CN102993434B - Preparation method of crude oil rapid demulsifying agent - Google Patents
Preparation method of crude oil rapid demulsifying agent Download PDFInfo
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Abstract
The invention relates to a preparation method of a crude oil rapid demulsifying agent. The method is that block copolymerization is carried out between initiator catecholamine resin and ethylene oxide and propylene epoxide to obtain a polyether demulsifying agent under a base catalyst, and then the polyether demulsifying agent is reacted with silicone oil and oleic acid to obtain a crosslinking demulsifying agent. The preparation method solves the problem that the existing demulsifying technology is high in demulsifying temperature, low in demulsifying speed, big in dosage and the like. The crude oil rapid demulsifying agent prepared by using the method has the advantages of rapid demulsification, small dosage, environmental protection and the like.
Description
Technical field
The present invention relates to a kind of preparation method of crude oil rapid demulsifier, belong to Petroleum Processing Technology field.
Background technology
In Oil extraction process, crude oil and water flow to ground through oil pipe simultaneously from stratum, and finally through pipeline, are transported to storage tank.In this process, crude oil and water flow through oil nozzle, valve, elbow, pipeline, stand violent mechanical shearing and form milk sap.When exploiting with oil pumper, oil pumper piston is more violent to the shearing of crude oil and water, therefore more easily forms milk sap.
Crude oil itself is a kind of multicomponent mixture, the hydrocarbon of different relative molecular mass different structures and a small amount of non-hydrocarbon compound matter, consists of.In crude oil, be dissolved in the inorganic salt, mechanical impurity, sand, clay of water and free hydrogen sulfide, hydrogenchloride etc. with in the multi-form colloid that is scattered in crude oil, bituminous matter, make crude oil emulsion more stable.
In recent years, along with the exploitation in oil field, in the crude oil of extraction, water content is more and more higher, adds the application of multiple intensified oil reduction technology, causes crude oil emulsion water content to increase severely.The existence of chemical oil displacement agent (as: alkali, tensio-active agent, polymkeric substance etc.) not only makes the salinity of stratum water quality significantly raise, and the emulsification degree of extraction crude oil is further strengthened, and the stability of crude oil emulsion significantly improves, and breakdown of emulsion difficulty strengthens.And the problem such as the emulsion splitter ubiquity breakdown of emulsion temperature that each oil field is used is at present high, emulsion splitter dosage is large, de-emulsification speed is slow, cause huge energy dissipation and high processing cost.In addition, quite a few Oilfield using oil-soluble demulsifier at present,, not only to environment, and there is potential safety hazard while using in the organic solvent using (as toluene).Therefore, make under water content in crude oil prerequisite up to standard, developing a kind of breakdown of emulsion temperature crude oil demulsifier low, that dosage is few, de-emulsification speed is fast and environmentally friendly becomes a current oil field difficult problem urgently to be resolved hurrily.
CN102030878A(CN201010548445.5) disclose a kind of preparation method of oil field demulsifier, the method be take polyethylene polyamine as raw material, by with oxyethane, propylene oxide reaction is post-crosslinking modified makes.First take polyethylene polyamine as initiator, under the existence of basic catalyst, react with propylene oxide and ethylene oxide and make polyethylene polyamine type polyethers emulsion splitter.Then under catalyst action, adopt polycarboxylic acid that polyethers emulsion splitter A is carried out to self-crosslinking reaction, make product B.Finally in solvent, adopt tolylene diisocyanate to carry out self-crosslinking reaction polyethers emulsion splitter A and product B, make final product high performance demulsifying agent.The emulsion splitter that the present invention makes, relative molecular weight is higher, dehydrating effect is desirable, broad spectrum is good, applicable to the breaking emulsion and dewatering of crude oil, deviates from that water quality is clear, consumption is few.The deficiency of this document technical scheme is mainly and adopts the larger TDI of human toxicity as linking agent, uses dimethylbenzene as solvent, has increased cost and to environment.
Summary of the invention
For the deficiencies in the prior art, in order to have solved the problems such as the breakdown of emulsion temperature that existing demulsification technology exists is high, de-emulsification speed is slow, dosage is large, the invention provides a kind of preparation method crude oil emulsion to the emulsion splitter of fast emulsion breaking ability.
