CN112299674B - Biodegradable microemulsion cleaning agent and preparation method and application thereof - Google Patents
Biodegradable microemulsion cleaning agent and preparation method and application thereof Download PDFInfo
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- 239000012459 cleaning agent Substances 0.000 title claims abstract description 111
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003921 oil Substances 0.000 claims abstract description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000004094 surface-active agent Substances 0.000 claims abstract description 33
- 239000010779 crude oil Substances 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 25
- 238000009826 distribution Methods 0.000 claims abstract description 21
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 21
- 235000019387 fatty acid methyl ester Nutrition 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004064 cosurfactant Substances 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 103
- 238000003756 stirring Methods 0.000 claims description 82
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 40
- 239000012752 auxiliary agent Substances 0.000 claims description 39
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical group CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 24
- 239000012530 fluid Substances 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 22
- 239000011780 sodium chloride Substances 0.000 claims description 20
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 18
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 14
- 239000002283 diesel fuel Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 12
- 229910052708 sodium Inorganic materials 0.000 claims description 12
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003350 kerosene Substances 0.000 claims description 10
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 8
- 239000001103 potassium chloride Substances 0.000 claims description 7
- 235000011164 potassium chloride Nutrition 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 13
- 125000005843 halogen group Chemical group 0.000 claims 2
- 239000013049 sediment Substances 0.000 abstract description 31
- 239000007788 liquid Substances 0.000 abstract description 29
- 238000004140 cleaning Methods 0.000 abstract description 26
- 230000007281 self degradation Effects 0.000 abstract description 10
- 239000012071 phase Substances 0.000 description 32
- 239000000203 mixture Substances 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 11
- 238000005553 drilling Methods 0.000 description 11
- 239000002699 waste material Substances 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 239000010802 sludge Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005063 solubilization Methods 0.000 description 3
- 230000007928 solubilization Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229960001701 chloroform Drugs 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 150000004820 halides Chemical group 0.000 description 1
- 238000011086 high cleaning Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000011499 joint compound Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- HSFQBFMEWSTNOW-UHFFFAOYSA-N sodium;carbanide Chemical group [CH3-].[Na+] HSFQBFMEWSTNOW-UHFFFAOYSA-N 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000010913 used oil Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Detergent Compositions (AREA)
Abstract
The invention relates to the field of oil exploitation, and discloses a biodegradable microemulsion cleaning agent, and a preparation method and application thereof. The cleaning agent is a middle-phase microemulsion and comprises the following components based on the total weight of the cleaning agent: 5-10wt% of oil phase, 0.5-5wt% of surfactant, 5-15wt% of cosurfactant, 1-6.5wt% of inorganic salt and 63.5-89.5wt% of water; wherein the surfactant is alpha-sulfo fatty acid methyl ester salt and/or alcohol ether sulfo succinic acid monoester salt; the particle size distribution range of the cleaning agent is 15-40nm. The cleaning agent can realize the efficient cleaning of crude oil in produced liquid sediments at normal temperature, and meanwhile, the cleaning agent has good self-degradation performance and strong adaptability and is convenient for field application. The oil removal rate of the cleaning agent at normal temperature reaches more than 93%, and the self-degradation rate in 7 days reaches more than 95%.
Description
Technical Field
The invention relates to the field of oil exploitation, and in particular relates to a biodegradable microemulsion cleaning agent and a preparation method and application thereof.
Background
During the development and treatment of petroleum, a large amount of oil sludge, waste drilling fluid and other produced liquid sediments can be generated. At present, most of domestic oil fields enter a high water content exploitation stage, a large amount of produced liquid sediments in a stratum are carried to the ground by drilling fluid, and the drilling fluid is complex in composition, high in water content and relatively stable in system, belongs to a dangerous solid waste which is difficult to treat, and can seriously pollute the environment if the produced liquid sediments are not treated properly. According to incomplete statistics, the total amount of produced liquid sediment produced in our country every year is over 500 million tons. At present, water shutoff and profile control are effective technical means for harmless utilization of produced liquid sediments, however, produced liquid sediments contain a large amount of crude oil, and if the crude oil is directly reinjected, huge resource waste is caused, and if oil in the produced liquid sediments can be effectively recovered, certain environmental benefits can be generated, and huge economic benefits can be obtained.
The treatment technology of the produced liquid sediment is various, and the treatment technology is closely related to wide sources and complex compositions of the produced liquid sediment. The produced liquid sediments from different sources have great property difference, and the oil content, the water content and the structural composition of the produced liquid sediments have obvious difference. The research on the produced liquid sediment treatment technology is carried out earlier abroad, particularly in Europe and America countries such as the United states, canada, denmark, the Netherlands and the like, the treatment and resource recovery technology is mature, and the technologies mainly comprise: mechanical dehydration process, heat treatment process, biological treatment process, supercritical fluid extraction process and the like. The research on the aspect of the treatment of the produced liquid sediments in China is late, and although many foreign advanced technologies have successful application cases, due to the limitation of various conditions, the technologies cannot be comprehensively applied in China. At present, the domestic produced liquid sediment treatment technologies mainly comprise a solvent extraction method, a thermal washing method, a micro-emulsion washing method, a chemical demulsification method, a solid-liquid separation method, an immobilization treatment method, a biological treatment method and the like. Although the methods can realize pollution treatment of produced liquid sediments to a certain extent, the methods are limited by the reasons of high dosage, investment and treatment temperature, low efficiency, complex process, secondary pollution and the like, and cannot be popularized and applied in China.
