CN112126420A - Crosslinking agent for fracturing and preparation method thereof - Google Patents
Crosslinking agent for fracturing and preparation method thereof Download PDFInfo
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- 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
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- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
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- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
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Abstract
The invention relates to the technical field of shale gas fracturing, which is used for solving the problem that the delay time of a conventional polyacrylamide and derivative crosslinking agent thereof is not adjustable and has narrow adaptability, and particularly relates to a crosslinking agent for fracturing and a preparation method thereof, wherein the crosslinking agent comprises the following components, by weight, 5-15 parts of zirconium oxychloride, 5-15 parts of a titanium compound, 5-15 parts of an aluminum salt, 35-65 parts of deionized water, 5-45 parts of polyhydric alcohol, 0.5-2 parts of a hydrolysis reaction catalyst, 5-35 parts of organic acid, 0.1-3 parts of a delay regulator and 1-5 parts of a dispersion stabilizer; the preparation method comprises mixing the raw materials, and refluxing under certain conditions; the cross-linking agent is prepared by adding a delay regulator into component raw materials for preparing the cross-linking agent, and simultaneously controlling the dosage ratio of the delay regulator to other components, so that the delay time of the cross-linking agent is freely adjusted to be 10-150 seconds, and meanwhile, the added dispersion stabilizer enables the cross-linking agent to have wider adaptability and good compatibility with most of polyacrylamide and derivatives thereof in the market.
Description
Technical Field
The invention relates to the technical field of shale gas fracturing, aims to solve the problem that a conventional crosslinking agent of polyacrylamide and derivatives thereof cannot delay time and has narrow adaptability, and particularly relates to a crosslinking agent for fracturing and a preparation method thereof.
Background
The shale has extremely low permeability and porosity, so a natural fracture network is required to exist for producing natural gas, in a shale area, fracturing is to form the natural fracture network and create a natural gas migration channel, and when fracturing is carried out by adopting a fracturing fluid method, the compatibility of the fracturing fluid needs to be considered, wherein a cross-linking agent is a main component.
Some researches on a crosslinking agent for fracturing also appear at present, for example, the general overview of the delayed crosslinking profile control technology disclosed in the 2006, the 01 st stage of Guangzhou chemical industry explains the important role of the delayed crosslinking profile control technology in the aspect of improving the recovery ratio of crude oil; the preparation of the organic zirconium composite cross-linking agent and the research on the cross-linking performance thereof are disclosed in a paper written by Lejunnie of the Western An Petroleum university, and particularly, the composite organic zirconium cross-linking agent is obtained by compounding glyoxal and zirconium oxide on the basis of organic zirconium; the synthesis and application of an organic zirconium crosslinking agent disclosed in journal of university of Shaanxi science and technology in 2013, 03, discloses preparation of an acidic organic zirconium crosslinking agent for a high-molecular polymer hydrolyzed polyacrylamide water-based fracturing fluid.
However, the problem that the delay time of the crosslinking agent is not adjustable and the adaptability is narrow still exists at present.
Disclosure of Invention
Aiming at the problem that the delay time of a cross-linking agent is still not adjustable and the adaptability is narrow at present, the application provides the cross-linking agent for fracturing and a preparation method thereof, the delay adjusting agent is added into component raw materials for preparing the cross-linking agent, and the dosage ratio of the delay adjusting agent to other components is controlled at the same time, so that the cross-linking agent and various PAM aqueous solutions with the dosage of 0.15-0.45 percent have the effect of freely adjusting the delay time to 10-150 seconds, and meanwhile, the cross-linking agent has wider adaptability and good compatibility with most polyacrylamide and derivatives thereof on the market.
The technical scheme provided by the invention is that the cross-linking agent for fracturing comprises, by weight, 5-15 parts of zirconium oxychloride, 5-15 parts of titanium compound, 5-15 parts of aluminum salt, 35-65 parts of deionized water, 5-45 parts of polyol, 0.5-2 parts of a hydrolysis reaction catalyst, 5-35 parts of organic acid, 0.1-3 parts of a delay regulator and 1-5 parts of a dispersion stabilizer.
