CN111019117A - Preparation method of modified multi-branched polyether demulsifier - Google Patents
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- CN111019117A CN111019117A CN201911352714.8A CN201911352714A CN111019117A CN 111019117 A CN111019117 A CN 111019117A CN 201911352714 A CN201911352714 A CN 201911352714A CN 111019117 A CN111019117 A CN 111019117A
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- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
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Abstract
A method for preparing a modified multi-branched polyether demulsifier. The method comprises the following steps: mixing 2, 2-bis (4-hydroxyphenyl) propane and triethylene tetramine, heating for dissolving, then carrying out heat preservation reaction in a formaldehyde solution, adding xylene for reflux dehydration, then heating for evaporating the xylene, and reacting the rest substances to generate an initiator; putting an initiator into a high-temperature high-pressure reaction kettle, sealing by using potassium hydroxide as a catalyst, vacuumizing, and adding propylene oxide to enable the reaction kettle to generate a polyether reaction to generate an intermediate product; putting the intermediate product into a high-temperature high-pressure reaction kettle, sealing by using potassium hydroxide as a catalyst, vacuumizing, and introducing ethylene oxide to enable the reaction kettle to generate polyether reaction to generate multi-branched polyether; and (3) taking potassium hydroxide as a catalyst, heating the multi-branched polyether in a water bath, and slowly dropwise adding epoxy chloropropane to modify the multi-branched polyether to generate the multi-branched polyether demulsifier. The modified multi-branched polyether demulsifier prepared by the invention has hydrophilic capacity and good wetting property and penetration effect.
Description
The technical field is as follows:
the invention relates to a preparation method of a modified multi-branched polyether demulsifier, belonging to the technical field of oilfield chemicals.
Background art:
the crude oil emulsion is mainly caused by the fact that crude oil contains a large amount of water, and then the emulsion is formed. In the process of crude oil exploitation, particularly at the positions of a choke, a valve, an oil pump, an oil pipeline and the like of an oil well, crude oil and water are strongly mixed to form a large amount of crude oil emulsion through friction, particularly under the shearing action of an oil pump blade and the scouring action of high-pressure liquid drops. Large amounts of crude oil emulsions seriously affect the transportation, application and processing of crude oil. Therefore, demulsification treatment of crude oil emulsion is very important. In addition, in the process of oil exploitation, along with the implementation of various enhanced oil recovery modes such as water injection oil recovery, thick oil thermal recovery, alkaline water oil displacement, polymer oil displacement, surfactant oil displacement and the like, the crude oil emulsion is more difficult to damage, and the requirement on a demulsifier is also improved.
The current demulsification methods can be divided into physical mechanical methods and physical chemical methods. Physical mechanical methods include electro-sedimentation, filtration, ultrasound, and the like; the physical and chemical method is mainly to change the interfacial property of the emulsion to break the emulsion, such as adding a demulsifier. At present, the demulsifier widely used in oil fields in China is a demulsifier mainly containing polyether, and different polyether demulsifiers are obtained through different initiators, propylene oxide and ethylene oxide with different addition numbers and proportions and different modifiers. The multi-branched polyether demulsifier is more excellent in reducing the surface tension of an oil-water interface than a common linear polyether demulsifier, and the rubber bundles formed by the multi-branched polyether are more compact, so that the multi-branched polyether demulsifier has a better effect on crude oil demulsification. However, the existing multi-branched polyether demulsifiers have the following problems in application: low dehydration rate, large dosage, weak hydrophilic ability, wettability and osmotic effect, and long time for reaching an oil-water interface, so that the existing multi-branched polyether demulsifier needs to be modified.
The invention content is as follows:
in order to solve the technical problems mentioned in the background technology, the invention provides a modified multi-branched polyether demulsifier and a preparation method thereof.
