CN103865070A - Preparation method of super heavy oil refined oil-soluble efficient electro-desalting demulsifying agent - Google Patents
Preparation method of super heavy oil refined oil-soluble efficient electro-desalting demulsifying agent Download PDFInfo
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- CN103865070A CN103865070A CN201410081712.0A CN201410081712A CN103865070A CN 103865070 A CN103865070 A CN 103865070A CN 201410081712 A CN201410081712 A CN 201410081712A CN 103865070 A CN103865070 A CN 103865070A
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Abstract
The invention discloses a preparation method of a super heavy oil refined oil-soluble efficient electro-desalting demulsifying agent, which comprises the steps of synthesizing phenol amine resin; performing condensation reaction of the phenol amine resin with epoxy propane and ethylene oxide sequentially to obtain block polyether; synthesizing thermoplastic phenolic resin by use of phenol, hydrochloric acid and formaldehyde; finally, performing a phenolic resin graft modification reaction between the obtained thermoplastic phenolic resin and the block polyether to obtain a product of super heavy oil refined oil-soluble efficient electro-desalting demulsifying agent. By adopting the preparation method disclosed by the invention, the oil-soluble efficient electro-desalting demulsifying agent can be efficiently prepared, the production cost is reduced, and the utilization rate of raw materials is improved; the demulsifying agent produced by the method can remarkably increase the desalting and dehydration speed of super heavy oil, saves the limited time and can effectively compensate for the shortcomings of a super heavy oil treatment process of a processing device.
Description
Technical field
The present invention relates to a kind of preparation method who refines oil emulsion splitter, be specifically related to a kind of preparation method of super viscous crude refining oil soluble efficient electric desalination emulsion splitter, belong to petrochemical industry.
Background technology
Along with the super viscous crude of Karamay oilfield is developed on a large scale, output improves constantly, and the refining of such high viscous crude processing is by the independent refining up till now of the low sticky crude oil mixing system in past.In crude oil desalting, dehydration, because this quasi-oil colloid, asphalt content are high, viscosity of crude is large, thereby, longer to such high viscous crude dewatering and desalting time.
Common water-soluble electric desalting emulsion splitter is injected in treatment system by returning water mixing, stage rests in the discontinuous phase water of milk sap in advance, later stage enters the water-oil interface of saline sewage by external phase crude oil, implement breaking emulsion and dewatering, desalination, visible, its process enters oil phase by water, then is adsorbed onto water-oil interface, diffusion time is longer, and the desalting and dewatering treatment time is longer.
Due to the water-soluble feature of such emulsion splitter self, velocity of diffusion resistance in oily external phase is larger, viscosity of crude is large, further increase the diffusional resistance of such medicament, velocity of diffusion is slow, the dewatering and desalting time needing is longer, its process is entered the long-time process of oil-continuous phase by discontinuous water in addition, make water-soluble electric desalting emulsion splitter in the technology of electric de-salting device in existing shorter treatment time, such medicament can not meet the process for processing of device to super viscous crude, the super viscous crude refining of Development and Production oil soluble efficient electric desalination emulsion splitter, significantly improve super viscous crude desalting and dewatering speed, save the limited time, can effectively make up processing unit (plant) and process the deficiency of super viscous crude process aspect.
Summary of the invention
The technical issues that need to address of the present invention are just to overcome the defect of prior art, a kind of preparation method of super viscous crude refining oil soluble efficient electric desalination emulsion splitter is provided, the method can efficiently be prepared oil soluble efficient electric desalination emulsion splitter, reduce production costs, improve raw material availability, the emulsion splitter that adopts the method to produce can significantly improve super viscous crude desalting and dewatering speed, saves the limited time, can effectively make up the deficiency of the super viscous crude process aspect of processing unit (plant) processing.
For addressing the above problem, the present invention adopts technical scheme to be: a kind of preparation method of super viscous crude refining oil soluble efficient electric desalination emulsion splitter, this preparation method's step is: synthetic phenol-amine resin, phenol-amine resin is successively carried out to condensation reaction with propylene oxide and oxyethane and obtain block polyether, re-use phenol, hydrochloric acid and formaldehyde synthetic thermoplastic resol, finally gained novolac resin and block polyether are carried out to resol graft modification reaction, obtain super viscous crude refining oil soluble efficient electric desalination demulsifier product.
