CN102993434A - 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
本发明涉及一种原油快速破乳剂的制备方法。本发明的方法是在碱催化剂存在下，将起始剂酚胺树脂与环氧乙烷、环氧丙烷进行嵌段共聚得到聚醚破乳剂，将所得聚醚破乳剂再与硅油和油酸反应得到交联破乳剂。本发明解决了现有破乳技术存在的破乳温度高、破乳速度慢、加量大等问题。本发明的破乳剂具有快速破乳、低加量、环保等特点。The invention relates to a preparation method of a quick demulsifier for crude oil. In the method of the present invention, in the presence of an alkali catalyst, the initiator phenolamine resin is block-copolymerized with ethylene oxide and propylene oxide to obtain a polyether demulsifier, and the obtained polyether demulsifier is reacted with silicone oil and oleic acid A cross-linked demulsifier is obtained. The invention solves the problems of high demulsification temperature, slow demulsification speed, large dosage and the like existing in the existing demulsification technology. The demulsifier of the invention has the characteristics of rapid demulsification, low 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 the Petroleum Processing Technology field.
Background technology
In the Oil extraction process, crude oil and water flow to ground through oil pipe simultaneously from the stratum, and finally are transported to storage tank through pipeline.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, the oil pumper piston is more violent to the shearing of crude oil and water, therefore easier formation milk sap.
Crude oil itself is a kind of multicomponent mixture, is comprised of the hydrocarbon of different relative molecular mass different structures and a small amount of non-hydrocarbon compound matter.Be dissolved in the inorganic salt, mechanical impurity, sand, clay of water and free hydrogen sulfide, hydrogenchloride etc. in the crude oil with in the multi-form colloid that is scattered in crude oil, the bituminous matter, so that crude oil emulsion is more stable.
In recent years, along with the exploitation in oil field, water content is more and more higher in the crude oil of extraction, adds the application of multiple intensified oil reduction technology, causes the 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 then the stability of crude oil emulsion significantly improves, and the breakdown of emulsion difficulty strengthens.And the emulsion splitter ubiquity breakdown of emulsion temperature of at present each oil field use is high, the emulsion splitter dosage is large, de-emulsification speed waits problem slowly, causes huge energy dissipation and high processing cost.In addition, present quite a few Oilfield using oil-soluble demulsifier, not only to environment, and there is potential safety hazard when using in employed organic solvent (such as toluene).Therefore, make under the 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 the difficult problem that current oil field needs to be resolved hurrily.
CN102030878A(CN201010548445.5) disclose a kind of preparation method of oil field demulsifier, the method is take polyethylene polyamine as raw material, by with oxyethane, propylene oxide reaction is post-crosslinking modified makes.At first take polyethylene polyamine as initiator, in the presence of basic catalyst, make polyethylene polyamine type polyethers emulsion splitter with propylene oxide and ethylene oxide reaction.Then under catalyst action, adopt polycarboxylic acid that polyethers emulsion splitter A is carried out self-crosslinking reaction, make product B.In solvent, adopt tolylene diisocyanate to carry out self-crosslinking reaction polyethers emulsion splitter A and product B at last, make the 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 who crude oil emulsion is had the emulsion splitter of fast emulsion breaking ability.
The present invention is realized by following technical scheme:
A kind of preparation method of crude oil rapid demulsifier comprises that step is as follows:
(1) drip the formaldehyde solution of 35-38wt% in the mixed system of vinyl-amine and phenol, dehydration reaction 0.5-3h under 20-200 ℃ of temperature makes the initiator phenol-amine resin;
The 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 the autoclave, add alkali as a catalyst, under 100-150 ℃, add propylene oxide, control pressure 0.1-0.4MPa reacts 2-4h, and aging 1h adds oxyethane again, 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 vacuum hydro-extraction, at 50-120 ℃ of lower silicone oil and the oleic acid of adding, Depressor response 25-35 minute, get crosslinked emulsion splitter;
The raw material weight proportioning is polyethers: silicone oil: oleic acid=1:0.1-2:0.01-1.
