CN109722273B - Produced liquid treating agent and application thereof - Google Patents
Produced liquid treating agent and application thereof Download PDFInfo
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- CN109722273B CN109722273B CN201711042994.3A CN201711042994A CN109722273B CN 109722273 B CN109722273 B CN 109722273B CN 201711042994 A CN201711042994 A CN 201711042994A CN 109722273 B CN109722273 B CN 109722273B
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Abstract
The invention discloses a produced liquid treating agent and application thereof, and belongs to the technical field of oil extraction engineering. The produced fluid treating agent comprises a degrading agent and a demulsifier; the degradation agent comprises the following components in percentage by mass: 80-85% of potassium persulfate, 5-10% of copper chloride and the balance of water; the demulsifier comprises the following components in percentage by mass: 45-65% of branched polyoxypropylene and polyoxyethylene block polyether taking polyethylene polyamine as an initiator, 20-30% of p-dodecanoylphenol amine polyether and the balance of water and xylene, wherein the mass ratio of the water to the xylene is 1 (0.9-1.1); the p-dodecanoylphenol amine polyether is prepared by the following preparation method: taking phenol, pyridine and dodecanoyl chloride as raw materials, and taking aluminum chloride as a catalyst to carry out reaction to obtain p-dodecanoyl phenol; p-dodecanoylphenol, ethylenediamine and formaldehyde are used as raw materials to react to obtain p-dodecanoylphenol amine resin; p-dodecanoylphenol amine resin, sodium hydroxide, propylene oxide and ethylene oxide are used as raw materials to react to obtain the p-dodecanoylphenol amine polyether.
Description
Technical Field
The invention relates to the technical field of oil extraction engineering, in particular to a produced liquid treating agent and application thereof.
Background
The ternary combination flooding technology is a technology of mixing alkali, surfactant and polymer in certain proportion and injecting the mixture into stratum to expand swept volume and raise recovery ratio. At present, as the oil field enters the later development stage, the ternary combination flooding technology is generally adopted to improve the recovery ratio of the oil field. However, the viscosity of produced liquid is increased, the crude oil is emulsified seriously, and an oil-water separation interface is unclear, so that the natural settling separation speed of oil and water is reduced, and the dehydration of the crude oil and the treatment of oily sewage are difficult. Therefore, it is necessary to provide a demulsifier that can reduce the viscosity of produced fluid and is advantageous for oil-water separation.
The prior art provides a demulsifier, which takes long-carbon-chain alcohol as an initiator and an alcohol block polyether demulsifier with a carbon chain length of 12-15. The demulsifier has good demulsification effect on oil and water of produced fluid after conventional water flooding, and when the produced fluid contains polymer and surfactant, the demulsification effect is greatly reduced. For example, indoor experiments of the lauryl alcohol block polyether demulsifier produced by Jiangsu Haian petrochemical industry show that when the produced fluid does not contain polymers and surfactants, the dehydration rate of the produced fluid can reach more than 85 percent, and when the total content of the polymers and the surfactants in the produced fluid exceeds 50mg/L, the dehydration rate of the produced fluid is reduced to below 50 percent.
The inventor finds that the prior art has at least the following problems:
the demulsifier provided by the prior art has poor broad-spectrum adaptability, and the demulsification effect on produced liquid cannot meet the required standard.
Disclosure of Invention
In order to solve the problems, the embodiment of the invention provides a produced liquid treating agent and application thereof. The technical scheme is as follows:
in one aspect, a production fluid treatment agent is provided, the production fluid treatment agent comprising a degrading agent and a demulsifying agent;
the degradation agent comprises the following components in percentage by mass: 80-85% of potassium persulfate, 5-10% of copper chloride and the balance of water;
the demulsifier comprises the following components in percentage by mass: 45-65% of branched polyoxypropylene and polyoxyethylene block polyether taking polyethylene polyamine as an initiator, 20-30% of p-dodecanoylphenol amine polyether and the balance of water and xylene, wherein the mass ratio of the water to the xylene is 1 (0.9-1.1);
the p-dodecanoylphenol amine polyether is prepared by the following preparation method:
taking phenol and dodecanoyl chloride as raw materials, pyridine as an acid binding agent and aluminum chloride as a catalyst, and reacting to obtain p-dodecanoyl phenol, wherein the molar ratio of the phenol to the pyridine to the dodecanoyl chloride to the aluminum chloride is (0.8-1): (0.3-0.5): (1-1.2): 0.05-0.08);
reacting the p-dodecanoylphenol, ethylenediamine and formaldehyde as raw materials to obtain p-dodecanoylphenol amine resin, wherein the molar ratio of the p-dodecanoylphenol, the ethylenediamine and the formaldehyde is (2.9-3.1) - (1.9-2.1) - (3.9-4.1);
the p-dodecanoylphenol amine polyether is obtained by reacting the p-dodecanoylphenol amine resin, sodium hydroxide, propylene oxide and ethylene oxide serving as raw materials, wherein the molar ratio of the p-dodecanoylphenol amine resin to the sodium hydroxide to the propylene oxide to the ethylene oxide is 1:0.5 (40-80) to (50-100).
Optionally, the branched polyoxypropylene and polyoxyethylene block polyether using polyethylene polyamine as an initiator is AE 10071.
Alternatively, the p-dodecanoyl phenol is prepared by the following method:
adding phenol, pyridine and a solvent into a reaction kettle;
dropwise adding lauroyl chloride into the reaction kettle at a first preset temperature, and stirring for a first preset time;
and adding aluminum chloride into the reaction kettle at the first preset temperature, stirring for a second preset time, and carrying out substitution reaction to obtain the p-dodecanoylphenol.
Optionally, the solvent is dichloromethane, chloroform or carbon tetrachloride.
Optionally, the first preset temperature is 20-30 ℃, and the first preset time is 1.4-1.6 hours;
the second preset time is 1.9-2.1 h.
