CN107474873A - A kind of super-viscous oil demulsifier and preparation method thereof - Google Patents

A kind of super-viscous oil demulsifier and preparation method thereof Download PDF

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CN107474873A
CN107474873A CN201710755588.5A CN201710755588A CN107474873A CN 107474873 A CN107474873 A CN 107474873A CN 201710755588 A CN201710755588 A CN 201710755588A CN 107474873 A CN107474873 A CN 107474873A
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demulsifier
oil
minutes
dehydration
temperature
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CN107474873B (en
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胡新生
胡毓桓
王方
郑百清
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Panjin Fu Long Chemical Co Ltd
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Panjin Fu Long Chemical Co Ltd
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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
    • 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
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
    • C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
    • C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
    • C08G65/2612—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aromatic or arylaliphatic hydroxyl groups
    • 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
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
    • C08G65/2618—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
    • C08G65/2621—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups
    • C08G65/2624—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups containing aliphatic amine groups
    • 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
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/32—Polymers modified by chemical after-treatment
    • C08G65/321—Polymers modified by chemical after-treatment with inorganic compounds
    • C08G65/328—Polymers modified by chemical after-treatment with inorganic compounds containing other elements
    • 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
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/32—Polymers modified by chemical after-treatment
    • C08G65/329—Polymers modified by chemical after-treatment with organic compounds
    • C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
    • C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
    • C08G65/3324—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof cyclic

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Polyethers (AREA)

Abstract

The invention discloses a kind of super-viscous oil demulsifier, it is made up of the component of following weight percentage：Reverse hair oil DP types crude oil demulsifier 40~65%, mix oil head MU types crude oil demulsifier 10~40%, the positive Abietyl modified phenol amine type crude oil demulsifier 20~45% of oil head PFA types, feature anion biosurfactant rhamnolipid 1~5%, and preparation method.Three kinds of demulsifiers and biosurfactant are well mixed according to a certain percentage, are the demulsifier of the present invention.The features such as due to the demulsifier various structures of the present invention, mutual compatibility and concertedness are extremely strong, for Liaohe Oil Field dawn oil recovery factory super-viscous oil, have demulsification efficiency high, and stability is good, and water edible vegetable oil is net after demulsification, and oil-water interfaces are clearly smooth.

Description

A kind of super-viscous oil demulsifier and preparation method thereof
Technical field
The present invention relates to oilfield chemical preparation technique field, especially super-viscous oil demulsifier, and preparation method thereof.
Background technology
Crude oil (CRUDE OIL) is the main energy sources of the world today, and it occupies very important status in national economy, Therefore also referred to as " gold of black ".According to various criterion, classification of crude oil is also different, wherein there is a kind of high viscosity, highdensity thick Oil, the Chinese viscous crude criteria for classification proposed according to China Liu Wenzhang chief engineer, there is a kind of super-viscous oil (bitumen), its power Viscosity (50 DEG C) >=50000mPa.s, density (20 DEG C) ＞ 0.98g/cm3。
The researchs such as Strausz show, 4-10 condensed aromatic system are contained in asphaltene molecules, aromatic ring cochain is connected to abundant Fatty construction unit, forming the branched structure of asphalitine may crimp, coiling, form asphaltene molecules in oil reservoir body Three-D space structure in system, the serious barrier that diffuses to form for demulsifier, while using condensed ring as core in asphaltene molecule Between unit thin slice, because intramolecular or intermolecular aromatic ring pi-electron cloud are overlapping and be complexed, the quasi-crystalline structure of partial order is formed, Demulsification agent molecule aligning in oil-water interfaces is hindered, super-viscous oil belongs to and its stable colloidal dispersion system, its dispersed phase It is using asphalitine as core, and invests the particle that its colloid is formed for solvated layer, it is prevented between asphaltene molecule Further flocculation and coalescence, therefore can these factors turn into be directed to the key factor that is effectively demulsified of super-viscous oil.
Liaohe Oil Field dawn oil recovery factory is domestic most notable super-viscous oil producing region, and the crude oil denseness world is rare, and its power glues Degree (50 DEG C) is up to 59989mPa.s, and density (20 DEG C) is up to 1.0572g/cm3.The demulsification of super-viscous oil annoyings each oil recovery always Factory, therefore specialize in and develop both at home and abroad for super-viscous oil demulsifier, achieve certain achievement.Patent CN 102373077A discloses a kind of special thick oil feature demulsifier, effectively increases the dehydrating effect of special thick oil, is only applicable to glue Spend the water-oil separating in 10000mPa.s viscous crude containing Saudi Arabia；Patent CN 102746470A disclose cycloalkyl special thick oil demulsifier, Suitable for the demulsification of Karamy area cycloalkyl special thick oil,《Finely and specialty chemicals》12 phases in 2005 disclose a kind of clear Water type is special, and (super) is thick demulsifier, has preferable demulsification to Liaohe River Leng Jia and the oily company of special type oil product, but to dawn The super-viscous oil demulsification of oil recovery factory is unsatisfactory.