Among the above methods, the microemulsion cleaning method is attracting attention. The microemulsion is used as a spontaneously formed thermodynamic stable system and has the excellent properties of ultralow interfacial tension, superstrong emulsification, solubilization, dispersion and the like. The microemulsion is adopted to remove the crude oil in the produced liquid sediment, and has the advantages of high cleaning rate, simple and convenient process and the like. However, microemulsions have many phases and not all types of microemulsions achieve good cleaning performance, and in some cases, the composition of the oil phase, inorganic salts, or produced fluid deposits in the microemulsion component may have a significant impact on cleaning performance.
CN107338118A discloses an emulsion type water-based cleaning agent for oil-containing sludge, and a preparation method and a use method thereof. The cleaning agent can realize high-efficiency cleaning of oily sludge at the temperature of 60-80 ℃, but has higher limitation on the used oil phase, when the oil phase is mixed benzene, the oil removal rate can reach 93%, but when the oil phase is diesel oil, the oil removal rate is only 43%.
CN107055990A discloses an oily sludge cleaning agent, a preparation method and application thereof. The cleaning agent can realize the separation of oil, water and mud at the temperature of 60-80 ℃, but the field application is limited because the cleaning agent needs to be heated in the using process.
In summary, the cleaning agent in the prior art needs to be used under the condition of heating at a higher temperature, the cleaning effect is restricted by components and a treatment object, and meanwhile, a large amount of surfactant is used to bring certain influence on the subsequent treatment of the cleaned crude oil. Therefore, the development of the biodegradable microemulsion cleaning agent which has strong adaptability and wide application range and can efficiently clean the crude oil at normal temperature is very necessary for realizing the resource treatment of the produced liquid sediment.
Disclosure of Invention
The invention aims to solve the problems that the existing cleaning agent has high use temperature, the cleaning effect is restricted by components and a treatment object, and a large amount of surfactant is used to influence the subsequent treatment of the cleaned crude oil, and provides a biodegradable microemulsion cleaning agent, and a preparation method and application thereof.
In order to achieve the above object, the present invention provides in a first aspect a biodegradable microemulsion cleaning agent, which is a medium-phase microemulsion cleaning agent, comprising, based on the total weight of the cleaning agent: 5-10wt% of oil phase, 0.5-5wt% of surfactant, 5-15wt% of cosurfactant, 1-6.5wt% of inorganic salt and 63.5-89.5wt% of water; wherein,
the surfactant is alpha-sulfo fatty acid methyl ester salt and/or alcohol ether sulfo succinic acid monoester salt; the particle size distribution range of the cleaning agent is 15-40nm.
The second aspect of the invention provides a preparation method of a biodegradable microemulsion cleaning agent, which comprises the following steps:
(1) Dissolving a surfactant by using an oil phase, and cooling a dissolved product to room temperature to prepare a solution a;
(2) Dissolving inorganic salt in water to prepare a solution b;
(3) Equally dividing the cosurfactant into an auxiliary agent I and an auxiliary agent II which are the same in weight, and equally dividing the solution b into a solution b1 and a solution b2 which are the same in weight; under the condition of stirring, adding the auxiliary agent I and the solution b1 into the solution a simultaneously to prepare a mixed solution; and heating the mixed solution, adding the auxiliary agent II and the solution b2 into the mixed solution simultaneously under the stirring condition, uniformly stirring, and cooling to room temperature to obtain the cleaning agent.
In a third aspect, the present invention provides a cleaning agent prepared by the method of the second aspect.
In a fourth aspect, the invention provides use of a cleaning agent as described in the previous third aspect for cleaning crude oil in recovered produced fluid deposits.
Through the technical scheme, the cleaning agent provided by the invention has the following beneficial effects:
(1) The oil phase and inorganic salt used in the components are less limited, the temperature required by preparation is lower, the raw material source is wide, the operation is simple, and the cost is low;
(2) The oil removing agent has strong adaptability and wide application, does not need heating when in use, has the oil removing rate of over 93 percent at normal temperature, and can realize efficient cleaning and recovery of crude oil in produced liquid sediments with different compositions at normal temperature;
(3) The self-degradation rate is high, the self-degradation rate in 7 days reaches more than 95%, the subsequent treatment of the cleaned crude oil is not affected, and the method is environment-friendly.
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.
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The invention provides a biodegradable microemulsion cleaning agent, which is a middle-phase microemulsion cleaning agent and comprises the following components in percentage by weight based on the total weight of the cleaning agent: 5-10wt% of oil phase, 0.5-5wt% of surfactant, 5-15wt% of cosurfactant, 1-6.5wt% of inorganic salt and 63.5-89.5wt% of water; wherein,
the surfactant is alpha-sulfo fatty acid methyl ester salt and/or alcohol ether sulfo succinic acid monoester salt; the particle size distribution range of the cleaning agent is 15-40nm.
