CN111808585A - Slow-crosslinking temperature-resistant salt type high-strength gel and preparation method and application thereof - Google Patents
Slow-crosslinking temperature-resistant salt type high-strength gel and preparation method and application thereof Download PDFInfo
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
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Abstract
The invention relates to a slow-crosslinking temperature-resistant salt type high-strength gel and a preparation method and application thereof, belonging to the technical field of oilfield chemistry, and the slow-crosslinking temperature-resistant salt type high-strength gel comprises the following components in percentage by mass: 6-7.5% of polyvinyl alcohol, 0.3-0.6% of aldehyde crosslinking agent, 0.25-0.5% of catalyst, 2-4% of stabilizer and the balance of water, wherein the sum of the mass percentages of the components is 100. Wherein the aldehyde crosslinking agent is terephthalaldehyde or m-phthalaldehyde; the catalyst is one of chloroacetic acid, trichloroacetic acid, methyl chloroacetate, isopropylbenzene sulfonic acid, butyl benzene sulfonic acid, naphthalene sulfonic acid and acrylamide methyl propane sulfonic acid; the stabilizer is nano-scale silicon dioxide particles. The jelly provided by the invention has excellent temperature resistance and salt tolerance, can realize slow crosslinking under a high-temperature condition, meets the requirements of profile control of a high-temperature and high-salt stratum, and has good field application value.
Description
The technical field is as follows:
the invention relates to a slowly-crosslinked temperature-resistant salt type high-strength gel, a preparation method and application thereof, and belongs to the technical field of oilfield chemistry.
Background art:
oil well water production is a common problem in the development process of water flooding oil fields. Due to the original and the later heterogeneity of the stratum, the difference of the fluid fluidity and other reasons, a water flow dominant channel is formed in the stratum, so that water coning, water channeling and water fingering are caused, and some oil wells are subjected to early water breakthrough or flooding, and water flooding is inefficient or ineffective in circulation. The profile control and water shutoff technology is always an effective means for improving the water injection development effect and realizing stable production of oil reservoirs in oil fields. However, with the development of oil fields, the characteristics and environment of oil reservoirs are constantly changed, particularly after the oil reservoirs enter a high-water-cut exploitation period, long-term water drive makes the contradiction of oil reservoir development more complex, and the existing profile control and water shutoff technology, particularly the technology capable of being effectively applied, always lags behind the requirements of oil field development. Aiming at a plurality of high-temperature and high-salinity deep well oil reservoirs in China at present, the jelly widely applied at present is polyacrylamide jelly, for example: CN106590560A discloses a jelly temporary plugging agent, which comprises the following components in percentage by mass: 0.3-0.4% of partially hydrolyzed polyacrylamide, 0.03-0.08% of phenolic crosslinking agent, 0.03-0.08% of aldehyde crosslinking agent, 0.05-0.20% of water-soluble polyvinyl alcohol, 0.05-0.50% of hydrochloric acid or acetic acid, 0.2-0.5% of antioxidant and the balance of water, wherein the sum of the mass percentages of the components is 100%, and the phenolic crosslinking agent is one or the combination of resorcinol and hydroquinone; the aldehyde crosslinking agent is urotropin; the antioxidant is one or the combination of diphenylamine, p-phenylenediamine and sodium fluoborate. However, polyacrylamide gel is susceptible to hydrolysis at high temperature and is subject to Ca2+、Mg2+The weakness of hardening is not suitable. The investigation finds that the polyvinyl alcohol is a nonionic polymer which has good water solubility and no hydrolysis problem at high temperature, the molecular chain of the polyvinyl alcohol has a plurality of active hydroxyl groups, and the polyvinyl alcohol can be crosslinked with a plurality of compounds to form jelly glue, is nontoxic and harmless, has good biocompatibility, can be used in large scale and has wide application prospect. For example, CN 109679604A discloses a formulation of polyvinyl alcohol jelly, in which the catalyst is hydrochloric acid with a mass fraction of 0.1% -0.25%, and the gel solution prepared by the formulation is gelled at 130 ℃The time is short, and the requirement of injecting the gel-forming liquid into a high-temperature and high-salinity stratum cannot be met. The profile control of the high-temperature and high-salt stratum usually needs to inject a certain amount of plugging agent for a long time, so that the plugging agent has long gelling time and good plugging effect. At present, the studied polyvinyl alcohol gel has a high gelling speed at high temperature, and the requirement of site construction is difficult to meet, so that the research of the high-strength temperature-resistant salt-resistant gel capable of realizing slow crosslinking is of great significance.
