CN111087996B - High-temperature-resistant composite gel plugging agent and preparation method and application thereof - Google Patents
High-temperature-resistant composite gel plugging agent and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of oil exploitation, and provides a high-temperature-resistant composite gel plugging agent, and a preparation method and application thereof. The high-temperature resistant composite gel plugging agent comprises: acrylamide polymer, water-soluble phenolic resin, organic chromium, oxygen scavenger, urea compound and water, wherein the urea compound has a structure shown in formula (1) and/or formula (2), R1And R2Each independently selected from hydrogen or 2-propynyl; r3、R4And R5Each independently selected from oxygen, sulfur or imino. The high-temperature-resistant composite gel plugging agent provided by the invention is simple in preparation method, can effectively plug a steam channeling channel for a long time (30-90 days) at a higher temperature (150-.
Description
Technical Field
The invention relates to the technical field of oil exploitation, in particular to a high-temperature-resistant composite gel plugging agent and a preparation method and application thereof.
Background
Steam stimulation is the main mode of heavy oil development, is considered to be a conventional, economical and effective method and is widely used by heavy oil fields. Along with the progress of the multiple times of huff and puff stages, the water invasion and steam channeling are serious, the water content of the oil well is greatly increased, different degrees of influence are brought to the thermal recovery of the heavy oil reservoir, and the thermal recovery effect is deteriorated. The high water content of an oil well in the thermal recovery process of a heavy oil reservoir becomes a main problem influencing the thermal recovery effect. At present, one of the most effective methods for solving the problem is to use a gel plugging agent to block a steam channeling channel and improve the utilization degree and recovery ratio of thick oil.
The existing gel plugging agent is compounded and injected into a stratum by taking a polyacrylamide aqueous solution as a thickening agent and phenolic resin as a crosslinking agent, and is crosslinked in situ at the deep part of the stratum to form gel for plugging water. However, the technology is only suitable for the environment below 120 ℃, and cannot stably block water for a long time in a high-temperature steam huff and puff environment, because the system is unstable at high temperature, the working fluid enters the stratum and is excessively crosslinked and dehydrated in the early stage, and the working fluid is thermally degraded in the later stage. Therefore, for the water shutoff operation of the steam huff and puff of the heavy oil reservoir, the construction success rate is not high, the oil increasing effective period is short, and the oil increasing effect is limited. The gel plugging agent which is effective for a long time at a higher temperature and in a longer time range is a current technical difficulty and needs to be broken through urgently.
Disclosure of Invention
Aiming at the problem that the existing gel plugging agent can not be effectively applied to higher temperature and realize longer-time water plugging, the invention aims to provide a novel high-temperature-resistant composite gel plugging agent, and a preparation method and application thereof. The high-temperature-resistant composite gel plugging agent can effectively plug a steam channeling channel in a higher temperature environment and in a longer time range, and realizes the high-efficiency development of a heavy oil reservoir.
According to a first aspect of the present invention, there is provided a high temperature resistant composite gel plugging agent comprising: acrylamide polymer, water-soluble phenolic resin, organic chromium, an oxygen scavenger, a urea compound and water, wherein the urea compound has a structure shown in a formula (1) and/or a formula (2),
wherein R is1And R2Each independently selected from hydrogen or 2-propynyl; r is3And R4Each independentlyOxygen, sulfur or imino;
the content of the urea compound is 0.1-2 wt% based on the total weight of the high-temperature resistant composite gel plugging agent.
According to a second aspect of the present invention, the present invention provides a method for preparing the high temperature resistant composite gel blocking agent, the method comprising:
(1) dissolving acrylamide polymer in water to obtain polymer water solution;
(2) and adding water-soluble phenolic resin, organic chromium, urea compounds and an oxygen scavenger into the polymer aqueous solution, and stirring until the mixture is dissolved to obtain the high-temperature-resistant composite gel plugging agent.
According to a third aspect of the invention, the invention provides application of the high-temperature-resistant composite gel plugging agent in thickened oil steam stimulation thermal recovery.
