CN110591677B - Cross-linking agent of polyacrylamide water shutoff agent, preparation method and application thereof - Google Patents
Cross-linking agent of polyacrylamide water shutoff agent, preparation method and application thereof Download PDFInfo
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- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
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Abstract
The invention relates to a cross-linking agent of a polyacrylamide water shutoff agent, a preparation method and application thereof, wherein the cross-linking agent comprises the following components in percentage by mass: 20 to 30 percent of chromium nicotinate complex, 3 to 5 percent of aluminum citrate, 15 to 30 percent of organic acid, 0.03 to 0.06 percent of sodium carboxymethyl cellulose, 15 to 20 percent of acidity regulator and 15 to 47 percent of deionized water. The weak gel formed by using the cross-linking agent is not easy to generate coagulation phenomenon during storage, can effectively delay gelling time, has good viscoelasticity and water retention, and also has good shearing resistance, low fluid loss and good injectability.
Description
Technical Field
The invention belongs to the field of chemical additives, and particularly relates to a cross-linking agent of a polyacrylamide water shutoff agent, and a preparation method and application thereof.
Background
The most important energy in China is petroleum, and in recent years, the petroleum not only occupies the first energy consumption of China, but also has ever-increasing proportion. At the present stage, almost all oil fields in China enter a tertiary oil recovery stage, the injection profile of the oil well is extremely uneven when oil recovery enters the middle and later stages, and injected water in some blocks quickly breaks through along a high permeable layer, so that the heterogeneity of the stratum is further expanded, a large amount of water is discharged from the oil well, and the water content is greatly increased. The water produced by the oil well brings a plurality of serious problems to the development of the oil field, even the oil field can not be continuously exploited finally, and the development benefit is seriously influenced. Therefore, the development of oil well water plugging technology is particularly important.
The chemical water shutoff agent is an important means for effectively preventing water from flowing out of an oil well, and is widely applied in the world and the domestic. At the present stage, the application of chemical water shutoff agent in petroleum production in China mainly adopts a polymer flooding composite ion depth profile control technology, wherein the polymer mainly adopts polyacrylamide, but the effect of singly using polyacrylamide is not good, and the performance is generally improved by adding a cross-linking agent containing metal ions. The water shutoff agent system can limit water output after being injected into stratum without influencing oil gas yield, is dissolved in water on the ground and injected into the well during construction, is safe and effective in production, and is a quite cheap treatment method.
However, at present, the gel formed by the cross-linking agent product is poor in strength and viscoelasticity, and a large amount of precipitates gradually appear at the bottom after the gel is placed, so that the storage of the gel is influenced.
Disclosure of Invention
The invention aims to provide a cross-linking agent of a polyacrylamide water shutoff agent, which aims to solve the problems of easy precipitation, high gelling speed and poor viscoelasticity of gel formed by using the existing cross-linking agent during storage.
The invention also aims to provide a preparation method and application of the cross-linking agent of the polyacrylamide water shutoff agent.
In order to achieve the purpose, the invention provides a cross-linking agent of a polyacrylamide water shutoff agent, which comprises the following components in percentage by mass: 20 to 30 percent of chromium nicotinate complex, 3 to 5 percent of aluminum citrate, 15 to 30 percent of organic acid, 0.03 to 0.06 percent of sodium carboxymethyl cellulose, 15 to 20 percent of acidity regulator and 15 to 47 percent of deionized water.
Preferably, the chromium nicotinate complex is Cr2(C6H4NO2)3Cl3。
Preferably, the organic acid is malonic acid.
Preferably, the acidity regulator is one or more of ammonia water, sodium carbonate and sodium bicarbonate.
In order to achieve the above object, the present invention further provides a preparation method of the cross-linking agent for the polyacrylamide water shutoff agent, comprising the following steps:
s1, sequentially adding deionized water, the chromium nicotinate complex, aluminum citrate, sodium carboxymethylcellulose and organic acid into a stirring reactor, and stirring and reacting for 6-9 h at 80-90 ℃; and
and S2, adding an acidity regulator into the mixed solution after the stirring reaction in the S1, and regulating the mixed solution to be neutral or alkaline to obtain a cross-linking agent product.
Preferably, in S2, the pH of the mixed solution is adjusted to 7-8 by using an acidity regulator.