A cross-linking agent for fracturing comprises, by weight, 8-12 parts of zirconium oxychloride, 8-12 parts of a titanium compound, 8-12 parts of an aluminum salt, 45-55 parts of deionized water, 10-25 parts of a polyol, 1-1.5 parts of a hydrolysis reaction catalyst, 10-25 parts of an organic acid, 0.5-1.5 parts of a retardation regulator, and 2-4 parts of a dispersion stabilizer. After 0.3 part of the synthetic product is mixed with 100 parts of various 0.3 percent PAM aqueous solutions, the effect of delaying 110s crosslinking can be achieved at 70 ℃, and the compatibility is good.
A cross-linking agent for fracturing comprises, by weight, 10 parts of zirconium oxychloride, 10 parts of a titanium compound, 10 parts of aluminum salt, 50 parts of deionized water, 20 parts of polyol, 1.2 parts of a hydrolysis reaction catalyst, 20 parts of an organic acid, 1 part of a delay regulator and 3 parts of a dispersion stabilizer. After 0.2 part of the synthetic product is mixed with 100 parts of 0.4 percent HPAM aqueous solution, the effect of delaying 130s crosslinking can be achieved at 70 ℃, and the compatibility is good.
By adopting the technical scheme, zirconium oxychloride, titanium compound and aluminum salt are used as main components, and are matched with the added delay regulator, so that the cross-linking agent and various PAM aqueous solutions with the addition of 0.15-0.6% have the effect of freely adjusting the delay time to 10-150 seconds, and meanwhile, the added dispersion stabilizer enables the cross-linking agent to have wider adaptability and good compatibility with most polyacrylamide and derivatives thereof in the market; meanwhile, when the cross-linking agent is prepared, the reaction effect among the components is better and the reaction is more complete by controlling the dosage ratio among the components, the performance of the cross-linking agent is improved, the yield of the product is higher, and the synergistic effect among the reactants is better.
Further, the titanium compound comprises one or more of tetrabutyl titanate, titanium tetrachloride and titanium dioxide.
Further, the aluminum salt comprises any one or more of aluminum trichloride, aluminum sulfate and aluminum potassium sulfate dodecahydrate; the polyhydric alcohol comprises any one or more of ethylene glycol, isopropanol, triethanolamine, glycerol and n-propanol.
Further, the hydrolysis reaction catalyst comprises any one or more of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
Further, the organic acid comprises any one or more of acetic acid, citric acid, salicylic acid, lactic acid and acetylacetone.
Further, the delay regulator comprises any one or more of xylitol, mannitol, maltitol, tartaric acid and sodium tartrate.
Further, the dispersion stabilizer comprises one or more of PEG400, PEG800, PEG10000, PEG20000, polyallyl alcohol 1788, polyoxyethylene ether and AEO-09.
In order to achieve the above object, the present application also provides a preparation method of the crosslinking agent for fracturing, which is characterized by comprising the following steps:
(1) proportionally adding zirconium oxychloride, a titanium compound, an aluminum salt and deionized water into a four-neck flask, heating a water bath kettle to 55-85 ℃, installing a condensing tube in the four-neck flask, and keeping refluxing for 10-30 minutes;
(2) adding polyhydric alcohol into the solution obtained in the step (1) according to the proportion, and mixing and stirring for 30-60 minutes;
(3) adding a hydrolysis reaction catalyst into the solution obtained in the step (2) in proportion, and uniformly stirring;
(4) adding organic acid into the solution obtained in the step (3) according to a certain proportion, and condensing and refluxing for 30-300 minutes at the temperature of 55-85 ℃;
(5) and (4) adding a delay regulator and a dispersion stabilizer into the solution obtained in the step (4) according to the proportion, and continuously carrying out condensation reflux for 30-60 minutes at the temperature of 55-85 ℃ to obtain a product.
Based on the explanation, compared with the prior art, the technical scheme of the application has the advantages that:
(1) the delay regulator added in the invention can freely adjust the delay time to 10-150 seconds according to the requirement;
(2) the dispersion stabilizer added in the invention has wider adaptability and good compatibility with most of polyacrylamide and derivatives thereof on the market;
(3) according to the invention, the dosage ratio of the raw material components is controlled, so that the reaction effect is better, the reaction is more complete, the performance of the obtained product is better, and the yield of the product is high;
(4) the preparation method of the cross-linking agent has simple process flow and high preparation efficiency.
