CN108929664B - Foamless cleaning agent and preparation method and application thereof - Google Patents

Foamless cleaning agent and preparation method and application thereof Download PDF

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CN108929664B
CN108929664B CN201810933900.XA CN201810933900A CN108929664B CN 108929664 B CN108929664 B CN 108929664B CN 201810933900 A CN201810933900 A CN 201810933900A CN 108929664 B CN108929664 B CN 108929664B
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parts
stirring
cleaning agent
oil
foamless
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CN108929664A (en
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金承平
杨亚东
余代美
许磊
王泽东
张超
陈波
黄波
黄建波
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Fluids Chem Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/52Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/54Compositions for in situ inhibition of corrosion in boreholes or wells

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Abstract

The invention discloses a foamless cleaning agent and a preparation method and application thereof. The oleic hydroxyethyl imidazoline in the foamless cleaning agent has the functions of corrosion inhibition and corrosion prevention, can pay attention to the corrosion prevention protection of underground casings and oil pipes and prolong the service life while cleaning, the isothiazolinone has the function of sterilization, and the xanthan gum can improve the viscosity of the cleaning agent to provide the suspension capacity for precipitated solid phase in the cleaning process, so that the carrying of high-density solid phase washed out at the bottom of a well is met; meanwhile, the spatial network structure of the xanthan gum can make the prepared cleaning agent product more stable.

Description

Foamless cleaning agent and preparation method and application thereof
Technical Field
The invention belongs to the technical field of petroleum drilling, and particularly relates to a foamless cleaning agent as well as a preparation method and application thereof.
Background
At present, in the exploration and development of oil and gas wells, with the increasing of deep wells, high-temperature wells and shale gas wells, the application of the oil-based drilling fluid is increased day by day, and although the application of the oil-based drilling fluid greatly reduces various complex conditions in the drilling process, the oil-based drilling fluid is easy to adhere to underground casings, oil pipes and tool strings and is not easy to remove; thereby causing great limitation to the multi-section bridge plug setting, electrical measurement, perforation operation and oil and gas production and transportation operation of well completion operation. Typically, oil-based drilling fluid residues adhering to the casing or tubing wall can cause setting failures of the bridge plug, failure of the electrical logging tool and perforating gun to the desired depth, and blockage of the oil and gas production tubing. In order to ensure the well completion and production operations to be carried out smoothly, the oil-based drilling fluid residues in the downhole casing and the oil pipe must be cleaned.
Oil-based drilling fluids are water-in-oil emulsion fluids with complex, colloidal structure that are stable, and the components usually contain highly adhesive organic colloids, oil phase, water phase, weighting agent, etc. Therefore, the following aspects must be considered in cleaning the residual oil-based drilling fluid left in the well: 1. the cleaning agent has good dissolving and dispersing capacity on the oil-based drilling fluid; 2. the cleaning agent has good temperature resistance so as to meet the requirement of still having good cleaning capability at high temperature at the bottom of a well; 3. the sand-carrying agent has certain sand-carrying performance so as to carry high-density solid-phase substances washed out of the well bottom; 4. when an oil pipe is cleaned, the condition that a cleaning agent can enter a production layer needs to be considered, and in order to ensure that the cleaning agent cannot cause hydration expansion of shale and blockage of a stratum oil and gas channel after entering a water-sensitive shale production layer, the cleaning agent needs to have good shale inhibition performance; 5. when an oil pipe is cleaned, if a large amount of foam exists in the back-discharged cleaning liquid, the shutdown of ground mining and transportation equipment is usually caused, so that the mining and transportation operation is influenced; therefore, the cleaning agent must be free of bubbles. 6. The cleaning agent has no corrosivity to metal casing and oil pipe. 7. The flash point is higher to ensure the safety of field operation. 8. The components of the cleaning agent are selected to be environment-friendly so as to avoid the influence of the cleaning liquid on the environment in the application process.
