CN105399907B - Oil-containing sludge gel particle profile control agent and preparation method thereof - Google Patents
Oil-containing sludge gel particle profile control agent and preparation method thereof Download PDFInfo
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- CN105399907B CN105399907B CN201510850229.9A CN201510850229A CN105399907B CN 105399907 B CN105399907 B CN 105399907B CN 201510850229 A CN201510850229 A CN 201510850229A CN 105399907 B CN105399907 B CN 105399907B
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Abstract
The invention relates to an oil-containing sludge gel particle profile control agent and a preparation method thereof, belonging to the technical field of profile control and water shutoff of oil fields. The oil-containing sludge gel particle profile control agent is prepared by mixing plant straws, oil-containing sludge slurry, a polymerization monomer, an initiator, a cross-linking agent and water. The method comprises the steps of adding specially treated plant straws into oil-containing sludge slurry to prepare an oil-containing sludge profile control agent core wrapped with the plant straws, filling the core into chemically synthesized gel to form a plant straw reinforced gel particle profile control agent, and adjusting the density and the strength of the profile control agent by adjusting the adding proportion of the plant straws, so that the profile control agent can be ensured to have higher strength while the density of the particle profile control agent is reduced, the water absorption can reach 4.8-9.5 times, the expansion time is 5-28 days, the profile control agent has good expansion capacity and delayed expansion performance, and the deep placement and the effective plugging of an oil reservoir can be realized.
Description
Technical Field
The invention relates to an oil-containing sludge gel particle profile control agent and a preparation method thereof, belonging to the technical field of profile control and water shutoff of oil fields.
Background
The oily sludge is oily solid waste generated in the processes of oil exploitation, transportation, refining and oily sewage treatment, and the yield is high. In the petrochemical industry of China, the average annual production is 80 multiplied by 104t tank bottom mud and pool bottom mud. The oily sludge contains a large amount of odorous toxic substances such as benzene series, phenols, anthracene, pyrene and the like, has complex components and great treatment difficulty, and if the oily sludge is not treated, the oily sludge not only pollutes the environment, but also causes waste of resources.
The method is a common sludge treatment method by directly utilizing oily sludge as a profile control agent, the sludge is injected into a reservoir, solid particles are utilized to block a core pore channel, so that subsequently injected water changes the seepage direction, and the wave and volume of the injected water are improved, but the particle size range of the solid particles in the sludge is narrow, the sludge cannot be used for a large pore channel or an ultra-high permeability oil reservoir, meanwhile, the oily sludge has more crude oil, low plugging strength and short validity period, and the middle and low permeability layers can be polluted in the injection process; ZL200410096430 discloses a method for preparing bulk-swelling particle profile control agent by utilizing oil production sludge, which comprises the steps of pickling oil-containing sludge with hot water to remove oil and then preparing water-swelling gel particles, wherein the oil-containing sludge is filled into a ternary polymerization system, and the prepared particle profile control agent has the characteristics of temperature resistance, salt resistance, good expansibility and good stability; the invention application with the application number of 201210426535.6 discloses a preparation method of an elastic particle profile control agent, which comprises the steps of crushing, sizing and screening oil-containing sludge to obtain slurry with the particle size of less than 200 meshes, naturally settling and dehydrating the slurry, and carrying out polymerization and crosslinking reaction on the dehydrated oil-containing sludge, a polymerization monomer, a crosslinking agent and the like to obtain the elastic particle profile control agent of the oil-containing sludge. The oily sludge adopted in the preparation method has high density, so that the obtained oily sludge elastic particle profile control agent has higher density (1.3-1.6 g/cm)3) The problem of poor suspension in injected water caused by higher density of the profile control agent exists in the injection construction process of the on-site profile control agentThe problem is that the profile control agent is easy to deposit at the bottom of a construction well, blocks a near well zone and cannot be constructed continuously, and if the content of oily sludge in the profile control agent is reduced, the content of rigid substances in the prepared profile control agent is reduced, so that the strength of the prepared granular profile control agent is reduced, the capability of blocking a large pore channel of a stratum is reduced, and the effective period of profile control is shortened.
