CN112048336A - Demulsification dehydration additive suitable for heavy crude oil and preparation method thereof - Google Patents
Demulsification dehydration additive suitable for heavy crude oil and preparation method thereof Download PDFInfo
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- CN112048336A CN112048336A CN202010754568.8A CN202010754568A CN112048336A CN 112048336 A CN112048336 A CN 112048336A CN 202010754568 A CN202010754568 A CN 202010754568A CN 112048336 A CN112048336 A CN 112048336A
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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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Abstract
The invention relates to a demulsification dehydration additive suitable for heavy crude oil and a manufacturing method thereof, wherein the demulsification dehydration additive comprises a polyoxyethylene ether component, the polyoxyethylene ether component accounts for about 10-40% of the total mass of the demulsification dehydration additive, and the polyoxyethylene ether component is preferably selected from one or two of polyoxypropylene polyoxyethylene ether and alkylphenol formaldehyde resin polyoxyethylene ether; hydrophilically treated inorganic particles, preferably selected from cement clinker particles; the mass ratio of the hydrophilically treated inorganic particles to the polyoxyethylene ether component is from about 1:20 to 1: 50; the balance of alkyl alcohol is used as solvent. The demulsification dehydration additive is particularly suitable for heavy oil treatment, and can improve and maintain an effective demulsification function on the basis of ensuring that the components of the additive do not increase the cost.
Description
Technical Field
The invention relates to the fields of polymer, organic chemistry and petrochemical industry, in particular to a demulsification composition, and more particularly relates to a demulsification dehydration additive suitable for heavy crude oil.
Background
China is a country with large energy demand and large energy consumption in the world, and energy sources such as petroleum and the like related to national safety are important for the operation development of industrial enterprises and the smooth operation of society. As crude oil production increases, heavy crude oil of poor quality or high consistency, which is difficult to handle, is also gradually taken into the focus of development.
However, in the process of crude oil development, heavy oil with high water content needs to be dehydrated to ensure subsequent processes such as processing and transportation. And the heavy crude oil is difficult to dehydrate, the existing demulsifiers have few varieties, and the demulsifiers particularly suitable for heavy oil development also have few varieties and high price.
Workers have developed demulsification processes and formulations for heavy oils. For example, chinese patent CN108913200A discloses a demulsifier for dewatering thick oil and a manufacturing method thereof. The demulsifier comprises 40-60 wt% of a demulsifier main agent, 1-2 wt% of a demulsifier auxiliary agent, 10-20 wt% of a polymer penetrant and the balance of water; the demulsifier additive is one of calcium nitrate and sodium chloride; the polymer penetrant is sulfomethylated polyacrylamide. The demulsifier has the characteristics of simple synthesis process, low cost, strong adaptability and high low-temperature demulsification rate, and the demulsification rate of the demulsifier to the thickened oil reaches more than 99.0 percent when the temperature is 50 ℃ and the concentration is 50 ppm. Therefore, the method can be widely applied to the dehydration and oil removal treatment of the thick oil. However, in practice, the demulsifier adopts the organic silicon surfactant, sulfomethylated polyacryl and the like as auxiliary materials, and the main raw materials and the auxiliary raw materials are expensive in cost and difficult to apply to actual large-scale oilfield exploitation. The additive contains a large amount of auxiliary additives, possibly brings secondary environmental pollution, and also has no practical application prospect.
Therefore, there is a need for a demulsifier and a method for producing the same, which has an improved demulsification effect, and simultaneously has application convenience and economic advantages, and is particularly suitable for demulsifying components in heavy oil field development.
Disclosure of Invention
From the above related art, one aspect of the present invention is to provide a demulsifying and dehydrating additive suitable for heavy crude oil, the demulsifying and dehydrating additive comprising the following components:
the polyoxyethylene ether component accounts for about 10-40% of the total mass of the demulsification dehydration additive, and is preferably selected from one or two of polyoxypropylene polyoxyethylene ether and alkylphenol formaldehyde resin polyoxyethylene ether;
hydrophilically treated inorganic particles, preferably selected from cement clinker particles; the mass ratio of the hydrophilically treated inorganic particles to the polyoxyethylene ether component is from about 1:20 to 1: 50;
the balance is alkyl alcohol with 1-3 carbon atoms as solvent.
