CN115368934A - Composite demulsifier and preparation process thereof - Google Patents
Composite demulsifier and preparation process thereof Download PDFInfo
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- CN115368934A CN115368934A CN202210783187.1A CN202210783187A CN115368934A CN 115368934 A CN115368934 A CN 115368934A CN 202210783187 A CN202210783187 A CN 202210783187A CN 115368934 A CN115368934 A CN 115368934A
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- demulsifier
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- C—CHEMISTRY; METALLURGY
- 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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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention provides a composite demulsifier and a preparation process thereof, wherein the composite demulsifier comprises the following raw materials in parts by weight: 3-5 parts of cationic demulsifier, 0.5-1 part of ethylene glycol phenyl ether, 0.1-0.5 part of eutectic solvent and 0.5-1 part of diethylene glycol monobutyl ether; the eutectic solvent is a mixture of choline chloride and glycol or urea, reduces the strength of an interfacial film, and is low-toxicity or non-toxic chemicals which are green.
Description
Technical Field
The invention relates to the technical field of crude oil exploitation, in particular to a composite demulsifier and a preparation process thereof.
Background
At present, crude oil exploitation in China gradually enters a middle and later stage, the content of asphaltene and colloid in the crude oil is increased, so that a crude oil emulsion becomes more stable, and in addition, the continuous development and application of an oil exploitation technology are added, a large amount of surfactant is added, so that the composition of the crude oil becomes extremely complex, the water content and the salt content of the crude oil extracted from an oil field are increased year by year, and therefore, the tasks of crude oil dehydration and desalination are increased for the oil field and a refinery. The crude oil contains the impurities, which can increase the load of a pump and a pipeline and cause the corrosion and the agglomeration of metal surfaces; the discharged water also contains oil, which causes environmental pollution and crude oil waste. From the environmental protection perspective and the economic perspective, the crude oil needs to be demulsified and dehydrated and sewage deoiled. The crude oil demulsification method comprises a sedimentation method, a heating method, electric dehydration, a chemical method and the like, wherein the chemical demulsification method is the most widely used demulsification method for oil fields, and the purpose of demulsification is achieved by changing the interfacial property of an emulsion system from more stable to unstable through adding a demulsifier.
The chemical agent capable of demulsifying and dewatering emulsified crude oil is called crude oil demulsifier. The properties of the demulsifier are mainly reflected in four aspects: the diffusion and adsorption properties of the agent, the wetting and film-forming properties of the agent, the flocculation and coalescence properties of the agent, and the wettability of the solid. The conventional polyether demulsifier can meet the demulsification requirement of the water-in-oil type emulsion in the produced liquid, and the cationic reverse demulsifier can better break the oil-in-water type emulsion, so that the conventional demulsifier is used under the specific process condition aiming at specific crude oil, has no broad spectrum, and has poor adaptability and demulsification comprehensive effect.
Disclosure of Invention
In order to solve the problems, the invention provides a composite demulsifier and a preparation process thereof.
The invention aims to provide a composite demulsifier, which comprises the following raw materials in parts by weight: 3-5 parts of cation demulsifier, 0.5-1 part of ethylene glycol phenyl ether, 0.1-0.5 part of eutectic solvent and 0.5-1 part of diethylene glycol monobutyl ether.
In a preferred embodiment, the cationic demulsifier is a cetyl quaternary amine salt.
In a preferred embodiment, the eutectic solvent is a mixture of choline chloride and ethylene glycol or urea, wherein the molar ratio of choline chloride to ethylene glycol or urea is 1:1-1:5.
The second purpose of the invention is to provide a preparation process of a composite demulsifier, which comprises the following steps:
(1) Uniformly mixing a cationic demulsifier and ethylene glycol phenyl ether according to a mass ratio to obtain a first mixed solution;
(2) Dissolving the eutectic solvent in a diethylene glycol monobutyl ether solution, and uniformly mixing to obtain a second mixed solution;
(3) And (3) adding the second mixed solution prepared in the step (2) into the first mixed solution prepared in the step (1), and uniformly stirring to prepare the composite demulsifier.
