CN115368885B - Dual-stimulus response type polymer thickened oil emulsifying viscosity reducer and preparation method thereof - Google Patents
Dual-stimulus response type polymer thickened oil emulsifying viscosity reducer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a dual-stimulus response type polymer thickened oil emulsification viscosity-reducing agent and a preparation method thereof, and relates to the technical field of oil and gas field development. The thickened oil emulsification viscosity reducer comprises the following components in percentage by mass: 0.05-0.3 wt% of functionalized polymer, 0.5-2.0 wt% of in-situ carbon generating agent and the balance of water; the polymer thickener is formed by polymerizing 60-70% of acrylamide, 10-20% of acrylic acid, 5.0-10% of sodium styrenesulfonate and 0.5-10% of responsive functional monomers in percentage by weight; the dual-stimulus response polymer thickened oil emulsification viscosity-reducing agent disclosed by the invention has the advantages of thickened oil viscosity-reducing rate up to 99.5%, simple preparation process, high yield, simple post-treatment, stable performance, low cost and wide market prospect.
Description
Technical Field
The invention relates to a dual-stimulus response type polymer thickened oil emulsification viscosity-reducing agent and a preparation method thereof, and relates to the technical field of oil and gas field development.
Background
With the continuous exploitation of conventional oil reservoirs, heavy oil reservoirs are used as main unconventional oil reservoirs, and gradually become the main direction and trend of future oil exploitation. The high content of colloid and asphaltene in the thick oil leads to high viscosity and poor fluidity, which clearly greatly increases the cost of thick oil exploitation and transportation. Therefore, the key in the process of thick oil exploitation is to reduce viscosity of the thick oil so as to improve the fluidity problem of the thick oil.
At present, the most commonly used viscous oil viscosity-reducing technology mainly comprises thermal viscosity-reducing, modifying viscosity-reducing, physical viscosity-reducing, microbial viscosity-reducing, emulsifying viscosity-reducing technology and the like. Emulsion viscosity reduction is considered as the most promising viscosity reduction method at present due to the characteristics of good viscosity reduction effect, simple process, low economic cost and the like. However, as the conditions of the exploited stratum and the construction conditions are more and more severe, the underground temperature and the mineralization degree of the stratum water are more and more high, so that the emulsifying performance of the conventional emulsifying viscosity reducer in a high-temperature and high-salt environment is greatly reduced, and the development of a deep heavy oil reservoir is seriously restricted.
CN 109097017A discloses a temperature-resistant and salt-resistant thick oil emulsifying viscosity reducer and a preparation method thereof, the temperature-resistant and salt-resistant thick oil emulsifying viscosity reducer is stable under severe conditions, has excellent salt resistance, calcium and magnesium resistance and temperature resistance, has low interfacial tension and strong surface activity, and can meet the requirements of the exploitation, emulsification and viscosity reduction of thick oil of offshore high-temperature and high-salt oil reservoirs; the principle of the comparison piece is that the viscosity reducer is prepared by phenolic aldehyde condensation reaction;
CN 110591012B is a water-soluble hyperbranched polymer thick oil viscosity reducer and a preparation method thereof, and is prepared by carrying out free radical polymerization reaction on 0.1-0.5% of functional framework monomer, 10-20% of acrylamide, 35-45% of modified nonionic polyoxyethylene ether and 40-50% of anionic monomer sodium olefin sulfonate in an aqueous solution at 45-60 ℃; the emulsion can be rapidly dissolved in water, has strong heat resistance and salt resistance, good mixing and emulsifying properties with crude oil, and the viscosity reduction rate of the middle-low viscosity thick oil is more than 85%, and the emulsion is easy to break; polymerizing the hyperbranched monomer, the sulfonic acid group and the ethoxy group to obtain the thickened oil viscosity reducer;
CN103450868A discloses a temperature-resistant salt-tolerant water-soluble amphiphilic polymer composite thickened oil viscosity reducer, which is formed by compounding A, B two components; the component A is an amphiphilic polymer formed by quaternary copolymerization of nonionic polyether acrylate and the like; the component B is a small molecular surfactant; the viscosity reducing agent has the viscosity reducing rate of over 95 percent for medium-low viscosity thick oil and 85 percent for medium-high ultrahigh viscosity thick oil; the viscosity reducing agent system is obtained by compounding a polymer and a surfactant.
