CN114395057A - Polyacrylamide containing chelating sites, chelating type variable-viscosity slickwater and preparation - Google Patents
Polyacrylamide containing chelating sites, chelating type variable-viscosity slickwater and preparation 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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- C09K8/60—Compositions for stimulating production by acting on the underground formation
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Abstract
The invention discloses polyacrylamide containing chelating sites, chelating type variable-viscosity slickwater and a preparation method thereof. The invention synthesizes a thickening slickwater system with reversible chelating crosslinking and chelating sites connected with the main chain, polyacrylic acid and amino acid are amidated under the catalysis of boric acid to synthesize polyacrylamide with carboxyl, and then organic amine containing chelating groups is added into the reaction system to carry out amination reaction, so as to obtain the polyacrylamide containing the chelating sites. The 0.05-2% aqueous solution of the polyacrylamide is added with high-valence metal soluble salt to generate reversible crosslinking, so that the thickening slickwater with the viscosity of 1-1000 mPas is formed, and the EDTA can break the gel to be below 5 mPas. The technology effectively overcomes the defects of low viscosity and weak sand carrying capacity of the conventional slickwater, and can realize continuous online mixing and high-proportion sand adding fracturing operation of the slickwater.
Description
Technical Field
The invention relates to the technical field of oil and gas field development, in particular to polyacrylamide containing chelating sites, chelating type variable-viscosity slickwater and preparation.
Background
The main functions of the fracturing fluid are to fracture the rock stratum to form fractures and carry a propping agent to complete sand laying, and the traditional fracturing fluid mainly takes cross-linked guar gum as a main component. Slickwater fracturing fluid is a high-drag-reduction and low-viscosity fracturing fluid system developed in recent years aiming at tight reservoir transformation, and the main components of the system are water, a small amount of drag reducer, clay stabilizer and surfactant. Compared with the conventional gel fracturing, the gel fracturing has the main advantages of low friction resistance, easy generation of complex fracture pores, realization of larger fracturing yield increase transformation and good economic benefit. But the viscosity of the slickwater fracturing fluid is low, usually only 1-2 mPa & s, and the slickwater fracturing fluid basically has no sand carrying capacity. Thus, tight reservoir fracturing operations often employ a hybrid process: on-line mixing of slick water with a small amount of fine sand as a front section and pre-hydration canning of linear gum or cross-linked guar gum with coarse sand as a rear section results in complex process equipment and obviously increased construction cost. In order to further reduce cost and improve efficiency, a slickwater system with variable viscosity and high sand carrying capacity needs to be developed so as to realize continuous online mixing of the fracturing fluid.
The slickwater fracturing fluid usually adopts polyacrylamide as a main agent of the fracturing fluid, and in order to realize the tackifying function of the slickwater fracturing fluid, methods such as hydrophobic association, ultrahigh molecular weight, anion-cation copolymerization, high-concentration polyacrylamide and the like can be adopted. For example, patent application CN201510890193.7 proposes a method for improving the solubility of hydrophobic monomers in water by the action of cyclodextrin host-guest, and copolymerizing the hydrophobic monomers and water-soluble monomers such as acrylamide, sodium acrylate, and sodium 2-acrylamido-2-methylpropanesulfonate in an inverse emulsion to obtain a high-viscosity polyacrylamide product. Patent application US7205262B2 proposes a method of achieving polyacrylamide high viscosity using a combination of cationic polymer and anionic surfactant. The American Petroleum institute paper SPE-199330-MS prefers anionic, medium hydrolysis, ultra high molecular weight polyacrylamide, and the system can keep 100 mesh quartz from settling in 39 min. However, the method of increasing viscosity using high concentration polyacrylamide leads to a substantial increase in the cost of the fracturing fluid; the solubility of the hydrophobically associating polyacrylamide is poor, the liquid preparation is difficult, and the cost of the hydrophobic monomer is high; the ultrahigh molecular weight polyacrylamide is very easy to be damaged by shearing, and the shearing viscosity is obviously reduced along with the time; in the anion and cation assembly method, the surfactant and the polymer have high cost, the stratum adsorption is serious, and the economy is poor; and the existing variable-viscosity technology cannot resist high temperature.
Therefore, there is a need to develop cost-effective, reversible physical or chemical crosslinking, temperature-, salt-, and shear-resistant slimy slickwater systems.
Disclosure of Invention
The invention aims to provide polyacrylamide containing chelating sites, chelating type variable-viscosity slickwater and preparation.