In a preferred embodiment, the preparation method of the eutectic solvent comprises the steps of adding choline chloride and ethylene glycol or urea into a three-neck flask according to a proportion, stirring and heating to 60-80 ℃, stirring for 30-120 minutes, and cooling to obtain the uniform eutectic solvent.
In a preferred embodiment, the mixing temperature of step (1) is 70-75 ℃ and the mixing time is 40-45min; the mixing temperature of the step (2) is 50-55 ℃, and the mixing time is 30-35min; the mixing temperature of the step (3) is 40-45 ℃, and the mixing time is 25-30min.
Compared with the prior art, the invention has the following beneficial effects:
(1) The eutectic solvent is a mixture of choline chloride and glycol or urea, reduces the strength of an interfacial film, and is low-toxicity or non-toxic chemicals which meet the requirement of green chemistry;
(2) The ethylene glycol phenyl ether is colorless transparent liquid with low volatility and high boiling point, and can be mixed with a plurality of organic solvents, has strong permeability, can be mixed with alcohol and ether, is commonly called as universal solvent, can completely dissolve other demulsifier components to form a unified fluid, and is convenient to use.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms also include the plural forms unless the context clearly dictates otherwise, and further, it is understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, devices, components, and/or combinations thereof.
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. 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.
Example 1
The composite demulsifier described in this embodiment 1 comprises the following raw materials in parts by weight: 4 parts of cation demulsifier, 0.7 part of ethylene glycol phenyl ether, 0.3 part of eutectic solvent and 0.5 part of diethylene glycol monobutyl ether. The preparation method of the eutectic solvent comprises the steps of adding choline chloride and urea into a three-neck flask according to a certain proportion, stirring and heating to 70 ℃, stirring for 60 minutes, and cooling to obtain the uniform eutectic solvent. The preparation process of the composite demulsifier comprises the following steps: (1) Uniformly mixing a cationic demulsifier and ethylene glycol phenyl ether according to a mass ratio to obtain a first mixed solution; (2) Dissolving the eutectic solvent in the diethylene glycol monobutyl ether solution, and uniformly mixing to obtain a second mixed solution; (3) And (3) adding the second mixed solution prepared in the step (2) into the first mixed solution prepared in the step (1), and uniformly stirring to prepare the composite demulsifier.
Wherein the mixing temperature in the step (1) is 70 ℃, and the mixing time is 45min; the mixing temperature of the step (2) is 55 ℃, and the mixing time is 35min; the mixing temperature in the step (3) is 45 ℃ and the mixing time is 30min.
Example 2
The composite demulsifier described in this embodiment 2 comprises the following raw materials in parts by weight: 4 parts of cation demulsifier, 0.5 part of ethylene glycol phenyl ether, 0.1 part of eutectic solvent and 0.5 part of diethylene glycol monobutyl ether. The preparation method comprises the steps of adding choline chloride and glycol or urea into a three-neck flask according to a proportion, stirring and heating to 60 ℃, stirring for 120 minutes, and then cooling to obtain the uniform eutectic solvent. The preparation process of the composite demulsifier comprises the following steps: (1) Uniformly mixing a cationic demulsifier and ethylene glycol phenyl ether according to a mass ratio to obtain a first mixed solution; (2) Dissolving the eutectic solvent in a diethylene glycol monobutyl ether solution, and uniformly mixing to obtain a second mixed solution; (3) And (3) adding the second mixed solution prepared in the step (2) into the first mixed solution prepared in the step (1), and uniformly stirring to prepare the composite demulsifier.
Wherein the mixing temperature in the step (1) is 75 ℃, and the mixing time is 45min; the mixing temperature of the step (2) is 55 ℃, and the mixing time is 35min; the mixing temperature in the step (3) is 45 ℃ and the mixing time is 30min.
