CN102321257B - Low-temperature demulsifier of thickened oil and preparation method thereof - Google Patents
Low-temperature demulsifier of thickened oil and preparation method thereof Download PDFInfo
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- CN102321257B CN102321257B CN 201110151087 CN201110151087A CN102321257B CN 102321257 B CN102321257 B CN 102321257B CN 201110151087 CN201110151087 CN 201110151087 CN 201110151087 A CN201110151087 A CN 201110151087A CN 102321257 B CN102321257 B CN 102321257B
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Abstract
The invention discloses a low-temperature demulsifier of thickened oil and a preparation method thereof. The preparation method comprises the following step of: in the presence of cross-linking agent and solvent, cross-linking mannitol polyether compound with polyamide-amide polyether compound to obtain the demulsifier. The demulsifier has good dewatering effect to thickened oil at low temperature, can be widely used in the fields of oil extraction and petroleum refining.
Description
Technical field
The present invention relates to a kind of viscous oil emulsion low-temperature demulsifying agent and preparation method thereof, belong to the Petroleum Processing Technology field.
Background technology
Oil is a kind of non-renewable natural resources, occupies very important status in national economy and daily life.In today of world's rapid economic development, human more and more heavier for the dependency of the product of being produced take oil as basic raw material.Oil field all over the world nearly all will experience moisture development stage, and global crude oil production fluid has about 80% to be that form with milk sap exists.
Crude oil water containing forms milk sap can make viscosity enlarge markedly, thereby cause the consumption of course of conveying medium power to increase, crude oil water containing can make total liquid measure increase when Oil extraction simultaneously, reduce the utilization ratio of pipeline and equipment, and cause the corrosion of pipeline and equipment, fouling is blocked, more seriously cause the poisoning of catalyzer, the oil refining expense is increased, so the dehydration of crude oil is indispensable step in crude production and the course of processing, crude oil is defeated outside before must to carry out breaking emulsion and dewatering.Defeated with in the chemical in oil production and collection, emulsion splitter is as a kind of important oilfield chemical auxiliary, and consumption is maximum.
Natural surface active agent plays a major role in the stability of crude oil emulsion.Surfactant mainly contains bituminous matter and colloid two classes in the crude oil.The characteristics that viscous crude has bituminous matter and gum level is high, relative density is large, viscosity is high.Bituminous matter in the viscous crude has take aromatic ring structure as main macromolecular structure, and the macromole of this special construction has very strong polarity, very easily is adsorbed on the water-oil interface, forms highly stable milk sap.For a long time, there are the characteristics such as dosage is large, dehydration temperaturre is high, dewatering time is long in heavy oil dehydration technique, has had a strong impact on viscous oil recovery and outer defeated.
Summary of the invention
The purpose of this invention is to provide a kind of emulsion splitter that at low temperatures viscous oil emulsion is had good breakdown of emulsion ability and preparation method thereof.
The preparation method of heavy oil low-temperature demulsifier provided by the invention comprises the steps: that N.F,USP MANNITOL polyether compound and polyamide-amide polyether compound carry out crosslinking reaction and namely get described emulsion splitter under the condition of linking agent and solvent existence.
Among the above-mentioned preparation method, described linking agent can be in oxalyl chloride, Adipoyl Chloride, tolylene diisocyanate and the isophorone diisocyanate any; Described solvent can be in toluene and the dimethylbenzene at least a.
Among the above-mentioned preparation method, described N.F,USP MANNITOL polyether compound can prepare according to the method that comprises the steps: under the condition of pyridine and basic cpd existence, N.F,USP MANNITOL and epoxy compounds carry out alkoxylation and namely get described N.F,USP MANNITOL polyether compound; Described epoxy compounds can be in propylene oxide and the oxyethane at least a.
Among the above-mentioned preparation method, described basic cpd can be in potassium hydroxide, sodium hydroxide and the sodium ethylate at least a.
Among the above-mentioned preparation method, the temperature of described alkoxylation can be 120 ℃-140 ℃, specifically can be 120 ℃, 130 ℃ or 140 ℃; Time can be 2 hours-12 hours, specifically can be 9 hours or 12 hours; Pressure can be 0.2MPa-0.8MPa, specifically can be 0.2MPa, 0.3MPa or 0.4MPa.