Disclosure of Invention
The invention aims to overcome the defect of poor suspension property of the conventional oily sludge gel particle profile control agent, and plant straws with lower density are filled into the sludge gel particles, so that the plant straw reinforced oily sludge gel particle profile control agent with adjustable density and strength is provided.
The invention also aims to provide a preparation method of the oily sludge gel particle profile control agent.
The invention is realized by the following technical scheme:
the oily sludge gel particle profile control agent is formed by mixing plant straws, oily sludge slurry, a polymerization monomer, an initiator, a cross-linking agent and water, wherein the mass concentrations of the components are respectively as follows: 5 to 10 percent of plant straw, 15 to 30 percent of oil-containing sludge slurry, 15 to 32 percent of polymerized monomer, 0.03 to 0.15 percent of initiator, 0.08 to 0.15 percent of cross-linking agent and the balance of water.
The plant straw is one or two of corn straw, rice straw and wheat straw.
The polymerized monomer is one or two of acrylamide, acrylic acid and methacrylic acid.
The initiator is one or two of potassium persulfate, ammonium persulfate and sodium bisulfite.
The cross-linking agent is one or two of N-methylol acrylamide and N, N' -methylene bisacrylamide.
A preparation method of an oily sludge gel particle profile control agent comprises the following steps:
(1) crushing plant straws physically and mechanically, and shearing the crushed plant straws into 5-10 mm;
(2) soaking the plant straws in the step (1) in the colloid treatment solution for 24-60h, rinsing the plant straws to be neutral by using clear water, and drying the plant straws in a drying oven;
(3) soaking the plant straws treated in the step (2) with the wettability improving solution for 4-6h, and then placing the plant straws in an oven for drying;
(4) adding the plant straws treated in the step (3) into the oily sludge slurry, and uniformly mixing and stirring to obtain the oily sludge wrapping the plant straws, wherein the mass ratio of the plant straws to the oily sludge slurry is 1:6-2: 3;
(5) according to the mass ratio, 20-40% of oily sludge wrapping plant straws, 15-32% of polymerized monomers, 0.03-0.15% of initiators, 0.08-0.15% of cross-linking agents and water are fully mixed, the pH value of the mixture is adjusted to be 5.0-7.0, and then the mixture is controlled to carry out cross-linking polymerization reaction at 15-55 ℃ to generate the oily sludge gel profile control agent.
The plant straw is one or two of corn straw, rice straw and wheat straw.
The polymerized monomer is one or two of acrylamide, acrylic acid and methacrylic acid.
The colloid treatment liquid is NaOH solution with the mass fraction of 3% -6% or acetic acid solution with the mass fraction of 3% -6%.
The wettability improving liquid is prepared from a silane coupling agent and ethanol according to the volume ratio of 1:2-1: 6.
The silane coupling agent is aminopropyl triethoxysilane or aniline methyl triethoxysilane.
The invention has the beneficial effects that: the method comprises the steps of adding specially treated plant straws into oil-containing sludge slurry to prepare an oil-containing sludge profile control agent core wrapped with the plant straws, filling the core into chemically synthesized gel to form a plant straw reinforced gel particle profile control agent, and adjusting the density and the strength of the profile control agent by adjusting the adding proportion of the plant straws, so that the profile control agent can be ensured to have higher strength while the density of the particle profile control agent is reduced, the water absorption can reach 4.8-9.5 times, the expansion time is 5-28 days, the profile control agent has good expansion capacity and delayed expansion performance, and the deep placement and the effective plugging of an oil reservoir can be realized.
Drawings
FIG. 1 is a graph showing the evaluation of the properties of example 1 of the present invention;
FIG. 2 is a graph showing the evaluation of the properties in example 2 of the present invention.
Detailed Description
The technical solution of the present invention will be further described with reference to the following examples.
Example 1:
an oily sludge gel particle profile control agent is realized by the following steps:
the method comprises the following steps of (1) carrying out physical mechanical crushing on corn straws, shearing the corn straws into 6mm, soaking the corn straws in clear water, throwing away excessive water, airing the corn straws, soaking the corn straws in NaOH solution with the mass fraction of 5% for 48 hours, rinsing the corn straws to be neutral by using tap water, and drying the corn straws in an oven set to be 105 ℃; soaking the corn straws in a solution prepared from aminopropyltriethoxysilane and ethanol according to the volume ratio of 1:4 for 6 hours, taking out, drying in a drying oven set to 105 ℃, adding 10g of the treated corn straws into 25g of oil-containing sludge slurry, and uniformly mixing and stirring to obtain the oil-containing sludge wrapping the corn straws.