Detailed Description
Example 1
The crosslinking agent for fracturing comprises, by weight, 5 parts of zirconium oxychloride, 5 parts of n-butyl titanate, 5 parts of aluminum trichloride, 35 parts of deionized water, 5 parts of ethylene glycol, 0.5 part of sodium hydroxide, 5 parts of acetic acid, 0.1 part of xylitol and 1 part of PEG 400. After 0.3 part of the synthetic product is mixed with 100 parts of 0.4% aqueous solution of anionic polyacrylamide from a manufacturer A, the effect of delaying 180s crosslinking can be achieved at 70 ℃, and the compatibility is good.
The preparation method comprises the following steps:
(1) proportionally adding zirconium oxychloride, n-butyl titanate, aluminum trichloride and deionized water into a four-neck flask, heating a water bath kettle to 55-85 ℃, installing a condenser pipe in the four-neck flask, and keeping refluxing for 10-30 minutes;
(2) adding ethylene glycol into the solution obtained in the step (1) according to a certain proportion, and mixing and stirring for 30-60 minutes;
(3) adding sodium hydroxide into the solution obtained in the step (2) according to a certain proportion, and uniformly stirring;
(4) adding acetic acid into the solution obtained in the step (3) according to a certain proportion, and condensing and refluxing for 30-300 minutes at the temperature of 55-85 ℃;
(5) adding xylitol and PEG400 into the solution obtained in the step (4) according to the proportion, and continuously condensing and refluxing for 30-60 minutes at the temperature of 55-85 ℃ to obtain the product.
Example 2
The cross-linking agent for fracturing comprises the following components, by weight, 15 parts of zirconium oxychloride, 15 parts of titanium tetrachloride, 15 parts of aluminum sulfate, 65 parts of deionized water, 45 parts of isopropanol, 2 parts of potassium hydroxide, 35 parts of citric acid, 3 parts of mannitol and 5 parts of PEG 800. After 0.3 part of the synthetic product is mixed with 100 parts of 0.6 percent aqueous solution of cationic PAM of a manufacturer B, the effect of delaying 50s of crosslinking can be achieved at 70 ℃, and the compatibility is good.
The preparation method specifically comprises the following steps:
(1) proportionally adding zirconium oxychloride, titanium tetrachloride, aluminum sulfate and deionized water into a four-neck flask, heating a water bath kettle to 55-85 ℃, installing a condenser pipe in the four-neck flask, and keeping refluxing for 10-30 minutes;
(2) adding isopropanol into the solution obtained in the step (1) according to a certain proportion, and mixing and stirring for 30-60 minutes;
(3) adding potassium hydroxide into the solution obtained in the step (2) according to a proportion, and uniformly stirring;
(4) adding citric acid into the solution obtained in the step (3) according to a certain proportion, and condensing and refluxing for 30-300 minutes at the temperature of 55-85 ℃;
(5) adding mannitol and PEG800 into the solution obtained in the step (4) according to the proportion, and continuously condensing and refluxing for 30-60 minutes at the temperature of 55-85 ℃ to obtain the product.
Example 3
A cross-linking agent for fracturing comprises, by weight, 8 parts of zirconium oxychloride, 8 parts of titanium dioxide, 8 parts of aluminum potassium sulfate dodecahydrate, 45 parts of deionized water, 10 parts of triethanolamine, 1 part of sodium carbonate, 10 parts of salicylic acid, 0.5 part of maltitol and 2 parts of PEG 10000. After 0.5 part of the synthetic product is mixed with 100 parts of 0.3% aqueous solution of zwitterionic polyacrylamide of manufacturer C, the crosslinking effect of delaying 40s can be achieved at 70 ℃, and the compatibility is good.
