CN114214087B - Efficient composite demulsifier and preparation method thereof - Google Patents
Efficient composite demulsifier and preparation method thereof Download PDFInfo
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- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
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Abstract
The invention relates to the technical field of demulsifiers for crude oil dehydration, in particular to a high-efficiency composite demulsifier and a preparation method thereof, wherein the raw materials comprise polyethylene polyamine, phenol, nonylphenol, potassium hydroxide, propylene oxide, ethylene oxide, xylene and formaldehyde, and the high-efficiency composite demulsifier is prepared by the following steps: firstly, mixing polyethylene polyamine, phenol, nonylphenol and potassium hydroxide, performing esterification reaction to obtain an initiator, adding propylene oxide, ethylene oxide and potassium hydroxide into the initiator, mixing, performing polymerization reaction, adding dimethylbenzene and formaldehyde for dissolution to obtain polyether, and finally adding methanol and water into the polyether for compounding to obtain the efficient composite demulsifier. The efficient composite demulsifier has the characteristics of excellent demulsification performance, low demulsifier addition amount, strong capability of removing suspended matters and good demulsification and dehydration effects.
Description
Technical Field
The invention relates to the technical field of demulsifiers for crude oil dehydration, in particular to a high-efficiency composite demulsifier and a preparation method thereof.
Background
In recent years, with the continuous development of crude oil, the continuous development of oil extraction technology and synthetic emulsion is promoted, and a large amount of high-grade emulsion is applied, so that the crude oil emulsion becomes more stable, the water content of the extracted crude oil is increased year by year, the equipment load in the processes of crude oil storage, transportation and refining is increased, the fuel consumption in the heating process is increased, and the dehydration of the crude oil is seriously affected due to the fact that the crude oil contains salts, sulfides, suspended matters, waxy crude oil and other substances, so that the demulsification and dehydration tasks of the crude oil are greatly aggravated. The demulsifier of the old type can not meet the field requirement. The reasons and demulsification mechanisms affecting the stability of the crude oil emulsion are required to be deeply researched, a novel water-soluble demulsifier is developed, and the dehydration rate of the crude oil is increased so as to achieve the purpose of on-site requirement.
Disclosure of Invention
The invention provides a high-efficiency composite demulsifier and a preparation method thereof, overcomes the defects of the prior art, and can effectively solve the problem of poor demulsification and dehydration effects of the prior demulsifier.
One of the technical schemes of the invention is realized by the following measures: the high-efficiency composite demulsifier comprises, by weight, 3 to 15 parts of polyethylene polyamine, 2 to 6 parts of phenol, 11 to 15 parts of nonylphenol, 0.5 to 2.3 parts of potassium hydroxide, 15 to 25 parts of propylene oxide, 30 to 50 parts of ethylene oxide, 2 to 8 parts of xylene and 1.3 to 1.8 parts of formaldehyde, wherein the high-efficiency composite demulsifier is prepared by the following steps:
firstly, isolating the reaction kettle from air, sequentially adding the polyethylene polyamine, phenol, nonylphenol and a part of potassium hydroxide with required amounts into the reaction kettle, fully and uniformly stirring, and performing esterification reaction to obtain an initiator, wherein the part of potassium hydroxide accounts for 5.0-6.0% of the weight of the potassium hydroxide;
secondly, isolating the reaction kettle containing the initiator from air again, adding propylene oxide, ethylene oxide and the balance of potassium hydroxide into the reaction kettle containing the initiator, fully and uniformly mixing, carrying out polymerization reaction, and then sequentially adding the required amount of dimethylbenzene and formaldehyde into the reaction kettle, and fully stirring and dissolving to obtain polyether;
and thirdly, adding methanol and water into a reaction kettle containing polyether, fully stirring uniformly, then adding glacial acetic acid into the reaction kettle, regulating the pH value of the mixed solution in the kettle to be neutral, and obtaining the demulsifier, wherein the addition amount of the methanol accounts for 18-22% of the weight of the polyethylene polyamine, and the addition amount of the water accounts for 34-36% of the weight of the polyethylene polyamine.
