CN112457877B - Preparation method of high-dehydration-rate oil field demulsifier - Google Patents
Preparation method of high-dehydration-rate oil field demulsifier Download PDFInfo
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- 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
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/04—Dewatering or demulsification of hydrocarbon oils with chemical means
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Abstract
The invention belongs to the technical field of oil gas development assistants, and particularly relates to a preparation method of a high-dehydration-rate oil field demulsifier, which comprises the following raw materials in parts by weight: 2-4 parts of demulsifying component, 6-8 parts of auxiliary component, 40-50 parts of deionized water, 10-12 parts of ethylene glycol monobutyl ether and 10-20 parts of Ninol; the preparation method of the high dehydration rate oil field demulsifier comprises the following steps: firstly, preparing demulsifying components and auxiliary components; and secondly, mixing the demulsifying component and the auxiliary component, adding deionized water, stirring for dissolving, then adding ethylene glycol monobutyl ether and Ninol, stirring and mixing for 10-20min at the temperature of 25 +/-2 ℃, so as to obtain the high-dehydration-rate oil field demulsifying agent, wherein dodecylamine has hydrophobicity, sugar rings on sodium alginate have hydrophilicity, the demulsifying component with both hydrophilic groups and hydrophobic groups is prepared, the processed chitosan is grafted on silicon dioxide nano particles, and the prepared auxiliary component is matched with the demulsifying component, so that the dehydration rate of crude oil is improved.
Description
Technical Field
The invention belongs to the technical field of oil and gas development auxiliaries, and particularly relates to a preparation method of a high-dehydration-rate oil field demulsifier.
Background
In oil recovery, crude oil often contains moisture and impurity salts. In order to improve the quality of crude oil and reduce the transportation cost, a demulsifier is generally added to remove water and impurity salts from the crude oil. The demulsifier used in China at present mainly comprises polyether single demulsifier. Because the crude oil has complex components and different molecular weights, the application effect of the polyether single demulsifier is not ideal, and the application range of the polyether single demulsifier is relatively narrow.
Disclosure of Invention
The invention provides an oil field demulsifier with high dehydration rate and a preparation method thereof.
The technical problems to be solved by the invention are as follows: the traditional demulsifier has the problems of low dehydration rate, turbid water quality, poor dehydration effect, large use amount and incapability of achieving ideal demulsification effect.
The purpose of the invention can be realized by the following technical scheme:
the high-dehydration-rate oil field demulsifier comprises the following raw materials in parts by weight: 2-4 parts of demulsifying component, 6-8 parts of auxiliary component, 40-50 parts of deionized water, 10-12 parts of ethylene glycol monobutyl ether and 10-20 parts of Ninol;
the high dehydration rate oil field demulsifier is prepared by the following steps:
firstly, preparing demulsifying components and auxiliary components;
secondly, mixing the demulsifying component and the auxiliary component, adding deionized water, stirring and dissolving, then adding ethylene glycol monobutyl ether and Ninol, and stirring and mixing for 10-20min at the temperature of 25 +/-2 ℃ to obtain the high-dehydration-rate oil field demulsifier;
the demulsifying component is prepared by the following steps:
step S11, mixing sodium alginate and absolute ethyl alcohol, setting the temperature to be 30 +/-2 ℃, stirring for 6-10min, adding a sodium periodate aqueous solution, keeping the temperature unchanged, reacting for 6 +/-1 h in a dark place, adding ethylene glycol after the reaction is finished, continuously stirring for 10 +/-2 min, then carrying out vacuum filtration, and washing the obtained filter cake for multiple times by using the ethanol aqueous solution to obtain a solid a;
step S12, setting the temperature to be 50 +/-5 ℃, mixing the solid a and deionized water, adding the mixture into dodecylamine, stirring for reaction for 12 +/-2 hours, setting the temperature to be 0-5 ℃ after the reaction is finished, adding sodium borohydride, continuing stirring for reaction for 12 +/-2 hours, mixing the obtained reaction liquid with three to five times of volume of absolute ethyl alcohol, separating out a precipitate, carrying out vacuum filtration, and carrying out vacuum freeze drying on the obtained filter cake to obtain a solid b;
step S13, mixing an antibacterial agent and distilled water, setting the temperature to be 30 +/-2 ℃, adding the solid b, stirring and reacting for 4-8 hours, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake with deionized water, and drying at 40 +/-2 ℃ to constant weight to obtain a demulsifying component;
the auxiliary components are prepared by the following steps:
step S31, adjusting the pH value of deionized water to 7-8 by using sodium hydroxide, setting the temperature to 50-60 ℃, adding hexadecyl trimethyl ammonium bromide, stirring for 30 +/-5 min, then dropwise adding tetraethoxysilane while stirring, keeping the temperature unchanged after dropwise adding, continuously stirring for 20-24h, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake by using deionized water and absolute ethyl alcohol in sequence, after the washing is finished, carrying out vacuum drying for 2h at the temperature of 80 +/-2 ℃, and then calcining for 6 +/-1 h at the temperature of 550 +/-10 ℃ to obtain a solid d;
step S32, mixing chitosan and acetic acid solution with the mass fraction of 1 +/-0.5%, setting the temperature to be 25 +/-2 ℃, dropwise adding the sodium perfluorononanoate solution while stirring, keeping the temperature unchanged after dropwise adding, and continuously stirring for 10 +/-2 min to obtain suspension;
step S33, mixing the solid d with absolute ethyl alcohol, carrying out ultrasonic treatment for 15 +/-5 min, adjusting the pH value to 3-5 with glacial acetic acid, adding gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and stirring for 3h at the temperature of 25 +/-2 ℃; adding the suspension obtained in the step S32 after stirring, keeping the temperature unchanged, continuously stirring for 24 +/-2 hours, then centrifuging, washing the obtained lower-layer precipitate with absolute ethyl alcohol and deionized water, and after washing, carrying out vacuum freeze drying to obtain auxiliary components;
the antibacterial agent is prepared by the following steps:
step S21, adding 9-bromo-1-nonanol and triethylamine into a three-neck flask, adding dichloromethane, setting the temperature to be 0-5 ℃, dropwise adding methacryloyl chloride while stirring, continuing to react for 24 +/-2 hours at the temperature of 20 +/-2 ℃ after dropwise adding, and evaporating the obtained reaction liquid to remove dichloromethane after the reaction is finished to obtain an intermediate c;
and step S22, adding the intermediate c, triphenylphosphine, hydroquinone and acetonitrile into a three-neck flask, setting the temperature to be 80 +/-2 ℃, stirring and reacting for 72 +/-2 hours, evaporating the obtained reaction liquid to remove the acetonitrile after the reaction is finished, and drying at 40 +/-2 ℃ to constant weight to obtain the antibacterial agent.