Chinese patent CN104152127A discloses a multifunctional cleaning agent for oil field and its preparation method and application, which is prepared from 0.2-1.0% of compound nonylphenol polyoxyethylene ether active agent and 0.2-1.0% of compound quaternary ammonium salt cation active agent chloride; 0 to 1.0 percent of composite acid pickling corrosion inhibitor, 0 to 1.0 percent of composite Fe ion chelating agent, 0 to 10.0 percent of organic carboxylate and the balance of water, wherein the cleaning agent is prepared by reacting CaCO with CaCO at the temperature of between 60 and 80 DEG C3、Fe2O3The FeS inorganic chemical scale has good acidolysis and dissolution removal effects, has dispersing and melting effects on oil scale, wax scale and heavy oil scale, has killing effects on oil field fungi, has stripping effect on clay scale, and is suitable for cleaning equipment such as oil well shafts, gathering and transportation pipelines, oil-water separation settling tanks, flocculation settling tanks, oil storage tanks, sewage storage tanks and the like. The cleaning agent is a water-soluble substance of a surfactant and other assistantsHowever, in the application process, the surfactant can generate a large amount of foams to influence the surface oil and gas production and transportation supercharging equipment, and in the later-stage cleaning liquid backflow process, chloride in the auxiliary agent has certain influence on the environment, and meanwhile, the carrying of high-density solid-phase substances at the bottom of a shaft is not involved.
Chinese patent CN103589412A discloses a shale gas development oil-based drilling fluid mud cake cleaning solution, which belongs to the technical field of petroleum drilling engineering chemical agents and comprises a cleaning agent, a weighting agent and water; the weight percentage of each component is as follows: 10-30% of cleaning agent, 0-60% of weighting agent and the balance of water, wherein the cleaning agent consists of nonionic surfactant and mutual solvent, and the weight ratio of the nonionic surfactant to the mutual solvent is 1:9-9: 1; the nonionic surfactant is fatty acid polyoxyethylene ether, polyoxyethylene fatty acid ester, polyoxypropylene fatty acid ester, etc., the mutual solvent is methanol, ethanol, isopropanol, etc., the weighting agent is superfine iron ore powder with a density of 4.90-5.20g/cm3. The invention can not solve the influence of a large amount of foam generated in the application process on ground oil gas production and transportation supercharging equipment, is only limited to the flushing of oil-based drilling fluid on the stratum rock during cementing, does not consider the corrosion prevention of the metal surface during cleaning in a casing and an oil pipe, does not consider the problems of oil gas channel blockage and the like caused by the fact that cleaning fluid enters a shale oil gas production layer to hydrate and expand the production layer, and can not meet the bubble-free requirement of oil pipe cleaning in gas production operation; the oil gas channel can be blocked by the solid phase of the weighting agent in the cleaning fluid.
Most of oil-based drilling fluid cleaning agents in the prior art are well cementation flushing agents, most of working interfaces of the oil-based drilling fluid cleaning agents are stratum rocks, and the cleaning of oil-based drilling fluid residues on metal interfaces of casing pipes and oil pipe walls and the corrosion prevention of production oil pipes are not involved; the components of the existing oil-based drilling fluid cleaning agent are surfactants or organic solvents, and a large amount of foam is easily generated in the cleaning process; no foamless cleaning agent aiming at the cleaning operation of the production oil pipe exists, and the water-based surfactant can generate a large amount of foam after the interfacial tension is reduced, thereby seriously influencing the normal work of the ground gas collection equipment in the gas production operation; the existing cleaning agent does not relate to carrying of high-density solid phase in oil stain; the protection of the shale stratum with strong water sensitivity when the oil pipe is cleaned is not involved.
The present invention has been made in view of the above circumstances.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a foamless cleaning agent and a preparation method and application thereof. The foamless cleaning agent disclosed by the invention realizes a high-efficiency foamless effect, solves the problem that gas production operation cannot be continuously carried out due to the influence of a large amount of foams on the normal operation of oil gas production, transportation and pressurization equipment in the field use process, pays attention to the anticorrosion protection of a downhole casing and an oil pipe and prolongs the service life of the underground casing and the oil pipe during cleaning, and can meet the requirement of carrying high-density solid-phase substances washed out from the bottom of a well during cleaning.
The first object of the invention provides a foamless cleaning agent, which comprises coco diethanolamide, n-decyl glucoside, polydimethylsiloxane, oleic hydroxyethyl imidazoline, isothiazolinone, potassium acetate, xanthan gum, paraffin oil and water.