The following are further optimizations and/or improvements to one of the above-described inventive solutions:
in the second step, the weight ratio of the epoxypropane to the epoxyethane is 1:2.
in the first step, the esterification reaction is carried out at 130-140 ℃ and under the pressure of not more than 0.25MPa for 1.0-1.5 h.
In the second step, the polymerization reaction is carried out at a temperature of 105-115 ℃ for 1.0-1.5 h, and the stirring is carried out at a temperature of 105-115 ℃ for 1.0-1.5 h.
In the third step, the temperature is 60 ℃ to 65 ℃ and the time is 1.0h to 1.5h when stirring.
The second technical scheme of the invention is realized by the following measures: the preparation method of the efficient composite demulsifier comprises the following raw materials, by weight, 3 to 15 parts of polyethylene polyamine, 2 to 6 parts of phenol, 11 to 15 parts of nonylphenol, 0.5 to 2.3 parts of potassium hydroxide, 15 to 25 parts of propylene oxide, 30 to 50 parts of ethylene oxide, 2 to 8 parts of dimethylbenzene and 1.3 to 1.8 parts of formaldehyde, wherein the raw materials are as follows:
firstly, isolating the reaction kettle from air, sequentially adding the polyethylene polyamine, phenol, nonylphenol and a part of potassium hydroxide with required amounts into the reaction kettle, fully and uniformly stirring, and performing esterification reaction to obtain an initiator, wherein the part of potassium hydroxide accounts for 5.0-6.0% of the weight of the potassium hydroxide;
secondly, isolating the reaction kettle containing the initiator from air again, adding propylene oxide, ethylene oxide and the balance of potassium hydroxide into the reaction kettle containing the initiator, fully and uniformly mixing, carrying out polymerization reaction, and then sequentially adding the required amount of dimethylbenzene and formaldehyde into the reaction kettle, and fully stirring and dissolving to obtain polyether;
and thirdly, adding methanol and water into a reaction kettle containing polyether, fully stirring uniformly, then adding glacial acetic acid into the reaction kettle, regulating the pH value of the mixed solution in the kettle to be neutral, and obtaining the demulsifier, wherein the addition amount of the methanol accounts for 18-22% of the weight of the polyethylene polyamine, and the addition amount of the water accounts for 34-36% of the weight of the polyethylene polyamine.
The following is a further optimization and/or improvement of the second technical scheme of the invention:
in the second step, the weight ratio of the epoxypropane to the epoxyethane is 1:2.
in the first step, the esterification reaction is carried out at 130-140 ℃ and under the pressure of not more than 0.25MPa for 1.0-1.5 h.
In the second step, the polymerization reaction is carried out at a temperature of 105-115 ℃ for 1.0-1.5 h, and the stirring is carried out at a temperature of 105-115 ℃ for 1.0-1.5 h.
In the third step, the temperature is 60 ℃ to 65 ℃ and the time is 1.0h to 1.5h when stirring.
Compared with the prior art, the invention has the beneficial effects that:
in the invention, during the first step of synthesizing the initiator, raw materials of nonylphenol and polyethylene polyamine are subjected to esterification reaction under the action of a potassium hydroxide catalyst to generate a plurality of stable polymers (namely the initiator) with cyclic structures, wherein the nonylphenol has better chain extension grafting effect on the polyethylene polyamine.
In the invention, when polyether is synthesized in the second step, the optimal weight ratio of propylene oxide to ethylene oxide is 1:2, and when the addition amount of ethylene oxide is too high, the proportion of the lipophilic groups of the demulsifier in molecules is too large, the lipophilic groups are too strong, the water cannot enter the water phase easily, and the adsorption of the molecules on an oil-water interface is unfavorable; when the addition amount of the ethylene oxide is too low, the demulsifier has stronger hydrophilicity and is also unfavorable for being adsorbed on an oil-water interface. Both conditions can reduce the strength of the interfacial adsorption film, and the demulsification effect of the demulsifier is poor. The demulsifier has a remarkable demulsification effect only if the demulsifier has a proper hydrophilic-lipophilic balance value.