Further preferably, the demulsifying component is prepared by:
step S11, mixing sodium alginate and absolute ethyl alcohol, setting the temperature to be 30 +/-2 ℃ and the rotating speed to be 400r/min, stirring for 6-10min, adding a sodium periodate aqueous solution, keeping the temperature and the rotating speed unchanged, reacting for 6 +/-1 h in a dark place, after the reaction is finished, adding ethylene glycol, continuing stirring for 10 +/-2 min, then carrying out vacuum filtration, and washing the obtained filter cake for three times by using an ethanol aqueous solution with the volume fraction of 70% to obtain a solid a;
s12, setting the temperature to be 50 +/-5 ℃ and the rotating speed to be 400r/min, mixing the solid a and deionized water, adding the mixture into dodecylamine, stirring and reacting for 12 +/-2 hours, setting the temperature to be 0-5 ℃ after the reaction is finished, keeping the rotating speed unchanged, adding sodium borohydride, continuing stirring and reacting for 12 +/-2 hours, mixing the obtained reaction liquid with three to five volumes of absolute ethyl alcohol, separating out a precipitate, carrying out vacuum filtration, and carrying out vacuum freeze drying on the obtained filter cake at-60 ℃ to obtain a solid b;
and step S13, adding the antibacterial agent and distilled water into a three-neck flask, mixing, setting the temperature to be 30 +/-2 ℃ and the rotating speed to be 500r/min, adding the solid b, stirring and reacting for 4-8h, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake with deionized water, and drying at 40 +/-2 ℃ to constant weight to obtain the demulsifying component. Sodium periodate oxidizes a sugar ring part on a sodium alginate molecular chain into an aldehyde group, nucleophilic addition is carried out on the oxidized aldehyde group and an amino group in dodecylamine, dodecylamine is connected onto the molecular chain of the sodium alginate in a carbon-nitrogen double bond mode, then the carbon-nitrogen double bond is reduced into a CH-NH group under the reduction action of sodium borohydride, the prepared solid b has an amphiphilic structure, and-COONa on the sodium alginate molecular chain is subjected to ion exchange with an antibacterial agent, so that the antibacterial agent is grafted onto the molecular chain of the sodium alginate.
Further, in step S11, the sodium periodate aqueous solution is sodium periodate and deionized water according to the dosage ratio of 3 mol: 1L of sodium alginate, absolute ethyl alcohol, sodium periodate aqueous solution and glycol, wherein the dosage ratio of the sodium alginate to the absolute ethyl alcohol to the sodium periodate aqueous solution is 5 g: (50-60 mL): 50mL of: 5 mL; and in the step S12, adding the sodium borohydride in three times of equal amount, wherein the dosage ratio of the solid a, the deionized water, the dodecylamine and the sodium borohydride is 5 g: 120mL of: (4.6-5 g): (0.8-0.9 g); in step S13, the dosage ratio of the antibacterial agent to the distilled water to the solid b is (50-60 mg): 10mL of: (1-3 g).
Further preferably, the antibacterial agent is prepared by the steps of:
step S21, adding 9-bromo-1-nonanol and triethylamine into a three-neck flask, adding dichloromethane, setting the temperature to be 0-5 ℃ and the rotating speed to be 300r/min, dropwise adding methacryloyl chloride while stirring, wherein the dropwise adding time is 2h, continuing to react for 24h at the temperature of 20 ℃ after dropwise adding, and after the reaction is finished, rotationally evaporating the obtained reaction liquid on a rotary evaporator to remove dichloromethane to obtain an intermediate c;
and step S22, adding the intermediate c, triphenylphosphine, hydroquinone and acetonitrile into a three-neck flask, setting the temperature at 80 ℃ and the rotating speed at 500r/min, stirring for reaction for 72 hours, removing the acetonitrile from the obtained reaction liquid by using a rotary evaporator after the reaction is finished, and drying at 40 +/-2 ℃ to constant weight to obtain the antibacterial agent. The antibacterial agent is a quaternary phosphonium salt compound, the quaternary phosphonium salt has higher thermal stability compared with quaternary ammonium salt, and the demulsifying component containing the quaternary phosphonium salt group has temperature resistance.
Further, in step S21, the use ratio of 9-bromo-1-nonanol, triethylamine, dichloromethane and methacryloyl chloride is 0.18 mol: (0.18-0.19 mol): 100mL of: 0.19 mol; in the step S22, the dosage ratio of the intermediate c, the triphenylphosphine, the hydroquinone and the acetonitrile is 2.5 g: 3.8 g: (0.3-0.4 g): 40 mL.
Further preferably, the auxiliary ingredient is prepared by:
step S31, adjusting the pH value of deionized water to 7-8 by using sodium hydroxide, setting the temperature to 50-60 ℃ and the rotating speed to 100r/min, adding hexadecyl trimethyl ammonium bromide, stirring for 30 +/-5 min, then dropwise adding tetraethoxysilane while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, continuing stirring for 20-24h, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake for three times by using deionized water and absolute ethyl alcohol in sequence, after the washing is finished, carrying out vacuum drying at 80 +/-2 ℃ for 2h, and then calcining at 550 +/-10 ℃ for 6 +/-1 h to obtain a solid d;
step S32, mixing chitosan and acetic acid solution with the mass fraction of 1 +/-0.5%, setting the temperature to be 25 +/-2 ℃ and the rotating speed to be 300r/min, dropwise adding the sodium perfluorononanoate solution while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, and continuously stirring for 10 +/-2 min to obtain suspension;
step S33, mixing the solid d with absolute ethyl alcohol, carrying out ultrasonic treatment for 15 +/-5 min under the condition of 40kHz, adjusting the pH value to 3-5 by using glacial acetic acid, adding gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and stirring for 3h at the temperature of 25 +/-2 ℃; and (3) after stirring, adding the suspension obtained in the step S32, keeping the temperature unchanged, continuously stirring for 24 +/-2 h, centrifuging at 7000r/min, washing the obtained lower-layer precipitate for three times by using absolute ethyl alcohol and deionized water, and after washing, drying in vacuum at-70 ℃ for 16h to obtain the auxiliary component. The protonated amino group in the chitosan molecule reacts with sodium perfluorononanoate to fluorinate chitosan, the solid d is mesoporous silica nano-particles with large specific surface area and pore volume, and a coupling agent gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane is used as a bridging agent to graft the treated chitosan onto the silica nano-particles, so that the affinity and the hydrophilicity of the nano-silica are further improved.
