CN116200182A - Crosslinking agent for ultralow-concentration vegetable gum fracturing fluid and synthesis process and application thereof - Google Patents
Crosslinking agent for ultralow-concentration vegetable gum fracturing fluid and synthesis process and application thereof Download PDFInfo
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- 239000012530 fluid Substances 0.000 title claims abstract description 73
- 239000003431 cross linking reagent Substances 0.000 title claims abstract description 51
- 229920001938 Vegetable gum Polymers 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 13
- 230000008569 process Effects 0.000 title claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 title abstract description 7
- 238000003786 synthesis reaction Methods 0.000 title abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910021538 borax Inorganic materials 0.000 claims abstract description 34
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 34
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 34
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 31
- 239000008103 glucose Substances 0.000 claims abstract description 31
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims abstract description 23
- 239000000600 sorbitol Substances 0.000 claims abstract description 23
- 229940015043 glyoxal Drugs 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims abstract description 7
- 150000007529 inorganic bases Chemical class 0.000 claims abstract description 5
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 25
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229920002907 Guar gum Polymers 0.000 abstract description 14
- 239000000665 guar gum Substances 0.000 abstract description 14
- 229960002154 guar gum Drugs 0.000 abstract description 14
- 235000010417 guar gum Nutrition 0.000 abstract description 14
- 239000000843 powder Substances 0.000 abstract description 5
- 238000010008 shearing Methods 0.000 abstract description 4
- 239000002562 thickening agent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 33
- 239000007788 liquid Substances 0.000 description 8
- 239000004971 Cross linker Substances 0.000 description 7
- 239000002585 base Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 5
- 230000006378 damage Effects 0.000 description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
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- 238000005516 engineering process Methods 0.000 description 3
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- 238000006703 hydration reaction Methods 0.000 description 3
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- 239000003973 paint Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
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- 238000010668 complexation reaction Methods 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
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- 230000035484 reaction time Effects 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 244000007835 Cyamopsis tetragonoloba Species 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
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- 238000005485 electric heating Methods 0.000 description 1
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- 238000009472 formulation Methods 0.000 description 1
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- 230000000887 hydrating effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920002521 macromolecule Polymers 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
- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
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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
- C09K8/84—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
- C09K8/887—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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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
- C09K8/84—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
- C09K8/90—Compositions based on water or polar solvents containing organic compounds macromolecular compounds of natural origin, e.g. polysaccharides, cellulose
- C09K8/905—Biopolymers
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- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a cross-linking agent for an ultralow-concentration vegetable gum fracturing fluid, and a synthesis process and application thereof. Mainly solves the problems of high guar gum usage and residue content of the prior vegetable gum fracturing fluid prepared by using a cross-linking agent. The method is characterized in that: the cross-linking agent comprises the following components: inorganic base, borax, glucose, glyoxal, sorbitol and the balance of water; the forming process comprises the following steps: (1) mixing deionized water and sodium hydroxide, heating and reacting; (2) adding borax into the solution in the step (1) in sequence; glucose; (3) Adding glyoxal and sorbitol into the solution in the step (2), performing airtight heating reaction, reacting for a certain time, and cooling to room temperature by water to obtain a product. The cross-linking agent breaks through the concentration ratio limit of the existing minimum guar gum powder of the fracturing fluid for the medium-high temperature well, the cross-linking agent and the vegetable gum thickening agent which is lower than 0.2% can form adjustable gel, the shearing resistance of the formed fracturing fluid system at 80-100 ℃ can meet the requirements of industry standards, and the residue content is low.
Description
Technical field:
the invention relates to the technical field of oilfield exploitation, in particular to a cross-linking agent for an ultralow-concentration vegetable gum fracturing fluid, and a synthesis process and application thereof.
