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CN101633837A - Polymer flooding oil-water separation agent and preparation method thereof - Google Patents

Polymer flooding oil-water separation agent and preparation method thereof Download PDF

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Publication number
CN101633837A
CN101633837A CN200910016000A CN200910016000A CN101633837A CN 101633837 A CN101633837 A CN 101633837A CN 200910016000 A CN200910016000 A CN 200910016000A CN 200910016000 A CN200910016000 A CN 200910016000A CN 101633837 A CN101633837 A CN 101633837A
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China
Prior art keywords
toluene
preparation
fatty alcohol
ratio
water separation
Prior art date
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CN200910016000A
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Chinese (zh)
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CN101633837B (en
Inventor
孙希明
刘晓松
李海丽
李成吉
呼士峰
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SHANDONG DONGFANG HUALONG INDUSTRIAL AND TRADE GROUP Co Ltd
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SHANDONG DONGFANG HUALONG INDUSTRIAL AND TRADE GROUP Co Ltd
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Priority to CN200910016000XA priority Critical patent/CN101633837B/en
Publication of CN101633837A publication Critical patent/CN101633837A/en
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Publication of CN101633837B publication Critical patent/CN101633837B/en
Expired - Fee Related legal-status Critical Current
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Abstract

A polymer flooding oil-water separation agent and a preparation method thereof are disclosed, the agent contains the following components based on parts by mass: 4-6 of bis-imidazoline, 500-600 of toluene or xylene, 20-25 of toluene di-isocyanate, 200-250 of fatty alcohol polyoxypropylene polyoxyethylene ether and 50-130 of oleamide; the preparation method thereof comprises the steps of: 1, the preparation of intermediate I: the ratio of bis-imidazoline, one tenth of the total amount of toluene or xylene to toluene di-isocyanate is 4-6:50-60:20-25 based on parts by mass, A, toluene di-isocyanate is added into a reaction kettle for reaction; B, the mixed solution of evenly-diluted bis-imidazoline and toluene or xylene is slowly added into the reaction kettle for reaction; 2, the preparation of intermediate II: the ratio of intermediate I, the rest of the total amount of toluene or xylene to fatty alcohol polyoxypropylene polyoxyethylene ether is 74-91:450-540:200-250 based on parts by mass, the intermediate I is firstly added into a polymerization reaction kettle, the mixed solution of fatty alcohol polyoxypropylene polyoxyethylene ether and toluene or xylene is slowly added into the reaction kettle for temperature-constant reaction for 3 hours; 3, the preparation of target substance: the ratio of the intermediate II to oleamide is 724-881:50-130 based on parts by mass, the intermediate II and oleamide are mixed evenly in the reaction kettle under room temperature.