Optionally, the p-dodecanoylphenol amine resin is prepared by the following preparation method:
adding ethylenediamine into the reaction kettle containing the p-dodecanoylphenol, introducing nitrogen gas, and heating to a second preset temperature;
dropwise adding formaldehyde into the reaction kettle, heating to a third preset temperature, reducing the pressure to a first preset pressure, and carrying out polymerization reaction;
and after the polymerization reaction is finished, vacuumizing for a third preset time at the third preset temperature and the first preset pressure, and cooling to the second preset temperature to obtain the p-dodecanoylphenol amine resin.
Optionally, the second preset temperature is 90-100 ℃;
the third preset temperature is 120-150 ℃, and the first preset pressure is 1.4-1.6 KPa;
the third preset time is 0.9-1.1 h.
Optionally, the p-dodecanoylphenol amine polyether is prepared by the following preparation method:
adding sodium hydroxide into the reaction kettle containing the p-dodecanoylphenol amine resin, introducing nitrogen gas until the pressure in the reaction kettle is increased to a second preset pressure, and heating to a fourth preset temperature;
adding epoxypropylene into the reaction kettle under the second preset pressure and the fourth preset temperature, and stirring for a fourth preset time;
and adding ethylene oxide into the reaction kettle under the second preset pressure and the fourth preset temperature, and stirring for a fifth preset time to obtain the p-dodecanoylphenol amine polyether.
Optionally, the second preset pressure is 0.2MPa to 0.4MPa, and the fourth preset temperature is 100 ℃ to 150 ℃;
the fourth preset time is 5-15 h;
the fifth preset time is 5-10 h.
In another aspect, there is provided a use of the produced fluid treating agent of the first aspect in demulsification treatment of oil field produced fluid;
the total concentration of the polymer and the surfactant in the oilfield produced fluid is greater than or equal to 30 mg/L.
Optionally, when the total concentration is lower than 50mg/L, the adding concentration of the used produced fluid treating agent is 30 mg/L-50 mg/L;
when the total concentration is more than 50mg/L and less than 100mg/L, the adding concentration is 50 mg/L-80 mg/L;
when the total concentration is more than 100mg/L, the adding concentration is 80 mg/L-200 mg/L;
wherein the mass of the degradation agent in the produced fluid treatment agent is 10-20% of the total mass of the polymer and the surfactant in the oilfield produced fluid.
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
according to the produced liquid treating agent provided by the embodiment of the invention, organic matters in the produced liquid are degraded by utilizing the oxidative degradation performance of potassium persulfate and copper chloride on the organic matters and the catalytic performance of high-valence metal ions, so that the viscosity of the produced liquid is reduced, an oil-water interface membrane is damaged, and the oil-water separation speed in the produced liquid is accelerated; and secondly, the water-soluble demulsifier (namely, branched polyoxypropylene and polyoxyethylene block polyether taking polyethylene polyamine as an initiator) and the oil-soluble demulsifier (namely, p-dodecanoylphenol amine polyether) are compounded for use, so that the demulsifier has better broad spectrum, the oil-water transition zone of produced liquid is reduced, the oil-water separation of the produced liquid is facilitated, and the treated sewage can easily reach the standard of oilfield reinjection sewage.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
The embodiment of the invention provides a produced fluid treating agent, which comprises a degrading agent and a demulsifier; wherein the degradation agent comprises the following components in percentage by mass: 80-85% of potassium persulfate and 5-10% of copper chloride; the demulsifier comprises the following components in percentage by mass: 45-65% of branched polyoxypropylene and polyoxyethylene block polyether taking polyethylene polyamine as an initiator, 20-30% of p-dodecanoylphenol amine polyether, and the balance of water and xylene, wherein the mass ratio of the water to the xylene is 1 (0.9-1.1). Further, the p-dodecanoylphenol amine polyether is obtained by the following preparation method: taking phenol and p-dodecanoyl chloride as raw materials, pyridine as an acid binding agent and aluminum chloride as a catalyst, and reacting to obtain p-dodecanoyl phenol, wherein the molar ratio of the phenol to the pyridine to the dodecanoyl chloride to the aluminum chloride is (0.8-1): 0.3-0.5): 1-1.2): 0.05-0.08; p-dodecanoylphenol, ethylenediamine and formaldehyde are used as raw materials to react to obtain p-dodecanoylphenol amine resin, wherein the molar ratio of the p-dodecanoylphenol to the ethylenediamine to the formaldehyde is (2.9-3.1) to (1.9-2.1) to (3.9-4.1); the method comprises the step of reacting p-dodecanoylphenol amine resin, sodium hydroxide, propylene oxide and ethylene oxide serving as raw materials to obtain the dodecanoylphenol amine polyether, wherein the molar ratio of the p-dodecanoylphenol amine resin to the sodium hydroxide to the propylene oxide to the ethylene oxide is 1:0.5 (40-80) to (50-100).
Branched polyoxypropylene and polyoxyethylene block polyethers starting from polyethylene polyamines are common in the art, and for example, the CN102876358A patent discloses block polyethers of this type, or AE10071 demulsifiers, which are commercially available and sold by Shandong Wan and eco-friendly companies.
Among them, branched polyoxypropylene, polyoxyethylene block polyethers, in which polyethylene polyamine is the initiator, are well known to those skilled in the art and are commonly used as water-soluble demulsifiers; the benzene ring in the p-dodecanoylphenol amine polyether and the long carbon chain structure linked by the benzene ring make the polymer molecule more lipophilic than hydrophilic, so the p-dodecanoylphenol amine polyether in the embodiment of the invention can be used as an oil-soluble demulsifier.