The content of the invention
The present invention in view of the shortcomings of the prior art, proposes a kind of super-viscous oil demulsifier, can be directed to Liaohe Oil Field dawn and recover the oil The super-viscous oil of factory is effectively demulsified, and the demulsifier has demulsification efficiency high, and stability is good, and water edible vegetable oil is net after demulsification, and oil-water interfaces are clear The features such as clear smooth, it is also proposed that the preparation method of the thick oil demulsifier.In order to realize foregoing invention purpose, the present invention provide with Lower technical scheme：
A kind of super-viscous oil demulsifier, is made up of the component of following weight percentage：Reverse hair oil DP types crude oil demulsifier 40 ~65%, mixing oil head MU types crude oil demulsifier 10~40%, the positive Abietyl modified phenol amine type crude oil demulsifier 20 of oil head PFA types ~45%, rhamnolipid 1~5%
Wherein reverse oil head DP type crude oil demulsifiers have following structure：
EO is in structure above --- CH2-CH2O ---, PO isM is 1~5 integer, N is 1~8 integer, and p is 1~7 integer, and k is 1~3 integer, and z is 1~3 integer.
Wherein mixing oil head MU type crude oil demulsifiers have following structure：
EO is in structure above --- CH2-CH2O ---, PO is；MO is that PO and EO is random Poly- unit is mixed, m is 1~10 integer, and n is 1~8 integer, and p is 1~9 integer.Wherein PFA types crude oil demulsifier has such as Lower structure：
EO is in structure above --- CH2-CH2O ---, PO is；M is 1~11 integer, N is 1~6 integer.
Rhamnolipid it is complicated various, mainly characterized with following four kinds of structures：
A kind of preparation method of super-viscous oil demulsifier as described above, it is preferred that comprise the following steps：
1. the preparation of reverse oil head DP type crude oil demulsifiers：
1.1 accurately weigh 1 part of bisphenol fluorene and the base catalyst of total number 0.1~0.3% and move into reactor, heating Stirring, 30~45 minutes are incubated when temperature reaches 225~230 DEG C, and it is de- to be then turned on vacuum (vacuum pressure≤- 0.09MPa) Water, temperature control are 225~230 DEG C, and dewatering time is 35~40 minutes, and 13~25 parts of epoxy is continuously passed through after dehydration Ethane, reaction temperature are 225~230 DEG C, and reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to protect Reaction temperature is held, is cured 30~45 minutes when pressure drops to below 0.02MPa, 90~100 DEG C of dischargings is cooled to, is demulsified Agent intermediate DPA.
Preferably, base catalyst includes potassium hydroxide, sodium hydroxide, calcium hydroxide, potassium alcoholate, sodium alkoxide etc., as preferred Item is applied to be used as catalyst for polymerization below.
Preferably, portion rate in formula：Bisphenol fluorene: oxirane=1: 15~21
1.2 accurately weigh 1 part of DPA and the base catalyst of total number 0.1~0.25% and move into reactor, and heating is stirred Mix, vacuum (vacuum pressure≤- 0.09MPa) dehydration is opened when temperature reaches 100~120 DEG C, dewatering time is 35~40 points Clock, dehydration finishing temperature is 120~130 DEG C, and 6~10 parts of expoxy propane, reaction temperature 130 are continuously passed through after dehydration ~135 DEG C, reaction pressure is 0.15MPa~0.4MPa, after expoxy propane has led to, continues to keep reaction temperature, works as pressure Then 0.1~0.7 part of oxirane is passed through when dropping to below 0.02MPa, reaction temperature is 120~130 DEG C, and reaction pressure is 0.15MPa~0.4MPa, after oxirane has led to, continue to keep reaction temperature, it is ripe when pressure drops to below 0.02MPa Change 30~45 minutes, with acetic acid and 90~100 DEG C of dischargings are cooled to behind material to PH=6~7, obtain demulsifier intermediate DPB。
Preferably, the portion rate in formula：DPA: expoxy propane: oxirane=1: 7~9: 0.5~0.6
1.3 accurately weigh 1 part of demulsifier intermediate DPB and move into reactor, heating stirring, treat temperature reach 90~ Start to be added dropwise the POCl3 of total number 3~6% at 115 DEG C, and open vacuum (vacuum pressure is maintained at -0.03~- 0.02MPa), 120~130 DEG C are warming up to after being added dropwise and is incubated 30~40 minutes, material pH value is then measured by sampling, works as PH 90~100 DEG C of dischargings are cooled to during value >=4, continue 120~130 DEG C of insulation when pH value≤4, are cooled to when pH value >=4 90~100 DEG C of dischargings.
Preferably, chain extender is POCl3, double dichloromethyl dimethylamino silanes, dichloroacetic acid, antiphen, phenyl dichloro oxygen Phosphorus, dichloro oxygen phosphorus, 1,3- bis- chloro- 2- propane diols etc..
Preferably, the dosage of POCl3 is the 3.5~5%. of total number
Preferably, the method for terminal sampling and measuring material pH value is：Sampling configuration 5% (mass fraction isopropanol: water= 3: 1) solution, determined from ranging for 2.7-4.7 precision test papers.
