CN102899070B - Binary flooding produced liquid comprehensive treatment agent and preparation method - Google Patents
Binary flooding produced liquid comprehensive treatment agent and preparation method Download PDFInfo
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Abstract
The invention relates to a binary flooding produced liquid comprehensive treatment agent and a preparation method. The binary flooding produced liquid comprehensive treatment agent comprises a demulsifier, a water purifying agent and a comprehensive treatment agent compounded by the demulsifier and the water purifying agent. The preparation method comprises the following steps that the demulsifier and the water purifying agent are firstly synthesized and then are compounded to form the binary flooding produced liquid comprehensive treatment agent. The demulsification problem of binary flooding produced W/O and O/W emulsion in oilfield is successfully solved, the demulsification effect is obvious, the transported sewage and the transported crude oil reach the required index, and polymer-bearing sludge is not generated in the demulsification process, thereby laying the foundation for polymer-bearing crude oil dehydration, standard reaching of polymer-bearing sewage treatment and wide use of polymer flooding technology.
Description
Technical field
The present invention relates to a kind of oil field binary flooding produced liquid comprehensive treatment agent and preparation method.
Background technology
On Chinese Continental, maturing field is mostly in High water cut or ultra-high water cut stage at present, and conventional waterflood development technique is difficult to slow down production rate decline.Chemical combined flooding is one of main method increasing substantially oil recovery factor.Wherein applying of binary combination flooding achieves obvious oil increasing effect.Binary combination flooding refers to the viscosity increasing displacing fluid by adding polymkeric substance in water, to improve sweep efficiency; Rely on the effect of tensio-active agent to reduce oil water interfacial tension, wettability change, emulsified crude oil to improve oil displacement efficiency simultaneously.Its essence gives full play to polymer viscosified effect, changes oil and water mobility ratio, to expand swept volume, simultaneously mating surface promoting agent change water-oil interface character be used for improve displacement sweep efficiency, thus realize a kind of combination flooding technology increasing substantially recovery ratio.Owing to containing polymkeric substance and tensio-active agent in oil field mining liquid during application binary combination flooding simultaneously, define W/O, O/W of emulsification type complexity and the mixed dispersion of multiple emulsification, further increase the stability of Produced Liquid, more difficult when causing oily water separation and sewage aftertreatment comparatively to use polymer flooding.
Current process binary flooding produced liquid uses conventional emulsion splitter in petrol station, breaking emulsion and dewatering effect is undesirable, to dispose of sewage employing flocculation technique, by water conditioner and interpolymer interaction, form the floc sedimentation carrying oil droplet and suspended particle, reach the object of water purification oil removing, but floc sedimentation floats and enters waste oil recovery and can affect dehydrating of crude oil, sinking can be formed containing poly-greasy filth.
Gudong field joint station carrys out liquid and contains binary flooding produced liquid, and stability is stronger.Upper emulsion splitter process binary used of standing drives extraction crude oil, and dehydrating effect is bad, and triphase separator divides oily moisture height, and outer oil transportation is moisture to exceed standard; Adopt flocculation technique to dispose of sewage simultaneously, produce containing poly-greasy filth (30m3/d) and ageing oil, cause waste oil recovery to affect dehydrating of crude oil, the problems such as greasy filth blocking gathering system.For binary flooding produced liquid, develop applicable comprehensive treatment agent, the outer oil transportation water of effective guarantee is up to standard.
Summary of the invention
The object of the invention provides a kind of binary flooding produced liquid comprehensive treatment agent and preparation method, can take into account dehydrating of crude oil and sewage degrease.In treating processes, dehydrating of crude oil speed is fast, and dehydration rate is high, and sewage disposal does not need to add flocculation water purification agent, and sewage degrease rate is high, and outer oil transportation water is all up to standard.