Among the above-mentioned preparation method, the ratio of quality and the number of copies of described N.F,USP MANNITOL, pyridine, basic cpd, epoxy compounds can be (0.5-5): (1-10): (0.5-5): (50-200), specifically can be 0.5: 5: 0.5: 220,1: 5: 1: 130 or 2: 8: 1: 120.
Among the above-mentioned preparation method, the temperature of described crosslinking reaction can be 0 ℃-50 ℃, specifically can be 0 ℃, 10 ℃, 20 ℃ or 30 ℃; Time can be 30 minutes-120 minutes, specifically can be 60 minutes.
Among the above-mentioned preparation method, the ratio of quality and the number of copies of described N.F,USP MANNITOL polyether compound, polyamide-amide polyether compound, solvent and linking agent can be (5-20): (10-30): (40-60): (1-5), specifically can be 16: 16: 40: 4,10: 20: 60: 2 or 10: 30: 50: 1.
Among the above-mentioned preparation method, described polyamide-amide polyether compound can be shown in compound shown in compound shown in the formula (I), the formula (II) and the formula (III) at least a in the compound; In formula (I), formula (II) and the formula (III),
Representative-CH
2CH
2CONHCH
2CH
2-, PO represents isopropoxy, EO represents oxyethyl group, x is the number of 10-200, specifically can be 30-127,80-132,30,44,80,127 or 132, y be the number of 5-100, specifically can be 10-58,30-58,10,20,30,56 or 58;
Emulsion splitter provided by the invention has strong interfacial activity and penetrating power, can arrive rapidly water-oil interface, replace interface active agent, form unsettled oil-water interfacial film, at low temperatures viscous oil emulsion is had good breakdown of emulsion ability, can be widely used in the fields such as Oil extraction, refining of petroleum.
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.
The polyether compound of polyamide-amide polyether compound shown in used formula (I), formula (II) and the formula (III) for being obtained through alkoxylation by polyamide-amide compound and epoxy compounds among the following embodiment of the present invention, it can prepare according to the method for record in the Chinese invention patent application 200710176351.8.Concrete preparation method is: (1) quadrol and methyl acrylate carry out the Michael addition reaction and obtain carbonate a, and this addition reaction at room temperature is swift in response, and have very high selectivity; (2) the carbonate a that obtains of step (1) at room temperature obtains 1.0 PAMAMs (this sentences Algebraic Expression polyamide-amide bulk of molecule, every can increase for 1 generation through above-mentioned steps (1) and step (2) two-step reaction molecule) with excessive reacting ethylenediamine.Constantly repeat the polyamide-amide that above-mentioned steps (1) and step (2) obtain the different algebraically that relative molecular mass progressively increases; (3) polyamide-amide that step (2) is obtained and catalyzer (potassium hydroxide, sodium hydroxide or sodium ethylate) add autoclave, when being warming up to 100 ℃, slowly add propylene oxide, the control temperature is at 120-140 ℃, and pressure is 0.2-0.4MPa, reacts 2-5 hour, be cooled to 100 ℃, and then oxyethane added reactor, with step alkoxylation same reaction conditions under continue again reaction 2-5 hour, with in the phosphoric acid with after namely get described polyether compound.
Wherein, 1.0 PAMAMs and propylene oxide and oxyethane obtain polyamide-amide polyethers shown in the formula (I) through alkoxylation; 2.0 PAMAM and propylene oxide and oxyethane obtain polyamide-amide polyethers shown in the formula (II) through alkoxylation; 3.0 PAMAM and propylene oxide and oxyethane obtain polyamide-amide polyethers shown in the formula (III) through alkoxylation.