As will be described in detail in the following detailed description of the present invention, the inventors have surprisingly found that the hydration effect of cement clinker particles when mixed with residual moisture in heavy oil can be better utilized, particularly after hydrophilic treatment, and the more fine residual moisture is carried into the water phase and separated from the heavy oil by utilizing the modified hydrophilic effect. The cement clinker particles of the present invention may preferably be selected from any slag cement clinker obtained, for example, by subjecting said slag cement clinker to a combination of aluminum oxide, silicon oxide, calcium oxide, and iron oxide, after high temperature calcination.
According to an alternative, wherein the hydrophilic-treated inorganic particles are coated-treated with a hydrophilic treatment agent, the hydrophilic treatment agent treatment is preferably selected from polyethylene glycol dimethacrylate.
According to a preferred embodiment, the alkyl alcohol having 1 to 3 carbon atoms is ethanol, and more preferably is anhydrous ethanol.
In a preferred embodiment, the mass ratio of the hydrophilically-treated inorganic particles to the polyoxyethylene ether component is about 1: 25.
In a further preferable scheme, the polyoxyethylene ether component is prepared from polyoxypropylene polyoxyethylene ether and alkylphenol formaldehyde resin polyoxyethylene ether according to the mass ratio of 1: 1.
In an alternative scheme, in the demulsification dehydration additive suitable for the heavy crude oil, the polyoxyethylene ether component is preferably polyoxypropylene polyoxyethylene ether.
In another aspect of the present invention, there is provided a method for producing a demulsifying and dehydrating additive suitable for use in heavy crude oil, the method comprising the steps of:
step 1), mixing cement clinker particles and a hydrophilic treatment agent according to a ratio of 1: 0.2-1: 1, said hydrophilic treatment agent being preferably selected from polyethylene glycol dimethacrylate, such that said hydrophilic treatment agent covers said cement clinker particles to obtain hydrophilically treated inorganic particles;
step 2), in a reaction vessel in which the hydrophilically treated inorganic particles are placed, according to the hydrophilically treated inorganic particles: the polyoxyethylene ether component is 1:20 to 1: 50, adding the polyoxyethylene ether component into a reaction container and stirring;
step 3), adding an alkyl alcohol with 1-3 carbon atoms as a solvent into a reaction vessel for completing the step 2), preferably stirring and heating the obtained mixed system for 15 minutes for a period of time, and then cooling to room temperature to obtain the demulsification and dehydration additive; and wherein
The polyoxyethylene ether component accounts for about 10-40% of the total mass of the demulsification dehydration additive.
In an alternative method, the alkyl alcohol with 1-3 carbon atoms is absolute ethyl alcohol, and the absolute ethyl alcohol accounts for about 58-85% of the total mass of the demulsification dehydration additive.
The technical solutions and advantages of the present invention will be explained and explained in more detail below with reference to specific embodiments. It should be understood that the contents presented in the description and the detailed description are only for more clearly illustrating the technical solutions and the advantages of the present invention, and do not limit the protection scope of the present invention. On the basis of the disclosure of the specification, a person skilled in the art can modify the technical solution according to various reasonable changes, and the modified technical solution should be understood as being included in the protection scope of the invention as long as the person does not depart from the spirit of the invention.
Detailed Description
The present invention is described in more detail below to facilitate an understanding of the invention.
Before the description of the specific embodiments, the essential fact that part of the main raw materials used have been sourced is described in the present specification. It should be noted that the sources of the raw materials described in the embodiments herein are not limiting, and those skilled in the art can select appropriate raw materials and testing equipment to perform the relevant tests and obtain the corresponding results according to the teaching and teaching of the present invention, and for raw materials which do not describe a specific manufacturer or route, those skilled in the art can select raw materials as the reaction starting materials to meet the corresponding requirements according to the disclosure and requirements of the present specification. It will also be understood from the disclosure of the present specification that the reaction starting materials for the synthesis of a portion of the compounds are derived from the initial product synthesized in the preceding step of the present invention.
