CN114316244A - Polymer flooding produced liquid demulsifier and preparation method thereof - Google Patents
Polymer flooding produced liquid demulsifier and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical agents, and particularly relates to a polymer flooding produced fluid demulsifier and a preparation method thereof. The demulsifier is a block copolymer generated by grafting propylene oxide and ethylene oxide on an octyl phenolic resin initiator. The initiator is self-made, the phenolic ratio can be changed as required, the molecular structure of the demulsifier is adjusted, the oil head ratio can reach more than 30%, the demulsifier can be ensured to be fully spread on an oil-water interface of an emulsion, the swept area is large, the collision probability of the demulsifier to dispersed water drops is improved, and the dehydration rate is improved. The demulsifier has high dehydration speed, can remove clear sewage, can effectively remove an emulsification intermediate layer, and has the demulsification rate of more than 98 percent.
Description
Technical Field
The invention belongs to the technical field of chemical agents, and particularly relates to a polymer flooding produced fluid demulsifier and a preparation method thereof.
Background
Oil fields such as Daqing, Shengli and the like in China generally enter the middle and later stages of development, the development difficulty is continuously increased, the water content rises quickly, the primary and secondary oil extraction technologies cannot meet the requirements of oil field exploitation, and a new oil displacement technology is urgently needed. Polymer flooding is a mature and efficient recovery efficiency improving technology and is widely applied to oil fields. The polymer used in the polymer flooding is mostly polyacrylamide and a modifier thereof, the polymer is reacted from the ground to the underground for a long time and then reaches the ground, the polymer becomes an amphiphilic polymer with relatively small molecular mass, and compared with crude oil produced by a conventional mode, the demulsification difficulty of the polymer flooding produced fluid is higher.
The oil-water sedimentation separation speed of the polymer flooding produced liquid is reduced, the emulsification interlayer is serious, and the oil content of the sewage is seriously increased along with the increase of the solubility of the polymer. The polymer flooding produced liquid has low oil-water interface tension and high viscosity, the demulsifier molecules have high diffusion difficulty on the oil-water interface, and the coalescence difficulty of water drops and oil droplets is high. The conventional resin demulsifier generally has large molecular weight, poor diffusion capability at an oil-water interface and poor demulsification effect, and cannot meet the demulsification requirement of polymer flooding produced fluid.
Therefore, the development of a demulsifier for polymer flooding produced fluid, which has a large initiator ratio, a relatively small molecular weight, a higher surface activity, a high dehydration speed and a clear wastewater removal, is urgent.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the polymer flooding produced liquid demulsifier and the preparation method thereof. The demulsifier is a block copolymer generated by grafting propylene oxide and ethylene oxide through a self-made novel initiator.
In order to achieve the purpose, the invention adopts the following technical scheme:
the polymer flooding produced liquid demulsifier is a block copolymer generated by grafting propylene oxide and ethylene oxide onto an octyl phenolic resin initiator.
The reaction equation is as follows:
wherein, P is more than or equal to 15 and more than or equal to 5, preferably more than or equal to 10 and more than or equal to 5;
m is more than or equal to 15 and more than or equal to 3, preferably more than or equal to 10 and more than or equal to 3;
15≥m1not less than 3, preferably not less than 10 m1≥3；
15≥m2Not less than 3, preferably not less than 10 m2≥3；
20 is more than or equal to n more than or equal to 3, preferably 15 is more than or equal to n more than or equal to 5;
20≥n1not less than 3, preferably not less than 15 n1≥5；
20≥n2Not less than 3, preferably not less than 15 n2≥5。
Preferably, the demulsifier comprises the following components in parts by weight: 20-40 parts of octyl phenolic resin initiator, 30-50 parts of propylene oxide and 20-45 parts of ethylene oxide.
Preferably, the octyl phenol-formaldehyde resin initiator is synthesized by the following method:
adding p-tert-octylphenol into a four-mouth bottle, heating and melting until the material is transparent, and adding a certain amount of formaldehyde solution and a catalyst; starting stirring, heating to reflux temperature, maintaining the temperature for reaction for 2-5 h, stopping heating and stirring, cooling the intermediate to about 60 ℃, adding dimethylbenzene, heating, carrying out reduced pressure distillation, removing dimethylbenzene and water in the system, and cooling and discharging after the quality requirement is met.