In view of the oleophylicity and hydrophilicity of the branched polyoxypropylene, polyoxyethylene block polyether and dodecanol phenol amine polyether which take the polyethylene polyamine as the initiator, the produced fluid treating agent provided by the embodiment of the invention firstly degrades the organic matters in the produced fluid by utilizing the oxidative degradation performance of potassium persulfate and copper chloride on the organic matters and the catalytic performance of high-valence metal ions, reduces the viscosity of the produced fluid, destroys an oil-water interface film, and accelerates the oil-water separation speed in the produced fluid; and secondly, the water-soluble demulsifier (namely, branched polyoxypropylene and polyoxyethylene block polyether taking polyethylene polyamine as an initiator) and the oil-soluble demulsifier (namely, p-dodecanoylphenol amine polyether) are compounded for use, so that the demulsifier has better broad spectrum, the oil-water transition zone of produced liquid is reduced, the oil-water separation of the produced liquid is facilitated, and the treated sewage can easily reach the standard of oilfield reinjection sewage.
As mentioned above, the degradation agent in the produced liquid treatment agent mainly degrades organic matters in the produced liquid. Wherein the mass percent of the potassium persulfate in the degradation agent is 80-85%, for example, 80%, 81%, 82%, 83%, 84%, 85% and the like; the mass percent of the copper chloride is 5-10%, for example, 5%, 6%, 7%, 8%, 9%, 10%, etc.; the balance being water.
It is understood that the water may be deionized, distilled, purified or tap water.
In addition, the demulsifier in the produced fluid processor can reduce the oil-water transition zone in the produced fluid. Wherein the mass percent of the branched polyoxypropylene block polyether and the polyoxyethylene block polyether which take the polyethylene polyamine as the initiator in the demulsifier is 45-65%, for example, 45%, 50%, 55%, 60%, 65%, and the like; the mass percentage of the p-lauroyl phenol amine polyether is 20%, 22%, 24%, 26%, 28%, 30% and the like; the balance of water and dimethylbenzene, and the mass ratio of the water to the dimethylbenzene can be set to be 1.0:0.9, 1.0:1.0 or 1.1:1.0 and the like.
Wherein, the branched polyoxypropylene block polyether and the polyoxyethylene block polyether which take the polyethylene polyamine as the initiator in the demulsifier are polyether demulsifiers, belonging to water-soluble demulsifiers. The polyether demulsifier is divided into various types according to the proportion of propylene oxide and ethylene oxide in a molecular midblock, for example, types of AE121, AE6952, AE1910, AE8051, AE7921, AE9901, AE10071 and the like. "AE" in these models refers to the two-block structure of propylene oxide and ethylene oxide after amino group, and the number after AE "represents the molecular ratio of propylene oxide and ethylene oxide participating in the block in the polyether demulsifier molecule using ethylenediamine as initiator, for example, the molecular ratio of propylene oxide and ethylene oxide in the polyether demulsifier of AE1910 is 19: 10.
Preferably, the branched polyoxypropylene and polyoxyethylene block polyether taking polyethylene polyamine as an initiator in the embodiment of the invention is AE10071, and the polyether demulsifier can effectively reduce an oil-water transition zone in produced liquid and is convenient for oil-water separation.
Further, the p-dodecanoylphenol amine polyether is prepared by the following preparation method:
in step 101, phenol and dodecanoyl chloride are used as raw materials, pyridine is used as an acid binding agent, and aluminum chloride is used as a catalyst to perform reaction, so that p-dodecanoyl phenol is obtained, wherein the molar ratio of the phenol, the pyridine, the dodecanoyl chloride and the aluminum chloride is (0.8-1): 0.3-0.5): 1-1.2): 0.05-0.08.
Wherein the molar ratio of phenol, pyridine, dodecanoyl chloride and aluminum chloride is (0.8-1): (0.3-0.5): 1-1.2): 0.05-0.08, and for example, the ratio can be set to 0.8:0.3:1:0.05, 0.9:0.4:1.1:0.05, 1.0:0.5:1.2:0.07 or 1:0.5:1.2: 0.08.
In this step 101, the p-dodecanoylphenol has the formula C18H28O2The molecular structure is
And a molar mass of 276.
As an embodiment, the step 101 may include:
in step 1011, phenol, pyridine and a solvent are added to the reaction vessel.
Wherein, the reaction kettle is a reaction vessel with heating and pressurizing functions.
In addition, the solvent mainly plays a role of dissolution and does not participate in chemical reactions. Alternatively, the solvent may be selected from dichloromethane, chloroform or carbon tetrachloride. Such types of solvents have the advantages of adequate dissolution and low boiling points.
It should be noted that the amount (volume) of the solvent added may be one half of the total volume of each reactant.
In step 1012, at a first predetermined temperature, dodecanoyl chloride is added dropwise into the reaction vessel, and the mixture is stirred for a first predetermined time to perform an acylation reaction.
Specifically, at a first preset temperature, adding dropwise dodecanoyl chloride into the reaction kettle while stirring; when the dropwise addition is completed, stirring is continued for a first preset time.
Optionally, the first predetermined temperature is 20 ℃ to 30 ℃, for example, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃ or 30 ℃ can be set. It is noted that when the indoor environment is 20-30 ℃, the reaction kettle does not need to be heated before the dodecayl chloride is dripped; when the indoor environment is less than 20-30 ℃, the reaction kettle needs to be heated before the dodecanoyl chloride is dripped.
Optionally, the first preset time is 1.4h to 1.6h, for example, 1.4h, 1.5h, or 1.6h may be set. Such setting of the first preset time may increase the reaction rate.
In step 1013, aluminum chloride is added to the reaction kettle at a first predetermined temperature and stirred for a second predetermined time in AlCl3Molecular rearrangement reaction is carried out under the catalysis, and the p-dodecanoylphenol is mainly obtained.
Specifically, at a first preset temperature, adding aluminum chloride into a reaction kettle while stirring; and then, after the aluminum chloride is added, continuously stirring for a second preset time to perform substitution reaction, thereby obtaining the p-dodecanoylphenol.