The individual components for the demulsifiers employed in the present invention are commercially available, and in the alternative, may be prepared by specific or specialized processes, which do not limit the ability of those skilled in the art to practice the invention upon reading this specification. For better illustration, the use and source of some of the main raw materials are described.
Polyoxypropylene polyoxyethylene ether: polyoxypropylene polyoxyethylene ether (F-38), purchased from Shanghai Beike chemical; referred to in the examples as feedstock a 1;
alkylphenol formaldehyde resin polyoxyethylene ether: procurement from chenchen station blue sky fine chemistry; referred to in the examples as feedstock a 2;
cement clinker particles (powder): slag cement clinker from shanxi witton;
a hydrophilic treatment agent: polyethylene glycol dimethacrylate; purchased from Jiangsu Nantong manor chemical Co., Ltd;
solvent: ethanol, preferably absolute ethanol with the content of more than or equal to 99.5 percent is purchased from south east chemical industry of Jiangsu.
Example 1: preparation of Components and preparation of demulsifiers
Step 1) taking 200g of cement clinker powder crushed to have an average particle size of below 500 mu m, adding 50g of polyethylene glycol dimethacrylate (according to the proportion of cement clinker particles to hydrophilic treatment agent polyethylene glycol dimethacrylate being 1: 0.25) and stirring until the hydrophilic treatment agent is uniformly mixed with the cement clinker particles, so that the hydrophilic treatment agent uniformly wraps the cement clinker particles; adding the treated particles to a reaction vessel;
step 2) adding 5Kg of polyoxypropylene polyoxyethylene ether into a reaction vessel, stirring while adding, and continuously stirring for 15 minutes;
and 3) adding 10Kg of ethanol into the system obtained in the step 2), heating to about 40 ℃, stirring for 15 minutes, cooling to room temperature, and discharging the prepared demulsifier from the container to a storage warehouse for storage.
Example 2: determination of dehydration ratio of heavy crude oil
The heavy crude oil in this experiment was taken from a sample from a victory oil field and tested to have a density of 918kg/m3The original water content of the crude oil is 41.5% (the volume water content is tested and calibrated according to the specification of a standard SY/T5402). The test of the dewatering rate was carried out according to the general standard Q/SH 10201418-2013. In the experiments of the present invention specifically:
the amount of the dehydration demulsifier used for the heavy crude oil in the test was 125 mg/L. The prepared crude oil emulsion is poured into a measuring cylinder of a specified volume (for example 100ml) and the crude oil emulsion is heated to 60 ℃ at constant temperature in a water bath.
Adding the demulsifier solution according to the dosing proportion. And (3) turning the measuring cylinder upside down for a plurality of times by closing the measuring cylinder, then resealing the measuring cylinder and violently shaking the measuring cylinder up and down for about 100 times after deflation, wherein the amplitude of each time is more than 10cm, and placing the measuring cylinder into the water bath again for sedimentation after fully mixing the materials again.
The crude oil dehydration rate S is calculated according to the following formula:
S＝V/(V0×Wv) X 100%, wherein S is the dehydration rate of the crude oil demulsifier, and V is the water yield (ml) of the crude oil emulsion after sedimentation; wvThe water content is the volume water content of the crude oil emulsion; v0Is the crude oil emulsion volume.
For each sample, 5 replicates and tests were made and the arithmetic mean was taken as the measurement.
The emulsified crude oil of example 1, when tested according to the test method of example 2, yielded a dehydration rate of about 99.6%, which far exceeded the application standard recognized in industry enterprise standard Q/SH10201418-2013 for heavy crude oil having a dehydration rate greater than 80%, while also being comparable to or superior to the demulsifier compositions of the related art. Meanwhile, the cost of the product applied by the patent technology is only 30-50% of the cost of the heavy oil treatment emulsion composition in the related technology, and the method has a large-scale application prospect with excellent improvement and optimistic economic benefit.