The oleic hydroxyethyl imidazoline added into the foamless cleaning agent has the effects of corrosion inhibition and corrosion prevention, can pay attention to the corrosion prevention protection of underground casings and oil pipes and prolong the service life while cleaning, has the function of sterilization, prevents the suspension agent xanthan gum from being biodegraded in the using process, ensures that the viscosity of the cleaning agent can be improved by the xanthan gum to provide the suspension capacity for the precipitated solid phase in the cleaning process, and meets the requirement of carrying of high-density solid phase substances washed out at the bottom of a well; meanwhile, the spatial network structure of the xanthan gum can enable the prepared cleaning agent oil-in-water emulsion type product to be more stable, in addition, the cleaning agent disclosed by the invention is an oil-in-water type cleaning agent, wherein the paraffin oil serving as an oil phase component has good dispersing and solubilizing capabilities on residues of the oil-based drilling fluid, and has the characteristic of high efficiency and no foam, and meanwhile, the polydimethylsiloxane in the components also has a good foam inhibition effect, so that when the cleaning agent disclosed by the invention is used for cleaning the residues of the oil-based drilling fluid, foam cannot be generated in a back-discharge cleaning solution, the shutdown of ground gas production supercharging equipment caused by a large amount of foam can be avoided, and the normal operation of the production; potassium ions of potassium acetate can inhibit hydration and dispersion of mud shale in an oil-gas production layer, so that blockage of hydration and dispersion clay on an oil-gas channel is effectively prevented, and potassium acetate is easily degradable organic salt so that the environment cannot be polluted by flowback liquid; the components are environment-friendly, non-toxic, harmless and non-corrosive.
Further, according to the parts by weight, the cleaning agent comprises 5-10 parts of coconut diethanolamide, 5-15 parts of n-decyl glucoside, 0.3-1 part of polydimethylsiloxane, 1-3 parts of oleic acid base hydroxyethyl imidazoline, 0.05-0.4 part of isothiazolinone, 7-11 parts of potassium acetate, 0.3-0.4 part of xanthan gum, 30-55 parts of paraffin oil and 30-40 parts of water.
Through a large number of experiments, the cleaning agent prepared by adopting the raw materials in the proportion has the advantages of excellent cleaning effect, better stability, lower foaming rate and the like, so that the cleaning agent compounded by adopting the raw materials in the specific proportion has better economic popularization value while meeting the technical requirements of field application of the oil field, and the inconvenience and the increase of application cost caused by the inconvenience and the influence on the fluidity of the product due to too low component and too high component can not meet the requirements of the field application of the oil field.
Further, according to parts by weight, the cleaning agent comprises 7.5 parts by weight of coconut diethanolamide, 10 parts by weight of n-decyl glucoside, 0.6 part by weight of polydimethylsiloxane, 2 parts by weight of oleic hydroxyethyl imidazoline, 0.22 part by weight of isothiazolinone, 9 parts by weight of potassium acetate, 0.35 part by weight of xanthan gum, 42 parts by weight of paraffin oil and 35 parts by weight of water.
The second purpose of the invention is to provide a preparation method of the foamless cleaning agent, which comprises the following steps:
(1) weighing the components according to the weight for later use;
(2) putting the weighed water into a stirring kettle, adding the weighed potassium acetate, uniformly stirring, and fully dissolving to obtain a potassium acetate aqueous solution for later use;
(3) under the condition of stirring, adding the weighed xanthan gum into a potassium acetate aqueous solution, and heating a stirring kettle;
(4) putting the solution heated in the step (3) into a circulating shearing kettle for shearing to obtain homogeneous liquid, and closing a shearing pump;
(5) putting the homogeneous liquid into a stirring kettle, and sequentially adding the coconut diethanolamide, n-decyl glucoside, polydimethylsiloxane, oleic hydroxyethyl imidazoline and isothiazolinone for standby in the stirring kettle under the stirring state, and fully stirring;
(6) and slowly adding paraffin oil into the stirring kettle at a constant speed through a circulating shear pump under the condition of stirring to obtain the foamless cleaning agent.
Further, the heating temperature in the step (3) is 40-50 ℃.
Further, the homogeneous liquid in the step (4) has an apparent viscosity of 35-50mpa · s at 30 ℃.
Further, the shear rate in the step (4) is 150-200s-1
Further, in the step (5), the stirring speed is 180-200rpm, and the stirring time is 25-35 min.
Further, the shear rate in step (6) is 160-180s-1The shearing and stirring time is 1.8-2.2 hours.