Further, in step S31, the ratio of the deionized water to the cetyl trimethyl ammonium bromide to the ethyl orthosilicate is 500 mL: 0.5 g: 3g, the concentration of the sodium perfluorononanate in the step S32 is 0.1mol/L, and the dosage ratio of the chitosan, the acetic acid solution with the mass fraction of 1 +/-0.5% and the sodium perfluorononanate solution is 50 mg: 25mL of: 5 mL; in the step S33, the dosage ratio of the solid d, the absolute ethyl alcohol and the gamma- (2,3 epoxypropoxy) propyl trimethoxy silane is 1 g: 100mL of: 0.2 g; the dosage ratio of the solid d to the suspension is 1 g: (6-10 mL).
The invention has the beneficial effects that:
sodium periodate oxidizes the sugar ring part on the molecular chain of sodium alginate into aldehyde group, nucleophilic addition is carried out between the oxidized aldehyde group and the amino group in dodecylamine, dodecylamine is connected to the molecular chain of sodium alginate in the form of carbon-nitrogen double bond, then the carbon-nitrogen double bond is reduced into CH-NH group under the reduction action of sodium borohydride, the prepared solid b has an amphiphilic structure, the-COONa on the molecular chain of sodium alginate and an antibacterial agent are subjected to ion exchange, the antibacterial agent is grafted to the molecular chain of sodium alginate, the dodecylamine contains long-chain alkyl which has hydrophobicity, the sugar ring on the molecular chain of sodium alginate has hydrophilicity, the demulsifying component with both hydrophilic group and hydrophobic group is prepared, and in the using process, nano-scale particles with inward hydrophobic group and outward hydrophilic group are formed. The antibacterial agent is a quaternary phosphonium salt compound, the quaternary phosphonium salt has higher thermal stability compared with quaternary ammonium salt, the demulsifying component containing the quaternary phosphonium salt group has temperature resistance, and the quaternary phosphonium salt group migrates to the surface of the demulsifying component, so that the cation density is greatly increased, and the demulsifying component is endowed with antibacterial property.
The protonized amino in chitosan molecules reacts with sodium perfluorononanoate to fluorinate chitosan, solid d is mesoporous silica nanoparticles with large specific surface area and pore volume, coupling agent gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane is used as a bridging agent to graft the treated chitosan onto the silica nanoparticles to prepare auxiliary components, so that the affinity and the hydrophilicity of the nano-silica are further improved, the auxiliary components can more easily penetrate through an oil-water interface membrane to obtain a water phase, the density of the water phase is increased, the membrane drainage and phase separation processes are facilitated, the auxiliary components are matched with demulsifying components, the oil-water interface tension and the interface membrane strength are reduced, the interface membrane is damaged, the demulsifying effect is achieved, and the dehydration rate of crude oil is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the case where no particular mention is made, commercially available conventional products are used as the starting materials in the respective examples.
Example 1
The high-dehydration-rate oil field demulsifier comprises the following raw materials in parts by weight: 2 parts of demulsifying component, 6 parts of auxiliary component, 40 parts of deionized water, 10 parts of ethylene glycol monobutyl ether and 10 parts of Ninol;
the high dehydration rate oil field demulsifier is prepared by the following steps:
firstly, preparing demulsifying components and auxiliary components;
and secondly, mixing the demulsifying component and the auxiliary component, adding deionized water, stirring and dissolving, then adding ethylene glycol monobutyl ether and Ninol, and stirring and mixing for 10min at the temperature of 25 +/-2 ℃ to obtain the high-dehydration-rate oil field demulsifier.
Wherein the demulsifying component is prepared by the following steps:
step S11, mixing sodium alginate and absolute ethyl alcohol, setting the temperature to be 30 +/-2 ℃ and the rotating speed to be 400r/min, stirring for 6min, adding a sodium periodate aqueous solution, keeping the temperature and the rotating speed unchanged, reacting for 6 +/-1 h in a dark place, after the reaction is finished, adding ethylene glycol, continuing stirring for 10 +/-2 min, then carrying out vacuum filtration, and washing the obtained filter cake for three times by using an ethanol aqueous solution with the volume fraction of 70% to obtain a solid a;
step S12, setting the temperature to be 50 +/-5 ℃ and the rotating speed to be 400r/min, mixing the solid a and deionized water, adding the mixture into dodecylamine, stirring and reacting for 12 +/-2 hours, setting the temperature to be 0 ℃ after the reaction is finished, keeping the rotating speed unchanged, adding sodium borohydride, continuing stirring and reacting for 12 +/-2 hours, mixing the obtained reaction liquid with three to five volumes of absolute ethyl alcohol, separating out a precipitate, carrying out vacuum filtration, and carrying out vacuum freeze drying on the obtained filter cake at-60 ℃ to obtain a solid b;
and step S13, adding the antibacterial agent and distilled water into a three-neck flask, mixing, setting the temperature to be 30 +/-2 ℃ and the rotating speed to be 500r/min, adding the solid b, stirring for reaction for 4 hours, carrying out vacuum filtration after the reaction is finished, washing the obtained filter cake with deionized water, and drying at 40 +/-2 ℃ to constant weight to obtain the demulsifying component.
