CN105778107A - Oil-soluble demulsifier and preparation method thereof - Google Patents

Oil-soluble demulsifier and preparation method thereof Download PDF

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Publication number
CN105778107A
CN105778107A CN201610146727.XA CN201610146727A CN105778107A CN 105778107 A CN105778107 A CN 105778107A CN 201610146727 A CN201610146727 A CN 201610146727A CN 105778107 A CN105778107 A CN 105778107A
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oil
long
soluble demulsifier
polyethers
preparation
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郭睿
杨江月
李欢乐
刘爱玉
程敏
甄建斌
王超
李晓芳
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/42—Block-or graft-polymers containing polysiloxane sequences
    • C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/38—Polysiloxanes modified by chemical after-treatment
    • 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 discloses an oil-soluble demulsifier and a preparation method thereof. The preparation method comprises the following steps: adding phenyl hydrogen-containing silicone oil and an organic solvent into a reaction kettle; heating to 70 to 75 DEG C with stirring; adding a suitable amount of catalyst at the temperature; then heating to 80 to 130 DEG C; dropwise adding a mixture of long-chain carbon olefins and polyether; after the mixture is dropwise added, reacting for 5 to 10 hours at the temperature; distilling under a reduced pressure to remove low-boiling-point substances and unreacted raw materials to obtain the novel oil-soluble demulsifier, wherein the molar ratio of the phenyl hydrogen-containing silicone oil to the mixture of polyether and long-chain alkyl is 1:(1-1.3); the molar ratio of polyether to long-chain carbon olefins is 1:(1-4). The novel oil-soluble demulsifier provided by the invention can prolong action time in demulsification application, and moreover, has the advantages of high-efficiency demulsifying effect, wide application range, small using amount and low toxicity.

Description

A kind of oil-soluble demulsifier and preparation method thereof
Technical field
The invention belongs to petrochemical industry, be applied to crude oil demulsification dehydration aspect, be specifically related to a kind of oil-soluble demulsifier and preparation method thereof.
Background technology
Oil extraction has been enter into tertiary phase, adds widely using of various oilfield additive, makes crude oil Produced Liquid composition more complicated, and crude oil emulsion is more stable, and breakdown of emulsion difficulty is increasing.Process according to conventional demulsifier, consumption and breakdown of emulsion temperature need to be improved, the increase of expense and the consumption of the energy certainly will be caused.Therefore, research and development needed badly by new and effective demulsifier.
Demulsifier on market is divided into water solublity and the big class of oil-soluble two, and mostly conventional demulsifier is the block polyether class demulsifier being monomer with oxirane and expoxy propane, and the type belongs to water-soluble demulsifier.Water-soluble demulsifier is the naturally occurring emulsifying agent by replacing oil-water interfaces, destroys emulsion interface film, causes the destruction of interfacial film, and then cause breakdown of emulsion.However as the complication of emulsion of crude oil the Nomenclature Composition and Structure of Complexes, water-soluble demulsifier can not well adapt to change, and breakdown of emulsion degree declines to some extent.And, from the viewpoint of environmental conservation, water-soluble demulsifier enters in water treatment system with the sewage discharged the most at last, and processing for follow-up water makes troubles, and affects environment.Therefore, from long term growth, oil-soluble demulsifier will be more and more popular to people.
Chinese patent CN101693846A discloses a kind of multiple combination oil soluble demulsifier, and it is fast that this oil-soluble demulsifier has dewatering speed, and water cut in purified is low and deviates from the feature that water oil content is low；Chinese patent CN104927896A discloses a kind of viscous crude field high efficient oil dissolubility demulsifier, and this demulsifier has the feature such as stronger surface activity, good hydrophilic and oleophilic performance.
But patent CN101693846A report is the demulsifier of a kind of Compositional type, when reaching similar demulsification, can cause the increase of cost of material.The oil-soluble demulsifier of this Recompounded multielement including 5～10% fluorine-containing surfactant, the use of fluorine-containing material can cause cost of material to be greatly improved, and causes environmental pollution.Although the demulsifier broad spectrum activity of this patent report is better, but it is low to there is dehydrating amount, the problem that dehydration rate is not high.The viscous crude field high efficient oil dissolubility demulsifier of patent CN104927896A report, in reactive mode, what adopt is that the mode being esterified is made, and the condition of esterification is wayward, belong to reversible reaction, generally reaction carries out not thorough, and this can cause the waste of raw material, also can make troubles to subsequent treatment.And be not suitable for large-scale production.It is big that the raw material Petroleum that this patent uses equally exists toxicity, the problem that human body and environment are worked the mischief.