The invention content is as follows:
aiming at the defects of the prior art, the invention provides a slow-crosslinking high-strength gel suitable for a high-temperature high-salinity stratum, and a preparation method and application thereof.
The technical scheme of the invention is as follows:
the slow-crosslinking temperature-resistant salt-type high-strength gel comprises the following components in percentage by mass:
6-7.5% of a main agent, 0.3-0.6% of an aldehyde cross-linking agent, 0.25-0.5% of a catalyst, 2-4% of a stabilizer and the balance of water, wherein the sum of the mass percentages of the components is 100%;
the main agent is polyvinyl alcohol, and the catalyst is chlorine-containing organic substance capable of continuously hydrolyzing HCl in water or lipophilic organic sulfonic acid.
According to the invention, preferably, the stabilizer is nano SiO2And (3) granules.
According to the present invention, it is preferable that the polyvinyl alcohol has an average molecular weight of 5X 104～1×105。
According to the present invention, preferably, the aldehyde crosslinking agent is one or a combination of terephthalaldehyde and isophthalaldehyde.
According to the present invention, preferably, the chlorinated organic compound capable of continuously hydrolyzing HCl in water is one or a combination of chloroacetic acid, trichloroacetic acid and methyl chloroacetate;
the lipophilic group-containing organic sulfonic acid is one or a combination of isopropylbenzene sulfonic acid, butyl benzene sulfonic acid, naphthalene sulfonic acid and acrylamido methyl propane sulfonic Acid (AMPS).
According to the invention, preferably, the slow crosslinking temperature-resistant salt type high-strength gel comprises the following components in percentage by mass:
7% of polyvinyl alcohol, 0.4% of terephthalaldehyde crosslinking agent, 0.25% of chloroacetic acid catalyst and nano SiO24 percent of stabilizing agent and the balance of water, wherein the sum of the mass percent of the components is 100 percent.
According to the invention, the preparation method of the slow-crosslinking temperature-resistant salt type high-strength gel comprises the following steps:
(1) stirring the stabilizer in water according to the proportion to fully dissolve the stabilizer; adding aldehyde cross-linking agent and polyvinyl alcohol according to a ratio, and stirring to fully dissolve the aldehyde cross-linking agent and the polyvinyl alcohol in a water bath at 70-80 ℃;
(2) cooling the prepared solution to room temperature, adding a catalyst while stirring to prepare a glue solution;
(3) aging the gel forming liquid in a closed environment at 60-130 deg.C to obtain the jelly.
According to the invention, the aging time is preferably 1.5-22 h. The gelling time of the invention is 1.5-2 h at 130 ℃, 1.5-4 h at 110 ℃, 3-8 h at 90 ℃ and 8-22 h at 60 ℃. Namely: the invention has flexible and controllable gel forming time, utilizes the catalytic reaction of organic sulfonic acid which is prepared by continuously hydrolyzing HCl in water or has proper lipophilic group to carry out, and simultaneously slows down the reaction and realizes the effect of slow crosslinking.
According to the invention, the slow-crosslinking temperature-resistant salt type high-strength gel is used as a plugging agent for profile control of an oil field.