Adding 20g of 40% acrylamide, 0.09g of N-hydroxymethyl propionamide, 35g of oily sludge wrapping corn straws and 44.84g of pure water into a mixing container with a stirring device, adjusting the pH value to 6.5 by using a reaction regulator sodium carbonate, adding 0.07g of potassium persulfate under the stirring condition, and carrying out a cross-linking polymerization reaction on the obtained mixture at the temperature of 25 ℃ to generate the oily sludge gel particle profile control agent.
And (3) granulating and screening the oily sludge gel particle profile control agent into oily sludge gel particle profile control agents with different particle sizes.
The density of the obtained oily sludge gel particle profile control agent is measured according to a 4.2.2 density bottle method in GB/T4472-2011 determination of density and relative density of chemical products, and the maximum expansion multiple of the oily sludge gel particle profile control agent is measured according to a 4.10 expansion multiple determination method in Q/SH 10250426-2009 pre-crosslinking particle profile control agent technical condition. Soaking the screened oily sludge gel particle profile control agent in 20 multiplied by 104mg/l (wherein Ca2++Mg2+5000mg/l) mineralizationThe swelling performance test is carried out in standard saline water at the temperature of 90 ℃, the maximum swelling multiple is 9.5, and the time required for reaching the maximum swelling multiple is 4 d. According to the method for measuring the elastic modulus 6.2 in technical conditions of Q/SH 10250426-2009 pre-crosslinked particle profile control agent, the screened oil-containing sludge gel particle profile control agent is subjected to 20 x 104mg/l (wherein Ca2++Mg2+5000mg/l) of mineralization degree for 24 hours, and measuring the elastic modulus of the water-soluble polymer by an RS150 rheometer under the conditions that the frequency is 0.316Hz and the stress is (1.5-2.5) Pa to be 5800 Pa.
The evaluation of the performance of the oil-containing sludge gel particle profile control agent obtained in this example is shown in table 2 and fig. 1.
Example 2:
an oily sludge gel particle profile control agent is realized by the following steps:
the method comprises the following steps of (1) physically and mechanically crushing rice straws, shearing the rice straws into 8mm, soaking the rice straws in clear water, throwing away excessive water, airing the rice straws, soaking the rice straws in an acetic acid solution with the mass fraction of 4% for 36 hours, rinsing the rice straws to be neutral by using tap water, and drying the rice straws in an oven set to be 105 ℃; soaking the rice straws with a solution prepared from aniline methyl triethoxysilane and ethanol according to the volume ratio of 1:6 for 4h, taking out, drying in a drying oven set to 105 ℃, adding 8g of the treated rice straws into 20g of oily sludge slurry, mixing and stirring uniformly to obtain the oily sludge wrapping the rice straws.
Adding 20g of 40% acrylamide and 0.09g of N-hydroxymethyl propionamide into a mixing container with a stirring device, adding 28g of oily sludge wrapping rice straws and 51.81g of pure water, adjusting the pH value to 7 by using a reaction regulator sodium carbonate, adding 0.08g of potassium persulfate and 0.02g of sodium bisulfite under the stirring condition, and carrying out a cross-linking polymerization reaction on the obtained mixture at the temperature of 35 ℃ to generate the oily sludge gel particle profile control agent.
And (3) granulating and screening the oily sludge gel particle profile control agent into oily sludge gel particle profile control agents with different particle sizes.
The performance of the gel particle profile control agent obtained in this example was evaluated in the same manner as in example 1, and the evaluation results are shown in Table 2 and FIG. 2.
Examples 3-7 were carried out in the same manner as in the above examples, and the specific compositions are shown in Table 1.
Table 1 examples 3-7 table of reactant amounts
The density of the oily sludge gel particle profile control agent obtained in the examples 3 to 7 is measured by the same density test method as that of the example 1; the oil-containing sludge gel particle profile control agent obtained in the examples 3 to 7 is tested for swelling performance by adopting the same swelling performance test method as the example 1; the oily sludge gel particle profile control agents obtained in examples 3 to 7 were tested for their elastic modulus by the same strength measurement method as in example 1, and the results are shown in Table 2.