In order to ensure that phenol and pyridine are completely reacted, a large amount of dodecanoyl chloride is added in the embodiment of the invention, and after the reaction is finished, the reaction kettle not only contains p-dodecanoyl phenol, but also contains a small amount of dodecanoyl chloride which does not participate in the reaction, a solvent and aluminum chloride. Therefore, in order to obtain dodecanoyl phenol, after the reaction is completed, the solvent in the reaction vessel can be removed by reduced pressure distillation or reduced pressure rotary evaporation, and the unreacted portion of dodecanoyl chloride can be removed. The principle is as follows: by reducing the pressure in the reaction kettle, the boiling points of the solvent and the dodecanoyl chloride can be reduced, and the solvent in the reaction kettle and the unreacted part of the dodecanoyl chloride can be volatilized out of the reaction kettle.
Since the amount of aluminum chloride added to the reaction vessel is extremely small, it is not necessary to remove the aluminum chloride in the reaction vessel.
Optionally, the second preset time is 1.9h to 2.1h, for example, may be set to 1.9h, 2.0h, or 2.1 h. The second preset time is set in such a way that phenol, pyridine dodecanoyl chloride and aluminum chloride can be fully reacted, and the reaction rate is improved.
In step 102, p-dodecanoylphenol, ethylenediamine and formaldehyde are used as raw materials to react to obtain p-dodecanoylphenol amine resin, wherein the molar ratio of p-dodecanoylphenol, ethylenediamine and formaldehyde is (2.9-3.1): (1.9-2.1): (3.9-4.1).
Specifically, the step 102 is mainly to obtain the p-dodecanoylphenol amine resin by polymerizing p-dodecanoylphenol, ethylenediamine and formaldehyde.
Wherein, the molar ratio of the p-dodecanoylphenol, the ethylenediamine and the formaldehyde is (2.9-3.1): (1.9-2.1): 3.9-4.1, for example, the molar ratio can be set to 2.9:1.9:3.9, 3:2:4 or 3.1:2.1: 4.1.
In addition, the chemical formula C of the p-dodecanoylphenol amine resin obtained in the step 10222n+24N2n+4O2n+2H38n+46The value of n is 0-2; has a molecular structure of
And a molar mass of 422 to 1146.
The value of n is related to the concentration, mass and reaction conditions of the reactants, and the molar mass of the dodecanoylphenol amine resin can be obtained by performing experiments, and the means for obtaining the molar mass is well known to those skilled in the art and will not be described here.
As an embodiment, the step 102 further includes:
in step 1021, ethylene diamine is added to the reaction vessel containing the p-dodecanoylphenol while nitrogen is introduced, and the reaction vessel is heated to a second predetermined temperature.
Specifically, at a first preset temperature, adding ethylenediamine into a reaction kettle containing p-dodecanoylphenol, and introducing nitrogen into the reaction kettle at the same time until all air in the reaction kettle is exhausted; and then heating to a second preset temperature.
Optionally, the second predetermined temperature in step 1021 is 90-100 ℃, for example, 90 ℃, 92 ℃, 94 ℃, 96 ℃, 98 ℃, or 100 ℃.
In step 1022, formaldehyde is added dropwise to the reaction kettle, and the mixture is heated to a third preset temperature, and then decompressed to a first preset pressure, so as to perform a polymerization reaction.
Specifically, formaldehyde is dripped into the reaction kettle at a second preset temperature; and then heating the reaction kettle to a third preset temperature, and reducing the internal pressure of the reaction kettle to the first preset pressure, so that the formaldehyde, the ethylenediamine and the p-dodecanoylphenol are subjected to polymerization reaction under the conditions of the first preset pressure and the third preset temperature.
Optionally, the third preset temperature in step 1022 is 120 ℃ to 150 ℃, for example, it may be set to 120 ℃, 130 ℃, 140 ℃ or 130 ℃, etc.; the first predetermined pressure is 1.4KPa to 1.6KPa, and for example, may be set to 1.4KPa, 1.5KPa, or 1.6 KPa. The third preset temperature and the first preset pressure are set in this way, so that the polymerization reaction of formaldehyde, ethylenediamine and p-dodecanoylphenol can be ensured.
In order to ensure the completion of the reaction in step 1022, the reaction kettle may be left standing for 2 to 3 hours, for example, 2 hours, 2.5 hours, or 3 hours without any treatment after the formaldehyde is added dropwise, so that the p-dodecanoylphenol, ethylenediamine, and formaldehyde may be sufficiently reacted.
In step 1023, after the polymerization reaction is finished, vacuumizing for a third preset time at a third preset temperature and a first preset pressure, and cooling to a second preset temperature to obtain the p-dodecanoylphenol amine resin.
Specifically, the reaction kettle is vacuumized for a third preset time at a third preset temperature and a first preset pressure, and unreacted reactants (ethylenediamine or formaldehyde) in the reaction kettle are removed; and then, cooling the reaction kettle to a second preset temperature to obtain the p-dodecanoylphenol amine resin.
The principle of removing the unreacted reactants in the reaction vessel is as follows: the boiling points of the ethylenediamine and the formaldehyde can be reduced by reducing the pressure in the reaction kettle; and then the ethylenediamine or the formaldehyde in the reaction kettle can be volatilized out of the reaction kettle by heating the reaction kettle.
The third preset time in the step 1023 is 0.9h to 1.1h, for example, 0.9h, 1.0h, or 1.1 h. The third preset time is set in such a way, so that unreacted reactants in the reaction kettle can be fully removed.
In step 103, p-dodecanoylphenol amine resin, sodium hydroxide, propylene oxide and ethylene oxide are used as raw materials to react to obtain p-dodecanoylphenol amine polyether, wherein the molar ratio of the p-dodecanoylphenol amine resin to the sodium hydroxide to the propylene oxide to the ethylene oxide is 1:0.5 (40-80) to (50-100).
