CN107557055A - A kind of preparation method of modified polyether crude oil rapid demulsifier - Google Patents
A kind of preparation method of modified polyether crude oil rapid demulsifier Download PDFInfo
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- CN107557055A CN107557055A CN201710990704.1A CN201710990704A CN107557055A CN 107557055 A CN107557055 A CN 107557055A CN 201710990704 A CN201710990704 A CN 201710990704A CN 107557055 A CN107557055 A CN 107557055A
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Abstract
The present invention relates to a kind of preparation method of modified polyether crude oil rapid demulsifier.Preparation method of the present invention includes:Ethylenediamine and expoxy propane, oxirane are first subjected to ring opening copolymer, obtain block polyether A, then phenol-amine resin and expoxy propane, oxirane are subjected to ring opening copolymer again, obtain block polyether B, after then two kinds of polyethers of gained are proportionally sufficiently mixed, react to obtain modified polyether demulsifier with modifying agent.Demulsifier that preparation method of the present invention obtains while dewatering speed can be realized soon and the abjection limpid two kinds of purposes of water, it is single polyether-modified to realize there is that low dosage, demulsification are quick, dehydration rate is high, it is limpid to deviate from water simultaneously.
Description
Technical field
The present invention relates to a kind of preparation method of modified polyether crude oil rapid demulsifier, belong to oil field chemical field.
Background technology
Contain a large amount of water in crude oil, and emulsion is formed with water.Crude oil emulsion is formed in recovery process, that is, is existed
Oil well restriction, valve, oil pump and petroleum pipeline etc., crude oil and water pass through strong friction, particularly cutting in oil pump paddle
Under the souring of the effect of cutting and high pressure drop, profit is mixed and forms crude oil emulsion strongly.Crude oil emulsion is to crude oil
Transport, application and processing can all produce strong influence.Therefore, have to enter crude oil emulsion after oil extraction out
Row demulsification.Breaking method is broadly divided into chemical demulsification method, physical demulsification method, biological demulsifying agent method, joint demulsification method and film demulsification
Method.At present, the application of chemical demulsifier method is most extensive.China oil field preferable demulsifier of using effect is based on polyethers
Demulsifier, it is different by initiator, the difference of oxirane, the adduct number of expoxy propane and ratio, it can obtain different polyethers and break
Emulsion.For nonionic polyoxyethylene block polymer Research Thinking be concentrated mainly on to traditional demulsifier carry out " change head,
Change tail plus bone, chain extension, grafting, hand over poly-, compounding " the methods of meet the needs of Oil Field is to demulsifier.But the above method
In there are still the shortcomings of preparation process is complicated, preparation condition is harsh or demulsification is undesirable.
South China Sea Oilfield offshore platform processing time is short, space are limited, can not indiscriminately imitate the existing experience in land oil field.At sea
Oil field, crude oil dehydration rate is relatively low to cause problems with:(1) burden of platform electric dehydrator is increased;(2) a large amount of emulsified waters are caused
Terminal is transported to offshore pipeline, increases the burden of offshore pipeline;(3) treating capacity and oil-polluted water of terminal wastewater treatment plant are added
Arrange magnanimity.
The content of the invention
In view of the shortcomings of the prior art, in order to solve, preparation process existing for existing demulsifier modification technology is excessive, prepares
Being demulsified during complex process, severe reaction conditions and demulsification, temperature is high, de-emulsification speed is slow, dosage is big, deviates from water muddiness etc.
Problem, present invention offer is a kind of to have fast emulsion breaking ability and the limpid and course of reaction of dehydration simply modified to crude oil emulsion
The preparation method of polyether demulsification agent, so as to mitigate the burden of platform electric dehydrator, the processing that and can mitigates land terminal is born
Load, reduce polluter smoking amount.
