CN115449394A - Demulsifier and preparation method thereof - Google Patents
Demulsifier and preparation method thereof Download PDFInfo
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- CN115449394A CN115449394A CN202110644549.4A CN202110644549A CN115449394A CN 115449394 A CN115449394 A CN 115449394A CN 202110644549 A CN202110644549 A CN 202110644549A CN 115449394 A CN115449394 A CN 115449394A
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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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- Oil, Petroleum & Natural Gas (AREA)
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- General Chemical & Material Sciences (AREA)
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention provides a demulsifier and a preparation method thereof. The demulsifier comprises: the first component is selected from one or a combination of a plurality of polyethylene polyamine polyoxypropylene polyoxyethylene ether and polyethylene polyamine polyoxypropylene polyoxyethylene ether; a second component selected from one or more of polyoxyethylene polyoxypropylene allyl glycol monoether and polyoxyethylene polyoxypropylene stearyl ether; a dissolution promoter; and a solvent. By applying the technical scheme of the invention, the technical effects of reducing the dosage of the demulsifier, reducing the oil content in the treated water phase, ensuring good water phase cleanliness and clear water-oil interface at the first stage with low water phase turbidity can be realized.
Description
Technical Field
The invention relates to the field of chemical production, in particular to a demulsifier and a preparation method thereof.
Background
In the petroleum cracking process, the ethylene pyrolysis gas is rich in unsaturated olefins of C5 to C9, so that water is required to be rapidly cooled. The cooling is aimed at preventing the polymerization of unsaturated olefin at high temp. and washing and desalting cracked oil. After the pyrolysis oil is cooled to below 100 ℃, the mixture is usually treated to allow for rapid and efficient separation of the organic phase from the aqueous phase in the mixture. The effective method at present is to add a demulsifier into the mixture, thereby eliminating emulsification to form an emulsification interface with certain strength and achieving the purpose of separating oil phase from water phase.
The demulsifier is a surfactant capable of breaking emulsion, and can break the structure of emulsified liquid so as to achieve the purpose of separating water phase from oil phase in the emulsion. The main components of the demulsifiers are generally composed of lipophilic groups, which are hydrocarbon groups, in particular long-chain hydrocarbon groups, and hydrophilic groups, which are composed of hydrophilic groups of ionic or nonionic type. According to the use condition of the current demulsifier, the demulsifier can be divided into a water-soluble demulsifier and an oil-soluble demulsifier. According to the classification method of the surfactant, the surfactant can be classified into: cationic, anionic, nonionic, zwitterionic demulsifiers. The anionic demulsifier comprises carboxylates, sulfonates, polyoxyethylene fatty sulfate and the like, and has the defects of large dosage, poor effect, easy effect reduction caused by electrolyte influence and the like; the cation type demulsifier mainly contains quaternary ammonium salt, has super strong reverse demulsification capability, has obvious separation effect on demulsification of thin oil, but has poor water purification capability; the non-ionic polyether mainly comprises block polyether taking amines, alcohols and phenolic resins as initiators, and is a polyether organic matter with relatively high molecular mass.
At present, the demulsifier of the cracked oil washing water of the domestic ethylene production device mainly adopts a cation or modified single demulsifier or an oil-soluble demulsifier, and has the defects of long demulsification time, large medicament dosage, low water phase clarity, residual impurities in an oil phase and the like. The prior art discloses an ethylene cracking gas quenching water demulsifier composition, which comprises a main body formed by saturated fatty acid and alkylamine and a solvent formed by kerosene or extraction oil and the like. The demulsifier has the defects of large using amount, high oil content of a treated water phase, poor clarity and residual organic phase in a solvent in the using process.
Disclosure of Invention
The invention mainly aims to provide a demulsifier, which solves the problems that the demulsifier in the prior art has large using amount in the using process, the processed water phase has high oil content, poor clarity and residual organic phase in a solvent.
In order to achieve the above object, according to one aspect of the present invention, there is provided a demulsifier comprising: the first component is selected from one or a combination of a plurality of polyethylene polyamine polyoxypropylene polyoxyethylene ether and polyethylene polyamine polyoxypropylene polyoxyethylene ether; a second component selected from one or more of polyoxyethylene polyoxypropylene glycol monoether and polyoxyethylene polyoxypropylene stearyl ether; a dissolution promoter; and a solvent.