The chelating type variable-viscosity slickwater is characterized in that polyacrylamide containing chelating sites is connected to a main chain, and the polymer can perform reversible chelating crosslinking on polyacrylamide with different chain segments through metal ions, so that the aim of thickening the slickwater is fulfilled.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of polyacrylamide containing chelating sites, which comprises the following steps:
carrying out amidation reaction on polyacrylic acid and amino acid aqueous solution under the catalysis of boric acid to obtain polyacrylamide with carboxyl;
and then adding organic amine containing a chelating group into the reaction system to carry out amination reaction to obtain the polyacrylamide containing the chelating site.
The main chain of the polyacrylamide obtained by the preparation method is connected with chelated metal sites, and the chelated metal sites can chelate metal ions, so that reversible crosslinking of polyacrylamide with different chain segments is realized. The slippery water prepared from polyacrylamide containing chelating sites has higher viscosity after chelating metal ions, and can break gel and reduce the viscosity after EDTA is added.
In addition, the preparation method is carried out in one step of two-step reaction, the intermediate product can be fed for the second-step reaction without being treated, and the preparation method is simple and easy to operate.
According to the preparation method of the invention, preferably, the polyacrylamide containing chelating sites contains 0.1-1.5% of chelating metal sites.
According to the production method of the present invention, preferably, the amino acid is in excess relative to polyacrylic acid; more preferably, the molar ratio of the amino acid to polyacrylic acid is 200: 1-1000: 1.
according to the production method of the present invention, preferably, the polyacrylic acid has a molecular weight of 300 ten thousand.
According to the preparation method of the invention, the mass fraction of the amino acid aqueous solution is preferably 1-37%.
According to the production method of the present invention, preferably, the amino acid in the amino acid solution is selected from one or a combination of two or more of glutamic acid, glycine and alanine.
According to the preparation method of the present invention, preferably, the organic amine containing a chelating group is a secondary amine or a primary amine of a bidentate or tridentate ligand having nitrogen, oxygen, or sulfur as a chelating site.
According to the production method of the present invention, preferably, the secondary amine is selected from iminodiacetic acid, 2' -hydrazonodiacetic acid, and diethanolamine; the primary amine is thiourea.
The organic amine comprising a chelating group is preferably iminodiacetic acid.
According to the preparation method of the present invention, preferably, the boric acid is an organoboron catalyst such as 5-methoxy-2-iodophenylboronic acid.
According to the production method of the present invention, preferably, the boric acid is used in an amount of 1% of the total molar amount of the polyacrylic acid, the amino acid, and the organic amine containing a chelating group.
According to the preparation method of the invention, the molar ratio of the polyacrylamide with carboxyl and the organic amine containing the chelating group is preferably 100 (0.1-1.5).
According to the preparation method of the present invention, preferably, the temperature of the amidation reaction is 60 ℃ and the time is 12 hours.
According to the preparation method of the invention, preferably, the temperature of the amination reaction is 60 ℃ and the time is 4-12 h.
In another aspect, the present invention provides a polyacrylamide containing a chelating site, which is obtained by the above preparation method.
In a further aspect of the invention, a chelating type slimy slickwater is provided comprising the above polyacrylamide with chelating sites.
According to the chelated varied-viscosity slickwater of the invention, preferably, the chelated varied-viscosity slickwater is obtained by diluting the polyacrylamide containing the chelating sites to the concentration of 0.05% -2% by using water or saline water, and then adding high-valence metal salt water solution; after the high-valence metal salt aqueous solution is added, the concentration of the high-valence metal salt in the system is 2mg/L-500 mg/L.
According to the chelated slimy slickwater of the present invention, preferably, the high-valence metal salt is selected from FeCl3、AlCl3、FeCl2、Fe2(SO4)3、Al2(SO4)3、CoSO4And CoCl2One or a combination of two or more of them.
According to the chelated slimy slickwater of the invention, preferably, the saline water is selected from potassium chloride, sodium chloride, ammonium chloride or a mixture thereof with the mass fraction of 0.1% -10%.
According to the chelating type variable-viscosity slickwater, the chelating type variable-viscosity slickwater is preferably used at the shearing frequency of 170s-1And a shear viscosity of 1 to 1000 mPas at a temperature of 0 to 150 ℃.
According to the chelate type viscidity smooth water, EDTA with the mass of 0.01-0.1% of the system is preferably added into the chelate type viscidity smooth water, so that gel breaking is realized, and the viscosity is reduced to be less than 5 mPas.
The beneficial effects of the invention include:
1) the oxygen of the carboxylic acid introduced into the amino acid has lone pair electrons, so that crosslinking can be more easily carried out, and the tackifying efficiency is higher;
2) the preparation is better controlled, and the preparation requirement can be met only by changing the concentration of the amino acid and the secondary amine or the primary amine;
3) the preparation of the polyacrylamide containing the chelating sites is simpler, the two reactions are carboxylic acid amidation, the catalysts are the same, and the next reaction can be immediately carried out after the first reaction;
4) the polyacrylamide containing the chelating sites has good solubility, and can be mixed with slick water on line; the modified group is a water-soluble group, the proportion of the modified group is only 0.1-1.5%, and the quick water solubility of polyacrylamide is not influenced;
5) the chelating type variable-viscosity slippery water has good temperature resistance, salt resistance and shearing resistance; the chelating sites are bidentate or tridentate ligands, have strong action with common metal ions and are reversible chelating action, so that the stability of crosslinking (high viscosity, high temperature resistance and salt resistance) can be ensured, and the shearing damage can be prevented.