The background technology is as follows:
the fracturing fluid is the most important component in the fracturing technology, and the performance of the fracturing fluid directly influences the fracturing efficiency and the post-fracturing productivity. The vegetable gum fracturing fluid consists of guar gum powder, a cross-linking agent and other additives, is one of the most common fracturing fluids in the fracturing process, and has the characteristics of low friction resistance, good stability, strong sand carrying capacity and the like. The damage of the fracturing fluid gel breaking liquid to the reservoir is mainly as follows: the water lock effect, the expansion of clay minerals, the particle migration, the adsorption retention, the change of reservoir wettability, the blockage of pore channels by residues and the formation of filter cakes by residues. Therefore, the content of the residues of the fracturing fluid can cause certain damage to the reservoir and influence the fracturing effect. And the source of the residues in the fracturing fluid system is guar gum, so that the consumption of the guar gum in the fracturing fluid system is effectively reduced, and the residue content can be reduced.
The boron crosslinked fracturing fluid has the advantages of good viscoelasticity and shearing resistance, is widely applied to fracturing fluid systems, and the dosage of the needed guar gum powder in the fracturing fluid systems at 80-100 ℃ is generally 0.28-0.40% by using the organic boron crosslinking agent developed at home at present.
The invention comprises the following steps:
the invention aims to solve the problems of high guar gum usage, high residue content and high construction cost of the existing vegetable gum fracturing fluid prepared by using the existing cross-linking agent in the background art, and provides the cross-linking agent for the ultralow-concentration vegetable gum fracturing fluid. The fracturing fluid system formed by the cross-linking agent has the advantages of good sand carrying performance and low residue content, not only can reduce the dosage of guar gum in single well construction, but also can reduce stratum injury, and breaks through the concentration proportioning limit of the existing minimum guar gum powder of the fracturing fluid for high-temperature wells at 80-100 ℃ in China. The invention provides a synthesis process and application of a cross-linking agent for an ultralow-concentration vegetable gum fracturing fluid.
In order to achieve the above purpose, the first aspect of the present invention provides a cross-linking agent for an ultra-low concentration vegetable gum fracturing fluid, comprising the following components: inorganic base, borax, glucose, glyoxal, sorbitol and the balance of water.
Preferably, the water is deionized water; the inorganic base is sodium hydroxide.
Preferably, the components are prepared from the following components in percentage by mass: 4.8 to 5.1 percent of inorganic alkali, 20.5 to 21.1 percent of borax, 15.3 to 15.8 percent of glucose, 2.5 to 3.1 percent of glyoxal, 3.2 to 3.6 percent of sorbitol and the balance of water.
The invention provides a process for synthesizing a cross-linking agent for an ultralow-concentration vegetable gum fracturing fluid, which comprises the following steps of:
(1) Mixing deionized water and sodium hydroxide according to a certain proportion, heating for reaction, and stirring until the solution is uniform;
(2) The reaction temperature is kept to be not higher than 80 ℃;
(3) Adding borax into the solution in the step (1) according to a proportion, and mixing and stirring until the borax is dissolved;
(4) Adding glucose into the solution in the step (3) according to a proportion, mixing and stirring until the glucose is dissolved;
(5) And (3) adding glyoxal and sorbitol into the solution in the step (4) according to a certain proportion, performing airtight heating reaction, reacting for a certain time, and cooling to room temperature by water to obtain a product.
Preferably, the heating reaction temperature in the step (1) is controlled to be 75-80 ℃. The closed reaction condition is that the reaction is carried out for 180min at 80 ℃.
Preferably, the closed reaction condition of the step (5) is that the reaction is carried out for 180min at 80 ℃.
The invention provides an application of a cross-linking agent for a vegetable gum fracturing fluid with ultralow concentration in the vegetable gum fracturing fluid.
Preferably, the cross-linking agent for the ultralow-concentration vegetable gum fracturing fluid is used in an amount of 0.25-0.35%.