The invention has the beneficial effects that:
1. the invention relates to a temperature-resistant and salt-resistant high-strength polyvinyl alcohol gel, which is formed into a three-dimensional network structure by cross-linking polyvinyl alcohol and an aldehyde cross-linking agent through an acetal reaction. The polyvinyl alcohol is a non-ionic polymer, has good water solubility, does not have hydrolysis problem under high temperature condition, and the jelly meets Ca2+、Mg2+No hardening, excellent temperature resistance and salt tolerance.
2. The catalyst used in the invention is chloroacetic acid or trichloroacetic acidAnd organic chlorine-containing substances such as methyl chloroacetate, and one or a combination of organic sulfonic acids such as isopropylbenzene sulfonic acid, butyl benzene sulfonic acid, naphthalene sulfonic acid, and acrylamido methyl propane sulfonic Acid (AMPS). The organic chlorine-containing substance can be utilized to continuously hydrolyze out HCl in water so as to continuously provide H for reaction+Thereby continuously catalyzing the reaction and achieving the effect of slow crosslinking; organic sulfonic acids such as cumene sulfonic acid, butyl benzene sulfonic acid, naphthalene sulfonic acid, acrylamido methyl propane sulfonic Acid (AMPS) are less acidic than p-toluene sulfonic acid because they contain relatively long lipophilic groups. The catalysts are selected to control the crosslinking speed of the polyvinyl alcohol, the gelling time is 1.5-22 h, and the gelling strength can reach 0.0091 MPa.
3. The jelly glue can realize slow crosslinking under the high temperature condition, meets the requirement of high temperature and high salt formation profile control, and has the mineralization degree of 22 multiplied by 10 at the temperature of 130 DEG C4The gel provided by the invention has the advantages of less dehydration and high strength after being evaluated for about 90 days under the condition of mg/L, which shows that the gel has excellent temperature resistance and salt tolerance and excellent plugging performance.
The specific implementation mode is as follows:
for a more clear understanding of the present invention, specific embodiments thereof are now described in detail, without limiting the scope of the invention thereto.
The polyvinyl alcohols used in the examples had an average molecular weight of 5X 104～1×105。
The catalyst used in the comparative example was 5% hydrochloric acid, 5% sulfuric acid, and was a strong acid aqueous solution.
The room temperature ranges from 20 to 28 ℃ as described in the examples and comparative examples.
Example 1:
88.35g of tap water was added with 4g of SiO2The granules and 7g of polyvinyl alcohol were stirred well to dissolve them sufficiently, and then 0.4g of a crosslinking agent was added. The prepared solution is placed in a water bath at 75 ℃ and fully stirred for two hours, so that the cross-linking agent is fully dissolved in the solution. After the solution was cooled to room temperature, 0.25g of the catalyst was added with stirring, and stirred uniformly. In this example, the crosslinking agent is terephthalaldehyde, and the catalyst is chloroacetic acid.
Placing the obtained gel-forming liquid in ampoule bottle sealed canister, and placing at 60 deg.C, 90 deg.C, 110 deg.C and 130 deg.C respectively for 14h, 5h, 2.5h and 1.5 h. The strength of the formed jelly is 0.0091MPa at 130 ℃.
Example 2:
89.85g of tap water was added with 2.5g of SiO2The granules and 7g of polyvinyl alcohol were stirred well to dissolve them sufficiently, and then 0.4g of a crosslinking agent was added. The prepared solution is placed in a water bath at 75 ℃ and fully stirred for two hours, so that the cross-linking agent is fully dissolved in the solution. After the solution was cooled to room temperature, 0.15g of the catalyst was added with stirring, and stirred uniformly. In this embodiment, the crosslinking agent is terephthalaldehyde, and the catalyst is trichloroacetic acid.
Placing the obtained gel-forming liquid in ampoule bottle sealed canister, and placing at 60 deg.C, 90 deg.C, 110 deg.C and 130 deg.C respectively for 16h, 5.5h, 2.5h and 1.5 h. The strength of the jelly formed at 130 ℃ was 0.0078 MPa.