The high-temperature-resistant composite gel plugging agent provided by the invention is simple in preparation method, can effectively plug a steam channeling channel for a long time (30-90 days) at a higher temperature (150-. Compared with the existing gel plugging agent, the gel plugging agent has higher plugging rate and longer plugging time, and can be suitable for large pore path plugging operation in heavy oil steam huff and puff thermal recovery operation.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
According to a first aspect of the present invention, the present invention provides a high temperature resistant composite gel blocking agent, comprising: acrylamide polymer, water-soluble phenolic resin, organic chromium, an oxygen scavenger, a urea compound and water.
In the present invention, the urea compound has a structure represented by formula (1) and/or formula (2),
wherein R is1And R2Each independently selected from hydrogen or 2-propynyl, R3And R4Each independently oxygen, sulfur or imino.
Preferably, the urea compound is one or more of urea, 2-propynyl urea, biuret, thiobiuret and 2-imino-4-thiobiuret.
More preferably, the urea-based compound is urea. Urea has a smaller molecular weight and volume relative to its dimer (e.g., biuret) and its substituted compound (e.g., 2-propynyl urea), has less steric hindrance and better mobility when reacted in the gellant system, and is able to compete better with polyacrylamide-based polymers to some extent during the condensation reaction with water-soluble phenolic resins.
In the invention, the content of the urea compound is 0.1-2 wt%, preferably 0.2-1 wt% based on the total weight of the high temperature resistant composite gel blocking agent.
In the present invention, the kind and amount of the acrylamide-based polymer can be selected with reference to the prior art, and the acrylamide-based polymer can be synthesized according to the prior art or obtained commercially. For the present invention, preferably, the acrylamide-based polymer is one or more of partially hydrolyzed polyacrylamide, partially hydrolyzed methylene polyacrylamide, acrylamide/acrylic acid/AMPS sodium salt copolymer, and acrylamide/acrylic acid/acrylonitrile sodium salt copolymer. Wherein the partially hydrolyzed polyacrylamide and the acrylamide/acrylic acid/AMPS sodium salt copolymer are available from Shandong Baumo et al.
Preferably, the viscosity average molecular weight of the acrylamide polymer is 800-3500 ten thousand, more preferably 1000-3000 ten thousand; the degree of hydrolysis of the acrylamide-based polymer is 8 to 35%, more preferably 10 to 25%.
In the present invention, the degree of hydrolysis is measured by the method for measuring the degree of hydrolysis of partially hydrolyzed polyacrylamide according to the national standard GB/T12005.6-1989.
Preferably, the content of the acrylamide polymer is 0.1-2 wt%, more preferably 0.2-1 wt%, based on the total weight of the high temperature resistant composite gel blocking agent.
In the present invention, the water-soluble phenol resin is preferably obtained by polymerizing phenol and formaldehyde monomers in a molar ratio of 0.2 to 0.75 under an alkaline condition. Generally, the water-soluble phenolic resin obtained by the reaction is a solid-liquid mixture with a pH value of more than 11 and a solid content of more than 40 weight percent.
Preferably, the content of the water-soluble phenolic resin is 0.1-2 wt%, more preferably 0.2-1 wt% based on the total weight of the high-temperature resistant composite gel blocking agent.
In the present invention, the organic chromium is preferably one or more of chromium acetate, chromium oxalate, chromium lactate, chromium propionate, chromium malonate, and chromium citrate, and more preferably chromium lactate. The organic acid chromium can be prepared according to the prior art, and according to one embodiment of the invention, chromium (II) is firstly reacted with sodium nitrite, reduced to chromium (III) and then complexed with an organic acid (preferably one or more of acetic acid, oxalic acid, lactic acid, propionic acid, malonic acid and citric acid), wherein the molar ratio of the reaction of chromium (II) and sodium nitrite is 1/4-1/3, the molar ratio of the complexation of chromium (III) and the reaction of organic acid is 1/50-1/10, the obtained organic chromium is dark green solution, the pH value is 4-10, and the effective content of chromium (III) is more than 2%.