In order to achieve the purpose, the invention also provides an application of the cross-linking agent in a polyacrylamide water shutoff agent, wherein the mass ratio of the cross-linking agent to the polyacrylamide is 3-6: 7-12
The invention has the beneficial effects that: the weak gel formed by using the cross-linking agent is not easy to generate coagulation phenomenon during storage, can effectively delay gelling time, has good viscoelasticity and water retention, and also has good shearing resistance, low fluid loss and good injectability.
Drawings
FIG. 1 is a graph showing the storage stability of a weak gel prepared in example 1.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A cross-linking agent of a polyacrylamide water shutoff agent comprises the following components in percentage by mass: 20 to 30 percent of chromium nicotinate complex, 3 to 5 percent of aluminum citrate, 15 to 30 percent of organic acid, 0.03 to 0.06 percent of sodium carboxymethyl cellulose, 15 to 20 percent of acidity regulator and 15 to 47 percent of deionized water.
The chromium nicotinate complex used by the cross-linking agent is stable at normal temperature, and the ligand is Cr3+The cross-linking agent is used as a center to form a reticular porous structure, and other substances in the cross-linking agent can be attached to the pore size, so that the coagulation phenomenon can be effectively avoided during storage. Meanwhile, the existence of the ligand enables the release speed of the chromium ions participating in the reaction to be slow, and when the chromium ions are combined with polyacrylamide substances in the using process, the colloid forming speed can be effectively prevented from being too fast. Chromium nicotinate complex dissolved in water to release Cr3+The reaction is a reversible reaction, and excessive chromium nicotinate complex can cause Cr3+The release is too fast, otherwise, the release is too slow, so that the chromium nicotinate complex in the cross-linking agent is controlled to be 20-30 percent, and the reaction with polyacrylamide substances at the later stage can be better adapted. The aluminum citrate ionizes to form citrate in water solution, which can be mixed with Cr3+When combined, a stable chelate is generated, and nonionic and negative charge type chelate is formed, so that the gel system is very stable. The sodium carboxymethylcellulose used can generate a large amount of carboxymethyl after being dissolved in water, the carboxymethyl has one unit of negative charge, free aluminum ions generated by the aluminum citrate has three units of positive charges, each aluminum ion and three carboxyl groups are bonded together by chemical bonds to form a thin net-shaped film, and the cross-linked film can lock water free in the gel, so that the formed gel network has good water retention. In addition, the molecular chain of the sodium carboxymethyl cellulose contains more sodium carboxylate groups, and resin substances can be grafted when the sodium carboxymethyl cellulose is combined with polyacrylamide substances at a later stage, so that a formed gel network has good viscoelasticity.
In an embodiment of the present invention, the chromium nicotinate complex is Cr2(C6H4NO2)3Cl3The preparation method comprises the following steps: 5.0g (4.4X 10) of nicotinic acid is taken-2mol) and a certain amount of sodium hydroxide solution are placed in a three-neck flask, a certain amount of distilled water is added, and simultaneously, the temperature is raised and the mixture is stirred until the mixture is completely dissolved, so that the sodium nicotinate solution is obtained. Then, 6.0g of CrCl was taken3·6H2O(2.2×10-2mol) is added with ethanol water solution for dissolution. Slowly dripping chromium trichloride solution into sodium nicotinate solution under rapid stirring, adjusting pH value to neutral, cooling to room temperature, filtering, washing, and drying to obtain gray chromium nicotinate complex Cr2(C6H4NO2)3Cl3。
The organic acid is malonic acid.
The acidity regulator is one or more of ammonia water, sodium carbonate and sodium bicarbonate.
A preparation method of a cross-linking agent of a polyacrylamide water shutoff agent comprises the following steps:
s1, sequentially adding deionized water, the chromium nicotinate complex, aluminum citrate, sodium carboxymethylcellulose and organic acid into a stirring reactor, and stirring and reacting for 6-9 h at 80-90 ℃; and
and S2, adding an acidity regulator into the mixed solution after the stirring reaction in the S1, and regulating the mixed solution to be alkaline to obtain a cross-linking agent product.
And in S2, the pH value of the mixed solution is adjusted to 7-8 by using an acidity regulator.
