CN116217797A - Instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickening agent and preparation method thereof - Google Patents
Instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickening agent and preparation method thereof Download PDFInfo
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- 239000012530 fluid Substances 0.000 title claims abstract description 48
- 239000002562 thickening agent Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 239000007788 liquid Substances 0.000 title claims abstract description 33
- 150000003839 salts Chemical class 0.000 title claims abstract description 22
- -1 alkyl tertiary amine Chemical class 0.000 claims abstract description 89
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 21
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 20
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 20
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 20
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims abstract description 20
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- 239000003960 organic solvent Substances 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 34
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 30
- 239000000047 product Substances 0.000 claims description 27
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 24
- 239000007864 aqueous solution Substances 0.000 claims description 22
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- 239000000178 monomer Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 13
- NHLUVTZJQOJKCC-UHFFFAOYSA-N n,n-dimethylhexadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCN(C)C NHLUVTZJQOJKCC-UHFFFAOYSA-N 0.000 claims description 11
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical group CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 10
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 10
- 229920000053 polysorbate 80 Polymers 0.000 claims description 10
- NAPSCFZYZVSQHF-UHFFFAOYSA-N dimantine Chemical compound CCCCCCCCCCCCCCCCCCN(C)C NAPSCFZYZVSQHF-UHFFFAOYSA-N 0.000 claims description 9
- 229950010007 dimantine Drugs 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 9
- 239000007762 w/o emulsion Substances 0.000 claims description 9
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims description 8
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 claims description 7
- BHELZAPQIKSEDF-UHFFFAOYSA-N allyl bromide Chemical compound BrCC=C BHELZAPQIKSEDF-UHFFFAOYSA-N 0.000 claims description 7
- 239000003921 oil Substances 0.000 claims 9
- 230000015784 hyperosmotic salinity response Effects 0.000 abstract description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 13
- 238000010276 construction Methods 0.000 description 12
- 229920000642 polymer Polymers 0.000 description 12
- 239000004576 sand Substances 0.000 description 8
- 229920002401 polyacrylamide Polymers 0.000 description 7
- 239000011780 sodium chloride Substances 0.000 description 7
- 230000009467 reduction Effects 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- JDXXTKLHHZMVIO-UHFFFAOYSA-N 2-(3-hydroxypropyl)guanidine Chemical compound NC(=N)NCCCO JDXXTKLHHZMVIO-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229920013818 hydroxypropyl guar gum Polymers 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/882—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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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
- C09K2208/30—Viscoelastic surfactants [VES]
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Abstract
The invention relates to an instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickener and a preparation method thereof. The thickening agent comprises long-chain alkyl tertiary amine, allyl halide, white oil, an emulsifier, water, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, ammonium persulfate and sodium bisulphite. It has salt tolerance and viscoelasticity, increases viscosity by increasing hydrodynamic volume, and exhibits good spatial network structure and elasticity.
Description
Technical Field
The invention relates to the technical field of preparation and application of fracturing fluid thickeners for low-permeability oil fields, in particular to a preparation method of an instant continuous liquid-preparation low-concentration salt-resistant fracturing fluid thickener.
Background
Along with the trend of poor quality of oil and gas resources in China becoming serious, unconventional and ultra-deep difficult-to-extract resources such as dense gas, coal bed gas, shale gas and the like gradually become the dominant force of oil and gas exploration and sustainable storage and production increase in China. The fracturing technology is one of important measures for increasing the production of oil reservoirs and increasing the injection of water wells. Fracturing fluids are one of the key parts of the fracturing technology. At present, various fracturing fluid systems exist at home and abroad, and are classified into oil-based fracturing fluid, water-based fracturing fluid, foam fracturing fluid, clean fracturing fluid and the like according to different physicochemical properties. The water-based fracturing fluid is widely used for oil reservoir production and injection at home and abroad due to the advantages of low cost, convenient preparation and use and the like. The thickening agent is used as an important component of the water-based fracturing fluid, and the properties of temperature resistance, viscosity increment, low residue and the like are directly related to the success or failure of fracturing construction. Currently, commonly used water-based fracturing fluid thickeners are mainly natural high-molecular modified substances (such as hydroxypropyl guar gum and cellulose), synthetic polymers and the like. The hydroxypropyl guanidine gum and cellulose natural polymer have the defects of high cost, no biodegradation, high residue after gel breaking, high damage to a reservoir and the like. The thickener in the traditional water-based fracturing fluid system is generally powder (solid particles), and firstly, the powder is easy to absorb water, moisture and deteriorate. Is difficult to dissolve after absorbing moisture and is easy to form fish eyes. Secondly, the powder thickener generally has longer dissolution time and longer liquid preparation time. Thirdly, equipment such as a sand mixing vehicle for liquid preparation is often used in a construction site, the liquid preparation steps are complicated, and the waste of materials is easy to cause; and finally, the construction period is long, and the construction efficiency is low.