The technical scheme of the invention is as follows: the structural general formula of the modified multi-branched polyether demulsifier is as follows:
wherein the content of the first and second substances,
the preparation method of the modified multi-branched polyether demulsifier comprises the following steps:
(1) 1 part of 2, 2-bis (4-hydroxyphenyl) propane and 2-3 parts of triethylene tetramine are placed into a four-way bottle and heated to 45-55 ℃ for complete dissolution, 0.4-0.6 part of formaldehyde solution with the concentration of 37-40% is slowly dripped at 35-55 ℃, heat preservation is carried out for 35-45 min, 1.7-2.3 parts of dimethylbenzene is added, heating is carried out to 100-110 ℃ for reflux dehydration, heating is carried out to 185-195 ℃ after 1.5-2.5 h, dimethylbenzene is evaporated, and the rest substances are fully reacted for 1-2 h to generate an initiator.
(2) And (2) putting 1 part of the initiator obtained in the step (1) and 0.18-1.08 part of potassium hydroxide into a high-temperature high-pressure reaction kettle, sealing, replacing air in the kettle by using a nitrogen purging mode, vacuumizing for 4-6 min to negative pressure by using a vacuum pump, opening a feed valve, slowly introducing 69-359 parts of propylene oxide, heating to 105-115 ℃, controlling the reading of a pressure gauge of the high-temperature high-pressure reaction kettle to be 0.19-0.21 MPa, closing the feed valve after the propylene oxide is added, and reducing the pressure in the reaction kettle to the end of negative pressure reaction to obtain an intermediate product.
(3) And (3) putting 1 part of the intermediate product obtained in the step (2) and 0.13-0.81 part of potassium hydroxide into a high-temperature high-pressure reaction kettle, sealing, replacing air in the kettle by using a nitrogen purging mode, vacuumizing for 4-6 min to negative pressure by using a vacuum pump, opening a feed valve, slowly introducing 18.9-180 parts of ethylene oxide, heating to 105-115 ℃, controlling the reading of a pressure gauge of the high-temperature high-pressure reaction kettle to be 0.19-0.21 MPa, closing the feed valve after the ethylene oxide is added, and reducing the pressure in the reaction kettle until the negative pressure reaction is finished to obtain the multi-branched polyether.
(4) Putting 10 parts of the multi-branched polyether obtained in the step (3) into a three-way flask, carrying out first-stage water bath heating, keeping the temperature after the temperature is 50-60 ℃, adding 0.11-0.13 part of potassium hydroxide, and then stirring for 15-25 min; performing water bath heating at the second stage, keeping the temperature after the temperature is 60-80 ℃, and slowly dripping 0.2-0.24 part of epoxy chloropropane for 2-3 hours; and (3) performing water bath heating to 80-90 ℃ in the third stage, preserving heat, and obtaining the modified multi-branched polyether demulsifier after 8 hours.
Wherein, the parts mentioned in the steps (1) to (4) are all parts by weight.
The invention has the following beneficial effects: the preparation method provided by the invention has the characteristics of simplicity, convenience in configuration, rapidness, high efficiency and low cost. Compared with the conventional surfactant or other polyether demulsifiers, the modified multi-branched polyether demulsifier prepared by the method has excellent demulsification effect and stronger dehydration rate, reduces the consumption, and can improve the crude oil extraction efficiency; in addition, the water-soluble polyurethane composite material also has stronger hydrophilic capacity, wettability and osmotic effect, can reach an oil-water interface quickly, and improves the efficiency and the efficiency of reducing the surface tension.
Description of the drawings:
FIG. 1 is a diagram showing the demulsification effect of samples 1-4 of the modified multi-branched polyether demulsifier prepared by the invention on crude oil in a certain oil field.
FIG. 2 is a diagram showing the demulsification effect of samples 5-8 of the modified multi-branched polyether demulsifier prepared by the invention on crude oil in a certain oil field.
FIG. 3 is a diagram showing the demulsification effect of samples 9-12 of the modified multi-branched polyether demulsifier prepared by the invention on crude oil in a certain oil field.
FIG. 4 is a diagram showing the demulsifying effect of samples 13-16 of the modified multi-branched polyether demulsifier prepared by the present invention on crude oil in a certain oil field.
FIG. 5 is a graph showing the demulsifying effect of samples 17-20 of the modified hyperbranched polyether demulsifier prepared by the present invention on crude oil in a certain oil field.
FIG. 6 is a graph showing the demulsifying effect of samples 21-24 of the modified multi-branched polyether demulsifier prepared by the present invention on crude oil in a certain oil field.