In the invention, the inventor finds that when the cleaning agent prepared based on each component in the invention is the middle-phase microemulsion, the cleaning effect on crude oil in produced fluid sediments is obviously higher than that of the upper-phase microemulsion and the lower-phase microemulsion prepared by the same component. Therefore, in order to obtain an ideal cleaning effect, in the presence of an oil phase and a water phase, a specific middle-phase microemulsion with strong solubilization and excellent thermodynamic stability is prepared by selecting specific types and dosage of surfactants, cosurfactants and electrolytes, the cleaning agent disclosed by the invention is the middle-phase microemulsion, the particle size distribution range of emulsion particles in the microemulsion is 15-40nm, and the particle size distribution range of D50 is 17-30nm, so that the high-efficiency cleaning of crude oil in produced liquid sediments can be realized. In particular, the inventors found in the research that, by changing the preparation conditions, when the particle size of the prepared cleaning agent does not satisfy the above range, the cleaning efficiency of the prepared cleaning agent on crude oil in produced fluid sediments is remarkably reduced.
In some embodiments of the invention, the oil phase has a distillation range of 150 to 380 ℃, preferably from at least one of kerosene, diesel oil and white oil, more preferably kerosene and/or diesel oil. The invention has little restriction on the selection of oil phase in the components, and the prepared cleaning agent has high-efficiency cleaning effect on crude oil at normal temperature by using the common oil phase in the distillation range, thereby having the advantages of strong adaptability, wide raw material source and low cost.
In some embodiments of the present invention, the surfactant is preferably sodium methyl alpha-sulfo fatty acid ester and/or disodium alcohol ether sulfosuccinate, which enables the structure of the surfactant to have a longer and more linear hydrophobic chain, thereby having good self-degradation performance, and the introduction of the ethoxy chain and the ether bond can further accelerate the self-degradation speed of the surfactant. Further preferably, the weight percentage of the surfactant is 1.5-4wt%, so that the formed middle-phase microemulsion has a high-efficiency cleaning effect on crude oil at normal temperature, and the self-degradation rate is high. Besides the characteristics, the surfactant used in the invention also has the characteristics of environmental protection and low use cost.
In some embodiments of the invention, the co-surfactant is selected from at least one of the saturated monohydric alcohols of C3-C7, preferably n-butanol. Further preferably, the weight percentage of the cosurfactant is 8-13wt%, so that the cosurfactant is more favorable for reducing interfacial tension, and a system spontaneously forms a phase microemulsion phase state, so that the crude oil is efficiently cleaned at normal temperature.
In some embodiments of the invention, the inorganic salt is selected from halides, preferably at least one of sodium chloride, magnesium chloride and potassium chloride, more preferably sodium chloride. Further preferably, the weight ratio of the inorganic salt is 2-4.5wt%, and further the solubilization effect on the oil phase is greatly improved, so that the formed middle-phase microemulsion has good stability, and the crude oil is efficiently cleaned at normal temperature.
The second aspect of the invention provides a preparation method of a biodegradable microemulsion cleaning agent, which comprises the following steps:
(1) Dissolving a surfactant by using an oil phase, and cooling a dissolved product to room temperature to prepare a solution a;
(2) Dissolving inorganic salt in water to prepare a solution b;
(3) Equally dividing the cosurfactant into an auxiliary agent I and an auxiliary agent II which are the same in weight, and equally dividing the solution b into a solution b1 and a solution b2 which are the same in weight; under the condition of stirring, adding the auxiliary agent I and the solution b1 into the solution a at the same time to prepare a mixed solution; and heating the mixed solution, adding the auxiliary agent II and the solution b2 into the mixed solution simultaneously under the stirring condition, uniformly stirring, and cooling to room temperature to obtain the cleaning agent.
In some embodiments of the present invention, in step (1), in order to sufficiently dissolve the surfactant in the oil phase, thereby obtaining the uniform and stable solution a, the dissolution may be performed under heating, preferably, the dissolution temperature may be 25 to 40 ℃, and the dissolution time may be 20 to 50min.
In the present invention, in the step (1), preferably, the dissolving condition further comprises stirring to enable the surfactant to be more sufficiently dissolved in the oil phase while increasing the dissolving rate, wherein the stirring rate may be 200 to 350 rpm.
In some embodiments of the present invention, in step (2), the purpose of dissolving with water is as long as a uniform and stable solution b can be obtained, preferably, the dissolving temperature is 25-40 ℃ and the dissolving time is 10-30min.
Further preferably, the dissolving conditions with water further comprise stirring at a rate of 100 to 200 rpm.
In some embodiments of the present invention, in step (3), the additive I and the solution b1 are added to the solution a simultaneously under normal temperature and stirring conditions, and the addition is completed synchronously by using a continuous addition manner or a dropwise addition manner to maintain uniform addition rates of the additive I and the solution b1, so as to obtain a mixed solution. And heating the mixed solution, adding the auxiliary agent II and the solution b2 into the mixed solution simultaneously under the stirring condition, wherein the continuous addition mode or the dropwise addition mode is adopted, so that the auxiliary agent II and the solution b2 are respectively kept at uniform addition rates, synchronously adding the auxiliary agent II and the solution b2, and cooling to room temperature after uniform stirring to prepare the cleaning agent.
