CN103965459A - Preparation method of demulsifying agent - Google Patents
Preparation method of demulsifying agent Download PDFInfo
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- CN103965459A CN103965459A CN201410199025.9A CN201410199025A CN103965459A CN 103965459 A CN103965459 A CN 103965459A CN 201410199025 A CN201410199025 A CN 201410199025A CN 103965459 A CN103965459 A CN 103965459A
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Abstract
The invention discloses a preparation method of a demulsifying agent. The preparation method comprises the steps of preheating an initiator through a preheating storage tank, performing stirring and heating reaction on the preheated initiator together with oxirane and epoxy propane in a polymerization kettle, adding epoxy chloropropane for continuously stirring and heating, adding steam and additives for continuously stirring, adding methanol, water and steam for continuously stirring, filtering, emptying the water and the steam, and filtering to obtain the demulsifying agent. The demulsifying agent prepared by adopting the method has the characteristics of low dosage, high demulsifying and dewatering speed, high dewatering quantity, good desalting effect and the like; a dosing process is simple, and the operation is convenient; raw oil subjected to demulsification can meet the requirements of output raw oil.
Description
Technical field
The present invention relates to a kind of emulsion splitter preparation method, belong to petrochemical complex oil field chemical.
Background technology
Because some solids are insoluble in water, when these solids, one or more are present in the aqueous solution in a large number, and under the stirring of waterpower or extrinsic motive, these solids can be present in water with the state of emulsification, form emulsion.This system is unsettled theoretically, if but existed in the situation of some tensio-active agents (soil particle etc.), make emulsified state very serious, even two-phase is difficult to separate, most typical is oil-water mixture in oily water separation and the water oil mixt in sewage disposal, in this two-phase, form more stable water-in-oil or oil-in-water structure, its theoretical basis is " double electrical layers ".
In the case, drop into some medicaments, to destroy stable double electrical layers, and stable emulsion system, thereby reach two objects that are separated.These that use destroy emulsifying effect medicament in order to reach is referred to as emulsion splitter.
Emulsion splitter is a kind of surfactant, and it can make the liquid structure of emulsification shape destroy, to reach the object that is respectively separated and comes in emulsion.Crude oil demulsification refers to and utilizes the chemical action of emulsion splitter that oil and water in the oil-water mixture of emulsification shape are separated, makes it to reach the object of dehydrating of crude oil, to ensure that crude oil exporting contains water quality standard.
Organic phase separates with the effective of water, and the simplest effective ways of one are to adopt emulsion splitter, eliminate emulsification and form the emulsification interface with some strength, reach two and are separated.But different emulsion splitters is different to organic phase breakdown of emulsion ability, the performance of emulsion splitter directly affects two-phase separating effect.In penicillin production process, an important procedure is with organic solvent (as N-BUTYL ACETATE) extracting penicillin from penicillin fermentation liquid, owing to containing the complicated thing of protein, carbohydrate, mycelium etc. in fermented liquid, when extraction, the interface of organic phase and water is unclear, be the emulsion band of some strength, very large on the impact of finished product yield.Must use emulsion splitter breakdown of emulsion for this reason, eliminate emulsion, reach two-phase and effectively separate fast.