Technical scheme of the present invention is implemented in the following manner:
The present invention first synthesizes emulsion splitter and water purification agent, then emulsion splitter and water purification agent are synthesized binary flooding produced liquid comprehensive treatment agent; Synthesis step is as follows:
A: emulsion splitter synthesizes: with macromole phenol-amine resin for initiator, basic cpd is catalyzer, first obtain propoxylation polyether compound with propylene oxide reaction, under alkaline catalysts effect, addition reaction is carried out again with oxyethane, the intermediate formed is priority and propylene oxide again, oxyethane reacts successively, then carries out polyreaction with propylene oxide, synthesis emulsion splitter;
Basic cpd is potassium hydroxide, in the first step reaction, and macromole phenol ammonia resin: basic cpd: propylene oxide=20 ~ 30:0.05 ~ 0.15:80 ~ 120; In second step reaction, propoxylation polyether compound: basic cpd: oxyethane=25 ~ 35:0.1 ~ 0.3:70 ~ 110; In three-step reaction, intermediate: basic cpd: propylene oxide=20 ~ 40:0.05 ~ 0.15:80 ~ 120; In four-step reaction, the intermediate of the 3rd step: basic cpd: oxyethane=15 ~ 35:0.1 ~ 0.2:70 ~ 120; In 5th step reaction, the intermediate of the 4th step: basic cpd: propylene oxide=20 ~ 30:0.05 ~ 0.15:80 ~ 140; Above proportioning is massfraction ratio;
B: water purification agent synthesizes: take propylene glycol as initiator, basic cpd is catalyzer, first obtains propoxylation polyether compound with propylene oxide reaction; Carry out under alkaline catalysts effect with propylene oxide being again obtained by reacting polyether compound; And by it under alkaline catalysts effect, obtain polyoxyethylene polyoxypropylene block copolymer with reacting ethylene oxide; Make chainextender with MALEIC ANHYDRIDE again, be catalyzer with tosic acid, carry out chain extension modification and obtain water purification agent;
In above-mentioned water purification agent building-up reactions, in the first step reaction, initiator: basic cpd: propylene oxide=15 ~ 20:0.05 ~ 0.15:110 ~ 160; In second step reaction, the intermediate of the first step, basic cpd, propylene oxide=15 ~ 20:0.05 ~ 0.25:110 ~ 160; In three-step reaction, the intermediate of second step, basic cpd, oxyethane=10 ~ 20:0.1 ~ 0.25:80 ~ 120; In four-step reaction, the intermediate of the 3rd step: catalyzer: chainextender=50 ~ 80:0.05 ~ 0.08:40 ~ 90; Above proportioning is massfraction ratio;
C, emulsion splitter and water purification agent are according to ratio of quality and the number of copies 1:(1 ~ 10) carry out composite, obtain GD-1 structural synthesis treatment agent.
The preparation method of emulsion splitter and water purification agent:
A preparation method for emulsion splitter, its preparation method is as follows:
(1) massfraction of macromole phenol-amine resin 20-30 and the massfraction of potassium hydroxide 0.05-0.15 are put into reactor,-0.08Mpa is evacuated to kettle, be warming up to temperature of reaction 100 ~ 140 DEG C, slowly pass into the massfraction of propylene oxide 80-120, in still, pressure constantly rises, and control pressure is at 0.3 ~ 0.4MPa simultaneously, reaction times is 6 ~ 8h, to propylene oxide complete reaction, in still, pressure terminates to negative pressure, obtained propoxylation polyether compound.
(2) the product propoxylation polyether compound 25-35 massfraction of (1) and potassium hydroxide 0.1-0.3 massfraction are put into reactor,-0.08Mpa is evacuated to kettle, be warming up to temperature of reaction 100 ~ 120 DEG C,, slowly pass into oxyethane 70-110 massfraction, in still, pressure constantly rises simultaneously, control pressure is at 0.2 ~ 0.3MPa, reaction times is 3 ~ 5h, and to oxyethane complete reaction, in still, pressure terminates to negative pressure.