The heating temperature is 30-40 ℃; preferably, the stirring speed is 300-600 rpm and the stirring time is 30-60min.
In the step (3) of the invention, the cosurfactant and the solution b are added into the solution a in batches and under different temperature conditions, so that the critical micelle concentration of the microemulsion can be obviously reduced, an adsorption film is formed, the prepared cleaning agent is in a phase-middle microemulsion phase state, and the crude oil is efficiently cleaned at normal temperature.
In a third aspect, the present invention provides a cleaning agent prepared by the method of the second aspect.
The cleaning agent prepared by the invention is a middle-phase microemulsion, and comprises the following components based on the total weight of the cleaning agent: 5-10wt% of oil phase, 0.5-5wt% of surfactant, 5-15wt% of cosurfactant, 1-6.5wt% of inorganic salt and 63.5-89.5wt% of water; wherein the surfactant is alpha-sulfo fatty acid methyl ester salt and/or alcohol ether sulfo succinic acid monoester salt; the particle size distribution range of the cleaning agent is 15-40nm. The cleaning agent has high-efficiency cleaning effect on crude oil at normal temperature, and has high self-degradation rate.
In a fourth aspect, the invention provides use of a cleaning agent as described in the previous third aspect for cleaning crude oil in recovered produced fluid deposits.
The present invention will be described in detail below by way of examples. In the following examples and comparative examples, the amounts of the respective raw materials are added in such amounts that the components required for the cleaning agent are satisfied, and the amounts are shown in parentheses after the raw materials.
The particle size index of the cleaner was measured using a laser particle size analyzer (malvern Mastersizer 3000).
In the case where no specific description is made, the materials used are those which are generally commercially available.
Example 1
(1) Dissolving disodium alcohol ether sulfosuccinate monoester (3.2 wt%) with diesel oil (9 wt%) at stirring rate of 300 r/min at 35 deg.C for 25min, and cooling to room temperature to obtain solution a;
(2) Dissolving sodium chloride (4.5 wt%) in water (73.3 wt%) at a stirring rate of 150 rpm at a dissolving temperature of 25 ℃ for 15min to obtain a solution b;
(3) N-butyl alcohol (10 wt%) is equally divided into an auxiliary agent I and an auxiliary agent II with the same weight, and the solution b is equally divided into a solution b1 and a solution b2 with the same weight; under the condition of stirring speed of 400 r/m, adding the auxiliary agent I and the solution b1 into the solution a at the same time to prepare a mixed solution; the mixture was heated to 35 ℃ and the auxiliary II and the solution b2 were added simultaneously to the mixture at a stirring rate of 400 rpm. Stirring for 45min, and cooling to room temperature to obtain the cleaning agent S1.
The cleaning agent S1 comprises the following components: 3.2wt% of disodium alcohol ether sulfosuccinate monoester, 10wt% of n-butanol, 9wt% of diesel oil, 4.5wt% of sodium chloride and 73.3wt% of water.
The particle size distribution range of the cleaning agent S1 is 15-25nm, and the D50 is 17nm.
Example 2
(1) Dissolving alpha-sulfo fatty acid methyl ester sodium (4 wt%) with kerosene (7.9 wt%) at a stirring rate of 300 r/min, wherein the dissolving temperature is 35 ℃, the dissolving time is 45min, and the dissolved product is cooled to room temperature to prepare a solution a;
(2) Dissolving sodium chloride (3.2 wt%) with water (71.9 wt%) at a stirring rate of 150 rpm at a dissolving temperature of 30 ℃ for 25min to obtain a solution b;
(3) N-butyl alcohol (13 wt%) is equally divided into an auxiliary agent I and an auxiliary agent II with the same weight, and the solution b is equally divided into a solution b1 and a solution b2 with the same weight; under the condition of stirring speed of 450 rpm, adding the auxiliary agent I and the solution b1 into the solution a simultaneously to prepare a mixed solution; the mixture is heated to 30 ℃ and the auxiliary II and the solution b2 are added simultaneously to the mixture at a stirring rate of 450 rpm. Stirring for 50min, and cooling to room temperature to obtain cleaning agent S2.
The cleaning agent S2 comprises the following components: 4wt% of alpha-sulfo fatty acid methyl ester sodium, 13wt% of n-butanol, 7.9wt% of kerosene, 3.2wt% of sodium chloride and 71.9wt% of water.
The particle size distribution range of the cleaning agent S2 is 18-29nm, and the D50 is 20.2nm.
Example 3
(1) Dissolving alpha-sulfo fatty acid methyl ester sodium (1.5 wt%) with diesel oil (8.5 wt%) at a stirring speed of 350 r/min at a dissolving temperature of 25 ℃ for 30min, and cooling the dissolved product to room temperature to obtain a solution a;
(2) Dissolving sodium chloride (2 wt%) with water (80 wt%) at a stirring rate of 200 r/min at 40 ℃ for 20min to obtain a solution b;
(3) N-butyl alcohol (8 wt%) is equally divided into an auxiliary agent I and an auxiliary agent II with the same weight, and the solution b is equally divided into a solution b1 and a solution b2 with the same weight; under the condition of stirring speed of 450 rpm, adding the auxiliary agent I and the solution b1 into the solution a simultaneously to prepare a mixed solution; the mixture is heated to 30 ℃ and the auxiliary II and the solution b2 are added simultaneously to the mixture at a stirring rate of 450 rpm. Stirring for 50min, and cooling to room temperature to obtain cleaning agent S3.
