CN105778985A - Novel magnetic demulsifying agent and preparation method of novel magnetic demulsifying agent - Google Patents

Novel magnetic demulsifying agent and preparation method of novel magnetic demulsifying agent Download PDF

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Publication number
CN105778985A
CN105778985A CN201610185692.0A CN201610185692A CN105778985A CN 105778985 A CN105778985 A CN 105778985A CN 201610185692 A CN201610185692 A CN 201610185692A CN 105778985 A CN105778985 A CN 105778985A
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preparation
demulsifying agent
polyether
magnetization
product
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CN201610185692.0A
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CN105778985B (en
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方申文
陈斌
段明
熊艳
施鹏
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SHANDONG ZHANHUA LUXIN CHEMICAL Co.,Ltd.
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Southwest Petroleum University
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G33/00Dewatering or demulsification of hydrocarbon oils
    • C10G33/04Dewatering or demulsification of hydrocarbon oils with chemical means
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10Feedstock materials
    • C10G2300/1033Oil well production fluids
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20Characteristics of the feedstock or the products
    • C10G2300/201Impurities

Abstract

The invention relates to a novel magnetized blocked polyether demulsifying agent and a preparation process of the novel magnetized blocked polyether demulsifying agent. The novel magnetized blocked polyether demulsifying agent contains blocked polyether and ferriferrous oxide at a certain ratio. A manufacturing method of the novel magnetized blocked polyether demulsifying agent comprises the following steps: adding the blocked polyether and iron acetylacetonate into a solvent thermal reaction kettle; after uniformly stirring, blowing and substituting with nitrogen gas; heating to a certain temperature and reacting for certain time; cooling to a room temperature and opening a kettle; washing a product with methanol and drying the product to obtain the novel magnetized blocked polyether demulsifying agent. The prepared magnetic demulsifying agent has an excellent demulsifying effect, has a strong external magnetic field response signal and is easy to recycle, so that the prepared magnetic demulsifying agent is an environment-friendly demulsifying agent and has an extremely good application value to demulsifying of crude oil; in the preparation method provided by the invention, used materials are cheap in price and wide in source; the magnetized demulsifying agent is synthesized by adopting a one-step method, so that the reaction time and the production cost are greatly saved and reduced; the preparation process is simple and efficient, is strong in repeatability and is easy to popularize.

