CN112961666B - Nano composite cross-linking agent for fracturing fluid and preparation method thereof - Google Patents
Nano composite cross-linking agent for fracturing fluid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano composite cross-linking agent for a fracturing fluid and a preparation method thereof, relating to the technical field of oil and gas development fracturing fluids; the cross-linking agent comprises a chelate synthesized by nano carbon quantum dots and metal ions. The invention also discloses a preparation method of the nano composite cross-linking agent for the fracturing fluid, which comprises the following steps: the method comprises the following steps: preparing nano carbon quantum dots; step two: and adding inorganic salt of metal ions into the prepared nano carbon quantum dots, and reacting for 1.5-3 h to obtain the nano cross-linking agent. The invention adopts chelate formed by chelating nano carbon quantum dots and metal ions as a composite crosslinking agent, and solves the problems of complex components and complex liquid preparation of the existing fracturing fluid crosslinking agent. Because one carbon quantum dot of the cross-linking agent has a plurality of cross-linking sites, more guanidine gum molecular chains can be cross-linked under the same addition amount; the dispersion is better, and the carbon quantum dots have a reinforcing effect on the fracturing fluid, so that the guanidine gum fracturing fluid crosslinked by using the crosslinking agent has a better temperature resistance effect compared with the existing crosslinking agent, and can reach 180-200 ℃.
Description
Technical Field
The invention belongs to the technical field of oil and gas development fracturing fluid, and particularly relates to a nano composite cross-linking agent for fracturing fluid and a preparation method thereof.
Background
The fracturing is an engineering operation process for oil and gas exploitation, and is a process for pressing a liquid with certain viscosity into underground rock fractures under high pressure by using pressure equipment, wherein the liquid with the viscosity adopted in the fracturing process is fracturing fluid. The fracturing fluid enters stratum rock under the action of high pressure, so that the rock is broken to generate cracks, and a propping agent material is added into the fracturing fluid to support the opening state of the underground cracks, so that an obviously opened rock crack is formed after the pumping of the fracturing fluid is stopped, the permeability of an oil-gas layer is improved, and the flow or the yield of oil gas passing through a crack channel is increased.
The fracturing fluid in the prior art mainly comprises a thickening agent, a gel breaker and a crosslinking agent. The crosslinking agent is used as an important additive in a fracturing fluid system, and the performance of the crosslinking agent has important influence on the crosslinking process of the whole fracturing fluid system. The cross-linking agent in the prior art is usually composed of a main agent, a phase transfer catalyst, a complexing agent and a cross-linking accelerator, and has the disadvantages of complex components, complex cross-linking process, complex operation, complex liquid preparation, difficult control and high requirement on fracturing construction. Therefore, the development of a cross-linking agent with simple liquid preparation and simple operation becomes one of the key points for the development and use of the fracturing fluid.
Disclosure of Invention
The invention provides a nano composite cross-linking agent for fracturing fluid aiming at the problems of complex components and complex fluid preparation of the existing cross-linking agent for fracturing fluid.
The invention also discloses a preparation method of the nano composite cross-linking agent for the fracturing fluid, which is simple and easy to popularize and use.
The specific technical scheme of the invention is as follows: a nano composite cross-linking agent for fracturing fluid comprises a chelate synthesized by nano carbon quantum dots and metal ions, and the structural expression of the chelate is as follows:
wherein M represents a metal ion.
In the technical scheme, the cross-linking agent is a chelate formed by chelating nano carbon quantum dots and metal ions, and because one carbon quantum dot of the cross-linking agent has a plurality of cross-linking point sites, more guanidine gum molecular chains can be cross-linked under the same addition amount; the dispersion is better, and the carbon quantum dots have a reinforcing effect on the fracturing fluid, so that the guanidine gum fracturing fluid crosslinked by using the crosslinking agent has a better temperature resistance effect compared with the existing crosslinking agent, and can reach 180-200 ℃.
Further, the metal ions are at least one of zirconium ions and titanium ions.
Further, the nano carbon quantum dots are nitrogen-doped carbon quantum dots.
The invention also discloses a preparation method of the nano composite cross-linking agent for the fracturing fluid, which comprises the following steps:
the method comprises the following steps: preparing nano carbon quantum dots;
step two: and adding inorganic salt of metal ions into the prepared nano carbon quantum dots, and reacting for 1.5-3 h to obtain the nano cross-linking agent.
Further, in the first step, the specific steps of preparing the nanocarbon quantum dots are as follows: dissolving citric acid with the effective concentration of more than 99.5% and organic amine with the effective concentration of more than 99.5% in deionized water to obtain a mixed solution, heating the mixed solution to 180-250 ℃, and reacting for 4-8 h to obtain the nano carbon quantum dot.
Further, the organic amine is at least one of ethanolamine, ethylenediamine, diethylenetriamine, triethylenetetramine and polyethyleneimine.
Further, the mass ratio of the citric acid to the organic amine is 1: 0.5-1.