The cleaning agent S3 comprises the following components: 1.5wt% of alpha-sulfo fatty acid methyl ester sodium, 8wt% of n-butanol, 8.5wt% of diesel oil, 2wt% of sodium chloride and 80wt% of water.
The particle size distribution range of the cleaning agent S3 is 20-33nm, and the D50 is 24.5nm.
Example 4
(1) Dissolving alpha-sulfo fatty acid methyl ester sodium (1.2 wt%) with diesel oil (5 wt%) under the condition of stirring speed of 200 r/min, wherein the dissolving temperature is 30 ℃, the dissolving time is 45min, and the dissolved product is cooled to room temperature to prepare solution a;
(2) Dissolving magnesium chloride (3.5 wt%) with water (83.3 wt%) at a stirring rate of 150 rpm at 35 deg.C for 10min to obtain solution b;
(3) N-propanol (7 wt%) is divided into an auxiliary agent I and an auxiliary agent II which have the same weight, and the solution b is divided into a solution b1 and a solution b2 which have the same weight; under the condition of stirring speed of 300 r/m, adding the auxiliary agent I and the solution b1 into the solution a at the same time to prepare a mixed solution; the mixture is heated to 40 ℃ and the auxiliary II and the solution b2 are added simultaneously to the mixture at a stirring rate of 300 revolutions per minute. Stirring for 35min, and cooling to room temperature to obtain cleaning agent S4.
The cleaning agent S4 comprises the following components: 1.2wt% of alpha-sulfo fatty acid methyl ester sodium, 7wt% of n-propanol, 5wt% of diesel oil, 3.5wt% of magnesium chloride and 83.3wt% of water.
The particle size distribution range of the cleaning agent S4 is 22-37nm, and the D50 is 26.3nm.
Example 5
(1) Dissolving 2wt% of disodium alcohol ether sulfosuccinate monoester with 6.5wt% of kerosene at the stirring speed of 250 rpm, wherein the dissolving temperature is 35 ℃, the dissolving time is 50min, and the dissolved product is cooled to room temperature to prepare a solution a;
(2) Dissolving sodium chloride (1 wt%) with water (76.5 wt%) at a stirring rate of 200 rpm at a dissolving temperature of 25 ℃ for 25min to obtain a solution b;
(3) Equally dividing n-pentanol (14 wt%) into an auxiliary agent I and an auxiliary agent II with the same weight, and equally dividing the solution b into a solution b1 and a solution b2 with the same weight; under the condition of stirring speed of 500 r/m, adding the auxiliary agent I and the solution b1 into the solution a at the same time to prepare a mixed solution; the mixture is heated to 38 ℃ and the auxiliary II and the solution b2 are added simultaneously to the mixture at a stirring rate of 500 rpm. Stirring for 40min, and cooling to room temperature to obtain cleaning agent S5.
The cleaning agent S5 comprises the following components: 2wt% of disodium alcohol ether sulfosuccinate, 14wt% of n-amyl alcohol, 6.5wt% of kerosene, 1wt% of sodium chloride and 76.5wt% of water.
The particle size distribution range of the cleaning agent S5 is 23-34nm, and the D50 is 27.8nm.
Example 6
(1) Dissolving 0.5wt% of disodium alcohol ether sulfosuccinate monoester with 7.5wt% of white oil at a stirring speed of 200 rpm, wherein the dissolving temperature is 40 ℃, the dissolving time is 20min, and the dissolved product is cooled to room temperature to prepare a solution a;
(2) Dissolving sodium chloride (6.5 wt%) with water (70.5 wt%) at a stirring rate of 100 rpm at a dissolving temperature of 30 ℃ for 30min to obtain a solution b;
(3) Equally dividing n-hexanol (15 wt%) into an auxiliary agent I and an auxiliary agent II which are the same in weight, and equally dividing the solution b into a solution b1 and a solution b2 which are the same in weight; under the condition of stirring speed of 600 r/m, adding the auxiliary agent I and the solution b1 into the solution a at the same time to prepare a mixed solution; the mixture was heated to 32 ℃ and the auxiliary II and the solution b2 were added simultaneously to the mixture at a stirring rate of 600 rpm. Stirring for 60min, and cooling to room temperature to obtain cleaning agent S6.
The cleaning agent S6 comprises the following components: 0.5wt% of disodium alcohol ether sulfosuccinate, 15wt% of n-hexanol, 7.5wt% of white oil, 6.5wt% of sodium chloride and 70.5wt% of water.
The particle size distribution range of the cleaning agent S6 is 21-37nm, and the D50 is 28.3nm.