The present invention is realized by following technical scheme:
A preparation method for crude oil rapid demulsifier, comprises that step is as follows:
(1) to the formaldehyde solution that drips 35-38wt% in the mixed system of vinyl-amine and phenol, dehydration reaction 0.5-3h at 20-200 ℃ of temperature, makes initiator phenol-amine resin;
Raw material weight proportioning is phenol: vinyl-amine: formaldehyde solution=1:1-20:0.5-10;
(2) the initiator phenol-amine resin of (1) gained is put in autoclave, add alkali as a catalyst, at 100-150 ℃, add propylene oxide, control pressure 0.1-0.4MPa reacts 2-4h, aging 1h, then add oxyethane, control pressure 0.1-0.4MPa reacts 1-3h, and aging 1h makes polyether demulsification agent;
Above-mentioned initiator phenol-amine resin: propylene oxide: oxyethane: alkali=1:100-500:50-300:0.45-24.
Continue following steps, make crosslinked emulsion splitter:
(3) (2) gained polyether demulsification agent is carried out to vacuum hydro-extraction, add silicone oil and oleic acid at 50-120 ℃, Depressor response 25-35 minute, obtains crosslinked emulsion splitter;
Raw material weight proportioning is polyethers: silicone oil: oleic acid=1:0.1-2:0.01-1.
In above-mentioned preparation method, in step (1), the phenol of phenol-amine resin is phenol, dihydroxyphenyl propane, Resorcinol or p-tert-butylphenol, and described vinyl-amine is quadrol, diethylenetriamine, triethylene tetramine, tetraethylene pentamine or five ethene hexamines.
In above-mentioned preparation method, preferably, in step (1), the mixed system of vinyl-amine and phenol is tetraethylene pentamine and dihydroxyphenyl propane, the formaldehyde solution that formaldehyde used is 36wt%, dihydroxyphenyl propane: tetraethylene pentamine: formaldehyde solution=1:2.5-4:1-2 weight ratio, temperature of reaction 30-40 ℃.
In above-mentioned preparation method, preferred, in step (1), the reactant of dehydration reaction is added to dimethylbenzene, be warming up to 100-110 ℃, back flow reaction 2h, after all steaming, then steams dimethylbenzene to water, obtains initiator phenol-amine resin.
In above-mentioned preparation method, alkaline catalysts described in step (2) is one or more of sodium hydroxide, potassium hydroxide, sodium ethylate.Preferred potassium hydroxide wherein.
In above-mentioned preparation method, preferred, stir while being warming up to 75-85 ℃ after adding alkali in step (2), reactor is evacuated to vacuum tightness for-0.1MPa, when temperature rises to 100 ℃, then adds propylene oxide.
In above-mentioned preparation method, linking agent silicone oil described in step (3) is MethylethoxylsiliconFluid Fluid, Methyl Hydrogen Polysiloxane Fluid or methyl hydroxy silicon oil.
The polyether demulsification agent product that above-mentioned steps of the present invention (2) makes can be used as emulsion splitter and uses, but effect is slightly inferior to the crosslinked emulsion splitter that step (3) obtains after modification.
The present invention be take phenol-amine resin as initiator, take alkali as catalyzer, and initiation oxyethane, propylene oxide carry out block copolymerization, obtain racemosus shape polyethers.This polyethers can be used as emulsion splitter separately, is made into 50% methanol solution, is diluted with water to aequum.Continue again gained polyethers to be reacted with linking agent silicone oil, make crosslinked emulsion splitter; During use, be made into massfraction and be 50% methanol solution, be diluted with water to aequum.
Emulsion splitter prepared by the present invention has the advantages such as quick, low dosage, environmental protection.The crosslinked emulsion splitter that particularly the present invention makes, in the situation that emulsion splitter dosage is 100mg/L, during 65 ℃ of temperature, in one hour, dehydration rate can reach more than 90%.This emulsion splitter is can various ratios water-soluble, because having used nontoxic silicone oil as linking agent, has avoided the use of noxious solvent toluene, has both been conducive to improve the security that emulsion splitter is used, and is also conducive to environment protection.
Embodiment
The experimental technique using in following embodiment if no special instructions, is ordinary method.
In following embodiment, material used, reagent etc., if no special instructions, all can obtain from commercial channels.