The present invention is in order to realize the efficient preparation of oil soluble efficient electric desalination emulsion splitter, and preferably technical scheme has, and this preparation method's concrete steps are:
(1) phenol-amine resin is synthetic: diphenylol propane, tetraethylene pentamine and dimethylbenzene are joined in the reactor with whipping appts, drip formaldehyde solution after being heated to 50～70 DEG C, maintain the temperature under 60～85 DEG C of conditions and carry out polyreaction; Then be warming up to 160～180 DEG C of xylene solvent and moisture of sloughing under reduced pressure in reactant, condensation obtains the phenol-amine resin of reddish-brown;
(2) block polyether is synthetic: gained phenol-amine resin in step (1) and catalyzer are joined in the first reactor of airtight nitrogen protection, stir, be warming up to 135～145 DEG C, adjusting pressure range is 0.3～0.35MPa, slowly add propylene oxide to carry out polyreaction to the first reactor, while no longer variation to the first reactor pressure, reaction finishes; Then be cooled to 125～135 DEG C, adjusting pressure range is 0.2～0.25MPa, in the first reactor, slowly adds oxyethane to carry out polyreaction, and in the time that the first reactor pressure no longer changes, reaction finishes, and obtains block polyether;
(3) novolac resin is synthetic: phenol, hydrochloric acid are joined in the second reactor with whipping appts, be warming up to 50～60 DEG C, then in the second reactor, drip formaldehyde solution, maintain the temperature under 60～85 DEG C of conditions and carry out polyreaction, polymerization process is by muddiness to the gluey state of oyster white, and then cooling gradually, reduces speed of response, the white jelly that obtains natural subsidence, white jelly is sloughed moisture and is obtained white novolac resin;
(4) resol graft modification reaction: add the 3rd reactor to carry out condensation reaction under acidic conditions the block polyether of the novolac resin of step (3) gained and step (2) gained, condensation reaction comprises the even collecting process of esterification process and high fat thing; After reaction finishes to add oil-dissolving solvent in backward products therefrom and stirs, obtain super viscous crude and refine oil soluble efficient electric desalination demulsifier product.
The present invention is in order to improve the effect of resol graft modification reaction, improve the quality of products, preferably technical scheme also has, the working method of step (4) resol graft modification reaction is: by step (2) gained block polyether, step (3) gained novolac resin, the catalyzer vitriol oil adds in the 3rd reactor, stirring is warming up to 80～95 DEG C, reflux dewatering reaction obtains reaction product in 2～3 hours till Separation of Water no longer increases, then be cooled to 50～60 DEG C, in reaction product, add oil-dissolving solvent, after stirring, obtain super viscous crude refining oil soluble efficient electric desalination demulsifier product.
The present invention is in order to improve resol graft modification reaction efficiency, and preferably technical scheme also has, catalyzer in step (4): novolac resin: the weight proportion that feeds intake of block polyether is for (0.2～0.3): (80～95): (5～20).
The present invention is in order to improve efficiency and the raw material availability of phenol-amine resin building-up reactions, preferably technical scheme also has, weight proportion in step (1) between diphenylol propane, tetraethylene pentamine, formaldehyde solution three is 1:(2～10): (0.5～5), the weight percent concentration of formaldehyde solution is 33%.
The present invention, in order to improve the raw material availability of block polyether building-up reactions, reduces production costs, and preferably technical scheme also has, and in step (2), the mass ratio that adds of phenol-amine resin, propylene oxide and oxyethane is 1:(100～150): (15～25).
The present invention is in order to improve the speed of reaction of novolac resin building-up reactions, improve raw material availability, preferably technical scheme also has, and in step (3), the weight ratio of phenol, formaldehyde solution add-on is 1:(2～6), the weight percent concentration of formaldehyde solution is 33%.
Advantage of the present invention and beneficial effect are: the emulsion splitter that preparation method of the present invention produces can significantly improve super viscous crude desalting and dewatering speed, saves the limited time, can effectively make up the deficiency of the super viscous crude process aspect of processing unit (plant) processing; Preparation method of the present invention can highly effective reaction, and the utilization ratio of raw material is higher, has reduced production cost, has reduced material loss; Preparation method of the present invention has stronger operability, can realize large-scale production application.
Embodiment
The following example will further illustrate the present invention.
embodiment 1
It is the preparation method of super viscous crude refining oil soluble efficient electric desalination emulsion splitter that the present invention adopts technical scheme, and this preparation method's concrete steps are:
(1) phenol-amine resin is synthetic: diphenylol propane, tetraethylene pentamine and dimethylbenzene are joined in the reactor with whipping appts, drip formaldehyde solution after being heated to 55 DEG C, maintain the temperature under 65 DEG C of conditions and carry out polyreaction; Then be warming up to 164 DEG C of xylene solvent and moisture of sloughing under reduced pressure in reactant, condensation obtains the phenol-amine resin of reddish-brown; Wherein the weight proportion between diphenylol propane, tetraethylene pentamine, formaldehyde solution three is 1:4:2, and the weight percent concentration of formaldehyde solution is 33%.