According to the technical requirements, the molecular structure of the polymer thickener of the low-concentration salt-resistant fracturing fluid is designed by combining the basic performance requirements of the polymer fracturing fluid through the molecular design theory and model concept:
(1) Salt tolerance of the polymer: at present, the research on salt tolerance of a polymer is mainly divided into two ideas, namely, introducing a plurality of rigid functional groups, and dissolving the polymer in a salt solution by virtue of association and steric effect of the groups; and secondly, increasing the molecular weight to increase the hydrodynamic volume of the polymer in solution and enhance the viscosity of the polymer in saline.
(2) Polymer viscoelasticity: the polymer solution is stretched in the aqueous solution by means of larger molecular weight, if the polymer has good elasticity, the viscosity is increased by increasing the hydrodynamic volume, the polymer needs to show good space network structure in the solution, the conventional polyacrylamide is linear macromolecule, the molecular chains are only intertwined, the functional monomer is introduced, and the space structure of the polymer in the solution is enhanced by utilizing the interaction between the monomer and the interaction between the monomer and the molecular chains, so that the elasticity is enhanced.
Disclosure of Invention
In order to overcome the defects of the prior art and realize instant continuous liquid preparation, the invention aims to provide a preparation method of an instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickener, which improves the liquid preparation efficiency and the construction efficiency of fracturing fluid products.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickener comprises the following steps of:
the method comprises the steps of firstly, dissolving long-chain alkyl tertiary amine in an organic solvent with the purity mass ratio of 2-6 times in a container at room temperature, wherein the long-chain alkyl tertiary amine is selected from industrial grade hexadecyl dimethyl amine and octadecyl dimethyl amine with the purity mass ratio of 1:1-5, and the organic solvent is selected from industrial grade acetone, benzene, toluene, acetonitrile and tetrahydrofuran with the purity of more than the industrial grade;
a second step of dissolving allyl halide in an amount ratio of 1:1-1.3 to long-chain alkyl tertiary amine substance in another container in an organic solvent, wherein the allyl halide is selected from industrial grade allyl chloride and allyl bromide with purity above and the organic solvent is selected from acetone, benzene, toluene, acetonitrile and tetrahydrofuran with purity above and industrial grade;
thirdly, dripping the allyl halide solution into the long-chain alkyl tertiary amine solution, stirring for 2-6 hours at 40-80 ℃ after the addition, cooling to room temperature, filtering out precipitate, namely allyl quaternary ammonium salt, and drying to constant weight at 60-80 ℃ for later use;
fourthly, adding white oil and an emulsifying agent into a reaction container at room temperature, wherein the mass ratio is 10:1-10:5, stirring uniformly until the white oil is dissolved, the white oil is selected from industrial grade and above white oil with purity, and the emulsifying agent is selected from span-80 and tween-80 with the industrial grade and above with the purity mass ratio of 1:1-3;
fifthly, adding water, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and allyl quaternary ammonium salt prepared in the third step into another container at room temperature, stirring until the mixture is completely dissolved, and adding ammonium persulfate accounting for 0.2-0.6% of the total mass of the monomers, wherein the water, the acrylamide, the 2-acrylamide-2-methylpropanesulfonic acid and the ammonium persulfate are all selected from industrial-grade and products with purity above the industrial-grade;
step six, dripping the aqueous solution prepared in the step five into the reactor in the step four at room temperature, fully stirring for 10-60min under the condition of introducing nitrogen, and maintaining the forward pressure in the reactor to obtain stable water-in-oil emulsion;
seventh, preparing sodium bisulphite accounting for 0.01-0.03% of the total mass of the monomers in the fifth step into 0.3-0.6% of aqueous solution at room temperature, dripping the aqueous solution into the reactor in the fourth step, and keeping the temperature in the reactor in the dripping process not to exceed 50 ℃, wherein the water and the sodium bisulphite are selected from industrial-grade and products with purity above;
and eighth, introducing nitrogen to maintain the forward pressure in the reactor, heating the reactant in the reactor in the fourth step to 40-50 ℃, reacting for 3-6h, and cooling to room temperature to obtain the instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickener.