Wherein, in the step S11, the sodium periodate aqueous solution is sodium periodate and deionized water according to the dosage ratio of 3 mol: 1L of sodium alginate, absolute ethyl alcohol, sodium periodate aqueous solution and glycol, wherein the dosage ratio of the sodium alginate to the absolute ethyl alcohol to the sodium periodate aqueous solution is 5 g: 50mL of: 50mL of: 5 mL; and in the step S12, adding the sodium borohydride in three times of equal amount, wherein the dosage ratio of the solid a, the deionized water, the dodecylamine and the sodium borohydride is 5 g: 120mL of: 4.6 g: 0.8 g; in step S13, the ratio of the antibacterial agent to the distilled water to the solid b is 50 mg: 10mL of: 1g of the total weight of the composition.
Wherein the antibacterial agent is prepared by the following steps:
step S21, adding 9-bromo-1-nonanol and triethylamine into a three-neck flask, adding dichloromethane, setting the temperature at 0 ℃ and the rotation speed at 300r/min, dropwise adding methacryloyl chloride while stirring, wherein the dropwise adding time is 2 hours, continuing to react for 24 hours at the temperature of 20 ℃ after the dropwise adding is finished, and after the reaction is finished, performing rotary evaporation on the obtained reaction solution on a rotary evaporator to remove dichloromethane to obtain an intermediate c;
and step S22, adding the intermediate c, triphenylphosphine, hydroquinone and acetonitrile into a three-neck flask, setting the temperature at 80 ℃ and the rotating speed at 500r/min, stirring for reaction for 72 hours, removing the acetonitrile from the obtained reaction liquid by using a rotary evaporator after the reaction is finished, and drying at 40 +/-2 ℃ to constant weight to obtain the antibacterial agent.
Wherein the dosage ratio of the 9-bromo-1-nonanol, the triethylamine, the dichloromethane and the methacryloyl chloride in the step S21 is 0.18 mol: 0.18 mol: 100mL of: 0.19 mol; in the step S22, the dosage ratio of the intermediate c, the triphenylphosphine, the hydroquinone and the acetonitrile is 2.5 g: 3.8 g: 0.3 g: 40 mL.
Wherein, the auxiliary components are prepared by the following steps:
step S31, adjusting the pH value of deionized water to 7 by using sodium hydroxide, setting the temperature to be 50 +/-5 ℃ and the rotating speed to be 100r/min, adding hexadecyl trimethyl ammonium bromide, stirring for 30 +/-5 min, then dropwise adding tetraethoxysilane while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, continuing stirring for 20h, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake for three times by using deionized water and absolute ethyl alcohol in sequence, after the washing is finished, carrying out vacuum drying for 2h at the temperature of 80 +/-2 ℃, and then calcining for 6 +/-1 h at the temperature of 550 +/-10 ℃ to obtain a solid d;
step S32, mixing chitosan and acetic acid solution with the mass fraction of 1 +/-0.5%, setting the temperature to be 25 +/-2 ℃ and the rotating speed to be 300r/min, dropwise adding the sodium perfluorononanoate solution while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, and continuously stirring for 10 +/-2 min to obtain suspension;
step S33, mixing the solid d with absolute ethyl alcohol, carrying out ultrasonic treatment for 15 +/-5 min under the condition of 40kHz, adjusting the pH value to 3 by using glacial acetic acid, adding gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and stirring for 3h under the condition of 25 +/-2 ℃; and (3) after stirring, adding the suspension obtained in the step S32, keeping the temperature unchanged, continuously stirring for 24 +/-2 h, centrifuging at 7000r/min, washing the obtained lower-layer precipitate for three times by using absolute ethyl alcohol and deionized water, and after washing, drying in vacuum at-70 ℃ for 16h to obtain the auxiliary component.
Wherein the dosage ratio of the deionized water, the hexadecyl trimethyl ammonium bromide and the ethyl orthosilicate in the step S31 is 500 mL: 0.5 g: 3g, the concentration of the sodium perfluorononanate in the step S32 is 0.1mol/L, and the dosage ratio of the chitosan, the acetic acid solution with the mass fraction of 1 +/-0.5% and the sodium perfluorononanate solution is 50 mg: 25mL of: 5 mL; in the step S33, the dosage ratio of the solid d, the absolute ethyl alcohol and the gamma- (2,3 epoxypropoxy) propyl trimethoxy silane is 1 g: 100mL of: 0.2 g; the dosage ratio of the solid d to the suspension is 1 g: 6 mL.
Example 2
The high-dehydration-rate oil field demulsifier comprises the following raw materials in parts by weight: 3 parts of demulsifying component, 7 parts of auxiliary component, 45 parts of deionized water, 11 parts of ethylene glycol monobutyl ether and 15 parts of Ninol;
the high dehydration rate oil field demulsifier is prepared by the following steps:
firstly, preparing demulsifying components and auxiliary components;
and secondly, mixing the demulsifying component and the auxiliary component, adding deionized water, stirring and dissolving, then adding ethylene glycol monobutyl ether and Ninol, and stirring and mixing for 15min at the temperature of 25 +/-2 ℃ to obtain the high-dehydration-rate oil field demulsifier.
Wherein the demulsifying component is prepared by the following steps:
step S11, mixing sodium alginate and absolute ethyl alcohol, setting the temperature to be 30 +/-2 ℃ and the rotating speed to be 400r/min, stirring for 8min, adding a sodium periodate aqueous solution, keeping the temperature and the rotating speed unchanged, reacting for 6 +/-1 h in a dark place, after the reaction is finished, adding ethylene glycol, continuing stirring for 10 +/-2 min, then carrying out vacuum filtration, and washing the obtained filter cake for three times by using an ethanol aqueous solution with the volume fraction of 70% to obtain a solid a;
s12, setting the temperature to be 50 +/-5 ℃ and the rotating speed to be 400r/min, mixing the solid a and deionized water, adding the mixture into dodecylamine, stirring and reacting for 12 +/-2 hours, setting the temperature to be 2 ℃ after the reaction is finished, keeping the rotating speed unchanged, adding sodium borohydride, continuing stirring and reacting for 12 +/-2 hours, mixing the obtained reaction liquid with four times of volume of absolute ethyl alcohol, separating out a precipitate, carrying out vacuum filtration, and carrying out vacuum freeze drying on the obtained filter cake at-60 ℃ to obtain a solid b;
and step S13, adding the antibacterial agent and distilled water into a three-neck flask, mixing, setting the temperature to be 30 +/-2 ℃ and the rotating speed to be 500r/min, adding the solid b, stirring and reacting for 6 hours, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake with deionized water, and drying at 40 +/-2 ℃ to constant weight to obtain the demulsifying component.
