CN107916099B - Alkali-free viscoelastic surfactant composition and preparation method and application thereof - Google Patents
Alkali-free viscoelastic surfactant composition and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a preparation method and application of an alkali-free viscoelastic surfactant, and mainly solves the problem that an existing oil displacement system is poor in oil displacement effect under the condition of a high-temperature low-permeability reservoir. By adopting the surfactant composition comprising betaine surfactant, anionic surfactant and water, the betaine surfactant is shown in the following formula (I); the anionic surfactant is at least one of (II) in the formula; the structure is shown as formula (I), R1Is selected from C8～C29At least one of alkyl and alkenyl of (A), R2And R3Are all independently selected from C1～C5At least one of alkylene and hydroxyl substituted alkylene of (a), X in the structural formula (II) is selected from at least one of carboxylate and sulfonate; the molar ratio of the amphoteric surfactant to the anionic surfactant is 1: 0.01-1: the technical scheme of 100 better solves the technical problem and can be applied to tertiary oil recovery in oil fields.
Description
Technical Field
The invention relates to a preparation method and application of an alkali-free viscoelastic surfactant in a low-permeability oil reservoir.
Background
In the newly discovered petroleum geological reserves of the petrifaction in China, the reserve of the low-permeability oil reservoir accounts for 60-70 percent, and the low-permeability oil reservoir is the main resource basis for increasing the storage and the production in a relatively long period in the future. In recent years, along with the reduction of the recoverable reserve of medium-high permeability oil reservoirs, the development of low permeability oil reservoirs is more and more emphasized by people. Surfactant flooding proved to be a very promising method for improving the recovery ratio of low-permeability oil fields, and becomes a hot spot of domestic and foreign research. Compared with medium and high permeability reservoirs, residual oil drops in the low permeability reservoir exist in pores with small throat radiuses, and capillary resistance of the residual oil drops is far greater than that of the medium and high permeability reservoirs under the same condition, so that lower oil-water interfacial tension is required for activating the residual oil drops. Secondly, the low-permeability reservoir has large seepage resistance and is only positioned atAt higher displacement pressures, the liquid can flow. In addition, the injection pressure is increased for improving the water injection development effect, but the water injection pressure is high, micro cracks are easy to open, water enters along the cracks suddenly, the oil displacement efficiency is reduced, the swept volume is small, and the casing damage is serious. Research shows that the surfactant solution can reduce the oil-water interfacial tension, reduce the capillary resistance of oleophylic oil layer, increase the capillary number and raise the oil displacing efficiency, so that proper surfactant can solve the said problems well and the main basis for screening oil displacing surfactant is whether it can lower the oil-water interfacial tension to ultra low (10)-3mN/m)。
At present, the most widely used surfactants for oil displacement at home and abroad are anionic surfactants mainly comprising sodium salt, which have the advantages of wide sources, large quantity and low price, and are successfully applied to common oil reservoirs (CN 1458219A). however, anionic surfactants are poor in salt tolerance, non-ionic surfactants are sensitive to temperature and are easy to separate out at high temperature, and are not suitable for large-scale use.
Therefore, the invention provides a chemical structure which is stable under the conditions of an alkali-free high-temperature low-permeability reservoir and can form 10 with crude oil－3～10－4The novel oil displacement system with the mN/m ultralow interfacial tension and the effective improvement of the crude oil recovery rate is an alkali-free viscoelastic surfactant composition comprising a betaine surfactant, an anionic surfactant and water, the bulk phase has high viscosity by controlling the self-assembly of the surfactant, and the surfactant has high interfacial activity, so that the recovery rate of a low-permeability oil reservoir is improved, and the novel oil displacement system is expanded to the application of harsh oil fields such as high-temperature low-permeability oil fields.
Disclosure of Invention
The invention aims to solve the technical problems that when a polymer in the existing chemical flooding is used for oil displacement of a low-permeability reservoir, stratum blockage is easily caused and injection is difficult, and provides a novel viscoelastic surfactant composition.
The second technical problem to be solved by the present invention is to provide a method for preparing a viscoelastic surfactant composition corresponding to the first technical problem.