FIG. 7 is a comparison graph of the demulsification effect of the currently used demulsifier of the oil field on crude oil of a certain oil field.
The specific implementation mode is as follows:
the invention will be further described with reference to the accompanying drawings in which:
the preparation method of the modified multi-branched polyether demulsifier comprises the following steps:
(1) 1 part of 2, 2-bis (4-hydroxyphenyl) propane and 2-3 parts of triethylene tetramine are placed into a four-way bottle and heated to 45-55 ℃ for complete dissolution, 0.4-0.6 part of formaldehyde solution with the concentration of 37-40% is slowly dripped at 35-55 ℃, heat preservation is carried out for 35-45 min, 1.7-2.3 parts of dimethylbenzene is added, heating is carried out to 100-110 ℃ for reflux dehydration, heating is carried out to 185-195 ℃ after 1.5-2.5 h, dimethylbenzene is evaporated, and the rest substances are fully reacted for 1-2 h to generate an initiator.
(2) Putting 1 part of initiator and 0.18-1.08 part of potassium hydroxide into a high-temperature high-pressure reaction kettle, sealing, replacing air in the kettle by using a nitrogen purging mode, vacuumizing for 4-6 min to negative pressure by using a vacuum pump, opening a feed valve, slowly introducing 69-359 parts of propylene oxide, heating to 105-115 ℃, controlling the reading of a pressure gauge to be 0.19-0.21 MPa, closing the feed valve after the propylene oxide is added, and reducing the pressure in the reaction kettle to the end of negative pressure reaction to obtain an intermediate product.
(3) Putting the intermediate product 1 and 0.13-0.81 part of potassium hydroxide into a high-temperature high-pressure reaction kettle, sealing, replacing air in the kettle by using a nitrogen purging mode, vacuumizing for 4-6 min to negative pressure by using a vacuum pump, opening a feed valve, slowly introducing 18.9-180 parts of ethylene oxide, heating to 105-115 ℃, controlling the reading of a pressure gauge to be 0.19-0.21 MPa, closing the feed valve after the ethylene oxide is added, and reducing the pressure in the reaction kettle until the negative pressure reaction is finished to obtain the multi-branched polyether.
(4) Putting 10 parts of multi-branched polyether into a three-way bottle, stirring, heating in water bath to 50-60 ℃, adding 0.11-0.13 part of potassium hydroxide, continuing heating in water bath to 60-80 ℃, slowly dropwise adding 0.2-0.24 part of epoxy chloropropane for about 2-3 h, heating in water bath to 80-90 ℃, preserving heat, and obtaining the modified multi-branched polyether demulsifier after 8 h.
In the steps (2) and (3), the catalyst for the polyether reaction is potassium hydroxide, and the dosage of the first catalyst is 0.18-1.08 parts, specifically 0.2% of the total parts. The dosage of the second catalyst is 0.13-0.81 parts, specifically 0.15% of the total parts.
According to the scheme, in the steps (2) and (3), the gas in the replacement kettle is nitrogen, the vacuumizing time is 4-6 min, and the gauge pressure of the reaction kettle is-0.09 Mpa.
According to the scheme, in the step (4), the catalyst for the modification reaction is potassium hydroxide, and the amount of the catalyst is 0.11-0.13 part, specifically 0.12 part.
According to the scheme, in the step (4), the first water bath is heated to 50-60 ℃, potassium hydroxide is added, and then stirring is needed for 15-25 min; heating in a water bath for the second time to 60-80 ℃, and dropwise adding the modifier; and heating in a water bath for the third time to 80-90 ℃, and keeping the temperature for 8 hours.
According to the scheme, in the step (4), the dropwise adding modifier epoxy chloropropane is added by 0.2-0.24 part, specifically 0.2 part, and the modifier epoxy chloropropane can be dropwise added by using a separating funnel for 2-3 hours.
The above process involves the following reaction scheme:
wherein:
several specific examples are given below.