(2) block polyether is synthetic: gained phenol-amine resin in step (1) and catalyzer are joined in the first reactor of airtight nitrogen protection, stir, be warming up to 138 DEG C, adjusting pressure is 0.3MPa, slowly add propylene oxide to carry out polyreaction to the first reactor, while no longer variation to the first reactor pressure, reaction finishes; Then be cooled to 125 DEG C, adjusting pressure is 0.2MPa, in the first reactor, slowly adds oxyethane to carry out polyreaction, and in the time that the first reactor pressure no longer changes, reaction finishes, and obtains block polyether; Wherein phenol-amine resin, propylene oxide and oxyethane add mass ratio for 1:110:17.
(3) novolac resin is synthetic: phenol, hydrochloric acid are joined in the second reactor with whipping appts, be warming up to 52 DEG C, then in the second reactor, drip formaldehyde solution, maintain the temperature under 68 DEG C of conditions and carry out polyreaction, polymerization process is by muddiness to the gluey state of oyster white, and then cooling gradually, reduces speed of response, the white jelly that obtains natural subsidence, white jelly is sloughed moisture and is obtained white novolac resin; Wherein the weight ratio of phenol, formaldehyde solution add-on is 1:3, and the weight percent concentration of formaldehyde solution is 33%.
(4) resol graft modification reaction: step (2) gained block polyether, step (3) gained novolac resin, the catalyzer vitriol oil are added in the 3rd reactor, stirring is warming up to 82 DEG C, reflux dewatering reaction obtains reaction product in 2 hours till Separation of Water no longer increases, then be cooled to 50 DEG C, in reaction product, add oil-dissolving solvent, after stirring, obtain super viscous crude refining oil soluble efficient electric desalination demulsifier product.Wherein catalyzer: novolac resin: the weight proportion that feeds intake of block polyether is 0.2:80:9.
embodiment 2
The present invention, in order further to enhance productivity, reduces raw materials for production cost, improves raw material availability, and preferably embodiment also has, and preparation method's operation steps of super viscous crude refining oil soluble efficient electric desalination emulsion splitter is:
(1) phenol-amine resin is synthetic: diphenylol propane, tetraethylene pentamine and dimethylbenzene are joined in the reactor with whipping appts, drip formaldehyde solution after being heated to 67 DEG C, maintain the temperature under 82 DEG C of conditions and carry out polyreaction; Then be warming up to 175 DEG C of xylene solvent and moisture of sloughing under reduced pressure in reactant, condensation obtains the phenol-amine resin of reddish-brown; Wherein the weight proportion between diphenylol propane, tetraethylene pentamine, formaldehyde solution three is 1:9:5, and the weight percent concentration of formaldehyde solution is 33%.
(2) block polyether is synthetic: gained phenol-amine resin in step (1) and catalyzer are joined in the first reactor of airtight nitrogen protection, stir, be warming up to 145 DEG C, adjusting pressure is 0.35MPa, slowly add propylene oxide to carry out polyreaction to the first reactor, while no longer variation to the first reactor pressure, reaction finishes; Then be cooled to 135 DEG C, adjusting pressure is 0.25MPa, in the first reactor, slowly adds oxyethane to carry out polyreaction, and in the time that the first reactor pressure no longer changes, reaction finishes, and obtains block polyether; Wherein phenol-amine resin, propylene oxide and oxyethane add mass ratio for 1:150:25.
(3) novolac resin is synthetic: phenol, hydrochloric acid are joined in the second reactor with whipping appts, be warming up to 60 DEG C, then in the second reactor, drip formaldehyde solution, maintain the temperature under 85 DEG C of conditions and carry out polyreaction, polymerization process is by muddiness to the gluey state of oyster white, and then cooling gradually, reduces speed of response, the white jelly that obtains natural subsidence, white jelly is sloughed moisture and is obtained white novolac resin; Wherein the weight ratio of phenol, formaldehyde solution add-on is 1:5, and the weight percent concentration of formaldehyde solution is 33%.
(4) resol graft modification reaction: step (2) gained block polyether, step (3) gained novolac resin, the catalyzer vitriol oil are added in the 3rd reactor, stirring is warming up to 95 DEG C, reflux dewatering reaction obtains reaction product in 3 hours till Separation of Water no longer increases, then be cooled to 60 DEG C, in reaction product, add oil-dissolving solvent, after stirring, obtain super viscous crude refining oil soluble efficient electric desalination demulsifier product.Wherein catalyzer: novolac resin: the weight proportion that feeds intake of block polyether is 0.3:95:20.
Finally it should be noted that: obviously, above-described embodiment is only for example of the present invention is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all embodiments.And the apparent variation of being amplified out thus or variation are still among protection scope of the present invention.