Example 3
The composite demulsifier described in this embodiment 3 comprises the following raw materials in parts by weight: 3 parts of cation demulsifier, 0.5 part of ethylene glycol phenyl ether, 0.1 part of eutectic solvent and 0.5 part of diethylene glycol monobutyl ether. The preparation method comprises the steps of adding choline chloride and glycol or urea into a three-neck flask according to a ratio, stirring and heating to 60 ℃, stirring for 30 minutes, and cooling to obtain the uniform eutectic solvent. The preparation process of the composite demulsifier comprises the following steps: (1) Uniformly mixing a cationic demulsifier and ethylene glycol phenyl ether according to a mass ratio to obtain a first mixed solution; (2) Dissolving the eutectic solvent in a diethylene glycol monobutyl ether solution, and uniformly mixing to obtain a second mixed solution; (3) And (3) adding the second mixed solution prepared in the step (2) into the first mixed solution prepared in the step (1), and uniformly stirring to prepare the composite demulsifier.
Wherein the mixing temperature in the step (1) is 70 ℃, and the mixing time is 40min; the mixing temperature in the step (2) is 50 ℃, and the mixing time is 30min; the mixing temperature in the step (3) is 40 ℃, and the mixing time is 25min.
Comparative example 1
The preparation process and the raw material composition of the composite demulsifier in the comparative example 1 are the same as those in the example 1, and the only difference is that the raw material in the comparative example 1 is different in the eutectic solvent, and the eutectic solvent is replaced by ethylene glycol.
TABLE 1 demulsifier application Performance test results
Remarking:
1. the method for measuring the dehydration rate comprises the following steps:
(1) Before the crude oil emulsion is used, the volume water content of the crude oil emulsion is firstly tested; (2) Pouring the prepared crude oil emulsion into a measuring cylinder with a plug to reach the scale of 80 ml; (3) Placing the crude oil emulsion into a constant-temperature water bath which is lower than the preset dehydration temperature by 5 ℃, wherein the liquid level of the water bath is higher than that of the crude oil emulsion in a stopple graduated cylinder, heating the constant-temperature water bath to be consistent with the actual operation temperature of a station, and keeping the constant temperature for 0.5 hour; (4) Adding 100mg/L of crude oil demulsifier solution prepared into the measuring cylinder with the plug by using a pipette; (5) Turning the bottle cap, reversing the measuring cylinder with the plug for 5 times, slowly loosening the bottle cap, deflating, screwing the bottle cap again, oscillating manually for 100 +/-10 times in a vertical vibration mode, wherein the amplitude is larger than 10 cm, loosening the bottle cap after fully and uniformly mixing, and placing the measuring cylinder with the plug in a constant-temperature water bath again for standing and settling; (6) record the amount of water phase removed in 30min.
2. Calculation of crude oil dehydration rate for 30 minutes: s = V/(V0 × WV) × 100%; in the formula: s-dehydration rate of crude oil demulsifier,%; v, water yield of the crude oil emulsion after 30min sedimentation, mL; v0-volume of crude oil emulsion, mL; WV is the volume water content of the crude oil emulsion.
3. Water phase cleanliness: and (3) when the mixture is settled for 30min, observing the color of the removed water phase, and judging the cleanliness of the water phase according to the following grades: level 1: the water is clear after being removed and is transparent or milky white; and 2, stage: the dehydrated water is relatively clear and is light yellow; and 3, level: the dehydrated water is turbid, yellow and brown; 4, level: turbid after dehydration, dark brown or black.
4. And (3) measuring the water content of the upper oil phase: and after 24h, a liquid extractor is used for inserting the middle position of the upper oil phase of the measuring cylinder with the plug after the dehydration rate measurement is finished, the middle position is fixed, an aurilave is inserted into a silica gel tube, about 10mL of crude oil is slightly sucked, and the fluctuation of an oil-water interface cannot be caused. Slowly moving the liquid taking device out of the measuring cylinder with the plug, firstly adding petroleum ether into the centrifugal tube to 50% of scales, then putting crude oil into the centrifugal tube to 100% of scales, shaking up and down, uniformly mixing, putting into a centrifugal machine, reading the scale value of outlet water in the centrifugal tube when the rotating speed of the centrifugal machine is 2000r/min and the centrifugal time is 10min, and measuring the water content of the crude oil according to GB/T8929.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (6)
1. The composite demulsifier is characterized by comprising the following raw materials in parts by weight: 3-5 parts of cation demulsifier, 0.5-1 part of ethylene glycol phenyl ether, 0.1-0.5 part of eutectic solvent and 0.5-1 part of diethylene glycol monobutyl ether.
