CN110713824B - Anti-adsorption composite oil displacement system and preparation method thereof - Google Patents
Anti-adsorption composite oil displacement system and preparation method thereof Download PDFInfo
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- C09K8/584—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
Abstract
The invention belongs to the field of oil extraction and displacement agents, and particularly relates to an anti-adsorption compound oil displacement system and a preparation method thereof; the anti-adsorption composite oil displacement system comprises 4-5 parts of cationic humic acid, 4-5 parts of a main agent and 10 parts of water. The cationized humic acid not only can be used as a sacrificial agent, but also can be used as a surfactant for reducing the oil-water interfacial tension. The aqueous solution of the compound also shows better oil-water interfacial activity. The oil-water interfacial tension of 0.3 percent cationic humic acid aqueous solution can reach 10‑1mN/m。
Description
Technical Field
The invention belongs to the field of oil extraction and displacement agents, and particularly relates to an anti-adsorption compound oil displacement system and a preparation method thereof.
Background
At present, the water content of most of oil well produced liquid in China is up to 90%, and the difficulty in improving the crude oil production degree is increased. The surfactant has excellent oil washing efficiency, emulsifying property, capability of reducing oil-water interfacial tension and the like, and is widely applied to the technology of improving the recovery ratio in tertiary oil recovery.
The surfactant applied to the field is a compound mixture of a plurality of components. The surfactant is mixed with crude oil in the oil displacement process and is also in contact with and adsorbed by reservoir rock minerals. One of the major factors affecting surfactant flooding economics is surfactant adsorption onto reservoir rock. The adsorption causes the loss of the surfactant in the surfactant slug, on one hand, the effective concentration of the surfactant is reduced, and the reduction of the oil displacement efficiency is caused; on the other hand, each component in the surfactant is selectively adsorbed, so that the chromatographic separation of the surfactant is caused, and the stability of the system formula is reduced.
The effects of temperature, salt, alkali, alcohol and the like on the adsorption performance of the compound alkylbenzene sulfonate system on the surface of the oil sand are studied by Buwei and the like. And S.A.hong et al summarize the feasibility of sodium lignosulfonate as an adsorption sacrificial agent through experimental results. CN101219355 points out that humic acid surfactants can improve the wettability and permeability of organic pesticides on the surfaces of plants and pests. CN101913945A points out that the humic acid-containing surfactant obtained by uniformly mixing 40-60 wt% of polyether-modified trisiloxane and 40-60 wt% of humic acid-containing compound can make up the defect of low surface activity of fulvic acid.
Disclosure of Invention
The invention aims to provide an anti-adsorption compound oil displacement system and a preparation method thereof in order to improve the surface activity of humic acid and develop the system economically.
In order to achieve the purpose, the invention adopts the following technical scheme:
an anti-adsorption composite oil displacement system comprises the following components in parts by mass: 4-5 parts of cationic humic acid and 4-5 parts of main agent, and when in use, 10 parts of water is added for mixing and storing.
The preparation method of the cationic humic acid comprises the following steps: adding a cationic etherifying agent 3-chloro-2-hydroxypropyl trimethyl ammonium chloride into the mixed solution of the purified humic acid, hexadecyl trimethyl ammonium chloride and NaOH solution, and stirring for reaction to obtain a black thick liquid crude product; and (3) adjusting the pH value of the system to 7-8 by using dilute hydrochloric acid, standing, performing centrifugal separation, drying, and sealing for storage for later use.
The mass ratio of the humic acid to the hexadecyl trimethyl ammonium chloride to the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride is as follows: 1: 0.1-0.2: 0.1-0.4.
The preparation method of the purified humic acid comprises the following steps: preparing humic acid into a 20% solution, adjusting the pH value to 12-13 with a NaOH solution, stirring for 1h, and standing for 1 h; centrifuging to remove insoluble impurities, adjusting pH to 4 with dilute hydrochloric acid, stirring for 1h, standing for 1h, centrifuging at 3000r/min to remove insoluble impurities and precipitate, evaporating to dry to obtain purified humic acid, and sealing for storage.