The fracturing fluid thickener product can flow freely at room temperature, can be directly poured into the water of a liquid preparation tank during site construction, and can reach the maximum viscosity after stirring for more than 10 minutes at room temperature, thereby ensuring continuous liquid preparation. The viscosity is evaluated according to the general technical condition of fracturing fluid (SYT 6376-2008), and the viscosity reaches the requirement of carrying sand for fracturing within 160 ℃.
Examples
The invention is further illustrated by the following examples. It should be understood that the methods described in the examples of the present invention are only for illustrating the present invention, and not for limiting the present invention, and that simple modifications to the preparation methods of the present invention under the concept of the present invention are within the scope of the present invention as claimed. All the starting materials and solvents used in the examples were commercially available products of the corresponding purity.
The invention is further described below in connection with specific embodiments.
Example 1
A first step of dissolving a long-chain alkyl tertiary amine in an organic solvent which is 2 times that of industrial-grade hexadecyldimethylamine in a container at room temperature, wherein the organic solvent is industrial-grade acetone;
a second step of dissolving an allyl halide in an amount ratio of 1:1 to hexadecyldimethylamine substance in a 6-fold organic solvent selected from technical grade allyl chloride, said organic solvent selected from technical grade acetone;
thirdly, dripping the allyl halide solution into the long-chain alkyl tertiary amine solution, stirring for 6 hours at 40 ℃ after the addition, cooling to room temperature, filtering out precipitate, namely allyl quaternary ammonium salt, and drying to constant weight at 60 ℃ for later use;
fourthly, adding white oil and an emulsifying agent with the mass ratio of 10:1 into a reaction container at room temperature, and uniformly stirring until the white oil is dissolved, wherein the white oil is selected from industrial-grade white oil, and the emulsifying agent is selected from span-80 and tween-80 with the mass ratio of 1:1;
fifthly, adding water, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and allyl quaternary ammonium salt prepared in the third step into another container at room temperature, stirring until the mixture is completely dissolved, and adding ammonium persulfate accounting for 0.2% of the total mass of the monomers, wherein the water, the acrylamide, the 2-acrylamide-2-methylpropanesulfonic acid and the ammonium persulfate are all selected from industrial products;
step six, dripping the water solution prepared in the step five into the reactor in the step four at room temperature, fully stirring for 10min under the condition of introducing nitrogen, and maintaining the forward pressure in the reactor to obtain stable water-in-oil emulsion;
seventh, preparing sodium bisulphite accounting for 0.01% of the total mass of the monomers in the fifth step into 0.6% aqueous solution at room temperature, dripping the aqueous solution into the reactor in the fourth step, and keeping the temperature in the reactor in the dripping process not to exceed 50 ℃, wherein the water and the sodium bisulphite are both selected from industrial-grade products;
and eighth, introducing nitrogen to maintain the forward pressure in the reactor, heating the reactant in the reactor in the fourth step to 50 ℃, reacting for 3 hours, and cooling to room temperature to obtain the instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickening agent.
The fracturing fluid thickener product can flow freely at room temperature, can be directly poured into the water of a liquid preparation tank during site construction, and can reach the maximum viscosity after being stirred for 15 minutes at room temperature, so that continuous liquid preparation is ensured. The viscosity is evaluated according to the general technical condition of fracturing fluid (SYT 6376-2008), the viscosity of 0.5% of the thickener is 82.5 mPa.s at 80 ℃, the requirement of carrying sand in fracturing is met, and the viscosity is increased by 26% compared with the current modified polyacrylamide thickener in oil fields. The viscosity reduction rate in 10% NaCl solution was 5.2%, showing a higher salt resistance.