Drawings
FIG. 1 is a schematic diagram of the preparation and operation of the chelating type viscoski water system of example 3.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
All numerical designations of the invention (e.g., temperature, time, concentration, weight, and the like, including ranges for each) may generally be approximations that vary (+) or (-) in increments of 0.1 or 1.0 as appropriate. All numerical designations should be understood as preceded by the term "about".
Example 1
This example prepares a solution of polyacrylamide with carboxyl groups H1
Adding a polyacrylic acid copolymer aqueous solution (Komaishi oil and gas field technology Co., Ltd.) with the molecular weight of 300 ten thousand into 250mL of four ports, installing a mechanical stirring pipe, a reflux condenser pipe, a thermometer and a constant pressure dropping funnel, adding a glycine aqueous solution with the excessive concentration of 10% (the molar ratio of polyacrylic acid to amino acid is 1:500), stirring and mixing uniformly, adding 5-methoxy-2-iodophenylboronic acid with the molar weight of 1% of the total molar weight of the monomers, adjusting the temperature to 60 ℃, and continuously stirring for 8 hours to obtain a polyacrylamide solution H1 with carboxyl, wherein the polyacrylamide solution H1 is directly used for the next reaction without further purification and with the reaction container unchanged.
Example 2
This example prepares a polyacrylamide CPMA1 containing 0.5% chelating sites
Iminodiacetic acid is slowly added into the reaction system in the embodiment 1, the molar ratio of the polyacrylamide with carboxyl and the iminodiacetic acid is 1:0.006, the effective content of the polymer is 34 percent, the temperature is kept at 60 ℃ and is kept unchanged, the temperature is kept constant, the mixture is uniformly stirred until the mixture reacts for 8 hours, and the polyacrylamide CPMA1 containing 0.5 percent of chelating sites is obtained.
The reaction process is as follows:
example 3
This example prepares a chelate type variable viscosity slickwater system CHVSW1
The sample obtained in example 2 was dissolved in 2% ammonium chloride salt water by mass under stirring, the concentration of polymer CPMA1 by mass was 0.5%, the stirring time was 2 hours, and the stirring speed was 600 rpm/min. After aging for 2 hours, the mixture was diluted to a polymer concentration of 0.1% by mass and the initial viscosity was 2.4 mPas. Adding FeCl3The concentration of the aqueous solution was adjusted to 12mg/L, and the system rapidly became viscous, to obtain chelate-type variable viscosity slickwater system CHVSW 1. Measured by a Haake rheometer at 85 deg.C and 170S-1The viscosity at shear frequency was 31.2 mPas, the test data are shown in # 2 in Table 1, which demonstrates that it can be used as an excellent slimy slick.
Table 1: viscosity test data
| Serial number | Temperature of | Shear frequency | Viscosity of the oil |
| 2# | 85℃ | 170S-1 | 31.2mPa·s |
In the same way, AlCl was tested3FeCl in an aqueous solution to a concentration of 10mg/L3Making the concentration of the water solution to be 30mg/L to obtain a viscous slickwater systemThe viscosity was 23.4 mPas and 18.6 mPas, respectively, indicating that the high-valent metal ion-reversible crosslinking agent had the optimum crosslinking concentration.
The preparation and action principle diagram of the whole chelate type variable-viscosity slippery water system is shown in figure 1, the reaction principle is that polyacrylic acid is utilized for amidation to obtain polyacrylamide polymer grafted with carboxyl, then the polymer with carboxyl and secondary amine are utilized for dehydration to obtain the polymer with chelating sites, L1, L2 and L3 represent different chelating sites, wherein the grafted chelating sites are respectively provided with one L2 by N in the secondary amine, and the two chelating sites are provided by oxygen of two carboxyl groups in the secondary amine, namely L1 and L3. The obtained polymer with chelating sites has metal ions such as Fe in the water meeting the formation3+The metal ions have chelation, which is equivalent to increasing the chain length of two polymers so as to achieve the aim of tackifying.
Example 4
This example prepares a chelate type variable viscosity slickwater system CHVSW2
The molar ratio of the reaction in example 2 to acrylamide: secondary amine (iminodiacetic acid) was changed to 1: 0.012, and the rest conditions were not changed, to obtain polyacrylamide CPMA2 containing 1% chelating sites.