Preferably, the content of the organic chromium is 0.01 to 2 wt%, more preferably 0.03 to 1.5 wt%, based on the total weight of the high temperature resistant composite gel blocking agent.
In the invention, the oxygen scavenger can reduce the oxidative degradation of the polymer in the system, and the type and the dosage of the oxygen scavenger can be selected according to the prior art. In the present invention, preferably, the oxygen scavenger is one or more of sodium thiosulfate, sodium sulfite, sodium bisulfite, sodium hydrosulfite and erythorbic acid.
Preferably, the weight of the oxygen scavenger is 0.05-1 wt% based on the total weight of the high-temperature resistant composite gel plugging agent.
In the present invention, water is used as the solvent and the reaction medium in the high temperature resistant composite gel blocking agent system, and the selection of the solvent and the reaction medium is not particularly limited in the present invention. The degree of mineralization of water is usually less than 500 mg, and can be natural water, such as rivers, lakes, atmospheric water, seawater, groundwater, etc., and artificial water, such as tap water, distilled water, deionized water, or heavy water. In the present invention, the content of water is 91 to 99.64 wt%, preferably 94.5 to 99.32 wt%, based on the total weight of the high temperature resistant composite gel blocking agent.
In the invention, the contents of all components in the high-temperature resistant composite gel plugging agent are calculated by the material feeding amount.
The high-temperature resistant composite gel plugging agent is particularly suitable for plugging a steam channeling pipeline in the process of steam huff and puff thermal thickened oil recovery. Specifically, hydroxyl groups in the water-soluble phenolic resin and amide groups of the acrylamide polymer can undergo an in-situ dehydration condensation reaction at high temperature, so that the acrylamide polymer is crosslinked; meanwhile, the organic chromium in the system and the carboxyl of the acrylamide polymer are subjected to coordination reaction, so that the acrylamide polymer is crosslinked, the system gradually forms gel along with the reaction, and a steam channeling pipeline is blocked in the process of steam huff and puff thermal recovery of the thick oil. In addition to the above reaction, the urea compound contained in the system can also undergo a dehydration condensation reaction with the water-soluble phenol resin, and the possible reaction mechanism is as follows (taking the urea compound represented by formula (1) as an example):
therefore, the urea compound competes with the condensation reaction of the acrylamide polymer and the water-soluble phenolic resin, thereby reducing the crosslinking speed of the acrylamide polymer and enabling the crosslinking reaction of the acrylamide polymer to be continuously carried out for a long time. Through determination, the high-temperature resistant composite gel plugging agent disclosed by the invention is gelled at a high temperature of 150 ℃ for two days to form plugging.
In addition, the addition of the urea compound reduces the density of crosslinking active points in the system, inhibits the dehydration phenomenon caused by excessive crosslinking of the acrylamide polymer, can adjust the distance between the crosslinking active points, slows down the degree of coverage of the crosslinking active points, improves the crosslinking efficiency, increases the strength of gel formed by the crosslinking system, and enables the formed gel system to be stable at a higher temperature.
According to a second aspect of the present invention, there is provided a method for preparing the high temperature resistant composite gel blocking agent according to the first aspect of the present invention, the method comprising:
(1) dissolving acrylamide polymer in water to obtain polymer water solution;
(2) and adding water-soluble phenolic resin, organic chromium, urea compounds and an oxygen scavenger into the polymer aqueous solution, and stirring until the mixture is completely dissolved to obtain the high-temperature-resistant composite gel plugging agent.
According to a third aspect of the invention, the invention provides application of the high-temperature-resistant composite gel plugging agent in thickened oil steam stimulation thermal recovery. As mentioned above, the high temperature resistant composite gel plugging agent is particularly suitable for plugging a steam channeling pipeline in the process of steam huff and puff thermal recovery of thick oil.
According to the invention, the application may comprise: and injecting the high-temperature resistant composite gel plugging agent into the stratum, so that the high-temperature resistant composite gel plugging agent is crosslinked in situ in the stratum to form gel.