TABLE 2 suspension property and swelling property of oil-containing sludge gel particle profile control agent
Comparative example 1: a particle profile control system is prepared by adopting the method for preparing the bulk-swelling particle profile control agent by utilizing the oil extraction sludge disclosed by ZL200410096430, the density and the elastic modulus of the prepared particle profile control system are measured by adopting the same evaluation method as that in the example 1, and the density range is 1.345-1.552g/cm3The elastic modulus ranges from 3500 and 4800 Pa.
Comparative example 2: a pellet Profile control System was prepared by the method of preparing an elastic pellet Profile control agent disclosed in the invention application No. 201210426535.6, and the density and elastic modulus of the prepared pellet Profile control System were measured by the same evaluation methods as in example 1, with the density ranging from 1.351 to 1.610g/cm3The elastic modulus ranges from 4200-6800 Pa.
Evaluation from comparative example 1 and comparative example 2As can be seen from the results, the prepared profile control agent has a high density (> 1.345 g/cm)3) And the elastic modulus is lower (less than 4500Pa) when the density is relatively low, the suspension property of the material in injected water is poor in the profile control process, the material is easy to deposit at the bottom of a construction well to block a near well zone, and the requirement of stratum profile control construction with a large pore canal is difficult to meet.
As can be seen from the results of the evaluation of Table 2 and comparative examples 1 and 2, the density of the oil-containing sludge gel particle profile control agent prepared by the present invention (1.182 g/cm)3-1.339g/cm3) The strength (4500-6000Pa) can be regulated, the water absorption can reach 4.8-9.5 times, the expansion time is 5-28 days, and the density and the strength of the prepared oily sludge gel particle profile control agent can be controlled by controlling the addition amount of the plant straws. In the reduction of the density of the profile control agent (< 1.339 mg/cm)3) Meanwhile, the profile control agent is ensured to have higher strength (higher than 4500Pa), has better suspension property, expansion capacity and delayed expansion performance in formation water with different degrees of mineralization, and can be used for deep placement and effective plugging of an oil reservoir.
Claims (10)
1. The oil-containing sludge gel particle profile control agent is characterized in that: the oil stain-containing sludge is prepared by mixing plant straws, oil stain-containing sludge body, polymerization monomer, initiator, cross-linking agent and water, wherein the mass concentrations of the components are as follows: 5 to 10 percent of plant straw, 15 to 30 percent of oil-containing sludge slurry, 15 to 32 percent of polymerized monomer, 0.03 to 0.15 percent of initiator, 0.08 to 0.15 percent of cross-linking agent and the balance of water;
the preparation method of the oily sludge gel particle profile control agent comprises the following steps:
(1) crushing plant straws physically and mechanically, and shearing the crushed plant straws into 5-10 mm;
(2) soaking the plant straws in the step (1) in the colloid treatment solution for 24-60h, rinsing the plant straws to be neutral by using clear water, and drying the plant straws in a drying oven;
(3) soaking the plant straws treated in the step (2) with the wettability improving solution for 4-6h, and then placing the plant straws in an oven for drying;
(4) adding the plant straws treated in the step (3) into the oily sludge slurry, and uniformly mixing and stirring to obtain the oily sludge wrapping the plant straws, wherein the mass ratio of the plant straws to the oily sludge slurry is 1:6-2: 3;
(5) fully mixing 20-40% of oily sludge wrapping plant straws, 15-32% of polymerized monomers, 0.03-0.15% of initiators, 0.08-0.15% of cross-linking agents and water according to the mass ratio, and adjusting the pH value of the mixture to 5.0-7.0; then the mixture is controlled to have cross-linking polymerization reaction at the temperature of 15-55 ℃ to generate the oil-containing sludge gel particle profile control agent.
2. The oil-containing sludge gel particle profile control agent as claimed in claim 1, which is characterized in that: the plant straw is one or two of corn straw, rice straw and wheat straw.
3. The oil-containing sludge gel particle profile control agent as claimed in claim 1, which is characterized in that: the polymerized monomer is one or two of acrylamide, acrylic acid and methacrylic acid.