In summary, in the prior art, a viscous oil emulsification viscosity-reducing agent system is mostly prepared by preparing a high molecular polymer or by utilizing the synergistic effect of the high molecular polymer and a small molecular surfactant; in addition, the oil-in-water emulsion breaking is realized by adding an organic demulsifier into the system, which brings great inconvenience to construction and engineering operation and increases the construction difficulty. The stimulus-response functional groups are introduced into the polymer results and the molecular structure of the polymer is regulated, so that a dual stimulus-response type polymer thickened oil emulsification viscosity-reducing agent system which simultaneously takes the temperature resistance and salt resistance of the polymer, the dissolution property and the emulsification property of the surfactant into consideration is developed and prepared, acid gas is generated in situ under the stimulus of temperature of the system, emulsion breaking is caused, oil-water separation is realized, and the system is more convenient for site construction and has important practical significance.
Disclosure of Invention
The invention aims to provide a dual-stimulus response type polymer thickened oil emulsifying viscosity reducer and a preparation method thereof, which solve the technical problems in the prior art.
In order to achieve the technical purpose and the technical effect, the invention is realized by the following technical scheme:
the dual stimulus response type polymer thick oil emulsifying viscosity reducer comprises 0.05-0.3 wt% of polymer emulsifier; 0.5 to 2.0 weight percent of in-situ carbon generating agent and the balance of water.
Further, the method comprises the steps of,the polymer emulsifier is prepared from 60-70% by mass of acrylamide, acrylic acid, sodium styrene sulfonate and a responsive functional monomer: 10-20%: 5.0 to 10 percent: 0.5-10% of polymerization, and obtaining the polymer with viscosity average molecular weight of 5 x 10 by adopting aqueous solution free radical polymerization 5 ～10×10 5 g/mol of a polymer emulsifier, the chemical structural formula of which is shown as follows:
further, R1 and R2 in the polymer structure are alkyl chains or aromatic rings with the carbon number of 1-6.
Further, the responsive functional monomer is one or more of N, N-dialkyl acrylamide, dimethylaminoethyl methacrylate and N-4-vinylphenyl-N, N-dimethylamine.
Further, the in-situ carbon generating agent is one or a combination of more of carbamide, sodium bicarbonate and ammonium bicarbonate;
the dual-stimulus responsive polymer thick oil emulsification viscosity reducer has hydrophilic groups and hydrophobic groups in the molecules of the water-soluble polymer emulsifier, so that the water-soluble polymer emulsifier and thick oil are emulsified under a certain oil-water ratio to form stable oil-in-water emulsion, the viscosity of the thick oil is greatly reduced, and the flowability of the thick oil is improved; the aromatic ring and the hydrophobic chain contained in the responsive monomer have similar chemical structures with colloid asphaltene in the thick oil molecules, so that the asphaltene in the thick oil molecules can be dispersed, and the viscosity of the thick oil is reduced; in addition, the existence of the aromatic ring and the hydrophobic chain and the amide group, the sulfonic group and other hydrophilic groups in the structure of the emulsifier endow the emulsifier with excellent surface activity, so that the emulsifying performance of the emulsifier and crude oil is improved.
When the emulsified low-viscosity crude oil is mined to the ground, the in-situ carbon generating agent in the system is thermally decomposed to generate carbon dioxide under the stimulation of temperature; the tertiary amine group in the polymer structure generates pH stimulus response under the action of carbon dioxide and water, and the hydrophobic part in the polymer structure is converted into a hydrophilic part, so that the oil-in-water emulsion is quickly demulsified, and the oil-water separation is realized.
The invention also aims to provide a preparation method of the dual-stimulus response type polymer thick oil emulsification viscosity reducing agent, which comprises the following steps:
s1: acrylamide, acrylic acid, sodium styrene sulfonate and a responsive functional monomer are mixed according to the mass percentage of 60-70 percent: 10-20%: 5.0 to 10 percent: adding 0.5-10% of the solution into deionized water in turn to prepare uniform solution, and cooling to about 5 ℃; 2% NaOH solution is adopted to adjust the pH value of the monomer solution to 6.5-7.5, and the temperature of the solution is kept to be no more than 25 ℃;
s2: pouring the solution in the step S1 into a vacuum flask, and introducing nitrogen for 30min to ensure that dissolved oxygen in the solution is removed;
s3: after the deoxidization is finished, sequentially adding a redox initiator and an azo initiator into the solution;
s4: and monitoring the temperature change of the system in the reaction process, keeping the temperature for 4 hours until the system temperature reaches a peak value, and crushing, drying and granulating the polymer for later use after the reaction is finished.