Example 3:
to 88.5g of tap water was added 4g of SiO2The granules and 7g of polyvinyl alcohol were stirred well to dissolve them sufficiently, and then 0.25g of a crosslinking agent was added. The prepared solution is placed in a water bath at 75 ℃ and fully stirred for two hours, so that the cross-linking agent is fully dissolved in the solution. After the solution was cooled to room temperature, 0.3g of the catalyst was added with stirring, and stirred uniformly. In this embodiment, the crosslinking agent is terephthalaldehyde, and the catalyst is cumene sulfonic acid.
Placing the obtained gel-forming liquid in ampoule bottle sealed canister, and placing at 60 deg.C, 90 deg.C, 110 deg.C and 130 deg.C respectively for 17h, 6.5h, 3.5h and 2 h. The strength of the formed jelly is 0.0067MPa at 130 ℃.
Example 4:
to 88.4g of tap water was added 4g of SiO2The granules and 7g of polyvinyl alcohol were stirred well to dissolve them sufficiently, and then 0.4g of a crosslinking agent was added. The prepared solution is placed in a water bath at 75 ℃ and fully stirred for two hours, so that the cross-linking agent is fully dissolved in the solution. Cooling the solution toAfter the reaction mixture was cooled to room temperature, 0.3g of the catalyst was added thereto under stirring, and the mixture was stirred uniformly. In this embodiment, the crosslinking agent is terephthalaldehyde, and the catalyst is naphthalene sulfonic acid.
Placing the obtained gel-forming liquid in ampoule bottle sealed canister, and placing at 60 deg.C, 90 deg.C, 110 deg.C and 130 deg.C respectively for 22h, 8h, 4h and 2 h. The strength of the jelly formed at 130 ℃ was 0.0079 MPa.
Example 5:
to 88.2g of tap water was added 4g of SiO2The granules and 7g of polyvinyl alcohol were stirred well to dissolve them sufficiently, and then 0.4g of a crosslinking agent was added. The prepared solution is placed in a water bath at 75 ℃ and fully stirred for two hours, so that the cross-linking agent is fully dissolved in the solution. After the solution was cooled to room temperature, 0.35g of the catalyst was added with stirring, and stirred uniformly. In this embodiment, the crosslinking agent is terephthalaldehyde, and the catalyst is acrylamidomethylpropanesulfonic acid.
Placing the obtained gel-forming liquid in ampoule bottle sealed canister, and placing at 60 deg.C, 90 deg.C, 110 deg.C and 130 deg.C respectively for 8h, 3.5h, 1.5h and 0.66 h. The strength of the formed jelly is 0.0081MPa at 130 ℃.
Comparative example 1:
to 83.6g of tap water was added 4g of SiO2The granules and 7g of polyvinyl alcohol were stirred well to dissolve them sufficiently, and then 0.4g of a crosslinking agent was added. The prepared solution is placed in a water bath at 75 ℃ and fully stirred for two hours, so that the cross-linking agent is fully dissolved in the solution. After cooling the solution to room temperature, 5g of 5% hydrochloric acid solution was added as a catalyst with stirring, and the mixture was stirred uniformly. Placing the obtained gel forming liquid in ampoule bottle (special sealed jar), and placing at 60 deg.C, 90 deg.C, 110 deg.C and 130 deg.C respectively for 0.5h, 0.25h, 0.2h and 10 min. The strength of the jelly formed at 130 ℃ was 0.0059 MPa.
