CN116218507B - Demulsification and drainage-assisting composite additive for fracturing and acidizing and preparation method thereof - Google Patents

Demulsification and drainage-assisting composite additive for fracturing and acidizing and preparation method thereof Download PDF

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Publication number
CN116218507B
CN116218507B CN202310506816.0A CN202310506816A CN116218507B CN 116218507 B CN116218507 B CN 116218507B CN 202310506816 A CN202310506816 A CN 202310506816A CN 116218507 B CN116218507 B CN 116218507B
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drainage
demulsification
assisting
composite additive
rhamnolipid
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CN116218507A (en
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李江银
丁全福
李娟�
李美玲
李江昆
李凯琛
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Dongying Jiangyuan Chemical Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60—Compositions for stimulating production by acting on the underground formation
    • C09K8/62—Compositions for forming crevices or fractures
    • C09K8/72—Eroding chemicals, e.g. acids
    • C09K8/74—Eroding chemicals, e.g. acids combined with additives added for specific purposes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60—Compositions for stimulating production by acting on the underground formation
    • C09K8/602—Compositions for stimulating production by acting on the underground formation containing surfactants

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Heterocyclic Carbon Compounds Containing A Hetero Ring Having Nitrogen And Oxygen As The Only Ring Hetero Atoms (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

Abstract

The invention relates to the technical field of oilfield chemical reagents, in particular to a demulsification and drainage-assisting composite additive for fracturing and acidizing and a preparation method thereof. The biological surfactant is adopted to replace chemical synthetic substances, the fatty acid glyceride and the biological surfactant are scientifically compounded, and alcohol substances and ether synergists are added to promote the synergy among the surfactants, so that the system surface activity can be obviously improved, and the environmental protection safety performance of the product can be further improved. The compound additive has scientific and reasonable formula, can effectively reduce the surface tension and interface tension of a system, has excellent demulsification and drainage-assisting capabilities, and can remarkably improve the harvesting efficiency.