In oil field, conventional non-ionic demulsifier mainly contains following several at present:
1. SP type emulsion splitter:
The main ingredient of SP type emulsion splitter is polyoxyethylene polyoxypropylene stearyl alcohol ether, and theoretical construct formula is R (PO) x (EO) y (PO) zH, in formula: EO-polyoxyethylene; PO-polyoxypropylene; R-fatty alcohol; X, y, z-polymerization degree.SP type emulsion splitter outward appearance is faint yellow paste substance, and HLB value is 10 ~ 12, water-soluble.SP type non-ionic demulsifier has good demulsification to paraffinic crude.Its hydrophobic part is made up of carbon 12 ~ 18 hydrocarbon chains, and its hydrophilic group is to form hydrogen bond by the hydroxyl in molecule (OH), ether (O-) and water effect to reach hydrophilic object.Due to hydroxyl, ether wetting ability a little less than, so only carbon 12 ~ 18 hydrocarbon chain hydrophobic groups can not be drawn in water by one or two hydroxyl or ether, must have multiple such hydrophilic groups, just can reach water-soluble object.The molecular weight of non-ionic demulsifier is larger, and molecular chain is longer, and contained hydroxyl and ether are more, and its pulling force is larger, stronger to the breakdown of emulsion ability of crude oil emulsion.The Another reason that SP type emulsion splitter is adapted to paraffinic crude is that paraffinic crude does not contain or seldom containing resin and asphalt, lipophilic surfactant material is less, and relative density is less.To the crude oil containing resin and asphalt higher (or moisture be greater than 20%), the breakdown of emulsion ability of SP type emulsion splitter a little less than, reason is that molecular structure is single, unbranched structure and aromatic structure.
2. AP type emulsion splitter:
AP type emulsion splitter is the polyoxyethylene polyoxypropylene polyethers taking polyethylene polyamine as initiator, the nonionic surface active agent molecular structural formula that is a kind of racemosus type is: D (PO) x (EO) y (PO) z H, in formula: EO-polyoxyethylene; PO-polyoxypropylene; R-fatty alcohol; D-polyethylene polyamine: x, y, z-polymerization degree.
The emulsion splitter of AP type structure is for the breakdown of emulsion of paraffinic crude milk sap, and effect is better than SP type emulsion splitter, and it is more suitable in crude oil water content higher than 20% crude oil demulsification, and can be issued at cold condition the effect of fast emulsion breaking.As SP type emulsion splitter sedimentation breakdown of emulsion in 55 ~ 60 DEG C, 2h, AP type emulsion splitter only need be at sedimentation breakdown of emulsion in 45 ~ 50 DEG C, 1.5h.This is due to due to the constructional feature of AP type emulsion splitter molecule.Initiator polyethylene polyamine has determined the structure formation of molecule: molecular chain length and side chain are many, and hydrophilic ability is higher than the single SP type emulsion splitter of molecular structure.The feature of higly branched chain has determined that AP type emulsion splitter has higher wettability and penetrating quality, in the time of crude oil emulsion breakdown of emulsion, the molecular energy of AP type emulsion splitter is penetrated on oil-water interfacial film rapidly, arrange and occupy more surface-area than the vertical type unimolecular film of SP type emulsion splitter molecule, thereby consumption is few, demulsification is obvious.Such emulsion splitter is that Daqing oil field uses good non-ionic demulsifier at present.
3. AE type emulsion splitter:
AE type emulsion splitter is the polyoxyethylene polyoxypropylene polyethers taking polyethylene polyamine as initiator, is a kind of nonionic surface active agent of racemosus type.Compared with AP type emulsion splitter, difference is that AE type emulsion splitter is a kind of polymkeric substance of two segment types, and its molecule is little, and side chain is short.Molecular structural formula is: D (PO) x (EO) yH, in formula: EO-polyoxyethylene: PO-polyoxypropylene: D-polyethylene polyamine; X, y-polymerization degree.Although the molecule appearance of AE type emulsion splitter and AP type emulsion splitter exists very large difference, a point subconstiuent is identical, just difference to some extent in monomer consumption and polymerization order.
(1) two kind of non-ionic demulsifier in the time that design is synthetic, its, the materials amount difference of tail, the length that produces polymerizable molecular is also different.
(2) molecule of AP type emulsion splitter is two-section type, taking polyethylene polyamine as initiator, form segmented copolymer with polyoxyethylene, polyoxypropylene polymerization: the molecule of AE type emulsion splitter is two-section type, taking polyethylene polyamine as initiator, form two sections of multipolymers with polyoxyethylene, polyoxypropylene polymerization, the molecule of the AP type emulsion splitter of therefore, designing should be longer than the molecule of AE type emulsion splitter.