Further, the molar ratio of the metal ions to the citric acid is 1: 1-5.
Further, the metal ion inorganic salt may be at least one of zirconium oxychloride, zirconium basic carbonate, zirconium fluoride, titanium chloride, and titanium fluoride.
The invention provides a nano composite cross-linking agent for fracturing fluid aiming at the problems of complex components and complex fluid preparation of the current cross-linking agent for fracturing fluid. Compared with the existing nano cross-linking agent, the carbon quantum dot type nano cross-linking agent has better dispersibility, and the fracturing fluid obtained by crosslinking the carbon quantum dot cross-linking agent has higher strength and better temperature resistance; and because a plurality of guar gum molecules can be crosslinked on one carbon quantum dot crosslinking unit, the dosage of the guar gum molecules can be effectively reduced.
The invention also discloses a preparation method of the nano composite cross-linking agent for the fracturing fluid, which is simple in preparation method and easy to popularize and use, and the prepared composite cross-linking agent is simple in liquid preparation and easy to use.
Drawings
FIG. 1 shows the chemical equation of the reaction of the nanocomposite cross-linking agent for fracturing fluid disclosed by the invention.
Detailed Description
Example 1
The embodiment prepares a nano composite cross-linking agent for fracturing fluid, and the formula of the nano composite cross-linking agent comprises the following components in terms of mole number: 5mol of citric acid, 2.5mol of diethylenetriamine, 5mol of zirconium oxychloride and 2000mL of deionized water.
The specific preparation method comprises the following steps:
the method comprises the following steps: weighing citric acid and diethylenetriamine according to the formula, adding into deionized water, and stirring and mixing to obtain a mixed solution; heating the mixed solution to 180 ℃, and reacting for 8 hours to obtain a liquid system of the nano carbon quantum dots;
step two: and adding zirconium oxychloride into the liquid system according to the formula, stirring to completely dissolve the zirconium oxychloride, and reacting for 1.5h to obtain the nano cross-linking agent A.
Example 2
The embodiment prepares a nano composite cross-linking agent for fracturing fluid, and the formula of the nano composite cross-linking agent comprises the following components in terms of mole number: 5mol of citric acid, 5mol of ethylenediamine, 25mol of zirconium oxychloride and 2000mL of deionized water.
The specific preparation method comprises the following steps:
the method comprises the following steps: weighing citric acid and ethylenediamine according to the formula, adding into deionized water, and stirring and mixing to obtain a mixed solution; heating the mixed solution to 250 ℃, and reacting for 4 hours to obtain a liquid system of the nano carbon quantum dots;
step two: and adding zirconium oxychloride into the liquid system according to the formula, stirring to completely dissolve the zirconium oxychloride, and reacting for 3 hours to obtain the nano cross-linking agent B.
Example 3
The embodiment prepares a nano composite cross-linking agent for fracturing fluid, and the formula of the nano composite cross-linking agent comprises the following components in terms of mole number: 5mol of citric acid, 4mol of diethylenetriamine, 15mol of zirconium oxychloride and 2000mL of deionized water.
The specific preparation method comprises the following steps:
the method comprises the following steps: weighing citric acid and diethylenetriamine according to the formula, adding into deionized water, and stirring and mixing to obtain a mixed solution; heating the mixed solution to 200 ℃, and reacting for 5 hours to obtain a liquid system of the nano carbon quantum dots;
step two: and adding zirconium oxychloride into the liquid system according to the formula, stirring to completely dissolve the zirconium oxychloride, and reacting for 2 hours to obtain the nano cross-linking agent C.
Example 4
The embodiment prepares a nano composite cross-linking agent for fracturing fluid, and the formula of the nano composite cross-linking agent comprises the following components in terms of mole number: 5mol of citric acid, 4mol of diethylenetriamine, 15mol of titanium chloride and 2000mL of deionized water.
The specific preparation method comprises the following steps:
the method comprises the following steps: weighing citric acid and diethylenetriamine according to the formula, adding into deionized water, and stirring and mixing to obtain a mixed solution; heating the mixed solution to 200 ℃, and reacting for 5 hours to obtain a liquid system of the nano carbon quantum dots;
step two: and adding titanium chloride into the liquid system according to the formula, stirring to completely dissolve the titanium oxychloride, and reacting for 2 hours to obtain the nano cross-linking agent D.
Example 5
The embodiment prepares a nano composite cross-linking agent for fracturing fluid, and the formula of the nano composite cross-linking agent comprises the following components in terms of mole number: 5mol of citric acid, 4mol of polyethyleneimine, 15mol of titanium chloride and 2000mL of deionized water.
The specific preparation method comprises the following steps:
the method comprises the following steps: weighing citric acid and polyethyleneimine according to the formula, adding the citric acid and the polyethyleneimine into deionized water, and stirring and mixing to obtain a mixed solution; heating the mixed solution to 200 ℃, and reacting for 5 hours to obtain a liquid system of the nano carbon quantum dots;
step two: and adding titanium chloride into the liquid system according to the formula, stirring to completely dissolve zirconium oxychloride, and reacting for 2h to obtain the nano cross-linking agent E.