The preparation of the foamless cleaning agent needs to be strictly controlled, for example, the stirring time, the stirring speed, the shearing time and the heating temperature are discovered by the applicant through a large amount of experiments and production debugging, the heating temperature is increased to 40-50 ℃, too much electric energy consumption and time are not needed, xanthan gum is more easily sheared and uniformly dispersed in the temperature range, caking is not easily generated, the performance of the obtained finished product is more stable, the low temperature is not beneficial to shearing and dispersing, and the excessive energy and time consumption can be caused if the temperature is too high; the apparent viscosity is controlled to be 35-50mPa.S, so that the quality of the product obtained in each batch is consistent and meets the sand carrying requirement of oil field application, the sand carrying is not facilitated when the product is too low, and the fluidity of the product during application is influenced when the product is too high; the shearing rate, the stirring rate and the shearing time are obtained by debugging according to the condition of production equipment and the production requirement of the cleaning agent, the quality of the prepared product is influenced if the shearing rate is too low, and the operation and the service life of the equipment are not facilitated if the shearing rate is too high; the cleaning agent prepared by the control conditions has low foaming rate and good stability, and meets the requirements of safe and efficient batch production.
The third purpose of the invention is to provide the application of the non-foaming cleaning agent in cleaning oil-based drilling fluid residues.
Compared with the prior art, the invention has the beneficial effects that:
(1) the oleic hydroxyethyl imidazoline in the cleaning agent has the functions of corrosion inhibition and corrosion prevention, can pay attention to the corrosion prevention protection of underground casings and oil pipes and prolong the service life while cleaning, the isothiazolinone has the function of sterilization, and the xanthan gum can improve the viscosity of the cleaning agent to provide the suspension capacity for a precipitated solid phase in the cleaning process, so that the carrying of a high-density solid phase object washed out at the bottom of a well is met; meanwhile, the prepared oil-in-water type cleaning agent product is more stable due to the spatial network structure of the xanthan gum, and in addition, the cleaning agent disclosed by the invention is an oil-in-water type cleaning agent, wherein the paraffin oil serving as an oil phase component has good dispersing and solubilizing capabilities on residues of the oil-based drilling fluid, and has the characteristic of high efficiency and no foam; potassium ions of potassium acetate can inhibit hydration and dispersion of mud shale in an oil-gas production layer, so that blockage of hydration and dispersion clay on an oil-gas channel is effectively prevented, and potassium acetate is easily degradable organic salt so that the environment cannot be polluted by flowback liquid; the components are environment-friendly, non-toxic, harmless and non-corrosive;
(2) the cleaning agent is easy to dissolve in water, has strong acid and alkali resistance, demulsification, suspension, dispersion, solubilization and wetting capacities, can play a very good cleaning effect on oil-based drilling fluid with complex components and stable colloid structure and various complex component oil stains, and can be carried out on the ground by the cleaning agent in the process of drilling rubber and cement plugs;
(3) the cleaning agent disclosed by the invention is high-temperature resistant, can reach more than 150 ℃, and can meet the construction requirements of high-temperature deep well cleaning operation;
(4) the oil-based drilling fluid has a good carrying effect on high-density solid-phase substances in oil stains of the oil-based drilling fluid, cleans a shaft while cleaning the oil stains, and avoids other complex conditions caused by the fact that the cleaned high-density solid-phase substances continue to remain in a sleeve and an oil pipe;
(5) the cleaning agent disclosed by the invention cannot damage a water-sensitive shale oil and gas production layer after entering the oil and gas production layer;
(6) the preparation method of the cleaning agent is simple and can be used for large-scale production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example 1
The foamless cleaning agent of the present example comprises 5kg of coconut diethanolamide, 5kg of n-decyl glucoside, 0.3kg of polydimethylsiloxane, 1kg of oleic hydroxyethyl imidazoline, 0.05kg of isothiazolinone, 7kg of potassium acetate, 0.3kg of xanthan gum, 30kg of paraffin oil and 30kg of water.
The preparation method of the foamless cleaning agent of the embodiment comprises the following steps:
(1) weighing the components according to the weight for later use;
(2) putting the weighed water into a stirring kettle, adding the weighed potassium acetate, uniformly stirring, and fully dissolving to obtain a potassium acetate aqueous solution for later use;
(3) under the condition of stirring, adding the weighed xanthan gum into a potassium acetate aqueous solution, and heating a stirring kettle to 40 ℃;
(4) adding step (3) toThe hot solution is put into a circulating shearing kettle for shearing, and the shearing rate is 150s-1Obtaining homogeneous liquid, and closing the shear pump when the apparent viscosity of the homogeneous liquid is 35mpa · s at the temperature of 30 ℃;
(5) putting the homogeneous liquid into a stirring kettle, and sequentially adding the coconut diethanolamide, n-decyl glucoside, polydimethylsiloxane, oleic hydroxyethyl imidazoline and isothiazolinone for standby in the stirring kettle under the stirring state, and fully stirring at the stirring speed of 180rpm for 25 min;
(6) under the condition of stirring, slowly adding paraffin oil into the stirring kettle at a constant speed through a circulating shear pump, wherein the shear rate is 160s-1And the shearing and stirring time is 1.8 hours, so that the foamless cleaning agent is obtained.