The present invention is realized by following technical scheme:
A kind of preparation method of modified polyether crude oil rapid demulsifier of the present invention, using vinylamine as initiator, using alkali to urge
Agent, trigger oxirane, expoxy propane to carry out block copolymerization, obtain polyether demulsification agent A, using phenol-amine resin as initiator, with
Alkali is catalyst, triggers oxirane, expoxy propane to carry out block copolymerization, obtains polyether demulsification agent B, then gained polyethers is demulsified
Agent A and B react to obtain modified emulsion breaker after compounding according to a certain percentage with modifying agent.Specific preparation process is as follows:
A kind of preparation method of modified polyether crude oil rapid demulsifier provided by the invention, comprises the following steps:
1) polyethers A synthesis:Vinylamine is put into autoclave, adds alkali as a catalyst, at 100-150 DEG C,
Expoxy propane is added, control pressure 0.1-0.4MPa reaction 4-8h, within aging 1h, adds oxirane, control pressure
Within 0.1-0.4MPa reactions 2-4h, aging 1h, polyethers A is made;
Raw material mass mixture ratio is vinylamine:Expoxy propane:Oxirane:Alkali=1:10-500:5-200:0.05-24;
(2) synthesis of initiator phenol-amine resin:It is molten that 35-38wt% formaldehyde is added dropwise into the mixed system of vinylamine and phenol
Liquid, 30-40 DEG C of reaction temperature, after reaction terminates, add dimethylbenzene, the dehydration 0.5-3h under the conditions of 20-200 DEG C, to water
After all steaming, then dimethylbenzene steamed, obtain initiator phenol-amine resin;
Raw material weight proportioning of soup processed is phenol:Vinylamine:Formalin=1:1-20:0.5-10;
(3) polyethers B synthesis:The initiator phenol-amine resin of gained in (2) is put into autoclave, adds alkali to urge
Agent, at 100-150 DEG C, add within expoxy propane control pressure 0.1-0.4MPa reactions 4-8h, aging 1h, add ring
Within oxidative ethane control pressure 0.1-0.4MPa reactions 2-4h, aging 1h, that is, polyethers B is made;
Raw material mass mixture ratio is initiator phenol-amine resin:Expoxy propane:Oxirane:Alkali=1:10-500:5-200:
0.45-24;
(4) modified-reaction:The polyethers A and polyethers B of gained in (1) and (3) are dissolved in dimethylbenzene, dropwise addition modifying agent/
Xylene solution;Smooth reaction 30-90 minutes, adding remaining dimethylbenzene makes product design that modified polyether be made after reaching 45-55%
Crude oil rapid demulsifier;Wherein raw material weight proportioning of soup processed is polyethers A:Polyethers B:Dimethylbenzene:Modifying agent=1:0.5-10:0.5-10:
0.01-0.5;
Wherein:Described alkali is sodium hydroxide, potassium hydroxide, the one or more of caustic alcohol;
Vinylamine described in step (1) is ethylenediamine, diethylenetriamine, triethylene tetramine, TEPA or five second
Alkene hexamine;
The phenol of phenol-amine resin is phenol, bisphenol-A, hydroquinones or p-t-butyl phenol in step (2);The vinylamine is
Ethylenediamine, diethylenetriamine, triethylene tetramine, TEPA or pentaethylene hexamine;
Modifying agent described in step (4) is toluene di-isocyanate(TDI), epoxychloropropane, acrylic acid, the one of dimethyl carbonate
Kind is several.
In above-mentioned preparation method, it is preferred that the vinylamine described in step (1) is ethylenediamine.
In above-mentioned preparation method, it is preferred that the vinylamine described in step (1) is TEPA.
In above-mentioned preparation method, it is preferred that the phenol of phenol-amine resin is bisphenol-A in step (2).
In above-mentioned preparation method, it is preferred that modifying agent described in step (4) is toluene di-isocyanate(TDI).