The humic acid is fulvic acid and potassium and sodium salts thereof, and the fulvic acid and potassium and sodium salts thereof.
The cationic humic acid serving as an adsorption sacrificial agent of the surfactant flooding has the oil washing effect of peeling crude oil on the surface of the rock.
The main agent comprises the following components in parts by mass: 2-3 parts of betaine surfactant, 6-7 parts of alkylbenzene sulfonate and 1-2 parts of nonylphenol polyoxyethylene ether.
The betaine surfactant is one of erucic acid betaine, lauramidopropyl hydroxysulfobetaine and cocamidopropyl betaine; the alkylbenzene sulfonate is C12-C16 linear alkylbenzene sulfonate; in the nonylphenol polyoxyethylene ether, the polymerization degree of an oxyethylene unit is 6-10.
The application also comprises a method for preparing the anti-adsorption composite oil displacement system, which is obtained by uniformly mixing all the components.
Compared with the prior art, the invention has the beneficial effects that:
(1) the cationized humic acid is used as a sacrificial agent and also used as a surfactant for reducing the oil-water interfacial tension. The aqueous solution of the compound also shows better oil-water interfacial activity. The oil-water interfacial tension of 0.3 percent cationic humic acid aqueous solution can reach 10-1mN/m。
(2) The compound oil displacement system has good stratum sand adsorption resistance. Compared with the compound oil displacement system without adding the cationic humic acid, the compound oil displacement system has the advantages that after 0.3 percent of water solution is subjected to six-stage adsorption by formation sand, the capability of reducing the oil-water interface tension is unchanged and can still reach 10-3mN/m ultra low interfacial tension level. After the system without adding the cationization humic acid is subjected to two-to-four-stage adsorption, the interfacial tension can not reach 10-3mN/m。
(3) Humic acid is taken as a degradable high molecular compound, and the introduction of a tertiary oil recovery surfactant for oil displacement has the advantage of environmental protection.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the following preferred embodiments.
The cationic chemical humic acid is used as an adsorption sacrificial agent in an adsorption-resistant composite oil displacement system, and the synthesis process is as follows:
(1) separation and purification of humic acid: humic acid is prepared into 20 percent solution, the pH value is adjusted to be more than 12 by using 40 percent NaOH solution until the humic acid is completely dissolved, and insoluble impurities are removed by centrifugation (3000 r/min). Adjusting pH to 4 with dilute sulfuric acid, standing, centrifuging at 3000r/min, drying, and sealing for storage.
(2) The cationization synthesis process comprises the following steps: 50g of purified humic acid, 5g of hexadecyltrimethylammonium chloride and 100mL of 40% NaOH solution were sequentially added into a 250mL three-necked flask equipped with a stirrer, a condenser and a thermometer. The reaction was stirred at 60 ℃ for 30 min. Slowly adding 30mL of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride aqueous solution with the mass concentration of 50% dropwise, and continuously stirring for reacting for 6 hours. At the end of the reaction, the product was stirred and cooled to room temperature to give a black viscous liquid. And (3) adjusting the pH of the system to 7-8 by using dilute hydrochloric acid, standing, performing centrifugal separation at 3000r/min, drying, and sealing for later use, wherein the mark is XFJ.
(3) Evaluating the interfacial tension of the cationized humic acid aqueous solution: preparing 0.3 percent XFJ solution by using field water, and testing the oil-water interfacial tension value by using a rotating drop method tensiometer. The tested interfacial tension value can reach 10-1mN/m order of magnitude.
And evaluating the adsorption performance of the adsorption-resistant composite oil displacement system.