Example 2
The method comprises the steps of firstly, dissolving long-chain alkyl tertiary amine in an organic solvent which is 3 times of the long-chain alkyl tertiary amine at room temperature, wherein the long-chain alkyl tertiary amine is selected from hexadecyl dimethyl amine and octadecyl dimethyl amine with the mass ratio of 1:1.2 in chemical purity, and the organic solvent is selected from chemically pure benzene;
a second step of dissolving an allyl halide in a ratio of 1:1.1 to the amount of long-chain alkyl tertiary amine material in another vessel in a 5-fold amount of an organic solvent selected from chemically pure allyl chloride, the organic solvent selected from chemically pure benzene;
thirdly, dripping the allyl halide solution into the long-chain alkyl tertiary amine solution, stirring for 4 hours at 55 ℃ after the addition, cooling to room temperature, filtering out precipitate, namely allyl quaternary ammonium salt, and drying to constant weight at 60 ℃ for later use;
fourthly, adding white oil and an emulsifying agent with the mass ratio of 10:2 into a reaction container at room temperature, and uniformly stirring until the white oil is dissolved, wherein the white oil is selected from chemically pure white oil, and the emulsifying agent is selected from span-80 and tween-80 with the chemical pure mass ratio of 1:1.5;
fifthly, adding water, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and allyl quaternary ammonium salt prepared in the third step into another container at room temperature, stirring until the mixture is completely dissolved, and adding ammonium persulfate accounting for 0.3% of the total mass of the monomers, wherein the water, the acrylamide, the 2-acrylamide-2-methylpropanesulfonic acid and the ammonium persulfate are all selected from chemical pure products;
step six, dripping the water solution prepared in the step five into the reactor in the step four at room temperature, fully stirring for 15min under the condition of introducing nitrogen, and maintaining the forward pressure in the reactor to obtain stable water-in-oil emulsion;
seventh, preparing sodium bisulphite accounting for 0.02% of the total mass of the monomers in the fifth step into 0.5% aqueous solution at room temperature, dripping the aqueous solution into the reactor in the fourth step, and keeping the temperature in the reactor in the dripping process not to exceed 50 ℃, wherein the water and the sodium bisulphite are both selected from chemical pure products;
and eighth, introducing nitrogen to maintain the forward pressure in the reactor, heating the reactant in the reactor in the fourth step to 42 ℃, reacting for 5 hours, and cooling to room temperature to obtain the instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickening agent.
The fracturing fluid thickener product can flow freely at room temperature, can be directly poured into the water of a liquid preparation tank during site construction, and can reach the maximum viscosity after stirring for 13 minutes at room temperature, so that continuous liquid preparation is ensured. The viscosity is evaluated according to the general technical condition of fracturing fluid (SYT 6376-2008), the viscosity of 0.6% of the thickener is 81.5 mPa.s at 100 ℃, the requirement of carrying sand in fracturing is met, and the viscosity is increased by 33% compared with the current modified polyacrylamide thickener in oil fields. The viscosity reduction rate in 15% NaCl solution was 5.1%, showing a higher salt resistance.
Example 3
A first step of dissolving a long-chain alkyl tertiary amine in an organic solvent which is 4 times that of a solvent selected from cetyl dimethylamine and stearyl dimethylamine in an analytically pure mass ratio of 1:3 in a container at room temperature;
a second step of dissolving an allyl halide in a ratio of 1:1.2 to the amount of long-chain alkyl tertiary amine material in a 4-fold amount of an organic solvent selected from analytically pure allyl bromide in a separate vessel, the organic solvent selected from analytically pure toluene;
thirdly, dripping the allyl halide solution into the long-chain alkyl tertiary amine solution, stirring for 2 hours at 80 ℃ after the addition, cooling to room temperature, filtering out precipitate, namely allyl quaternary ammonium salt, and drying to constant weight at 80 ℃ for later use;
fourth, adding the following components in mass ratio of 10:3 and an emulsifier, stirring uniformly until the white oil is dissolved, wherein the white oil is selected from analytically pure white oil, and the emulsifier is selected from span-80 and tween-80 with the analytically pure mass ratio of 1:2;
fifthly, adding water, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and allyl quaternary ammonium salt prepared in the third step into another container at room temperature, stirring until the mixture is completely dissolved, and adding ammonium persulfate accounting for 0.4% of the total mass of the monomers, wherein the water, the acrylamide, the 2-acrylamide-2-methylpropanesulfonic acid and the ammonium persulfate are all selected from analytically pure products;
step six, dripping the water solution prepared in the step five into the reactor in the step four at room temperature, fully stirring for 25 minutes under the condition of introducing nitrogen, and maintaining the forward pressure in the reactor to obtain stable water-in-oil emulsion;
seventh, preparing sodium bisulphite accounting for 0.03 percent of the total mass of the monomers in the fifth step into 0.36 percent of aqueous solution at room temperature, dripping the aqueous solution into the reactor in the fourth step, and keeping the temperature in the reactor in the dripping process not to exceed 50 ℃, wherein the water and the sodium bisulphite are both selected from analytically pure products;
and eighth, introducing nitrogen to maintain the forward pressure in the reactor, heating the reactant in the reactor in the fourth step to 50 ℃, reacting for 3 hours, and cooling to room temperature to obtain the instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickening agent.