Claims (7)
1. the preparation method of a super viscous crude refining oil soluble efficient electric desalination emulsion splitter, it is characterized in that, this preparation method's step is: synthetic phenol-amine resin, phenol-amine resin is successively carried out to condensation reaction with propylene oxide and oxyethane and obtain block polyether, re-use phenol, hydrochloric acid and formaldehyde synthetic thermoplastic resol, finally gained novolac resin and block polyether are carried out to resol graft modification reaction, obtain super viscous crude refining oil soluble efficient electric desalination demulsifier product.
2. the preparation method of super viscous crude refining oil soluble efficient electric desalination emulsion splitter as claimed in claim 1, is characterized in that, this preparation method's concrete steps are:
(1) phenol-amine resin is synthetic: diphenylol propane, tetraethylene pentamine and dimethylbenzene are joined in the reactor with whipping appts, drip formaldehyde solution after being heated to 50～70 DEG C, maintain the temperature under 60～85 DEG C of conditions and carry out polyreaction; Then be warming up to 160～180 DEG C of xylene solvent and moisture of sloughing under reduced pressure in reactant, condensation obtains the phenol-amine resin of reddish-brown;
(2) block polyether is synthetic: gained phenol-amine resin in step (1) and catalyzer are joined in the first reactor of airtight nitrogen protection, stir, be warming up to 135～145 DEG C, adjusting pressure range is 0.3～0.35MPa, slowly add propylene oxide to carry out polyreaction to the first reactor, while no longer variation to the first reactor pressure, reaction finishes; Then be cooled to 125～135 DEG C, adjusting pressure range is 0.2～0.25MPa, in the first reactor, slowly adds oxyethane to carry out polyreaction, and in the time that the first reactor pressure no longer changes, reaction finishes, and obtains block polyether;
(3) novolac resin is synthetic: phenol, hydrochloric acid are joined in the second reactor with whipping appts, be warming up to 50～60 DEG C, then in the second reactor, drip formaldehyde solution, maintain the temperature under 60～85 DEG C of conditions and carry out polyreaction, polymerization process is by muddiness to the gluey state of oyster white, and then cooling gradually, reduces speed of response, the white jelly that obtains natural subsidence, white jelly is sloughed moisture and is obtained white novolac resin;
(4) resol graft modification reaction: add the 3rd reactor to carry out condensation reaction under acidic conditions the block polyether of the novolac resin of step (3) gained and step (2) gained, condensation reaction comprises the even collecting process of esterification process and high fat thing; After reaction finishes to add oil-dissolving solvent in backward products therefrom and stirs, obtain super viscous crude and refine oil soluble efficient electric desalination demulsifier product.
3. the preparation method of super viscous crude refining oil soluble efficient electric desalination emulsion splitter as claimed in claim 2, it is characterized in that, the working method of step (4) resol graft modification reaction is: by step (2) gained block polyether, step (3) gained novolac resin, the catalyzer vitriol oil adds in the 3rd reactor, stirring is warming up to 80～95 DEG C, reflux dewatering reaction obtains reaction product in 2～3 hours till Separation of Water no longer increases, then be cooled to 50～60 DEG C, in reaction product, add oil-dissolving solvent, after stirring, obtain super viscous crude refining oil soluble efficient electric desalination demulsifier product.
4. the preparation method of super viscous crude refining oil soluble efficient electric desalination emulsion splitter as claimed in claim 3, it is characterized in that catalyzer in step (4): novolac resin: the weight proportion that feeds intake of block polyether is for (0.2～0.3): (80～95): (5～20).
5. the preparation method of super viscous crude refining oil soluble efficient electric desalination emulsion splitter as claimed in claim 4, it is characterized in that, weight proportion in step (1) between diphenylol propane, tetraethylene pentamine, formaldehyde solution three is 1:(2～10): (0.5～5), the weight percent concentration of formaldehyde solution is 33%.
6. the preparation method of super viscous crude refining oil soluble efficient electric desalination emulsion splitter as claimed in claim 5, is characterized in that, in step (2), the mass ratio that adds of phenol-amine resin, propylene oxide and oxyethane is 1:(100～150): (15～25).
7. the preparation method of super viscous crude refining oil soluble efficient electric desalination emulsion splitter as claimed in claim 6, is characterized in that, in step (3), the weight ratio of phenol, formaldehyde solution add-on is 1:(2～6), the weight percent concentration of formaldehyde solution is 33%.
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Cited By (3)
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| CN105885029A (en) * | 2016-05-07 | 2016-08-24 | 中国海洋石油总公司 | Polyether demulsifying agent based on hydramine-modified phenolic resin and synthesizing method thereof |
| CN110343545A (en) * | 2019-06-28 | 2019-10-18 | 山东德仕石油工程集团股份有限公司 | A kind of figure crude oil demulsifier and its preparation method and application |
| CN114644742A (en) * | 2022-04-22 | 2022-06-21 | 彤程电子材料(镇江)有限公司 | Preparation process of high-uniformity phenolic resin |
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