1. And testing the oil-water interface tension value of the oil displacement system. The interfacial tension test method refers to the surface and interfacial tension determination method, SY/T5370-1999, which is the oil and gas industry standard of the people's republic of China. The method comprises the following specific steps: surfactant solutions with different concentrations are prepared by using reservoir injection water, and interfacial tension values of the surfactant solutions and reservoir crude oil are measured by using a Texas-500TM rotating drop ultra-low interfacial tension instrument (Keno, USA) at reservoir temperature. When the interfacial tension value reaches 10-3The following evaluation was continued for an oil displacing system of the order of mN/m.
2. And evaluating the static adsorption performance of the formation sand. The method comprises the following specific steps: (1) taking the oil displacement system solution with the interfacial tension value meeting the requirement; (2) adding 60-120 mesh stratum sand (oilfield stratum sand in Gangxi province) and the oil displacement system solution into a closed bottle according to the solid-liquid mass ratio of 1:10, shaking uniformly, putting into a thermostat at a set temperature, and oscillating after half an hour to ensure that sand grains are fully contacted with the solution. Standing for 24h at constant temperature; (3) taking out the upper layer solution after 24h, testing the oil-water interfacial tension value, and recording as the interfacial tension value after the first-stage adsorption; and taking the upper layer solution of the mixed sample after the first-stage adsorption, adding the upper layer solution and the formation sand into a closed bottle according to the solid-liquid mass ratio of 1:10, and recording the interface tension value after the two-stage adsorption as the same operation.
Example 1:
raw materials: erucamidopropyl betaine; hexadecyl benzene sulfonate; nonylphenol polyoxyethylene ether (TX-10). The above raw materials are all purchased from the market. The experimental water is: on-site water is taken from a certain block in harbors and west of the great port oil field for reinjection of sewage; the experimental oil was: crude oil obtained after dehydration and degassing treatment of a certain block of oil wells in the harbor and the west of the Hongkong oil field.
First, the performance of a complex flooding system added with cationic humic acid was evaluated.
(1) Preparing the main agent of the surfactant. The experimental steps are as follows: 0.2g of erucic acid betaine, 0.6g of hexadecylbenzene sulfonate and 0.2g of nonylphenol polyoxyethylene ether are respectively weighed and mixed uniformly to obtain the main agent I.
(2) And preparing 0.3 percent of compound oil displacement system solution. Respectively weighing 1.0g of XFJ and 1.0g of main agent I to obtain a composite oil displacement system, and preparing 0.3% solution by adopting field water. The oil-water interfacial tension value of the solution is tested by referring to SY/T5370-1999 industry standard-surface and interfacial tension determination method. The oil-water interfacial tension is 1.2 multiplied by 10 after testing-3mN/m。
(3) And evaluating the oil-water interfacial tension of the compound oil displacement system after two-stage adsorption. According to the operation steps of evaluating the static adsorption performance of the formation sand, the interfacial tension values after the five-level and six-level adsorption are respectively 3.5 multiplied by 10-3、5.1×10-3mN/m。
Comparative example 1: and evaluating the performance of the composite oil displacement system without adding the cationic humic acid.
(1) Preparing the main agent of the surfactant. The experimental procedure is as before.
(2) And preparing 0.3 percent of compound oil displacement system solution. 1.0g of the base agent I was weighed out and a 0.3% solution was prepared with field water. The oil-water interfacial tension value is tested by referring to the SY/T5370-1999 industry standard-surface and interfacial tension determination method. The oil-water interfacial tension is 6.8 multiplied by 10 after testing-3mN/m。
(3) And evaluating the oil-water interfacial tension of the compound oil displacement system after two-stage adsorption. According to the operation steps of evaluating the static adsorption performance of the formation sand, the interfacial tension values after the first-stage adsorption and the second-stage adsorption are respectively 6.2 multiplied by 10-2、4.9×10-1mN/m。
As can be seen from the comparative example 1, the compound oil displacement system added with the cationic humic acid has the capability of resisting the adsorption of the formation sand, and the oil-water interfacial tension can still reach 10 after the two-stage formation sand adsorption-3mN/m order of magnitude. WhileThe oil-water interfacial tension of the compound oil displacement system without adding cationic humic acid is increased after two-stage adsorption, so that the requirements cannot be met.