The fracturing fluid thickener product can flow freely at room temperature, can be directly poured into the water of a liquid preparation tank during site construction, and can reach the maximum viscosity after being stirred for 16 minutes at room temperature, so that continuous liquid preparation is ensured. The viscosity is evaluated according to the general technical condition of fracturing fluid (SYT 6376-2008), the viscosity of 0.75% of the thickener is 96.0 mPa.s at 110 ℃, the requirement of carrying sand in fracturing is met, and the viscosity is increased by 31% compared with the current modified polyacrylamide thickener in oil fields. The viscosity reduction rate in 18% NaCl solution was 4.5%, showing a higher salt resistance.
Example 4
The method comprises the steps of firstly, dissolving long-chain alkyl tertiary amine in an organic solvent which is 5 times of long-chain alkyl tertiary amine in a container at room temperature, wherein the long-chain alkyl tertiary amine is selected from hexadecyl dimethyl amine and octadecyl dimethyl amine with the chemical purity mass ratio of 1:3, and the organic solvent is selected from analytically pure acetonitrile;
a second step of dissolving an allyl halide in a ratio of 1:1 to 1.3 to the amount of long-chain alkyl tertiary amine material in a 3-fold amount of an organic solvent selected from analytically pure allyl bromide in a separate vessel, the organic solvent selected from analytically pure acetonitrile;
thirdly, dripping the allyl halide solution into the long-chain alkyl tertiary amine solution, stirring for 5 hours at 60 ℃ after the addition, cooling to room temperature, filtering out precipitate, namely allyl quaternary ammonium salt, and drying to constant weight at 65 ℃ for later use;
step four, adding white oil and an emulsifying agent with the mass ratio of 10:2.5 into a reaction container at room temperature, and uniformly stirring until the white oil is dissolved, wherein the white oil is analytically pure white oil, and the emulsifying agent is selected from span-80 and tween-80 with the mass ratio of 1:2.5;
fifthly, adding water, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and the allyl quaternary ammonium salt prepared in the third step into another container at room temperature, stirring until the allyl quaternary ammonium salt is completely dissolved, and adding ammonium persulfate accounting for 0.5% of the total mass of the monomers, wherein the water, the acrylamide, the 2-acrylamido-2-methylpropanesulfonic acid and the ammonium persulfate are all selected from analytically pure products;
step six, dripping the water solution prepared in the step five into the reactor in the step four at room temperature, fully stirring for 50min under the condition of introducing nitrogen, and maintaining the forward pressure in the reactor to obtain stable water-in-oil emulsion;
seventh, preparing sodium bisulphite accounting for 0.02% of the total mass of the monomers in the fifth step into 0.5% aqueous solution at room temperature, dripping the aqueous solution into the reactor in the fourth step, and keeping the temperature in the reactor in the dripping process not to exceed 50 ℃, wherein the water and the sodium bisulphite are both selected from analytically pure products;
and eighth, introducing nitrogen to maintain the forward pressure in the reactor, heating the reactant in the reactor in the fourth step to 45 ℃, reacting for 5 hours, and cooling to room temperature to obtain the instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickening agent.
The fracturing fluid thickener product can flow freely at room temperature, can be directly poured into the water of a liquid preparation tank during site construction, and can reach the maximum viscosity after stirring for 12 minutes at room temperature, so that continuous liquid preparation is ensured. The viscosity is evaluated according to the general technical condition of fracturing fluid (SYT 6376-2008), the viscosity of 0.6% of the thickener is 79.6 mPa.s at 120 ℃, the requirement of carrying sand in fracturing is met, and the viscosity is increased by 19.8% compared with the viscosity of the modified polyacrylamide thickener used in the current oil field. The viscosity reduction rate in 20% NaCl solution was 6.0%, showing a higher salt resistance.