Description

Demulsification and drainage-assisting composite additive for fracturing and acidizing and preparation method thereof
Technical Field
The invention relates to the technical field of oilfield chemical reagents, in particular to a demulsification and drainage-assisting composite additive for fracturing and acidizing and a preparation method thereof.
Background
The fracturing acidification is a main technology for increasing the yield and the injection of the oil field, and has wide application scenes. However, the more the working fluid is injected in the fracturing and acidifying process, the larger the fluid loss is, and the larger the damage to the rock core is, so one of the methods for reducing the damage to the stratum during the mining is to reduce the fluid loss of the working fluid and accelerate the flowback of the working fluid. In various drainage-assisting measures, demulsification drainage-assisting chemical agents with excellent performance are added into the acidizing and fracturing treatment fluid, and the agents can generate extremely low surface tension, so that capillary resistance is reduced, the working fluid is thoroughly discharged back out of the stratum, the stratum is prevented from being blocked, and the method is a widely used economic and efficient method.
The traditional chemical demulsification reagent is generally a chemical synthetic substance, and the high molecular property of the chemical demulsification reagent is easy to cause the reagent to be difficult to degrade after being used, so that the environmental pollution is large. Biosurfactants are generally less or non-toxic, excellent in biodegradability, strong in demulsification and capable of emulsifying hydrocarbon and stabilizing an emulsifying system. However, compared with the conventional chemical synthesis surfactants, the biosurfactant has relatively low surface activity, and the biosurfactant alone used as a demulsification and drainage aid agent cannot effectively reduce the surface tension, so that the actual production requirements cannot be completely met.
Therefore, it is necessary to develop a demulsification and drainage-assisting agent for fracture acidizing which is excellent in demulsification and drainage-assisting performance and good in environmental protection performance.
Disclosure of Invention
The invention aims to provide a demulsification and drainage-assisting composite additive for fracturing and acidizing, which solves the problems of poor demulsification and drainage-assisting effects, serious environmental pollution and the like of the conventional additive.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the demulsification and drainage-assisting composite additive for fracturing and acidizing is characterized by comprising a biosurfactant and fatty glyceride, wherein the fatty glyceride has the following structural formula: r is R 1 OCH 2 (OR 2 )CH 2 OR 3 Wherein R is 1 、R 2 And R is 3 Each independently is R 4 CO-group or H, wherein R 4 A C9 to C18 alkyl chain that is linear or branched, saturated or unsaturated; alternatively, R 1 、R 2 And R is 3 One of them is (HOOC) n R 5 A group, wherein R is 5 Is a linear or branched, saturated or unsaturated alkyl chain of C9 to C16, n=1-4.
Wherein the mass ratio of the biological surface activity to the fatty glyceride is (4-7): 1.
Further, the biosurfactant is selected from one or more of alkyl glycoside, rhamnolipid and lecithin.
In addition to the above components, the composite additive of the present invention may further comprise alcohols, synergists, and water. The alcohol is one or more of methanol, ethanol, isopropanol, n-butanol and isobutanol; the synergistic agent is one or more of propylene glycol methyl ether, dipropylene glycol methyl ether and diethylene glycol monobutyl ether.
Preferably, the rhamnolipid comprises a rhamnolipid having an alkyl chain which is a saturated or unsaturated alkyl chain of C8-C12. Further, the rhamnolipid comprises 80wt% of a rhamnolipid or more.
Preferably, the composite additive of the present invention comprises the following components in terms of the total mass of the additive: the biological surfactant contains 20-35%, the fatty glyceride contains 4-8%, the alcohol contains 5-10%, the synergist contains 3-6%, and the rest is water.
Preferably, the composite additive of the present invention comprises the following components in terms of the total mass of the additive: 10-20% of rhamnolipid, 10-17.5% of alkyl glycoside, 5-7% of ethanol, 5-7% of isobutanol, 1-3% of propylene glycol methyl ether, 1-3% of dipropylene glycol methyl ether, 1-3% of diethylene glycol monobutyl ether and the balance of water.
The invention also provides a preparation method of the demulsification and drainage-assisting composite additive for fracturing and acidizing, which comprises the following steps: and adding the biosurfactant and the fatty glyceride into water for uniform dispersion, sequentially adding the synergist and the alcohol, and uniformly stirring to obtain the demulsification and drainage-assisting composite additive for fracture acidification.
The invention has the beneficial effects that:
the biosurfactant with higher surface activity is adopted to replace chemical synthetic substances, so that the system surface tension and interfacial tension are reduced, and the biodegradability of the product is improved; on the basis, the fatty glyceride and the biosurfactant are added for scientific compounding, so that the system surface activity is further improved, and the environmental protection and safety performances of the product are further improved. Besides the surfactant, the composite additive also contains alcohol substances and ether synergists, so that all components of the additive can be well compatible, and the synergists among the surfactants are promoted. The compound additive has scientific and reasonable formula, can effectively reduce the surface tension and interface tension of a system, has excellent demulsification and drainage assisting capability and can remarkably improve the harvesting efficiency through a performance test.