Specifically, p-dodecanoylphenol amine resin, sodium hydroxide, propylene oxide and ethylene oxide are subjected to polymerization reaction to obtain the p-dodecanoylphenol amine polyether.
Wherein, formula C of p-dodecanoylphenol amine polyether in the step 10322n+24+(n+1)(3x+2y)N2n+ 4O2n+2+(n+1)(x+y)H38n+46+(n+1)(6x+4y)N ranges from 0 to 2, and x and y ranges from 10 to 30; has a molecular structure of
And a molar mass of 1410 to 10326.
The values of n, x and y are related to the concentration, mass and reaction conditions of the reactants, and the molar mass of the dodecanoylphenol amine polyether can be obtained by performing experiments, and the obtaining means is well known to those skilled in the art and will not be described herein.
Optionally, the molar ratio of the diacylphenol amine resin, the sodium hydroxide, the propylene oxide and the ethylene oxide is 1:0.5 (40-80): 50-100, and for example, the molar ratio may be set to 1:0.5:40:50, 1:0.5:50:60, 1:0.5:60:70, 1:0.5:70:80, 1:0.5:80:90 or 1:0.5:80:100, etc.
As an implementation method, the step 103 further includes:
in step 1031, sodium hydroxide is added to the reaction kettle containing the p-lauroyl phenol amine resin, and simultaneously nitrogen is introduced until the pressure in the reaction kettle is increased to a second preset pressure.
Specifically, at a second preset temperature, adding sodium hydroxide into a reaction kettle containing the p-dodecanoylphenol amine resin, and introducing nitrogen into the reaction kettle until the internal pressure of the reaction kettle is increased to a second preset pressure; and then, heating the reaction kettle to a fourth preset temperature.
Optionally, the second preset pressure is 0.2MPa to 0.4MPa, for example, 0.2MPa, 0.3MPa or 0.4 MPa; the fourth predetermined temperature is 100 ℃ to 150 ℃, and can be set to 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃ or 150 ℃, for example. The second preset pressure and the fourth preset temperature are set in such a way, so that polymerization reaction of propylene oxide and ethylene oxide in subsequent steps after the lauroyl phenol amine resin and the sodium hydroxide can be guaranteed.
In step 1032, the epoxypropylene is added to the reaction kettle at a second predetermined pressure and a fourth predetermined temperature, and stirred for a fourth predetermined time.
Specifically, firstly, adding epoxypropylene into a reaction kettle under a second preset pressure and a fourth preset temperature; thereafter, stirring is performed for a fourth preset time.
Optionally, the fourth preset time is 5h to 15h, for example, 5h, 10h, or 15h may be set. The fourth preset time is set in this way, so that complete reaction of the dodecanoylphenol amine resin, the sodium hydroxide, the epoxypropylene and the epoxyethylene in the subsequent steps can be ensured.
In step 1033, ethylene oxide is added to the reactor at a second predetermined pressure and a fourth predetermined temperature, and stirred for a fifth predetermined time.
Specifically, at a second preset pressure and a fourth preset temperature, adding ethylene oxide into a reaction kettle; after that, the mixture is stirred for a fifth preset time.
Optionally, the fifth preset time is 5h to 10h, for example, 5h, 6h, 7h, 8h, 9h, or 10h may be set. The fifth preset time is set in such a way, so that complete reaction of the dodecanoylphenol amine resin, the sodium hydroxide, the propylene oxide and the ethylene oxide can be ensured.
The produced fluid treating agent provided by the embodiment of the invention can be applied to demulsification treatment of oil field produced fluid; and the total concentration of the polymer and the surfactant in the oilfield produced fluid is greater than or equal to 30 mg/L.
Optionally, when the total concentration (i.e. the total concentration of the polymer and the surfactant in the produced fluid) is lower than 50mg/L, the demulsifier in the used produced fluid treating agent is added to the produced fluid at a concentration of 30mg/L to 50 mg/L; when the total concentration is more than 50mg/L and less than 100mg/L, the concentration is 50 mg/L-80 mg/L; when the total concentration is more than 100mg/L, the concentration is 80 mg/L-200 mg/L; wherein the mass of the degradation agent in the used produced fluid treatment agent is 10-20% of the total mass of the polymer and the surfactant in the oilfield produced fluid.
It should be noted that the demulsifier addition concentration in the used production fluid treatment agent refers to the mass of demulsifier added per unit volume of production fluid.
According to the method, the produced fluid treating agents with different qualities are correspondingly added according to the total concentration of the polymer and the surfactant in the produced fluid, so that the purpose of reducing the adding amount of the demulsifier can be achieved on the premise of effectively demulsifying the produced fluid, and the treatment cost can be reduced.
When the produced fluid is demulsified, a degradation agent in the produced fluid treatment agent is added to the produced fluid at certain intervals (for example, 30-60 min), and then a demulsifier in the produced fluid treatment agent is added to the produced fluid.
As described above, the embodiment of the present invention illustrates the addition amount of the produced fluid treatment agent, which means that the addition amount of the degradation agent and the demulsifier in the produced fluid treatment agent is clear, for example, when demulsification treatment is performed on an oil field produced fluid with a capacity of 1L and a total concentration of the polymer and the surfactant of 100mg/L, since the total mass of the polymer and the surfactant in the oil field produced fluid is 100mg, the mass of the degradation agent is 10mg, which is 10% of the mass of the polymer and the surfactant in the oil field produced fluid, and in addition, since the total concentration of the polymer and the surfactant is within a range of 50 to 100mg/L, the addition concentration of the demulsifier in the produced fluid treatment agent used in the embodiment is 50mg/L, which is 50mg/L of the addition mass.