The preparation method specifically comprises the following steps:
(1) proportionally adding zirconium oxychloride, titanium dioxide, aluminum potassium sulfate dodecahydrate and deionized water into a four-neck flask, heating a water bath kettle to 55-85 ℃, installing a condensing tube in the four-neck flask, and keeping refluxing for 10-30 minutes;
(2) adding triethanolamine into the solution obtained in the step (1) according to a proportion, and mixing and stirring for 30-60 minutes;
(3) adding sodium carbonate into the solution obtained in the step (2) according to a certain proportion, and uniformly stirring;
(4) adding salicylic acid into the solution obtained in the step (3) according to a certain proportion, and condensing and refluxing for 30-300 minutes at the temperature of 55-85 ℃;
(5) and (4) adding maltitol and PEG10000 into the solution in the step (4) according to the proportion, and continuously condensing and refluxing for 30-60 minutes at the temperature of 55-85 ℃ to obtain the product.
Example 4
The cross-linking agent for fracturing comprises, by weight, 12 parts of zirconium oxychloride, 12 parts of a composition of n-butyl titanate and titanium tetrachloride, 12 parts of a composition of aluminum trichloride and aluminum sulfate, 55 parts of deionized water, 25 parts of glycerol, 1.5 parts of potassium carbonate, 25 parts of lactic acid, 1.5 parts of tartaric acid and 4 parts of PEG 20000. After 0.5 part of the synthetic product is mixed with 100 parts of HPAM 0.4% water solution of manufacturer D, the effect of delaying 15s crosslinking can be achieved at 70 ℃, and the compatibility is good.
The preparation method specifically comprises the following steps:
(1) adding zirconium oxychloride, a composition of n-butyl titanate and titanium tetrachloride, a composition of aluminum trichloride and aluminum sulfate and deionized water into a four-neck flask according to a proportion, heating the temperature of a water bath to 55-85 ℃, installing a condenser pipe in the four-neck flask, and keeping refluxing for 10-30 minutes;
(2) adding glycerol into the solution obtained in the step (1) according to a certain proportion, and mixing and stirring for 30-60 minutes;
(3) adding potassium carbonate into the solution obtained in the step (2) according to a proportion, and uniformly stirring;
(4) adding lactic acid into the solution obtained in the step (3) according to a certain proportion, and condensing and refluxing for 30-300 minutes at the temperature of 55-85 ℃;
(5) adding tartaric acid and PEG20000 into the solution obtained in step (4) in proportion, and continuously performing condensation reflux at 55-85 deg.C for 30-60 min to obtain the product.
Example 5
A cross-linking agent for fracturing comprises, by weight, 10 parts of zirconium oxychloride, 10 parts of a composition of titanium tetrachloride and titanium dioxide, 10 parts of a composition of aluminum sulfate and potassium aluminum sulfate dodecahydrate, 50 parts of deionized water, 20 parts of n-propanol, 1.2 parts of a composition of potassium hydroxide and sodium carbonate, 20 parts of acetylacetone, 1 part of sodium tartrate and 3 parts of a dispersion stabilizer. After 0.3 part of the synthetic product is mixed with 100 parts of 0.2% of anionic polyacrylamide aqueous solution of a manufacturer E, the effect of delaying the crosslinking for 90s can be achieved at 70 ℃, and the compatibility is good.
The preparation method specifically comprises the following steps:
(1) adding zirconium oxychloride, a composition of titanium tetrachloride and titanium dioxide, a composition of aluminum sulfate and aluminum potassium sulfate dodecahydrate and deionized water into a four-neck flask according to a proportion, heating the temperature of a water bath to 55-85 ℃, installing a condenser pipe in the four-neck flask, and keeping refluxing for 10-30 minutes;
(2) adding n-propanol into the solution obtained in the step (1) according to a ratio, and mixing and stirring for 30-60 minutes;
(3) adding the composition of potassium hydroxide and sodium carbonate into the solution obtained in the step (2) according to the proportion, and uniformly stirring;
(4) adding acetylacetone into the solution obtained in the step (3) according to the proportion, and condensing and refluxing for 30-300 minutes at the temperature of 55-85 ℃;
(5) and (4) adding sodium tartrate and polyoxyethylene ether into the solution obtained in the step (4) according to the proportion, and continuously carrying out condensation reflux for 30-60 minutes at the temperature of 55-85 ℃ to obtain the product.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (10)
1. The cross-linking agent for fracturing is characterized by comprising, by weight, 5-15 parts of zirconium oxychloride, 5-15 parts of titanium compound, 5-15 parts of aluminum salt, 35-65 parts of deionized water, 5-45 parts of polyol, 0.5-2 parts of a hydrolysis reaction catalyst, 5-35 parts of organic acid, 0.1-3 parts of a delay regulator and 1-5 parts of a dispersion stabilizer.