Description of the embodiments
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The invention is further described in the following detailed description.
Examples
The demulsification and drainage-assisting composite additive for fracturing and acidizing is characterized by comprising 20% of rhamnolipid, 4% of glyceryl stearyl ester, 5% of methanol, 1% of propylene glycol methyl ether, 1% of dipropylene glycol methyl ether, 1% of diethylene glycol monobutyl ether and 68% of water according to the total mass of the additive;
the preparation method comprises the following steps: adding rhamnolipid and glyceryl stearyl ester into water, dispersing uniformly, sequentially adding propylene glycol methyl ether, dipropylene glycol methyl ether, diethylene glycol monobutyl ether and methanol, and stirring uniformly to obtain the demulsification and drainage-assisting composite additive for fracture acidification.
Examples 2-8, comparative examples 1-8 additives were prepared in a similar manner to example 1, except that the additives were added in an amount and with or without the addition of a component, as shown in tables 1 and 2, respectively, in accordance with the specific materials and amounts of example 1.
TABLE 1
TABLE 2
Rhamnolipid: containing wt90% of a ditrhamnolipid, available from Sigma-Aldrich (Shanghai) trade company, inc;
alkyl glycoside: available from Shanghai Michlin Biochemical technologies Co., ltd;
lecithin: obtained from Shanghai Yi En chemical technologies limited;
sodium perfluorononenoxybenzenesulfonate: available from zheng Ai Kem chemical industry limited;
glyceryl stearyl ester: obtained from Jining Malus hupehensis chemical Co., ltd;
diglycerol monolaurate: obtained from Shanghai Bohr chemical Co., ltd;
alcohols: obtained from Shanghai Ala Biochemical technologies Co., ltd;
propylene glycol methyl ether: obtained from Dongguan city, galaxy chemical Co., ltd;
dipropylene glycol methyl ether: obtained from Xiamen Yude chemical products Co., ltd;
diethylene glycol monobutyl ether: obtained from clarinet (Shandong) Biotech Co.
The demulsification performance and the oil-water interface condition of each sample of the examples and the comparative examples are tested by referring to SY/T5280-2018 general technical Condition of crude oil demulsifier; the surface tension, interfacial tension and drainage assisting performance of each sample of the examples and the comparative examples are tested by referring to SY/T5755-2016 method for evaluating the performance of drainage assisting agent for fracture acidizing; the anti-swelling performance test was performed on each sample of examples and comparative examples with reference to SY/T5971-2016 method for evaluating the performance of clay stabilizer for fracture acidizing and Water injection of oil and gas field. The test items of the examples and the comparative examples were repeated three times, and the test data were averaged, and the results are shown in Table 3.
TABLE 3 Table 3
Surface tension/mN.m -1 Interfacial tension/mN.m -1 Dehydration rate/% Rate of drainage aid/% Expansion resistance/% Interface condition
Example 1 17.35 0.41 93.1 95.4 69.2 Clear and level interface
Example 2 17.04 0.39 93.3 95.5 69.1 Clear and level interface
Example 3 17.01 0.38 93.4 95.7 69.2 Clear and level interface
Example 4 16.92 0.35 93.7 95.8 69.2 Clear and level interface
Example 5 16.13 0.30 94.2 96.3 69.5 Clear and level interface
Example 6 16.17 0.31 94.3 96.2 69.5 Clear and level interface
Example 7 16.08 0.29 94.5 96.3 69.6 Clear and level interface
Example 8 16.18 0.31 85.8 96.1 69.4 Clear and level interface
Comparative example 1 19.25 0.53 85.2 87.7 61.2 Clear and level interface
Comparative example 2 25.76 0.71 79.1 80.5 56.4 Clear and level interface
Comparative example 3 24.19 0.67 79.3 80.6 56.9 Clear and level interface
Comparative example 4 27.82 0.75 77.9 78.9 53.0 Clear and level interface
Comparative example 5 18.94 0.50 86.8 88.0 61.5 Clear and level interface
Comparative example 6 26.33 0.72 77.5 78.3 53.7 Clear and level interface
Comparative example 7 28.61 0.79 76.0 76.7 51.8 Clear and level interface
Comparative example 8 19.75 0.54 85.6 87.8 61.2 Clear and level interface
The invention mixes the biological surfactant with the specific surfactant fatty glyceride for use, improves the system surface activity through alcohol substances, and adds the synergistic agent to improve the component compatibility, so that the finally prepared composite additive has the characteristics of low surface tension and low interfacial tension, and meanwhile, the demulsification and drainage assisting performance is excellent.
Table 3 test results show that the surface tension of the composite additives of examples 1 to 8 of the present invention is 16 to 17.5 mN.m -1 The interfacial tension is basically 0.29-0.4 mN.m -1 Within the range, the surface tension of the demulsification and drainage aiding agent which is commonly used in the industry and has better performance is 20 mN.m -1 About, the interfacial tension was 0.6 mN.m -1 About, it can be seen that the composite additive of the present invention has significant advantages in terms of surface activity.