Further, in the above demulsifier, the weight part of the first component is 25 to 30 parts by weight based on 100 parts by weight of the demulsifier; the weight part of the second component is 10 to 15 weight parts; 5 to 10 parts by weight of a dissolution promoter; and the weight part of the solvent is 45 to 60 parts by weight.
Further, in the above demulsifier, the dissolution promoter is an alcohol or an alcohol ether.
Further, in the demulsifier, the dissolution promoter is one or any combination of methanol, ethanol, isopropanol, n-butanol, cyclohexanol, benzyl alcohol, terpineol, propylene glycol, glycerol, ethylene glycol, pentanol, hexanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, propylene glycol monoethyl ether, and propylene glycol monobutyl ether.
Further, in the above demulsifier, the solvent is water.
According to another aspect of the invention, a preparation method of the demulsifier is provided, which comprises the following steps: s1, mixing a first component, a second component and a solvent to obtain a mixture; and S2, mixing the mixture with a dissolution promoter to obtain the demulsifier.
Further, in the above method, in step S1, mixing is performed under stirring.
Further, in the above method, in step S2, a dissolution promoter is added to the mixture at a temperature ranging from 45 ℃ to 55 ℃.
Further, in the above method, in step S2, after the dissolution promoter is added to the mixture, the mixture is left to stand for 60 to 80 minutes.
By applying the technical scheme of the invention, the technical effects of reducing the using amount of the demulsifier, reducing the oil content in the treated water phase, having good water phase cleanliness and a clear water-oil interface at the first level with low water phase turbidity can be realized.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As can be understood from the background art, the demulsifier in the prior art has the defects of large using amount, high oil content of treated water phase, poor clarity and residual organic phase of solvent in the using process. In view of the above-described technical problems, in an exemplary embodiment of the present application, there is provided a demulsifier, comprising: the first component is selected from one or a combination of a plurality of polyethylene polyamine polyoxypropylene polyoxyethylene ether and polyethylene polyamine polyoxypropylene polyoxyethylene ether; a second component selected from one or more of polyoxyethylene polyoxypropylene allyl glycol monoether and polyoxyethylene polyoxypropylene stearyl ether; a dissolution promoter; and a solvent.
Unlike the demulsifiers in the prior art, the demulsifier of the present application comprises at the same time a first component selected from one or more combinations of polyethylene polyamine polyoxypropylene polyoxyethylene ether and polyethylene polyamine polyoxypropylene polyoxyethylene ether; a second component selected from the group consisting of one or more of polyoxyethylene polyoxypropylene glycol monoethers and polyoxyethylene polyoxypropylene stearyl ether. The first component of the present application is a polyethylene polyamine polyoxypropylene polyoxyethylene ether or a polyethylene polyamine polyoxypropylene polyoxyethylene ether. In some embodiments, the first component of the present application is effective in demulsifying water-oil emulsions having relatively high water contents. Wherein the higher water content is greater than 20% water content, preferably about 30%, more preferably greater than 40%. And due to the presence of the first component, the demulsifier of the present application can be demulsified at a relatively low temperature, for example, at a temperature of less than 75 ℃, preferably less than 65 ℃, and even more preferably at a temperature of 55 ℃, and has a high low-temperature dehydration rate. The first component of the present application has the structural characteristics of polyethylenepolyamine (or polyethylenepolyamine), and thus it contains more branched chains, and thus has the characteristics of high hydrophilicity, and thus has high solubility, good diffusivity, and diffusion rate. After the demulsifier of the present application comprising the first component is added to the emulsion, the multi-branched chains allow the first component to better wet and penetrate to the interfacial film between the water phase and the oil phase, thereby occupying more surface area. Good demulsification effect can be realized under the condition of only using a small amount of the demulsifier.
The second component of the present application is a polyoxyethylene polyoxypropylene glycol monoether or polyoxyethylene polyoxypropylene stearyl ether. In some embodiments, the second component of the present application comprises polyoxyethylene polyoxypropylene stearyl ether, the lipophilic part (hydrophobic part) of which consists of octadecyl groups, the hydrophilicity of which is a result of hydrogen bonding through hydroxyl groups, ether groups in the chain segment, to hydrogen atoms in water, thus achieving hydrophilicity. In addition, the second component also has the effects of strong flocculation capacity on particles in the emulsion, reduction of the water interface of emulsion oil, and strong water purification and desalination.