Summary of the invention
For overcoming the problems of the prior art, it is an object of the invention to provide a kind of oil-soluble demulsifier and preparation method thereof, demulsifier prepared by the method has that de-emulsification speed is fast, dehydration rate is high, make consumption few and feature that toxicity is little, and synthesis technique and reaction principle are simple, the method adopts one kettle way, both save operating procedure, also improved reaction efficiency, reduce production cost.
For achieving the above object, the present invention is realized by following technical proposals:
A kind of oil-soluble demulsifier, the structural formula of this oil-soluble demulsifier is as follows:
Wherein, R1For-CH2CH2CH2O(C2H4O)m(C3H6O)nR3, R3For-H ,-CH3、-C2H5Or-C3H7；R2For-CaH2a+1, a is 10～20；x、y1、y2, z be integer, x, y1、y2, z be 10～200；M, n are integer, m=0～40, n=0～30, and are 0 during m, n difference.
A kind of preparation method of oil-soluble demulsifier, phenyl hydrogen-containing silicon oil and organic solvent are added in reactor, 70～75 DEG C it are warming up under stirring, add catalyst at this temperature, then heat to 80～130 DEG C, then drip the mixture of long-chain carbon olefin and polyethers, after dropwising, after reacting 5～10h at 80～130 DEG C of temperature, decompression distillation, obtain oil-soluble demulsifier；Wherein, the mol ratio of the mixture of phenyl hydrogen-containing silicon oil and long-chain carbon olefin and polyethers is 1:(1～1.3), the mol ratio of polyethers and long-chain carbon olefin is 1:(1～4), the ratio of the quality of catalyst and the mixture gross mass of phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers is 30～40 μ g:1g, and catalyst is the aqueous isopropanol of chloroplatinic acid.
In described phenyl hydrogen-containing silicon oil, hydrogeneous mass percent is 0.1～0.5%, is 20～40% containing benzene mass percent, and viscosity is 10～30mpa s, and index of refraction is 1.50.
Described polyethers is allyl alcohol polyether, and structural formula is
Wherein, R3For-H ,-CH3、-C2H5Or-C3H7；；M, n are integer, m=0～40；N=0～30, and be 0 during m, n difference.
Described long-chain carbon olefin is carbon number is 10 to the carbene that carbon atom is between 20.
Described long-chain carbon olefin purity is 99～99.9%.
Described organic solvent is toluene or isopropanol.
The quality of described organic solvent is the 30% of the gross mass of the mixture of phenyl hydrogen-containing silicon oil and long-chain carbon olefin and polyethers.
The mass concentration of the aqueous isopropanol of described chloroplatinic acid is 2%.
Described time for adding is 10～60min.
Compared with prior art, this technology has the advantages that
1., owing to naturally occurring emulsifying agents based on asphalitine, colloid many in crude oil exist, asphalitine material is made up of complicated aromatic condensed ring and side chain.Colloid also has similar chemical constitution.Therefore according to the similar principle mixed, demulsifier molecule has on crude oil and oil-water interfacial film and well dissolves diffusibility, it is made can quickly to arrive oil-water interfacial film and replace replacement part naturally occurring emulsifying agent, to reduce interfacial film strength and to cause that it breaks, it is achieved oil-water separation.The present invention directly uses phenyl hydrogen-containing silicon oil to be raw material, and the introducing of phenyl can not only improve demulsification, and phenyl hydrogen-containing silicon oil is than methyl-silicone oil or other modified containing hydrogen silicone oil, has better resistance to elevated temperatures, radiation resistance, greasy property and solubility property.
2. the present invention is by regulating the mol ratio of hydrophilic polyethers and oil loving long-chain carbon olefin, is prepared for a kind of novel oil-soluble demulsifier.The introducing of polyether group can not only make product have low surface tension, high-low temperature resistant, hydrophobic etc., there is again the special natures such as the lubrication of polyether segment offer, good spreadability and emulsion stability simultaneously, polyether modified siloxane is carried out modified surfactant again there is more excellent application effect.
3. new oil-soluble demulsifier provided by the invention, can extend action time when breakdown of emulsion is applied, and has efficient demulsification and applied widely and make consumption few and advantage that toxicity is little.Experiment proves: at breakdown of emulsion temperature 75 DEG C, breakdown of emulsion time 2.5h, during demulsifier consumption 200mg/L, demulsification efficiency may be up to more than 90%.