Comparative example 2:
to 83.6g of tap water was added 4g of SiO2The granules and 7g of polyvinyl alcohol were stirred well to dissolve them sufficiently, and then 0.4g of a crosslinking agent was added. Placing the prepared solution in 75 deg.C water bath and fillingStirring was carried out for two hours to dissolve the crosslinking agent sufficiently in the solution. After the solution was cooled to room temperature, 5g of 5% sulfuric acid solution was added as a catalyst with stirring, and the mixture was stirred uniformly. Placing the obtained gel forming liquid in ampoule bottle (special sealed jar), and placing at 60 deg.C, 90 deg.C, 110 deg.C and 130 deg.C respectively for 0.5h, 0.2h, 10min and 8 min. The strength of the jelly formed at 130 ℃ was 0.0054 MPa.
Test example 1 examination of temperature resistance and salt tolerance
The jelly obtained in examples 1 to 5 was used as a subject of experimental study, and the high temperature and salt resistance of the jelly of the present invention was examined.
The specific experimental process is as follows:
in the process of making jelly, 20g of jelly is injected into an ampoule bottle, the ampoule bottle is placed in an environment of 130 ℃ for 1.5 hours to be gelatinized, and then the jelly is taken out, so that cylindrical jelly blocks with the height of about 10cm and the diameter of 1cm are prepared, the cylindrical jelly blocks are divided into five groups with the serial numbers of 1#, 2#, 3#, 4#, and 5#, the five groups of jelly are soaked in a high-temperature tank, and the mineralization degree of the jelly is 22 multiplied by 104In saline (Cl)/ml-137529.5mg/L；HCO3 -183.6mg/L；Ca2+11272.5mg/L；Mg2+1518.8mg/L；Na++K+73298.4mg/L), placing the high-temperature tank in an oven at 130 ℃, respectively placing for 10 days, 20 days and 30 days, quickly taking out, and wiping the surface of the test article with filter paper. Weighing the mass of five groups of test articles respectively, comparing the mass with the mass before placing, and calculating the dehydration rate of the test articles; and secondly, respectively measuring the elastic modulus of the five groups of test articles, and observing the strength change of the test articles in a high-temperature and high-salt environment. The results are shown in Table 1.
Table 1 evaluation results table
The above experimental results show that: the gel provided by the invention can be gelled for a long time at a high temperatureAnd the injection requirement to the deep stratum on site can be met. The gel provided by the invention has the mineralization degree of 22 multiplied by 10 at the temperature of 130 DEG C4The jelly glue is less dehydrated and high in strength after being evaluated for about 90 days under the condition of mg/L, and the excellent temperature resistance and salt tolerance of the jelly glue are proved. As can be seen from the comparative example, the use of a strong acid (without hydrolysis to decompose H)+Process), the reaction speed is too fast, the requirement of on-site use on injection time is not met, and the stability of the prepared jelly in a high-temperature and high-salt environment is not good in the experimental example.
Test example 2 examination of plugging ability
The gels obtained in examples 1 to 5 were used as the subjects of investigation to examine the plugging ability of the gels provided by the present invention.
The specific experimental process is as follows:
filling quartz sand into five sand filling pipes with the inner diameter of 2.5cm and the length of 20cm to obtain simulated cores which are respectively marked as 1#, 2#, 3#, 4# and 5#, and driving water until the pressure is stable to obtain the original permeability k1Then, the gelling liquids in examples 1 to 5 were reversely injected into the six sand-packed pipes respectively, the injection volume was 0.25PV (core pore volume), then 0.25PV water was injected for replacement, then five sand-packed pipes were placed in an oven at 130 ℃ for aging for 30 days and 90 days, finally water was driven until the pressure was stable, and the post-plugging permeability k of the simulated core was measured2And according to the formula E ═ k1-k2)/k1And calculating the core plugging rate E by 100 percent, wherein the experimental result is shown in the following table 2.
TABLE 2
The above experimental results show that: the jelly provided by the invention has excellent plugging performance at a high temperature of 130 ℃.