(3) massfraction of the product Intermediate 20-40 of (2) and the massfraction of potassium hydroxide 0.05-0.15 are added in reactor,-0.08Mpa is evacuated to kettle, be warming up to temperature of reaction 100 ~ 140 DEG C, slowly pass into the massfraction of propylene oxide 80-120 simultaneously, in still, pressure-controlling is at 0.3 ~ 0.4MPa, and the reaction times is 6 ~ 8h, to propylene oxide complete reaction, in still, pressure terminates to negative pressure, makes intermediate;
(4) massfraction of the intermediate 15-35 of (3) and the massfraction of potassium hydroxide 0.1-0.2 are added in reactor,-0.08Mpa is evacuated to kettle, be warming up to temperature of reaction 100 ~ 140 DEG C, slowly pass into the massfraction of oxyethane 70-120 simultaneously, control pressure is at 0.3 ~ 0.4MPa, and the reaction times is 6 ~ 8h, to oxyethane complete reaction, in still, pressure terminates to negative pressure, makes intermediate;
(5) the intermediate 15-35 massfraction of (4) and the massfraction of potassium hydroxide 0.1-0.2 are added in reactor,-0.08Mpa is evacuated to kettle, be warming up to temperature of reaction 100 ~ 140 DEG C, slowly pass into the massfraction of propylene oxide 80-140 simultaneously, control pressure is at 0.3 ~ 0.4MPa, and the reaction times is 6 ~ 8h, to propylene oxide complete reaction, in still, pressure terminates to negative pressure, makes emulsion splitter;
A preparation method for water purification agent, be water purification agent according to claim 1, its preparation method is as follows:
(1) propylene glycol 15-20 massfraction and potassium hydroxide 0.05-0.15 massfraction are added reactor,-0.08Mpa is evacuated to kettle, starting heats up stirs, temperature of reaction controls at 100 ~ 130 DEG C, start to pass into propylene oxide 110-160 massfraction, control pressure is at 0.3 ~ 0.4MPa, and reaction 4 ~ 5 h, obtain intermediate;
(2) the intermediate 15-20 massfraction of (1) and potassium hydroxide 0.05-0.15 massfraction are added reactor,-0.08Mpa is evacuated to kettle, starting heats up stirs, temperature of reaction controls at 100 ~ 130 DEG C, start to pass into propylene oxide 110-160 massfraction, control pressure is at 0.3 ~ 0.4MPa, and reaction 4 ~ 5 h, obtain intermediate;
(3) the intermediate 10-20 massfraction of (2) and potassium hydroxide 0.0-0.25 massfraction are joined in autoclave,-0.08Mpa is evacuated to kettle, starting heats up stirs, temperature of reaction controls at 100 ~ 120 DEG C, again 80-120 oxyethane is added in reactor, control pressure is at 0.3 ~ 0.4MPa, and reaction 3 ~ 4 h, obtain intermediate polyoxyethylene polyoxypropylene block copolymer;
(4) by the intermediate 50-80 massfraction MALEIC ANHYDRIDE 0.5-0.8 massfraction of (3) and tosic acid 40-90 massfraction, add in reactor, Depressor response is carried out after temperature range internal reflux 2 h of 120 ~ 140 DEG C, its vacuum degree control is between 0. 08 ~ 0. 09 MPa, temperature of reaction controls, between 140 ~ 160 DEG C, to have reacted and obtained water purification agent.
Prepared by comprehensive treatment agent, by the emulsion splitter of above-mentioned preparation and water purification agent by massfraction than 1:(1-10) carry out compositely obtaining GD-1 structural synthesis treatment agent.
The present invention successfully solves the breakdown of emulsion problem that oil field binary drives W/O and the O/W milk sap of extraction, demulsification is remarkable, waste water displacement and outer output oil is made to reach set quota, and do not produce containing poly-greasy dirt in breakdown of emulsion process, for laying a good foundation containing poly-dehydrating of crude oil and polymer-bearing waste-water process employing polymer displacement of reservoir oil tech up to standard and extensive.