Example 1
Adding 2g, 2-bis (4-hydroxyphenyl) propane and 50g triethylene tetramine into a four-neck bottle, heating in a water bath, stirring until the mixture is completely dissolved at 50 ℃, then preserving heat for 15min, then slowly dropwise adding 10g of formaldehyde solution, preserving heat for reaction for 30min after the dropwise adding is finished, adding 40g of dimethylbenzene, carrying out reflux dehydration after the temperature is increased to 105 ℃, gradually increasing the temperature to 190 ℃ after 2h, then gradually increasing the transparency of reactants and the dimethylbenzene, completely evaporating the dimethylbenzene at 190 ℃, and keeping the reaction for 1h to finish the reaction. The product was a dark red viscous liquid, giving the starter.
4g of the initiator and 0.832g of potassium hydroxide are added into a high-temperature high-pressure reaction kettle, and the reaction kettle is sealed. Purging and replacing air by using nitrogen before heating, then vacuumizing by using a vacuum pump, starting heating after 5min, stopping heating when the temperature rises to 110 ℃, opening a feed valve, introducing 276g of propylene oxide, controlling the pressure within 0.2 +/-0.01 MPa, keeping the temperature unchanged, and continuing to react for 25min after the materials in the kettle are reacted and the pressure falls to-0.09 MPa after the pressure falls; finally, cooling, opening the kettle and discharging to obtain an intermediate product.
And adding the intermediate product after the reaction and 0.624g of potassium hydroxide into a high-temperature high-pressure reaction kettle, and sealing the reaction kettle. Purging and replacing air by using nitrogen before heating, then vacuumizing by using a vacuum pump, starting heating after 5min, stopping heating when the temperature rises to 110 ℃, opening a feed valve, introducing 140g of ethylene oxide, controlling the pressure within 0.2 +/-0.01 MPa, keeping the temperature unchanged, and continuing to react for 25min after the materials in the kettle are reacted and the pressure falls to-0.09 MPa after the pressure falls; finally cooling and opening the kettle, and discharging to obtain the multi-branched polyether.
And (2) putting 80g of multi-branched polyether into a trisection bottle, stirring, heating in a water bath to 55 ℃, adding 0.96g of potassium hydroxide, stirring for 20min, continuing heating in the water bath to 70 ℃, slowly dropwise adding 1.6g of epoxy chloropropane for about 2.5h, heating in the water bath to 85 ℃, preserving heat, and obtaining a modified multi-branched polyether demulsifier sample 1 after 8 h.
Example 2:
adding 2g, 2-bis (4-hydroxyphenyl) propane and 50g triethylene tetramine into a four-neck bottle, heating in a water bath, stirring until the mixture is completely dissolved at 50 ℃, then preserving heat for 15min, then slowly dropwise adding 10g of formaldehyde solution, preserving heat for reaction for 30min after the dropwise adding is finished, adding 40g of dimethylbenzene, carrying out reflux dehydration after the temperature is increased to 105 ℃, gradually increasing the temperature to 190 ℃ after 2h, then gradually increasing the transparency of reactants and the dimethylbenzene, completely evaporating the dimethylbenzene at 190 ℃, and keeping the reaction for 1h to finish the reaction. The product was a dark red viscous liquid, giving the starter.
4g of the initiator and 4.312g of potassium hydroxide were added to a high-temperature high-pressure reaction vessel, which was then sealed. Purging and replacing air by using nitrogen before heating, then vacuumizing by using a vacuum pump, starting heating after 5min, stopping heating when the temperature rises to 110 ℃, opening a feed valve, introducing 1436g of propylene oxide, controlling the pressure within 0.2 +/-0.01 MPa, keeping the temperature unchanged, and continuing to react for 25min after the materials in the kettle are reacted and the pressure falls to-0.09 MPa after the pressure falls; finally, cooling, opening the kettle and discharging to obtain an intermediate product.
And adding the intermediate product after the reaction and 3.234g of potassium hydroxide into a high-temperature high-pressure reaction kettle, and sealing the reaction kettle. Purging and replacing air by using nitrogen before heating, then vacuumizing by using a vacuum pump, starting heating after 5min, stopping heating when the temperature rises to 110 ℃, opening a feed valve, introducing 720g of ethylene oxide, controlling the pressure within 0.2 +/-0.01 MPa, keeping the temperature unchanged, and continuing to react for 25min after the materials in the kettle are reacted and the pressure falls to-0.09 MPa after the pressure falls; finally cooling and opening the kettle, and discharging to obtain the multi-branched polyether.