Example 2:
raw materials: lauramidopropyl hydroxysultaine; dodecyl benzene sulfonate; nonylphenol polyoxyethylene ether (TX-6). The above raw materials are all purchased from the market. The experimental water is: on-site water is taken from a certain block in harbors and west of the great port oil field for reinjection of sewage; the experimental oil was: crude oil obtained after dehydration and degassing treatment of a certain block of oil wells in the harbor and the west of the Hongkong oil field.
(1) Preparing the main agent of the surfactant. The experimental steps are as follows: 0.3g of lauramidopropyl hydroxysulfobetaine, 0.6g of dodecylbenzene sulfonate and 0.1g of TX-6 are respectively weighed and mixed uniformly to obtain a main agent II.
(2) And preparing 0.3 percent of compound oil displacement system solution. Respectively weighing 1.2g of XFJ and 1.0g of a main agent II to obtain a composite oil displacement system, and preparing 0.3 percent solution by adopting field water. The oil-water interfacial tension value of the solution is tested by referring to SY/T5370-1999 industry standard-surface and interfacial tension determination method. The oil-water interfacial tension is 1.0 multiplied by 10 after testing-3mN/m。
(3) And evaluating the oil-water interfacial tension of the compound oil displacement system after two-stage adsorption. According to the operation steps of evaluating the static adsorption performance of the formation sand, the interfacial tension values after the five-level and six-level adsorption are respectively 2.6 multiplied by 10-3、5.5×10-3mN/m。
Comparative example 2: and evaluating the performance of the composite oil displacement system without adding the cationic humic acid.
(1) Preparing a surfactant main agent. The experimental procedure is as before.
(2) And preparing 0.3 percent of compound oil displacement system solution. 1.0g of the base compound II was weighed out and a 0.3% solution was prepared with field water. The oil-water interfacial tension value is tested by referring to the SY/T5370-1999 industry standard-surface and interfacial tension determination method. The oil-water interfacial tension is 5.6 multiplied by 10 after testing-3mN/m。
(3) And evaluating the oil-water interfacial tension of the compound oil displacement system after two-stage adsorption. According to the operation steps of evaluating the static adsorption performance of the formation sand, the interfacial tension values after the first-stage and the second-stage adsorption are respectively8.0×10-2、9.3×10-1mN/m。
As can be seen from the comparative example 2, the compound oil displacement system added with the cationic humic acid has the capability of resisting the adsorption of the formation sand, and the oil-water interfacial tension can still reach 10 after the two-stage formation sand adsorption-3mN/m order of magnitude. And the oil-water interfacial tension is increased after two-stage adsorption of a compound oil displacement system without adding cationic humic acid, so that the requirements cannot be met.
Example 3:
raw materials: cocamidopropyl betaine; hexadecyl benzene sulfonate; nonylphenol polyoxyethylene ether (TX-9). The above raw materials are all purchased from the market. The experimental water is: on-site water is taken from a certain block in harbors and west of the great port oil field for reinjection of sewage; the experimental oil was: crude oil obtained after dehydration and degassing treatment of a certain block of oil wells in the harbor and the west of the Hongkong oil field.
(1) Preparing the main agent of the surfactant. The experimental steps are as follows: 0.2g of cocamidopropyl betaine, 0.7g of hexadecylbenzene sulfonate and 0.1g of TX-9 are respectively weighed and mixed uniformly to obtain a main agent III.