AE type is the crude oil demulsifier of two sections of multi-brancheds, is adapted to equally the breakdown of emulsion of asphaltic crude milk sap.In crude asphaltic petroleum, the surfactant content of oleophylic is more, and viscous force is stronger, and profit density difference is little, is difficult for breakdown of emulsion.And adopt AE type emulsion splitter de-emulsification speed fast, meanwhile, AE type emulsion splitter is again good paraffin inhibitor and viscosity inhibitor.Due to the multi-branched of its molecule, very easily form small network, make established paraffin monocrystalline in crude oil fall into these networks, hinder the free movement of paraffin single crystal, can not interconnect, form the reticulated structure of paraffin, reduce former oil viscosity and zero pour, prevent that wax crystalline substance is coalescent, thereby reach the object of wax control.
4. AR type emulsion splitter:
The non-ionic demulsifier of AR type emulsion splitter and the new oil-soluble that form poly-by alkyl phenolic resin (AR resin) and polyoxyethylene, polyoxypropylene, HLB value is in 4 ~ 8 left and right, and breakdown of emulsion temperature is low reaches 35 ~ 45 DEG C.Molecular structural formula is: AR (PO) x (EO) y H, in formula: EO-polyoxyethylene; PO-polyoxypropylene; AR-resin; X, y, z-polymerization degree.AR resin, in the process of synthetic emulsion splitter, had both played initiator, entered again in the molecule of emulsion splitter and became oleophilic group.The feature of AR type emulsion splitter is: molecule is little, there are good dissolving, diffusion, osmotic effect higher than 5 DEG C in the situation that at former oil freezing point, impel emulsification water droplet flocculation, coalescent, can be below 45 DEG C, more than water ratio, the water in the crude oil of 50 % ~ 70 % is deviate from 80 % in 45 min, this be SP type, AP type emulsion splitter can not be than.
Existing emulsion splitter can not solve high-hydrogen sulfide crude oil and the former wet goods breaking emulsion and dewatering of high salinity, and not only chemical feeding quantity is high, and processed in units cost is high, and crude oil is de-rear moisture higher, and saliferous is higher, does not often reach outer output oil requirement.Affect crude oil following process.
Summary of the invention
The features such as the technical issues that need to address of the present invention are just to overcome the defect of prior art, and a kind of emulsion splitter preparation method is provided, and emulsion splitter chemical feeding quantity prepared by the present invention is low, and breaking emulsion and dewatering speed is fast, and dehydrating amount is high, and desalting effect is good.Dosing technique is simple, easy to operate.Can meet outer output oil requirement through breakdown of emulsion crude oil after treatment.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of emulsion splitter preparation method, described method is:
Initiator 2.5kg constant temperature 30 minutes after pre-hot tank is preheated to 110 DEG C, add additive 4.2kg initiation reaction, progressively pass into propylene oxide 600kg, oxyethane 400kg, in polymeric kettle under the condition that is not less than 120 DEG C stirring reaction 2h, add again epoxy chloropropane 25kg to continue to stir, thermostatically heating 1.5h at 120 DEG C, after dry agent has been reacted, enter in work in-process tank and be cooled to 50～60 DEG C, then to do agent: the ratio of methyl alcohol: water=6:3:1, adds methyl alcohol, water to continue to stir, filter, unwatering, filters again, obtains emulsion splitter.Wherein steam act as the temperature that constant temperature keeps half product, to guarantee half-finished mobility.
In the present invention, described initiator is propylene glycol or alkyl phenolic resin.
In the present invention, described additive is potassium hydroxide.
The features such as emulsion splitter chemical feeding quantity prepared by the present invention is low, and breaking emulsion and dewatering speed is fast, and dehydrating amount is high, and desalting effect is good.Dosing technique is simple, easy to operate.Can meet outer output oil requirement through breakdown of emulsion crude oil after treatment.