Example 2
The foamless cleaning agent comprises 7.5kg of coconut diethanolamide, 10kg of n-decyl glucoside, 0.6kg of polydimethylsiloxane, 2kg of oleic hydroxyethyl imidazoline, 0.22kg of isothiazolinone, 9kg of potassium acetate, 0.35kg of xanthan gum, 42kg of paraffin oil and 35kg of water.
The preparation method of the foamless cleaning agent of the embodiment comprises the following steps:
(1) weighing the components according to the weight for later use;
(2) putting the weighed water into a stirring kettle, adding the weighed potassium acetate, uniformly stirring, and fully dissolving to obtain a potassium acetate aqueous solution for later use;
(3) under the condition of stirring, adding the weighed xanthan gum into a potassium acetate aqueous solution, and heating a stirring kettle to 45 ℃;
(4) putting the solution heated in the step (3) into a circulating shearing kettle for shearing, wherein the shearing rate is 175s-1Obtaining a homogeneous liquid, and closing the shear pump when the apparent viscosity of the homogeneous liquid is 45mpa · s at the temperature of 30 ℃;
(5) putting the homogeneous liquid into a stirring kettle, and sequentially adding the coconut diethanolamide, n-decyl glucoside, polydimethylsiloxane, oleic hydroxyethyl imidazoline and isothiazolinone for standby in the stirring kettle under the stirring state, and fully stirring at the stirring speed of 190rpm for 30 min;
(6) under the condition of stirring, slowly adding paraffin oil into the stirring kettle at a constant speed through a circulating shear pump, wherein the shear rate is 170s-1And shearing and stirring for 2.0 hours to obtain the foamless cleaning agent.
Example 3
The foamless cleaning agent comprises 10kg of coconut diethanolamide, 15kg of n-decyl glucoside, 1kg of polydimethylsiloxane, 3kg of oleic hydroxyethyl imidazoline, 0.4kg of isothiazolinone, 11kg of potassium acetate, 0.4kg of xanthan gum, 55kg of paraffin oil and 40kg of water.
The preparation method of the foamless cleaning agent of the embodiment comprises the following steps:
(1) weighing the components according to the weight for later use;
(2) putting the weighed water into a stirring kettle, adding the weighed potassium acetate, uniformly stirring, and fully dissolving to obtain a potassium acetate aqueous solution for later use;
(3) under the condition of stirring, adding the weighed xanthan gum into a potassium acetate aqueous solution, and heating a stirring kettle to 50 ℃;
(4) putting the solution heated in the step (3) into a circulating shearing kettle for shearing, wherein the shearing rate is 200s-1Obtaining homogeneous liquid, and closing the shear pump when the apparent viscosity of the homogeneous liquid is 50mpa · s at the temperature of 30 ℃;
(5) putting the homogeneous liquid into a stirring kettle, and sequentially adding the coconut diethanolamide, n-decyl glucoside, polydimethylsiloxane, oleic hydroxyethyl imidazoline and isothiazolinone for standby in the stirring kettle under the stirring state, and fully stirring at the stirring speed of 200rpm for 35 min;
(6) under the condition of stirring, slowly adding paraffin oil into the stirring kettle at a constant speed through a circulating shear pump, wherein the shear rate is 180s-1The shearing and stirring time is 2.2 hours, and the non-foaming type is obtainedAnd (4) cleaning agent.
Test example 1
The foamability, oil evolution time, water evolution time, corrosivity, shale recovery rate, flash point and pour point of the foamless detergents prepared in examples 1 to 3 were respectively characterized, and the results are shown in Table 2, and the measurement methods are as follows.