(2) And preparing 0.3 percent of compound oil displacement system solution. Respectively weighing 1.2g of XFJ and 1.0g of a main agent III to obtain a composite oil displacement system, and preparing 0.3% solution by adopting field water. The oil-water interfacial tension value of the solution is tested by referring to SY/T5370-1999 industry standard-surface and interfacial tension determination method. The oil-water interfacial tension is 3.0 multiplied by 10 after testing-3mN/m。
(3) And evaluating the oil-water interfacial tension of the compound oil displacement system after two-stage adsorption. According to the operation steps of evaluating the static adsorption performance of the formation sand, the interfacial tension values after the fifth-level and the sixth-level absorption are respectively 3.2 multiplied by 10-3、4.5×10-3mN/m。
Comparative example 3: and evaluating the performance of the composite oil displacement system without adding the cationic humic acid.
(1) Preparing a surfactant main agent. The experimental procedure is as before.
(2) And preparing 0.3 percent of compound oil displacement system solution. 1.0g of the base compound II was weighed out and a 0.3% solution was prepared with field water. Testing the oil-water interfacial tension value by referring to SY/T5370-1999 industry standard-surface and interfacial tension determination method. The oil-water interfacial tension is 4.6 multiplied by 10 after testing-3mN/m。
(3) And evaluating the oil-water interfacial tension of the compound oil displacement system after two-stage adsorption. According to the operation steps of evaluating the static adsorption performance of the formation sand, the interfacial tension values after the five-level and six-level adsorption are respectively 7.8 multiplied by 10-2、8.9×10-1mN/m。
As can be seen by comparison, the composite oil displacement system added with the cationic humic acid has the capability of resisting the adsorption of formation sand, and the oil-water interfacial tension can still reach 10 after the adsorption of the five-level formation sand-3mN/m order of magnitude. And the oil-water interfacial tension is increased after two-stage adsorption of a compound oil displacement system without adding cationic humic acid, so that the requirements cannot be met.
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
Claims (5)
1. An anti-adsorption composite oil displacement system is characterized by comprising the following components in parts by mass: 4-5 parts of cationic humic acid and 4-5 parts of a main agent;
the main agent comprises the following components in parts by mass: 2-3 parts of betaine surfactant, 6-7 parts of alkylbenzene sulfonate and 1-2 parts of nonylphenol polyoxyethylene ether;
the preparation method of the cationic humic acid comprises the following steps: adding a cationic etherifying agent 3-chloro-2-hydroxypropyl trimethyl ammonium chloride into the mixed solution of the purified humic acid, hexadecyl trimethyl ammonium chloride and NaOH solution, and stirring for reaction to obtain a black thick liquid crude product; adjusting the pH of the system to 7-8 by using dilute hydrochloric acid, standing, performing centrifugal separation, drying, and then sealing and storing for later use; the mass ratio of the humic acid to the hexadecyl trimethyl ammonium chloride to the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride is as follows: 1: 0.1-0.2: 0.1-0.4.
2. The anti-adsorption composite oil displacement system according to claim 1, wherein the preparation method of the purified humic acid comprises the following steps: preparing humic acid into a 20% solution, adjusting the pH value to 12-13 with a NaOH solution, stirring for 1h, and standing for 1 h; centrifuging to remove insoluble impurities, adjusting pH to 4 with dilute hydrochloric acid, stirring for 1h, standing for 1h, centrifuging at 3000r/min to remove insoluble impurities and precipitate, evaporating to dry to obtain purified humic acid, and sealing for storage.
3. The adsorption-resistant composite oil displacement system of claim 2, wherein the humic acid is fulvic acid and potassium and sodium salts thereof, and the fulvic acid and potassium and sodium salts thereof.
4. The anti-adsorption complex oil displacement system of claim 1, wherein the betaine surfactant is one of erucic acid betaine, lauramidopropyl hydroxysultaine and cocamidopropyl betaine; the alkylbenzene sulfonate is C12-C16 linear alkylbenzene sulfonate; in the nonylphenol polyoxyethylene ether, the polymerization degree of an oxyethylene unit is 6-10.
5. A method for preparing the anti-adsorption complex oil displacement system of any one of claims 1 to 4, which is characterized in that the components are uniformly mixed to obtain the anti-adsorption complex oil displacement system.
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