Example 5
The method comprises the steps of firstly, dissolving long-chain alkyl tertiary amine in an organic solvent which is 6 times of long-chain alkyl tertiary amine in a container at room temperature, wherein the long-chain alkyl tertiary amine is selected from hexadecyl dimethyl amine and octadecyl dimethyl amine with the mass ratio of 1:5 in industrial grade, and the organic solvent is selected from industrial grade acetonitrile;
a second step of dissolving an allyl halide in a ratio of the amount of the allyl halide to the amount of the long-chain alkyl tertiary amine substance of 1:1 to 1.3 in an organic solvent of 2 times, wherein the allyl halide is selected from industrial grade allyl bromide, and the organic solvent is selected from industrial grade acetonitrile;
thirdly, dripping the allyl halide solution into the long-chain alkyl tertiary amine solution, stirring for 4 hours at 65 ℃ after the addition, cooling to room temperature, filtering out precipitate, namely allyl quaternary ammonium salt, and drying to constant weight at 70 ℃ for later use;
fourthly, adding white oil and an emulsifying agent with the mass ratio of 10:3 into a reaction container at room temperature, and uniformly stirring until the white oil is dissolved, wherein the white oil is selected from industrial-grade white oil, and the emulsifying agent is selected from span-80 and tween-80 with the mass ratio of 1:1;
fifthly, adding water, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and allyl quaternary ammonium salt prepared in the third step into another container at room temperature, stirring until the mixture is completely dissolved, and adding ammonium persulfate accounting for 0.6% of the total mass of the monomers, wherein the water, the acrylamide, the 2-acrylamido-2-methylpropanesulfonic acid and the ammonium persulfate are all selected from industrial products;
step six, dripping the water solution prepared in the step five into the reactor in the step four at room temperature, fully stirring for 60min under the condition of introducing nitrogen, and maintaining the forward pressure in the reactor to obtain stable water-in-oil emulsion;
seventh, preparing sodium bisulphite accounting for 0.01% of the total mass of the monomers in the fifth step into 0.6% aqueous solution at room temperature, dripping the aqueous solution into the reactor in the fourth step, and keeping the temperature in the reactor in the dripping process not to exceed 50 ℃, wherein the water and the sodium bisulphite are both selected from industrial-grade products;
and eighth, introducing nitrogen to maintain the forward pressure in the reactor, heating the reactant in the reactor in the fourth step to 50 ℃, reacting for 6 hours, and cooling to room temperature to obtain the instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickening agent.
The fracturing fluid thickener product can flow freely at room temperature, can be directly poured into the water of a liquid preparation tank during site construction, and can reach the maximum viscosity after stirring for 14 minutes at room temperature, so that continuous liquid preparation is ensured. The viscosity is evaluated according to the general technical condition of fracturing fluid (SYT 6376-2008), the viscosity of 1% of the thickener is 146 mPa.s at 120 ℃, the requirement of fracturing sand carrying is met, and the viscosity is increased by 28% compared with the current modified polyacrylamide thickener used in oil fields. The viscosity reduction rate in 18% NaCl solution was 4.6%, showing a higher salt resistance.
Example 6
The method comprises the steps of firstly, dissolving long-chain alkyl tertiary amine in an organic solvent which is 3 times of the long-chain alkyl tertiary amine at room temperature, wherein the long-chain alkyl tertiary amine is selected from cetyl dimethyl amine and stearyl dimethyl amine with the mass ratio of 1:1 in industrial grade, and the organic solvent is selected from industrial grade tetrahydrofuran;
a second step of dissolving an allyl halide in a ratio of the amount of the allyl halide to the amount of the long-chain alkyl tertiary amine substance of 1:1 to 1.3 in an organic solvent of 3 times, wherein the allyl halide is selected from industrial grade allyl chloride, and the organic solvent is selected from industrial grade tetrahydrofuran;
thirdly, dripping the allyl halide solution into the long-chain alkyl tertiary amine solution, stirring for 4 hours at 60 ℃ after the addition, cooling to room temperature, filtering out precipitate, namely allyl quaternary ammonium salt, and drying to constant weight at 80 ℃ for later use;
fourthly, adding white oil and an emulsifying agent with the mass ratio of 10:1.5 into a reaction container at room temperature, and uniformly stirring until the white oil is dissolved, wherein the white oil is selected from industrial-grade white oil, and the emulsifying agent is selected from span-80 and tween-80 with the analytical purity mass ratio of 1:1.5;
fifthly, adding water, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and the allyl quaternary ammonium salt prepared in the third step into another container at room temperature, stirring until the mixture is completely dissolved, and adding ammonium persulfate accounting for 0.5% of the total mass of the monomers, wherein the water, the acrylamide, the 2-acrylamido-2-methylpropanesulfonic acid and the ammonium persulfate are all selected from chemical pure products;
step six, dripping the water solution prepared in the step five into the reactor in the step four at room temperature, fully stirring for 30min under the condition of introducing nitrogen, and maintaining the forward pressure in the reactor to obtain stable water-in-oil emulsion;
seventh, preparing sodium bisulphite accounting for 0.03 percent of the total mass of the monomers in the fifth step into 0.4 percent of aqueous solution at room temperature, dripping the aqueous solution into the reactor in the fourth step, and keeping the temperature in the reactor in the dripping process not to exceed 50 ℃, wherein the water and the sodium bisulphite are both selected from industrial-grade and above-purity products;
and eighth, introducing nitrogen to maintain the forward pressure in the reactor, heating the reactant in the reactor in the fourth step to 45 ℃, reacting for 5 hours, and cooling to room temperature to obtain the instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickening agent.
