon nano tube tube-surface is introduced simultaneously has the effect improving crosslinking degree.In addition, add further growth and the viscoelastic improvement of system of appropriate gegenion salt and the favourable vermiculate glues of auxiliary agent, rely on these synergies effectively can improve the heatproof of viscoelastic surfactant viscosifying agent, resistant to shearing and anti-filtration property.
The present invention compared with prior art has the following advantages: the present invention adopt the carbon nanotube of modification and viscoelastic surfactant composite, carbon nanotube and dosage of surfactant few, greatly reduce the cost of viscosifying agent; In addition, the selectable kinds of surfactants of carbon nanotube complex thickener of the present invention greatly increases, and includes conventional positively charged ion and both sexes class viscoelastic surfactant, further increases suitability and the range of application of this technology.
Accompanying drawing explanation
Fig. 1 is viscoelastic surfactant micella and modified carbon nano tube tube particle crosslinking structure model.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment one
Present embodiments provide a kind of carbon nanotube complex thickener, be calculated in mass percent,
Preparation method is as follows:
Be configured to the aqueous solution by the stirring that to be added to the water by palmityl trimethyl ammonium chloride of above proportioning under normal temperature, then add carbon nanotube particulate and gegenion salt successively in proportion, stir, carbon nanotube complex thickener can be obtained.Adopt MCR102 rheometer test 100s
-1viscosifying agent viscosity during lower differing temps is as shown in table 1.
The viscosity table of table 1. differing temps lower surface promoting agent and modified carbon nano-tube compound system
As can be seen from the table, add a small amount of modified carbon nano tube tube material in viscoelastic surfactant fluids after, the viscosity increasing degree of compound system is remarkable, and heat resistance is also significantly improved.
Embodiment two
Present embodiments provide a kind of carbon nanotube complex thickener, be calculated in mass percent,
Preparation method is as follows:
Be configured to the aqueous solution by the stirring that octadecyl trimethyl ammonium chloride to be added to the water of above proportioning under normal temperature, then add carbon nanotube particulate and gegenion salt successively in proportion, stir, carbon nanotube complex thickener can be obtained.Adopt MCR102 rheometer test 100s
-1viscosifying agent viscosity during lower differing temps is as shown in table 2.
The viscosity table of table 2. differing temps lower surface promoting agent and modified carbon nano-tube compound system
As can be seen from the table, add a small amount of modified carbon nano tube tube material in viscoelastic surfactant fluids after, the viscosity increasing degree of compound system is remarkable, and heat resistance is also significantly improved.
Embodiment three
Present embodiments provide a kind of carbon nanotube complex thickener, be calculated in mass percent,
Preparation method is as follows:
Be configured to the aqueous solution by the stirring that to be added to the water by erucicamide base sodium sulfonate of above proportioning under normal temperature, then add carbon nanotube particulate, gegenion salt and auxiliary agent successively in proportion, stir, carbon nanotube complex thickener can be obtained.Adopt MCR102 rheometer test 100s
-1viscosifying agent viscosity during lower differing temps is as shown in table 3.
The viscosity table of table 3. differing temps lower surface promoting agent and modified carbon nano-tube compound system
| Temperature (DEG C) | 3%LA-22+6% chlorination | 3%LA-22+6% Repone K+2% lauryl alcohol+ |
| Potassium+2% lauryl alcohol | 0.15% modified carbon nano-tube | |
| 30 | 410 | 436 |
| 40 | 356 | 408 |
| 50 | 195 | 384 |
| 60 | 153 | 267 |
| 70 | 44 | 133 |
| 80 | 23 | 81 |
| 90 | — | 35 |
As can be seen from the table, add a small amount of modified carbon nano tube tube material in viscoelastic surfactant fluids after, the viscosity increasing degree of compound system is remarkable, and heat resistance is also significantly improved.
Embodiment four
Present embodiments provide a kind of carbon nanotube complex thickener, be calculated in mass percent,
Preparation method is as follows:
Be configured to the aqueous solution by the stirring that to be added to the water by methyl sodiosul foaliphatate of above proportioning under normal temperature, then add carbon nanotube particulate and gegenion salt successively in proportion, stir, carbon nanotube complex thickener can be obtained.Adopt MCR102 rheometer test 100s
-1viscosifying agent viscosity during lower differing temps is as shown in table 4.