When the device is applied, a pipeline dosing mode is generally adopted, and a produced fluid treating agent is added into produced fluid by using dosing equipment. Wherein, the needed medicine adding equipment comprises a medicine adding tank, a metering pump, an auxiliary pipeline, a valve and the like. The steps of adding the produced fluid treating agent to the produced fluid may specifically be: firstly, installing dosing equipment consisting of a dosing tank, a metering pump, an auxiliary pipeline, a valve and the like at the outlet end of a three-phase separator, and then adding a degrading agent in produced liquid; and then, adding a demulsifier in the produced liquid treating agent through a metering pump, an auxiliary pipeline, a valve and the like of the settling tank.
The use conditions of the produced fluid treating agent are as follows: is suitable for produced liquid with the temperature of 40-90 ℃.
The present invention will be further described below by way of specific examples.
In the following examples, those whose operations are not subject to the conditions indicated, are carried out according to the conventional conditions or conditions recommended by the manufacturer. The raw materials are conventional products which can be obtained commercially by manufacturers and specifications.
Among them, potassium persulfate, copper chloride, xylene, phenol, pyridine, methylene chloride, dodecanoyl chloride, aluminum chloride, ethylenediamine, formaldehyde, sodium hydroxide, propylene oxide, and ethylene oxide were purchased from the Kemiou chemical reagent development center. Branched polyoxypropylene and polyoxyethylene block polyethers with polyethylene polyamines as initiators were purchased from Shandongwen and environmental protection and energy conservation Co.
Example 1
The embodiment provides a produced fluid treating agent, wherein the produced fluid comprises a degrading agent and a demulsifier; the degradation agent comprises the following components in percentage by mass: 80% of potassium persulfate, 10% of copper chloride and the balance of water; wherein, the demulsifier comprises the following components in percentage by mass: the polyethylene polyamine-based epoxy resin is prepared from 45% of branched polyoxypropylene block polyether and 45% of polyoxyethylene block polyether which are AE10071 and take polyethylene polyamine as an initiator, 20% of p-dodecanoylphenol amine polyether, and the balance of water and xylene, wherein the mass ratio of the water to the xylene is 1:1.
Further, the p-dodecanoylphenol amine polyether is obtained by the following preparation method:
sequentially adding phenol, pyridine and a dichloromethane solvent into a reaction kettle; dropwise adding lauroyl chloride into the reaction kettle at 25 ℃ while stirring; after the dropwise addition is finished, stirring is continued for 1.5 h; adding aluminum chloride into the reaction kettle at 25 ℃, stirring for 2 hours, and removing a dichloromethane solvent in the reaction kettle by using a reduced pressure rotary evaporation method to obtain the p-dodecanoylphenol. Wherein the molar ratio of phenol, pyridine, dichloromethane, dodecanoyl chloride to aluminum chloride is 0.8:0.3:1: 0.05.
Adding ethylenediamine into a reaction kettle containing p-dodecanoylphenol at 20 ℃, and introducing nitrogen at the same time until all air in the reaction kettle is exhausted, and heating to 95 ℃; then dripping formaldehyde into the reaction kettle at 95 ℃; then heating the reaction kettle to 120 ℃, and reducing the internal pressure of the reaction kettle to 1.5KPa, so that formaldehyde, ethylenediamine and p-dodecanoylphenol are subjected to polymerization reaction; after the reaction is finished, vacuumizing for 1h at 120 ℃ and under the pressure of 1.5KPa, and cooling to 95 ℃ to obtain the p-dodecanoylphenol amine resin. Wherein the molar mass ratio of the p-dodecanoylphenol, the ethylenediamine and the formaldehyde is 3:2: 4.
Firstly, adding sodium hydroxide into a reaction kettle containing p-lauroyl phenol amine resin at 95 ℃, and introducing nitrogen into the reaction kettle until the internal pressure is increased to 0.2 MPa; then, heating the reaction kettle to 120 ℃; adding epoxy propylene into the reaction kettle at the temperature of 120 ℃ under 0.2MPa, and stirring for 10 hours; adding ethylene oxide into the reaction kettle at the temperature of 120 ℃ under the pressure of 0.2MPa, and stirring for 10 hours to obtain the p-dodecanoylphenol amine polyether. Wherein the molar mass ratio of the p-dodecanoylphenol amine resin, the sodium hydroxide, the epoxypropylene and the epoxyethane is 1:0.5:40: 50.
Example 2
The embodiment provides a produced fluid treating agent, wherein the produced fluid comprises a degrading agent and a demulsifier; the degradation agent comprises the following components in percentage by mass: 85% of potassium persulfate, 10% of copper chloride and the balance of water; wherein, the demulsifier comprises the following components in percentage by mass: the polyethylene polyamine-based epoxy resin is prepared from 50% of branched polyoxypropylene block polyether and 50% of polyoxyethylene block polyether which are AE10071 and take polyethylene polyamine as an initiator, 30% of p-dodecanoylphenol amine polyether, and the balance of water and xylene, wherein the mass ratio of the water to the xylene is 1:1.
Further, the p-dodecanoylphenol amine polyether is obtained by the following preparation method:
sequentially adding phenol, pyridine and a dichloromethane solvent into a reaction kettle; dropwise adding lauroyl chloride into the reaction kettle at 20 ℃ while stirring; after the dropwise addition is finished, stirring is continued for 1.6 h; adding aluminum chloride into the reaction kettle at the temperature of 20 ℃, stirring for 2.1h, and removing a dichloromethane solvent in the reaction kettle by using a reduced pressure rotary evaporation method to obtain the p-dodecanoylphenol. Wherein the molar ratio of phenol, pyridine, dichloromethane, dodecanoyl chloride and aluminum chloride is 1:0.5:1.2: 0.07.