The efficient composite demulsifier is water-soluble, has excellent demulsification performance, flash point up to 30 degrees and performance higher than the national standard, and has the characteristics of low demulsifier addition amount, strong capability of removing suspended matters and good demulsification and dehydration effects.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments can be determined according to the technical scheme and practical situations of the present invention. The various chemical reagents and chemical supplies mentioned in the invention are all commonly known and used in the prior art unless specified otherwise; the percentages in the invention are mass percentages unless otherwise specified.
The invention is further described below with reference to examples:
example 1: the high-efficiency composite demulsifier comprises, by weight, 3 to 15 parts of polyethylene polyamine, 2 to 6 parts of phenol, 11 to 15 parts of nonylphenol, 0.5 to 2.3 parts of potassium hydroxide, 15 to 25 parts of propylene oxide, 30 to 50 parts of ethylene oxide, 2 to 8 parts of xylene and 1.3 to 1.8 parts of formaldehyde, wherein the high-efficiency composite demulsifier is prepared by the following steps:
firstly, isolating the reaction kettle from air, sequentially adding the polyethylene polyamine, phenol, nonylphenol and a part of potassium hydroxide with required amounts into the reaction kettle, fully and uniformly stirring, and performing esterification reaction to obtain an initiator, wherein the part of potassium hydroxide accounts for 5.0-6.0% of the weight of the potassium hydroxide;
secondly, isolating the reaction kettle containing the initiator from air again, adding propylene oxide, ethylene oxide and the balance of potassium hydroxide into the reaction kettle containing the initiator, fully and uniformly mixing, carrying out polymerization reaction, and then sequentially adding the required amount of dimethylbenzene and formaldehyde into the reaction kettle, and fully stirring and dissolving to obtain polyether;
and thirdly, adding methanol and water into a reaction kettle containing polyether, fully stirring uniformly, then adding glacial acetic acid into the reaction kettle, regulating the pH value of the mixed solution in the kettle to be neutral, and obtaining the demulsifier, wherein the addition amount of the methanol accounts for 18-22% of the weight of the polyethylene polyamine, and the addition amount of the water accounts for 34-36% of the weight of the polyethylene polyamine.
Example 2: as an optimization of the above examples, in the second step, the weight ratio of propylene oxide to ethylene oxide was 1:2.
example 3: as the optimization of the above examples, in the first step, the esterification reaction was carried out at 130 to 140℃and at a pressure of not more than 0.25MPa for a reaction time of 1.0 to 1.5 hours.
Example 4: as the optimization of the above examples, in the second step, the polymerization reaction was carried out at a temperature of 105 to 115℃for a reaction time of 1.0 to 1.5 hours, and at a temperature of 105 to 115℃for a time of 1.0 to 1.5 hours while stirring.
Example 5: as an optimization of the above examples, in the third step, the temperature was 60℃to 65℃and the time was 1.0h to 1.5h while stirring.