Embodiment
For disclosing technical scheme of the present invention further, elaborate below by specific embodiment:
The present invention first synthesizes emulsion splitter and water purification agent, then emulsion splitter and water purification agent are synthesized binary flooding produced liquid comprehensive treatment agent; Synthesis step is as follows:
A: emulsion splitter synthesizes: with macromole phenol-amine resin for initiator, basic cpd is catalyzer, first obtain propoxylation polyether compound with propylene oxide reaction, under alkaline catalysts effect, addition reaction is carried out again with oxyethane, the intermediate formed is priority and propylene oxide again, oxyethane reacts successively, then carries out polyreaction with propylene oxide, synthesis emulsion splitter;
Basic cpd is potassium hydroxide, in the first step reaction, and macromole phenol ammonia resin: basic cpd: propylene oxide=20 ~ 30:0.05 ~ 0.15:80 ~ 120; In second step reaction, propoxylation polyether compound: basic cpd: oxyethane=25 ~ 35:0.1 ~ 0.3:70 ~ 110; In three-step reaction, intermediate: basic cpd: propylene oxide=20 ~ 40:0.05 ~ 0.15:80 ~ 120; In four-step reaction, the intermediate of the 3rd step: basic cpd: oxyethane=15 ~ 35:0.1 ~ 0.2:70 ~ 120; In 5th step reaction, the intermediate of the 4th step: basic cpd: propylene oxide=20 ~ 30:0.05 ~ 0.15:80 ~ 140; Above proportioning is massfraction ratio;
B: water purification agent synthesizes: take propylene glycol as initiator, basic cpd is catalyzer, first obtains propoxylation polyether compound with propylene oxide reaction; Carry out under alkaline catalysts effect with propylene oxide being again obtained by reacting polyether compound; And by it under alkaline catalysts effect, obtain polyoxyethylene polyoxypropylene block copolymer with reacting ethylene oxide; Make chainextender with MALEIC ANHYDRIDE again, be catalyzer with tosic acid, carry out chain extension modification and obtain water purification agent;
In above-mentioned water purification agent building-up reactions, in the first step reaction, initiator: basic cpd: propylene oxide=15 ~ 20:0.05 ~ 0.15:110 ~ 160; In second step reaction, the intermediate of the first step, basic cpd, propylene oxide=15 ~ 20:0.05 ~ 0.25:110 ~ 160; In three-step reaction, the intermediate of second step, basic cpd, oxyethane=10 ~ 20:0.1 ~ 0.25:80 ~ 120; In four-step reaction, the intermediate of the 3rd step: catalyzer: chainextender=50 ~ 80:0.05 ~ 0.08:40 ~ 90; Above proportioning is massfraction ratio;
C, emulsion splitter and water purification agent are according to ratio of quality and the number of copies 1:(1 ~ 10) carry out composite, obtain GD-1 structural synthesis treatment agent.
Example (proportioning is massfraction ratio) prepared by emulsion splitter
(1) by macromole phenol-amine resin 26 parts, reactor put into by 0.18 part, potassium hydroxide,-0.08Mpa is evacuated to kettle, be warming up to temperature of reaction 100 ~ 140 DEG C, slowly pass into propylene oxide 88g, in still, pressure constantly rises simultaneously, control pressure is at 0.3 ~ 0.4MPa, reaction times is 6 ~ 8h, and to propylene oxide complete reaction, in still, pressure terminates to negative pressure.
(2) by the product 21 parts of (1), reactor put into by 0.08 part, potassium hydroxide,-0.08Mpa is evacuated to kettle, is warming up to temperature of reaction 100 ~ 120 DEG C, slowly pass into 82 parts, oxyethane simultaneously, in still, pressure constantly rises, and control pressure is at 0.2 ~ 0.3mpa, and the reaction times is 3 ~ 5h, to oxyethane complete reaction, in still, pressure terminates to negative pressure.
(3) by the product 26 parts of (2), 0.12 part, potassium hydroxide, propylene oxide 75 parts, adds reaction kettle for reaction, and process is same 1..
(4) by the product 25 parts of (3), 0.1 part, potassium hydroxide, oxyethane, adds reaction kettle for reaction by 95 parts, and process is with (1).
(5) by the product 28 parts of (4), 0.2 part, potassium hydroxide, propylene oxide, adds reaction kettle for reaction by 90 parts, and process, with 1., obtains emulsion splitter.
Water purification agent synthesizes: by propylene glycol 16 parts, 0.08 part, potassium hydroxide, add reactor, be evacuated to-0.08Mpa to kettle, starting heats up stirs, and temperature of reaction controls at 100 ~ 130 DEG C, start to pass into propylene oxide 120 parts, control pressure is at 0.3 ~ 0.4MPa, and reaction 4 ~ 5 h, obtain intermediate product A.By same synthetic method and the operation steps of intermediate product A, get 20 parts of A, 110 parts of propylene oxide, 0.1 part, potassium hydroxide obtains intermediate product B..
Again 15 parts of B and 0.2 part potassium hydroxide are joined in autoclave,-0.08Mpa is evacuated to kettle, starting heats up stirs, temperature of reaction controls at 100 ~ 120 DEG C, again 85 parts of oxyethane are added in reactor, control pressure is at 0.3 ~ 0.4MPa, and reaction 3 ~ 4 h, obtain product polyoxyethylene polyoxypropylene block copolymer C.