Compared with example 5, the comparison example 1 uses fluorine-containing surfactant sodium perfluorononenoxybenzenesulfonate to replace biological surfactant rhamnolipid and alkyl glycoside, the comparison example 2 uses sodium perfluorononenoxybenzenesulfonate to replace alkyl glycoside, the comparison example 3 uses sodium perfluorononenoxybenzenesulfonate to replace rhamnolipid, the comparison example 4 omits rhamnolipid and alkyl glycoside, equal mass lecithin and sodium perfluorononenoxybenzenesulfonate are added, the comparison example 5 uses sodium perfluorononenoxybenzenesulfonate to replace fatty glyceride glyceryl octadecanoate and diglycerol mono-month silicate, and the comparison examples 1-5 have relatively low surface tension, interfacial tension, dehydration rate, drainage rate and anti-swelling rate. Generally speaking, the fluorine-containing surfactant has very high surface activity, however, the fluorine-containing surfactant cannot be well compatible with the surfactant of the invention, and the surfactant cannot be used for remarkably improving the surface activity of the system because ideal surface tension and interfacial tension cannot be obtained by compounding the fluorine-containing surfactant with the surfactant or the fatty glyceride, and a chemical system with complex interaction can be constructed probably due to the compounding of the surfactant. Comparative example 1 contains a greater amount of sodium perfluorononenoxybenzenesulfonate, and although the surface activity is somewhat reduced as compared with example 5, the high surface activity of sodium perfluorononenoxybenzenesulfonate itself still allows the properties of comparative example 1, such as surface tension, to be at a better level; comparative examples 2-4 contained half of the sodium perfluorononenoxybenzenesulfonate of comparative example 1, and the results of the surface tension and the like were significantly worse; comparative example 5 contained less sodium perfluorononenoxybenzenesulfonate and the test results were worst in comparative examples 1-5. Compared with the example 5 without the synergist, the comparative example 6 has slightly worse test performance than the example 5, but slightly better test performance than the comparative example 1, the construction of the surfactant system of the invention is more reasonable from the side, and the surfactant with higher surface activity than that of the surfactant containing fluorine is obtained by compounding the biosurfactant and the fatty glyceride, so that the composite additive has better overall performance. The comparative example 7 only uses the fluorine-containing surfactant with high surface activity and has larger dosage, however, the test result of the comparative example 7 is quite unsatisfactory, and each performance is almost the worst in all comparative examples, which can indicate that the demulsification and drainage-assisting additive is not simply added with the high surface active substance, and the compatibility among the components needs to be fully considered, so that antagonism among the components is avoided, and the final performance of the additive is influenced. The absence of alcohol in comparative example 8 is probably due to the fact that the surfactant micelles are more easily formed and help to build a higher surface activity chemical system than in example 5, and thus the performance of each test in comparative example 8 without alcohol is slightly reduced.
Further, to verify the performance of the composite additive of the present invention, comparative examples 9 to 11 explored the effect of fluorosurfactant and surfactant dosage on the system of the present invention, and the composition of the components and the results of the performance test are shown in Table 4.
TABLE 4 Table 4
Comparative examples 9 to 11 were further charged with sodium perfluorononenoxybenzenesulfonate and gradually increased in the amount thereof as compared with example 5. As can be seen from the results in Table 4, after the sodium perfluorononenoxybenzenesulfonate is added, the surface tension and other properties of comparative example 9 are basically at the same level as those of certain examples of the present invention, but the surface tension and other properties of comparative example 5 are reduced to a certain extent compared with those of example 5, which shows that the addition of the high-surface-activity fluorine-containing surfactant can not continue to improve the properties of the composite additive of the present invention, and the use amount of the fluorine-containing surfactant is further improved in comparative examples 9-10, so that the properties of the additive are obviously reduced, probably because the fluorine-containing surfactant is not well compatible with the additive system of the present invention, and the use amount of the fluorine-containing surfactant is increased to enhance the antagonism, so that the properties of the additive are deteriorated. In addition, although the fluorine-containing surfactant has the characteristic of high activity, the fluorine-containing surfactant has the defects of high price, relatively difficult degradation and the like, and is difficult to meet the application requirements of green and environment-friendly production.
As can be seen from comparative examples 12-13, the ratio of biosurfactant to fatty glyceride used is different, although the same as in example 5, and the properties of the final composite additive are not ideal.
The above embodiments are preferred embodiments of the present invention, and besides, the present invention may be implemented in other ways, and any obvious substitution is within the scope of the present invention without departing from the concept of the present invention.