2. the preparation of mixing head MU type crude oil demulsifiers：
2.1 accurately weigh 1 part of N methyldiethanol amine and the base catalyst of total number 0.1~0.3% and move into anti- Kettle is answered, heating stirring, vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature control are opened when temperature reaches 100~110 DEG C For 100~110 DEG C, dewatering time is 35~40 minutes, and 15~25 parts of expoxy propane and epoxy are continuously passed through after dehydration The mixture (mass ratio PO: EO=2: 1) of ethane, reaction temperature be 120~130 DEG C, reaction pressure be 0.15MPa~ 0.4MPa；After expoxy propane has led to, continue to keep reaction temperature, 30~45 are cured when pressure drops to below 0.02MPa Minute, 90~100 DEG C of dischargings are cooled to, obtain demulsifier intermediate MUA.
Preferably, portion rate in formula：N methyldiethanol amine: expoxy propane and ethylene oxide mixture (mass ratio PO: EO=2: 1)=1: 20~23.
2.2 accurately weigh 1 part of intermediate MUA and the base catalyst of total number 0.1~0.2% and move into reactor, Heating stirring, vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature control 100 are opened when temperature reaches 100~110 DEG C ~110 DEG C, dewatering time is 35~40 minutes, and 5~8 parts of oxirane, reaction temperature 125 are continuously passed through after dehydration ~140 DEG C, reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to keep reaction temperature, work as pressure The expoxy propane that below 0.02MPa is then passed through 8~12 parts is dropped to, reaction temperature is 120~130 DEG C, and reaction pressure is 0.15MPa~0.4MPa, after expoxy propane has led to, continue to keep reaction temperature, it is ripe when pressure drops to below 0.02MPa Change 30~45 minutes, with acetic acid and 90~100 DEG C of dischargings are cooled to behind material to PH=6~7, obtain demulsifier MU.
Preferably, portion rate in formula：Intermediate MUA: oxirane: expoxy propane=1: 5.5~7: 9~10
It is prepared by 3.PFA type rosin esterifications crude oil demulsifier：
The preparation of 3.1PFA type resins：The accurate phenol, 6~8 parts of pentaethylene hexamines, 10~15 parts of dimethylbenzene for weighing 1 part And move into kettle, heating stirring and insulation 45~55 DEG C 30~45 minutes, the industrial first that content is 35~37% is then added dropwise 3~8 parts of aldehyde, 45~55 DEG C of material in kettle is kept being added dropwise during formaldehyde, after being added dropwise, be incubated 30~45 minutes, then Start slowly heating material and, until there is backflow to produce, stop heating when when temperature is at 140~145 DEG C more than constant half an hour, 90~100 DEG C of dischargings are cooled to, obtain PFA type resins.
Preferably, portion rate in formula：Phenol: pentaethylene hexamine: formaldehyde (35~37%): dimethylbenzene=1:: 6.5~ 7.5: 4.5~6: 12~14.
Preferably, phenols is phenol in formula, nonyl phenol, octyl phenol, p-t-butyl phenol, naphthols, bisphenol S, Bisphenol F Deng.
Preferably, amine is ethylenediamine, diethanol amine, triethanolamine, isopropanolamine, phenylenediamine, diethylenetriamine, three second Alkene tetramine, TEPA, pentaethylene hexamine, polyethylene polyamine etc..
Preferably, aldehydes is formaldehyde, acetaldehyde, paraformaldehyde.
It is prepared by 3.2PFA types demulsifier：
The accurate PFA types resin weighed in 3~7 part 3.2 and the base catalyst of total number 0.1~0.3% simultaneously move into anti- Kettle is answered, heating stirring, vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature control are opened when temperature reaches 100~110 DEG C For 100~110 DEG C, dewatering time is 35~40 minutes, is continuously passed through after dehydration：0.5~3 part of oxirane, reaction Temperature is 120~130 DEG C, and reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to keep reaction temperature Degree, cures 30~45 minutes when pressure drops to below 0.02MPa, cools to 90~100 DEG C of dischargings, obtain PFA type demulsifiers.
Preferably, portion rate in formula：PFA type portions of resin oxirane=4.5~5.5: 0.8~1.5
3.3PFA types demulsifier is esterified
Accurate 8~11 parts of PFA types demulsifier, 3~5 parts of hydrogenated rosins and the total number 0.1~0.3% weighed in 3.2 The concentrated sulfuric acid (concentration 98%) and move into kettle, stirring is warming up to 220~230 DEG C, opens vacuum (vacuum pressure -0.03- 0.05MPa) it is dehydrated, viscosimetric is sampled after 5~8 hours, as viscosity ＜ 35000mPa.s, continues vacuum dehydration, until sampling 90~100 DEG C of dischargings are cooled to when determining viscosity >=35000mPa.s, obtain PFA type rosin esterification crude oil demulsifiers.
Preferably, it is formulated mid-score ratio：PFA type demulsifiers: hydrogenated rosin=9.5~10: 3.5~4
Preferably, hydrogenated rosin is primes.
Preferably, viscosity >=42000mPa.s, viscosimetric analysis standard is according to GB/T 12008.8-1992.
4. sandlwood Tang ester (RHAMNOLIPID) derives from commodity.