Preferably, the heating temperature of the p-tert-octylphenol is 90-100 ℃; the reflux reaction temperature is 110 ℃, and the reaction lasts for 3 hours; the temperature of reduced pressure distillation is 150-160 ℃.
Preferably, the solubility of the formaldehyde solution is 36% (mass ratio); the catalyst is one or two of potassium hydroxide and sodium hydroxide.
Preferably, the mass ratio of the p-tert-octylphenol, the formaldehyde solution, the xylene and the catalyst is as follows: 55-60: 30-35: 10-15: 0.3-0.4.
Preferably, the oil head of the demulsifier accounts for more than 30%, and the demulsification rate is more than 98%.
The invention also discloses a preparation method of the polymer flooding produced liquid demulsifier, which comprises the following steps:
(1) synthesis of octyl phenolic resin initiator: synthesizing an octyl phenol-formaldehyde resin initiator according to the method of any one of claims 3 to 6;
(2) synthesizing a polymer flooding produced liquid demulsifier: putting an octyl phenolic resin initiator into a high-pressure reaction kettle, adding a catalyst, heating to a certain temperature, carrying out vacuum treatment for 30min, closing a vacuum pump, continuously heating to 130 ℃, opening a propylene oxide feeding valve, and carrying out heat preservation reaction to-0.04 MPa after feeding is finished; cooling to about 120 ℃, carrying out vacuum treatment for 30 minutes, after the vacuum treatment is finished, closing a vacuum pump, opening an ethylene oxide feeding valve, after the feeding is finished, carrying out heat preservation reaction to-0.04 MPa, cooling to 120 ℃, carrying out vacuum treatment for 20 minutes, after the vacuum treatment is finished, cooling, adding a neutralizing agent, neutralizing and discharging to obtain the polymer flooding produced liquid demulsifier.
Preferably, the vacuum treatment temperature is 110-120 ℃, and the vacuum degree is more than or equal to 0.9 Mpa; the reaction temperature of the epoxypropane is 135-145 ℃; the reaction temperature of the ethylene oxide is 120-130 ℃; the reaction pressure of the epoxypropane and the epoxyethane is 0.01-0.4 MPa, and the reaction is carried out under the condition of heat preservation until the pressure reaches-0.04 MPa.
Preferably, the catalyst is one or two of potassium hydroxide and sodium hydroxide; the neutralizing agent is acetic acid; the mass ratio of the propylene oxide to the catalyst to the neutralizer is 1000: 3.5-4.0: 3.2 to 4.2.
Advantageous effects
The polymer flooding produced liquid has low oil-water interface, high water phase viscosity, high oil-water emulsification degree, small oil drop and water drop particle size and difficult coalescence. The common oil head ratio of the domestic resin demulsifiers is smaller, generally less than 1%, the molecular weight is larger, the demulsifiers are difficult to disperse in produced liquid, and the swept area is small, so that the dehydration speed and the dehydration rate of the demulsifiers are poor. Compared with the domestic common demulsifier, the invention has the following advantages: the initiator is self-made, the phenolic ratio can be changed as required, the molecular structure of the demulsifier is adjusted, the oil head ratio can reach more than 30%, the demulsifier can be ensured to be fully spread on an oil-water interface of an emulsion, the swept area is large, the collision probability of the demulsifier to dispersed water drops is improved, and the dehydration rate is improved.
The polymer flooding produced liquid demulsifier provided by the invention has the advantages of high dehydration speed, clear wastewater removal, capability of effectively removing an emulsification intermediate layer, wide application in the aspect of treating polymer flooding produced liquid, application to various oil fields at home and abroad, good application effect and capacity of reaching more than 98% of demulsification rate in oil fields such as Daqing, Shengli and the like.