1. Method for measuring foaming ratio
Respectively measuring 400ml of the cleaning agent prepared in the embodiment 1-3 in a high-speed stirring cup, and stirring for 5 minutes at a high speed by a high-frequency stirrer under the condition of 11000 +/-300 revolutions per minute; pouring the high stirring cup sample into a 1000mL measuring cylinder within 10 seconds, and reading the volume within 10 seconds and recording as V; the foaming ratio D was calculated by the formula (1).
Figure BDA0001767020220000091
2. Oil separating time measuring method
Measuring 400ml of high-speed stirring cups of the cleaning solution prepared in the embodiment 1-3 respectively, and stirring for 10 minutes at a high speed by a high-frequency stirrer under the condition of 11000 +/-300 revolutions per minute; the high stir cup sample was poured into a 1000mL graduated cylinder and timing was started and the time at which it started to separate oil, i.e. the time at which oil and water separated, was recorded.
The stability of the cleaning agent can be judged through the oil separating time, and the stability is better when the oil separating time is longer, and the stability is poorer when the oil separating time is shorter.
3. Method for measuring water separating time
3.1 preparation of Standard test solution
Measuring 320ml 0# diesel oil, adding 12.0g organic soil under the stirring of 11000 +/-300 rpm, adding 16.0ml Span-80 by using an injector without stopping a stirrer, adding 4.0g quick lime, and stirring at high speed for 10 min. Slowly adding 80ml of calcium chloride brine with the concentration of calcium chloride of 25% without stopping the stirring machine, adding 24g of sulfonated asphalt, and stirring at high speed for 30 min; testing the demulsification voltage at room temperature, wherein the demulsification voltage is required to be more than 400V; if the demulsification voltage is lower than 400V, the addition of Span-80 is increased to be more than 400V.
3.2 preparation of sample slurries
Three portions of 80ml clear water are respectively measured and added into a beaker, 4.0ml of the cleaning agent prepared in the embodiment 1-3 is added under the stirring of the load of 1000 +/-300 rpm, the stirrer is not stopped, 20ml of standard test solution is continuously measured and added into the beaker, and the mixture is stirred for 1 minute at a low speed.
3.3 time to separate Water
Pouring the 3.2 sample into a 100ml measuring cylinder, and measuring the time for separating out 20% clear water (16ml) to obtain the water separating-out time.
The dissolving and dispersing capacity of the cleaning agent on the residue of the oil-based drilling fluid can be judged through the water separating time, and experimental findings and application show that the technical requirements of field application of an oil field can be met when the water separating time is more than 2 min.
4. Determination of degree of corrosion
4.1 preparation of test Steel sheet
Under the condition of drying, selecting a No. 10 steel sheet with the thickness of 50mm multiplied by 25mm as a test steel sheet, and polishing two surfaces and edges of the test steel sheet to be bright by using sand paper or abrasive cloth; a40 mm by 20mm square frame is carved in the center of a No. 10 standard steel sheet with the thickness of 50mm by 25mm, 50 squares with the thickness of 4mm by 4mm are carved in the square frame, and the width of a grid scribing line is not more than 0.1 mm. The test steel sheet is immersed in absolute ethyl alcohol, clamped by tweezers, cleaned by absorbent cotton, taken out and air-dried.
4.2 evaluation of degree of Corrosion
The prepared test steel sheets in 4.1 are respectively immersed in the bubble-free type oil stain cleaning agent prepared in the embodiment 1-3, a group of parallel tests are carried out by using clean water, after the test steel sheets are placed at room temperature for 24 hours, the test steel sheets are taken out to observe the corrosion condition of the surfaces of the test steel sheets, and the evaluation standard is shown in the table 1.
TABLE 1
Number of rusty lattice Degree of staining (%)
0 0
1-5 2-10
6-10 12-20
11-25 22-50
26-50 52-100
5. Shale recovery rate determination
5.1 preparation of test shale granules
And (3) passing the crushed shale particles through a standard sieve with the size of 5-10 meshes, and selecting the shale particles with the particle size of 5-10 meshes as a test sample.
5.2 shale recovery evaluation experiment
Respectively weighing 300mL of the foamless oil stain cleaning agent prepared in the examples 1-3 into a high-temperature aging kettle, weighing 30g of 5.1 medium shale particles, pouring the particles into the aging kettle, and slightly and uniformly stirring the particles by using a glass rod to obtain experimental slurry; rolling the experimental slurry at 100 ℃ for 16 hours, taking out the experimental slurry, passing the experimental slurry through a 100-mesh screen, and washing the screen and the surfaces of shale particles clean by using clear water; placing shale particles in a 100-mesh sieve in a constant-temperature drying box, drying at the constant temperature of 105 +/-3 ℃ for 4 hours, taking out the shale particles, placing the shale particles in a drying dish, cooling for 30 minutes, and weighing the mass of the shale particles, wherein the mass is marked as M; shale recovery was calculated using equation (2):
Figure BDA0001767020220000111
6. flash point determination
The open flash point of the test specimens is specified in GB/T3536-2008.