4. the demulsifier that prepared by the method has that de-emulsification speed is fast, dehydration rate is high, make consumption few and feature that toxicity is little, and synthesis technique and reaction principle are simple, the method adopts one kettle way, has both saved operating procedure, also improve reaction efficiency, reduce production cost.
Further, what the present invention adopted is the allyl alcohol polyether of methyl blocking, and the methyl of inertia substantially reduces the generation of side reaction.
Accompanying drawing explanation
Fig. 1 is the synthetic route chart of the present invention.
Fig. 2 is the infrared spectrogram of the product that the embodiment of the present invention 5 prepares.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further details, but is not limited to the practical range of the present invention.
A kind of oil-soluble demulsifier provided by the invention, its structural formula is as follows:
Wherein, R1For-CH2CH2CH2O(C2H4O)m(C3H6O)nR3, R3For-H ,-CH3、-C2H5Or-C3H7, R3For-C3H7Time, it is possible to for n-pro-pyl, isopropyl；R2For-CaH2a+1, a is 10～20, i.e. R2It is the alkyl of 10 to 20 for carbon number, the straight chain of side chain.x、y1、y2, z be integer, x, y1、y2, z range be 10～200；M, n are integer, m=0～40；N=0～30, and be 0 during m, n difference.
In the present invention, to be carbon number be long-chain carbon olefin 10 to the carbene that carbon atom is between 20, the straight chain of side chain；Long-chain carbon olefin purity is 99～99.9%.
Referring to Fig. 1, the preparation method of the oil-soluble demulsifier of said structure is: add in reactor by phenyl hydrogen-containing silicon oil and organic solvent, 70～75 DEG C it are warming up under stirring, add appropriate catalyst at this temperature, then heat to 80～130 DEG C, then drip the mixture of long-chain carbon olefin and polyethers, after dropwising, after reacting 5～10h at this temperature, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier.
X, y in Fig. 11、y2, z value be that the molecular weight of the viscosity according to phenyl hydrogen-containing silicon oil and material is determined.The value of m, n is determined according to polyethers ethylene oxide (EO) and expoxy propane (PO) segment ratio.
Further illustrate below by specific embodiment that the present invention will be described.
Phenyl hydrogen-containing silicon oil in embodiments of the invention 1-6 is colourless transparent liquid, and hydrogeneous mass percent is 0.5%, is 20% containing benzene mass percent, and viscosity is 28mpa s (25 DEG C), and index of refraction is 1.50.
Polyethers in embodiments of the invention 1-6 is 1-propenol-3 methyl blocking polyether AM15-10, below m=15, n=10, R in structural formula3For methyl.
In embodiments of the invention, catalyst is the aqueous isopropanol of the chloroplatinic acid that mass concentration is 2%, and the ratio of the quality of catalyst and phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers gross mass is 30～40 μ g:1g.
Embodiment 1
1.25g phenyl hydrogen-containing silicon oil and 1.19g isopropanol are added in reactor, is warming up to 70 DEG C under stirring, adds 1.19 × 10 at this temperature-4G catalyst, then heats to 80 DEG C, then drips 0.8416g1-laurylene and the mixture of 1.875g polyethers, time for adding is 10min, after dropwising, reacts 5h at 80 DEG C, then, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier.
Embodiment 2
1.25g phenyl hydrogen-containing silicon oil and 1.23g isopropanol are added in reactor, is warming up to 70 DEG C under stirring, adds 1.23 × 10 at this temperature-4G catalyst, then heats to 90 DEG C, then drips 0.8837g1-laurylene and the mixture of 1.969g polyethers, time for adding is 20min, after dropwising, reacts 6h at 90 DEG C, then, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier.
Embodiment 3
1.25g phenyl hydrogen-containing silicon oil and 1.27g isopropanol are added in reactor, is warming up to 70 DEG C under stirring, adds 1.27 × 10 at this temperature-4G catalyst, then heats to 100 DEG C, then drips 0.9258g1-laurylene and the mixture of 2.063g polyethers, time for adding is 30min, after dropwising, reacts 7h at 100 DEG C, then, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier.