Example 3:
example 3 is similar to example 1, except that in the main components of the demulsifier used in this example, the mass ratio of polyoxypropylene polyoxyethylene ether to alkylphenol formaldehyde resin polyoxyethylene ether is 1:1 (2.5 Kg each) was used as the process flow of step 2) of example 1, and the other process steps were the same as in example 1, and the description thereof was omitted.
The emulsifier of example 3 was tested with a sample of the same field to give about 99.8% test results.
Comparative example 1:
comparative example 1 the same procedure as in example 1 was used. But no hydrophilized inorganic particles are used. In the specific implementation process, 5Kg of polyoxypropylene polyoxyethylene ether is added into a reaction vessel, and the mixture is properly stirred after the addition; and adding 10Kg of ethanol into the system, heating the system to about 40 ℃, stirring the mixture for 15 minutes, cooling the mixture to room temperature, and discharging the prepared demulsifier from a container to a storage warehouse for storage.
Comparative example 1'
Comparative example 1' the same procedure as in example 2 was used. But no hydrophilized inorganic particles are used. Adding 2.5Kg of polyoxypropylene polyoxyethylene ether and alkylphenol formaldehyde resin polyoxyethylene ether into a reaction vessel, properly stirring, adding 10Kg of ethanol into the system, heating to about 40 ℃, stirring for 15 minutes, cooling to room temperature, and discharging the prepared demulsifier from a container to a storage warehouse for storage.
Comparative example 1 and comparative example 1 'were each tested according to the experimental method of example 2, and the results showed that comparative example 1 obtained a water-oil separation rate of about 94.5%, comparative example 1' obtained a separation rate of about 96%, and the separation rates were not improved compared to examples 1 and 2.
The inventors do not wish to be bound by any theory, but one possible explanation is that the cement clinker particles themselves have a strong hydration behavior, mainly formed by high temperature calcination of aluminum, silicon oxides, calcium oxides and/or slag oxides, which enables further entrainment of residual moisture in the heavy crude oil in an oily environment. The hydrophilic treating agent plays a role in temporarily protecting cement clinker particles, and avoids the cement clinker particles from violently forming slurry with water and preventing adhesive substances from being retained in the emulsion oil layer. Meanwhile, the film layer of the hydrophilic treatment agent further drives clinker particles to enter the water phase, so that unnecessary residues in crude oil are avoided.
The cement clinker particles and powders of the embodiments of the present invention may be obtained from commercial sources, or may be manufactured by processes known in the art, such as slag cement clinker manufactured according to the chinese patent publication CN103435281A process, or activated cement clinker sintered by the self-service demulsifier processing company.
Example 4
In this example, the ratio (mass ratio) of the cement clinker to the polyoxyethylene ether component is adjusted:
table 1: dehydration performance of different cement clinker and polyoxyethylene ether components
As can be seen from Table 1, whether A1 (polyoxyethylene polyoxypropylene ether) alone or a combination of A1 and A2 (polyoxyethylene alkylphenol formaldehyde resin) is used, the ratio of the polyoxyethylene ether components in the cement clinker to the components of the present invention is from 1: between 50 and 1:20, a more excellent dewatering ratio is achieved. When the ratio exceeds 1:20, the efficiency does not rise significantly (see 1:10 in the table and the dewatering effect of example 3), and when the ratio exceeds 1:10 and is closer to 1:1, the improvement in efficiency is reduced, and the reason for the reduction may be the result of premature hydration during use due to the increase in the ratio of cement clinker, resulting in failure to bring residual water into the aqueous phase in a dispersed and effective state.
In a preferred embodiment of the invention, the emulsion breaker component preferably does not contain moisture during the use of the inorganic cement clinker, and the ethanol preferably uses high-purity ethanol, so as to prevent cement clinker particles from releasing their hydration properties in advance even under the protection of hydrophilic components.