Under the environment of steam huff and puff thermal recovery of thickened oil, the gel plugging agent formed by the high-temperature resistant composite gel plugging agent can be kept for 30-90 days at the temperature of 150-180 ℃.
The present invention will be described in detail below by way of examples.
Example 1
This example is used to illustrate the high temperature resistant composite gel blocking agent and the preparation method thereof.
At room temperature, 20 g of partially hydrolyzed polyacrylamide (viscosity average molecular weight 800 ten thousand, degree of hydrolysis 8%) is dissolved in 1L of water, and the mixture is stirred at 500 rpm until the partially hydrolyzed polyacrylamide is completely dissolved; and then sequentially adding 20 g of water-soluble phenolic resin (the molar ratio of phenol to formaldehyde is 0.3), 20 g of chromium acetate, 10 g of urea and 10 g of sodium thiosulfate, and stirring until the mixture is completely dissolved to obtain the high-temperature-resistant composite gel plugging agent.
The blocking performance of the high temperature resistant composite gel blocking agent at the temperature of 150 ℃ and the standing time of 60 days is tested, and the results are shown in table 1.
The Darcy principle is applied to the test of the plugging performance, and the prior art can be specifically referred to. The plugging performance test method comprises the following steps:
filling a simulation core (the diameter d of the core is 25mm, the length L of the core is 200mm), injecting water into the core at the flow rate of 2 ml/min (injection rate Q) after vacuumizing, and measuring the permeability (k) before core plugging0) (ii) a And then injecting 1.0-1.5PV of the high-temperature-resistant composite gel plugging agent of the embodiment into the core model, plugging two ends of the core by using screws, putting the core into a constant temperature box with the temperature of 150 ℃ for standing for 60 days, injecting water again until the pressure is stable, recording the reading on a pressure gauge to obtain injection pressure difference, and calculating the permeability (k') after the core is plugged so as to calculate the plugging rate.
For ease of description and explanation, k will be given0And k' are collectively called as core permeability k, and the calculation formula is as follows:
wherein Q is the injection rate, mL · s-1(ii) a μ is fluid viscosity, mPa · s; a is the cross section area of the sand-filled model in cm2，A＝πd2(ii)/4; Δ P is the injection pressure difference, 10-1MPa；k，μm2。
In addition, the plugging rate (eta) is taken as a parameter for representing the plugging performance of the plugging agent, and the calculation formula is as follows:
example 2
This example is used to illustrate the high temperature resistant composite gel blocking agent and the preparation method thereof.
At room temperature, 4 g of acrylamide/acrylic acid/AMPS sodium salt copolymer (viscosity average molecular weight is 2500 ten thousand, hydrolysis degree is 20%) is dissolved in 1L of water, and stirring is carried out at a speed of 500 revolutions per minute until the acrylamide/acrylic acid/AMPS sodium salt copolymer is completely dissolved; 4 g of water-soluble phenolic resin (the molar ratio of phenol to formaldehyde is 0.3), 2 g of chromium lactate, 2 g of urea and 2 g of isoascorbic acid are added in sequence and stirred until all the components are dissolved, so as to obtain the high-temperature resistant composite gel plugging agent of the embodiment.
The blocking rate of the high-temperature resistant composite gel blocking agent is tested under the conditions of 150 ℃/60 days, 150 ℃/75 days, 150 ℃/90 days, 165 ℃/60 days and 180 ℃/60 days, the testing method is the same as that of example 1, and the testing results are shown in tables 1 and 2.
Example 3
This example is used to illustrate the high temperature resistant composite gel blocking agent and the preparation method thereof.
At room temperature, 1 g of acrylamide/acrylic acid/AMPS sodium salt copolymer (viscosity average molecular weight is 3500 ten thousand, hydrolysis degree is 35%) is dissolved in 1L of water, and the mixture is stirred at 500 revolutions per minute until the acrylamide/acrylic acid/AMPS sodium salt copolymer is completely dissolved; and then sequentially adding 1 g of water-soluble phenolic resin (the molar ratio of phenol to formaldehyde is 0.3), 0.1 g of chromium oxalate, 1.5 g of urea and 0.5 g of sodium bisulfite, and stirring until the mixture is completely dissolved to obtain the high-temperature resistant composite gel plugging agent.