Example 6
The embodiment prepares a nano composite cross-linking agent for fracturing fluid, and the formula of the nano composite cross-linking agent comprises the following components in terms of mole number: 5mol of citric acid, 2mol of ethanolamine, 2mol of triethylene tetramine, 15mol of titanium chloride and 2000mL of deionized water.
The specific preparation method comprises the following steps:
the method comprises the following steps: weighing citric acid, ethanolamine and triethylene tetramine according to the formula, adding into deionized water, and stirring and mixing to obtain a mixed solution; heating the mixed solution to 200 ℃, and reacting for 5 hours to obtain a liquid system of the nano carbon quantum dots;
step two: and adding titanium chloride into the liquid system according to the formula, stirring to completely dissolve zirconium oxychloride, and reacting for 2 hours to obtain the nano cross-linking agent F.
Example 7
The embodiment prepares a nano composite cross-linking agent for fracturing fluid, and the formula of the nano composite cross-linking agent comprises the following components in terms of mole number: 5mol of citric acid, 2mol of ethanolamine, 2mol of triethylene tetramine, 10mol of titanium chloride, 5mol of zirconium oxychloride and 2000mL of deionized water.
The specific preparation method comprises the following steps:
the method comprises the following steps: weighing citric acid, ethanolamine and triethylene tetramine according to the formula, adding into deionized water, and stirring and mixing to obtain a mixed solution; heating the mixed solution to 200 ℃, and reacting for 5 hours to obtain a liquid system of the nano carbon quantum dots;
step two: and adding titanium chloride and zirconium oxychloride into the liquid system according to the formula, stirring to completely dissolve the zirconium oxychloride, and reacting for 2h to obtain the nano cross-linking agent G.
Comparative example 1
Formulation in moles: 5mol of citric acid, 2mol of ethanolamine, 2mol of triethylene tetramine, 2000mL of deionized water were used as comparative example 1, and the preparation method was the same as the time step one of example 7, to obtain comparative sample 1 of comparative example 1.
Comparative example 2
Comparative sample 2 of comparative example 2 was prepared with 10 moles of titanium chloride, 5 moles of zirconium oxychloride, and 2000mL of deionized water.
Adding the products A-G obtained in examples 1-7 and comparative examples 1-2 and the comparative samples 1-2 into a phosphate gelling agent respectively, adding the phosphate gelling agent into n-hexane for crosslinking to prepare fracturing fluid gel, and measuring the viscosity of the prepared products at room temperature respectively; shearing the viscosity for 2 hours at the rotating speed of 120 ℃ and 170r/min and shearing the viscosity for 2 hours at the rotating speed of 150 ℃ and 170r/min to determine the temperature resistance and the shearing resistance of the products A to G and the comparison samples 1 to 2; the mass fractions of the products A to G and the comparative samples 1 to 2 added with normal hexane are both 4%; the mass fraction of the phosphate gelling agent added into n-hexane is 6%, and the test result is as follows:
from the above evaluation results, it can be seen that the cross-linking agent prepared by the present application has good viscosity, excellent temperature resistance and shear resistance, and is simple to prepare and good in stability.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (8)
1. The nano composite cross-linking agent for the fracturing fluid is characterized by comprising a chelate synthesized by nano carbon quantum dots and metal ions, wherein the metal ions are at least one of zirconium ions and titanium ions.
2. The nanocomposite cross-linking agent for the fracturing fluid of claim 1, wherein the nanocarbon quantum dots are nitrogen-doped carbon quantum dots.
3. The preparation method of the nanocomposite cross-linking agent for the fracturing fluid, which is described in any one of claims 1 to 2, is characterized by comprising the following steps:
the method comprises the following steps: preparing nano carbon quantum dots;
step two: and adding inorganic salt of metal ions into the prepared nano carbon quantum dots, and reacting for 1.5-3 h to obtain the nano cross-linking agent.
4. The preparation method according to claim 3, wherein in the first step, the specific steps for preparing the nano carbon quantum dots are as follows: dissolving citric acid with the effective concentration of more than 99.5% and organic amine with the effective concentration of more than 99.5% in deionized water to obtain a mixed solution, heating the mixed solution to 180-250 ℃, and reacting for 4-8 hours to obtain the nano carbon quantum dot.
5. The method according to claim 4, wherein the organic amine is at least one of ethanolamine, ethylenediamine, diethylenetriamine, triethylenetetramine, and polyethyleneimine.
6. The preparation method according to claim 4, wherein the mass ratio of the citric acid to the organic amine is 1: 0.5-1.
7. The preparation method according to claim 4, wherein the molar ratio of the metal ions to the citric acid is 1: 1-5.
8. The method according to claim 3, wherein the inorganic salt of metal ion is at least one of zirconium oxychloride, zirconium basic carbonate, zirconium fluoride, titanium chloride and titanium fluoride.
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