Preferably, purity is 75~80%, PH=7-8, HLB=20~25 compared with prior art, the present invention have with Lower advantage：
1. there is the construction unit similar to gum asphalt molecule on two kinds of component agent structures and side chain in demulsifier, profit In the dispersal behavior of demulsification agent molecule；
2. a kind of component does beginning agent and another component by reverse oil head and does beginning agent to mix oil head in demulsifier, solution Determined demulsification agent molecule in oil-water interfaces because one end hydrophily deficiency causes it to be demulsified when oil-water interfaces align The defects of oil-water interfaces are uneven caused by agent molecule is curled and escaped.
3. a kind of component structure is multiple-branching construction in demulsifier, coalescence and flocculation beneficial to aqueous phase.
4. a kind of component is to be lived with amphipathic and specified chemical structural functionality anion biological surface in demulsifier Property agent, the positive charge of water droplet can be neutralized, cut down electrostatic repulsion, destroy the interfacial film by same sex electric protection, infiltration wetability protrudes, There is fabulous concertedness with demulsifier.
5. therefore, the demulsifier has demulsification efficiency high, stability is good, and water edible vegetable oil is net after demulsification, the clear light of oil-water interfaces The features such as sliding.
Embodiment
With reference to embodiment, the present invention will be described in detail, the description of this part be only it is exemplary and explanatory, no Reply protection scope of the present invention has any restriction effect.
Embodiment 1
Demulsifier DMPRA preparation comprises the following steps
1. the preparation of reverse oil head's DP type crude oil demulsifiers：
1.1 accurately weigh 1 part of bisphenol fluorene and the potassium hydroxide of total number 0.25% and move into reactor, heating stirring, 30~45 minutes are incubated when temperature reaches 225~230 DEG C, is then turned on vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature Degree control is 225~230 DEG C, and dewatering time is 35~40 minutes, and 16 parts of oxirane, reaction are continuously passed through after dehydration Temperature is 225~230 DEG C, and reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to keep reaction temperature Degree, cures 30~45 minutes when pressure drops to below 0.02MPa, cools to 90~100 DEG C of dischargings, obtain demulsifier intermediate DP01。
1.2 accurately weigh 1 part of DP-1 and the potassium hydroxide of total number 0.2% and move into reactor, heating stirring, treat temperature Degree opens vacuum (vacuum pressure≤- 0.09MPa) dehydration when reaching 100~120 DEG C, dewatering time is 35~40 minutes, dehydration Finishing temperature is 120~130 DEG C, and 8.5 parts of expoxy propane is continuously passed through after dehydration, and reaction temperature is 130~135 DEG C, Reaction pressure is 0.15MPa~0.4MPa, after expoxy propane has led to, continues to keep reaction temperature, when pressure drops to Then 0.55 part of oxirane is passed through during below 0.02MPa, reaction temperature is 120~130 DEG C, reaction pressure 0.15MPa ~0.4MPa, after oxirane has led to, continue keep reaction temperature, when pressure drops to below 0.02MPa cure 30~ 45 minutes, with acetic acid and 90~100 DEG C of dischargings are cooled to behind material to PH=6~7, obtain demulsifier intermediate DP02.
1.3 accurately weigh 1 part of demulsifier intermediate DPB and move into reactor, heating stirring, treat temperature reach 90~ Start to be added dropwise the POCl3 of total number 4.5% at 115 DEG C, and open vacuum (vacuum pressure is maintained at -0.03~- 0.02MPa), 120~130 DEG C are warming up to after being added dropwise and is incubated 30~40 minutes, material pH value is then measured by sampling, works as PH 90~100 DEG C of dischargings are cooled to during value >=4, continue 120~130 DEG C of insulation when pH value≤4, are cooled to when pH value >=4 90~100 DEG C of dischargings obtain demulsifier DPA.
2. the preparation of mixing head MU type crude oil demulsifiers：
2.1 accurately weigh 1 part of N methyldiethanol amine and the potassium hydroxide of total number 0.25% and move into reactor, rise Temperature stirring, when temperature reaches 100~110 DEG C open vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature control be 100~ 110 DEG C, dewatering time is 35~40 minutes, and 22 parts of expoxy propane and the mixture of oxirane are continuously passed through after dehydration (mass ratio PO: EO=2: 1), reaction temperature are 120~130 DEG C, and reaction pressure is 0.15MPa~0.4MPa；Work as expoxy propane After having led to, continue to keep reaction temperature, cured 30~45 minutes when pressure drops to below 0.02MPa, cool to 90~100 DEG C discharging, obtain demulsifier intermediate MU01.
2.2 accurately weigh 1 part of intermediate MUA01 and the potassium hydroxide of total number 0.1~0.2% and move into reactor, Heating stirring, vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature control 100 are opened when temperature reaches 100~110 DEG C ~110 DEG C, dewatering time is 35~40 minutes, and 6.5 parts of oxirane, reaction temperature 125 are continuously passed through after dehydration ~140 DEG C, reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to keep reaction temperature, work as pressure Drop to the expoxy propane that below 0.02MPa is then passed through 9 parts, reaction temperature is 120~130 DEG C, reaction pressure be 0.15MPa~ 0.4MPa, after expoxy propane has led to, continue to keep reaction temperature, 30~45 are cured when pressure drops to below 0.02MPa Minute, with acetic acid and 90~100 DEG C of dischargings are cooled to behind material to PH=6~7, obtain demulsifier MUA.