2. The crosslinking agent for fracturing of claim 1, which comprises, by weight, 8 to 12 parts of zirconium oxychloride, 8 to 12 parts of titanium compound, 8 to 12 parts of aluminum salt, 45 to 55 parts of deionized water, 10 to 25 parts of polyol, 1 to 1.5 parts of hydrolysis catalyst, 10 to 25 parts of organic acid, 0.5 to 1.5 parts of retardation regulator, and 2 to 4 parts of dispersion stabilizer.
3. The crosslinking agent for fracturing of claim 1, which comprises, in parts by weight, 10 parts of zirconium oxychloride, 10 parts of titanium compound, 10 parts of aluminum salt, 50 parts of deionized water, 20 parts of polyol, 12 parts of hydrolysis catalyst, 20 parts of organic acid, 1 part of retardation regulator, and 3 parts of dispersion stabilizer.
4. A crosslinking agent for fracturing according to any one of claims 1 to 3, wherein the titanium compound comprises one or more of n-butyl titanate, titanium tetrachloride and titanium dioxide.
5. A crosslinking agent for fracturing according to any one of claims 1 to 3, wherein the aluminum salt comprises any one or more of aluminum trichloride, aluminum sulfate, aluminum potassium sulfate dodecahydrate; the polyhydric alcohol comprises any one or more of ethylene glycol, isopropanol, triethanolamine, glycerol and n-propanol.
6. A crosslinking agent for fracturing according to any one of claims 1 to 3, wherein the hydrolysis catalyst comprises any one or more of sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
7. A crosslinking agent for fracturing according to any one of claims 1 to 3, wherein the organic acid comprises any one or more of acetic acid, citric acid, salicylic acid, lactic acid and acetylacetone.
8. The crosslinking agent for fracturing of any one of claims 1 to 3, wherein the retardation regulator comprises any one or more of xylitol, mannitol, maltitol, tartaric acid and sodium tartrate.
9. The crosslinking agent for fracturing of any one of claims 1 to 3, wherein the dispersion stabilizer comprises one or more of PEG400, PEG800, PEG10000, PEG20000, polyallyl alcohol 1788, polyoxyethylene ether, and AEO-09.
10. The preparation method of the crosslinking agent for fracturing, which is characterized by comprising the following steps:
(1) proportionally adding zirconium oxychloride, a titanium compound, an aluminum salt and deionized water into a four-neck flask, heating a water bath kettle to 55-85 ℃, installing a condensing tube in the four-neck flask, and keeping refluxing for 10-30 minutes;
(2) adding polyhydric alcohol into the solution obtained in the step (1) according to the proportion, and mixing and stirring for 30-60 minutes;
(3) adding a hydrolysis reaction catalyst into the solution obtained in the step (2) in proportion, and uniformly stirring;
(4) adding organic acid into the solution obtained in the step (3) according to a certain proportion, and condensing and refluxing for 30-300 minutes at the temperature of 55-85 ℃;
(5) and (4) adding a delay regulator and a dispersion stabilizer into the solution obtained in the step (4) according to the proportion, and continuously carrying out condensation reflux for 30-60 minutes at the temperature of 55-85 ℃ to obtain a product.
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| CN114292636A (en) * | 2021-12-31 | 2022-04-08 | 昆山京昆油田化学科技有限公司 | Titanium-zirconium cross-linking agent and preparation method thereof |
| CN116726788A (en) * | 2023-08-10 | 2023-09-12 | 克拉玛依市紫光技术有限公司 | Preparation method of cross-linking agent for fracturing |
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Application publication date: 20201225 |