Adding ethylenediamine into a reaction kettle containing p-dodecanoylphenol at 20 ℃, and introducing nitrogen at the same time until all air in the reaction kettle is exhausted, and heating to 100 ℃; then, dropwise adding formaldehyde into the reaction kettle at 100 ℃; then heating the reaction kettle to 130 ℃, and reducing the internal pressure of the reaction kettle to 1.4KPa, so that formaldehyde, ethylenediamine and p-dodecanoylphenol are subjected to polymerization reaction; after the reaction is finished, vacuumizing for 1h at 130 ℃ and 1.4KPa, and cooling to 100 ℃ to obtain the p-dodecanoylphenol amine resin. Wherein the molar mass ratio of the dodecanoylphenol to the ethylenediamine to the formaldehyde is 2.9:2: 3.9.
Firstly, adding sodium hydroxide into a reaction kettle containing p-lauroyl phenol amine resin at 100 ℃, and introducing nitrogen into the reaction kettle until the internal pressure is increased to 0.3 MPa; then, heating the reaction kettle to 150 ℃; adding epoxy propylene into the reaction kettle at the temperature of 150 ℃ under the pressure of 0.3MPa, and stirring for 5 hours; adding ethylene oxide into the reaction kettle at the temperature of 150 ℃ under the pressure of 0.3MPa, and stirring for 8 hours to obtain the p-dodecanoylphenol amine polyether. Wherein the molar mass ratio of the p-dodecanoylphenol amine resin, the sodium hydroxide, the epoxypropylene and the epoxyethane is 1:0.5:60: 80.
Example 3
The embodiment provides a produced fluid treating agent, wherein the produced fluid comprises a degrading agent and a demulsifier; the degradation agent comprises the following components in percentage by mass: 85% of potassium persulfate, 5% of copper chloride and the balance of water; wherein, the demulsifier comprises the following components in percentage by mass: the polyethylene polyamine-based epoxy resin composition is prepared from 65% of branched polyoxypropylene block polyether and 65% of polyoxyethylene block polyether which are AE10071 and take polyethylene polyamine as an initiator, 20% of p-dodecanoylphenol amine polyether, and the balance of water and xylene, wherein the mass ratio of the water to the xylene is 1:1.
Further, the p-dodecanoylphenol amine polyether is obtained by the following preparation method:
sequentially adding phenol, pyridine and a dichloromethane solvent into a reaction kettle; dropwise adding lauroyl chloride into the reaction kettle at 30 ℃ while stirring; after the dropwise addition is finished, stirring is continued for 1.4 h; adding aluminum chloride into the reaction kettle at 30 ℃, stirring for 2 hours, and removing a dichloromethane solvent in the reaction kettle by using a reduced pressure rotary evaporation method to obtain the p-dodecanoylphenol. Wherein the molar ratio of phenol, pyridine, dichloromethane, dodecanoyl chloride and aluminum chloride is 1:0.5:1.2: 0.08.
Adding ethylenediamine into a reaction kettle containing p-dodecanoylphenol at 30 ℃, introducing nitrogen at the same time until all air in the reaction kettle is exhausted, and heating to 95 ℃; then dripping formaldehyde into the reaction kettle at 95 ℃; then heating the reaction kettle to 140 ℃, and reducing the internal pressure of the reaction kettle to 1.6KPa, so that formaldehyde, ethylenediamine and p-dodecanoylphenol are subjected to polymerization reaction; after the reaction is finished, vacuumizing for 1h at 140 ℃ and 1.6KPa, and cooling to 95 ℃ to obtain the p-dodecanoylphenol amine resin. Wherein the molar mass ratio of the p-dodecanoylphenol, the ethylenediamine and the formaldehyde is 2.9:2.1: 4.1.
Firstly, adding sodium hydroxide into a reaction kettle containing p-lauroyl phenol amine resin at 95 ℃, and introducing nitrogen into the reaction kettle until the internal pressure is increased to 0.4 MPa; then, heating the reaction kettle to 120 ℃; adding epoxypropylene into the reaction kettle at the temperature of 120 ℃ under the pressure of 0.4MPa, and stirring for 8 hours; adding ethylene oxide into the reaction kettle at the temperature of 120 ℃ under the pressure of 0.4MPa, and stirring for 8 hours to obtain the p-dodecanoylphenol amine polyether. Wherein the molar mass ratio of the p-dodecanoylphenol amine resin, the sodium hydroxide, the epoxypropylene and the epoxyethane is 1:0.5:80: 100.
Comparative example
This comparison example provides a demulsifier of type CY4, and the demulsifier of this type mainly comprises: the polysiloxane polyoxyethylene polyoxypropylene ether can be purchased from petrochemical engineering of Tiancheng province in Hebei province.
Application examples
This application example evaluates the effectiveness of the demulsifiers of type CY4 provided in examples 1-3 and the control. The demulsifiers of examples 1-3 and the control, model CY4, were selected as samples and numbered sequentially as No. 1, No. 2, No. 3, and No. 4.
On one hand, each sample is added into produced fluid with the same volume but different total concentrations of the polymer and the surfactant for demulsification treatment. And then measuring the thickness of an oil-water transition zone of the produced liquid corresponding to each sample, and the oil content and the water content of crude oil in water after the produced liquid is separated, wherein the results are shown in table 1.
TABLE 1
The total concentration in table 1 indicates the total concentration of the polymer and the surfactant.
As can be seen from Table 1, compared with the demulsifier provided by the prior art, the produced fluid treating agent provided by the embodiment of the invention has the advantages that the oil content in the water after the produced fluid is treated is averagely reduced by 39.05%, the water content of the crude oil is averagely reduced by 52.38%, and the thickness of the oil-water excess zone is reduced by 41.5%. Therefore, the produced liquid treating agent provided by the embodiment of the invention can reduce an oil-water transition zone and is beneficial to oil-water separation.
On the other hand, the above samples were subjected to demulsification performance evaluation tests in accordance with SY/T5281-2000 standards to obtain dehydration ratios corresponding to the respective samples, as shown in Table 2.
TABLE 2
In table 2, the total concentration of the polymer and the surfactant is shown as the total concentration.