Under the condition of simultaneously containing a first component and a second component, the two compounds in the demulsifier can be crosslinked and compounded and have a mutual synergistic effect, so that excellent hydrophilicity and lipophilicity can be simultaneously shown, the interfacial tension of an oil-in-water (O/W) or water-in-oil (W/O) emulsion is effectively improved, and the demulsifier has good adaptability to emulsions with complex water quality, such as high oil-water emulsification degree, high suspension with small particle size, high polymer content and the like. In addition, the demulsifier of the application also shows excellent demulsification effect at high water content and lower temperature.
According to some embodiments of the present application, the solvent used in the present application is water. In the case of using water as a solvent, the first component and the second component of the present application are more easily uniformly mixed and uniformly interpenetrated in an aqueous medium. In addition, under the condition of using the demulsifier of the application, because the emulsion contains aqueous phase, the demulsifier using water as a medium can be mixed with the emulsion more quickly, thereby quickly realizing the demulsification effect.
In summary, the demulsifier of the present application, which comprises a first component selected from one or a combination of polyethylene polyamine polyoxypropylene polyoxyethylene ether or polyethylene polyamine polyoxypropylene polyoxyethylene ether, a second component selected from one or a combination of polyoxyethylene polyoxypropylene glycol monoether or polyoxyethylene polyoxypropylene stearyl ether, a dissolution promoter, and a solvent, can achieve the technical effects of reduced dosage, low oil content in the treated aqueous phase, good aqueous phase cleanliness, and clear aqueous-oil interface at the first stage.
According to some embodiments of the present application, the weight part of the first component is 25 to 30 weight parts based on 100 weight parts of the demulsifier; the weight part of the second component is 10 to 15 weight parts; 5 to 10 parts by weight of a dissolution promoter; and the weight part of the solvent is 45 to 60 weight parts. In the water-up range, the demulsifiers of the present application can better balance hydrophilicity and lipophilicity, thereby effectively improving the interfacial tension of oil-in-water (O/W) or water-in-oil (W/O) emulsions. In a preferred embodiment, the first component amount is 26 to 29 parts by weight, more preferably 27 to 28 parts by weight. In another preferred embodiment, the amount of the second component is 11 to 14 parts by weight, more preferably 12 to 13 parts by weight.
According to some embodiments of the present application, the dissolution promoter in the demulsifier of the present application is an alcohol or an alcohol ether. The dissolution promoter of the present application serves to better dissolve the first and second components in the solvent, thereby making the demulsifier formed a homogeneous material. Due to the addition of the dissolution promoter, the situation that the demulsification effect is reduced due to the fact that the first component and the second component are not uniform in the application process can be avoided.
According to some embodiments of the present application, the dissolution accelerating agent of the present application is selected from one or any combination of methanol, ethanol, isopropanol, n-butanol, cyclohexanol, benzyl alcohol, terpineol, propylene glycol, glycerol, ethylene glycol, pentanol, hexanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monobutyl ether. In the case of using the above-mentioned dissolution promoter, the first component and the second component of the present application can be effectively dissolved in the solvent, thereby forming the demulsifier of uniform composition. The above examples of the dissolution accelerating agent are merely illustrative, and any substance capable of achieving the technical effects of the present invention may be used.
In another exemplary embodiment of the present application, there is provided a method for preparing a demulsifier, comprising the steps of: s1, mixing a first component, a second component and a solvent to obtain a mixture; and S2, mixing the mixture with a dissolution promoter to obtain the demulsifier. In the method, the first component and the second component are dissolved in the solvent, and then the dissolution accelerating agent is added, so that the first component and the second component can be better dissolved, and a uniform demulsifier is formed. In addition, in the case of using the first component and the second compound described above, the demulsifier prepared by the method of the application can achieve the technical effects of reduced dosage, low oil content in the water phase after treatment, good water phase cleanliness, low water phase turbidity and clear water-oil interface.