Embodiment 1, emulsion splitter A's is synthetic
(1) N.F,USP MANNITOL polyethers GLC01's is synthetic
1g N.F,USP MANNITOL, 5g pyridine and 1g KOH are added autoclave; The sealed reaction pot systems, with nitrogen flooding for the air in autoclave, feed chamber and the feed-pipe.Stir and intensification, when temperature rises to 100 ℃, slowly add the 100g propylene oxide, the control temperature of reaction is at 120 ℃, and pressure is at 0.2Mpa; Behind the reaction 6h, aging 1h is cooled to 100 ℃; 30g oxyethane is added feed chamber, is that 120 ℃, pressure are to react under the 0.2Mpa condition in temperature; In this system, the ratio of quality and the number of copies of N.F,USP MANNITOL, pyridine, KOH, epoxy compounds (total mass of propylene oxide and oxyethane) is 1: 5: 1: 130; Behind the reaction 3h, being 120 ℃, pressure in temperature removes pyridine for distillation under the-0.2Mpa condition, and reaction product is neutralized to neutrality with phosphoric acid, namely gets N.F,USP MANNITOL polyethers GLC01.
(2) the polyamide-amide polyethers is synthetic
1g 3.0 PAMAMs and 1g KOH are added autoclave, successively carry out alkoxylation with 150g propylene oxide, 50g oxyethane, reaction product is neutralized to neutrality with phosphoric acid, namely get polyamide-amide polyethers shown in the formula (III), wherein, x is that 127, y is 56.
(3) emulsion splitter A's is synthetic
Polyamide-amide polyethers shown in 10g N.F,USP MANNITOL polyethers GLC01 and the 30g formula (III) is dissolved in the 30g m-xylene, with 1g 2, the 4-tolylene diisocyanate is dissolved in the 20g m-xylene, in this system, the ratio of quality and the number of copies of polyamide-amide polyethers, m-xylene and 2,4 toluene diisocyanate is 10: 30: 50 shown in N.F,USP MANNITOL polyethers GLC01, the formula (III): 1; Under 30 ℃ of normal pressures, slowly drip 2,4 toluene diisocyanate solution to polyethers solution, reaction 1h namely gets emulsion splitter A.
Embodiment 2, emulsion splitter B's is synthetic
(1) N.F,USP MANNITOL polyethers GLC02's is synthetic
0.5g N.F,USP MANNITOL, 5g pyridine and 0.5g KOH are added autoclave; The sealed reaction pot systems, with nitrogen flooding for the air in autoclave, feed chamber and the feed-pipe.Stir and intensification, when temperature rises to 100 ℃, slowly add the 150g propylene oxide, the control temperature of reaction is at 140 ℃, and pressure is at 0.4Mpa; Behind the reaction 8h, aging 1h is cooled to 100 ℃; 70g oxyethane is added feed chamber, is that 140 ℃, pressure are to react under the 0.4Mpa condition in temperature; In this system, the ratio of quality and the number of copies of N.F,USP MANNITOL, pyridine, KOH, epoxy compounds (total mass of propylene oxide and oxyethane) is 0.5: 5: 0.5: 220; Being 120 ℃, pressure in temperature behind the reaction 4h removes pyridine for distillation under the-0.2Mpa condition, and reaction product is neutralized to neutrality with phosphoric acid, namely gets N.F,USP MANNITOL polyethers GLC02.
(2) the polyamide-amide polyethers is synthetic
1g 2.0 PAMAMs and 1g KOH are added autoclave, successively carry out alkoxylation with 150g propylene oxide, 50g oxyethane, reaction product is neutralized to neutrality with phosphoric acid, namely get polyamide-amide polyethers shown in the formula (II), wherein, x is that 132, y is 58.
(3) emulsion splitter B's is synthetic
Polyamide-amide polyethers shown in 20g N.F,USP MANNITOL polyethers GLC02 and the 20g formula (II) is dissolved in the 30g m-xylene, the 5g isophorone diisocyanate is dissolved in the 20g m-xylene; In this system, the ratio of quality and the number of copies of polyamide-amide polyethers, m-xylene and isophorone diisocyanate is 4: 4: 10 shown in N.F,USP MANNITOL polyethers GLC02, the formula (II): 1; Under 20 ℃ of normal pressures, slowly drip isophorone diisocyanate solution to polyethers solution, reaction 1h namely gets emulsion splitter B.