The present invention has prepared the emulsion splitter that a kind of oil development easy to use, that effect remarkable, processed in units cost is low is used, and this product is mainly used in Tahe heavy oil section, and being applicable to density is 0.93g/cm
3-0.98 g/cm
3, viscosity is not more than the crude oil of 5000mPaS.
Beneficial effect of the present invention is:
Emulsion splitter prepared by the present invention is applicable to sulfide hydrogen crude oil and the former wet goods breaking emulsion and dewatering of high salinity, and chemical feeding quantity is low, does not affect crude oil following process.The features such as breaking emulsion and dewatering effect is high, and desalting effect is good.Dosing technique is simple, easy to operate.Can meet outer output oil requirement through breakdown of emulsion crude oil after treatment.
Embodiment
In embodiment, all raw materials are industrial goods below, require purity to be not less than 96%, require to produce in process of production in strict accordance with formula.
embodiment 1
Initiator propylene glycol 2.5kg constant temperature 30 minutes after pre-hot tank is preheated to 110 DEG C, add additive potassium hydroxide 3kg initiation reaction, progressively pass into propylene oxide 550kg, oxyethane 450kg, in polymeric kettle under the condition that is not less than 120 DEG C stirring reaction 2h, add again epoxy chloropropane 20kg to continue to stir, thermostatically heating 1.5h at 120 DEG C, after dry agent has been reacted, enter in work in-process tank and be cooled to 50～60 DEG C, again to do agent: the ratio of methyl alcohol: water=6:2:2, add methyl alcohol, water continues to stir, filter, unwatering, again filter, obtain emulsion splitter, wherein steam act as the temperature that constant temperature keeps half product, to guarantee half-finished mobility.
embodiment 2
Initiator alkyl phenolic resin 2.5kg constant temperature 30 minutes after pre-hot tank is preheated to 110 DEG C, add additive potassium hydroxide 3kg initiation reaction, progressively pass into propylene oxide 550kg, oxyethane 450kg, in polymeric kettle under the condition that is not less than 120 DEG C stirring reaction 2h, add again epoxy chloropropane 20kg to continue to stir, thermostatically heating 1.5h at 120 DEG C, after dry agent has been reacted, enter in work in-process tank and be cooled to 50～60 DEG C, again to do agent: the ratio of methyl alcohol: water=6:2:2, add methyl alcohol, water continues to stir, filter, unwatering, again filter, obtain emulsion splitter, wherein steam act as the temperature that constant temperature keeps half product, to guarantee half-finished mobility.
embodiment 3
Dry agent: 1.5 parts of propylene glycol, 1.5 parts of alkyl phenolic resins, oxyethane is 3 parts, 4 parts of propylene oxide, 0.2 part of epoxy chloropropane.
Finished product: dry agent: methyl alcohol: water=6:2:2.
embodiment 4
Dry agent: 1 part of propylene glycol, 2 parts of alkyl phenolic resins, oxyethane is 3 parts, 4 parts of propylene oxide, 0.2 part of epoxy chloropropane.
Finished product: dry agent: methyl alcohol: water=6:2:2.
embodiment 5
Dry agent: 1.5 parts of propylene glycol, 1.5 parts of alkyl phenolic resins, oxyethane is 2 parts, 5 parts of propylene oxide, 0.2 part of epoxy chloropropane.
Finished product: dry agent: methyl alcohol: water=6:3.5:0.5.
embodiment 6
Dry agent: 1 part of propylene glycol, 2 parts of alkyl phenolic resins, oxyethane is 3 parts, 4 parts of propylene oxide, 0.2 part of epoxy chloropropane.
Finished product: dry agent: methyl alcohol: water=6:3:1.