In a further embodiment, in step S1, the mixing is performed under stirring. In some embodiments, the first component, the second component, and the solvent are added simultaneously with stirring, such that the first component and the second component are rapidly dispersed in the solvent under the action of shear forces, thereby forming a mixture in the form of a solution or suspension. In other embodiments, the solvent and first component are added with stirring, and the second component is added after the first component is completely dispersed in the solvent. In still other embodiments, the solvent and the second component are added with stirring, and the first component is added after the second component is completely dispersed in the solvent.
In a further embodiment, in step S2, a dissolution promoter is added to the mixture at a temperature in the range of 45 ℃ to 55 ℃. In some embodiments, the dissolution promoter more readily dissolves the first component and the second component in the solvent at a temperature in the range of 45 ℃ to 55 ℃. In a preferred embodiment, the dissolution promoter is added to the mixture at a temperature in the range of 47 ℃ to 50 ℃.
In a further embodiment, in step S2, after adding the dissolution promoter to the mixture, it is left standing for 60 to 80 minutes at a temperature in the range of 45 to 55 ℃. In some embodiments, after the dissolution promoter is added to the mixture, the demulsifier is typically allowed to stand for 60 to 80 minutes, preferably 70 to 80 minutes, in order to ensure good dissolution of the compound and the second component in the solvent. After the demulsifier is allowed to stand at a temperature ranging from 45 ℃ to 55 ℃, the first component and the second component are sufficiently dissolved in the solvent and form a homogeneous phase.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Both the polyethylenepolyamine polyoxypropylene polyoxyethylene ether and the polyethylenepolyamine polyoxypropylene polyoxyethylene ether used in the following examples are commercially available from Dow chemical; polyoxyethylene polyoxypropylene propylene glycol monoether is commercially available from Haian petrochemical plant of Jiangsu province under the trade name PPE; and polyoxyethylene polyoxypropylene stearyl ether is commercially available from Daqing Rede chemical Co., ltd under the trade name YL-06.
Preparation of demulsifiers of examples 1 to 12
The first component, the second component and the solvent of the present application are first added simultaneously to a stirred vessel. The first component, the second component, and the solvent are mixed with stirring to form a mixture. The stirred vessel was then warmed to 50 ℃ and the dissolution promoter was added to the mixture. Stirring is continued to completely dissolve the first component and the second component in the solvent. Stopping stirring, keeping the mixture for 60-80 minutes under the condition of standing, and cooling the mixture to room temperature, thereby obtaining the demulsifier of the example 1-the example 12. The specific types and amounts of the first component, the second component, the dissolution promoter, and the solvent are given in table 1 below.
Table 1: demulsifier proportion and components
The parts by weight in the table above are all based on 100 parts by weight of the demulsifier.
Example 13 to example 34 demulsifier Performance assays
The demulsifiers prepared in examples 1 to 12 above were mixed at a cracked oil concentration of 5 to 10mg/kg and a volume ratio of 1:1.0 to 1:1.2 of ethylene pyrolysis oil washing water is added into the colorimetric tube together. Placing the colorimetric tube in a constant temperature oscillator, oscillating for 4 minutes at 55 ℃ and 200 times/min, taking out and placing in a constant temperature water bath at the temperature, standing for 30 minutes to break emulsion, observing and recording the interface condition of oil and water phases and the cleanliness of the water phase, taking a separated water sample to perform oil content and turbidity analysis, wherein a turbidity meter with the model of SIN-PTU300 is used for measuring the turbidity of the separated water sample, and the GB/T16488-1996 standard is used for measuring the oil content of the water phase. The experimental results are shown in table 2 below.
Examples 35 to 40 were tested as performance tests for other demulsifiers of comparative examples.
In examples 35 to 38, a single first component or a single second component was used, and the same test method as in example 13 was used to determine the performance. The experimental results are shown in table 2 below.
In example 39 and example 40, a demulsifier was not used, and the same test method as in example 13 was used to judge the performance. The experimental results are shown in table 2 below.