Embodiment 4
1.25g phenyl hydrogen-containing silicon oil and 1.31g isopropanol are added in reactor, is warming up to 70 DEG C under stirring, adds 1.31 × 10 at this temperature-4G catalyst, then heats to 110 DEG C, then drips 0.9678g1-laurylene and the mixture of 2.156g polyethers, time for adding is 40min, after dropwising, reacts 8h at 110 DEG C, then, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier.
Embodiment 5
1.25g phenyl hydrogen-containing silicon oil and 1.32g isopropanol are added in reactor, is warming up to 70 DEG C under stirring, adds 1.35 × 10 at this temperature-4G catalyst, then heats to 120 DEG C, then drips 1.010g1-laurylene and the mixture of 2.25g polyethers, time for adding is 50min, after dropwising, reacts 9h at 120 DEG C, then, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier.
Represent the infrared spectrum of raw material referring to Fig. 2, a, b represents the infrared spectrum of product, 2156cm-1Place is the Si-H characteristic absorption peak of raw material (phenyl hydrogen-containing silicon oil), and product relevant position absworption peak disappears, and illustrates that Si-H has been participating in reaction；Product is at 1642cm-1There is faint C=C characteristic absorption peak in place, because polyethers and chain alkyl content are more in raw material；3513cm-1Place is-OH stretching vibration absworption peak；2922.33cm-1And 2858.06cm-1Specific strength is remarkably reinforced by the two peak and raw material, is 2965cm-1The c h bond absworption peak at place splits point generation: 2922.33cm-1It is CH2Antisymmetric stretching vibration peak, 2858.06cm-1It is CH2Symmetrical stretching vibration peak, the change splitting peak and peak intensity is owing to introducing caused by chain alkyl 1-laurylene on polysiloxane molecule chain, 2988cm-1Place is-CH3Stretching vibration absworption peak；2950cm-1～2870cm-1The C-H stretching vibration peak at place broadens, and is caused by a large amount of methylene contained in the polyethers being introduced on containing hydrogen silicone oil chain；1725 places be allyl alcohol polyether exist isomerization reaction produce C=O cause；1595cm-1,1457cm-1Place is the skeleton peak of phenyl ring；1373cm-1Place is C-H bending vibration peak in-CH2-；1260cm-1Place is Si-CH3In-CH3Bending vibration peak.This confirms that phenyl hydrogen-containing silicon oil there occurs graft reaction with chain alkyl and polyethers.
Embodiment 6
1.25g phenyl hydrogen-containing silicon oil and 1.39g isopropanol are added in reactor, is warming up to 70 DEG C under stirring, adds 1.39 × 10 at this temperature-4G catalyst, then heats to 130 DEG C, then drips 1.052g1-laurylene and the mixture of 2.343g polyethers, time for adding is 60min, after dropwising, reacts 10h at 130 DEG C, then, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier.
PFA8311, AE2010, PR4041 and the SP169 demulsifier sold on the crude oil demulsifier prepare above example 1-embodiment 6 and market carry out breakdown of emulsion experiment: crude oil comes from Chen Zhuan crude oil；Crude oil emulsion (W/O) configures by profit volume ratio 7:3；Breakdown of emulsion standard, according to oil and gas industry standard SY/T5821-2000；Evaluation index is with dehydrating amount, the neat situation in interface and deviates from the water quality of water and judges.
Trying method with bottle and above-mentioned demulsifier is evaluated experiment, concrete outcome is in Table 1,2,3.
The different demulsifier of table 1 tests (breakdown of emulsion temperature 75 DEG C, breakdown of emulsion time 2.5h) at the breaking emulsion and dewatering of different amounts
The different demulsifier of table 2 is at breaking emulsion and dewatering experiment (breakdown of emulsion temperature 75 DEG C, demulsifier consumption is 200mg/L) of different breakdown of emulsion times
The different demulsifier of table 3 is at breaking emulsion and dewatering experiment (breakdown of emulsion time 2.5h, demulsifier consumption is 200mg/L) of different breakdown of emulsion temperature
Be can be seen that by data in above table, the new oil-soluble demulsifier of the present invention is respectively provided with higher demulsification efficiency, demulsification is better than the demulsifier on market, especially the demulsifier of embodiment 5, breakdown of emulsion temperature 75 DEG C, breakdown of emulsion time 2.5h, during demulsifier consumption 200mg/L, demulsification efficiency may be up to more than 90%.This is because containing aromatic ring structure in the demulsifier molecule of this invention, according to the similar principle that mixes, it has on crude oil and oil-water interfacial film well dissolves diffusibility, it is made can quickly to arrive oil-water interfacial film and replace replacement part naturally occurring emulsifying agent, to reduce interfacial film strength and to cause that it breaks, it is achieved oil-water separation.Can drawing by comparing, the demulsifier of this invention has that de-emulsification speed is fast, dehydration rate is high, make consumption few and advantage that toxicity is little, is a kind of novel oil-soluble demulsifier.