Description

A kind of novel magnetic demulsifier and preparation method thereof
Technical field
The present invention relates to water in oil crude oil emulsion process field in oil exploitation oil extraction transportation processing procedure, particularly relate to a kind of novel magnetic demulsifier and preparation method thereof.
Background technology
In recent years, the oil extraction in China's major part oil field has been enter into high water-cut stage, along with the exploitation of " tertiary oil recovery " technology and number of polymers, surfactant, alkali application, Produced Liquid water content rises, and part oil field mining liquid moisture content has reached more than 90%, and oil-water separation slows, even show serious emulsifying tendency, profit regardless of, define stable emulsion, cause sizable difficulty to Produced Liquid processed.
For above-mentioned situation, in the process that water-in-oil emulsion processes, it is generally required to adopt demulsifier that emulsion is carried out breakdown of emulsion process, some functional compounds loads at magnetic-particle (such as Fe3O4) surface, functional magnetic granule can be obtained.These functional magnetic granules remain the functional compound advantage being supported, for instance breakdown of emulsion, flocculation, absorption etc., also have stronger saturation magnetic field intensity simultaneously and are easily isolated recovery.
At present, both at home and abroad water-in-oil emulsion is processed the demulsifier adopted to conduct extensive research, also achieve some achievements, as) application number be 201310534158.2 " preparation method of a kind of magnetic antiphase demulsifier ", application number be 201410494294.8 " a kind of heavy oil dewater the preparation method with magnetic double-face granular pattern demulsifier ", application number be 201410324184.7 " high-efficient demulsifier of the controlled recovery of magnetic for water-in-oil system emulsion and preparation method thereof ".But these demulsifiers, in cost of manufacture and technology difficulty, still have much room for improvement.
In currently used demulsifier, block polyether owing to its de-emulsification speed is fast, water-in-oil emulsion is processed after water-oil phase degree of purity very popular compared with advantages of higher.But how to reduce its production and application cost, allow the process procedure more environmental protection of whole breakdown of emulsion, also day by day have become as the problem urgently overcome.Therefore, block polyether is combined with magnetochemistry as a kind of functional compounds with demulsification performance, while retaining demulsification performance so that it is can recycle, convenient production, reduce production and application cost, oil field is produced and is significant.
Summary of the invention
For the problems referred to above, it is an object of the invention to the deficiency overcoming prior art to exist, it is provided that a kind of magnetization block polymer demulsifier, technical scheme is as follows:
A kind of magnetization block polymer demulsifier, containing block polyether and ferroso-ferric oxide, the structural formula of described block polyether is:
In the structural formula of described block polyether: m=1, n=6, p=9.
Its preparation method comprises the following steps:
(1) in solvent thermal reaction still, add block polyether and ferric acetyl acetonade, and stir, form suspension;
(2) with nitrogen, hot solvent reactor is purged displacement, the oxygen within kettle is taken away, replaces with nitrogen;
(3) solvent thermal reaction still is heated, allowing is in isoperibol inside kettle, the suspension in step (1) is made to react, ferric acetyl acetonade generation redox reaction generates ferroso-ferric oxide later, under the parcel of block polyether, ferroso-ferric oxide becomes the magnetic nano-particle presenting monodisperse status, forms the product of the nucleocapsid structure of stable chemical performance;
(4) open hot solvent reactor after being cooled to room temperature, take out the product generated in step (3), and with block polyether excessive after methanol washing reaction;
(5) dry the methanol of residual on the product after washing, obtain finished product.
Further, in the step (1) of described preparation method, the mass ratio of block polyether and ferric acetyl acetonade be following any one: 1:1,2:1,3:1,4:1 and 5:1.
Further, in the step (2) of described preparation method, passing into nitrogen from reactor kettle bottom, and discharged from kettle top by air, it is 30 minutes that nitrogen purges time swap.
Further, in the step (3) of described preparation method, generating product and start to increase with temperature increase from 180 DEG C, reaction temperature tends towards stability after 200 DEG C.
Further, in the step (3) of described preparation method, reaction temperature be following any one: 200 DEG C, 210 DEG C or 220 DEG C.
Further, in the step (3) of described preparation method, the response time is 6~10 hours.
Further, in the step (3) of described preparation method, the response time be following any one: 6 hours, 7 hours, 8 hours, 9 hours and 10 hours.
It is an advantage of the current invention that:
1, demulsifier provided by the invention for water-in-oil system emulsion, efficiently can quickly realize breakdown of emulsion process, and utilize magnetic field to reclaim completely, it is easy to separates, it is to avoid demulsifier causes the drawback of extra power consumption and the wasting of resources because not reclaiming.Demulsifier after separation, through cleaning process simply and reusable, even if repeatedly its breakdown of emulsion efficiency still remains stable for, can be widely applied to the process field of oil exploitation oil-polluted water;
2, the preparation method of the present invention uses material price is cheap, wide material sources;
3, comparing traditional method to need to adopt multiple devices, carry out multi-step processing and could prepare product up to standard, the present invention adopts one-step method can synthesize magnetization demulsifier, and its preparation technology is simply efficient, repeatable strong, it is easy to promote.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of the embodiment of the present invention 1 magnetic demulsifier;
Fig. 2 is the embodiment of the present invention 1 magnetic demulsifier XRD spectra;
Fig. 3 is the thermogravimetric curve figure of the embodiment of the present invention 1 block polyether and magnetic demulsifier;
Fig. 4 is the embodiment of the present invention 1 magnetic demulsifier hysteresis curve figure.
Detailed description of the invention
Below in conjunction with the embodiment in the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
The experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, all commercially obtain.