Embodiment 1. polyether demulsification agent A's is synthetic
(1) initiator phenol-amine resin is synthetic
By the dihydroxyphenyl propane of 25g, 82.5g tetraethylene pentamine adds and in 500ml there-necked flask, adds out that stirring heats up dissolves dihydroxyphenyl propane, after dihydroxyphenyl propane dissolves completely, be cooled to 35 ℃, drip the formaldehyde solution that 37.5g massfraction is 36%, keep temperature 30-40 ℃, dropwise rear insulation reaction 40min.The dimethylbenzene that adds 72.5g, is warming up to 100-110 ℃.Back flow reaction 2h.Slowly heat up and under reflux conditions water is taken out of, after all steaming to water, then dimethylbenzene is steamed and obtained initiator phenol-amine resin.
(2) polyether demulsification agent A's is synthetic
Gained initiator phenol-amine resin 1g in step (1) and potassium hydroxide 1g are added in autoclave, sealed reactor, start and stir and heat up, when temperature rises to 80 ℃ of left and right, with vacuum pump, reactor is vacuumized, the vacuum tightness that vacuumizes approximately 20 minutes in still during for-0.1MPa, stops vacuumizing.Continue to stir heat up, when temperature rises to 100 ℃, slowly add 199g propylene oxide, control temperature of reaction at 120-140 ℃, pressure is at 0.2-0.4MPa, reaction times 3h.After completion of the reaction, aging 2.5h, is cooled to 100 ℃.Again 133g oxyethane is added to reactor, control temperature of reaction at 120-140 ℃, pressure is at 0.2-0.4MPa, reaction times 1-3h, and after completion of the reaction, aging 1h, obtains polyether demulsification agent A.
When polyether demulsification agent A is used, be first made into massfraction and be 50% methanol solution, be diluted with water to aequum.
Embodiment 2. crosslinked emulsion splitter B's is synthetic
The 10g polyether demulsification agent A of embodiment 1 preparation is added in 25ml single port bottle, be warming up to 100 ℃ of left and right vacuum hydro-extractions.After dehydration, add 0.5g MethylethoxylsiliconFluid Fluid and 0.07g oleic acid, Depressor response 30 minutes.Material retrogradation termination reaction while having wire drawing.Reaction gained is crosslinked emulsion splitter B.
Embodiment 3. crosslinked emulsion splitter C's is synthetic
As described in example 2 above, the charging capacity of different is MethylethoxylsiliconFluid Fluid changes 1g into, and the charging capacity of oleic acid changes 0.13g into, and reaction gained is crosslinked emulsion splitter C.
Embodiment 4. crosslinked emulsion splitter D's is synthetic
As described in example 2 above, the charging capacity of different is MethylethoxylsiliconFluid Fluid changes 1.5g into, and the charging capacity of oleic acid changes 0.2g into, and reaction gained is crosslinked emulsion splitter D.
The crosslinked emulsion splitter of above-described embodiment 2-4, is made into massfraction and is 50% methanol solution during use, be diluted with water to aequum.
Embodiment 5. polyether demulsification agent E's is synthetic
By embodiment 1(1) initiator phenol-amine resin 1g and the 1.5g potassium hydroxide of gained adds in autoclave, sealed reactor, start and stir and heat up, when temperature rises to 80 ℃, with vacuum pump, reactor is vacuumized, the vacuum tightness that vacuumizes approximately 20 minutes in still during for-0.1Mpa, stops vacuumizing.Continue to stir and heat up, when temperature rises to 100 ℃, slowly add 299g propylene oxide, temperature of reaction 120-140 ℃, pressure 0.2-0.4MPa, reaction times 3h.Aging 1h, is cooled to 100 ℃ after completion of the reaction, 199g oxyethane is added, and temperature of reaction 120-140 ℃, pressure is at 0.2-0.4MPa, reaction times 2h.Aging 1h obtains polyether demulsification agent E after completion of the reaction.During use, be made into massfraction and be 50% methanol solution, be diluted with water to aequum.
Embodiment 6. crosslinked emulsion splitter F's is synthetic
The 10g polyether demulsification agent E that embodiment 5 is made adds in 25ml single port bottle, is warming up to 100 ℃ of left and right vacuum hydro-extractions.After dehydration, add 0.3g MethylethoxylsiliconFluid Fluid and 0.04g oleic acid, Depressor response 30 minutes.Termination reaction until material retrogradation and while having wire drawing.Reaction gained is crosslinked emulsion splitter F.