Wherein, in the step S11, the sodium periodate aqueous solution is sodium periodate and deionized water according to the dosage ratio of 3 mol: 1L of sodium alginate, absolute ethyl alcohol, sodium periodate aqueous solution and glycol, wherein the dosage ratio of the sodium alginate to the absolute ethyl alcohol to the sodium periodate aqueous solution is 5 g: 55mL of: 50mL of: 5 mL; and in the step S12, adding the sodium borohydride in three times of equal amount, wherein the dosage ratio of the solid a, the deionized water, the dodecylamine and the sodium borohydride is 5 g: 120mL of: 4.8 g: 0.8 g; in step S13, the ratio of the antibacterial agent to the distilled water to the solid b is 55 mg: 10mL of: 2g of the total weight.
Wherein the antibacterial agent is prepared by the following steps:
step S21, adding 9-bromo-1-nonanol and triethylamine into a three-neck flask, adding dichloromethane, setting the temperature to be 2 ℃ and the rotating speed to be 300r/min, dropwise adding methacryloyl chloride while stirring, wherein the dropwise adding time is 2 hours, continuing to react for 24 hours at the temperature of 20 ℃ after the dropwise adding is finished, and after the reaction is finished, performing rotary evaporation on the obtained reaction liquid on a rotary evaporator to remove dichloromethane to obtain an intermediate c;
and step S22, adding the intermediate c, triphenylphosphine, hydroquinone and acetonitrile into a three-neck flask, setting the temperature at 80 ℃ and the rotating speed at 500r/min, stirring for reaction for 72 hours, removing the acetonitrile from the obtained reaction liquid by using a rotary evaporator after the reaction is finished, and drying at 40 +/-2 ℃ to constant weight to obtain the antibacterial agent.
Wherein the dosage ratio of the 9-bromo-1-nonanol, the triethylamine, the dichloromethane and the methacryloyl chloride in the step S21 is 0.18 mol: 0.18 mol: 100mL of: 0.19 mol; in the step S22, the dosage ratio of the intermediate c, the triphenylphosphine, the hydroquinone and the acetonitrile is 2.5 g: 3.8 g: 0.3 g: 40 mL.
Wherein, the auxiliary components are prepared by the following steps:
step S31, adjusting the pH value of deionized water to 7 by using sodium hydroxide, setting the temperature to 55 ℃ and the rotating speed to 100r/min, adding hexadecyl trimethyl ammonium bromide, stirring for 30 +/-5 min, then dropwise adding tetraethoxysilane while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, continuing stirring for 22h, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake for three times by using deionized water and absolute ethyl alcohol in sequence, after the washing is finished, carrying out vacuum drying for 2h at the temperature of 80 +/-2 ℃, and then calcining for 6 +/-1 h at the temperature of 550 +/-10 ℃ to obtain a solid d;
step S32, mixing chitosan and acetic acid solution with the mass fraction of 1 +/-0.5%, setting the temperature to be 25 +/-2 ℃ and the rotating speed to be 300r/min, dropwise adding the sodium perfluorononanoate solution while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, and continuously stirring for 10 +/-2 min to obtain suspension;
step S33, mixing the solid d with absolute ethyl alcohol, carrying out ultrasonic treatment for 15 +/-5 min under the condition of 40kHz, adjusting the pH value to 4 by using glacial acetic acid, adding gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and stirring for 3h under the condition of 25 +/-2 ℃; and (3) after stirring, adding the suspension obtained in the step S32, keeping the temperature unchanged, continuously stirring for 24 +/-2 h, centrifuging at 7000r/min, washing the obtained lower-layer precipitate for three times by using absolute ethyl alcohol and deionized water, and after washing, drying in vacuum at-70 ℃ for 16h to obtain the auxiliary component.
Wherein the dosage ratio of the deionized water, the hexadecyl trimethyl ammonium bromide and the ethyl orthosilicate in the step S31 is 500 mL: 0.5 g: 3g, the concentration of the sodium perfluorononanate in the step S32 is 0.1mol/L, and the dosage ratio of the chitosan, the acetic acid solution with the mass fraction of 1 +/-0.5% and the sodium perfluorononanate solution is 50 mg: 25mL of: 5 mL; in the step S33, the dosage ratio of the solid d, the absolute ethyl alcohol and the gamma- (2,3 epoxypropoxy) propyl trimethoxy silane is 1 g: 100mL of: 0.2 g; the dosage ratio of the solid d to the suspension is 1 g: 8 mL.
Example 3
The high-dehydration-rate oil field demulsifier comprises the following raw materials in parts by weight: 4 parts of demulsifying component, 8 parts of auxiliary component, 50 parts of deionized water, 12 parts of ethylene glycol monobutyl ether and 20 parts of Ninol;
the high dehydration rate oil field demulsifier is prepared by the following steps:
firstly, preparing demulsifying components and auxiliary components;
and secondly, mixing the demulsifying component and the auxiliary component, adding deionized water, stirring and dissolving, then adding ethylene glycol monobutyl ether and Ninol, and stirring and mixing for 20min at the temperature of 25 +/-2 ℃ to obtain the high-dehydration-rate oil field demulsifier.
Wherein the demulsifying component is prepared by the following steps:
step S11, mixing sodium alginate and absolute ethyl alcohol, setting the temperature to be 30 +/-2 ℃ and the rotating speed to be 400r/min, stirring for 10min, adding a sodium periodate aqueous solution, keeping the temperature and the rotating speed unchanged, reacting for 6 +/-1 h in a dark place, after the reaction is finished, adding ethylene glycol, continuing stirring for 10 +/-2 min, then carrying out vacuum filtration, and washing the obtained filter cake for three times by using an ethanol aqueous solution with the volume fraction of 70% to obtain a solid a;
step S12, setting the temperature to be 50 +/-5 ℃ and the rotating speed to be 400r/min, mixing the solid a and deionized water, adding the mixture into dodecylamine, stirring and reacting for 12 +/-2 hours, setting the temperature to be 5 ℃ after the reaction is finished, keeping the rotating speed unchanged, adding sodium borohydride, continuing stirring and reacting for 12 +/-2 hours, mixing the obtained reaction liquid with three to five volumes of absolute ethyl alcohol, separating out a precipitate, carrying out vacuum filtration, and carrying out vacuum freeze drying on the obtained filter cake at-60 ℃ to obtain a solid b;
and step S13, adding the antibacterial agent and distilled water into a three-neck flask, mixing, setting the temperature to be 30 +/-2 ℃ and the rotating speed to be 500r/min, adding the solid b, stirring and reacting for 8 hours, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake with deionized water, and drying at 40 +/-2 ℃ to constant weight to obtain the demulsifying component.