The invention further aims to provide an application of the dual-stimulus response type polymer thickened oil emulsification viscosity reducing agent in the preparation of thickened oil emulsification viscosity reducing products;
the application is as follows: preparing a polymer concentration solution by emulsifying and viscosity-reducing agent of the polymer thick oil, and then viscosity-reducing the thick oil according to a certain oil-water ratio;
the invention has the beneficial effects that:
according to the dual-stimulus responsive polymer thickened oil emulsifying viscosity reducer, under the stimulus of temperature, a carbon generating agent is decomposed to release carbon dioxide, and then under the action of the carbon dioxide, tertiary amine groups in the emulsifier obtain protons, so that the polymer loses surface activity, and an O/W emulsion is demulsified, so that oil-water separation is realized;
the dual-stimulus responsive polymer thick oil emulsification viscosity reducer comprises a polymer emulsifier and an in-situ carbon generator; the invention adjusts the emulsification-demulsification process between the viscosity reducing agent and the thick oil by the response group in the molecular structure of the emulsification viscosity reducing agent and the carbon generating agent in the system, thereby realizing the efficient exploitation of the thick oil;
the dual-stimulus responsive polymer thickened oil emulsification viscosity-reducing agent disclosed by the invention has the advantages that the surface activity of the polymer type emulsification viscosity-reducing agent is improved by utilizing the small molecular polymer, so that the emulsification capacity of the viscosity-reducing agent is improved;
the dual-stimulus response polymer thickened oil emulsifying viscosity reducer has the advantages that the high temperature or only the temperature is required to be increased in the demulsification process, so that the carbon dioxide is generated in situ by the carbon generating agent, and the demulsification of the emulsified thickened oil is realized;
the invention discloses a specific preparation method of a dual-stimulus response polymer thickened oil emulsification viscosity-reducing agent, which has the advantages of simple preparation process, high yield, simple post-treatment, stable performance, low cost and wide market prospect.
Of course, it is not necessary for any one product to practice the invention to achieve all of the advantages set forth above at the same time.
Detailed Description
In order to more clearly describe the technical scheme of the embodiment of the present invention, the present invention will be described in detail with reference to specific embodiments.
A preparation method of a dual stimulus response type polymer thick oil emulsification viscosity reducing agent comprises the following steps:
acrylamide, acrylic acid, sodium styrene sulfonate and a responsive functional monomer are mixed according to the mass percentage of 60-70 percent: 10-20%: 5.0 to 10 percent: adding 0.5-10% of the solution into deionized water in turn to prepare uniform solution, adjusting the pH of the solution to 6.5-7.5, and introducing nitrogen to deoxidize;
the responsive functional monomer is one or more of N, N-dialkyl acrylamide, dimethylaminoethyl methacrylate and N-4-vinyl phenyl-N, N-dimethylamine;
after the deoxidization is finished, adding an initiator into the solution, and after the reaction is finished, crushing, drying and granulating the polymer;
the polymer thick oil emulsifying viscosity reducing agent is prepared into a solution with a certain polymer concentration.
The chemical reaction has the structural formula as follows:
the invention is illustrated below with reference to specific examples:
comparative examples and examples 1 to 4 were set according to the raw materials of the polymer thickened oil emulsion viscosity-reducing agent, and the kinds and technical parameters of the raw materials in the examples and comparative examples are shown in Table 1
Table 1 kinds and technical parameters of the respective raw materials in examples and comparative examples
Analysis of results:
emulsifying property and viscosity-reducing rate test
The viscosity reducing performance of the polymer type emulsified viscosity reducing agent obtained in examples 1 to 4 and comparative example was examined in this experimental example. The detection method comprises the following steps: the polymer type emulsifying viscosity reducer obtained in examples 1-4 and comparative example is prepared into 0.8% polymer solution by using simulated saline with the mineralization degree of 10000mg/L respectively, and is aged for 24 hours at 160 ℃, then Liaohe thick oil is mixed with the simulated saline in a mass ratio of 4:6, and the simulated stratum is subjected to low shear rate for 5-50 s < -1 > at 50 ℃ to form stable oil-in-water emulsion. The viscosity of the thickened oil and the oil-in-water emulsion is respectively measured at 50 ℃ by using the rotational viscosity agent, and the viscosity reduction rate of the viscosity reducing agent is calculated according to the viscosity reduction rate calculation method as follows:
η in the formula-viscosity-reducing rate;
mu 0-50 ℃ viscosity of the thick oil sample, mPa.s;
mu-viscosity of the thick oil emulsion after addition of the sample solution, mPa.s.