Example 6: the high-efficiency composite demulsifier comprises, by weight, 3 parts of polyethylene polyamine, 2 parts of phenol, 11 parts of nonylphenol, 0.5 part of potassium hydroxide, 15 parts of propylene oxide, 30 parts of ethylene oxide, 2 parts of xylene and 1.3 parts of formaldehyde, wherein the raw materials are obtained by the following steps:
firstly, isolating the reaction kettle from air, enabling the inside of the reaction kettle to be in a nitrogen atmosphere, sequentially adding the polyethylene polyamine, phenol, nonylphenol and a part of potassium hydroxide with required amount, fully and uniformly stirring, and performing esterification reaction to obtain an initiator, wherein the part of potassium hydroxide accounts for 5.0% of the weight of the potassium hydroxide, the temperature is 130 ℃ and the pressure is not more than 0.25MPa during the esterification reaction, and the reaction time is 1.0h;
secondly, isolating the reaction kettle containing the initiator from air again, enabling the inside of the reaction kettle to be in a nitrogen atmosphere, adding propylene oxide, ethylene oxide and the balance of potassium hydroxide into the reaction kettle containing the initiator, fully and uniformly mixing, carrying out polymerization reaction, sequentially adding the required amount of dimethylbenzene and formaldehyde into the reaction kettle, and fully stirring and dissolving to obtain polyether, wherein the weight ratio of the propylene oxide to the ethylene oxide is 1:2, during polymerization reaction, the temperature is 105 ℃, the reaction time is 1.0h, and during stirring, the temperature is 105 ℃ and the reaction time is 1.0h;
and thirdly, adding methanol and water into a reaction kettle containing polyether, fully and uniformly stirring, then adding glacial acetic acid into the reaction kettle, and regulating the pH value of the mixed solution in the reaction kettle to be neutral to obtain the demulsifier, wherein the addition amount of the methanol accounts for 18% of the weight of the polyethylene polyamine, the addition amount of the water accounts for 34% of the weight of the polyethylene polyamine, and the temperature is 60 ℃ and the time is 1.0h during stirring.
Example 7: the high-efficiency composite demulsifier comprises, by weight, 15 parts of polyethylene polyamine, 6 parts of phenol, 15 parts of nonylphenol, 2.3 parts of potassium hydroxide, 25 parts of propylene oxide, 50 parts of ethylene oxide, 8 parts of xylene and 1.8 parts of formaldehyde, wherein the raw materials are obtained by the following steps:
firstly, isolating the reaction kettle from air, enabling the inside of the reaction kettle to be in a nitrogen atmosphere, sequentially adding the polyethylene polyamine, phenol, nonylphenol and a part of potassium hydroxide with required amount, fully and uniformly stirring, and performing esterification reaction to obtain an initiator, wherein the part of potassium hydroxide accounts for 6.0% of the weight of the potassium hydroxide, the temperature is 140 ℃ and the pressure is not more than 0.25MPa during the esterification reaction, and the reaction time is 1.5h;
secondly, isolating the reaction kettle containing the initiator from air again, enabling the inside of the reaction kettle to be in a nitrogen atmosphere, adding propylene oxide, ethylene oxide and the balance of potassium hydroxide into the reaction kettle containing the initiator, fully and uniformly mixing, carrying out polymerization reaction, sequentially adding the required amount of dimethylbenzene and formaldehyde into the reaction kettle, and fully stirring and dissolving to obtain polyether, wherein the weight ratio of the propylene oxide to the ethylene oxide is 1:2, during polymerization reaction, the temperature is 115 ℃, the reaction time is 1.5h, and during stirring, the temperature is 115 ℃ and the reaction time is 1.5h;
and thirdly, adding methanol and water into a reaction kettle containing polyether, fully and uniformly stirring, then adding glacial acetic acid into the reaction kettle, and regulating the pH value of the mixed solution in the reaction kettle to be neutral to obtain the demulsifier, wherein the addition amount of the methanol accounts for 22% of the weight of the polyethylene polyamine, the addition amount of the water accounts for 36% of the weight of the polyethylene polyamine, and the temperature is 65 ℃ and the time is 1.5h during stirring.