Embodiment 3, emulsion splitter C's is synthetic
Polyamide-amide polyethers shown in 10g N.F,USP MANNITOL polyethers GLC01 and the 30g formula (III) (x is that 80, y is 30) is dissolved in the 30g m-xylene, the 1g Adipoyl Chloride is dissolved in the 20g m-xylene; In this system, the ratio of quality and the number of copies of polyamide-amide polyethers, m-xylene and Adipoyl Chloride is 10: 30: 50 shown in N.F,USP MANNITOL polyethers GLC01, the formula (III): 1; Under 30 ℃ of normal pressures, slowly drip Adipoyl Chloride solution to polyethers solution, reaction 1h namely gets emulsion splitter C.
Embodiment 4, emulsion splitter D's is synthetic
Polyamide-amide polyethers shown in 20g N.F,USP MANNITOL polyethers GLC02 and the 20g formula (II) (x is that 30, y is 10) is dissolved in the 30g m-xylene, the 5g oxalyl chloride is dissolved in the 20g m-xylene; In this system, the ratio of quality and the number of copies of polyamide-amide polyethers, m-xylene and oxalyl chloride is 4: 4: 10 shown in N.F,USP MANNITOL polyethers GLC02, the formula (II): 1; Under 10 ℃ of normal pressures, slowly drip oxalyl chloride solution to polyethers solution, reaction 1h namely gets emulsion splitter D.
Embodiment 5, emulsion splitter E's is synthetic
(1) the N.F,USP MANNITOL polyethers is synthetic
2g N.F,USP MANNITOL, 8g pyridine and 1g KOH are added autoclave; The sealed reaction pot systems, with nitrogen flooding for the air in autoclave, feed chamber and the feed-pipe.Stir and intensification, when temperature rises to 100 ℃, slowly add the 90g propylene oxide, the control temperature of reaction is at 130 ℃, and pressure is at 0.3Mpa; Behind the reaction 5h, aging 1h is cooled to 100 ℃.30g oxyethane is added feed chamber, is that 130 ℃, pressure are to react under the 0.3Mpa condition in temperature; In this system, the ratio of quality and the number of copies of N.F,USP MANNITOL, pyridine, KOH, epoxy compounds (total mass of propylene oxide and oxyethane) is 2: 8: 1: 120; Being 120 ℃, pressure in temperature behind the reaction 4h removes pyridine for distillation under the-0.2Mpa condition, and reaction product is neutralized to neutrality with phosphoric acid, namely gets N.F,USP MANNITOL polyethers GLC03.
(2) the polyamide-amide polyethers is synthetic
2g 1.0 PAMAMs and 1g KOH are added autoclave, successively carry out alkoxylation with 120g propylene oxide, 40g oxyethane, reaction product is neutralized to neutrality with phosphoric acid, namely get polyamide-amide polyethers shown in the formula (I), wherein, x is that 44, y is 20.
(3) emulsion splitter E's is synthetic
Polyamide-amide polyethers shown in 10g N.F,USP MANNITOL polyethers GLC03 and the 20g formula (I) is dissolved in the 40g m-xylene, the 2g 2,4 toluene diisocyanate is dissolved in the 20g m-xylene; In this system, the ratio of quality and the number of copies of polyamide-amide polyethers, m-xylene and 2,4 toluene diisocyanate is 5: 10: 30 shown in N.F,USP MANNITOL polyethers GLC03, the formula (I): 1; Under 0 ℃ of normal pressure, slowly drip 2,4 toluene diisocyanate solution to polyethers solution, reaction 1h namely gets emulsion splitter E.
Embodiment 6: the emulsion splitter performance evaluation experiment of embodiment 1-5 preparation
The Bohai Bay Oil viscous crude is carried out the test of bottle examination method breakdown of emulsion under differing temps, present on-the-spot dehydration temperaturre is 70 ℃.Experimental result is shown in table 1～3.
This bottle examination method is with reference to China National Petroleum industry standard SY/T5281-2000 " crude oil demulsifier use properties detection method (bottle examination method) " and China National Offshore Oil Corporation (CNOOC) company standard Q/HS2020-2004.Concrete experimental procedure is:
Ready crude oil production fluid sample is poured in the dehydration test bottle, and heating in water bath continues constant temperature to the homo(io)thermism and is no less than 15min.