In above-mentioned preparation method, it is preferred that in step (4), the polyether demulsification agent A and B of gained are dissolved in dimethylbenzene,
10-100 DEG C is heated to, 10% modifying agent/xylene solution is slowly added dropwise, smooth reaction 30-90 points during dropwise addition
Clock, adding remaining dimethylbenzene makes product design reach 45-55%, weight proportion polyethers A:Polyethers B:Dimethylbenzene:Modifying agent=1:
2:2-4:0.01-0.2。
Polyethers A is linear polyether in the present invention, can quickly be dispersed to oil-water interfaces in demulsification, have dewatering speed
The characteristics of fast, but final dewatering rate is not high, and it is more muddy to deviate from water.Polyethers B is more dendritic polyethers, and molecular volume is larger,
Diffusion velocity is slower in profit, so its dewatering speed is slower, but because its molecular volume is larger, can more preferably reduce profit
Interfacial tension, so dehydrating effect is more preferable, abjection water is more limpid.Polyethers A and B product can also use as demulsifier, but
Effect is inferior to the modified emulsion breaker that modified step (4) obtains.The present invention is broken as obtained by polyethers A and polyethers B mixing post-modifications
Emulsion has dewatering speed concurrently soon and the characteristics of abjection water is limpid, single polyether-modified to realize both results simultaneously.
Compared with prior art, this method has that preparation process is simple, reaction condition is gentle to the present invention, and what is be prepared changes
Property crude polyether rapid demulsifier be demulsified quick, low dosage, the advantages that abjection water is limpid, taken off in 80 DEG C of temperature in 20min
Water rate can reach more than 85%.
Embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.Institute in following embodiments
Material, reagent etc., unless otherwise specified, commercially obtain.
The modified emulsion breaker C of embodiment 1. synthesis
(1) polyethers A synthesis
Ethylenediamine 2g and potassium hydroxide 0.5g is added in autoclave, seals reactor, starts and stirs and heat up, treat
When temperature rises to 80 DEG C or so, reactor is vacuumized with vavuum pump, vacuumizes and treats within about 20 minutes that vacuum is -0.1MPa in kettle
When, stop vacuumizing.Continue stirring heating, when temperature rises to 100 DEG C, be slowly added to 138g expoxy propane, control reaction temperature
Degree is at 120-140 DEG C, and pressure is in 0.2-0.4MPa, reaction time 3h.After completion of the reaction, aging 1h, 100 DEG C are cooled to.By 35g
Oxirane adds reactor, and controlling reaction temperature is at 120-140 DEG C, and pressure is in 0.2-0.4MPa.Reaction time 1.5h reacts
After, aging 1h produces polyethers A.
(2) polyethers B synthesis
By 22.8g bisphenol-A, 75.6g TEPAs, which add addition in 500ml there-necked flasks, which opens stirring heating, makes bisphenol-A
Dissolving, until completely dissolved, 35 DEG C are cooled to, the formalin that 33.3g mass fractions are 36%, keeping temperature 30-40 is added dropwise
DEG C, rear insulation reaction 40min is added dropwise.65.8g dimethylbenzene is added, is warming up to 100-110 DEG C.Back flow reaction 2h.Slowly
Heating under reflux conditions takes water out of, after all being steamed to water, then dimethylbenzene is steamed and produces initiator phenol-amine resin.
Above-mentioned gained initiator phenol-amine resin 2g and potassium hydroxide 0.8g is added in autoclave, seals reactor,
Start and stir and heat up, when temperature rises to 80 DEG C or so, reactor is vacuumized with vavuum pump, vacuumizes about 20 minutes and treats kettle
When interior vacuum is -0.1MPa, stop vacuumizing.Continue stirring heating, when temperature rises to 100 DEG C, be slowly added to 198g rings
Ethylene Oxide, controlling reaction temperature is at 120-140 DEG C, and pressure is in 0.2-0.4MPa, reaction time 3h.After completion of the reaction, aging 1h,
It is cooled to 100 DEG C.73g oxirane is added into reactor, controlling reaction temperature is at 120-140 DEG C, and pressure is in 0.2-0.4MPa.