Claims (10)
1. The slow-crosslinking temperature-resistant salt-type high-strength jelly is characterized by comprising the following components in percentage by mass:
6-7.5% of a main agent, 0.3-0.6% of an aldehyde cross-linking agent, 0.25-0.5% of a catalyst, 2-4% of a stabilizer and the balance of water, wherein the sum of the mass percentages of the components is 100%;
the main agent is polyvinyl alcohol, and the catalyst is chlorine-containing organic substance capable of continuously hydrolyzing HCl in water or lipophilic organic sulfonic acid.
2. The slow-crosslinking temperature-resistant salt-type high-strength jelly as claimed in claim 1, wherein the stabilizer is nano-SiO2And (3) granules.
3. The slow crosslinking temperature-resistant salt-resistant high-strength jelly as claimed in claim 1, wherein the polyvinyl alcohol has an average molecular weight of 5X 104～1×105。
4. The slow-crosslinking temperature-resistant salt-type high-strength jelly as claimed in claim 1, wherein the aldehyde crosslinking agent is one or a combination of terephthalaldehyde and isophthalaldehyde.
5. The slow-crosslinking temperature-resistant salt-type high-strength jelly as claimed in claim 1, wherein the chlorinated organic compound capable of hydrolyzing HCl in water continuously is one or a combination of chloroacetic acid, trichloroacetic acid and methyl chloroacetate.
6. The slow-crosslinking temperature-resistant salt-type high-strength jelly as claimed in claim 1, wherein the lipophilic organic sulfonic acid is one or a combination of cumene sulfonic acid, butyl benzene sulfonic acid, naphthalene sulfonic acid and acrylamido methyl propane sulfonic acid.
7. The slow-crosslinking temperature-resistant salt type high-strength jelly as claimed in claim 1, which comprises the following components in percentage by mass:
polyvinyl alcohol 7%, p-phenylenediFormaldehyde crosslinking agent 0.4%, chloroacetic acid catalyst 0.25%, nano SiO24 percent of stabilizing agent and the balance of water, wherein the sum of the mass percent of the components is 100 percent.
8. The preparation method of the slow-crosslinking temperature-resistant salt type high-strength jelly of claim 1, which comprises the following steps:
(1) stirring the stabilizer in water according to the proportion to fully dissolve the stabilizer; adding aldehyde cross-linking agent and polyvinyl alcohol according to a ratio, and stirring to fully dissolve the aldehyde cross-linking agent and the polyvinyl alcohol in a water bath at 70-80 ℃;
(2) cooling the prepared solution to room temperature, adding a catalyst while stirring to prepare a glue solution;
(3) aging the gel forming liquid in a closed environment at 60-130 deg.C to obtain the jelly.
9. The preparation method of the slow-crosslinking temperature-resistant salt type high-strength jelly according to claim 8, wherein the aging time is 1.5-22 h.
10. The slow-crosslinking temperature-resistant salt-type high-strength gel of claim 1, which is used as a plugging agent for profile control of oil fields.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114085657A (en) * | 2021-12-06 | 2022-02-25 | 中石化石油工程技术服务有限公司 | Temporary plugging material for shale gas well and preparation method thereof |
| CN115838589A (en) * | 2022-12-16 | 2023-03-24 | 中国石油大学(华东) | High-strength particle temporary plugging agent for fracturing diversion and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114085657A (en) * | 2021-12-06 | 2022-02-25 | 中石化石油工程技术服务有限公司 | Temporary plugging material for shale gas well and preparation method thereof |
| CN114085657B (en) * | 2021-12-06 | 2023-01-31 | 中石化石油工程技术服务有限公司 | Temporary plugging material for shale gas well and preparation method thereof |
| CN115838589A (en) * | 2022-12-16 | 2023-03-24 | 中国石油大学(华东) | High-strength particle temporary plugging agent for fracturing diversion and preparation method and application thereof |
| CN115838589B (en) * | 2022-12-16 | 2024-04-19 | 中国石油大学(华东) | High-strength particle temporary plugging agent for fracturing diversion and preparation method and application thereof |
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| CN111808585B (en) | 2022-12-27 |
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