The fracturing fluid thickener product can flow freely at room temperature, can be directly poured into the water of a liquid preparation tank during site construction, and can reach the maximum viscosity after being stirred for 16 minutes at room temperature, so that continuous liquid preparation is ensured. The viscosity is evaluated according to the general technical condition of fracturing fluid (SYT 6376-2008), the viscosity of 1% of the thickener is 80.1 mPa.s at 1500 ℃, the requirement of carrying sand in fracturing is met, and the viscosity is increased by 31% compared with the current modified polyacrylamide thickener used in oil fields. The viscosity reduction rate in 25% NaCl solution was 7.8%, showing a higher salt resistance.
Claims (5)
1. A fracturing fluid thickener characterized by comprising: long-chain alkyl tertiary amine, allyl halide, white oil, emulsifier, water, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, ammonium persulfate and sodium bisulphite; wherein the ratio of the allyl halide to the long-chain alkyl tertiary amine is 1:1-1.3; the mass ratio of the water to the acrylamide to the 2-acrylamido-2-methylpropanesulfonic acid is 10:5-6:2-3.
2. The fracturing fluid thickener of claim 1 wherein: the long-chain alkyl tertiary amine is selected from industrial grade hexadecyl dimethyl amine and octadecyl dimethyl amine with the purity mass ratio of 1:1-5; the allyl halide is selected from industrial grade allyl chloride and allyl bromide with purity above; the emulsifier is selected from span-80 and tween-80 with purity mass ratio of 1:1-3.
3. The fracturing fluid thickener of claim 1, which is prepared by the following method: the method comprises the steps of firstly, dissolving long-chain alkyl tertiary amine in an organic solvent with the purity mass ratio of 2-6 times in a container at room temperature, wherein the long-chain alkyl tertiary amine is selected from industrial grade hexadecyl dimethyl amine and octadecyl dimethyl amine with the purity mass ratio of 1:1-5, and the organic solvent is selected from industrial grade acetone, benzene, toluene, acetonitrile and tetrahydrofuran with the purity of more than the industrial grade;
a second step of dissolving allyl halide in an amount ratio of 1:1-1.3 to long-chain alkyl tertiary amine substance in another container in an organic solvent, wherein the allyl halide is selected from industrial grade allyl chloride and allyl bromide with purity above and the organic solvent is selected from acetone, benzene, toluene, acetonitrile and tetrahydrofuran with purity above and industrial grade;
thirdly, dripping the allyl halide solution into the long-chain alkyl tertiary amine solution, stirring for 2-6 hours at 40-80 ℃ after the addition, cooling to room temperature, filtering out precipitate, namely allyl quaternary ammonium salt, and drying to constant weight at 60-80 ℃ for later use;
fourthly, adding white oil and an emulsifying agent into a reaction container at room temperature, wherein the mass ratio is 10:1-10:5, stirring uniformly until the white oil is dissolved, the white oil is selected from industrial grade and the white oil with purity above, and the emulsifying agent is selected from span-80 and tween-80 with purity mass ratio of 1:1-3;
fifthly, adding water, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and allyl quaternary ammonium salt prepared in the third step into another container at room temperature, stirring until the mixture is completely dissolved, and adding ammonium persulfate accounting for 0.2-0.6% of the total mass of the monomers, wherein the water, the acrylamide, the 2-acrylamide-2-methylpropanesulfonic acid and the ammonium persulfate are all selected from industrial-grade and products with purity above the industrial-grade;
step six, dripping the aqueous solution prepared in the step five into the reactor in the step four at room temperature, fully stirring for 10-60min under the condition of introducing nitrogen, and maintaining the forward pressure in the reactor to obtain stable water-in-oil emulsion;
seventh, preparing sodium bisulphite accounting for 0.01-0.03% of the total mass of the monomers in the fifth step into 0.3-0.6% of aqueous solution at room temperature, dripping the aqueous solution into the reactor in the fourth step, and keeping the temperature in the reactor in the dripping process not to exceed 50 ℃, wherein the water and the sodium bisulphite are selected from industrial-grade and products with purity above;
and eighth, introducing nitrogen to maintain the forward pressure in the reactor, heating the reactant in the reactor in the fourth step to 40-50 ℃, reacting for 3-6h, and cooling to room temperature to obtain the instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickener.