Drawings
FIG. 1: an infrared spectrum of the initiator a synthesized in example 1 of the present invention;
FIG. 2: the infrared spectrum of the demulsifier 1 synthesized in example 1 of the present invention.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Example 1
(1) Synthesis of octyl phenol-formaldehyde resin initiator
253.82g of p-tert-octylphenol is added into a 500ml four-mouth bottle, heated and melted until the material is bright, 138.45 percent of formaldehyde solution (36 percent) and 1.38g of KOH are added; starting stirring, heating to reflux temperature of 110 ℃, keeping the temperature for reaction for 3h, stopping heating and stirring, cooling the intermediate to about 60 ℃, adding 69.22g of dimethylbenzene, slowly heating to 150-160 ℃, carrying out reduced pressure distillation, removing dimethylbenzene and water in the system, cooling and discharging after the quality requirement is met, and obtaining an initiator A, wherein an infrared spectrogram is shown in figure 1.
(2) Synthesis of polymer flooding produced liquid demulsifier
Adding 250g of initiator A into a high-pressure reaction kettle, adding 0.93g of KOH, stirring, heating to 100 ℃, carrying out vacuum treatment for 30min, closing a vacuum pump, continuously heating to 130 ℃, opening a propylene oxide feeding valve (the propylene oxide feeding amount is 233.33g), controlling the temperature to be 135-145 ℃, controlling the reaction pressure to be 0.2-0.4 MPa, carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 30min, closing the vacuum pump after the vacuum treatment is finished, opening an ethylene oxide feeding valve (the ethylene oxide feeding amount is 350g), carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 20 min, carrying out vacuum treatment, cooling, adding 0.98g of acetic acid, cooling and discharging to obtain the demulsifier 1 of the example, wherein an infrared spectrogram is shown in figure 2.
Example 2
Synthesis of polymer flooding produced liquid demulsifier
Adding 250g of initiator A into a high-pressure reaction kettle, adding 0.80g of KOH, stirring, heating to 100 ℃, carrying out vacuum treatment for 30min, closing a vacuum pump, continuously heating to 130 ℃, opening a propylene oxide feeding valve (the propylene oxide feeding amount is 200g), controlling the temperature to be 135-145 ℃, controlling the reaction pressure to be 0.2-0.4 MPa, carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 30min, closing the vacuum pump after the vacuum treatment is finished, opening an ethylene oxide feeding valve (the ethylene oxide feeding amount is 264.29g), carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 20 min, carrying out vacuum treatment, cooling, adding 0.84g of acetic acid, cooling and discharging to obtain the demulsifier 2 in the example.
Example 3
Synthesis of polymer flooding produced liquid demulsifier
Adding 250g of initiator A into a high-pressure reaction kettle, adding 1.33g of KOH, stirring, heating to 100 ℃, carrying out vacuum treatment for 30min, closing a vacuum pump, continuously heating to 130 ℃, opening a propylene oxide feeding valve (the propylene oxide feeding amount is 333.33g), controlling the temperature to be 135-145 ℃, controlling the reaction pressure to be 0.2-0.4 MPa, carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 30min, closing the vacuum pump after the vacuum treatment is finished, opening an ethylene oxide feeding valve (the ethylene oxide feeding amount is 250g), carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 20 min, carrying out vacuum treatment, cooling, adding 1.40g of acetic acid, cooling and discharging to obtain the demulsifier of the example 3.
Example 4
(1) Synthesis of octyl phenol-formaldehyde resin initiator
248.5g of p-tert-octylphenol is added into a 500ml four-mouth bottle, heated and melted until the material is bright, 144.96 formaldehyde solution (36 percent) and 1.66g of KOH are added; starting stirring, heating to a reflux temperature of 110 ℃, maintaining the temperature for reaction for 3 hours, stopping heating and stirring, cooling the intermediate to about 60 ℃, adding 62.13g of dimethylbenzene, slowly heating to 150-160 ℃, carrying out reduced pressure distillation, removing dimethylbenzene and water in the system, cooling after the quality requirement is met, and discharging to obtain the initiator B.
(2) Synthesis of polymer flooding produced liquid demulsifier
Adding 250g of initiator B into a high-pressure reaction kettle, adding 0.93g of KOH, stirring, heating to 100 ℃, carrying out vacuum treatment for 30min, closing a vacuum pump, continuously heating to 130 ℃, opening a propylene oxide feeding valve (the propylene oxide feeding amount is 233.33g), controlling the temperature to be 135-145 ℃, controlling the reaction pressure to be 0.2-0.4 MPa, carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 30min, closing the vacuum pump after the vacuum treatment is finished, opening an ethylene oxide feeding valve (the ethylene oxide feeding amount is 350g), carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 20 min, carrying out vacuum treatment, cooling, adding 0.98g of acetic acid, cooling and discharging to obtain the demulsifier 4 of the example.