7. Pour point determination
The pour point of the test specimen is specified with reference to GB/T3535-2006.
TABLE 2
Figure BDA0001767020220000121
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims (9)

1. The foamless cleaning agent is characterized by comprising, by weight, 5-10 parts of coconut diethanolamide, 5-15 parts of n-decyl glucoside, 0.3-1 part of polydimethylsiloxane, 1-3 parts of oleic hydroxyethyl imidazoline, 0.05-0.4 part of isothiazolinone, 7-11 parts of potassium acetate, 0.3-0.4 part of xanthan gum, 30-55 parts of paraffin oil and 30-40 parts of water.
2. The foamless detergent as claimed in claim 1, wherein said detergent comprises, in parts by weight, cocodiethanolamide 7.5 parts, n-decyl glucoside 10 parts, polydimethylsiloxane 0.6 parts, oleic hydroxyethyl imidazoline 2 parts, isothiazolinone 0.22 parts, potassium acetate 9 parts, xanthan gum 0.35 parts, paraffin oil 42 parts, and water 35 parts.
3. A method for preparing the foamless detergent as claimed in claim 1 or 2, which comprises the steps of:
(1) weighing the components according to the weight for later use;
(2) putting the weighed water into a stirring kettle, adding the weighed potassium acetate, uniformly stirring, and fully dissolving to obtain a potassium acetate aqueous solution for later use;
(3) under the condition of stirring, adding the weighed xanthan gum into a potassium acetate aqueous solution, and heating a stirring kettle;
(4) putting the solution heated in the step (3) into a circulating shearing kettle for shearing to obtain homogeneous liquid, and closing a shearing pump;
(5) putting the homogeneous liquid into a stirring kettle, and sequentially adding the coconut diethanolamide, n-decyl glucoside, polydimethylsiloxane, oleic hydroxyethyl imidazoline and isothiazolinone for standby in the stirring kettle under the stirring state, and fully stirring;
(6) and slowly adding paraffin oil into the stirring kettle at a constant speed through a circulating shear pump under the condition of stirring to obtain the foamless cleaning agent.
4. The method for producing a foam-free cleaning agent according to claim 3, wherein the heating temperature in the step (3) is 40 to 50 ℃.
5. The method for producing a foamless detergent as claimed in claim 3 or 4, wherein said homogeneous liquid in step (4) has an apparent viscosity of 35 to 50 mpa-s at 30 ℃.
6. The method for preparing a foam-free cleaning agent as claimed in claim 3, wherein the shear rate in the step (4) is 150-200s-1
7. The method for preparing a foamless detergent as claimed in claim 3, wherein the stirring speed in step (5) is 180-200rpm and the stirring time is 25-35 min.
8. The method for preparing a foam-free cleaning agent as claimed in claim 3, wherein the shear rate in step (6) is 160-180s-1The shearing and stirring time is 1.8-2.2 hours.
9. Use of a non-foaming cleaner according to claim 1 or 2 for cleaning oil-based drilling fluid residues.
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USH1147H (en) * 1990-12-28 1993-03-02 Method of inhibiting corrosion in oil field produced fluids
US7309684B2 (en) * 2005-05-12 2007-12-18 The Lubrizol Corporation Oil-in-water emulsified remover comprising an ethoxylated alcohol surfactant
WO2008006677A1 (en) * 2006-07-13 2008-01-17 L'oreal Fluid cosmetic composition with a water-soluble heat-induced gelling polymer, a continuous aqueous phase, an oily phase and organic uv-screening agent
CN100513509C (en) * 2007-06-20 2009-07-15 中国石油天然气股份有限公司 Non-pollution well detergent and method of producing the same
CN101362942B (en) * 2008-09-26 2011-09-28 大庆石油管理局 Formation opener agent for low permeable reservoir of oilfield
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CN106634913B (en) * 2016-11-18 2019-09-03 广汉市福客科技有限公司 A kind of oil base drilling fluid cleaning agent, preparation method and evaluation method

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