By 20 parts of C, 22 parts of MALEIC ANHYDRIDE, tosic acid 0.02 part, add in reactor, Depressor response is carried out after temperature range internal reflux 2 h of 120 ~ 140 DEG C, its vacuum degree control is between 0. 08 ~ 0. 09 MPa, and temperature of reaction controls, between 140 ~ 160 DEG C, to have reacted and obtained water purification agent.
Comprehensive treatment agent application example:
The comprehensive treatment agent of invention has carried out the field application test of 36 days by a definite date at Gudong field joint station, and eastern one carrys out liquid measure 48000m
3/ d, comprehensive water cut 96-97%.With the lonely eastern binary flooding produced liquid of GD-1 structural synthesis treatment agent process, do not change site technique flow process, well array chemical feeding quantity is 35mg/L.Outer oil transportation is moisture drops to 1.06% by 1.53% before testing, and waste water displacement oil-containing has dropped to 21mg/L, is not formed containing poly-greasy filth.Result shows, comprehensive treatment agent drives W/O, O/W milk sap to binary good demulsification.
Claims (2)
1. a binary flooding produced liquid comprehensive treatment agent, comprises emulsion splitter, water purification agent and emulsion splitter and the composite comprehensive treatment agent of water purification agent, first synthesizes emulsion splitter and water purification agent, then emulsion splitter and water purification agent are re-dubbed binary flooding produced liquid comprehensive treatment agent; Synthesis step is as follows:
A: emulsion splitter synthesizes: with macromole phenol-amine resin for initiator, basic cpd is catalyzer, first obtain propoxylation polyether compound with propylene oxide reaction, under alkaline catalysts effect, addition reaction is carried out again with oxyethane, the intermediate formed is priority and propylene oxide again, oxyethane reacts successively, then carries out polyreaction with propylene oxide, synthesis emulsion splitter;
Basic cpd is potassium hydroxide, in the first step reaction, and macromole phenol ammonia resin: basic cpd: propylene oxide=20 ~ 30:0.05 ~ 0.15:80 ~ 120; In second step reaction, propoxylation polyether compound: basic cpd: oxyethane=25 ~ 35:0.1 ~ 0.3:70 ~ 110; In three-step reaction, intermediate: basic cpd: propylene oxide=20 ~ 40:0.05 ~ 0.15:80 ~ 120; In four-step reaction, the intermediate of the 3rd step: basic cpd: oxyethane=15 ~ 35:0.1 ~ 0.2:70 ~ 120; In 5th step reaction, the intermediate of the 4th step: basic cpd: propylene oxide=20 ~ 30:0.05 ~ 0.15:80 ~ 140; Above proportioning is massfraction ratio;
B: water purification agent synthesizes: take propylene glycol as initiator, basic cpd is catalyzer, first obtains propoxylation polyether compound with propylene oxide reaction; Carry out under alkaline catalysts effect with propylene oxide being again obtained by reacting polyether compound; And by it under alkaline catalysts effect, obtain polyoxyethylene polyoxypropylene block copolymer with reacting ethylene oxide; Make chainextender with MALEIC ANHYDRIDE again, be catalyzer with tosic acid, carry out chain extension modification and obtain water purification agent;
In above-mentioned water purification agent building-up reactions, in the first step reaction, initiator: basic cpd: propylene oxide=15 ~ 20:0.05 ~ 0.15:110 ~ 160; In second step reaction, the intermediate of the first step, basic cpd, propylene oxide=15 ~ 20:0.05 ~ 0.25:110 ~ 160; In three-step reaction, the intermediate of second step: basic cpd: oxyethane=10 ~ 20:0.1 ~ 0.25:80 ~ 120; In four-step reaction, the intermediate of the 3rd step: catalyzer: chainextender=50 ~ 80:0.05 ~ 0.08:40 ~ 90; Above proportioning is massfraction ratio;
C, emulsion splitter and water purification agent are according to ratio of quality and the number of copies 1:(1 ~ 10) carry out composite, obtain GD-1 structural synthesis treatment agent.