After completion of the reaction, aging 1h produces polyethers B to reaction time 1.5h.
(3) modified emulsion breaker C synthesis
20g polyether demulsification agent B and the 10g diformazans that will be prepared in the 10g polyether demulsification agent A embodiments 2 prepared in embodiment 1
Benzene is added in the there-necked flask equipped with electromagnetic and mechanical stirring and constant pressure funnel, is heated to 60 DEG C with oil bath pan, fully
It is well mixed.0.15g toluene di-isocyanate(TDI) is made into 10% xylene solution, 10% toluene two is added dropwise into there-necked flask
Isocyanate solution, keep 60 DEG C of constant temperature.When toluene di-isocyanate(TDI) is added dropwise, rate of addition is slowly steady, after being added dropwise,
Polyether solutions smooth reaction 45 minutes, adding dimethylbenzene makes product design obtain modified emulsion breaker C up to 50%.
The modified emulsion breaker D of embodiment 2. synthesis
As described in embodiment 1 (3), the difference is that the inventory of toluene di-isocyanate(TDI) is changed to 0.3g, reaction gained is
Modified emulsion breaker D.
The modified emulsion breaker E of embodiment 3. synthesis
As described in embodiment 1 (3), the difference is that the inventory of toluene di-isocyanate(TDI) is changed to 0.45g, reaction gained is
Modified emulsion breaker E.
Demulsifier henchnmrk test prepared by bottle examination EXPERIMENTAL EXAMPLE 1-3
To carrying out bottle examination method demulsification experiment at South China Sea Oilfield crude oil at the scene 80 DEG C of temperature, with onsite application demulsifier BP-
10 compare, and experimental result is as shown in table 1.
Bottle examination method is with reference to China National Petroleum professional standard SY/T 5281-2000《Crude oil demulsifier performance is examined
Survey method (bottle examination method)》And China National Offshore Oil Corporation company standard Q/HS 2020-2004.
Specific experiment step is:
Ready crude oil production fluid sample is poured into dehydration test bottle pipe, heating water bath, it is permanent to the constant rear continuation of temperature
Warm 15min.
With micro syringe to dehydration test tube in inject a certain amount of demulsifier (demulsifier C, demulsifier D, demulsifier E and
BP-10).The vibration of dehydration test tube uses artificial succusion.It is after screwing bottle cap, dehydration test tube is reverse 2-5 times, slowly loosen bottle
After plug is deflated, bottle stopper is screwed again, mode directly vibrates by hand.After left hand vibrates 100 times, after slowly loosening bottle stopper deflation,
Again bottle stopper is screwed.The right hand is changed again to vibrate 100 times, after being sufficiently mixed uniformly, loosens bottle stopper, and dehydration test tube is placed in perseverance again
Standing sedimentation in tepidarium.
The abjection water of different time is recorded, when dehydration terminates, observes and records sewage color and oil-water interfaces situation.Experiment
As a result it is as shown in table 1.