2. The composite demulsifier of claim 1, wherein the cationic demulsifier is a hexadecyl quaternary ammonium salt.
3. The composite demulsifier of claim 1, wherein the eutectic solvent is a mixture of choline chloride and ethylene glycol or urea, wherein the molar ratio of choline chloride to ethylene glycol or urea is 1:1-1:5.
4. A preparation process of a composite demulsifier is characterized by comprising the following steps: the method comprises the following steps:
uniformly mixing a cationic demulsifier and ethylene glycol phenyl ether according to a mass ratio to obtain a first mixed solution;
dissolving the eutectic solvent in a diethylene glycol monobutyl ether solution, and uniformly mixing to obtain a second mixed solution;
(3) And (3) adding the second mixed solution prepared in the step (2) into the first mixed solution prepared in the step (1), and uniformly stirring to prepare the composite demulsifier.
5. The preparation process of the composite demulsifier according to claim 4, wherein the preparation method of the eutectic solvent comprises the steps of adding choline chloride and ethylene glycol or urea into a three-neck flask according to a proportion, stirring and heating to 60-80 ℃, stirring for 30-120 minutes, and cooling to obtain the uniform eutectic solvent.
6. The preparation process of the composite demulsifier according to claim 4, wherein the mixing temperature in step (1) is 70-75 ℃ and the mixing time is 40-45min; the mixing temperature of the step (2) is 50-55 ℃, and the mixing time is 30-35min; the mixing temperature of the step (3) is 40-45 ℃, and the mixing time is 25-30min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210783187.1A CN115368934A (en) | 2022-07-05 | 2022-07-05 | Composite demulsifier and preparation process thereof |
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| CN202210783187.1A CN115368934A (en) | 2022-07-05 | 2022-07-05 | Composite demulsifier and preparation process thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115772400A (en) * | 2022-12-01 | 2023-03-10 | 克拉玛依中科恒信科技有限责任公司 | Composite demulsifier for acidizing and fracturing and preparation method thereof |
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| CN1876217A (en) * | 2005-06-06 | 2006-12-13 | 中国科学院化学研究所 | Chemical demulsifier |
| CN112048337A (en) * | 2020-09-01 | 2020-12-08 | 宁波锋成先进能源材料研究院有限公司 | Low-temperature demulsifier and preparation method thereof |
| CN112427047A (en) * | 2019-08-10 | 2021-03-02 | 石家庄搏澳增塑材料科技有限公司 | Method for large-scale preparation of urea-choline chloride green catalyst and solvent |
| CN112877112A (en) * | 2021-01-15 | 2021-06-01 | 宋子云 | Efficient lubricating oil demulsifier and production method thereof |
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2022
- 2022-07-05 CN CN202210783187.1A patent/CN115368934A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1876217A (en) * | 2005-06-06 | 2006-12-13 | 中国科学院化学研究所 | Chemical demulsifier |
| CN112427047A (en) * | 2019-08-10 | 2021-03-02 | 石家庄搏澳增塑材料科技有限公司 | Method for large-scale preparation of urea-choline chloride green catalyst and solvent |
| CN112048337A (en) * | 2020-09-01 | 2020-12-08 | 宁波锋成先进能源材料研究院有限公司 | Low-temperature demulsifier and preparation method thereof |
| CN112877112A (en) * | 2021-01-15 | 2021-06-01 | 宋子云 | Efficient lubricating oil demulsifier and production method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115772400A (en) * | 2022-12-01 | 2023-03-10 | 克拉玛依中科恒信科技有限责任公司 | Composite demulsifier for acidizing and fracturing and preparation method thereof |
| CN115772400B (en) * | 2022-12-01 | 2023-06-23 | 克拉玛依中科恒信科技有限责任公司 | Composite demulsifier for acidizing and fracturing and preparation method thereof |
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