Embodiment 7. crosslinked emulsion splitter G's is synthetic
As described in example 6 above, the charging capacity of different is MethylethoxylsiliconFluid Fluid changes 0.5g into, and the charging capacity of oleic acid changes 0.07g into, and reaction gained is crosslinked emulsion splitter G.
Embodiment 8. crosslinked emulsion splitter H's is synthetic
As described in example 6 above, the charging capacity of different is MethylethoxylsiliconFluid Fluid changes 1g into, and the charging capacity of oleic acid changes 0.13g into, and reaction gained is crosslinked emulsion splitter H.
The crosslinked emulsion splitter of above-described embodiment 6-8, is made into massfraction and is 50% methanol solution during use, be diluted with water to aequum.
Emulsion splitter performance evaluation experiment prepared by embodiment 9. embodiment 1-8
Bohai Bay Oil crude oil is carried out to the test of bottle examination method breakdown of emulsion at 65 ℃ of temperature at the scene, and experimental result is as shown in table 1.
This bottle of examination method is with reference to China National Petroleum industry standard SY/T 5281-2000 < < crude oil demulsifier use properties detection method (bottle examination method) > > and the company standard Q/HS 2020-2004 of China National Offshore Oil Corporation (CNOOC).
Specific experiment step is:
Ready crude oil production fluid sample is poured in dehydration test bottle pipe, and heating in water bath continues constant temperature 15min to homo(io)thermism.
With syringe, in dehydration test tube, inject a certain amount of emulsion splitter A-H).The vibration of dehydration test tube adopts artificial succusion.Screw after bottle cap, dehydration test tube is put upside down 2-5 time, slowly, after loosening bottle stopper venting, again screw bottle stopper, mode is directly vibrated by hand.After left hand vibration 100 times, slowly, after loosening bottle stopper venting, again screw bottle stopper.Change again right hand vibration 100 times, after fully mixing, loosening bottle stopper, and again dehydration test tube is placed in to water bath with thermostatic control standing sedimentation.
Record the water yield of deviating from of different time, when dehydration stops, observed and recorded sewage color and water-oil interface situation.Experimental result is as shown in table 1.
The breakdown of emulsion experimental result of the emulsion splitter of table 1 embodiment 1-8 to Bohai Bay Oil crude oil
Claims (3)
1. a preparation method for crude oil rapid demulsifier, comprises that step is as follows:
(1) to the formaldehyde solution that drips 36wt% in the mixed system of tetraethylene pentamine and dihydroxyphenyl propane, dehydration reaction 0.5-3h at 30-40 ℃ of temperature, the reactant of dehydration reaction is added to dimethylbenzene, be warming up to 100-110 ℃, back flow reaction 2h, after all steaming to water, then dimethylbenzene is steamed, obtain initiator phenol-amine resin;
Raw material weight proportioning is dihydroxyphenyl propane: tetraethylene pentamine: formaldehyde solution=1:2.5-4:1-2 weight ratio;
(2) the initiator phenol-amine resin of (1) gained is put in autoclave, add alkali as a catalyst, at 100-150 ℃, add propylene oxide, control pressure 0.1-0.4MPa reacts 2-4h, aging 1h, then add oxyethane, control pressure 0.1-0.4MPa reacts 1-3h, and aging 1h makes polyether demulsification agent;
Above-mentioned initiator phenol-amine resin: propylene oxide: oxyethane: alkali=1:100-500:50-300:0.45-24;
(3) (2) gained polyether demulsification agent is carried out to vacuum hydro-extraction, add MethylethoxylsiliconFluid Fluid and oleic acid at 50-120 ℃, raw material weight proportioning is polyethers: silicone oil: oleic acid=1:0.1-2:0.01-1, Depressor response 25-35 minute, obtains crosslinked emulsion splitter.
2. the preparation method of crude oil rapid demulsifier according to claim 1, is characterized in that alkaline catalysts described in step (2) is one or more of sodium hydroxide, potassium hydroxide, sodium ethylate.
3. the preparation method of crude oil rapid demulsifier according to claim 1, stirs while being warming up to 75-85 ℃ after it is characterized in that adding alkali in step (2), and reactor is evacuated to vacuum tightness for-0.1MPa, when temperature rises to 100 ℃, then adds propylene oxide.
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