A0.3% aqueous slippery solution of polyacrylamide CPMA2 having a viscosity of 3.9 mPas was obtained according to the solution preparation method in example 3. According to a loop friction resistance tester, testing the resistance reduction rate of the pipe column, wherein the flow rate is greater than 6.91m/s, and the lease reduction rate is greater than 50%. FeCl was added to a 0.3% aqueous slip of polyacrylamide CPMA23The concentration of the aqueous solution is 15mg/L, a chelate variable-viscosity slickwater system CHVSW2 is obtained, and the viscosity of the preparation system is remarkably thickened; 85 ℃ and 170S-1The shear frequency reached 203 mPas. When EDTA was further added to the system (to a mass concentration of 0.1%), the system broke and the viscosity decreased to 4.0 mPas.
In summary, it can be seen that reversible crosslinking viscosity-changing slickwater with good water solubility can be obtained by amidating polyacrylic acid, grafting secondary amine with chelating sites, and adding 0.1-1.5% of chelating sites on the main chain. The reversible coordination crosslinking agent may be a high valent metal ion with a large chelation constant. The system has low cost, temperature resistance, shear resistance and good solubility, and the concentration of the used cross-linking agent is extremely low, so the system is a better viscosity-changing slickwater system.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (10)
1. A preparation method of polyacrylamide containing chelating sites is characterized by comprising the following steps:
carrying out amidation reaction on polyacrylic acid and amino acid aqueous solution under the catalysis of boric acid to obtain polyacrylamide with carboxyl;
and then adding organic amine containing a chelating group into the reaction system to carry out amination reaction to obtain the polyacrylamide containing the chelating site.
2. The method according to claim 1, wherein the polyacrylamide having chelating sites contains 0.1% to 1.5% of chelating metal sites.
3. The method according to claim 1, wherein the molar ratio of the amino acid to the polyacrylic acid is 200: 1-1000: 1;
preferably, the polyacrylic acid has a molecular weight of 300 ten thousand.
4. The preparation method according to claim 1, wherein the mass fraction of the amino acid aqueous solution is 1% -37%;
preferably, the amino acid in the aqueous amino acid solution is selected from one or a combination of two or more of glutamic acid, glycine and alanine.
5. The method according to claim 1, wherein the organic amine containing a chelating group is a secondary amine or a primary amine of a bidentate or tridentate ligand having nitrogen, oxygen, or sulfur as a chelating site.
6. The process of claim 5, wherein the secondary amine is selected from iminodiacetic acid, 2' -hydrazonodiacetic acid, and diethanolamine; the primary amine is thiourea;
preferably, the organic amine comprising a chelating group is iminodiacetic acid.
7. The method according to claim 1, wherein the boric acid is 5-methoxy-2-iodophenylboronic acid.
8. The method according to claim 1, wherein the amount of the boric acid is 1% of the total molar amount of the polyacrylic acid, the amino acid and the organic amine containing a chelating group;
preferably, the molar ratio of the polyacrylamide with carboxyl and the organic amine containing the chelating group is 100 (0.1-1.5);
preferably, the temperature of the amidation reaction is 60 ℃ and the time is 12 h;
preferably, the amination reaction is carried out at a temperature of 60 ℃ for a time of 4h to 12 h.
9. A polyacrylamide having a chelating site, which is obtained by the production method according to any one of claims 1 to 8.
10. A chelating type slimy slickwater comprising the polyacrylamide containing chelating sites of claim 9;
preferably, the chelating type slimy slickwater is obtained by diluting the polyacrylamide containing the chelating site according to claim 9 to a concentration of 0.05% to 2% using water or saline, and then adding a high-valence metal salt aqueous solution; after a high-valence metal salt aqueous solution is added, the concentration of the high-valence metal salt in the system is 2mg/L-500 mg/L;
preferably, the high-valence metal salt is selected from FeCl3、AlCl3、FeCl2、Fe2(SO4)3、Al2(SO4)3、CoSO4And CoCl2One or a combination of two or more of them;
preferably, the brine is selected from potassium chloride, sodium chloride, ammonium chloride or a mixed solution thereof with the mass fraction of 0.1-10%;
preferably, the chelating type variable viscosity slick water has a shear frequency of 170s-1Under the condition of 0-150 ℃, the shear viscosity is 1-1000 mPa & s;
preferably, when 0.01-0.1% by mass of EDTA is added to the chelate type viscid and slick water, the viscosity is reduced to less than 5 mPas by gel breaking.
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| CN117659985A (en) * | 2024-02-01 | 2024-03-08 | 大庆恒辉石油钻采技术有限公司 | Suspension type slick water drag reduction fracturing fluid and preparation method thereof |
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| CN114395057B (en) | 2022-12-23 |
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