It is prepared by 3.PFA type rosin esterifications crude oil demulsifier：
The preparation of 3.1PFA type resins：
The accurate phenol for weighing 1 part, 6.8 parts of pentaethylene hexamines, 12.3 parts of diformazan benzos are moved into kettle, and heating is stirred and protected It is incubated 45~55 DEG C 30~45 minutes, 5 parts of the industrial formol that content is 35~37% is then added dropwise, is protected during formaldehyde is added dropwise 45~55 DEG C of material in kettle are held, after being added dropwise, are incubated 30~45 minutes, the material that then starts slowly to heat up is until there is backflow to produce It is raw, stop heating when when temperature is at 140~145 DEG C more than constant half an hour, be cooled to 90~100 DEG C of dischargings, obtain PFA types Resin.
It is prepared by 3.2PFA types demulsifier：
Accurate 6 parts of the PFA types resin weighed in 3.1 and the base catalyst of total number 0.3% simultaneously move into reactor, rise Temperature stirring, when temperature reaches 100~110 DEG C open vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature control be 100~ 110 DEG C, dewatering time is 35~40 minutes, is continuously passed through 1.2 parts of oxirane after dehydration, reaction temperature is 120~ 130 DEG C, reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to keep reaction temperature, work as pressure drop Cured 30~45 minutes to during below 0.02MPa, cool to 90~100 DEG C of dischargings, obtain demulsifier PFA01.
3.3 demulsifier PFA01 are esterified
The accurate 9.7 parts of demulsifier PFA01 claimed in 3.2,3.7 parts of hydrogenated rosins and total number 0.3% concentrated sulfuric acid and shifting Enter in kettle, stirring is warming up to 220~230 DEG C, opens vacuum (vacuum pressure -0.03-0.05MPa) dehydration, is taken after 5~8 hours Sample viscosimetric, 90~100 DEG C of dischargings are cooled to as viscosity >=35000mPa.s, obtain rosin esterification crude oil demulsifier PFA23.
It is 4. component (DPA: MUA: PFA23: RHAMNOLIPID=52%: 16%: 30%: 2%) by weight percentage is normal The lower well mixed demulsifier DMPRA for producing the present invention of temperature
Demulsifier DMPRA physical and chemical index difference is as follows：
1st, outward appearance：Rufous clear viscous liquids
2nd, solid content：97.1%
3rd, density (20 DEG C)：0.91g/cm3
4th, pH value：7.5
5th, flash-point (cup of remaining silent)：40 DEG C of ＞
6th, freezing point：＜ -35 DEG C
7th, viscosity：(50℃)：42150mPa.s
Above index meets China National Petroleum professional standard SY/T5280-2000 crude oil demulsifier general technology bars The requirement of part water-soluble demulsifier operating specification.
Embodiment 2
Demulsifier DMPRB preparation comprises the following steps
1. the preparation of reverse oil head DP type crude oil demulsifiers：
1.1 accurately weigh 1 part of bisphenol fluorene and the potassium hydroxide of total number 0.2% and move into reactor, heating stirring, treat Temperature is incubated 30~45 minutes when reaching 225~230 DEG C, is then turned on vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature Control as 225~230 DEG C, dewatering time is 35~40 minutes, and 18 parts of oxirane, reaction temperature are continuously passed through after dehydration Spend for 225~230 DEG C, reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to keep reaction temperature, Cured 30~45 minutes when pressure drops to below 0.02MPa, cool to 90~100 DEG C of dischargings, obtain demulsifier intermediate DP03。
1.2 accurately weigh 1 part of DP03 and the potassium hydroxide of total number 0.25% and move into reactor, heating stirring, treat Temperature opens vacuum (vacuum pressure≤- 0.09MPa) dehydration when reaching 100~120 DEG C, dewatering time is 35~40 minutes, is taken off Water finishing temperature is 120~130 DEG C, and 10 parts of expoxy propane is continuously passed through after dehydration, and reaction temperature is 130~135 DEG C, Reaction pressure is 0.15MPa~0.4MPa, after expoxy propane has led to, continues to keep reaction temperature, when pressure drops to Then be passed through 0.7 part of oxirane during below 0.02MPa, reaction temperature is 120~130 DEG C, reaction pressure be 0.15MPa~ 0.4MPa, after oxirane has led to, continue to keep reaction temperature, 30~45 are cured when pressure drops to below 0.02MPa Minute, with oxalic acid and 90~100 DEG C of dischargings are cooled to behind material to PH=6~7, obtain demulsifier intermediate DP04.
1.3 accurately weigh 1 part of demulsifier intermediate DP04 and the sodium hydroxide of total number 7% and move into reactor, rise Temperature stirring, start that the chloro- 2- propane diols of 1,3- bis- of total number 6% is added dropwise when temperature reaches 90~115 DEG C, risen after being added dropwise Temperature is to 120~130 DEG C and is incubated 30~40 minutes, and material pH value is then measured by sampling and is neutralized with citric acid to 6~7 and is broken Emulsion DPB.