Example 8: the high-efficiency composite demulsifier comprises, by weight, 10 parts of polyethylene polyamine, 4 parts of phenol, 13 parts of nonylphenol, 1.5 parts of potassium hydroxide, 20 parts of propylene oxide, 40 parts of ethylene oxide, 6 parts of xylene and 1.5 parts of formaldehyde, wherein the raw materials are obtained by the following steps:
firstly, isolating the reaction kettle from air, enabling the inside of the reaction kettle to be in a nitrogen atmosphere, sequentially adding the polyethylene polyamine, phenol, nonylphenol and a part of potassium hydroxide with required amount, fully and uniformly stirring, and performing esterification reaction to obtain an initiator, wherein the part of potassium hydroxide accounts for 5.6% of the weight of the potassium hydroxide, the temperature is 140 ℃ and the pressure is not more than 0.25MPa, and the reaction time is 1.0h;
secondly, isolating the reaction kettle containing the initiator from air again, enabling the inside of the reaction kettle to be in a nitrogen atmosphere, adding propylene oxide, ethylene oxide and the balance of potassium hydroxide into the reaction kettle containing the initiator, fully and uniformly mixing, carrying out polymerization reaction, sequentially adding the required amount of dimethylbenzene and formaldehyde into the reaction kettle, and fully stirring and dissolving to obtain polyether, wherein the weight ratio of the propylene oxide to the ethylene oxide is 1:2, during polymerization reaction, the temperature is 115 ℃, the reaction time is 1.0h, and during stirring, the temperature is 115 ℃ and the reaction time is 1.0h;
and thirdly, adding methanol and water into a reaction kettle containing polyether, fully and uniformly stirring, then adding glacial acetic acid into the reaction kettle, and regulating the pH value of the mixed solution in the reaction kettle to be neutral to obtain the demulsifier, wherein the addition amount of the methanol accounts for 20% of the weight of the polyethylene polyamine, the addition amount of the water accounts for 35% of the weight of the polyethylene polyamine, and the temperature is 65 ℃ and the time is 1.0h during stirring.
The crude oil treated by the high-efficiency composite demulsifier prepared in the embodiments 6 to 8 has clear oil-water interface after dehydration, has the characteristics of low demulsifier addition amount, strong capability of removing suspended matters and good demulsification and dehydration effects, and is characterized by examining the influence of the addition ratio of raw materials of propylene oxide and ethylene oxide on the demulsification performance of the high-efficiency composite demulsifier and the demulsification performance of the high-efficiency composite demulsifier prepared in the embodiment 8.
Test 1: the influence of the adding proportion of the raw materials of propylene oxide and ethylene oxide on the demulsification performance of the efficient composite demulsifier
The test method comprises the following steps: the weight ratio of propylene oxide to ethylene oxide in the embodiment 8 of the invention is changed to 15 parts, the weight ratio of propylene oxide to ethylene oxide is respectively set to 1:0.2, 1:0.4, 1:0.6, 1:0.8, 1:1.0, 1:1.2, 1:1.4, 1:1.6, 1:1.8, 1:2.0, 1:2.2, 1:2.4 and 1:2.6, the weight ratio of ethylene oxide is calculated according to the weight ratio of propylene oxide to ethylene oxide, the addition amount of the rest raw materials and the process steps are respectively set to 1:0.2, 1:3, 4, 5, 6, 7, 8, 9, 10, 11, 12 and 13, the samples 1 to 13 are added to crude oil, the water content of the crude oil is 63% of the crude oil is detected by a fire flooding, the water content of the crude oil is examined, the samples are added to the oil recovery sample with a fire-breaking effect of the oil field of 100mg, and the oil recovery concentration is added to the oil recovery sample with a Clara.
Test results: as shown in table 1, the demulsification and dehydration effects of samples 1 to 13 on crude oil show that the optimal addition ratio of propylene oxide to ethylene oxide is 1:2, and when the addition ratio of ethylene oxide is too high, the proportion of the demulsifier lipophilic groups in the molecules is too large, the lipophilicity is too strong, the demulsifier is not easy to enter into an aqueous phase, and the adsorption of the molecules on an oil-water interface is unfavorable; when the addition amount of the ethylene oxide is too low, the demulsifier has stronger hydrophilicity and is also unfavorable for being adsorbed on an oil-water interface. Both of these conditions reduce the strength of the interfacial adsorption film, and deteriorate the demulsification effect. The demulsifier has a remarkable demulsification effect only if the demulsifier has a proper hydrophilic-lipophilic balance value. Therefore, when the adding amount ratio of the propylene oxide to the ethylene oxide is 1:2, the obtained high-efficiency composite demulsifier has the optimal demulsification and dehydration effects.