Example 5
Synthesis of polymer flooding produced liquid demulsifier
Adding 250g of initiator B into a high-pressure reaction kettle, adding 0.80g of KOH, stirring, heating to 100 ℃, carrying out vacuum treatment for 30min, closing a vacuum pump, continuously heating to 130 ℃, opening a propylene oxide feeding valve (the propylene oxide feeding amount is 200g), controlling the temperature to be 135-145 ℃, controlling the reaction pressure to be 0.2-0.4 MPa, carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 30min, closing the vacuum pump after the vacuum treatment is finished, opening an ethylene oxide feeding valve (the ethylene oxide feeding amount is 264.29g), carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 20 min, carrying out vacuum treatment, cooling, adding 0.84g of acetic acid, cooling and discharging to obtain the demulsifier 5 in the example.
Example 6
Synthesis of polymer flooding produced liquid demulsifier
Adding 250g of initiator B into a high-pressure reaction kettle, adding 1.03g of KOH, stirring, heating to 100 ℃, carrying out vacuum treatment for 30min, closing a vacuum pump, continuously heating to 130 ℃, opening a propylene oxide feeding valve (the feeding amount of propylene oxide is 257.58g), controlling the temperature to be 135-145 ℃, controlling the reaction pressure to be 0.2-0.4 MPa, carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 30min, closing the vacuum pump after the vacuum treatment is finished, opening an ethylene oxide feeding valve (the feeding amount of ethylene oxide is 250g), carrying out heat preservation reaction to-0.04 MPa after the feeding is finished, cooling to 120 ℃, carrying out vacuum treatment for 20 min, carrying out vacuum treatment, cooling, adding 1.08g of acetic acid, cooling and discharging to obtain the demulsifier of the example 6.
Example 7 demulsifier indoor evaluation experiment
The produced fluid of Daqing oilfield polymer flooding is subjected to a bottle test demulsification experiment.
The demulsification experiment refers to a petroleum and natural gas industry standard SY/T5281-2000 & lt & gt crude oil demulsifier use performance detection method (bottle test method) & gt of the people's republic of China, and the crude oil water content measurement refers to a crude oil water content measurement distillation method & lt & gt of the people's republic of China GB/T8929 & lt & gt 2006 & gt crude oil water content.
The polymer flooding produced fluid demulsifier synthesized by the above example is compared with the field demulsifier and the common polymer flooding demulsifier, and the experimental results are shown in table 1.
TABLE 1.50 deg.C demulsification experiment for Daqing oilfield polymer flooding produced fluids
And (4) analyzing results: compared with other demulsifiers, the new synthesized demulsifier has better demulsification effect, better dehydration rate than field agents, dehydration rate of more than 98.5 percent, clear removed sewage and thin middle layer under the conditions of dosage of 60ppm and demulsification temperature of 50 ℃ for crude oil of the combined station.
Example 8 demulsifier indoor evaluation experiment
A bottle test demulsification experiment is carried out on polymer flooding produced fluid of a victory oil field island oil production plant.
The polymer flooding produced fluid demulsifier synthesized by the above example is compared with the field demulsifier and the common polymer flooding demulsifier, and the experimental results are shown in table 2.
TABLE 2.70 deg.C demulsification experiment for polymer flooding produced fluid of victory oil field island oil production plant
And (4) analyzing results: compared with other demulsifiers, the new synthesized demulsifier has better demulsification effect, better dehydration rate than field-used agents and higher dehydration rate than 98.5% under the conditions of the dosage of 100ppm and the demulsification temperature of 70 ℃ of crude oil of the united station.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (10)
1. The polymer flooding produced liquid demulsifier is characterized in that the demulsifier is a block copolymer generated by grafting propylene oxide and ethylene oxide on an octyl phenolic resin initiator.