The viscosity reduction rates of the dual stimulus-responsive polymer emulsion viscosity reduction agents in examples and comparative examples are shown in table 2:
TABLE 2 viscosity reduction Rate of each emulsifier in examples and comparative examples
Interfacial activity test
Interface activity test conditions and steps: the surface tension of the aqueous solution of the dual stimulus-responsive polymer emulsion viscosity-reducing agent was measured by a hanger method using a DSA30S surface interfacial tensiometer from Kruss, germany, the experimental temperature was 25 ℃, and the results are shown in table 3 below.
TABLE 3 surface tension of the emulsifiers of examples and comparative examples
Demulsification test
After the emulsified viscosity-reduced thick oil is extracted to the ground, the existing 2.0% of carbon generating agent sodium bicarbonate in the system is decomposed into carbon dioxide under the action of temperature, so that emulsion is demulsified, oil-water separation is realized, and the experimental results are shown in table 4.
Table 4 example demulsification test
| Time (h) | Example 1 | Example 2 | Example 3 | Example 4 |
| 0.5 | - | - | - | - |
| 1.0 | Demulsification | Demulsification | - | - |
| 1.5 | - | - | - | Demulsification |
| 2.0 | - | - | Demulsification | - |
In the description of the present specification, reference to the term "one embodiment" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (7)
1. A dual stimulus response type polymer thickened oil emulsification viscosity reducing agent is characterized in that: comprises 0.05 to 0.3 weight percent of polymer emulsifier; 0.5 to 2.0 weight percent of in-situ carbon generating agent and the balance of water;
the polymer emulsifier is prepared from 60-70% by mass of acrylamide, acrylic acid, sodium styrene sulfonate and a responsive functional monomer: 10-20%: 5.0 to 10 percent: 0.5-10% of polymerization, and adopting aqueous solution free radical polymerization to obtain a polymer emulsifier;
the polymer emulsifier has the following structural characteristics:
wherein: r1 and R2 are alkyl chains or aromatic rings with the carbon number of 1-6.
2. The dual stimulus-responsive polymer thick oil emulsification viscosity reducing agent of claim 1, wherein: the mass percentages of the acrylamide, the acrylic acid, the sodium styrenesulfonate and the responsive functional monomer in the polymer emulsifier are 65%, 18%, 7% and 10% respectively.
3. The dual stimulus-responsive polymer thick oil emulsification viscosity reducing agent of claim 2, wherein: the responsive functional monomer is one or more of N, N-dialkyl acrylamide, dimethylaminoethyl methacrylate and N-4-vinyl phenyl-N, N-dimethylamine.
4. The dual stimulus-responsive polymer thick oil emulsification viscosity reducing agent of claim 1, wherein: the in-situ carbon generating agent is one or a combination of more of carbamide, sodium bicarbonate and ammonium bicarbonate.
5. A process for preparing the dual stimulus-responsive polymeric viscous oil emulsification viscosity reducing agent of any one of claims 1-4, characterized by: the polymer emulsifier is prepared by the following steps:
s1: acrylamide, acrylic acid, sodium styrene sulfonate and a responsive functional monomer are mixed according to the mass percentage of 60-70 percent: 10-20%: 5.0 to 10 percent: adding 0.5-10% of the solution into deionized water in turn to prepare uniform solution, and cooling to about 5 ℃; 2% NaOH solution is adopted to adjust the pH value of the monomer solution to 6.5-7.5, and the temperature of the solution is kept to be no more than 25 ℃;
s2: pouring the solution in the step S1 into a vacuum flask, and introducing nitrogen for 30min to ensure that dissolved oxygen in the solution is removed;
s3: after the deoxidization is finished, sequentially adding a redox initiator and an azo initiator into the solution;
s4: and monitoring the temperature change of the system in the reaction process, keeping the temperature for 4 hours until the system temperature reaches a peak value, and crushing, drying and granulating the polymer after the reaction is finished.
6. The method for preparing the dual stimulus-responsive polymer thick oil emulsification viscosity reducing agent as claimed in claim 5, wherein: free radical polymerization in aqueous solution to give a viscosity average molecular weight of 5X 10 5 ～10×10 5 g/mol of polymer emulsifier.
7. Use of a dual stimulus-responsive polymer thickened oil emulsion viscosity reducing agent according to any one of claims 1-4 in the preparation of thickened oil emulsion viscosity reducing products or in thickened oil emulsion viscosity reducing.
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