Embodiment 1,
Weigh 12 grams of block polyethers according to block polyether and mass ratio that ferric acetyl acetonade is 4:1 and 3 grams of ferric acetyl acetonades are placed in solvent thermal reaction still, after stirring, pass into nitrogen and purge displacement oxygen 30 minutes, it is subsequently placed in the baking oven of 200 DEG C and reacts 6 hours, after solvent thermal reaction still is cooled to room temperature, open still methanol washed product, drying product magnetic demulsifier.
The structural characterization of magnetic demulsifier of the present invention is analyzed, analyzes situation as follows.
As it is shown in figure 1, carry out IR spectrum scanning with Fourier infrared spectrograph after the magnetic demulsifier pellet technique tabletting prepared by embodiment 1, obtain Fig. 1 gained infrared spectrum, 3426cm in spectrogram-1And 1627cm-1Represent stretching vibration absworption peak and bending vibration absworption peak, the 1405cm of hydroxyl in block polyether respectively-1And 1115cm-1Represent the vibration absorption peak of carbonyl and carbon-oxygen bond, 565cm in block polyether ester group respectively-1For Fe3O4Extraordinary absworption peak.
As in figure 2 it is shown, use PertProX-ray diffractometer (Cu target, wavelength=0.1541nm, tube voltage 40kV, tube current 20mA) to measure crystal structure the magnetic demulsifier prepared by the present invention, obtain XRD spectra.It is 30.09 ° at 2 jiaos, 35.44 °, 43.07 °, 53.43 °, 56.96 °, distinguishes corresponding Fe with the diffraction maximum of 74.00 ° for 62.55 °3O4(220), (311), (400), (422), (511), (440) and (533) crystal face.
As it is shown on figure 3, block polyether is carried out thermogravimetric analysis with the magnetic demulsifier obtained by the present invention in nitrogen atmosphere.Block polyether decomposes by 300 DEG C, decomposes completely during to 410 DEG C, and magnetic demulsifier also occurs in this temperature range at 630 DEG C, first time is weightless, occurs that second time is weightless, and second time is weightless is because the steam reduction Fe that Organic substance decomposes3O4Caused by.
As shown in Figure 4, prepared magnetic demulsifier is carried out saturation magnetic field strength test with vibrating specimen magnetometer between magnetic field intensity-20000 oersted to 20000 oersteds.The saturation magnetic field intensity of magnetic demulsifier is 41emu/g, and remanent magnetism and coercivity are 0, present superparamagnetism.
In conjunction with above-mentioned three kinds of analysis means it can be seen that be successfully prepared magnetic demulsifier by block polyether and ferric acetyl acetonade, organic component therein is polyethers, and inorganic component is ferroso-ferric oxide.
The magnetic demulsifier demulsification performance that the present invention is prepared carries out dewatering experiment, and process is as follows:
With 80mL crude oil emulsion, (the centesimal sodium-chloride water solution of crude oil+50% by 50% is constituted, comprehensive water cut 50%) for processing object, magnetization demulsifier consumption is 0.05g, when temperature is 70 DEG C, using the product synthesized by embodiment 1 as demulsifier, when temperature is 70 DEG C, the dehydrating effect of difference demulsifier dosage is in Table 1.As shown in Table 1, when magnetizing demulsifier dosage more than 0.05g, dehydrating effect can reach 100%.
Demulsifier dosage and dehydration rate relation in table 1 embodiment 1
With above-mentioned crude oil for processing object, using the product synthesized by embodiment 1 as demulsifier, temperature is 70 DEG C, when demulsifier dosage is 0.05g, magnetizes the impact on dehydrating effect of the demulsifier recovered frequency in Table 3.As shown in Table 3, magnetization demulsifier still has good dehydrating effect after recycling at three times, and dehydration rate still has more than 85%.
Table 2 embodiment 1 magnetizes demulsifier recovered frequency and dehydration rate relation
Embodiment 2,
Adopting the manufacture method in embodiment 1, the mass ratio adjusting block polyether and ferric acetyl acetonade is 1:1, and arranging temperature of reaction kettle is 220 DEG C, reacts 10 hours.
Experimental technique described in products therefrom embodiment 1 is carried out breakdown of emulsion experiment, breakdown of emulsion experiment effect as shown in Table 3 and Table 4:
Demulsifier dosage and dehydration rate relation in table 3 embodiment 2
Table 4 embodiment 2 magnetizes demulsifier recovered frequency and dehydration rate relation
Embodiment 3,
Adopting the manufacture method in embodiment 1, the mass ratio adjusting block polyether and ferric acetyl acetonade is 3:1, and arranging temperature of reaction kettle is 200 DEG C, reacts 8 hours.
Experimental technique described in products therefrom embodiment 1 is carried out breakdown of emulsion experiment, breakdown of emulsion experiment effect as shown in table 5 and table 6:
Demulsifier dosage and dehydration rate relation in table 5 embodiment 3
Table 6 embodiment 3 magnetizes demulsifier recovered frequency and dehydration rate relation
Embodiment 4,
Adopting the manufacture method in embodiment 1, the mass ratio adjusting block polyether and ferric acetyl acetonade is 1:1,2:1,3:1,4:1 and 5:1, and arranging temperature of reaction kettle is 200 DEG C, reacts 8 hours.With above-mentioned crude oil for processing object, different product dehydration rates under different time are as shown in table 7.
The different product dehydration rate under different time of table 7
To sum up Evaluation results, from embodiment 1~4 it can be seen that the magnetic demulsifier prepared by the present invention has outstanding demulsification, and additional magnetic responsiveness signal is strong, it is easily recycled, is the demulsifier of a kind of environmental protection, crude oil emulsion breakdown of emulsion is had fabulous using value.
Nucleocapsid structure is formed when block polyether and ferric acetyl acetonade reaction, ferroso-ferric oxide is in intermediate formation core, outside is coated block polyether, in water-in-oil emulsion processing procedure, block polyether plays main demulsification, after end processes, just magnetization demulsifier can being inhaled by arranging externally-applied magnetic field (as put block Magnet outside dehydration bottle), separating step is easy and simple to handle, easy to spread, demulsifier is reusable edible after treatment.
The above is only the preferred embodiment of the present invention, it is noted that the invention is not limited in aforesaid way, under the premise without departing from the principles of the invention, moreover it is possible to improve further, and these improvement also should be regarded as protection scope of the present invention.