Table 2: the effect of the demulsifier on treating washing water of ethylene pyrolysis oil
From the above table 2, it can be seen that the above examples of the present invention show that the demulsifier of the present application can be demulsified at a relatively low temperature, and a clear water-oil interface can be obtained during demulsification. As can be seen when comparing example 39 and example 40 (without demulsifier), not only was the water phase cleanliness much improved, but the water phase turbidity to water phase oil content values were also significantly less than for the examples without demulsifier after using the demulsifier of the present application. Furthermore, it can be seen from examples 35-38 that, whilst a clear water-oil interface can be obtained with the use of a demulsifier of a single composition, the water phase cleanliness is significantly less than that of examples 13-34 using the demulsifiers of the applications. Also, while the aqueous phase turbidity and aqueous phase oil content after the use of a single demulsifier was superior to examples 39 and 40 where no demulsifier was used, examples 35-38 still exhibited satisfactory results compared to the demulsifier of the present application. Unlike the results of examples 35 to 40, examples 13 to 34 of the present application all exhibited excellent turbidity of the aqueous phase and oil content of the aqueous phase.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A demulsifier, comprising:
a first component selected from one or more of polyoxyethylene polyamine polyoxypropylene polyoxyethylene ether and polyoxyethylene polyamine polyoxypropylene polyoxyethylene ether;
a second component selected from the group consisting of polyoxyethylene polyoxypropylene glycol monoether and polyoxyethylene polyoxypropylene stearyl ether in combination of one or more thereof;
a dissolution promoter; and
a solvent.
2. The demulsifier of claim 1, wherein the first component is present in an amount of from 25 to 30 parts by weight, based on 100 parts by weight of the demulsifier; the weight part of the second component is 10 to 15 weight parts; the weight part of the dissolution promoter is 5 to 10 weight parts; and the weight part of the solvent is 45 to 60 parts by weight.
3. The demulsifier of claim 1, wherein the dissolution promoter is an alcohol or an alcohol ether.
4. The demulsifier of claim 3, wherein the dissolution promoter is selected from the group consisting of methanol, ethanol, isopropanol, n-butanol, cyclohexanol, benzyl alcohol, terpineol, propylene glycol, glycerol, ethylene glycol, pentanol, hexanol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monobutyl ether, or any combination thereof.
5. The demulsifier of claim 1, wherein the solvent is water.
6. A method for preparing the demulsifier of any one of claims 1-5, comprising the steps of
S1, mixing a first component, a second component and a solvent to obtain a mixture;
and S2, mixing the mixture with a dissolution promoter to obtain the demulsifier.
7. The method according to claim 6, characterized in that in step S1, mixing is performed under stirring.
8. The method according to claim 6 or 7, characterized in that in step S2, the dissolution accelerating agent is added to the mixture at a temperature in the range of 45 ℃ to 55 ℃.
9. The method according to claim 8, wherein in the step S2, after the dissolution accelerating agent is added to the mixture, the mixture is left to stand for 60 to 80 minutes.
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| CN101121898A (en) * | 2007-07-30 | 2008-02-13 | 辽宁大学 | Fast emulsion breaking method |
| US20090186782A1 (en) * | 2007-06-28 | 2009-07-23 | High Grade Technology Co., Ltd. | Mixed demulsifier of asp flooding produced liquid |
| CN103937539A (en) * | 2014-05-13 | 2014-07-23 | 陕西省石油化工研究设计院 | method for preparing condensate oil demulsifier and application thereof |
| CN103965459A (en) * | 2014-05-13 | 2014-08-06 | 新疆福利精细化工厂 | Preparation method of demulsifying agent |
| CN109943360A (en) * | 2017-12-21 | 2019-06-28 | 中国石油化工股份有限公司 | A kind of Compositional type heavy oil low-temperature demulsifier |
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2021
- 2021-06-09 CN CN202110644549.4A patent/CN115449394A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090186782A1 (en) * | 2007-06-28 | 2009-07-23 | High Grade Technology Co., Ltd. | Mixed demulsifier of asp flooding produced liquid |
| CN101121898A (en) * | 2007-07-30 | 2008-02-13 | 辽宁大学 | Fast emulsion breaking method |
| CN103937539A (en) * | 2014-05-13 | 2014-07-23 | 陕西省石油化工研究设计院 | method for preparing condensate oil demulsifier and application thereof |
| CN103965459A (en) * | 2014-05-13 | 2014-08-06 | 新疆福利精细化工厂 | Preparation method of demulsifying agent |
| CN109943360A (en) * | 2017-12-21 | 2019-06-28 | 中国石油化工股份有限公司 | A kind of Compositional type heavy oil low-temperature demulsifier |
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