The invention aims to solve the technical problem and provides a method for using the viscoelastic surfactant composition for oil displacement in a low-permeability reservoir, which corresponds to the technical problem. The composition of the viscoelastic surfactant is suitable for cores with common permeability, and the invention is characterized by being suitable for cores with low permeability in view of the fact that oil displacement of low permeability cores faces more difficulty in the field. For example, the technical scheme is characterized in that the range of the permeability of the rock core is 0.1-500 mD; the core permeability range is 2-40 mD.
In order to solve one of the above technical problems, the technical scheme adopted by the invention is as follows: an alkali-free viscoelastic surfactant composition comprises a betaine surfactant, an anionic surfactant and water, wherein the molar ratio of the betaine surfactant to the anionic surfactant is 1: 0.01-1: 100; the betaine surfactant is selected from at least one of structures shown in a formula (I):
in the formula (I), R1Is selected from C8～C29At least one of alkyl and alkenyl of (A), R2And R3Are all independently selected from C1～C5At least one of alkylene and hydroxy-substituted alkylene of (A), R4And R5Are all independently selected from C1～C4At least one of alkyl and hydroxyl-substituted alkyl; more preferably R4And R5Are all selected from methyl, in which case the betaine surfactant is selected from at least one of the structures shown in formula (I'):
at the moment, the interfacial tension performance of the composition with the organic acid salt is better;
the anionic surfactant is selected from at least one of structures shown as a formula (II):
in the formula (II), X is at least one selected from carboxylate and sulfonate.
In the technical scheme, R is preferably selected1Is C12～C25At least one of alkyl or alkenyl of (a), R2Is C2～C3At least one of alkylene or hydroxy-substituted alkylene of (A), R3Is C1～C3An alkylene group of (a).
From the viewpoint of improving the recovery ratio, the most preferable technical scheme is as follows: r is C16～C22At least one of alkyl or alkenyl of (a), R2Is C3At least one of alkylene or hydroxy-substituted alkylene of (A), R3Is C1～C2An alkylene group of (a); the anionic surfactant is at least one selected from naphthalene sulfonate and alkyl substituted naphthalene carboxylate.
In the above technical scheme, the betaine surfactant is selected from two or more of structures shown in formula (I) or formula (I'), such as R, from the perspective of synergistically reducing interfacial tension and improving recovery efficiency1Two or more betaine surfactants having different carbon atoms, in which case R1Two or more betaine surfactants having different carbon atoms have good synergistic effect with anionic surfactant, preferably R1Is C15～C29Long carbon chain carboxylate betaine surfactant and R1Is C8～C14And a combination of two or more of the short carbon chain carboxylate betaine surfactants of (a).
In the above-mentioned technical means, the molar ratio of the amphoteric surfactant to the organic acid salt is preferably (1:0.1) to (1: 10).
In the technical scheme, the composition of the viscoelastic surfactant for oil displacement also comprises water, and is particularly suitable for water flooding by using the surfactant.
To solve the second technical problem, the invention adopts the following technical scheme: a process for the preparation of a viscoelastic surfactant composition as claimed in one of the above technical problems, comprising the steps of:
a) reacting fatty acid or ester thereof with a required amidation reagent at 100-160 ℃ for 3-20 hours; then adding carboxylation reagent ZR3Continuously reacting COOM at 50-100 ℃ for 2-20 hours to obtain the betaine surfactant shown in the formula (I); wherein, fatty acid methyl ester: amidation reagent: the molar ratio of carboxylation reagent is 1: (1-3): (1-4); z is selected from any one of hydrogen, hydroxyl, halogen and amino, and M is selected from any one of alkali metal, alkaline earth metal and ammonium ion;
b) respectively dissolving an anionic surfactant and the betaine surfactant obtained according to the step a) in water, and then adding a surfactant in a molar ratio of (1:0.1) to (1:10) and uniformly mixing to obtain the surfactant composition.
In the above technical scheme, in the step a), the preferable amidation reagent is NH2-R2-N(CH3)2(ii) a The preferred range of the betaine surfactant to anionic surfactant molar ratio in step b) is (1:0.1) to (1: 10).
The technical scheme adopted by the invention for solving the technical problem is as follows: a method for displacing oil in a low-permeability reservoir comprises the step of injecting the oil displacement composition into the low-permeability reservoir to displace oil.