Taking propylene glycol and alkyl phenolic resin as the synthetic rare polyoxypropylene propylene glycol of the polyoxy second emulsion splitter general formula of initiator as follows:
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 (3)
1. an emulsion splitter preparation method, is characterized in that, described method is:
Initiator 2-3kg constant temperature 30 minutes after pre-hot tank is preheated to 110 DEG C, add additive 3kg initiation reaction, progressively pass into propylene oxide 550kg, oxyethane 450kg, in polymeric kettle under the condition that is not less than 120 DEG C stirring reaction 2h, add again epoxy chloropropane 20kg to continue to stir, thermostatically heating 1.5h at 120 DEG C, after dry agent has been reacted, enter in work in-process tank and be cooled to 50～60 DEG C, then to do agent: the weight ratio of methyl alcohol: water=6:2:2, adds methyl alcohol, water to continue to stir, filter, unwatering, filters again, obtains emulsion splitter; Wherein steam act as the temperature that constant temperature keeps half product, to guarantee half-finished mobility.
2. emulsion splitter preparation method as claimed in claim 1, is characterized in that, described initiator is propylene glycol or alkyl phenolic resin.
3. emulsion splitter preparation method as claimed in claim 2, is characterized in that, described additive is potassium hydroxide.
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| CN201410199025.9A CN103965459A (en) | 2014-05-13 | 2014-05-13 | Preparation method of demulsifying agent |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105527366A (en) * | 2015-12-01 | 2016-04-27 | 赵林萍 | Detection method for antibiotic residues in feeds |
| CN105527367A (en) * | 2015-12-01 | 2016-04-27 | 郑州中道生物技术有限公司 | Detection method for antibiotic residues in meat products |
| CN105622918A (en) * | 2014-10-28 | 2016-06-01 | 中国石油化工股份有限公司 | Polymer, and preparation method and use thereof |
| CN106947517A (en) * | 2017-04-21 | 2017-07-14 | 四川省广汉市阜康化工科技开发有限公司 | A kind of oil-soluble condensate demulsifier and preparation method thereof |
| CN107722257A (en) * | 2017-09-28 | 2018-02-23 | 句容宁武高新技术发展有限公司 | One kind is applied to high water-content crude oil demulsifier and preparation method thereof |
| CN109652116A (en) * | 2018-10-18 | 2019-04-19 | 东营施普瑞石油工程技术有限公司 | Crude oil Produced Liquid low temperature dewatering demulsifier and preparation method thereof |
| CN112807748A (en) * | 2019-11-15 | 2021-05-18 | 佛山市江河化工有限公司 | Environment-friendly deoiling agent |
| CN115449394A (en) * | 2021-06-09 | 2022-12-09 | 中国石油天然气股份有限公司 | Demulsifier and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105622918A (en) * | 2014-10-28 | 2016-06-01 | 中国石油化工股份有限公司 | Polymer, and preparation method and use thereof |
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| CN105527366A (en) * | 2015-12-01 | 2016-04-27 | 赵林萍 | Detection method for antibiotic residues in feeds |
| CN105527367A (en) * | 2015-12-01 | 2016-04-27 | 郑州中道生物技术有限公司 | Detection method for antibiotic residues in meat products |
| CN106947517A (en) * | 2017-04-21 | 2017-07-14 | 四川省广汉市阜康化工科技开发有限公司 | A kind of oil-soluble condensate demulsifier and preparation method thereof |
| CN107722257A (en) * | 2017-09-28 | 2018-02-23 | 句容宁武高新技术发展有限公司 | One kind is applied to high water-content crude oil demulsifier and preparation method thereof |
| CN109652116A (en) * | 2018-10-18 | 2019-04-19 | 东营施普瑞石油工程技术有限公司 | Crude oil Produced Liquid low temperature dewatering demulsifier and preparation method thereof |
| CN112807748A (en) * | 2019-11-15 | 2021-05-18 | 佛山市江河化工有限公司 | Environment-friendly deoiling agent |
| CN115449394A (en) * | 2021-06-09 | 2022-12-09 | 中国石油天然气股份有限公司 | Demulsifier and preparation method thereof |
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