The viscosity table of table 4. differing temps lower surface promoting agent and modified carbon nano-tube compound system
As can be seen from the table, add a small amount of modified carbon nano tube tube material in viscoelastic surfactant fluids after, the viscosity increasing degree of compound system is remarkable, and heat resistance is also significantly improved.
Embodiment five
Present embodiments provide a kind of carbon nanotube complex thickener, be calculated in mass percent,
Preparation method is as follows:
Be configured to the aqueous solution by the stirring that to be added to the water by octodecyl betaine of above proportioning under normal temperature, then add carbon nanotube particulate, gegenion salt and auxiliary agent successively in proportion, stir, carbon nanotube complex thickener can be obtained.Adopt MCR102 rheometer test 100s
-1viscosifying agent viscosity during lower differing temps is as shown in table 5.
The viscosity table of table 5. differing temps lower surface promoting agent and modified carbon nano-tube compound system
As can be seen from the table, add a small amount of modified carbon nano tube tube material in viscoelastic surfactant fluids after, the viscosity increasing degree of compound system is remarkable, and heat resistance is also significantly improved.
Embodiment six
Present embodiments provide a kind of carbon nanotube complex thickener, be calculated in mass percent,
Preparation method is as follows:
Be configured to the aqueous solution by the stirring that amine hydroxybenzene CAB to be added to the water of above proportioning under normal temperature, then add carbon nanotube particulate and auxiliary agent in proportion successively, stir, carbon nanotube complex thickener can be obtained.Adopt MCR102 rheometer test 100s
-1viscosifying agent viscosity during lower differing temps is as shown in table 6.
The viscosity table of table 6. differing temps lower surface promoting agent and modified carbon nano-tube compound system
As can be seen from the table, add a small amount of modified carbon nano tube tube material in viscoelastic surfactant fluids after, the viscosity increasing degree of compound system is remarkable, and heat resistance is also significantly improved.
Claims (2)
1. a carbon nanotube complex thickener, is characterized in that, it is as follows that raw material composition presses mass percent:
Described modified multiwalled carbon nanotube be technical grade carbon nanotube in the NaOH solution of 2mol/L, 90-110 DEG C of reflux 2h, is cooled to room temperature, and filtration washing is to neutral, and at 100 DEG C, dry 2h obtains pretreated carbon nanotube product; Gained pre-treatment product are that the concentrated nitric acid of 3:1 and the vitriol oil are in 50-70 DEG C of reflux 0.5h through volume ratio again, be cooled to room temperature, filtration washing is to neutral, at 100 DEG C, dry 2h obtains modified multiwalled carbon nanotube product, this modified multiwalled carbon nanotube material diameter is less than 5nm, and length is less than 2 μm;
Described tensio-active agent is: cats product alkyl quaternary ammonium salts, alkyl carbon chain lengths 16-22; Or anion surfactant fatty acid acyl amido sulfonate sodium, Sulfonated Fatty Acid Methyl Ester, fatty acid chain length is 18-22; Or amphoterics alkyl betaine, alkylamide propyl-betaine, alkyl carbon chain lengths is 18-22;
Described gegenion salt is the one in sodium salicylate, sodium-chlor, Repone K, ammonium chloride;
Described auxiliary agent is the one in lauryl alcohol, sodium lauryl sulphate.