Example 7
(1) Dissolving alpha-sulfo fatty acid methyl ester sodium (5 wt%) with diesel oil (10 wt%) at a stirring speed of 350 r/min at 25 ℃ for 35min, and cooling the dissolved product to room temperature to obtain a solution a;
(2) Dissolving potassium chloride (3 wt%) in water (73 wt%) at a stirring rate of 170 rpm at a dissolving temperature of 35 ℃ for 15min to obtain a solution b;
(3) Equally dividing n-pentanol (9 wt%) into an auxiliary agent I and an auxiliary agent II with the same weight, and equally dividing the solution b into a solution b1 and a solution b2 with the same weight; under the condition of stirring speed of 550 rpm, adding the auxiliary agent I and the solution b1 into the solution a simultaneously to prepare a mixed solution; the mixture was heated to 37 ℃ and the auxiliary II and the solution b2 were added simultaneously to the mixture at a stirring rate of 550 rpm. Stirring for 30min, and cooling to room temperature to obtain cleaning agent S7.
The composition of the cleaning agent S7 is as follows: 5wt% of alpha-sulfo fatty acid methyl ester sodium, 9wt% of n-amyl alcohol, 10wt% of diesel oil, 3wt% of potassium chloride and 73wt% of water.
The particle size distribution range of the cleaning agent S7 is 20-35nm, and the D50 is 28.9nm.
Example 8
(1) Dissolving alpha-sulfo fatty acid methyl ester sodium (2.5 wt%) by white oil (9.5 wt%) under the condition of stirring speed of 250 revolutions per minute, wherein the dissolving temperature is 35 ℃, the dissolving time is 45min, and the dissolved product is cooled to room temperature to prepare a solution a;
(2) Dissolving magnesium chloride (6 wt%) with water (77 wt%) at a stirring rate of 130 r/min at 40 ℃ for 25min to obtain a solution b;
(3) Equally dividing n-heptanol (5 wt%) into an auxiliary agent I and an auxiliary agent II with the same weight, and equally dividing the solution b into a solution b1 and a solution b2 with the same weight; under the condition of stirring speed of 350 r/m, adding the auxiliary agent I and the solution b1 into the solution a at the same time to prepare a mixed solution; the mixture was heated to 36 ℃ and the auxiliary II and the solution b2 were added simultaneously to the mixture at a stirring rate of 350 rpm. Stirring for 55min, and cooling to room temperature to obtain cleaning agent S8.
The composition of the cleaning agent S8 is as follows: 2.5wt% of alpha-sulfo fatty acid methyl ester sodium, 5wt% of n-heptanol, 9.5wt% of white oil, 6wt% of magnesium chloride and 77wt% of water.
The particle size distribution range of the cleaning agent S8 is 25-40nm, and the D50 is 30nm.
Comparative example 1
The procedure of example 1 was followed except that disodium alcohol ether sulfosuccinate was used in an amount of 0.2wt%. Other conditions were the same as in example 1. Thus obtaining a cleaning agent D1.
The particle size distribution range of the cleaning agent D1 is 78-92nm, and the D50 is 85.7nm.
Comparative example 2
The procedure of example 1 was followed except that the surfactant was sodium dodecylbenzenesulfonate. Other conditions were the same as in example 1. Thus obtaining a cleaning agent D2.
The particle size distribution range of cleaning agent D2 is 117-133nm, and the D50 is 123.3nm.
Comparative example 3
The procedure is as in example 1, except that the co-surfactant is n-octanol. Other conditions were the same as in example 1. Thus obtaining a cleaning agent D3.
The particle size distribution range of the cleaning agent D3 is 89-106nm, and the D50 is 95.1nm.
Comparative example 4
The procedure of example 1 was followed except that, in step (3), the mixed solution was not heated, and the auxiliary II and the solution b2 were simultaneously added to the mixed solution at normal temperature. Other conditions were the same as in example 1. Thus obtaining a cleaning agent D4.
The particle size distribution range of the cleaning agent D4 is 92-110nm, and the D50 is 99.5nm.
Comparative example 5
The procedure of example 1 was followed except that, in step (3), the solution a was heated to 35 ℃ first, and then n-butanol and the solution b were added to the solution a at once and simultaneously. Other conditions were the same as in example 1. Thus obtaining a cleaning agent D5.
The particle size distribution range of cleaning agent D5 is 106-122nm, and D50 is 113.7nm.
Test example
The cleaning agents prepared in examples 1-8 and comparative examples 1-5 are used for treating produced fluid sediments, and the degradation rate is tested to evaluate the application effect of the cleaning agent provided by the invention in cleaning crude oil in recovered produced fluid sediments and the degradability of the cleaning agent.
The produced liquid sediment adopted in the test example is taken from a victory oil field, and the oil content of the produced liquid sediment is 20.2-52.1wt%.