Example 5:
in order to take into account the effect of the invention on heavy oils, the inventors obtained oils from different oil fields, wherein the light oil had a crude oil density of 860kg/m3The density of the medium crude oil is 905kg/m3The dehydration rate of the demulsifier component is higher than 99.5% when the demulsifier component is applied to medium and light crude oil, which shows that the demulsification and dehydration effects of the demulsifier are hardly reduced when the demulsifier component is applied to light crude oil to heavy crude oil. The product of the invention is particularly suitable for the oil field exploitation of heavy crude oil and has market value of large-scale application.
According to the embodiments and technical contents described in the present specification, the present invention can provide at least the following technical means: while the present disclosure includes specific embodiments, it will be apparent to those skilled in the art that various substitutions or alterations in form and detail may be made to these embodiments without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents. The embodiments described herein are to be considered in all respects only as illustrative and not restrictive. The description of features and aspects in each embodiment is believed to be applicable to similar features and aspects in other embodiments. Therefore, the scope of the present disclosure should be defined not by the detailed description but by the claims, and all changes within the scope of the claims and equivalents thereof should be construed as being included in the technical solution of the present disclosure.
The invention at least provides the following technical scheme:
scheme 1. a demulsifying and dehydrating additive suitable for heavy crude oil, which is characterized in that
The demulsification dehydration additive comprises the following components:
the polyoxyethylene ether component accounts for about 10-40% of the total mass of the demulsification dehydration additive, and is preferably selected from one or two of polyoxypropylene polyoxyethylene ether and alkylphenol formaldehyde resin polyoxyethylene ether;
hydrophilically treated inorganic particles, preferably selected from cement clinker particles; the mass ratio of the hydrophilically treated inorganic particles to the polyoxyethylene ether component is from about 1:20 to 1: 50;
the balance is alkyl alcohol with 1-3 carbon atoms as solvent.
Scheme 2. the demulsifying and dehydrating additive suitable for heavy crude oil according to scheme 1, wherein the hydrophilic-treated inorganic particles are coated with a hydrophilic treatment agent, preferably selected from polyethylene glycol dimethacrylate.
Scheme 3. the demulsifying and dehydrating additive suitable for heavy crude oil according to scheme 1 or 2, wherein the alkyl alcohol with 1-3 carbon atoms is ethanol, and more preferably absolute ethanol.
Scheme 4. the demulsifying and dehydrating additive suitable for heavy crude oil according to any one of the schemes 1 to 3,
wherein the mass ratio of the hydrophilically treated inorganic particles to the polyoxyethylene ether component is about 1: 25.
Scheme 5. the demulsifying and dehydrating additive suitable for heavy crude oil according to any one of the schemes 1 to 4,
the polyoxyethylene ether component is prepared from polyoxypropylene polyoxyethylene ether and alkylphenol formaldehyde resin polyoxyethylene ether according to the mass ratio of 1: 1.
Scheme 6. the demulsifying and dehydrating additive suitable for heavy crude oil according to any one of the schemes 1 to 5,
wherein the polyoxyethylene ether component is polyoxypropylene polyoxyethylene ether.
Scheme 7. a method of making the demulsifying and dehydrating additive suitable for use in heavy crude oil according to any one of schemes 1 to 6, the method comprising the steps of:
step 1), mixing cement clinker particles and a hydrophilic treatment agent according to a ratio of 1: 0.2-1: 1, said hydrophilic treatment agent being preferably selected from polyethylene glycol dimethacrylate, such that said hydrophilic treatment agent covers said cement clinker particles to obtain hydrophilically treated inorganic particles;
step 2), in a reaction vessel in which the hydrophilically treated inorganic particles are placed, according to the hydrophilically treated inorganic particles: the polyoxyethylene ether component is 1:20 to 1: 50, adding the polyoxyethylene ether component into a reaction container and stirring;
step 3), adding an alkyl alcohol with 1-3 carbon atoms as a solvent into a reaction vessel for completing the step 2), preferably stirring and heating the obtained mixed system for 15 minutes for a period of time, and then cooling to room temperature to obtain the demulsification and dehydration additive; and wherein
The polyoxyethylene ether component accounts for about 10-40% of the total mass of the demulsification dehydration additive.