Wherein, in the step S11, the sodium periodate aqueous solution is sodium periodate and deionized water according to the dosage ratio of 3 mol: 1L of sodium alginate, absolute ethyl alcohol, sodium periodate aqueous solution and glycol, wherein the dosage ratio of the sodium alginate to the absolute ethyl alcohol to the sodium periodate aqueous solution is 5 g: 60mL of: 50mL of: 5 mL; and in the step S12, adding the sodium borohydride in three times of equal amount, wherein the dosage ratio of the solid a, the deionized water, the dodecylamine and the sodium borohydride is 5 g: 120mL of: 5 g: 0.9 g; in step S13, the ratio of the antibacterial agent to the distilled water to the solid b is 60 mg: 10mL of: 3g of the total weight.
Wherein the antibacterial agent is prepared by the following steps:
step S21, adding 9-bromo-1-nonanol and triethylamine into a three-neck flask, adding dichloromethane, setting the temperature to be 5 ℃ and the rotation speed to be 300r/min, dropwise adding methacryloyl chloride while stirring, wherein the dropwise adding time is 2 hours, continuing to react for 24 hours at the temperature of 20 ℃ after the dropwise adding is finished, and performing rotary evaporation on the obtained reaction liquid on a rotary evaporator to remove dichloromethane after the reaction is finished to obtain an intermediate c;
and step S22, adding the intermediate c, triphenylphosphine, hydroquinone and acetonitrile into a three-neck flask, setting the temperature at 80 ℃ and the rotating speed at 500r/min, stirring for reaction for 72 hours, removing the acetonitrile from the obtained reaction liquid by using a rotary evaporator after the reaction is finished, and drying at 40 +/-2 ℃ to constant weight to obtain the antibacterial agent.
Wherein the dosage ratio of the 9-bromo-1-nonanol, the triethylamine, the dichloromethane and the methacryloyl chloride in the step S21 is 0.18 mol: 0.19 mol: 100mL of: 0.19 mol; in the step S22, the dosage ratio of the intermediate c, the triphenylphosphine, the hydroquinone and the acetonitrile is 2.5 g: 3.8 g: 0.4 g: 40 mL.
Wherein, the auxiliary components are prepared by the following steps:
step S31, adjusting the pH value of deionized water to 8 by using sodium hydroxide, setting the temperature to be 60 ℃ and the rotating speed to be 100r/min, adding hexadecyl trimethyl ammonium bromide, stirring for 30 +/-5 min, then dropwise adding tetraethoxysilane while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, continuing stirring for 24h, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake for three times by using deionized water and absolute ethyl alcohol in sequence, after the washing is finished, carrying out vacuum drying for 2h at the temperature of 80 +/-2 ℃, and then calcining for 6 +/-1 h at the temperature of 550 +/-10 ℃ to obtain a solid d;
step S32, mixing chitosan and acetic acid solution with the mass fraction of 1 +/-0.5%, setting the temperature to be 25 +/-2 ℃ and the rotating speed to be 300r/min, dropwise adding the sodium perfluorononanoate solution while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, and continuously stirring for 10 +/-2 min to obtain suspension;
step S33, mixing the solid d with absolute ethyl alcohol, carrying out ultrasonic treatment for 15 +/-5 min under the condition of 40kHz, adjusting the pH value to 5 by using glacial acetic acid, adding gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and stirring for 3h under the condition of 25 +/-2 ℃; and (3) after stirring, adding the suspension obtained in the step S32, keeping the temperature unchanged, continuously stirring for 24 +/-2 h, centrifuging at 7000r/min, washing the obtained lower-layer precipitate for three times by using absolute ethyl alcohol and deionized water, and after washing, drying in vacuum at-70 ℃ for 16h to obtain the auxiliary component.
Wherein the dosage ratio of the deionized water, the hexadecyl trimethyl ammonium bromide and the ethyl orthosilicate in the step S31 is 500 mL: 0.5 g: 3g, the concentration of the sodium perfluorononanate in the step S32 is 0.1mol/L, and the dosage ratio of the chitosan, the acetic acid solution with the mass fraction of 1 +/-0.5% and the sodium perfluorononanate solution is 50 mg: 25mL of: 5 mL; in the step S33, the dosage ratio of the solid d, the absolute ethyl alcohol and the gamma- (2,3 epoxypropoxy) propyl trimethoxy silane is 1 g: 100mL of: 0.2 g; the dosage ratio of the solid d to the suspension is 1 g: 10 mL.
Comparative example 1
The auxiliary components in example 1 were not added, and the rest of the raw materials and the preparation process remained unchanged.
Comparative example 2
The comparative example is an oil field demulsifier produced by a company in Beijing.
The demulsifiers of examples 1-3 and comparative examples 1-2 were subjected to a performance test;
preheating natural crude oil with free water removed at about 60 deg.C for 30min, pumping 200mL with injector, injecting into tissue mashing and homogenizing machine, adding 500mL distilled water preheated to about 60 deg.C into homogenizing machine for 5 times, and stirring at 5000r/min for 40min to obtain water-stirred oil; standing and aging for about 24 hours at room temperature for later use; respectively absorbing 100mL of stirring oil by using a syringe, adding the stirring oil into 100mL of stoppers with different numbers, placing the stoppers in a 55 ℃ glass thermostatic water bath for preheating for 3min, absorbing a demulsifier solution by using a transfer pipette, adding the demulsifier solution into the stoppers, rapidly and violently oscillating by hand, placing a water clamp on an oscillator, oscillating for 3min at the maximum oscillation speed, placing the water clamp back in the water bath, measuring the dehydration rate once per hour under the conditions that the addition amount is 50mg/L and the test temperature is 55 ℃, and observing the water color condition after two hours, wherein the dehydration rate is the average value of three parallel experiments.