The core permeability range in any one of the above technical schemes is 0.1-500 mD; the core permeability range is 2-40 mD.
The surfactant prepared by compounding the zwitterion and the anion in the viscoelastic surfactant oil displacement agent has the advantages of high viscosity, increased surface activity, reduced critical micelle concentration, solubilization effect and the like due to the compounding of the anion and the zwitterion surfactant. The hydrophilic group in the anionic surfactant and the positive charge in the zwitterionic surfactant have electrostatic attraction, so that the repulsion between the same charges on the surface of the solution can be reduced, the hydrophobic hydrocarbon chains of the hydrophilic group and the hydrophobic hydrocarbon chains of the anionic surfactant have certain hydrophobic effect, different surfactant molecules are promoted to adopt a tighter arrangement mode, and therefore the anionic surfactant has higher surface activity. Two surfactants in the compound surfactant are both ionic, and the compound agent also shows the characteristics of the ionic surfactant, namely excellent temperature resistance. Therefore, the surfactant has excellent temperature resistance and excellent interface activity, and can solve the problem of surface activityThe dosage can not reach 10-3The problem of ultra-low interfacial tension value of mN/m enables the surfactant to be adopted in the tertiary oil recovery process in the underground migration process, and the surfactant composition has high interfacial activity.
By adopting the technical scheme of the invention, the composite surfactant composition can still form 10 with underground crude oil in the scene water with the mineralization degree of 3 ten thousand mg/L and the calcium and magnesium ion content of 400 mg/L under the condition that the dosage of the composite surfactant composition is 0.01-1 w.t%-3～10- 4An ultra-low interfacial tension of mN/m; the oil washing capacity is strong, and the recovery ratio can be improved to 15.1%; the surfactant composition has the advantages of simple system and the like, and obtains better technical effect.
The invention is further illustrated by the following examples.
Detailed Description
[ example 1 ]
1. Surfactant preparation
(1) Erucamide carboxybetaine surfactant (R)1＝C21，R2＝C3、R3＝C2) Preparation of
a) Adding 0.5 mol of methyl erucate and required amount of amidation reagent N, N-dimethyl propane diamine into a reaction kettle, reacting for 8 hours at 140 ℃, starting a vacuum pump, pumping out methanol and excessive N, N-dimethyl propane diamine generated by the reaction to obtain an erucyl tertiary amine product, adding required amount of sodium chloroacetate, reacting for 9 hours at 75 ℃, recrystallizing and purifying with absolute ethyl alcohol to obtain the long-carbon-chain betaine surfactant; wherein the molar ratio of methyl erucate to N, N-dimethyl propane diamine to sodium chloroacetate is 1:2.5: 1.5.
b) Respectively dissolving naphthalene sulfonate and the erucamide carboxyl betaine surfactant prepared by the invention in water, stirring for 30 minutes to prepare an aqueous solution, and uniformly mixing the surfactants according to the molar ratio of the betaine surfactant to the anionic surfactant of 1:0.7 to obtain the viscoelastic surfactant composition.
2. Evaluation of surfactant Properties
a) Viscosity determination
Adopting a Brookfield DV-III viscometer at 85 deg.C and 7.34S-1Under the conditions, the results of measuring the viscosity of the oil displacement agent with the concentration of 0.3 percent and the field water (shown in table 3) of the Jiangsu shaqi oil field are shown in table 2.
b) Evaluation of interfacial tension
The results of measuring the interfacial tension between the oil-displacing agent of 0.1% concentration and the dehydrated crude oil of the oil field of Jiangsu shaqi at 85 ℃ and 6000 rpm by using a TX-500C rotary drop interfacial tension meter manufactured by Texas university, USA, are shown in Table 2.
c) Evaluation of oil displacement experiment
According to the test of the physical simulated oil displacement effect of the composite oil displacement system in the SY/T6424-2000 composite oil displacement system performance test method, a simulated oil displacement experiment is carried out on a rock core with the length of 30cm, the diameter of 2.5cm and the permeability of 20 millidarcy at 87 ℃. Firstly, water flooding is carried out until the water content is 98%, after the water flooding is finished, 0.3pv (core pore volume) of the oil displacement agent accounting for 0.3% is injected, then the water flooding is carried out until the water content is 100%, and the result of improving the crude oil recovery ratio is shown in a table 2.