Among the above-mentioned preparation method, the phenol of phenol-amine resin is phenol, dihydroxyphenyl propane, Resorcinol or p-tert-butylphenol in the step (1), and described vinyl-amine is quadrol, diethylenetriamine, triethylene tetramine, tetraethylene pentamine or five ethene hexamines.
Among the above-mentioned preparation method, preferably, the mixed system of vinyl-amine and phenol is tetraethylene pentamine and dihydroxyphenyl propane in the step (1), and used formaldehyde is the formaldehyde solution of 36wt%, dihydroxyphenyl propane: tetraethylene pentamine: formaldehyde solution=1:2.5-4:1-2 weight ratio, temperature of reaction 30-40 ℃.
Among the above-mentioned preparation method, preferred, in the step (1), the reactant of dehydration reaction is added dimethylbenzene, be warming up to 100-110 ℃, back flow reaction 2h after all steaming to water, steams dimethylbenzene again, gets the initiator phenol-amine resin.
Among the above-mentioned preparation method, alkaline catalysts described in the step (2) is one or more of sodium hydroxide, potassium hydroxide, sodium ethylate.Preferred potassium hydroxide wherein.
Among the above-mentioned preparation method, preferred, stir when being warming up to 75-85 ℃ after adding alkali in the step (2), reactor is evacuated to vacuum tightness and is-0.1MPa, when treating that temperature rises to 100 ℃, adds propylene oxide again.
Among the above-mentioned preparation method, linking agent silicone oil described in the 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 slightly is inferior to the crosslinked emulsion splitter that step (3) obtains after the modification.
The present invention is take phenol-amine resin as initiator, and take alkali as catalyzer, initiation oxyethane, propylene oxide carry out block copolymerization, obtain racemosus shape polyethers.This polyethers can use as emulsion splitter separately, is made into 50% methanol solution, and thin up is to aequum.Continue again gained polyethers and linking agent silicone oil to be reacted, make crosslinked emulsion splitter; Be made into massfraction during use and be 50% methanol solution, thin up is to aequum.
The advantages such as the emulsion splitter of the present invention's preparation has fast, low dosage, environmental protection.Particularly the crosslinked emulsion splitter that makes of the present invention is in the situation of 100mg/L at the emulsion splitter dosage, 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, both has been conducive to improve the security that emulsion splitter uses, and also is conducive to environment protection.
Embodiment
Employed experimental technique is ordinary method if no special instructions among the following embodiment.
Used material, reagent etc. if no special instructions, all can obtain from commercial channels among the following embodiment.
Embodiment 1. polyether demulsification agent A's is synthetic
(1) the initiator phenol-amine resin is synthetic
With the dihydroxyphenyl propane of 25g, adding is opened the stirring intensification and is made the dihydroxyphenyl propane dissolving in the 82.5g tetraethylene pentamine adding 500ml there-necked flask, after dihydroxyphenyl propane dissolves fully, be cooled to 35 ℃, dropping 37.5g massfraction is 36% formaldehyde solution, keeps 30-40 ℃ of temperature, dropwises rear insulation reaction 40min.Add the dimethylbenzene of 72.5g, be warming up to 100-110 ℃.Back flow reaction 2h.Slowly heat up and under refluxad water is taken out of, after all steaming to water, dimethylbenzene is steamed namely get the initiator phenol-amine resin again.
(2) polyether demulsification agent A's is synthetic
Gained initiator phenol-amine resin 1g in the step (1) and potassium hydroxide 1g are added in the autoclave, sealed reactor, start and stir and intensification, when treating that temperature rises to 80 ℃ of left and right sides, with vacuum pump reactor is vacuumized, when vacuumizing about 20 minutes and treat in the still vacuum tightness for-0.1MPa, stop to vacuumize.Continue to stir heat up, when treating that temperature rises to 100 ℃, slowly add the 199g propylene oxide, the control temperature of reaction is at 120-140 ℃, and pressure is at 0.2-0.4MPa, reaction times 3h.React complete after, aging 2.5h is cooled to 100 ℃.133g oxyethane is added reactor, the control temperature of reaction is at 120-140 ℃ again, and pressure is at 0.2-0.4MPa, reaction times 1-3h, react complete after, the 1h that wears out namely gets polyether demulsification agent A.