The crosslinking agent for the ultralow-concentration vegetable gum fracturing fluid has the following action mechanism: and directly modifying borax by utilizing hydrolysis reaction and complexation reaction to form larger particle size of the organic boron crosslinking agent. Firstly, borax is hydrolyzed to prepare borate aqueous solution, chemical reagents are added according to a certain sequence, and the reaction temperature and the synthesis time are strictly controlled. Wherein, the addition of sodium hydroxide provides an environment for the hydrolysis of borax, which is favorable for the forward hydrolysis reaction; glyoxal and sorbitol can improve the stability of the solution and avoid precipitation; the polyhydroxy macromolecular compound glucose is coordinated with borax to carry out complexation reaction, so that the formed organic boron cross-linking agent has larger particle size, FHG molecules with longer distance in the solution can be connected together to form gel, and the use amount of FHG is reduced. The novel cross-linking agent prepared by the method has good performance, stable state and convenient storage.
Compared with the background technology, the invention has the following beneficial effects:
the fracturing fluid system formed by the cross-linking agent has the advantages of good sand carrying performance, low residue content and the like, can reduce the dosage of guar gum in single well construction, can reduce stratum injury, and breaks through the concentration proportioning limit of the minimum guar gum powder in the prior fracturing fluid for high-temperature wells at 80-100 ℃ in China.
The pH value of the cross-linking agent synthesized by the invention is 11, the gel forming time of the cross-linking agent and 0.18 percent of quick hydration guar gum aqueous solution is 20s, and the gel is at 90 ℃ for 170s -1 Shearing for 60min until the viscosity is about 58 mPa.s; the residue is 96.2mg/L; the viscosity of the gel-breaking solution is 2.1 Pa.s after 6 hours.
Drawings
FIG. 1 is a graph showing the shear profile of a fracturing fluid using a cross-linking agent for an ultra-low concentration vegetable gum fracturing fluid in accordance with an embodiment of the present invention.
The specific embodiment is as follows:
the invention is further illustrated by the following examples in conjunction with the accompanying drawings:
the following examples were conducted to determine the pH value, crosslinking time, temperature and shear resistance, gel breaking property, and residue content, respectively:
(1) pH value: measured with a precision pH test paper or a pH meter.
(2) Crosslinking time: the time taken for the cross-linking agent to be added to the blender until the vortex disappeared to slightly protrude from the liquid surface was recorded with a stopwatch based on 400mL of base solution.
(3) Temperature and shear resistance: measuring base liquid according to the requirements of sample cylinders of rheometers of different models, placing the base liquid in a beaker, adding crosslinking liquid into the base liquid according to the crosslinking proportion in the fracturing liquid formula, crosslinking the base liquid into gel, placing the crosslinked gel in the sample cup of the rheometer, heating the sample after the temperature reaches the temperature required to be tested, and rotating for 170s -1 The shear rate is rotated, the shear rate and temperature are maintained unchanged until the required shear time is reached, and the final viscosity is recorded.
(4) Gel breaking performance: putting the fracturing fluid gel into a closed container, heating in a constant temperature drying oven to constant temperature, taking the gel breaking fluid supernatant fluid after 6 hours, and measuring the gel breaking fluid viscosity by using a capillary viscometer, wherein the measurement temperature is about room temperature (25 ℃).
(5) Residue content: measuring 50mL of fracturing fluid, placing the fracturing fluid into a closed container, heating the fracturing fluid at a constant temperature, thoroughly breaking the gel at the constant temperature of a reservoir, pouring all the gel-breaking fluid into a centrifuge tube with dried constant weight, placing the centrifuge tube into the centrifuge, centrifuging for 30min at a rotating speed of 3000r/min +/-150 r/min, slowly pouring out supernatant, adding distilled water to 50mL, stirring and washing a residue sample by using a glass rod, placing the residue sample into the centrifuge, centrifuging for 20min, pouring the supernatant, placing the centrifuge tube into a constant-temperature electric heating drying oven, and drying to constant temperature at 110+/-1 ℃. And calculating the residue content.
Example 1:
the cross-linking agent for the ultralow-concentration vegetable gum fracturing fluid comprises the following components in parts by weight, 52 parts of deionized water, 5 parts of sodium hydroxide, 21 parts of borax, 15.5 parts of glucose, 3 parts of glyoxal and 3.5 parts of sorbitol.