[ example 2 ]
1. Surfactant preparation
(1) Triacontanoic acid amide carboxybetaine surfactant (R)1＝C29，R2＝C2、R3＝C2) Preparation of
a) Adding 0.5 mol of long-carbon-chain methyl triacontanoate and required amount of amidation reagent N, N-dimethylethylenediamine into a reaction kettle, reacting for 6 hours at 130 ℃, starting a vacuum pump, pumping out methanol and excessive N, N-dimethylethylenediamine generated by the reaction to obtain a triacontanoic acyl tertiary amine product, adding required amount of sodium chloroacetate, reacting for 15 hours at 85 ℃, and recrystallizing and purifying by absolute ethyl alcohol to obtain the long-carbon-chain betaine surfactant; wherein the molar ratio of the methyl triacontanoate to the N, N-dimethylethylenediamine to the sodium chloroacetate is 1:2: 1.5.
b) Naphthalene sulfonate and the triacontanoic amide carboxyl betaine surfactant prepared by the method are respectively dissolved in water, stirred for 30 minutes to prepare aqueous solution, and then the surfactants are uniformly mixed according to the molar ratio of the betaine surfactant to the anionic surfactant of 1:0.7 to obtain the composition of the viscoelastic surfactant.
2. Evaluation of surfactant Properties
The performance evaluation method was the same as in example 1 except that the oil-displacing agent composition was different. The compositions of the oil-displacing agents are shown in Table 1 for comparison, and the evaluation results are shown in Table 2.
[ example 3 ]
1. Surfactant preparation
(1) Pelargonic acid amide carboxyl betaine surfactant (R)1＝C8，R2＝C3、R3＝C3) Preparation of
a) Adding 0.5 mol of methyl nonanoate and required amount of amidation reagent N, N-dimethylpropylenediamine into a reaction kettle, reacting for 10 hours at 135 ℃, starting a vacuum pump, pumping out methanol and excessive N, N-dimethylpropylenediamine generated by the reaction to obtain a nonanoic acyl tertiary amine product, adding required amount of β -sodium chloropropionate, reacting for 10 hours at 75 ℃, and recrystallizing and purifying by absolute ethyl alcohol to obtain the long-carbon-chain betaine surfactant, wherein the molar ratio of methyl nonanoate to N, N-dimethylpropylenediamine to β -sodium chloropropionate is 1:2: 1.6.
b) Respectively dissolving naphthalene sulfonate and the nonanoic acid amide carboxyl betaine surfactant prepared by the method in water, stirring for 30 minutes to prepare an aqueous solution, and uniformly mixing the surfactants according to the molar ratio of the betaine surfactant to the anionic surfactant of 1:0.7 to obtain the viscoelastic surfactant composition.
2. Evaluation of surfactant Properties
The performance evaluation method was the same as in example 1 except that the oil-displacing agent composition was different. The compositions of the oil-displacing agents are shown in Table 1 for comparison, and the evaluation results are shown in Table 2.
[ example 4 ]
1. Surfactant preparation
(1) Lauric acid amide carboxybetaine surfactant (R)1＝C11，R2＝C3、R3＝C3) Preparation of
a) Adding 0.5 mol of methyl laurate and required amount of amidation reagent N, N-dimethylpropylenediamine into a reaction kettle, reacting for 10 hours at 140 ℃, starting a vacuum pump, pumping out methanol and excessive N, N-dimethylpropylenediamine generated by the reaction to obtain a lauric acyl tertiary amine product, adding required amount of β -sodium chloropropionate, reacting for 10 hours at 75 ℃, recrystallizing and purifying with absolute ethyl alcohol to obtain the long-carbon-chain betaine surfactant, wherein the molar ratio of the methyl laurate to the N, N-dimethylpropylenediamine to the β -sodium chloropropionate is 1:2.5: 1.5.
b) Naphthalene sulfonate and the lauric acid amide carboxyl betaine surfactant prepared by the invention are respectively dissolved in water, stirred for 30 minutes to prepare aqueous solution, and then the surfactants are uniformly mixed according to the molar ratio of the betaine surfactant to the anionic surfactant of 1:0.7 to obtain the composition of the viscoelastic surfactant.