Demulsification experimental result of the embodiment 1-3 of table 1 demulsifier to South China Sea Oilfield crude oil
Claims (6)
1. a kind of preparation method of modified polyether crude oil rapid demulsifier, including step are as follows:
(1) polyethers A synthesis:Vinylamine is put into autoclave, adds alkali as a catalyst, at 100-150 DEG C, is added
Expoxy propane, control pressure 0.1-0.4MPa reaction 4-8h, within aging 1h, adds oxirane, control pressure 0.1-
Within 0.4MPa reactions 2-4h, aging 1h, polyethers A is made;
Raw material mass mixture ratio is vinylamine:Expoxy propane:Oxirane:Alkali=1:10-500:5-200:0.05-24;
(2) synthesis of initiator phenol-amine resin:35-38wt% formalins are added dropwise into the mixed system of vinylamine and phenol, instead
After answering 30-40 DEG C of temperature, reaction to terminate, dimethylbenzene is added, the dehydration 0.5-3h under the conditions of 20-200 DEG C, is all steamed to water
After going out, then dimethylbenzene steamed, obtain initiator phenol-amine resin;
Raw material weight proportioning of soup processed is phenol:Vinylamine:Formalin=1:1-20:0.5-10;
(3) polyethers B synthesis:The initiator phenol-amine resin of gained in (2) is put into autoclave, adds alkali to be catalyzed
Agent, at 100-150 DEG C, add within expoxy propane control pressure 0.1-0.4MPa reactions 4-8h, aging 1h, add epoxy
Within ethane control pressure 0.1-0.4MPa reactions 2-4h, aging 1h, that is, polyethers B is made;
Raw material mass mixture ratio is initiator phenol-amine resin:Expoxy propane:Oxirane:Alkali=1:10-500:5-200:0.45-
24;
(4) modified-reaction:The polyethers A and polyethers B of gained in (1) and (3) are dissolved in dimethylbenzene, modifying agent/diformazan is added dropwise
Benzole soln;Smooth reaction 30-90 minutes, adding remaining dimethylbenzene makes product design that modified polyether original be made after reaching 45-55wt%
Oily rapid demulsifier;Wherein raw material weight proportioning of soup processed is polyethers A:Polyethers B:Dimethylbenzene:Modifying agent=1:0.5-10:0.5-10:
0.01-0.5;
Wherein:Described alkali is sodium hydroxide, potassium hydroxide, the one or more of caustic alcohol;
Vinylamine described in step (1) is ethylenediamine, diethylenetriamine, triethylene tetramine, TEPA or five ethene six
Amine;
The phenol of phenol-amine resin is phenol, bisphenol-A, hydroquinones or p-t-butyl phenol in step (2);The vinylamine is second two
Amine, diethylenetriamine, triethylene tetramine, TEPA or pentaethylene hexamine;
Modifying agent described in step (4) be toluene di-isocyanate(TDI), epoxychloropropane, acrylic acid, one kind of dimethyl carbonate or
It is several.
2. the preparation method of modified polyether crude oil rapid demulsifier according to claim 1, it is characterised in that step (1)
Described in vinylamine be ethylenediamine.
3. the preparation method of modified polyether crude oil rapid demulsifier according to claim 1, it is characterised in that step (1)
Described in vinylamine be TEPA.
4. the preparation method of modified polyether crude oil rapid demulsifier according to claim 1, it is characterised in that step (2)
The phenol of middle phenol-amine resin is bisphenol-A.
5. the preparation method of modified polyether crude oil rapid demulsifier according to claim 1, it is characterised in that step (4)
Described in modifying agent be toluene di-isocyanate(TDI).
6. the preparation method of modified polyether crude oil rapid demulsifier according to claim 1, it is characterised in that step (4)
In, the polyether demulsification agent A and B of gained are dissolved in dimethylbenzene, are heated to 10-100 DEG C, be slowly added dropwise 10% modifying agent/
Xylene solution, the smooth reaction 30-90 minutes during dropwise addition, adding remaining dimethylbenzene makes product design reach 45-
55%, weight proportion polyethers A:Polyethers B:Dimethylbenzene:Modifying agent=1:2:2-4:0.01-0.2.
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CN109705832B (en) * | 2019-01-29 | 2021-09-10 | 中国海洋石油集团有限公司 | High-temperature anti-emulsion synergist and preparation and application thereof |
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CN113684054A (en) * | 2021-10-26 | 2021-11-23 | 胜利油田海发环保化工有限责任公司 | Demulsifier and preparation method thereof |
CN113684054B (en) * | 2021-10-26 | 2022-02-08 | 胜利油田海发环保化工有限责任公司 | Demulsifier and preparation method thereof |
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