Be made into first massfraction when polyether demulsification agent A uses and be 50% methanol solution, thin up is to aequum.
Embodiment 2. crosslinked emulsion splitter B's is synthetic
The 10g polyether demulsification agent A of embodiment 1 preparation is added in the 25ml single port bottle, be warming up to 100 ℃ of left and right sides vacuum hydro-extractions.Dewater complete after, add 0.5g MethylethoxylsiliconFluid Fluid and 0.07g oleic acid, Depressor response 30 minutes.Material retrogradation and termination reaction when wire drawing is arranged.The 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 the 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 the 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, thin up is to aequum.
Embodiment 5. polyether demulsification agent E's is synthetic
With embodiment 1(1) the initiator phenol-amine resin 1g of gained and 1.5g potassium hydroxide adds in the autoclave, sealed reactor, start and stir and intensification, when treating that temperature rises to 80 ℃, with vacuum pump reactor is vacuumized, when vacuumizing about 20 minutes and treat in the still vacuum tightness for-0.1Mpa, stop to vacuumize.Continue to stir and heat up, when treating that temperature rises to 100 ℃, slowly add the 299g propylene oxide, temperature of reaction 120-140 ℃, pressure 0.2-0.4MPa, reaction times 3h.React complete rear aging 1h, be cooled to 100 ℃, 199g oxyethane is added, temperature of reaction 120-140 ℃, pressure is at 0.2-0.4MPa, reaction times 2h.React complete rear aging 1h and namely get polyether demulsification agent E.Be made into massfraction during use and be 50% methanol solution, thin up is to aequum.
Embodiment 6. crosslinked emulsion splitter F's is synthetic
The 10g polyether demulsification agent E that embodiment 5 is made adds in the 25ml single port bottle, is warming up to 100 ℃ of left and right sides vacuum hydro-extractions.Dewater complete after, add 0.3g MethylethoxylsiliconFluid Fluid and 0.04g oleic acid, Depressor response 30 minutes.Termination reaction when treating the material retrogradation and wire drawing being arranged.The 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 the 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 the 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, thin up is to aequum.
The emulsion splitter performance evaluation experiment of embodiment 9. embodiment 1-8 preparation
Bohai Bay Oil crude oil is carried out the test of bottle examination method breakdown of emulsion under 65 ℃ of the temperature at the scene, and experimental result is as shown in table 1.
This bottle 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 China National Offshore Oil Corporation (CNOOC) company standard Q/HS 2020-2004.
Concrete experimental procedure is:
Ready crude oil production fluid sample is poured in the dehydration test bottle pipe, and heating in water bath continues constant temperature 15min to homo(io)thermism.
In the dehydration test tube, inject a certain amount of emulsion splitter A-H with syringe).Artificial succusion is adopted in the vibration of dehydration test tube.After screwing bottle cap, the test tube that will dewater is put upside down 2-5 time, slowly after the loosening bottle stopper venting, again screws bottle stopper, and mode is directly vibrated by hand.After the left hand vibration 100 times, slowly after the loosening bottle stopper venting, again screw bottle stopper.Change again right hand vibration 100 times, after fully mixing, loosening bottle stopper, and the test tube that again will dewater places the 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 emulsion splitter of table 1 embodiment 1-8 is to the breakdown of emulsion experimental result of Bohai Bay Oil crude oil
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| CN114890909B (en) * | 2022-03-28 | 2024-01-12 | 黑龙江省瑞庆化工有限公司 | Surfactant for oil displacement, synthesis method and application thereof in oil displacement system |
| CN115261060A (en) * | 2022-08-30 | 2022-11-01 | 克拉玛依市正诚有限公司 | Demulsifier suitable for high-pour-point oil |
| CN116023667A (en) * | 2022-12-28 | 2023-04-28 | 荆州市东泽化工科技有限公司 | Demulsifier and preparation method and application thereof |
| CN116023667B (en) * | 2022-12-28 | 2024-02-20 | 荆州市东泽化工科技有限公司 | Demulsifier and preparation method and application thereof |
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| CN102993434B (en) | 2014-10-22 |
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