And putting 80g of multi-branched polyether into a trisection bottle, stirring, heating in a water bath to 55 ℃, adding 0.96g of potassium hydroxide, stirring for 20min, continuing heating in the water bath to 70 ℃, slowly dropwise adding 1.6g of epoxy chloropropane for about 2.5h, heating in the water bath to 85 ℃, preserving heat, and obtaining a modified multi-branched polyether demulsifier sample 2 after 8 h.
Example 3:
adding 2g, 2-bis (4-hydroxyphenyl) propane and 50g triethylene tetramine into a four-neck bottle, heating in a water bath, stirring until the mixture is completely dissolved at 50 ℃, then preserving heat for 15min, then slowly dropwise adding 10g of formaldehyde solution, preserving heat for reaction for 30min after the dropwise adding is finished, adding 40g of dimethylbenzene, carrying out reflux dehydration after the temperature is increased to 105 ℃, gradually increasing the temperature to 190 ℃ after 2h, then gradually increasing the transparency of reactants and the dimethylbenzene, completely evaporating the dimethylbenzene at 190 ℃, and keeping the reaction for 1h to finish the reaction. The product was a dark red viscous liquid, giving the starter.
4g of the initiator and 1.746g of potassium hydroxide were added to a high-temperature high-pressure reaction vessel, and the reaction vessel was sealed. Purging and replacing air by using nitrogen before heating, then vacuumizing by using a vacuum pump, starting heating after 5min, stopping heating when the temperature rises to 110 ℃, opening a feed valve, introducing 636g of propylene oxide, controlling the pressure within 0.2 +/-0.01 MPa and keeping the temperature unchanged, and continuing to react for 25min after the materials in the kettle are reacted and the pressure returns after the materials in the kettle are reacted, so that the pressure is reduced to-0.09 MPa; finally, cooling, opening the kettle and discharging to obtain an intermediate product.
And adding the intermediate product after the reaction and 1.31g of potassium hydroxide into a high-temperature high-pressure reaction kettle, and sealing the reaction kettle. Purging and replacing air by using nitrogen before heating, then vacuumizing by using a vacuum pump, starting heating after 5min, stopping heating when the temperature rises to 110 ℃, opening a feed valve, introducing 237g of ethylene oxide, controlling the pressure within 0.2 +/-0.01 MPa, keeping the temperature unchanged, and continuing to react for 25min after the materials in the kettle are reacted and the pressure falls to-0.09 MPa after the pressure falls; finally cooling and opening the kettle, and discharging to obtain the multi-branched polyether.
And putting 80g of multi-branched polyether into a trisection bottle, stirring, heating in a water bath to 55 ℃, adding 0.96g of potassium hydroxide, stirring for 20min, continuing heating in the water bath to 70 ℃, slowly dropwise adding 1.6g of epoxy chloropropane for about 2.5h, heating in the water bath to 85 ℃, preserving heat, and obtaining a modified multi-branched polyether demulsifier sample 3 after 8 h.
Referring to examples 1 to N, the synthesis initiator and the modification step are the same, different multi-branched polyethers are obtained only by changing the mass parts of the introduced propylene oxide and the ethylene oxide, and the different modified multi-branched polyether demulsifiers 4 to 24 are obtained by modification.
And (3) evaluating the dehydration effect of different modified multi-branched polyether demulsifier samples 1-24, and taking the crude oil produced liquid of a certain oil field as a treatment object. The results of the experiments are given in the following table
The invention has the best effect of being water-soluble 2-159(3.7:1) (number 12 in the table), and compared with a comparison sample (number 25 in the table) made by the existing demulsifier in a certain oil field, the invention has the advantages of excellent demulsification effect, high demulsification speed, good demulsification effect and the like.
According to the experimental results, the modified multi-branched polyether demulsifier prepared by the method has the advantages of excellent demulsification effect, strong dehydration rate, low consumption, high crude oil exploitation efficiency, strong hydrophilic capacity, high wettability and high permeation effect, can reach an oil-water interface quickly, has good efficiency and efficiency for reducing surface tension, promotes the demulsification effect, and has better effect than the traditional demulsifier.