Claims (8)

1. a magnetization block polymer demulsifier, it is characterised in that containing block polyether and ferroso-ferric oxide, the structural formula of described block polyether is:
In the structural formula of described block polyether: m=1, n=6, p=9.
2. a kind of magnetization block polymer demulsifier according to claim 1, it is characterised in that the present invention also provides for preparation method, comprises the following steps:
(1) in solvent thermal reaction still, add block polyether and ferric acetyl acetonade, and stir, form suspension;
(2) with nitrogen, hot solvent reactor is purged displacement, the oxygen within kettle is taken away, replaces with nitrogen;
(3) solvent thermal reaction still is heated, allowing is in isoperibol inside kettle, the suspension in step (1) is made to react, ferric acetyl acetonade generation redox reaction generates ferroso-ferric oxide later, under the parcel of block polyether, ferroso-ferric oxide becomes the magnetic nano-particle presenting monodisperse status, forms the product of the nucleocapsid structure of stable chemical performance;
(4) open hot solvent reactor after being cooled to room temperature, take out the product generated in step (3), and with block polyether excessive after methanol washing reaction;
(5) dry the methanol of residual on the product after washing, obtain finished product.
3. the preparation method of a kind of magnetization block polymer demulsifier according to claim 2, it is characterized in that, in the step (1) of described preparation method, the mass ratio of block polyether and ferric acetyl acetonade be following any one: 1:1,2:1,3:1,4:1 and 5:1.
4. the preparation method of a kind of magnetization block polymer demulsifier according to claim 2, it is characterized in that, in the step (2) of described preparation method, nitrogen is passed into from hot solvent reactor kettle bottom, and air is discharged from kettle top, it is 30 minutes that nitrogen purges time swap.
5. the preparation method of a kind of magnetization block polymer demulsifier according to claim 2, it is characterized in that, in the step (3) of described preparation method, generating product and start to increase with temperature increase from 180 DEG C, reaction temperature tends towards stability after 200 DEG C.
6. the preparation method of a kind of magnetization block polymer demulsifier according to claim 5, it is characterised in that in the step (3) of described preparation method, reaction temperature be following any one: 200 DEG C, 210 DEG C and 220 DEG C.
7. the preparation method of a kind of magnetization block polymer demulsifier according to claim 2, it is characterised in that in the step (3) of described preparation method, the response time is 6-10 hour.
8. the preparation method of a kind of magnetization block polymer demulsifier according to claim 7, it is characterized in that, in the step (3) of described preparation method, the response time be following any one: 6 hours, 7 hours, 8 hours, 9 hours and 10 hours.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106830248A (en) * 2017-03-14 2017-06-13 长江大学 For the preparation method of the magnetic Nano water treatment agent of oilfield sewage
CN112138430A (en) * 2020-09-07 2020-12-29 同济大学 Magnetic nanorod demulsifier, preparation method thereof and method for treating nanoemulsion by using magnetic nanorod demulsifier

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103553181A (en) * 2013-10-31 2014-02-05 东南大学 Preparation method of magnetic antiphase demulsifier
CN103739837A (en) * 2013-12-20 2014-04-23 西南石油大学 Block polyether oilfield sewage treatment agent taking N'N-dimethyl ethanolamine as initiator and preparation method thereof
CN104073287A (en) * 2014-07-08 2014-10-01 清华大学 High-efficiency magnetic demulsifier capable of being controllably recovered aiming at water-in-oil system emulsion and preparation method thereof
CN104370333A (en) * 2014-10-24 2015-02-25 中国海洋石油总公司 Preparation method of high-interfacial-activity reverse demulsifier
CN104387712A (en) * 2014-11-03 2015-03-04 遵义医学院 Nano composite carrier with superparamagnetism and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103553181A (en) * 2013-10-31 2014-02-05 东南大学 Preparation method of magnetic antiphase demulsifier
CN103739837A (en) * 2013-12-20 2014-04-23 西南石油大学 Block polyether oilfield sewage treatment agent taking N'N-dimethyl ethanolamine as initiator and preparation method thereof
CN104073287A (en) * 2014-07-08 2014-10-01 清华大学 High-efficiency magnetic demulsifier capable of being controllably recovered aiming at water-in-oil system emulsion and preparation method thereof
CN104370333A (en) * 2014-10-24 2015-02-25 中国海洋石油总公司 Preparation method of high-interfacial-activity reverse demulsifier
CN104387712A (en) * 2014-11-03 2015-03-04 遵义医学院 Nano composite carrier with superparamagnetism and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106830248A (en) * 2017-03-14 2017-06-13 长江大学 For the preparation method of the magnetic Nano water treatment agent of oilfield sewage
CN112138430A (en) * 2020-09-07 2020-12-29 同济大学 Magnetic nanorod demulsifier, preparation method thereof and method for treating nanoemulsion by using magnetic nanorod demulsifier

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