Embodiment 7
Phenyl hydrogen-containing silicon oil and toluene are added in reactor, 75 DEG C it are warming up under stirring, add catalyst at this temperature, then heating to 130 DEG C, then drip the mixture of long-chain carbon olefin and polyethers, time for adding is 10min, after dropwising, after reacting 5h at 130 DEG C, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier；Wherein, the mol ratio of the mixture of phenyl hydrogen-containing silicon oil and long-chain carbon olefin and polyethers and polyethers is 1:1.3, the mol ratio of polyethers and long-chain carbon olefin is 1:3, the ratio of the quality of catalyst and phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers gross mass is 32 μ g:1g, and catalyst is mass concentration is the aqueous isopropanol of the chloroplatinic acid of 2%.
Wherein, in described phenyl hydrogen-containing silicon oil, hydrogeneous mass percent is 0.1%, is 30% containing benzene mass percent, and viscosity is 10mpa s, and index of refraction is 1.50.
Polyethers is allyl alcohol polyether, and structural formula is:
Wherein, R3For-H；M=0；N=10.
Described long-chain carbon olefin is purity be 99～99.9% 1-endecatylene.
The quality of described toluene is the 30% of the gross mass of the mixture of phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers.
Embodiment 8
Phenyl hydrogen-containing silicon oil and isopropanol are added in reactor, 72 DEG C it are warming up under stirring, add catalyst at this temperature, then heating to 110 DEG C, then drip the mixture of long-chain carbon olefin and polyethers, time for adding is 30min, after dropwising, after reacting 6h at 110 DEG C, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier；Wherein, the mol ratio of the mixture of phenyl hydrogen-containing silicon oil and long-chain carbon olefin and polyethers and polyethers is 1:1.2, the mol ratio of polyethers and long-chain carbon olefin is 1:2, the ratio of the quality of catalyst and phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers gross mass is 35 μ g:1g, and catalyst is mass concentration is the aqueous isopropanol of the chloroplatinic acid of 2%.
Wherein, in described phenyl hydrogen-containing silicon oil, hydrogeneous mass percent is 0.2%, is 40% containing benzene mass percent, and viscosity is 25mpa s, and index of refraction is 1.50.
Polyethers is allyl alcohol polyether, and structural formula is:
Wherein, R3For-CH3；M=10；N=20.
Described long-chain carbon olefin is purity is the tetradecene of 99～99.9%.
The quality of described isopropanol is the 30% of the gross mass of the mixture of phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers.
Embodiment 9
Phenyl hydrogen-containing silicon oil and isopropanol are added in reactor, 73 DEG C it are warming up under stirring, add catalyst at this temperature, then heating to 100 DEG C, then drip the mixture of long-chain carbon olefin and polyethers, time for adding is 40min, after dropwising, after reacting 8h at 100 DEG C, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier；Wherein, the mol ratio of the mixture of phenyl hydrogen-containing silicon oil and long-chain carbon olefin and polyethers and polyethers is 1:1.1, the mol ratio of polyethers and long-chain carbon olefin is 1:1, the ratio of the quality of catalyst and phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers gross mass is 30 μ g:1g, and catalyst is mass concentration is the aqueous isopropanol of the chloroplatinic acid of 2%.
Wherein, in described phenyl hydrogen-containing silicon oil, hydrogeneous mass percent is 0.3%, is 25% containing benzene mass percent, and viscosity is 22mpa s, and index of refraction is 1.50.
Polyethers is allyl alcohol polyether, and structural formula is:
Wherein, R3For n-pro-pyl；M=12；N=25.
Described long-chain carbon olefin is purity is the cetene of 99～99.9%.
The quality of described isopropanol is the 30% of the gross mass of the mixture of phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers.