2. Evaluation of surfactant Properties
The performance evaluation method was the same as in example 1 except that the oil-displacing agent composition was different. The compositions of the oil-displacing agents are shown in Table 1 for comparison, and the evaluation results are shown in Table 2.
[ example 5 ]
1. Surfactant preparation
Erucamide carboxybetaine surfactant in example 1, lauric acid amide carboxybetaine surfactant in example 4, and naphthalenesulfonate were dissolved in water, respectively, and stirred for 30 minutes to prepare an aqueous solution, and then the surfactants were uniformly mixed according to the molar ratio of erucamide carboxybetaine amphoteric, pelargonic acid amide carboxybetaine surfactant, and anionic surfactant of 0.5:0.5:0.7 to obtain a viscoelastic surfactant composition.
2. Evaluation of surfactant Properties
The performance evaluation method was the same as in example 1 except that the oil-displacing agent composition was different. The compositions of the oil-displacing agents are shown in Table 1 for comparison, and the evaluation results are shown in Table 2.
[ example 6 ]
1. Surfactant preparation
Erucamide carboxybetaine surfactant in example 1, pelargonic acid amide carboxybetaine surfactant in example 3, and naphthalenesulfonate were dissolved in water, respectively, and stirred for 30 minutes to prepare an aqueous solution, and then the surfactants were uniformly mixed according to the erucamide carboxybetaine amphiphilicity, and the molar ratio of pelargonic acid amide carboxybetaine surfactant to anionic surfactant of 0.5:0.5:0.7, to obtain a viscoelastic surfactant composition.
2. Evaluation of surfactant Properties
The performance evaluation method was the same as in example 1 except that the oil-displacing agent composition was different. The compositions of the oil-displacing agents are shown in Table 1 for comparison, and the evaluation results are shown in Table 2.
[ COMPARATIVE EXAMPLE 1 ]
1. Surfactant preparation
Respectively dissolving naphthalene sulfonate and docosyl carboxyl betaine surfactants in water, stirring for 30 minutes to prepare an aqueous solution, and uniformly mixing the surfactants according to the molar ratio of the betaine surfactants to the anionic surfactants of 1:1 to obtain the viscoelastic surfactant composition.
2. Evaluation of surfactant Properties
The performance evaluation method was the same as in example 1 except that the oil-displacing agent composition was different. The compositions of the oil-displacing agents are shown in Table 1 for comparison, and the evaluation results are shown in Table 2.
[ COMPARATIVE EXAMPLE 2 ]
1. Surfactant preparation
According to the method described in patent CN103242816B, a surfactant of the following structure was synthesized: c11H23CON(CH2CH2OH)2Respectively dissolving naphthalenesulfonate and a synthetic surfactant in water, stirring for 30 minutes to prepare an aqueous solution, and uniformly mixing the surfactants according to the molar ratio of the synthetic surfactant to an anionic surfactant of 1:1 to obtain the viscoelastic surfactant composition.
2. Evaluation of surfactant Properties
The performance evaluation method was the same as in example 1 except that the oil-displacing agent composition was different. The compositions of the oil-displacing agents are shown in Table 1 for comparison, and the evaluation results are shown in Table 2.
[ COMPARATIVE EXAMPLE 3 ]
1. Surfactant preparation
Erucamide carboxybetaine surfactant in example 1 and pelargonic acid amide carboxybetaine surfactant in example 3 were dissolved in water, respectively, and stirred for 30 minutes to prepare aqueous solutions, and then the surfactants were mixed uniformly in a molar ratio of erucamide carboxybetaine amphoteric to pelargonic acid amide carboxybetaine surfactant of 1:1 to obtain a surfactant composition.
2. Evaluation of surfactant Properties
The performance evaluation method was the same as in example 1 except that the oil-displacing agent composition was different. The compositions of the oil-displacing agents are shown in Table 1 for comparison, and the evaluation results are shown in Table 2.