4. The method for preparing the fracturing fluid thickener of claim 1, which is characterized by comprising the following steps:
the method comprises the steps of firstly, dissolving long-chain alkyl tertiary amine in an organic solvent with the purity mass ratio of 2-6 times in a container at room temperature, wherein the long-chain alkyl tertiary amine is selected from industrial grade hexadecyl dimethyl amine and octadecyl dimethyl amine with the purity mass ratio of 1:1-5, and the organic solvent is selected from industrial grade acetone, benzene, toluene, acetonitrile and tetrahydrofuran with the purity of more than the industrial grade;
a second step of dissolving allyl halide in an amount ratio of 1:1-1.3 to long-chain alkyl tertiary amine substance in another container in an organic solvent, wherein the allyl halide is selected from industrial grade allyl chloride and allyl bromide with purity above and the organic solvent is selected from acetone, benzene, toluene, acetonitrile and tetrahydrofuran with purity above and industrial grade;
thirdly, dripping the allyl halide solution into the long-chain alkyl tertiary amine solution, stirring for 2-6 hours at 40-80 ℃ after the addition, cooling to room temperature, filtering out precipitate, namely allyl quaternary ammonium salt, and drying to constant weight at 60-80 ℃ for later use;
fourthly, adding white oil and an emulsifying agent into a reaction container at room temperature, wherein the mass ratio is 10:1-10:5, stirring uniformly until the white oil is dissolved, the white oil is selected from industrial grade and the white oil with purity above, and the emulsifying agent is selected from span-80 and tween-80 with purity mass ratio of 1:1-3;
fifthly, adding water, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and allyl quaternary ammonium salt prepared in the third step into another container at room temperature, stirring until the mixture is completely dissolved, and adding ammonium persulfate accounting for 0.2-0.6% of the total mass of the monomers, wherein the water, the acrylamide, the 2-acrylamide-2-methylpropanesulfonic acid and the ammonium persulfate are all selected from industrial-grade and products with purity above the industrial-grade;
step six, dripping the aqueous solution prepared in the step five into the reactor in the step four at room temperature, fully stirring for 10-60min under the condition of introducing nitrogen, and maintaining the forward pressure in the reactor to obtain stable water-in-oil emulsion;
seventh, preparing sodium bisulphite accounting for 0.01-0.03% of the total mass of the monomers in the fifth step into 0.3-0.6% of aqueous solution at room temperature, dripping the aqueous solution into the reactor in the fourth step, and keeping the temperature in the reactor in the dripping process not to exceed 50 ℃, wherein the water and the sodium bisulphite are selected from industrial-grade and products with purity above;
and eighth, introducing nitrogen to maintain the forward pressure in the reactor, heating the reactant in the reactor in the fourth step to 40-50 ℃, reacting for 3-6h, and cooling to room temperature to obtain the instant continuous liquid preparation low-concentration salt-resistant fracturing fluid thickener.
5. Use of the fracturing fluid thickener of any of claims 1-2 in petrochemical industry.
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CN114380946A (en) * | 2020-10-22 | 2022-04-22 | 中国石油天然气股份有限公司 | Self-tackifying steering acid liquid thickener and preparation method and application thereof |
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