1. Oil removal test of cleaning agent
Weighing the produced liquid sediment with the mass m, and placing the produced liquid sediment with the mass m 0 Pouring a proper amount of toluene into the flask, uniformly stirring, sealing the flask and placing the flask into an ultrasonic groove; after ultrasonic treatment, the produced liquid is repeatedly washed by toluene to precipitateFiltering the deposit to obtain a solid phase, and carrying out reduced pressure distillation on the filtrate to separate out toluene; after the washing, the flask was dried, and the mass m of the flask was measured 1 ；
Calculating according to a formula (1) to obtain the oil content C of the produced fluid sediment,
C＝(m 1 -m 0 )/m×100％ (1)
with reference to the above method, the oil content C of the produced fluid deposit before cleaning is determined 0 And the oil content C of the cleaned produced liquid sediment 1 ；
The oil removal rate R is calculated according to the formula (2),
R＝(C 0 -C 1 )/C 0 ×100％ (2)
the test results are shown in table 1.
TABLE 1
| Test item | Oil removal Rate/% (Normal temperature) |
| S1 is utilized to clean waste drilling fluid (oil content is 49.9%) | 97.1 |
| S2 is utilized to clean waste drilling fluid (oil content is 20.3%) | 96.4 |
| S3 is utilized to clean oil sludge sand (oil content 52.1%) | 96.7 |
| Cleaning oil sludge sand (oil content 49.9%) by S4 | 95.1 |
| Cleaning abandoned drill by S5Well fluid (oil content 35.9%) | 94.3 |
| S6 is utilized to clean waste drilling fluid (oil content is 43.7%) | 93.2 |
| Oil sludge sand (oil content 20.2%) is cleaned by S7 | 94.9 |
| Oil sludge sand (oil content 35.4%) is cleaned by S8 | 94.1 |
| D1 is utilized to clean waste drilling fluid (oil content is 49.9%) | 50.3 |
| D2 cleaning waste drilling fluid (oil content 49.9%) | 23.6 |
| D3 cleaning waste drilling fluid (oil content 49.9%) | 46.1 |
| D4 cleaning waste drilling fluid (oil content 49.9%) | 41.7 |
| D5 cleaning waste drilling fluid (oil content 49.9%) | 30.4 |
As can be seen from Table 1, the cleaning agent provided by the invention can be used for efficiently cleaning and recovering crude oil in produced liquid sediments with different types and oil contents, the oil removal rate reaches over 93% at normal temperature, and the cleaning agent is low in use temperature and more beneficial to field application. Examples 1 to 3 have significantly better results, whereas the comparative examples, which did not employ the process according to the invention, had lower oil removal rates.
In particular, as can be seen from comparison between example 1 and comparative examples 4 to 5, the prepared cleaning agent can effectively clean crude oil at normal temperature by adopting the process used in the specific preparation method of the invention. While comparative examples 4-5 did not employ this method, the oil removal rate was significantly low.
2. Degradation rate test of cleaning agent
Weighing a certain amount of cleaning agent as a sample, extracting according to a specified procedure, measuring the absorbance of the sample at the wavelength of 650nm by using a spectrophotometer (taking trichloromethane extraction liquid of a blank test as reference), drawing a standard curve of the quality of the cleaning agent and the absorbance, and comparing the absorbance of the self-degraded cleaning agent with the standard curve to obtain the quality of the self-degraded cleaning agent.
The degradation rate is calculated according to the following formula:
D＝(m 0 -m n )/m 0 ×100％
in the formula: d is the degradation rate of the surfactant after the nth day; m is 0 Is the initial surfactant mass; m is n Is the surfactant mass after the nth day.
The test results are shown in table 2.
TABLE 2
As can be seen from Table 2, the self-degradation rate of the cleaning agent provided by the invention reaches more than 95% on the 7 th day, and the subsequent treatment of the cleaned crude oil is not affected. Examples 1-3 have significantly better results, while comparative example 2 has no surfactant used in the process of the present invention and has a lower self-degradation rate.
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 (30)
1. A biodegradable microemulsion cleaning agent is characterized in that the cleaning agent is a medium-phase microemulsion and comprises the following components based on the total weight of the cleaning agent: 5-10wt% of oil phase, 0.5-5wt% of surfactant, 5-15wt% of cosurfactant, 1-6.5wt% of inorganic salt and 63.5-89.5wt% of water; wherein,
the surfactant is alpha-sulfo fatty acid methyl ester salt and/or alcohol ether sulfo succinic acid monoester salt; the particle size distribution range of the cleaning agent is 15-40nm;
the distillation range of the oil phase is 150-380 ℃;
the cosurfactant is selected from at least one of saturated monohydric alcohols of C3-C7;
the inorganic salt is selected from halides.
2. The cleaning agent according to claim 1, wherein the oil phase is at least one selected from kerosene, diesel oil and white oil.
3. The cleaning agent according to claim 2, wherein the oil phase is kerosene and/or diesel oil.
4. The cleaning agent according to any one of claims 1 to 3,
the surfactant is alpha-sulfo fatty acid methyl ester sodium and/or alcohol ether sulfo succinic acid monoester disodium;
the cosurfactant is n-butyl alcohol.
5. The cleaning agent according to any one of claims 1 to 3, wherein the inorganic salt is at least one of sodium chloride, magnesium chloride and potassium chloride.
6. The cleaning agent according to claim 5, wherein the inorganic salt is sodium chloride.
7. The cleaning agent according to claim 4, wherein the inorganic salt is at least one of sodium chloride, magnesium chloride and potassium chloride.