2. the preparation of reverse MU type crude oil demulsifier：
2.1 accurately weigh 1 part of N methyldiethanol amine and the potassium hydroxide of total number 0.25% and move into reactor, rise Temperature stirring, when temperature reaches 100~110 DEG C open vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature control be 100~ 110 DEG C, dewatering time is 35~40 minutes, and 25 parts of expoxy propane and the mixture of oxirane are continuously passed through after dehydration (mass ratio PO: EO=2: 1), reaction temperature are 120~130 DEG C, and reaction pressure is 0.15MPa~0.4MPa；Work as expoxy propane After having led to, continue to keep reaction temperature, cured 30~45 minutes when pressure drops to below 0.02MPa, cool to 90~100 DEG C discharging, obtain demulsifier intermediate MU02.
2.2 accurately weigh 1 part of intermediate MU01 and the potassium hydroxide of total number 0.2% and move into reactor, and heating is stirred Mix, vacuum (vacuum pressure≤- 0.09MPa) dehydration is opened when temperature reaches 100~110 DEG C, temperature control is 100~110 DEG C, dewatering time is 35~40 minutes, and 7.2 parts of oxirane is continuously passed through after dehydration, and reaction temperature is 125~140 DEG C, reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to keep reaction temperature, when pressure drops to Below 0.02MPa is then passed through 10.3 parts of expoxy propane, and reaction temperature is 120~130 DEG C, reaction pressure be 0.15MPa~ 0.4MPa, after expoxy propane has led to, continue to keep reaction temperature, 30~45 are cured when pressure drops to below 0.02MPa Minute, with acetic acid and 90~100 DEG C of dischargings are cooled to behind material to PH=6~7, obtain demulsifier MUB.
It is prepared by 3.PFA type rosin esterifications crude oil demulsifier：
The preparation of 3.1PFA type resins：
The accurate phenol for weighing 1 part, 6.8 parts of pentaethylene hexamines, 12.3 parts of diformazan benzos are moved into kettle, and heating is stirred and protected It is incubated 45~55 DEG C 30~45 minutes, 5 parts of the industrial formol that content is 35~37% is then added dropwise, is protected during formaldehyde is added dropwise 45~55 DEG C of material in kettle are held, after being added dropwise, are incubated 30~45 minutes, the material that then starts slowly to heat up is until there is backflow to produce It is raw, stop heating when when temperature is at 140~145 DEG C more than constant half an hour, be cooled to 90~100 DEG C of dischargings, obtain PFA types Resin.
It is prepared by 3.2PFA types demulsifier：
Accurately weigh 6 parts in 3.1 of PFA types resin and the base catalyst of total number 0.3% and move into reactor, heat up Stirring, when temperature reaches 100~110 DEG C open vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature control be 100~ 110 DEG C, dewatering time is 35~40 minutes, is continuously passed through 1.2 parts of oxirane after dehydration, reaction temperature is 120~ 130 DEG C, reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to keep reaction temperature, work as pressure drop Cured 30~45 minutes to during below 0.02MPa, cool to 90~100 DEG C of dischargings, obtain demulsifier PFA02.
3.3PFA types demulsifier is esterified
Accurately weigh the concentrated sulfuric acid of 10.2 parts of demulsifier PFA02,4.5 parts of hydrogenated rosins and total number 0.25% in 3.2 simultaneously Move into kettle, stirring is warming up to 220~230 DEG C, vacuum (vacuum pressure -0.03-0.05MPa) dehydration is opened, after 5~8 hours Viscosimetric is sampled, 90~100 DEG C of dischargings are cooled to as viscosity >=35000mPa.s, obtain rosin esterification crude oil demulsifier PFA25。
It is 4. component (DPB: MUB: PFA25: RHAMNOLIPID=48%: 21%: 28%: 3%) by weight percentage is normal The lower well mixed demulsifier DMPRB for producing the present invention of temperature.
Demulsifier DMPRB physical and chemical index difference is as follows：
1st, outward appearance：Rufous clear viscous liquids
2nd, solid content：96.9%
3rd, density (20 DEG C)：0.90g/cm3
4th, pH value：7.5
5th, flash-point (cup of remaining silent)：40 DEG C of ＞
6th, freezing point：＜ -35 DEG C
7th, viscosity：(50℃)：43057mPa.s
Above index meets China National Petroleum professional standard SY/T5280-2000 crude oil demulsifier general technology bars The requirement of part water-soluble demulsifier operating specification.
For the contrast of Liaohe Oil Field dawn oil recovery factory super-viscous oil demulsification as shown in Table 1 and Table 2.During evaluation criterion uses State's oil and gas industry standard SY/T5281-2000 crude oil demulsifier performances detection method (bottle examination method).
The different model Demulsifying effect of demulsifier of table 1 contrasts
The different model Demulsifying effect of demulsifier of table 2 contrasts
Demulsifier of the present invention is can be seen that from the data of Tables 1 and 2 and is directed to Liaohe Oil Field dawn oil recovery factory super-viscous oil, is had Have that dewatering speed is fast, the strong advantage of demulsification ability.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (3)

  1. A kind of 1. super-viscous oil demulsifier, it is characterised in that：It is made up of the component of following weight percentage：Reverse hair oil DP type crude oil Demulsifier 40~65%, mixing oil head MU types crude oil demulsifier 10~40%, the positive Abietyl modified phenol amine type crude oil of oil head PFA types Demulsifier 20~45%, rhamnolipid 1~5%.Wherein reverse oil head DP type crude oil demulsifiers have following structure：
    EO is in structure above --- CH2-CH2O ---, PO isM be 1~5 integer, n 1 ~8 integer, p are 1~7 integer, and k is 1~3 integer, and z is 1~3 integer.