The preparation method comprises the following steps:
(1) Adding 52 parts of deionized water and 5 parts of sodium hydroxide into a reaction kettle in proportion, controlling the temperature of the reaction kettle to be 75-80 ℃, and stirring until the solution is uniform;
(2) Maintaining the temperature of the reaction kettle at 80 ℃ (not higher than the temperature);
(3) Adding 21 parts of borax into the solution in the step (1) according to a proportion, mixing and stirring until the borax is dissolved;
(4) Adding 15.5 parts of glucose into the solution in the step (3) according to a proportion, mixing and stirring until the glucose is dissolved;
(5) Adding 3 parts of glyoxal and 3.5 parts of sorbitol into the solution in the step (4) according to a proportion, sealing the reaction kettle, reacting for 180min at 80 ℃, and cooling to room temperature by water to obtain the product.
The fracturing fluid system using the cross-linking agent prepared in example 1 (fracturing fluid formula: 0.18% of fast hydration guar gum+0.1% of sodium carbonate+0.02% of sodium bicarbonate+0.3% of cross-linking agent for a vegetable gum fracturing fluid) continuously shears for 60 minutes at 90 ℃ and 170s < -1 > to meet the industrial production requirements, the content of residues is far lower than that of a common vegetable gum water-based fracturing fluid, the overall performance evaluation of the fracturing fluid using the cross-linking agent for the vegetable gum fracturing fluid with the ultra-low concentration is compared with that of the fracturing fluid with the common vegetable gum water-based fracturing fluid, the shear curve of the fracturing fluid using the cross-linking agent for the vegetable gum fracturing fluid with the ultra-low concentration is shown in figure 1.
Comparative example 2:
the water-based paint comprises, by weight, 49 parts of deionized water, 5 parts of sodium hydroxide, 24 parts of borax, 15.5 parts of glucose, 3 parts of glyoxal and 3.5 parts of sorbitol.
The preparation method comprises the following steps:
(1) Adding 49 parts of deionized water and 5 parts of sodium hydroxide into a reaction kettle in proportion, controlling the temperature of the reaction kettle to be 75-80 ℃, and stirring until the solution is uniform;
(2) Maintaining the temperature of the reaction kettle at 80 ℃ (not higher than the temperature);
(3) Adding 24 parts of borax into the solution in the step (1) according to a proportion, mixing and stirring until the borax is dissolved;
(4) Adding 15.5 parts of glucose into the solution in the step (3) according to a proportion, mixing and stirring until the glucose is dissolved;
(5) Adding 3 parts of glyoxal and 3.5 parts of sorbitol into the solution in the step (4) according to a proportion, sealing the reaction kettle, reacting for 180min at 80 ℃, and cooling to room temperature by water to obtain the product.
The performance of the synthetic cross-linking agent with different borax amounts is compared with that shown in Table 1.
TABLE 1 comparison of the properties of the synthetic crosslinkers with different borax usage
Comparative example 3:
the water-based paint comprises the following components, by weight, 46.5 parts of deionized water, 5 parts of sodium hydroxide, 21 parts of borax, 21 parts of glucose, 3 parts of glyoxal and 3.5 parts of sorbitol.
The preparation method comprises the following steps:
(1) Adding 46.5 parts of deionized water and 5 parts of sodium hydroxide into a reaction kettle in proportion, controlling the temperature of the reaction kettle to be 75-80 ℃, and stirring until the solution is uniform;
(2) Maintaining the temperature of the reaction kettle at 80 ℃ (not higher than the temperature);
(3) Adding 21 parts of borax into the solution in the step (1) according to a proportion, mixing and stirring until the borax is dissolved;
(4) Adding 21 parts of glucose into the solution in the step (3) according to a proportion, mixing and stirring until the glucose is dissolved;
(5) Adding 3 parts of glyoxal and 3.5 parts of sorbitol into the solution in the step (4) according to a proportion, sealing the reaction kettle, reacting for 180min at 80 ℃, and cooling to room temperature by water to obtain the product.
The performance of the synthetic cross-linker for different amounts of glucose is compared in Table 2.