Description

Polymer flooding oil-water separation agent and preparation method
One, technical field
The present invention relates to the technology of preparing of petroleum assistant, particularly a kind of polymer flooding oil-water separation agent and preparation method.
Two, background technology
Additional producing energy is the main path that oil production realizes stable high yield.At present, extensively adopt the intensified oil reduction technology of injecting oil-displacing agent, as steam drive, oil production technology technology such as polymer flooding, surfactant flooding and ternary composite driving.Yet the existence of oil-displacing agent strengthens the stability of crude oil emulsion, and dehydration, breakdown of emulsion difficulty strengthen.Oily water separation technique becomes present distinct issues.The tradition breaking method can not adapt to oily water separation technology in the present intensified oil reduction, especially to steam drive, the extraction liquid of oil production technology technology such as polymer flooding, surfactant flooding and ternary composite driving, oily water separation is more difficult.
Three, summary of the invention
The purpose of this invention is to provide a kind of polymer flooding oil-water separation agent and preparation method, modification by molecular designing, crosslinked chain extension, and the method for the composite performance of multi-agent " synergistic effect ", the shortcoming or the deficiency that overcome effectively or avoid above-mentioned prior art to exist are carried out the oily water separation of extraction liquid effectively.
Polymer flooding oil-water separation agent of the present invention, its component are mass parts:
(1) the bicyclic imidazo quinoline 4~6
(2) toluene or dimethylbenzene 500~600
(3) tolylene diisocyanate 20~25
(4) the fatty alcohol polyoxypropylene Soxylat A 25-7 200~250
(5) amine hydroxybenzene 50~130
Wherein, described tolylene diisocyanate is a Toluene-2,4-diisocyanate, and 4-vulcabond, commodity abbreviate 80/20 trade mark of DTI as.Described its molecular weight of fatty alcohol polyoxypropylene Soxylat A 25-7 is 2200~2550.EO content is mass percent 20%~30%.
The preparation method of polymer flooding oil-water separation agent of the present invention comprises preparation intermediate and target compound:
(1) preparation intermediate compound I: with bicyclic imidazo quinoline first: 1/10th of benzene or dimethylbenzene total amount: tolylene diisocyanate is with 4~650 :~602: 0~25 mass parts ratio, at first (A) adds reactor with tolylene diisocyanate, start stirring with 50~70 rev/mins, and heat to 30~60 ℃; (B) mixing solutions that will dilute uniform bicyclic imidazo quinoline and toluene or dimethylbenzene slowly added reactor, with 70 ℃ of following isothermal reactions 3 hours;
(2) preparation intermediate II: with intermediate compound I: the remainder of toluene or dimethylbenzene total amount: the fatty alcohol polyoxypropylene Soxylat A 25-7 is by mass ratio 74~91: 450~540: 200~250 ratio, and at first (a) is earlier with in the intermediate 1 adding polymerization reaction kettle; (b) under the condition that X rev/min stirring and system temperature are 30~80 ℃, slowly add in the reactor toluene (or dimethylbenzene) solution of fatty alcohol polyoxypropylene Soxylat A 25-7 again; (c) constant temperature is 70 ℃, stirs 60 rev/mins and reacts 3 hours down;
(3) preparation target compound: with intermediate II: amine hydroxybenzene is with 724~881: the ratio of 50~130 mass ratioes under 60 rev/mins agitation condition and normal temperature, mixes intermediate II and amine hydroxybenzene and gets final product in reactor.
The present invention has following advantage compared with the prior art:
(1) the products molecule structure is formed scientific and reasonable, with the bicyclic imidazo quinoline polyoxypropylene, polyoxyethylene blocks polyethers have been carried out graft modification according to the requirement success of polymer flooding, ternary composite driving oily water separation, and carry out compositely with an amount of amine hydroxybenzene and the intermediate that makes, oil-water separation can be improved and the cost of medicine can be reduced;
(2) production technique is simple, reaction conditions is gentle, energy consumption is low and the three-waste free pollution problem, and environmental protection can not cause secondary pollution in the use;
(3) good product dispersibility, the diffusion excellent adsorption in liquid, wetting film forming ability height, the flocculation coalescence effect is strong, and it is convenient to use.
Five, embodiment
A kind of polymer flooding oil-water separation agent, its component are mass parts:
(1) the bicyclic imidazo quinoline 4~6
(2) toluene or dimethylbenzene 500~600
(3) tolylene diisocyanate 20~25
(4) the fatty alcohol polyoxypropylene Soxylat A 25-7 200~250
(5) amine hydroxybenzene 50~130.
Used tolylene diisocyanate is a Toluene-2,4-diisocyanate, and 4-vulcabond, commodity abbreviate 80/20 trade mark of DTI as.Fatty alcohol polyoxypropylene Soxylat A 25-7, its molecular weight are 2200~2550.EO content is mass percent 20%~30%.
The preparation method of polymer flooding oil-water separation agent comprises preparation intermediate and target compound:
(1) preparation intermediate compound I: with bicyclic imidazo quinoline first: 1/10th of benzene or dimethylbenzene total amount: tolylene diisocyanate is with 4~65: 0~60: 20~25 mass parts ratio, at first (A) adds reactor with tolylene diisocyanate, change branch with 50~70 and start stirring, and heat to 30~60 ℃; (B) will dilute uniform bicyclic imidazo quinoline and toluene or dimethylbenzene mixing solutions and slowly add reactor, with 80 ℃ of following isothermal reactions 3 hours.