4. The oil-containing sludge gel particle profile control agent as claimed in claim 1, which is characterized in that: the initiator is one or two of potassium persulfate and ammonium persulfate.
5. The oil-containing sludge gel particle profile control agent as claimed in claim 1, which is characterized in that: the cross-linking agent is one or two of N-methylol acrylamide and N, N' -methylene bisacrylamide.
6. A method for preparing the oil-containing sludge gel particle profile control agent according to claim 1, comprising the following steps:
(1) crushing plant straws physically and mechanically, and shearing the crushed plant straws into 5-10 mm;
(2) soaking the plant straws in the step (1) in the colloid treatment solution for 24-60h, rinsing the plant straws to be neutral by using clear water, and drying the plant straws in a drying oven;
(3) soaking the plant straws treated in the step (2) with the wettability improving solution for 4-6h, and then placing the plant straws in an oven for drying;
(4) adding the plant straws treated in the step (3) into the oily sludge slurry, and uniformly mixing and stirring to obtain the oily sludge wrapping the plant straws, wherein the mass ratio of the plant straws to the oily sludge slurry is 1:6-2: 3;
(5) fully mixing 20-40% of oily sludge wrapping plant straws, 15-32% of polymerized monomers, 0.03-0.15% of initiators, 0.08-0.15% of cross-linking agents and water according to the mass ratio, and adjusting the pH value of the mixture to 5.0-7.0; then the mixture is controlled to have cross-linking polymerization reaction at the temperature of 15-55 ℃ to generate the oil-containing sludge gel particle profile control agent.
7. The method for preparing the oil-containing sludge gel particle profile control agent according to claim 6, which is characterized by comprising the following steps: the plant straw is one or two of corn straw, rice straw and wheat straw.
8. The method for preparing the oil-containing sludge gel particle profile control agent according to claim 6, which is characterized by comprising the following steps: the polymerized monomer is one or two of acrylamide, acrylic acid and methacrylic acid.
9. The method for preparing the oil-containing sludge gel particle profile control agent according to claim 6, which is characterized by comprising the following steps: the colloid treatment liquid is NaOH solution with the mass fraction of 3% -6% or acetic acid solution with the mass fraction of 3% -6%.
10. The method for preparing the oil-containing sludge gel particle profile control agent according to claim 6, which is characterized by comprising the following steps: the wettability improving liquid is prepared from a silane coupling agent and ethanol according to the volume ratio of 1:2-1: 6.
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| CN106753298B (en) * | 2016-12-28 | 2021-02-12 | 华鼎鸿基采油技术服务（北京）有限公司 | Cationic dispersion gel composite emulsification type profile control water plugging agent prepared by using oily sludge as base material |
| CN106800920B (en) * | 2016-12-28 | 2019-06-11 | 中国石油天然气股份有限公司 | Plugging modifier and preparation method and application thereof |
| CN110527501B (en) * | 2018-05-25 | 2022-05-10 | 中国石油天然气股份有限公司 | Salt-tolerant oil sludge profile control agent and preparation method thereof |
| CN110805408B (en) * | 2019-05-31 | 2021-08-31 | 大港油田集团有限责任公司 | Profile control process method for water injection well with packer pipe column |
| CN113493682A (en) * | 2020-04-03 | 2021-10-12 | 中国石油天然气股份有限公司 | Composite profile control agent and oil sludge composite slug profile control channeling sealing process |
| CN112625666A (en) * | 2020-12-17 | 2021-04-09 | 黑龙江佳宜宏大科技有限公司 | Oil field oil-containing sludge plugging agent and preparation method thereof |
| CN116574492A (en) * | 2023-03-31 | 2023-08-11 | 中科海创环境科技（大连）有限公司 | Gel profile control agent prepared from oily sludge and used for deep liquid flow diversion, and preparation method and application thereof |
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| CN102898562A (en) * | 2012-10-31 | 2013-01-30 | 中国石油化工股份有限公司 | Method for preparing elastic particle flooding/profiling agent |
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| CN101575966A (en) * | 2009-06-09 | 2009-11-11 | 中国石油天然气股份有限公司 | Method for underground polymerization water shutoff and profile control of oil production sludge |
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