Embodiment 10
Phenyl hydrogen-containing silicon oil and isopropanol are added in reactor, 70 DEG C it are warming up under stirring, add catalyst at this temperature, then heating to 80 DEG C, then drip the mixture of long-chain carbon olefin and polyethers, time for adding is 60min, after dropwising, after reacting 10h at 80 DEG C, decompression is distilled off low-boiling-point substance and unreacted raw material, obtains oil-soluble demulsifier；Wherein, the mol ratio of the mixture of phenyl hydrogen-containing silicon oil and long-chain carbon olefin and polyethers and polyethers is 1:1, the mol ratio of polyethers and long-chain carbon olefin is 1:4, the ratio of the quality of catalyst and phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers gross mass is 40 μ g:1g, and catalyst is mass concentration is the aqueous isopropanol of the chloroplatinic acid of 2%.
Wherein, in described phenyl hydrogen-containing silicon oil, hydrogeneous mass percent is 0.4%, is 350% containing benzene mass percent, and viscosity is 30mpa s, and index of refraction is 1.50.
Polyethers is allyl alcohol polyether, and structural formula is:
Wherein, R3For isopropyl；M=40；N=30.
Described long-chain carbon olefin is purity be 99～99.9% 1-eicosylene.
The quality of described isopropanol is the 30% of the gross mass of the mixture of phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers.
Above content is in conjunction with concrete preferred implementation further description made for the present invention; it cannot be assumed that the specific embodiment of the present invention is only limitted to this; for general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; some simple deduction or replace can also be made, all should be considered as belonging to the present invention and be determined scope of patent protection by submitted claims.

Claims (10)

1. an oil-soluble demulsifier, it is characterised in that the structural formula of this oil-soluble demulsifier is as follows:
Wherein, R1For-CH2CH2CH2O(C2H4O)m(C3H6O)nR3, R3For-H ,-CH3、-C2H5Or-C3H7；R2For-CaH2a+1, a is 10～20；x、y1、y2, z be integer, x, y1、y2, z be 10～200；M, n are integer, m=0～40, n=0～30, and are 0 during m, n difference.
2. the preparation method of an oil-soluble demulsifier, it is characterized in that, phenyl hydrogen-containing silicon oil and organic solvent are added in reactor, is warming up to 70～75 DEG C under stirring, adds catalyst at this temperature, then heat to 80～130 DEG C, drip the mixture of long-chain carbon olefin and polyethers again, after dropwising, after reacting 5～10h at 80～130 DEG C of temperature, decompression distillation, obtains oil-soluble demulsifier；Wherein, the mol ratio of the mixture of phenyl hydrogen-containing silicon oil and long-chain carbon olefin and polyethers is 1:(1～1.3), the mol ratio of polyethers and long-chain carbon olefin is 1:(1～4), the ratio of the quality of catalyst and the mixture gross mass of phenyl hydrogen-containing silicon oil, long-chain carbon olefin and polyethers is 30～40 μ g:1g, and catalyst is the aqueous isopropanol of chloroplatinic acid.
3. the preparation method of oil-soluble demulsifier according to claim 2, it is characterised in that in described phenyl hydrogen-containing silicon oil, hydrogeneous mass percent is 0.1～0.5%, is 20～40% containing benzene mass percent, and viscosity is 10～30mpa s, and index of refraction is 1.50.
4. the preparation method of oil-soluble demulsifier according to claim 2, it is characterised in that described polyethers is allyl alcohol polyether, structural formula is
Wherein, R3For-H ,-CH3、-C2H5Or-C3H7；；M, n are integer, m=0～40；N=0～30, and be 0 during m, n difference.
5. the preparation method of oil-soluble demulsifier according to claim 2, it is characterised in that described long-chain carbon olefin is carbon number is 10 to the carbene that carbon atom is between 20.
6. the preparation method of oil-soluble demulsifier according to claim 2, it is characterised in that described long-chain carbon olefin purity is 99～99.9%.
7. the preparation method of oil-soluble demulsifier according to claim 2, it is characterised in that described organic solvent is toluene or isopropanol.
8. the preparation method of the oil-soluble demulsifier according to claim 2 or 7, it is characterised in that the quality of described organic solvent is the 30% of the gross mass of the mixture of phenyl hydrogen-containing silicon oil and long-chain carbon olefin and polyethers.
9. the preparation method of oil-soluble demulsifier according to claim 2, it is characterised in that the mass concentration of the aqueous isopropanol of described chloroplatinic acid is 2%.
10. the preparation method of oil-soluble demulsifier according to claim 2, it is characterised in that described time for adding is 10～60min.
CN201610146727.XA 2016-03-15 2016-03-15 Oil-soluble demulsifier and preparation method thereof Pending CN105778107A (en)

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