2. The polymer flooding production fluid demulsifier of claim 1, wherein the demulsifier has the following chemical structural formula:
wherein P is more than or equal to 15 and more than or equal to 5; m is more than or equal to 15 and more than or equal to 3; 15 is more than or equal to m1≥3；15≥m2≥3；20≥n≥3；20≥n1≥3；20≥n2≥3。
3. The polymer flooding produced fluid demulsifier of claim 2, wherein 10 is greater than or equal to P is greater than or equal to 5; m is more than or equal to 10 and more than or equal to 3; m1 is more than or equal to 10 and more than or equal to 3; m2 is more than or equal to 10 and more than or equal to 3; n is more than or equal to 15 and more than or equal to 5; 15 is more than or equal to n1 is more than or equal to 5; 15 is more than or equal to n2 is more than or equal to 5.
4. The polymer flooding produced fluid demulsifier of claim 1, wherein the demulsifier comprises the following components in parts by weight: 20-40 parts of octyl phenolic resin initiator, 30-50 parts of propylene oxide and 20-45 parts of ethylene oxide.
5. The polymer flooding production fluid demulsifier of claim 1, wherein the octyl phenolic resin initiator is synthesized by the following method:
adding p-tert-octylphenol into a reaction vessel, heating and melting until the materials are transparent, adding a formaldehyde solution and a catalyst, carrying out reflux reaction, cooling after the reaction is finished, adding xylene, heating, carrying out reduced pressure distillation, removing xylene and water in the system, cooling, and discharging to obtain the octyl phenolic resin initiator.
6. The polymer flooding produced fluid demulsifier of claim 5, wherein the heating temperature of p-tert-octylphenol is 90-100 ℃; the reflux reaction temperature is 110 ℃, and the reaction lasts for 3 hours; the temperature of reduced pressure distillation is 150-160 ℃; the solubility of the formaldehyde solution is 36 percent (mass ratio); the catalyst is one or two of potassium hydroxide and sodium hydroxide; the mass ratio of the p-tert-octylphenol to the formaldehyde solution to the xylene to the catalyst is as follows: 55-60: 30-35: 10-15: 0.3-0.4.
7. The polymer flooding produced fluid demulsifier of any one of claims 1-6, wherein the oil head percentage of the demulsifier is up to 30% or more, and the demulsification rate is up to 98% or more.
8. A preparation method of a polymer flooding produced liquid demulsifier is characterized by comprising the following steps:
(1) synthesis of octyl phenolic resin initiator: synthesizing an octyl phenol-formaldehyde resin initiator according to the method of any one of claims 3 to 6;
(2) synthesizing a polymer flooding produced liquid demulsifier: putting an octyl phenolic resin initiator into a reaction vessel, adding a catalyst, carrying out vacuum treatment, feeding propylene oxide, and carrying out heat preservation reaction; cooling, vacuum treatment, feeding ethylene oxide, and heat preservation reaction; cooling, vacuum treating, cooling, adding a neutralizing agent, neutralizing and discharging to obtain the polymer flooding produced liquid demulsifier.
9. The preparation method of the polymer flooding produced liquid demulsifier according to claim 8, wherein the vacuum treatment temperature is 110-120 ℃, and the vacuum degree is not less than 0.9 Mpa; the reaction temperature of the epoxypropane is 135-145 ℃; the reaction temperature of the ethylene oxide is 120-130 ℃; the reaction pressure of the epoxypropane and the epoxyethane is 0.01-0.4 MPa, and the reaction is carried out under the condition of heat preservation until the pressure reaches-0.04 MPa.
10. The method for preparing the demulsifier for polymer flooding produced fluid according to claim 1, wherein the catalyst is one or both of potassium hydroxide and sodium hydroxide; the neutralizing agent is acetic acid; the mass ratio of the propylene oxide to the catalyst to the neutralizer is 1000: 3.5-4.0: 3.2 to 4.2.
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Effective date of registration: 20221221 Address after: No.869, Huanghe 5th Road, Bincheng District, Binzhou City, Shandong Province Applicant after: Binhua Technology Co.,Ltd. Applicant after: BEFAR GROUP Co.,Ltd. Applicant after: SHANDONG BEFAR DONGRUI CHEMICAL CO.,LTD. Address before: 256600 No. 888, Huanghe fifth road, Bincheng District, Binzhou City, Shandong Province Applicant before: BEFAR GROUP Co.,Ltd. Applicant before: SHANDONG BEFAR DONGRUI CHEMICAL CO.,LTD. |