    Wherein mixing oil head MU type crude oil demulsifiers have following structure：
    EO is in structure above --- CH2-CH2O ---, PO isMO is PO and EO randomly mixed poly- Unit, m are 1~10 integer, and n is 1~8 integer, and p is 1~9 integer.
    Positive oil head PFA type crude oil demulsifiers have following structure：
    EO is in structure above --- CH2-CH2O ---, PO isM be 1~11 integer, n 1 ~6 integer.
    Rhamnolipid it is complicated various, mainly characterized with following four kinds of structures：
  2. A kind of 2. preparation method of super-viscous oil demulsifier as claimed in claim 1, it is characterised in that：Reverse DP type crude oil demulsifiers Initiator bis-phenol used is fluorene structured similar to bituminous texture, synthesizes reverse oil head with oxirane ethoxylation using elder generation, and adopt Chain extension is carried out with crosslinking agent.Mixing oil head MU type crude oil demulsifiers use N methyldiethanol amine as initiator, first and epoxy second The mixture alkoxylate of alkane and expoxy propane synthesis mixing oil head, positive PFA types demulsifier using phenol-amine resin as initiator, then With modified by hydrogenated rosin, also there is the structure similar to asphaltene molecule in molecular structure, sandlwood Tang ester is as caused by pseudomonad A kind of biosurfactant of biological metabolism property, belongs to a kind of sugared lipid surfactant, is by a variety of structures of the same clan The mixture of composition, it possesses the essential characteristic of general surfactant, and its hydrophilic radical is typically by the rhamnose of 1~2 molecule Ring is formed, and hydrophobic group then by 1~2 molecule there is the saturation of different carbon chain lengths or unrighted acid to form.
  3. A kind of 3. preparation method of super-viscous oil demulsifier as claimed in claim 1, it is characterised in that：Comprise the following steps (following Described " part " refers both to quality)：
    3.1. the preparation of reverse oil head DP type crude oil demulsifiers：
    3.1.1 1 part of bisphenol fluorene and the base catalyst of total number 0.1~0.3% are accurately weighed and moves into reactor, heating is stirred Mix, 30~45 minutes be incubated when temperature reaches 225~230 DEG C, be then turned on vacuum (vacuum pressure≤- 0.09MPa) dehydration, Temperature control is 225~230 DEG C, and dewatering time is 35~40 minutes, and 13~25 parts of epoxy second is continuously passed through after dehydration Alkane, reaction temperature are 225~230 DEG C, and reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to keep Reaction temperature, cured 30~45 minutes when pressure drops to below 0.02MPa, cool to 90~100 DEG C of dischargings, obtain demulsifier Intermediate DPA.
    3.1.2 1 part of DPA and the base catalyst of total number 0.1~0.25% are accurately weighed and moves into reactor, heating is stirred Mix, vacuum (vacuum pressure≤- 0.09MPa) dehydration is opened when temperature reaches 100~120 DEG C, dewatering time is 35~40 points Clock, dehydration finishing temperature is 120~130 DEG C, and 6~10 parts of expoxy propane, reaction temperature 130 are continuously passed through after dehydration ~135 DEG C, reaction pressure is 0.15MPa~0.4MPa, after expoxy propane has led to, continues to keep reaction temperature, works as pressure Then 0.1~0.7 part of oxirane is passed through when dropping to below 0.02MPa, reaction temperature is 120~130 DEG C, and reaction pressure is 0.15MPa~0.4MPa, after oxirane has led to, continue to keep reaction temperature, it is ripe when pressure drops to below 0.02MPa Change 30~45 minutes, with acetic acid and 90~100 DEG C of dischargings are cooled to behind material to PH=6~7, obtain demulsifier intermediate DPB。
    3.1.3 accurately weigh 1 part of demulsifier intermediate DPB and move into reactor, heating stirring, treat that temperature reaches 90~115 DEG C when start that the POCl3 of total number 3~6% is added dropwise, and open vacuum (vacuum pressure is maintained at -0.03~-0.02MPa), 120~130 DEG C are warming up to after being added dropwise and is incubated 30~40 minutes, material pH value is then measured by sampling, is dropped when pH value >=4 Temperature continues 120~130 DEG C of insulation to 90~100 DEG C of dischargings when pH value≤4, and 90~100 DEG C are cooled to when pH value >=4 Discharging.
    The preparation of 3.2 mixing oil head MU type crude oil demulsifiers：
    3.2.1 1 part of N methyldiethanol amine and the base catalyst of total number 0.1~0.3% are accurately weighed and moves into reaction Vacuum (vacuum pressure≤- 0.09MPa) dehydration is opened in kettle, heating stirring when temperature reaches 100~110 DEG C, and temperature control is 100~110 DEG C, dewatering time is 35~40 minutes, and 15~25 parts of expoxy propane and epoxy second are continuously passed through after dehydration The mixture (mass ratio PO: EO=2: 1) of alkane, reaction temperature are 120~130 DEG C, and reaction pressure is 0.15MPa~0.4MPa； After the mixture of expoxy propane and oxirane has led to, continue to keep reaction temperature, it is ripe when pressure drops to below 0.02MPa Change 30~45 minutes, cool to 90~100 DEG C of dischargings, obtain demulsifier intermediate MUA.