Claims (2)
1. A modified multi-branched polyether demulsifier has a structural general formula as follows:
the preparation method of the modified multi-branched polyether demulsifier comprises the following steps:
(1) putting 1 part of 2, 2-bis (4-hydroxyphenyl) propane and 2-3 parts of triethylene tetramine into a four-way bottle, heating to 45-55 ℃ for complete dissolution, slowly dripping 0.4-0.6 part of formaldehyde solution with the concentration of 37-40% at 35-55 ℃, keeping the temperature for 35-45 min, then adding 1.7-2.3 parts of dimethylbenzene, heating to 100-110 ℃ for reflux dehydration, heating to 185-195 ℃ after 1.5-2.5 h for dimethylbenzene evaporation, and fully reacting the rest substances for 1-2 h to generate an initiator;
(2) putting 1 part of the initiator obtained in the step (1) and 0.18-1.08 part of potassium hydroxide into a high-temperature high-pressure reaction kettle for sealing, replacing air in the kettle by using a nitrogen purging mode, vacuumizing for 4-6 min to negative pressure by using a vacuum pump, opening a feed valve, slowly introducing 69-359 parts of propylene oxide, heating to 105-115 ℃, controlling the reading of a pressure gauge of the high-temperature high-pressure reaction kettle to be 0.19-0.21 MPa, closing the feed valve after the propylene oxide is added, and reducing the pressure in the reaction kettle to the end of negative pressure reaction to obtain an intermediate product;
(3) putting 1 part of the intermediate product obtained in the step (2) and 0.13-0.81 part of potassium hydroxide into a high-temperature high-pressure reaction kettle for sealing, replacing air in the kettle by using a nitrogen purging mode, vacuumizing for 4-6 min to negative pressure by using a vacuum pump, opening a feed valve, slowly introducing 18.9-180 parts of ethylene oxide, heating to 105-115 ℃, controlling the reading of a pressure gauge of the high-temperature high-pressure reaction kettle to be 0.19-0.21 MPa, closing the feed valve after the ethylene oxide is added, and reducing the pressure in the reaction kettle until the negative pressure reaction is finished to obtain the multi-branched polyether;
(4) putting 10 parts of the multi-branched polyether obtained in the step (3) into a three-way flask, carrying out first-stage water bath heating, keeping the temperature after the temperature is 50-60 ℃, adding 0.11-0.13 part of potassium hydroxide, and then stirring for 15-25 min; performing water bath heating at the second stage, keeping the temperature after the temperature is 60-80 ℃, and slowly dripping 0.2-0.24 part of epoxy chloropropane for 2-3 hours; heating in water bath to 80-90 ℃ in the third stage, preserving heat, and preparing the modified multi-branched polyether demulsifier after 8 hours;
wherein, the parts mentioned in the steps (1) to (4) are all parts by weight.
2. The preparation method of the modified hyperbranched polyether demulsifier of claim 1, wherein the modified hyperbranched polyether demulsifier comprises: 69-359 parts of propylene oxide is added in the step (2); adding 18.9-180 parts of ethylene oxide in the step (3); and (3) controlling the reaction temperature after the temperature rise in the step (2) and the step (3) to be between 110 and 115 ℃, and adjusting the opening of a feed valve during the reaction to keep the reading of a pressure gauge of the high-temperature high-pressure reaction kettle within 0.2 +/-0.01 MPa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114214087A (en) * | 2021-12-16 | 2022-03-22 | 克拉玛依新科澳石油天然气技术股份有限公司 | High-efficiency composite demulsifier and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111777757A (en) * | 2020-07-27 | 2020-10-16 | 滨州学院 | Preparation method of super heavy oil demulsifier |
| CN111777757B (en) * | 2020-07-27 | 2022-10-04 | 滨州学院 | Preparation method of super heavy oil demulsifier |
| CN114214087A (en) * | 2021-12-16 | 2022-03-22 | 克拉玛依新科澳石油天然气技术股份有限公司 | High-efficiency composite demulsifier and preparation method thereof |
| CN114214087B (en) * | 2021-12-16 | 2023-06-30 | 克拉玛依新科澳石油天然气技术股份有限公司 | Efficient composite demulsifier and preparation method thereof |
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