The blocking rate of the high temperature resistant composite gel blocking agent at the temperature of 150 ℃ and the standing time of 60 days is tested, the test method is the same as that of example 1, and the test results are shown in table 1.
Example 4
This example is used to illustrate the high temperature resistant composite gel blocking agent and the preparation method thereof.
At room temperature, 4 g of acrylamide/acrylic acid/AMPS sodium salt copolymer (viscosity average molecular weight is 2500 ten thousand, hydrolysis degree is 20%) is dissolved in 1L of water, and stirring is carried out at 500 revolutions per minute until the acrylamide/acrylic acid/AMPS sodium salt copolymer is completely dissolved; and then, sequentially adding 4 g of water-soluble phenolic resin (the molar ratio of phenol to formaldehyde is 0.3), 2 g of chromium lactate, 5 g of biuret and 2 g of isoascorbic acid, and stirring until the mixture is completely dissolved to obtain the high-temperature-resistant composite gel plugging agent.
The blocking rate of the high temperature resistant composite gel blocking agent at the temperature of 150 ℃ and the standing time of 60 days is tested, the test method is the same as that of example 1, and the test results are shown in table 1.
Example 5
This example is used to illustrate the high temperature resistant composite gel blocking agent and the preparation method thereof.
At room temperature, 20 g of partially hydrolyzed polyacrylamide (viscosity average molecular weight 800 ten thousand, degree of hydrolysis 10%) is dissolved in 1L of water, and the mixture is stirred at 500 rpm until the partially hydrolyzed polyacrylamide is completely dissolved; and then sequentially adding 20 g of water-soluble phenolic resin (the molar ratio of phenol to formaldehyde is 0.3), 20 g of chromium acetate, 20 g of urea and 10 g of sodium thiosulfate, and stirring until the chromium acetate, the urea and the sodium thiosulfate are completely dissolved to obtain the high-temperature-resistant composite gel plugging agent.
The blocking rate of the high temperature resistant composite gel blocking agent at the temperature of 150 ℃ and the standing time of 60 days is tested, the test method is the same as that of example 1, and the test results are shown in table 1.
Comparative example 1
At room temperature, 4 g of acrylamide/acrylic acid/AMPS sodium salt copolymer (viscosity average molecular weight is 2500 ten thousand, hydrolysis degree is 20%) is dissolved in 1L of water, and stirring is carried out at a speed of 500 revolutions per minute until the acrylamide/acrylic acid/AMPS sodium salt copolymer is completely dissolved; 4 g of water-soluble phenol resin (phenol/formaldehyde molar ratio of 0.3), 2 g of chromium lactate and 2 g of isoascorbic acid were added in this order and stirred until all were dissolved to obtain the gel blocking agent of the comparative example.
The gel blocking agent was tested for blocking rate at 150 ℃ for 60 days, the test method was the same as in example 1, and the test results are shown in table 1.
And (3) a plugging rate test result:
TABLE 1
Note: table 1 shows the results of the test of the plugging rate (150 ℃ C./60 days) of examples and comparative examples.
TABLE 2
Note: table 2 shows the results of the plugging rate tests of example 2 under different test conditions.