The test results are shown in table 1 below:
TABLE 1
From the above table 1, it can be seen that the demulsifier prepared by the present invention has a better dehydration effect, wherein protonated amino groups in chitosan molecules react with sodium perfluorononanoate to fluorinate chitosan, the solid d is mesoporous silica nanoparticles with a large specific surface area and pore volume, the coupling agent gamma- (2,3 epoxypropoxy) propyl trimethoxysilane is used as a bridging agent to graft the treated chitosan onto the silica nanoparticles to obtain an auxiliary component, which further improves the affinity and hydrophilicity of the silica nanoparticles, so that the auxiliary component can more easily penetrate through an oil-water interfacial film to obtain a water phase, the density of the water phase is increased, which is beneficial to the occurrence of film drainage and phase separation processes, the auxiliary component cooperates with the demulsifying component to reduce the oil-water interfacial tension and the interfacial film strength, resulting in the interfacial film destruction, achieving the demulsification effect, improving the dehydration rate of crude oil, and simultaneously during the use process, the demulsifying component forms nano-scale particles with inward hydrophobic groups and outward hydrophilic groups, plays a role in flocculation and can adsorb heavy metal ions in water, so that the water color is clearer.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. The preparation method of the high-dehydration-rate oil field demulsifier is characterized by comprising the following raw materials in parts by weight: 2-4 parts of demulsifying component, 6-8 parts of auxiliary component, 40-50 parts of deionized water, 10-12 parts of ethylene glycol monobutyl ether and 10-20 parts of Ninol;
the high dehydration rate oil field demulsifier is prepared by the following steps:
firstly, preparing demulsifying components and auxiliary components;
secondly, mixing the demulsifying component and the auxiliary component, adding deionized water, stirring and dissolving, then adding ethylene glycol monobutyl ether and Ninol, and stirring and mixing for 10-20min at the temperature of 25 +/-2 ℃ to obtain the high-dehydration-rate oil field demulsifier;
the demulsifying component is prepared by the following steps:
step S11, mixing sodium alginate and absolute ethyl alcohol, setting the temperature to be 30 +/-2 ℃, stirring for 6-10min, adding a sodium periodate aqueous solution, keeping the temperature unchanged, reacting for 6 +/-1 h in a dark place, adding ethylene glycol after the reaction is finished, continuously stirring for 10 +/-2 min, then carrying out vacuum filtration, and washing the obtained filter cake for multiple times by using the ethanol aqueous solution to obtain a solid a;
step S12, setting the temperature to be 50 +/-5 ℃, mixing the solid a and deionized water, adding the mixture into dodecylamine, stirring for reaction for 12 +/-2 hours, setting the temperature to be 0-5 ℃ after the reaction is finished, adding sodium borohydride, continuing stirring for reaction for 12 +/-2 hours, mixing the obtained reaction liquid with three to five times of volume of absolute ethyl alcohol, separating out a precipitate, carrying out vacuum filtration, and carrying out vacuum freeze drying on the obtained filter cake to obtain a solid b;
step S13, mixing an antibacterial agent and distilled water, setting the temperature to be 30 +/-2 ℃, adding the solid b, stirring and reacting for 4-8 hours, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake with deionized water, and drying at 40 +/-2 ℃ to constant weight to obtain a demulsifying component;
the auxiliary components are prepared by the following steps:
step S31, adjusting the pH value of deionized water to 7-8 by using sodium hydroxide, setting the temperature to 50-60 ℃, adding hexadecyl trimethyl ammonium bromide, stirring for 30 +/-5 min, then dropwise adding tetraethoxysilane while stirring, keeping the temperature unchanged after dropwise adding, continuously stirring for 20-24h, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake by using deionized water and absolute ethyl alcohol in sequence, after the washing is finished, carrying out vacuum drying for 2h at the temperature of 80 +/-2 ℃, and then calcining for 6 +/-1 h at the temperature of 550 +/-10 ℃ to obtain a solid d;
step S32, mixing chitosan and acetic acid solution with the mass fraction of 1 +/-0.5%, setting the temperature to be 25 +/-2 ℃, dropwise adding the sodium perfluorononanoate solution while stirring, keeping the temperature unchanged after dropwise adding, and continuously stirring for 10 +/-2 min to obtain suspension;
step S33, mixing the solid d with absolute ethyl alcohol, carrying out ultrasonic treatment for 15 +/-5 min, adjusting the pH value to 3-5 with glacial acetic acid, adding gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and stirring for 3h at the temperature of 25 +/-2 ℃; adding the suspension obtained in the step S32 after stirring, keeping the temperature unchanged, continuously stirring for 24 +/-2 hours, then centrifuging, washing the obtained lower-layer precipitate with absolute ethyl alcohol and deionized water, and after washing, carrying out vacuum freeze drying to obtain auxiliary components;
the antibacterial agent is prepared by the following steps:
step S21, adding 9-bromo-1-nonanol and triethylamine into a three-neck flask, adding dichloromethane, setting the temperature to be 0-5 ℃, dropwise adding methacryloyl chloride while stirring, continuing to react for 24 +/-2 hours at the temperature of 20 +/-2 ℃ after dropwise adding, and evaporating the obtained reaction liquid to remove dichloromethane after the reaction is finished to obtain an intermediate c;
and step S22, adding the intermediate c, triphenylphosphine, hydroquinone and acetonitrile into a three-neck flask, setting the temperature to be 80 +/-2 ℃, stirring and reacting for 72 +/-2 hours, evaporating the obtained reaction liquid to remove the acetonitrile after the reaction is finished, and drying at 40 +/-2 ℃ to constant weight to obtain the antibacterial agent.