(2) preparation intermediate II: with intermediate compound I: the remainder of toluene or dimethylbenzene total amount: the fatty alcohol polyoxypropylene Soxylat A 25-7 is by mass ratio 74~91: 450~540: 200~250 ratio, and at first (a) is earlier with in the intermediate 1 adding polymerization reaction kettle; (b) again with fatty alcohol polyoxypropylene Soxylat A 25-7 and toluene or xylene solution under the condition that 50~70 rev/mins stirring and system temperature are 30~80 ℃, slowly add in the reactor; (c) constant temperature is 50~80 ℃, stirs 50~70 rev/mins and reacts 3 hours down;
(3) preparation target compound: with intermediate II: amine hydroxybenzene is with 724~881: the ratio of 50-130 mass ratio under 50~70 rev/mins agitation condition and normal temperature, mixes intermediate II and amine hydroxybenzene and gets final product in reactor.
Provide the specific embodiment that polymer flooding oil-water separation agent is a mass parts below,
Embodiment 1:
Component is for being mass parts
(1) the bicyclic imidazo quinoline 4
(2) toluene or dimethylbenzene 500
(3) tolylene diisocyanate 20
(4) the fatty alcohol polyoxypropylene Soxylat A 25-7 200
(5) amine hydroxybenzene 50
Preparation technology:
(1) with tetrahydroglyoxaline: 1/10th of toluene total amount: tolylene diisocyanate was with 4: 50: 20 mass parts ratio, and at first (A) stirs 60 rev/mins and start, 30 ℃ of system temperatures in 20 parts of adding reactors of tolylene diisocyanate; (B) bicyclic imidazo quinoline and toluene homogeneous solution are slowly added reactor, reacted 3 hours down at 60 rev/mins.
(2) preparation intermediate II: with intermediate compound I: the remainder of toluene total amount: the fatty alcohol polyoxypropylene Soxylat A 25-7 is in 74: 450: 200 ratio of mass ratio, and at first (a) answers 74 parts intermediate compound I adding in the still; (b), under 70 rev/mins stirrings and system temperature are 30 ℃ condition, slowly add in the reactor again with the mixed solution of 450 parts of toluene and 200 parts of fatty alcohol polyoxypropylene Soxylat A 25-7s; (c) reaction 3 hours under the stirring of 45 ℃ and 60 rev/mins;
(3) preparation target compound: with intermediate II: amine hydroxybenzene adds intermediate II in the reactor earlier with the ratio of 724: 50 mass ratioes, amine hydroxybenzene is added in the reactor again, gets final product to stir under 60 rev/mins stirring velocity and normal temperature.
Embodiment 2
Component is a mass parts:
(1) the bicyclic imidazo quinoline 5
(2) toluene or dimethylbenzene 550
(3) tolylene diisocyanate 22
(4) the fatty alcohol polyoxypropylene Soxylat A 25-7 220
(5) amine hydroxybenzene 100
Preparation technology: (one) prepares intermediate compound I: with the bicyclic imidazo quinoline: 1/10th of toluene total amount: tolylene diisocyanate was with 5: 55: 22 mass parts ratio, at first (A) adds tolylene diisocyanate in the reactor, start stirring with 70 rev/mins, and heat to 50 ℃; (B) bicyclic imidazo quinoline and toluene mixing solutions are slowly added reactor, 50 ℃ of following isothermal reactions 3 hours.
(2) preparation intermediate II: with intermediate compound I: the remainder of toluene total amount: the fatty alcohol polyoxypropylene Soxylat A 25-7 is in 77: 495: 220 mass parts ratio of mass ratio, and at first (a) answers the intermediate compound I adding in the still; (b) again with the mixed solution of fatty alcohol polyoxypropylene Soxylat A 25-7 and toluene, be slowly to add in the reactor below 60 ℃ in 60 rev/mins stirrings and system temperature; (c) constant temperature is 50 ℃, and 60 rev/mins stirring was reacted 3 hours down;
(3) preparation target compound: with intermediate II: amine hydroxybenzene is with the ratio of 797: 100 mass ratioes, earlier with intermediate II and amine hydroxybenzene under 60 rev/mins stirring velocity and normal temperature, stirring in reactor gets final product.
Embodiment 3
The quality component:
(1) the bicyclic imidazo quinoline 6
(2) toluene or dimethylbenzene 600
(3) tolylene diisocyanate 25
(4) the fatty alcohol polyoxypropylene Soxylat A 25-7 250
(5) amine hydroxybenzene 130
Preparation technology: (one) prepares intermediate compound I: with the bicyclic imidazo quinoline: 1/10th of dimethylbenzene total amount: tolylene diisocyanate was with 6: 60: 25 mass parts ratio, at first (A) is with in 25 parts the tolylene diisocyanate adding reactor, start with 60 rev/mins, and heat to 60 ℃ of degree; (B) slowly add 6 parts bicyclic imidazo quinoline and 60 parts toluene mixing solutions in the reactor; (C) 60 rev/mins, 60 ℃ following isothermal reactions 3 hours.
(2) preparation intermediate II: with intermediate compound I: the remainder of toluene total amount: the fatty alcohol polyoxypropylene Soxylat A 25-7 is in 91: 540: 250 mass parts ratio of mass ratio, and at first (a) answers 91 parts intermediate compound I adding in the still; (b) again with the dimethylbenzene of 250 parts fatty alcohol polyoxypropylene Soxylat A 25-7 and 540 parts mixed solution, be slowly to add in the reactor below 50 ℃ in 70 rev/mins stirrings and system temperature; (c) constant temperature is 50 ℃, and 60 rev/mins stirring was reacted 3 hours down;
(3) preparation target compound: with intermediate II: amine hydroxybenzene is in the ratio of 881: 130 mass ratioes, first with intermediate II and amine hydroxybenzene under 60 rev/mins stirring velocity and normal temperature, stirring in reactor gets final product.
Polymer flooding oil-water separation agent of the present invention, having outward appearance is light yellow uniform liquid, density is 1.03-1.09 effective content>50% is with characteristics such as water dissolve each other.