Claims (6)

1. A demulsification and drainage-assisting composite additive for fracture acidizing, which is characterized by comprising the following components in percentage by mass: the biological surfactant contains 20-45%, the fatty glyceride contains 4-10%, the alcohol contains 5-10%, the synergist contains 3-6%, and the rest is water; the fatty acid glyceride has the following structural formula: r is R 1 OCH 2 (OR 2 )CH 2 OR 3 Wherein R is 1 、R 2 And R is 3 Each independently is R 4 CO-group or H, wherein R 4 A C9 to C18 alkyl chain that is linear or branched, saturated; alternatively, R 1 、R 2 And R is 3 One of them is (HOOC) n R 5 A group, wherein R is 5 Is a linear or branched, saturated alkyl chain of C9 to C16, n=1-4; wherein the mass ratio of the biosurfactant to the fatty glyceride is (4-7): 1; the biosurfactant is selected from one or more of alkyl glycoside, rhamnolipid and lecithin; the synergistic agent is one or more of propylene glycol methyl ether, dipropylene glycol methyl ether and diethylene glycol monobutyl ether.
2. The demulsification and drainage-aiding composite additive for fracture acidizing according to claim 1, wherein the alcohol is one or more of methanol, ethanol, isopropanol, n-butanol and isobutanol.
3. The demulsification and drainage-aiding composite additive for fracture acidizing according to claim 1, wherein the rhamnolipid comprises a rhamnolipid with a saturated alkyl chain of C8-C12.
4. The demulsification and drainage-aiding composite additive for fracture acidizing according to claim 3, wherein the rhamnolipid comprises 80wt% or more of the rhamnolipid.
5. The demulsification and drainage-assisting composite additive for fracture acidizing according to any one of claims 1 to 4, wherein the additive comprises 10 to 20% of rhamnolipid, 10 to 20% of alkyl glycoside, 5 to 7% of ethanol, 5 to 7% of isobutanol, 1 to 3% of propylene glycol methyl ether, 1 to 3% of dipropylene glycol methyl ether, 1 to 3% of diethylene glycol monobutyl ether and the balance of water by total mass of the additive.
6. The method for preparing the demulsification and drainage-assisting composite additive for fracturing acidification according to any one of claims 1 to 4, comprising the following steps: and adding the biosurfactant and the fatty glyceride into water for uniform dispersion, sequentially adding the synergist and the alcohol, and uniformly stirring to obtain the demulsification and drainage-assisting composite additive for fracture acidification.
CN202310506816.0A 2023-05-08 2023-05-08 Demulsification and drainage-assisting composite additive for fracturing and acidizing and preparation method thereof Active CN116218507B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102618250A (en) * 2012-03-02 2012-08-01 陕西延长石油(集团)有限责任公司研究院 Preparation method of environmental-friendly demulsify-cleanup additive for fracture acidizing
CN105062452A (en) * 2015-07-15 2015-11-18 国勘石油技术有限公司 Demulsification and discharge aiding agent and preparation method thereof as well as treatment method of oil field reservoir
CN105295888A (en) * 2015-09-29 2016-02-03 中国石油天然气股份有限公司 Cleanup additive for fracture acidizing, and manufacturing method and using method thereof
CN107120103A (en) * 2017-05-17 2017-09-01 成都百联油田技术服务有限公司 A kind of fracture acidizing cleanup additive
CN112480899A (en) * 2020-12-11 2021-03-12 德仕能源科技集团股份有限公司 Demulsification cleanup additive for fracturing and preparation method thereof
CN112724949A (en) * 2019-10-14 2021-04-30 中国石油天然气股份有限公司 Lactic acidlike blocking remover for blocking removal of thick oil well and application thereof
CN115785940A (en) * 2022-12-01 2023-03-14 克拉玛依中科恒信科技有限责任公司 Demulsification cleanup additive for fracture acidizing and preparation method and use method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102618250A (en) * 2012-03-02 2012-08-01 陕西延长石油(集团)有限责任公司研究院 Preparation method of environmental-friendly demulsify-cleanup additive for fracture acidizing
CN105062452A (en) * 2015-07-15 2015-11-18 国勘石油技术有限公司 Demulsification and discharge aiding agent and preparation method thereof as well as treatment method of oil field reservoir
CN105295888A (en) * 2015-09-29 2016-02-03 中国石油天然气股份有限公司 Cleanup additive for fracture acidizing, and manufacturing method and using method thereof
CN107120103A (en) * 2017-05-17 2017-09-01 成都百联油田技术服务有限公司 A kind of fracture acidizing cleanup additive
CN112724949A (en) * 2019-10-14 2021-04-30 中国石油天然气股份有限公司 Lactic acidlike blocking remover for blocking removal of thick oil well and application thereof
CN112480899A (en) * 2020-12-11 2021-03-12 德仕能源科技集团股份有限公司 Demulsification cleanup additive for fracturing and preparation method thereof
CN115785940A (en) * 2022-12-01 2023-03-14 克拉玛依中科恒信科技有限责任公司 Demulsification cleanup additive for fracture acidizing and preparation method and use method thereof

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