2. a preparation method for carbon nanotube complex thickener, is characterized in that, comprises the steps:
Be configured to the aqueous solution by the stirring that to be added to the water by tensio-active agent of following mass percent proportioning under normal temperature, then add carbon nanotube particulate, gegenion salt and auxiliary agent successively, stir, carbon nanotube complex thickener can be obtained; Modified multiwalled carbon nanotube 0.05-0.4%; Tensio-active agent 1-5%; Gegenion salt 0-8%; Auxiliary agent 0-3%; Water surplus;
Described modified multiwalled carbon nanotube be technical grade carbon nanotube in the NaOH solution of 2mol/L, 90-110 DEG C of reflux 2h, is cooled to room temperature, and filtration washing is to neutral, and at 100 DEG C, dry 2h obtains pretreated carbon nanotube product; Gained pre-treatment product again through volume ratio be the concentrated nitric acid of 3:1 and the vitriol oil in 50-70 DEG C of reflux 0.5h, be cooled to room temperature, filtration washing is to neutral, and at 100 DEG C, dry 2h obtains modified multiwalled carbon nanotube product.This modified multiwalled carbon nanotube material diameter is less than 5nm, and length is less than 2 μm;
Described tensio-active agent is: cats product alkyl quaternary ammonium salts, alkyl carbon chain lengths 16-22; Or anion surfactant fatty acid acyl amido sulfonate sodium, Sulfonated Fatty Acid Methyl Ester, fatty acid chain length is 18-22; Or amphoterics alkyl betaine, alkylamide propyl-betaine, alkyl carbon chain lengths is 18-22;
Described gegenion salt is the one in sodium salicylate, sodium-chlor, Repone K, ammonium chloride;
Described auxiliary agent is the one in lauryl alcohol, sodium lauryl sulphate.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106433603A (en) * | 2016-09-14 | 2017-02-22 | 西南石油大学 | Carbon nano-tube doped fracturing fluid system |
| CN107033868A (en) * | 2017-04-14 | 2017-08-11 | 中国石油大学(华东) | Nano material reinforcing clean fracturing fluid and preparation method thereof |
| CN107418531A (en) * | 2017-05-26 | 2017-12-01 | 西南石油大学 | Non-sulfonated high temperature resistance filtrate reducing water-base drilling fluid |
| CN110938415A (en) * | 2019-12-02 | 2020-03-31 | 西南石油大学 | Micro-nano plugging anti-collapse drilling fluid and preparation method and application thereof |
| CN112322265A (en) * | 2020-10-09 | 2021-02-05 | 西南石油大学 | Finger-advancing front edge locking nano-worm and preparation method thereof |
| CN114106811A (en) * | 2021-11-10 | 2022-03-01 | 中国石油大学(华东) | Two-dimensional nano material reinforced clean fracturing fluid and preparation method and application thereof |
| CN116589998A (en) * | 2023-07-18 | 2023-08-15 | 克拉玛依市正诚有限公司 | Composite thickening agent for fracturing and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106433603A (en) * | 2016-09-14 | 2017-02-22 | 西南石油大学 | Carbon nano-tube doped fracturing fluid system |
| CN106433603B (en) * | 2016-09-14 | 2018-10-19 | 西南石油大学 | A kind of carbon nano tube-doped fracturing fluid system |
| CN107033868A (en) * | 2017-04-14 | 2017-08-11 | 中国石油大学(华东) | Nano material reinforcing clean fracturing fluid and preparation method thereof |
| CN107418531A (en) * | 2017-05-26 | 2017-12-01 | 西南石油大学 | Non-sulfonated high temperature resistance filtrate reducing water-base drilling fluid |
| CN107418531B (en) * | 2017-05-26 | 2020-02-14 | 西南石油大学 | Non-sulfonated high-temperature-resistant fluid loss water-based drilling fluid |
| CN110938415A (en) * | 2019-12-02 | 2020-03-31 | 西南石油大学 | Micro-nano plugging anti-collapse drilling fluid and preparation method and application thereof |
| CN110938415B (en) * | 2019-12-02 | 2021-10-19 | 西南石油大学 | Micro-nano plugging anti-collapse drilling fluid and preparation method and application thereof |
| CN112322265A (en) * | 2020-10-09 | 2021-02-05 | 西南石油大学 | Finger-advancing front edge locking nano-worm and preparation method thereof |
| CN114106811A (en) * | 2021-11-10 | 2022-03-01 | 中国石油大学(华东) | Two-dimensional nano material reinforced clean fracturing fluid and preparation method and application thereof |
| CN116589998A (en) * | 2023-07-18 | 2023-08-15 | 克拉玛依市正诚有限公司 | Composite thickening agent for fracturing and preparation method thereof |
| CN116589998B (en) * | 2023-07-18 | 2023-10-03 | 克拉玛依市正诚有限公司 | Composite thickening agent for fracturing and preparation method thereof |
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