8. The cleaning agent according to claim 7, wherein the inorganic salt is sodium chloride.
9. A preparation method of a biodegradable microemulsion cleaning agent is characterized by comprising the following steps:
(1) Dissolving a surfactant by using an oil phase, and cooling a dissolved product to room temperature to prepare a solution a;
(2) Dissolving inorganic salt in water to prepare a solution b;
(3) Equally dividing the cosurfactant into an auxiliary agent I and an auxiliary agent II which are the same in weight, and equally dividing the solution b into a solution b1 and a solution b2 which are the same in weight; under the condition of stirring, adding the auxiliary agent I and the solution b1 into the solution a simultaneously to prepare a mixed solution; heating the mixed solution, adding the auxiliary agent II and the solution b2 into the mixed solution simultaneously under the condition of stirring, uniformly stirring, and cooling to room temperature to prepare the cleaning agent; wherein,
the surfactant is alpha-sulfo fatty acid methyl ester salt and/or alcohol ether sulfo succinic acid monoester salt;
the distillation range of the oil phase is 150-380 ℃;
the cosurfactant is selected from at least one of saturated monohydric alcohols of C3-C7;
the inorganic salt is selected from halides;
the particle size distribution range of the cleaning agent is 15-40nm.
10. The method of claim 9, wherein the oil phase is selected from at least one of kerosene, diesel fuel, and white oil.
11. The method of claim 10, wherein the oil phase is kerosene and/or diesel.
12. The method of any one of claims 9-11,
the surfactant is alpha-sulfo fatty acid methyl ester sodium and/or alcohol ether sulfo succinic acid monoester disodium;
the cosurfactant is n-butanol.
13. The method of any one of claims 9-11, wherein the inorganic salt is at least one of sodium chloride, magnesium chloride, and potassium chloride.
14. The method of claim 13, wherein the inorganic salt is sodium chloride.
15. The method of claim 12, wherein the inorganic salt is at least one of sodium chloride, magnesium chloride, and potassium chloride.
16. The method of claim 15, wherein the inorganic salt is sodium chloride.
17. The production method according to any one of claims 9 to 11 and 14 to 16, wherein in the step (1), the dissolving conditions include: the dissolving temperature is 25-40 deg.C, and the dissolving time is 20-50min;
and/or, the dissolving condition also comprises stirring, and the stirring speed is 200-350 r/m.
18. The production method according to claim 12, wherein in step (1), the conditions for dissolution include: the dissolving temperature is 25-40 deg.C, and the dissolving time is 20-50min;
and/or, the dissolving condition also comprises stirring, and the stirring speed is 200-350 r/m.
19. The production method according to claim 13, wherein in step (1), the conditions for dissolution include: the dissolving temperature is 25-40 deg.C, and the dissolving time is 20-50min;
and/or, the dissolving condition also comprises stirring, and the stirring speed is 200-350 r/m.
20. The production method according to any one of claims 9 to 11, 14 to 16, and 18 to 19, wherein in the step (2), the conditions for dissolution with water include: the dissolving temperature is 25-40 deg.C, and the dissolving time is 10-30min;
and/or, the condition of dissolving by water also comprises stirring, and the stirring speed is 100-200 r/min.
21. The production method according to claim 12, wherein in the step (2), the conditions for dissolution with water include: the dissolving temperature is 25-40 deg.C, and the dissolving time is 10-30min;
and/or, the condition of dissolving by water also comprises stirring, and the stirring speed is 100-200 r/min.
22. The production method according to claim 13, wherein in the step (2), the conditions for dissolution with water include: the dissolving temperature is 25-40 deg.C, and the dissolving time is 10-30min;
and/or, the condition of dissolving by water also comprises stirring, and the stirring speed is 100-200 r/min.
23. The method of claim 17, wherein, in the step (2), the conditions for dissolving with water include: the dissolving temperature is 25-40 deg.C, and the dissolving time is 10-30min;
and/or, the condition of dissolving by water also comprises stirring, and the stirring speed is 100-200 r/min.
24. The production method according to any one of claims 9 to 11, 14 to 16, 18 to 19, and 21 to 23, wherein, in the step (3), the temperature of heating is 30 to 40 ℃;
and/or the stirring speed is 300-600 r/m, and the stirring time is 30-60min.
25. The production method according to claim 12, wherein, in the step (3), the temperature of the heating is 30 to 40 ℃;
and/or the stirring speed is 300-600 r/m, and the stirring time is 30-60min.
26. The production method according to claim 13, wherein, in the step (3), the temperature of the heating is 30 to 40 ℃;
and/or the stirring speed is 300-600 r/m, and the stirring time is 30-60min.
27. The production method according to claim 17, wherein, in the step (3), the temperature of the heating is 30 to 40 ℃;
and/or the stirring speed is 300-600 r/m, and the stirring time is 30-60min.
28. The production method according to claim 20, wherein, in the step (3), the temperature of the heating is 30 to 40 ℃;
and/or the stirring speed is 300-600 r/m, and the stirring time is 30-60min.
29. A cleaning agent produced by the production method according to any one of claims 9 to 28.
30. Use of the cleaning agent of claim 29 to clean crude oil in recovered production fluid deposits.
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