Scheme 8. the method of scheme 7, wherein the alkyl alcohol having 1-3 carbon atoms is absolute ethanol, and the absolute ethanol accounts for about 58-85%, preferably 60-70% of the total mass of the demulsifying and dehydrating additive.
Claims (8)
1. The demulsification dehydration additive suitable for the heavy crude oil is characterized by comprising the following components:
the polyoxyethylene ether component accounts for about 10-40% of the total mass of the demulsification dehydration additive, and is preferably selected from one or two of polyoxypropylene polyoxyethylene ether and alkylphenol formaldehyde resin polyoxyethylene ether;
hydrophilically treated inorganic particles, preferably selected from cement clinker particles; the mass ratio of the hydrophilically treated inorganic particles to the polyoxyethylene ether component is from about 1:20 to 1: 50;
the balance of the solvent is an alkyl alcohol having 1 to 3 carbon atoms.
2. The demulsification dehydration additive suitable for heavy crude oil according to claim 1, wherein the hydrophilic treated inorganic particles are coated with a hydrophilic treatment agent, preferably selected from polyethylene glycol dimethacrylate.
3. The demulsification dehydration additive suitable for heavy crude oil according to claim 1 or 2, wherein the alkyl alcohol with 1-3 carbon atoms is ethanol, more preferably anhydrous ethanol.
4. The demulsification dehydration additive suitable for heavy crude oil according to any of claims 1 to 3,
wherein the mass ratio of the hydrophilically treated inorganic particles to the polyoxyethylene ether component is about 1: 25.
5. The demulsification dehydration additive suitable for heavy crude oil according to any of claims 1 to 4,
the polyoxyethylene ether component is prepared from polyoxypropylene polyoxyethylene ether and alkylphenol formaldehyde resin polyoxyethylene ether according to the mass ratio of 1: 1.
6. The demulsification dehydration additive suitable for heavy crude oil according to any of claims 1 to 5,
wherein the polyoxyethylene ether component is polyoxypropylene polyoxyethylene ether.
7. A method of making the demulsifying and dehydrating additive suitable for heavy crude oil of any one of claims 1 to 6, the method comprising the steps of:
step 1), mixing cement clinker particles and a hydrophilic treatment agent according to a ratio of 1: 0.2-1: 1, said hydrophilic treatment agent being preferably selected from polyethylene glycol dimethacrylate, such that said hydrophilic treatment agent covers said cement clinker particles to obtain hydrophilically treated inorganic particles;
step 2), in a reaction vessel in which the hydrophilically treated inorganic particles are placed, according to the hydrophilically treated inorganic particles: the polyoxyethylene ether component is 1:20 to 1: 50, adding the polyoxyethylene ether component into a reaction container and stirring;
step 3), adding an alkyl alcohol with 1-3 carbon atoms as a solvent into a reaction vessel for completing the step 2), preferably stirring and heating the obtained mixed system for 15 minutes for a period of time, and then cooling to room temperature to obtain the demulsification and dehydration additive; and wherein
The polyoxyethylene ether component accounts for about 10-40% of the total mass of the demulsification dehydration additive.
8. The method of claim 7, wherein the alkyl alcohol with 1-3 carbon atoms is absolute ethanol, and the absolute ethanol accounts for about 58-85%, preferably 60-70% of the total mass of the demulsification and dehydration additive.
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| CN109704623A (en) * | 2018-11-21 | 2019-05-03 | 南京工业大学 | A kind of MgO expansion agent and its preparation method and application that in-situ polymerization surface is modified |
| 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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| CN1044290A (en) * | 1990-02-01 | 1990-08-01 | 中国石油化工总公司 | With filtration method to the oil desalting and dewatering |
| US20100167168A1 (en) * | 2005-12-15 | 2010-07-01 | Kim Dong-Pyo | Hydrophilic Adjuvant |
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| CN109704623A (en) * | 2018-11-21 | 2019-05-03 | 南京工业大学 | A kind of MgO expansion agent and its preparation method and application that in-situ polymerization surface is modified |
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