TABLE 2 different glucose levels comparison of synthetic crosslinker Properties
Comparative example 4:
the water-based paint comprises the following components, by weight, 45 parts of deionized water, 5 parts of sodium hydroxide, 21 parts of borax, 15.5 parts of glucose, 3 parts of glyoxal and 10.5 parts of sorbitol.
The preparation method comprises the following steps:
(1) Adding 45 parts of deionized water and 5 parts of sodium hydroxide into a reaction kettle in proportion, controlling the temperature of the reaction kettle to be 75-80 ℃, and stirring until the solution is uniform;
(2) Maintaining the temperature of the reaction kettle at 80 ℃ (not higher than the temperature);
(3) Adding 21 parts of borax into the solution in the step (1) according to a proportion, mixing and stirring until the borax is dissolved;
(4) Adding 15.5 parts of glucose into the solution in the step (3) according to a proportion, mixing and stirring until the glucose is dissolved;
(5) Adding 3 parts of glyoxal and 10.5 parts of sorbitol into the solution in the step (4) according to a proportion, sealing the reaction kettle, reacting for 180min at 80 ℃, and cooling to room temperature by water to obtain the product.
The performance of the synthetic cross-linking agent for different sorbitol levels is compared in Table 3.
TABLE 3 comparison of the Properties of the synthetic Cross-linking Agents with different sorbitol usage
Comparative example 5:
the cross-linking agent for the ultralow-concentration vegetable gum fracturing fluid comprises the following components in parts by weight, 52 parts of deionized water, 5 parts of sodium hydroxide, 21 parts of borax, 15.5 parts of glucose, 3 parts of glyoxal and 3.5 parts of sorbitol.
The preparation method comprises the following steps:
(1) Adding 52 parts of deionized water and 5 parts of sodium hydroxide into a reaction kettle in proportion, controlling the temperature of the reaction kettle to be 65-70 ℃, and stirring until the solution is uniform;
(2) Maintaining the temperature of the reaction kettle at 70 ℃ (not higher than the temperature);
(3) Adding 21 parts of borax into the solution in the step (1) according to a proportion, mixing and stirring until the borax is dissolved;
(4) Adding 15.5 parts of glucose into the solution in the step (3) according to a proportion, mixing and stirring until the glucose is dissolved;
(5) Adding 3 parts of glyoxal and 3.5 parts of sorbitol into the solution in the step (4) according to a proportion, sealing the reaction kettle, reacting for 180min at 70 ℃, and cooling to room temperature by water to obtain the product.
The comparison of the properties of the synthetic cross-linker at different reaction temperatures is shown in Table 4.
TABLE 4 comparison of the properties of the synthetic crosslinkers at different reaction temperatures
Comparative example 6:
the cross-linking agent for the ultralow-concentration vegetable gum fracturing fluid comprises the following components in parts by weight, 52 parts of deionized water, 5 parts of sodium hydroxide, 21 parts of borax, 15.5 parts of glucose, 3 parts of glyoxal and 3.5 parts of sorbitol.
The preparation method comprises the following steps:
(1) Adding 52 parts of deionized water and 5 parts of sodium hydroxide into a reaction kettle in proportion, controlling the temperature of the reaction kettle to be 75-80 ℃, and stirring until the solution is uniform;
(2) Maintaining the temperature of the reaction kettle at 80 ℃ (not higher than the temperature);
(3) Adding 21 parts of borax into the solution in the step (1) according to a proportion, mixing and stirring until the borax is dissolved;
(4) Adding 15.5 parts of glucose into the solution in the step (3) according to a proportion, mixing and stirring until the glucose is dissolved;
(5) Adding 3 parts of glyoxal and 3.5 parts of sorbitol into the solution in the step (4) according to a proportion, sealing the reaction kettle, reacting for 120min at 80 ℃, and cooling to room temperature by water to obtain the product.
The comparison of the properties of the synthetic cross-linker at different reaction times is shown in Table 5.