As can be seen from table 2, the produced fluid treatment agent provided in the embodiment of the present invention has a better treatment performance on the produced crude oil emulsion containing an ASP ternary complex system (i.e., ternary complex flooding composed of alkali, surfactant, and polymer), and compared with the demulsifier provided in the prior art, the produced fluid treatment agent provided in the embodiment of the present invention can increase the final dehydration rate of crude oil treatment by 14.4% on average.
All the above optional technical solutions may be combined arbitrarily to form the optional embodiments of the present disclosure, and are not described herein again.
The above description is only exemplary of the present invention and should not be taken as limiting the scope of the present invention, as any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (11)
1. The produced fluid treating agent is characterized by comprising a degrading agent and a demulsifier;
the degradation agent comprises the following components in percentage by mass: 80-85% of potassium persulfate, 5-10% of copper chloride and the balance of water;
the demulsifier comprises the following components in percentage by mass: 45-65% of branched polyoxypropylene and polyoxyethylene block polyether taking polyethylene polyamine as an initiator, 20-30% of p-dodecanoylphenol amine polyether and the balance of water and xylene, wherein the mass ratio of the water to the xylene is 1 (0.9-1.1);
the p-dodecanoylphenol amine polyether is prepared by the following preparation method:
taking phenol and dodecanoyl chloride as raw materials, pyridine as an acid binding agent and aluminum chloride as a catalyst, and reacting to obtain p-dodecanoyl phenol, wherein the molar ratio of the phenol to the pyridine to the dodecanoyl chloride to the aluminum chloride is (0.8-1): (0.3-0.5): (1-1.2): 0.05-0.08);
reacting the p-dodecanoylphenol, ethylenediamine and formaldehyde as raw materials to obtain p-dodecanoylphenol amine resin, wherein the molar ratio of the p-dodecanoylphenol, the ethylenediamine and the formaldehyde is (2.9-3.1) - (1.9-2.1) - (3.9-4.1);
the p-dodecanoylphenol amine polyether is obtained by reacting the p-dodecanoylphenol amine resin, sodium hydroxide, propylene oxide and ethylene oxide serving as raw materials, wherein the molar ratio of the p-dodecanoylphenol amine resin to the sodium hydroxide to the propylene oxide to the ethylene oxide is 1:0.5 (40-80) to (50-100).
2. The production fluid treating agent according to claim 1, wherein the branched polyoxypropylene and polyoxyethylene block polyether using polyethylene polyamine as an initiator has a model number of AE 10071.
3. The production fluid treating agent according to claim 1, wherein the p-dodecanoylphenol is prepared by the following method:
adding phenol, pyridine and a solvent into a reaction kettle;
dropwise adding lauroyl chloride into the reaction kettle at a first preset temperature, and stirring for a first preset time;
and adding aluminum chloride into the reaction kettle at the first preset temperature, stirring for a second preset time, and carrying out substitution reaction to obtain the p-dodecanoylphenol.
4. The production fluid treatment agent of claim 3, wherein the solvent is dichloromethane, chloroform or carbon tetrachloride.
5. The produced fluid treating agent according to claim 3, wherein the first preset temperature is 20 ℃ to 30 ℃ and the first preset time is 1.4h to 1.6 h;
the second preset time is 1.9-2.1 h.
6. The production fluid treating agent according to claim 3, wherein the p-dodecanoylphenol amine resin is prepared by the following preparation method:
adding ethylenediamine into the reaction kettle containing the p-dodecanoylphenol, introducing nitrogen gas, and heating to a second preset temperature;
dropwise adding formaldehyde into the reaction kettle, heating to a third preset temperature, reducing the pressure to a first preset pressure, and carrying out polymerization reaction;
and after the polymerization reaction is finished, vacuumizing for a third preset time at the third preset temperature and the first preset pressure, and cooling to the second preset temperature to obtain the p-dodecanoylphenol amine resin.
7. The produced fluid treating agent according to claim 6, wherein the second predetermined temperature is 90 ℃ to 100 ℃;
the third preset temperature is 120-150 ℃, and the first preset pressure is 1.4-1.6 KPa;
the third preset time is 0.9-1.1 h.
8. The production fluid treating agent according to claim 6, wherein the p-dodecanoylphenol amine polyether is prepared by the following preparation method:
adding sodium hydroxide into the reaction kettle containing the p-dodecanoylphenol amine resin, introducing nitrogen gas until the pressure in the reaction kettle is increased to a second preset pressure, and heating to a fourth preset temperature;
adding propylene oxide into the reaction kettle under the second preset pressure and the fourth preset temperature, and stirring for a fourth preset time;
and adding ethylene oxide into the reaction kettle under the second preset pressure and the fourth preset temperature, and stirring for a fifth preset time to obtain the p-dodecanoylphenol amine polyether.
9. The produced fluid treating agent according to claim 8, wherein the second predetermined pressure is 0.2MPa to 0.4MPa, and the fourth predetermined temperature is 100 ℃ to 150 ℃;
the fourth preset time is 5-15 h;
the fifth preset time is 5-10 h.
10. Use of the production fluid treatment agent of any one of claims 1 to 9 in demulsification treatment of oilfield production fluids;
the total concentration of the polymer and the surfactant in the oilfield produced fluid is greater than or equal to 30 mg/L.
11. The use of claim 10, wherein when the total concentration is less than 50mg/L, the demulsifier in the used production fluid treatment agent is added at a concentration of 30mg/L to 50 mg/L;
when the total concentration is more than 50mg/L and less than 100mg/L, the adding concentration is 50 mg/L-80 mg/L;
when the total concentration is more than 100mg/L, the adding concentration is 80 mg/L-200 mg/L;
wherein the mass of the degradation agent in the produced fluid treatment agent is 10-20% of the total mass of the polymer and the surfactant in the oilfield produced fluid.
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