The application of the cross-linking agent in the polyacrylamide water shutoff agent is characterized in that the mass ratio of the cross-linking agent to the polyacrylamide is 3-6: 7-12.
Example 1
Selecting raw materials according to weight percentage
The preparation method comprises the following specific steps:
(1) deionized water and Cr are mixed according to the mass ratio2(C6H4NO2)3Cl3Adding the aluminum citrate, the sodium carboxymethylcellulose and the malonic acid into a stirring reactor in sequence, and stirring and reacting for 6 hours at the temperature of 80 ℃.
(2) And (2) adding ammonia water into the mixed solution after the stirring reaction in the step (1) is finished, and adjusting the mixed solution to 7 to obtain a cross-linking agent product.
Preparing a water plugging agent: polyacrylamide (industrial grade, Sanyo chemical Co., Japan) with a molecular weight of 1400 ten thousand is selected, 4.5g of the polyacrylamide is added into 1000mL of water, stirred and dissolved, and then 1.6g of cross-linking agent is added and stirred sufficiently to prepare weak gel.
The viscosity retention and gelling time of the weak gels are shown in tables 1 and 2. The storage stability of the weak gel is shown in FIG. 1. As can be seen from FIG. 1, the weak gel was stable for more than one year at 70 ℃ and 80 ℃ for a long period of time without dehydration. The strength of the formed gel reaches the maximum value within 1 month, and then is slightly reduced, but the annual loss rate is always kept within 5 percent, and the gel has good water retention and stability.
Example 2
Selecting raw materials according to weight percentage
The preparation method comprises the following specific steps:
(1) deionized water and Cr are mixed according to the mass ratio2(C6H4NO2)3Cl3Adding the aluminum citrate, the sodium carboxymethylcellulose and the malonic acid into a stirring reactor in sequence, and stirring and reacting for 9 hours at 90 ℃.
(2) And (2) adding a sodium carbonate aqueous solution into the mixed solution after the stirring reaction in the step (1), and adjusting to 8 to obtain a cross-linking agent product.
Preparing a water plugging agent: the same as in example 1.
The viscosity retention and gelling time of the weak gels are shown in tables 1 and 2.
Example 3
Selecting raw materials according to weight percentage
The preparation method comprises the following specific steps:
(1) deionized water and Cr are mixed according to the mass ratio2(C6H4NO2)3Cl3Adding the aluminum citrate, the sodium carboxymethylcellulose and the malonic acid into a stirring reactor in sequence, and stirring and reacting for 6 hours at 90 ℃.
(2) And (2) adding a sodium bicarbonate aqueous solution into the mixed solution after the stirring reaction in the step (1), and adjusting to 7.5 to obtain a cross-linking agent product.
Preparing a water plugging agent: the same as in example 1.
The viscosity retention and gelling time of the plugging agent are shown in tables 1 and 2.
TABLE 1
| Viscosity before shearing (mPa. s) | Viscosity after shearing (mPa. s) | Viscosity retention (%) | |
| Example 1 | 3200 | 3070 | 95.9 |
| Example 2 | 3400 | 3280 | 96.5 |
| Examples3 | 3560 | 3420 | 96.0 |
Note: 1. viscosity after shearing was 45 s-1Viscosity values measured after 30 min shearing at shear rate.
2. The ratio of the viscosity after shearing to the viscosity before shearing was the viscosity retention.
As can be seen from Table 1, the shear viscosity retention of the crosslinked gel system is above 95%, indicating that it has excellent shear resistance. Meanwhile, the viscosity of a gel system formed under the action of the cross-linking agent is more than 3000mPa & s and less than 5000mPa & s, the low-strength weak gel has certain fluidity and viscosity, the fluidity enables the low-strength weak gel to have good injection performance, and the viscosity enables the gel system to be obviously reduced in tiny cracks after being injected into a stratum in the later period, so that the gel system can accurately reach a high-permeability area.