In predetermined dehydration test bottle, inject a certain amount of emulsion splitter (A, B, C, D and E) with syringe.
Mechanical oscillation method or artificial succusion are adopted in the vibration of dehydration test bottle.A) mechanical oscillation method: after screwing bottle cap trial jar is placed on rapidly on the oscillator, concussion 0.5～5min, fully mixing takes off dehydration test bottle, loosening bottle cap, and again trial jar is placed quiescent settling in the water bath with thermostatic control.B) artificial succusion: after screwing bottle cap, dehydration test bottle is put upside down 2～5 times, after the slowly loosening bottle cap venting, again screw bottle cap, mode is directly vibrated by hand, also trial jar can be placed in the artificial vibration case, level vibration 50～200 times, amplitude should be greater than 20cm, after fully mixing, loosening bottle cap, and again dehydration test bottle is placed the water bath with thermostatic control standing sedimentation.
The water yield of deviating from of different time is recorded in range estimation, when stopping sedimentation, and observed and recorded sewage color and water-oil interface situation.
The emulsion splitter of table 1 embodiment 1-5 is under the breakdown of emulsion experimental result-70 of Bohai Bay Oil viscous crude ℃
The emulsion splitter of table 2 embodiment 1-5 is under the breakdown of emulsion experimental result-65 of Bohai Bay Oil viscous crude ℃
The emulsion splitter of table 3 embodiment 1-5 is under the breakdown of emulsion experimental result-60 of Bohai Bay Oil viscous crude ℃
Above result shows, heavy oil low-temperature demulsifier of the present invention still has good demulsification performance for heavy oil under the condition than low 10 ℃ of scene, especially emulsion splitter A, dehydration rate reaches more than 80% under low concentration, reaches the requirement of on-the-spot chemical dehydration rate 〉=80%.
Claims (6)
1. the preparation method of a heavy oil low-temperature demulsifier comprises the steps: that N.F,USP MANNITOL polyether compound and polyamide-amide polyether compound carry out crosslinking reaction and namely get described emulsion splitter under the condition of linking agent and solvent existence;
Described polyamide-amide polyether compound is at least a in the compound shown in compound shown in compound, the formula II shown in the formula (I) and the formula III; In formula (I), formula II and the formula III,
Representative-CH
2CH
2CONHCH
2CH
2-, PO represents isopropoxy, and EO represents oxyethyl group, and x is the number of 10-200, and y is the number of 5-100;
Described linking agent be in oxalyl chloride, Adipoyl Chloride, tolylene diisocyanate and the isophorone diisocyanate any; Described solvent is at least a in toluene and the dimethylbenzene;
The temperature of described crosslinking reaction is 0 ℃-50 ℃; Time is 30 minutes-120 minutes;
The ratio of quality and the number of copies of described N.F,USP MANNITOL polyether compound, polyamide-amide polyether compound, solvent and linking agent is (5-20): (10-30): (40-60): (1-5).
2. method according to claim 1, it is characterized in that: described N.F,USP MANNITOL polyether compound prepares according to the method that comprises the steps: under the condition of pyridine and basic cpd existence, N.F,USP MANNITOL and epoxy compounds carry out alkoxylation and namely get described N.F,USP MANNITOL polyether compound; Described epoxy compounds is at least a in propylene oxide and the oxyethane.
3. method according to claim 2, it is characterized in that: described basic cpd is at least a in potassium hydroxide, sodium hydroxide and the sodium ethylate.
4. method according to claim 3, it is characterized in that: the temperature of described alkoxylation is 120 ℃-140 ℃; Time is 2 hours-12 hours; Pressure is 0.2MPa-0.8MPa.
5. method according to claim 4 is characterized in that: the ratio of quality and the number of copies of described N.F,USP MANNITOL, pyridine, basic cpd, epoxy compounds is (0.5-5): (1-10): (0.5-5): (50-200).
6. the emulsion splitter that each described method prepares among the claim 1-5.
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Address after: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Patentee after: China National Offshore Oil Corporation Patentee after: CNOOC Research Institute Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Patentee before: China National Offshore Oil Corporation Patentee before: CNOOC Research Center |
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