    3.2.2 1 part of intermediate MUA and the base catalyst of total number 0.1~0.2% are accurately weighed and moves into reactor, is risen Temperature stirring, when temperature reaches 100~110 DEG C open vacuum (vacuum pressure≤- 0.09MPa) dehydration, temperature control be 100~ 110 DEG C, dewatering time is 35~40 minutes, is continuously passed through 5~8 parts of oxirane after dehydration, reaction temperature is 125~ 140 DEG C, reaction pressure is 0.15MPa~0.4MPa；After oxirane has led to, continue to keep reaction temperature, work as pressure drop 8~12 parts of expoxy propane is then passed through to below 0.02MPa, reaction temperature is 120~130 DEG C, reaction pressure 0.15MPa ~0.4MPa, after expoxy propane has led to, continue keep reaction temperature, when pressure drops to below 0.02MPa cure 30~ 45 minutes, with acetic acid and 90~100 DEG C of dischargings are cooled to behind material to PH=6~7, obtain demulsifier MU.
    It is prepared by 3.3 positive oil head PFA type rosin esterifications crude oil demulsifiers：
    3.3.1 the preparation of PFA types resin：The accurate phenol, 6~8 parts of pentaethylene hexamines, 10~15 parts of diformazan benzos for weighing 1 part Move into kettle, heating stirring and insulation 45~55 DEG C 30~45 minutes, the industrial formol 3 that content is 35~37% is then added dropwise ~8 parts, 45~55 DEG C of material in kettle is kept being added dropwise during formaldehyde, after being added dropwise, 30~45 minutes is incubated, then starts Slowly heating material stops heating, cooling when when temperature is at 140~145 DEG C more than constant half an hour until there is backflow to produce To 90~100 DEG C of dischargings, PFA type resins are obtained.
    3.3.2 prepared by PFA types demulsifier：The PFA types resin and total number 0.1 of the accurate 3.3.1 kinds for weighing 3~7 parts~ 0.3% base catalyst simultaneously moves into reactor, heating stirring, vacuum (vacuum pressure is opened when temperature reaches 100~110 DEG C Power≤- 0.09MPa) dehydration, temperature control is 100~110 DEG C, and dewatering time is 35~40 minutes, is continuously led to after dehydration Enter 0.5~3 part of oxirane, reaction temperature is 120~130 DEG C, and reaction pressure is 0.15MPa~0.4MPa；When epoxy second After alkane has led to, continue to keep reaction temperature, cured 30~45 minutes when pressure drops to below 0.02MPa, cool to 90~ 100 DEG C of dischargings, obtain PFA type demulsifiers.
    3.3.3 PFA types demulsifier is esterified：Accurate 8~11 parts of the PFA types demulsifier weighed in 3.3.2,3~5 parts of hydrogenation pines Fragrant and total number 0.1~0.3% the concentrated sulfuric acid is simultaneously moved into kettle, and stirring is warming up to 220~230 DEG C, opens vacuum (vacuum pressure Power -0.03-0.05MPa) dehydration, viscosimetric is sampled after 5~8 hours, 90~100 DEG C of dischargings are cooled to after qualified, obtain PFA types Rosin esterification crude oil demulsifier.
    3.4 sandlwood Tang esters derive from commodity, and purity is 75~80%.
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CN111454745A (en) * 2020-04-02 2020-07-28 万达集团股份有限公司 Demulsifier and preparation method thereof
CN113948685A (en) * 2021-09-09 2022-01-18 广州理文科技有限公司 Silicon-based composite negative electrode material of lithium ion battery and preparation method thereof
CN114891150A (en) * 2022-04-14 2022-08-12 山东大学 Super heavy oil copolymer demulsifier and preparation method and application thereof

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CN102260523A (en) * 2011-06-23 2011-11-30 中国石油天然气股份有限公司 Crude oil dehydrating low-temperature emulsion breaker and preparation method thereof
CN105132009A (en) * 2015-08-25 2015-12-09 盘锦富隆化工有限公司 High pour point and high-viscosity crude oil demulsifier and preparation method therefor

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CN102260523A (en) * 2011-06-23 2011-11-30 中国石油天然气股份有限公司 Crude oil dehydrating low-temperature emulsion breaker and preparation method thereof
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Publication number Priority date Publication date Assignee Title
CN111454745A (en) * 2020-04-02 2020-07-28 万达集团股份有限公司 Demulsifier and preparation method thereof
CN113948685A (en) * 2021-09-09 2022-01-18 广州理文科技有限公司 Silicon-based composite negative electrode material of lithium ion battery and preparation method thereof
CN113948685B (en) * 2021-09-09 2023-11-28 广州理文科技有限公司 Silicon-based composite negative electrode material of lithium ion battery and preparation method thereof
CN114891150A (en) * 2022-04-14 2022-08-12 山东大学 Super heavy oil copolymer demulsifier and preparation method and application thereof
CN114891150B (en) * 2022-04-14 2023-10-10 山东大学 Super-thick oil copolymer demulsifier and preparation method and application thereof

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