TABLE 2
As can be seen from Table 2, the gelling time of the gel system is gradually shortened with the increase of the temperature, but the viscosity of the system is not changed greatly, the gel strength is about 3336 mPa.s, the toughness change is similar to the gel strength change, which shows that the temperature has little influence on the performance of the gel system and the gel has good thermal stability.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. The cross-linking agent of the polyacrylamide water shutoff agent is characterized by comprising the following components in percentage by mass: 20 to 30 percent of chromium nicotinate complex, 3 to 5 percent of aluminum citrate, 15 to 30 percent of organic acid, 0.03 to 0.06 percent of sodium carboxymethyl cellulose, 15 to 20 percent of acidity regulator and 15 to 47 percent of deionized water, wherein the chromium nicotinate complex is Cr2(C6H4NO2)3Cl3(ii) a The organic acid is malonic acid.
2. The crosslinking agent for a polyacrylamide type water shutoff agent according to claim 1, wherein the acidity regulator is one or more selected from the group consisting of aqueous ammonia, sodium carbonate and sodium bicarbonate.
3. The method for preparing the crosslinking agent for the polyacrylamide type water shutoff agent according to any one of claims 1 to 2, which comprises the steps of:
s1, sequentially adding deionized water, the chromium nicotinate complex, aluminum citrate, sodium carboxymethylcellulose and organic acid into a stirring reactor, and stirring and reacting for 6-9 h at 80-90 ℃; and
and S2, adding an acidity regulator into the mixed solution after the stirring reaction in the S1, and regulating the mixed solution to be neutral or alkaline to obtain a cross-linking agent product.
4. The method for producing a crosslinking agent for a polyacrylamide type water shutoff agent according to claim 3, wherein pH of the mixed solution is adjusted to 7 to 8 by using an acidity adjusting agent in S2.
5. The use of the cross-linking agent of any one of claims 1 to 2 in a polyacrylamide water shutoff agent, wherein the mass ratio of the cross-linking agent to the polyacrylamide is 3 to 6:7 to 12.
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| CN109609109A (en) * | 2019-01-17 | 2019-04-12 | 长江大学 | A kind of profile control system and preparation method thereof |
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| US5194615A (en) * | 1983-07-08 | 1993-03-16 | The William Seroy Group | Synthetic GTF chromium nicotinate material and its preparation |
| US20110214860A1 (en) * | 2010-03-05 | 2011-09-08 | Narongsak Tonmukayakul | Clean Viscosified Treatment Fluids and Associated Methods |
| US20110214868A1 (en) * | 2010-03-05 | 2011-09-08 | Funkhouser Gary P | Clean Viscosified Treatment Fluids and Associated Methods |
| US8960290B2 (en) * | 2011-12-19 | 2015-02-24 | Halliburton Energy Services, Inc. | Method for delayedly crosslinking environmentally friendly fluids |
| US10421894B2 (en) * | 2016-06-27 | 2019-09-24 | Research Triangle Institute | Methods and materials for controlled release of materials in a subterranean reservoir |
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| CN1197101A (en) * | 1997-04-22 | 1998-10-28 | 高英敏 | Application of cross-linking agent in polymer displacement of reservoir oil tech. |
| CN101649194A (en) * | 2009-09-15 | 2010-02-17 | 克拉玛依市正诚有限公司 | Compound multivalent metallic ion crosslinking agent and production method and use method thereof |
| CN104403648A (en) * | 2014-10-24 | 2015-03-11 | 西安石油大学 | Oily sludge profile control agent and preparation method thereof |
| CN105041261A (en) * | 2015-05-30 | 2015-11-11 | 西南石油大学 | Well-killing workover method used with water plugging |
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Inventor after: Zhai Pengda Inventor after: Wang Hong Inventor after: Wu Haixia Inventor after: Xing Zhongping Inventor after: Zhang Yu Inventor after: Tian Yumin Inventor after: Wang Kuitao Inventor before: Wang Hong Inventor before: Wu Haixia Inventor before: Zhai Pengda Inventor before: Xing Zhongping Inventor before: Zhang Yu Inventor before: Tian Yumin Inventor before: Wang Kuitao |
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Effective date of registration: 20221020 Address after: 051430 Jing Zhao Line (North of Xigao Village), Luancheng District, Shijiazhuang City, Hebei Province Patentee after: Shijiazhuang Baowei Environmental Protection Technology Co.,Ltd. Address before: 050000 26 Yuxiang Street, Shijiazhuang City, Hebei Province Patentee before: HEBEI University OF SCIENCE AND TECHNOLOGY |