2. The method for preparing the oilfield demulsifier with high dehydration rate according to claim 1, wherein the demulsifying component is prepared by the following steps:
step S11, mixing sodium alginate and absolute ethyl alcohol, setting the temperature to be 30 +/-2 ℃ and the rotating speed to be 400r/min, stirring for 6-10min, adding a sodium periodate aqueous solution, keeping the temperature and the rotating speed unchanged, reacting for 6 +/-1 h in a dark place, after the reaction is finished, adding ethylene glycol, continuing stirring for 10 +/-2 min, then carrying out vacuum filtration, and washing the obtained filter cake for three times by using an ethanol aqueous solution with the volume fraction of 70% to obtain a solid a;
s12, setting the temperature to be 50 +/-5 ℃ and the rotating speed to be 400r/min, mixing the solid a and deionized water, adding the mixture into dodecylamine, stirring and reacting for 12 +/-2 hours, setting the temperature to be 0-5 ℃ after the reaction is finished, keeping the rotating speed unchanged, adding sodium borohydride, continuing stirring and reacting for 12 +/-2 hours, mixing the obtained reaction liquid with four times of volume of absolute ethyl alcohol, separating out a precipitate, carrying out vacuum filtration, and carrying out vacuum freeze drying on the obtained filter cake at-60 ℃ to obtain a solid b;
and step S13, adding the antibacterial agent and distilled water into a three-neck flask, mixing, setting the temperature to be 30 +/-2 ℃ and the rotating speed to be 500r/min, adding the solid b, stirring and reacting for 4-8h, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake with deionized water, and drying at 40 +/-2 ℃ to constant weight to obtain the demulsifying component.
3. The method for preparing the high dehydration rate oilfield demulsifier according to claim 1 or 2, wherein the aqueous solution of sodium periodate in step S11 is prepared from sodium periodate and deionized water according to a dosage ratio of 3 mol: 1L of sodium alginate, absolute ethyl alcohol, sodium periodate aqueous solution and glycol, wherein the dosage ratio of the sodium alginate to the absolute ethyl alcohol to the sodium periodate aqueous solution is 5 g: (50-60 mL): 50mL of: 5 mL; and in the step S12, adding the sodium borohydride in three times of equal amount, wherein the dosage ratio of the solid a, the deionized water, the dodecylamine and the sodium borohydride is 5 g: 120mL of: (4.6-5 g): (0.8-0.9 g); in step S13, the dosage ratio of the antibacterial agent to the distilled water to the solid b is (50-60 mg): 10mL of: (1-3 g).
4. The preparation method of the high dehydration rate oilfield demulsifier according to claim 1 or 2, wherein the antibacterial agent is prepared by the following steps:
step S21, adding 9-bromo-1-nonanol and triethylamine into a three-neck flask, adding dichloromethane, setting the temperature to be 0-5 ℃ and the rotating speed to be 300r/min, dropwise adding methacryloyl chloride while stirring, wherein the dropwise adding time is 2h, continuing to react for 24h at the temperature of 20 ℃ after dropwise adding, and after the reaction is finished, rotationally evaporating the obtained reaction liquid on a rotary evaporator to remove dichloromethane to obtain an intermediate c;
and step S22, adding the intermediate c, triphenylphosphine, hydroquinone and acetonitrile into a three-neck flask, setting the temperature at 80 ℃ and the rotating speed at 500r/min, stirring for reaction for 72 hours, removing the acetonitrile from the obtained reaction liquid by using a rotary evaporator after the reaction is finished, and drying at 40 +/-2 ℃ to constant weight to obtain the antibacterial agent.
5. The method for preparing the oilfield demulsifier with high dehydration rate according to claim 4, wherein the amount ratio of the 9-bromo-1-nonanol, the triethylamine, the dichloromethane and the methacryloyl chloride in step S21 is 0.18 mol: (0.18-0.19 mol): 100mL of: 0.19 mol; in the step S22, the dosage ratio of the intermediate c, the triphenylphosphine, the hydroquinone and the acetonitrile is 2.5 g: 3.8 g: (0.3-0.4 g): 40 mL.
6. The preparation method of the high dehydration rate oilfield demulsifier according to claim 1, wherein the auxiliary component is prepared by the following steps:
step S31, adjusting the pH value of deionized water to 7-8 by using sodium hydroxide, setting the temperature to 50-60 ℃ and the rotating speed to 100r/min, adding hexadecyl trimethyl ammonium bromide, stirring for 30 +/-5 min, then dropwise adding tetraethoxysilane while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, continuing stirring for 20-24h, after the reaction is finished, carrying out vacuum filtration, washing the obtained filter cake for three times by using deionized water and absolute ethyl alcohol in sequence, after the washing is finished, carrying out vacuum drying at 80 +/-2 ℃ for 2h, and then calcining at 550 +/-10 ℃ for 6 +/-1 h to obtain a solid d;
step S32, mixing chitosan and acetic acid solution with the mass fraction of 1 +/-0.5%, setting the temperature to be 25 +/-2 ℃ and the rotating speed to be 300r/min, dropwise adding the sodium perfluorononanoate solution while stirring, keeping the temperature and the rotating speed unchanged after dropwise adding, and continuously stirring for 10 +/-2 min to obtain suspension;
step S33, mixing the solid d with absolute ethyl alcohol, carrying out ultrasonic treatment for 15 +/-5 min under the condition of 40kHz, adjusting the pH value to 3-5 by using glacial acetic acid, adding gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and stirring for 3h at the temperature of 25 +/-2 ℃; and (3) after stirring, adding the suspension obtained in the step S32, keeping the temperature unchanged, continuously stirring for 24 +/-2 h, centrifuging at 7000r/min, washing the obtained lower-layer precipitate for three times by using absolute ethyl alcohol and deionized water, and after washing, drying in vacuum at-70 ℃ for 16h to obtain the auxiliary component.
7. The preparation method of the high dehydration rate oilfield demulsifier according to claim 1 or 6, wherein the amount ratio of the deionized water to the cetyltrimethylammonium bromide to the ethyl orthosilicate in step S31 is 500 mL: 0.5 g: 3g, the concentration of the sodium perfluorononanate in the step S32 is 0.1mol/L, and the dosage ratio of the chitosan, the acetic acid solution with the mass fraction of 1 +/-0.5% and the sodium perfluorononanate solution is 50 mg: 25mL of: 5 mL; in the step S33, the dosage ratio of the solid d, the absolute ethyl alcohol and the gamma- (2,3 epoxypropoxy) propyl trimethoxy silane is 1 g: 100mL of: 0.2 g; the dosage ratio of the solid d to the suspension is 1 g: (6-10 mL).
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