It can be seen from table 1 that the high temperature resistant composite gel plugging agents of examples 1 to 5 have higher plugging rates than the composite gel plugging agent not containing urea compounds in comparison with comparative example 1 under the condition of standing at 150 ℃ for 60 days. As can be seen from Table 2, the high temperature resistant composite gel plugging agent can stably exist for at least 90 days at the temperature of 150 ℃, and keeps a higher plugging rate; when the temperature is increased to 180 ℃, the composite material can still stably exist for at least 60 days. Therefore, the high-temperature-resistant composite gel plugging agent is applied to heavy oil steam huff-puff thermal recovery, can effectively plug a steam channeling channel at a high temperature (150-.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (12)
1. A high temperature resistant composite gel plugging agent, comprising: acrylamide polymer, water-soluble phenolic resin, organic chromium, an oxygen scavenger, a urea compound and water, wherein the urea compound has a structure shown in a formula (1) and/or a formula (2),
wherein R is1And R2Each independently selected from hydrogen or 2-propynyl, R3And R4Each independently selected from oxygen, sulfur or imino;
the content of the urea compound is 0.1-2% by weight based on the total weight of the high-temperature resistant composite gel plugging agent;
based on the total weight of the high-temperature resistant composite gel plugging agent, the content of the acrylamide polymer is 0.1-2 wt%, the content of the water-soluble phenolic resin is 0.1-2 wt%, the content of the organic chromium is 0.01-2 wt%, and the content of the oxygen scavenger is 0.05-1 wt%;
the water-soluble phenolic resin is prepared from phenol and formaldehyde according to the weight ratio of 0.2-0.75: 1, is polymerized.
2. The high temperature resistant composite gel blocking agent of claim 1, wherein the content of the urea compound is 0.2-1 wt% based on the total weight of the high temperature resistant composite gel blocking agent.
3. The high temperature resistant composite gel blocking agent of claim 1 or 2, wherein the urea compound is one or more of urea, 2-propynyl urea, biuret, thiobiuret, and 2-imino-4-thiobiuret.
4. The high temperature resistant composite gel blocking agent of claim 3, wherein the urea compound is urea.
5. The high temperature resistant composite gel blocking agent of claim 1, wherein the acrylamide-based polymer is one or more of partially hydrolyzed polyacrylamide, partially hydrolyzed methylene polyacrylamide, acrylamide/acrylic acid/AMPS sodium salt copolymer, and acrylamide/acrylic acid/acrylonitrile sodium salt copolymer.
6. The high-temperature-resistant composite gel blocking agent of claim 5, wherein the viscosity-average molecular weight of the acrylamide polymer is 800-3500 ten thousand, and the hydrolysis degree of the acrylamide polymer is 8-35%.
7. The high temperature resistant composite gel blocking agent of claim 1, wherein the oxygen scavenger is one or more of sodium thiosulfate, sodium sulfite, sodium bisulfite, sodium hydrosulfite and erythorbic acid.
8. The high temperature resistant composite gel blocking agent of claim 1, wherein the organic chromium is one or more of chromium acetate, chromium oxalate, chromium lactate, chromium propionate, chromium malonate and chromium citrate.
9. The high temperature resistant composite gel blocking agent of claim 1, wherein the organic chromium is chromium lactate.
10. A method for preparing the high temperature resistant composite gel blocking agent of any one of claims 1 to 9, wherein the method comprises:
(1) dissolving the acrylamide polymer in water to obtain a polymer aqueous solution;
(2) and adding water-soluble phenolic resin, organic chromium, urea compounds and an oxygen scavenger into the polymer aqueous solution, and stirring until the mixture is dissolved to obtain the high-temperature-resistant composite gel plugging agent.
11. Use of the high temperature resistant composite gel block agent of any one of claims 1 to 9 in heavy oil steam stimulation thermal recovery.
12. The application of claim 11, wherein the application comprises: and injecting the high-temperature-resistant composite gel plugging agent into the stratum, so that the high-temperature-resistant composite gel plugging agent is crosslinked in situ in the stratum to form gel.
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| CN115746808B (en) * | 2021-09-06 | 2024-04-30 | 中国石油天然气股份有限公司 | Plugging agent and application thereof |
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| CN107286917A (en) * | 2017-06-19 | 2017-10-24 | 中国地质大学（北京） | Retarded crosslinking gel diverting agent and preparation method thereof and composition and application |
| CN107699219A (en) * | 2017-10-25 | 2018-02-16 | 中国石油化工股份有限公司 | High temperature resistance and high strength gel adjusts stifled system and preparation method thereof |
| CN108395884A (en) * | 2018-04-12 | 2018-08-14 | 盘锦阳辉科技有限公司 | High-temperature-resistant water shutoff profile control agent and preparation method thereof |
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