TABLE 1 compositions of surfactant compositions in examples and comparative examples
TABLE 2 evaluation of oil-displacing agent Performance in examples and comparative examples
| Viscosity (mPa.s) | Interfacial tension (mN/m) | Enhanced recovery ratio% | |
| Example 1 | 20.7 | 0.0078 | 14.2 |
| Example 2 | 16.7 | 0.0058 | 13.7 |
| Example 3 | 15.8 | 0.0083 | 12.6 |
| Example 4 | 15.7 | 0.0080 | 12.5 |
| Example 5 | 22.5 | 0.00027 | 15.1 |
| Example 6 | 21.6 | 0.00050 | 14.8 |
| Comparative example 1 | 9.5 | 0.012 | 7.9 |
| Comparative example 2 | 2.6 | 0.015 | 5.1 |
| Comparative example 3 | 6.0 | 0.014 | 8.5 |
TABLE 3 field Water of Jiangsu Odong san Qi
| Unit of | Na++K+ | Mg2+ | Ca2+ | Cl- | SO4 2- | HCO3 - | TDS |
| mg/L | 8730.8 | 154 | 220 | 10224 | 1507.7 | 5152.5 | 25830 |
Claims (6)
1. An alkali-free viscoelastic surfactant composition comprises a betaine surfactant and an anionic surfactant, wherein the molar ratio of the betaine surfactant to the anionic surfactant is 1: 0.1-1: 10; the betaine surfactant is selected from at least one of structures shown in a formula (I):
in the formula (I), R1Is selected from C8～C14At least one of alkyl and alkenyl of (A), R2And R3Are all independently selected from C1～C5At least one of alkylene and hydroxy-substituted alkylene of (A), R4And R5Are all independently selected from C1～C4At least one of alkyl and hydroxyl-substituted alkyl;
the anionic surfactant is selected from at least one of structures shown as a formula (II):
in the formula (II), X is at least one selected from carboxylate and sulfonate.
2. The alkali-free viscoelastic surfactant composition according to claim 1, characterized in that the composition comprises water.
3. The alkali-free viscoelastic surfactant composition as claimed in claim 1, wherein the anionic surfactant is selected from at least one of benzene carboxylates, halogenated benzene sulfonates, hydroxy-substituted benzene sulfonates, naphthalene sulfonates, and hydrocarbyl-substituted naphthalene carboxylates.
4. A process for the preparation of an alkali-free viscoelastic surfactant composition as claimed in any one of claims 1 to 3, comprising the steps of:
a) reacting fatty acid or ester thereof with a required amidation reagent at 100-160 ℃ for 3-20 hours; then adding carboxylation reagent ZR3Continuously reacting COOM at 50-100 ℃ for 2-20 hours to obtain the betaine surfactant shown in the formula (I); wherein, fatty acid methyl ester: amidation reagent: the molar ratio of carboxylation reagent is 1: (1-3): (1-4); z is selected from any one of hydrogen, hydroxyl, halogen and amino, and M is selected from any one of alkali metal, alkaline earth metal and ammonium ion;
b) respectively dissolving an anionic surfactant and the betaine surfactant obtained according to the step a) in water, and then adding a surfactant in a molar ratio of (1:0.1) to (1:10) and uniformly mixing to obtain the surfactant composition.
5. An oil displacement method in a low-permeability reservoir, which comprises the step of injecting the oil displacement composition of any one of claims 1-3 into the low-permeability reservoir to displace oil.
6. The method of displacing oil in a low-permeability reservoir of claim 5, wherein the permeability in the low-permeability reservoir is 1-40 mD.
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| CN1263481A (en) * | 1997-06-10 | 2000-08-16 | 罗狄亚公司 | Fluids containing viscoelastic surfactant and methods for using the same |
| CN101757874A (en) * | 1997-06-10 | 2010-06-30 | 罗狄亚公司 | Viscoelastic surfactant fluids and related methods of use |
| CN101955448A (en) * | 2010-03-19 | 2011-01-26 | 中国石油天然气股份有限公司 | Amide group-containing hydroxysulfobetaine and preparation and application thereof |
| CN102851017A (en) * | 2012-08-16 | 2013-01-02 | 四川西普化工股份有限公司 | Viscous-elastic clean fracturing fluid containing erucic acid betaines |
| CN104109518A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | Oil displacement composition used for low permeability oil reservoirs, and preparation method thereof |
| CN104073235A (en) * | 2014-06-19 | 2014-10-01 | 西安石油大学 | Long-carbon-chain amide glycine betaine clean fracturing fluid and preparation method thereof |
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