TABLE 5 comparison of the properties of the synthetic crosslinkers at different reaction times
Comparative example 1 was performed:
fracturing fluid formulation using other cross-linking agents:
0.30% fast hydrating guar +0.1% sodium carbonate +0.02% sodium bicarbonate +0.3% cross-linking agent for fracturing fluid; the performance of the fracturing fluid using the cross-linking agent for the ultra-low concentration vegetable gum fracturing fluid prepared in example 1 of the present invention is compared with that of the common vegetable gum base fracturing fluid, and is shown in table 6.
Table 6 table of fracturing fluid and plain vegetable gum base fracturing fluid performance using cross-linking agent for ultra low concentration vegetable gum fracturing fluid
Table 6 shows that the above results show that the pH of the synthesized cross-linking agent of the invention is 11, the gel time with 0.18% of quick hydration guar gum aqueous solution is 20s, the gel is at 90 ℃ for 170s -1 Shearing for 60min until the viscosity is about 58 mPa.s; the residue is 96.2mg/L; the viscosity of the gel-breaking solution is 2.1 Pa.s after 6 hours. The fracturing fluid system formed by the cross-linking agent has the advantages of good sand carrying performance, low residue content and the like. Can reduce the damage of residues to stratum after breaking the vegetable gum fracturing fluid, and improve the recovery ratio.
It should be noted that the above-described embodiments are only for explaining the present invention and do not constitute any limitation of the present invention. The invention has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the invention as defined in the appended claims, and the invention may be modified without departing from the scope and spirit of the invention. Although the invention is described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, as the invention extends to all other means and applications which perform the same function. Therefore, it is intended that the invention not be limited to the embodiments disclosed as the best mode contemplated for carrying out this invention, but that the invention will include all equivalent modifications and variations upon the scope of the present invention as defined by the appended claims.
Claims (8)
1. A cross-linking agent for an ultralow-concentration vegetable gum fracturing fluid is characterized in that: the composition comprises the following components: inorganic base, borax, glucose, glyoxal, sorbitol and the balance of water.
2. The cross-linking agent for the ultralow-concentration vegetable gum fracturing fluid according to claim 1, which is characterized in that: the water is deionized water; the inorganic base is sodium hydroxide.
3. The cross-linking agent for the ultralow-concentration vegetable gum fracturing fluid according to claim 1, which is characterized in that: the components are as follows in percentage by mass: 4.8 to 5.1 percent of inorganic alkali, 20.5 to 21.1 percent of borax, 15.3 to 15.8 percent of glucose, 2.5 to 3.1 percent of glyoxal, 3.2 to 3.6 percent of sorbitol and the balance of water.
4. A process for synthesizing a cross-linking agent for an ultralow-concentration vegetable gum fracturing fluid, which comprises the following steps:
(1) Mixing deionized water and sodium hydroxide according to a certain proportion, heating for reaction, and stirring until the solution is uniform;
(2) The reaction temperature is kept to be not higher than 80 ℃;
(3) Adding borax into the solution in the step (1) according to a proportion, and mixing and stirring until the borax is dissolved;
(4) Adding glucose into the solution in the step (3) according to a proportion, mixing and stirring until the glucose is dissolved;
(5) And (3) adding glyoxal and sorbitol into the solution in the step (4) according to a certain proportion, performing airtight heating reaction, reacting for a certain time, and cooling to room temperature by water to obtain a product.
5. The process for synthesizing the cross-linking agent for the ultralow-concentration vegetable gum fracturing fluid, which is characterized by comprising the following steps of: the heating reaction temperature in the step (1) is controlled at 75-80 ℃; the closed reaction condition is that the reaction is carried out for 180min at 80 ℃.
6. The process for synthesizing the cross-linking agent for the ultralow-concentration vegetable gum fracturing fluid, which is characterized by comprising the following steps of: the closed reaction condition of the step (5) is that the reaction is carried out for 180min at 80 ℃.
7. The use of a cross-linking agent for a vegetable gum fracturing fluid of ultra-low concentration according to claim 1 in a vegetable gum fracturing fluid.
8. The use according to claim 7, characterized in that: the cross-linking agent for the ultralow-concentration vegetable gum fracturing fluid is used in an amount of 0.25-0.35%.
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