Test 2: examination of the demulsification Performance of the high-efficiency composite demulsifier of the present invention
The test method comprises the steps of selecting No. 1 crude oil and No. 2 crude oil in the test, wherein the No. 1 crude oil is fireflood crude oil of a Kramay oil field oil extraction plant (because the fireflood crude oil adopts a fire burning oil layer mode in the oil field development process, a great amount of suspended matters and impurities are contained in the fireflood crude oil), and the water content of the No. 1 crude oil is 63%; the No. 2 crude oil is the red and shallow carbon dioxide flooding crude oil of a Krama oil field oil extraction factory, the water content of the No. 2 crude oil is 17.5%, the high-efficiency composite demulsifier prepared in the embodiment 8 of the invention is respectively added into the No. 1 crude oil and the No. 2 crude oil, so that the concentration of the high-efficiency composite demulsifier in the No. 1 crude oil and the No. 2 crude oil is respectively 100mg/L, the dehydration test is carried out on the No. 1 crude oil and the No. 2 crude oil respectively added with the high-efficiency composite demulsifier prepared in the embodiment 8 of the invention, meanwhile, the existing demulsifier (model No. LH-14 of Krama sinceric Co., ltd.) is adopted as a comparison, the dehydration test of the crude oil is carried out by referring to a method specified in SY/T5280-2018 general technical condition of the crude oil demulsifier, the dehydration temperature in the test is controlled at 75 ℃ in the test, and the vibration method of a dehydration test bottle in the test is adopted by an artificial vibration method.
The test results show that the dehydration rate of the No. 1 crude oil added with the high-efficiency composite demulsifier prepared in the embodiment 8 of the invention is shown in the table 2, and the dehydration rate of the No. 2 crude oil added with the high-efficiency composite demulsifier prepared in the embodiment 8 of the invention is 98.7% for the No. 1 crude oil (fireflood crude oil), and the dehydration rate of the high-efficiency composite demulsifier of the invention is 97.1% for the No. 2 crude oil (carbon dioxide flood crude oil), as shown in the table 3 and the tables 2 and 3, so that the high-efficiency composite demulsifier has good demulsification and dehydration performances.
In conclusion, the efficient composite demulsifier is a water-soluble demulsifier, has excellent demulsification performance, a flash point of 30 degrees, and higher performance than the national standard, and the crude oil treated by the efficient composite demulsifier has clear oil-water interface after dehydration, and has the characteristics of low demulsifier addition amount, strong capability of removing suspended matters and good demulsification and dehydration effects.
The technical characteristics form the embodiment of the invention, have stronger adaptability and implementation effect, and can increase or decrease unnecessary technical characteristics according to actual needs so as to meet the requirements of different situations.
Claims (6)
1. The efficient composite demulsifier is characterized by comprising 3 to 15 parts of polyethylene polyamine, 2 to 6 parts of phenol, 11 to 15 parts of nonylphenol, 0.5 to 2.3 parts of potassium hydroxide, 15 to 25 parts of propylene oxide, 30 to 50 parts of ethylene oxide, 2 to 8 parts of dimethylbenzene and 1.3 to 1.8 parts of formaldehyde in parts by weight, and is prepared by the following steps:
firstly, isolating the reaction kettle from air, sequentially adding the polyethylene polyamine, phenol, nonylphenol and a part of potassium hydroxide with required amounts into the reaction kettle, fully and uniformly stirring, and performing esterification reaction to obtain an initiator, wherein the part of potassium hydroxide accounts for 5.0-6.0% of the weight of the potassium hydroxide;
secondly, isolating the reaction kettle containing the initiator from air again, adding propylene oxide, ethylene oxide and the balance of potassium hydroxide into the reaction kettle containing the initiator, fully and uniformly mixing, carrying out polymerization reaction, and then sequentially adding the required amount of dimethylbenzene and formaldehyde into the reaction kettle, and fully stirring and dissolving to obtain polyether; wherein the weight ratio of the epoxypropane to the epoxyethane is 1:2;
and thirdly, adding methanol and water into a reaction kettle containing polyether, fully stirring uniformly, then adding glacial acetic acid into the reaction kettle, regulating the pH value of the mixed solution in the kettle to be neutral, and obtaining the demulsifier, wherein the addition amount of the methanol accounts for 18-22% of the weight of the polyethylene polyamine, and the addition amount of the water accounts for 34-36% of the weight of the polyethylene polyamine.