2. a preparation method for emulsion splitter, be emulsion splitter according to claim 1, its preparation method is as follows:
(1) massfraction of macromole phenol-amine resin 20-30 and the massfraction of potassium hydroxide 0.05-0.15 are put into reactor;-0.08Mpa is evacuated to kettle; be warming up to temperature of reaction 100 ~ 140 DEG C; slowly pass into the massfraction of propylene oxide 80-120, in still, pressure constantly rises, and control pressure is at 0.3 ~ 0.4MPa simultaneously; reaction times is 6 ~ 8h; to propylene oxide complete reaction, in still, pressure terminates to negative pressure, obtained propoxylation polyether compound;
(2) the product propoxylation polyether compound 25-35 massfraction of (1) and potassium hydroxide 0.1-0.3 massfraction are put into reactor;-0.08Mpa is evacuated to kettle; be warming up to temperature of reaction 100 ~ 120 DEG C;, slowly pass into oxyethane 70-110 massfraction, in still, pressure constantly rises simultaneously; control pressure is at 0.2 ~ 0.3MPa; reaction times is 3 ~ 5h, and to oxyethane complete reaction, in still, pressure terminates to negative pressure;
(3) massfraction of the product Intermediate 20-40 of (2) and the massfraction of potassium hydroxide 0.05-0.15 are added in reactor,-0.08Mpa is evacuated to kettle, be warming up to temperature of reaction 100 ~ 140 DEG C, slowly pass into the massfraction of propylene oxide 80-120 simultaneously, in still, pressure-controlling is at 0.3 ~ 0.4MPa, and the reaction times is 6 ~ 8h, to propylene oxide complete reaction, in still, pressure terminates to negative pressure, makes intermediate;
(4) massfraction of the intermediate 15-35 of (3) and the massfraction of potassium hydroxide 0.1-0.2 are added in reactor,-0.08Mpa is evacuated to kettle, be warming up to temperature of reaction 100 ~ 140 DEG C, slowly pass into the massfraction of oxyethane 70-120 simultaneously, control pressure is at 0.3 ~ 0.4MPa, and the reaction times is 6 ~ 8h, to oxyethane complete reaction, in still, pressure terminates to negative pressure, makes intermediate;
(5) by the intermediate of the 4th step: basic cpd: the massfraction of propylene oxide=20 ~ 30:0.05 ~ 0.15:80 ~ 140 and potassium hydroxide 0.1-0.2 adds in reactor,-0.08Mpa is evacuated to kettle, be warming up to temperature of reaction 100 ~ 140 DEG C, slowly pass into the massfraction of propylene oxide 80-140 simultaneously, control pressure is at 0.3 ~ 0.4MPa, and the reaction times is 6 ~ 8h, to propylene oxide complete reaction, in still, pressure terminates to negative pressure, makes emulsion splitter.
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| CN103666541B (en) * | 2013-12-03 | 2015-09-30 | 北京易斯普罗石油工程技术有限公司 | A kind of crude oil demulsifier and preparation method thereof |
| CN106832254B (en) * | 2017-02-22 | 2019-01-04 | 济南惠信实业有限公司 | The preparation method of desalination type demulsifier |
| CN110437820B (en) * | 2019-08-15 | 2021-06-15 | 山东滨州昱诚化工科技有限公司 | Preparation method and application of emulsifier for oilfield fracturing acidification |
| CN111482176B (en) * | 2020-04-26 | 2023-04-25 | 江苏森茂能源发展有限公司 | Method for recycling pyrolysis residues of oil sludge |
| CN116286091B (en) * | 2023-05-22 | 2023-08-11 | 新疆科力新技术发展股份有限公司 | Oil field produced liquid composite treatment medicament and preparation method thereof |
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| CN1537924A (en) * | 2003-10-22 | 2004-10-20 | 山东大学 | Low-temperature quick deemulsifying agent for water-containing wax-containing erude oil and its preparation method |
| CN1772844A (en) * | 2005-11-15 | 2006-05-17 | 中国石化胜利油田有限公司孤东采油厂 | Binary re-compound oil soluble demulsifier |
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| CN1537924A (en) * | 2003-10-22 | 2004-10-20 | 山东大学 | Low-temperature quick deemulsifying agent for water-containing wax-containing erude oil and its preparation method |
| CN1772844A (en) * | 2005-11-15 | 2006-05-17 | 中国石化胜利油田有限公司孤东采油厂 | Binary re-compound oil soluble demulsifier |
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