2. The efficient complex demulsifier as claimed in claim 1, wherein in the first step, the esterification reaction is carried out at a temperature of 130 ℃ to 140 ℃ and a pressure of not more than 0.25MPa and a reaction time of 1.0h to 1.5h.
3. The efficient complex demulsifier as claimed in claim 1 or 2, wherein in the second step, the polymerization is carried out at a temperature of 105 to 115 ℃ for a reaction time of 1.0 to 1.5 hours and the stirring is carried out at a temperature of 105 to 115 ℃ for a time of 1.0 to 1.5 hours.
4. The efficient complex demulsifier as claimed in claim 1 or 2, wherein in the third step, the temperature is 60 ℃ to 65 ℃ and the time is 1.0h to 1.5h when stirring.
5. The efficient complex demulsifier as claimed in claim 3, wherein in the third step, the temperature is 60 to 65 ℃ and the time is 1.0 to 1.5 hours when stirring.
6. The preparation method of the efficient composite demulsifier according to any one of claims 2 to 5, characterized in that the raw materials comprise 3 to 15 parts by weight of polyethylene polyamine, 2 to 6 parts by weight of phenol, 11 to 15 parts by weight of nonylphenol, 0.5 to 2.3 parts by weight of potassium hydroxide, 15 to 25 parts by weight of propylene oxide, 30 to 50 parts by weight of ethylene oxide, 2 to 8 parts by weight of xylene and 1.3 to 1.8 parts by weight of formaldehyde, and the preparation method comprises the following steps:
firstly, isolating the reaction kettle from air, sequentially adding the polyethylene polyamine, phenol, nonylphenol and a part of potassium hydroxide with required amounts into the reaction kettle, fully and uniformly stirring, and performing esterification reaction to obtain an initiator, wherein the part of potassium hydroxide accounts for 5.0-6.0% of the weight of the potassium hydroxide;
secondly, isolating the reaction kettle containing the initiator from air again, adding propylene oxide, ethylene oxide and the balance of potassium hydroxide into the reaction kettle containing the initiator, fully and uniformly mixing, carrying out polymerization reaction, and then sequentially adding the required amount of dimethylbenzene and formaldehyde into the reaction kettle, and fully stirring and dissolving to obtain polyether; wherein the weight ratio of the epoxypropane to the epoxyethane is 1:2;
and thirdly, adding methanol and water into a reaction kettle containing polyether, fully stirring uniformly, then adding glacial acetic acid into the reaction kettle, regulating the pH value of the mixed solution in the kettle to be neutral, and obtaining the demulsifier, wherein the addition amount of the methanol accounts for 18-22% of the weight of the polyethylene polyamine, and the addition amount of the water accounts for 34-36% of the weight of the polyethylene polyamine.
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| US4537701A (en) * | 1977-05-04 | 1985-08-27 | Basf Aktiengesellschaft | Demulsifiers for breaking crude-oil emulsions and their use |
| CN111019117A (en) * | 2019-12-25 | 2020-04-17 | 东北石油大学 | Preparation method of modified multi-branched polyether demulsifier |
| CN112694910A (en) * | 2020-12-13 | 2021-04-23 | 东北石油大学 | Preparation method of anionic demulsifier suitable for offshore oil field |
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