Claims (4)

1, a kind of polymer flooding oil-water separation agent, its component are mass parts:
(1) the bicyclic imidazo quinoline 4~6
(2) toluene or dimethylbenzene 500~600
(3) tolylene diisocyanate 20~25
(4) the fatty alcohol polyoxypropylene Soxylat A 25-7 200~250
(5) amine hydroxybenzene 50~130
2, polymer flooding oil-water separation agent according to claim 1 is characterized in that described tolylene diisocyanate is a Toluene-2,4-diisocyanate, and 4-vulcabond, commodity abbreviate 80/20 trade mark of DTI as.
3, polymer flooding oil-water separation agent according to claim 1 is characterized in that described fatty alcohol polyoxypropylene Soxylat A 25-7, and its molecular weight is 2200~2550, EO content is mass percent 20%~30%.
4, a kind of preparation method of polymer flooding oil-water separation agent comprises preparation intermediate and target compound, it is characterized in that being prepared as of described intermediate and target compound:
(1) preparation intermediate compound I: with the bicyclic imidazo quinoline: 1/10th of toluene or dimethylbenzene total amount: tolylene diisocyanate is with 4~6: 50~60: 20~25 mass parts ratio, at first (A) adds reactor with tolylene diisocyanate, stir with 50~70 rev/mins speed, and heat to 30~60 ℃; (B) will dilute uniform bicyclic imidazo quinoline and toluene or dimethylbenzene mixing solutions and slowly add reactor, with 80 ℃ of following isothermal reactions 3 hours;
(2) preparation intermediate II: with intermediate compound I: the remainder of toluene or dimethylbenzene total amount: the fatty alcohol polyoxypropylene Soxylat A 25-7 is by mass ratio 74~91: 450~540: 200~250 ratio, and at first (a) is first adds intermediate compound I in the polymerization reaction kettle; (b) under the condition that 50~70 rev/mins stirring and system temperature are 30~80 ℃, slowly add in the reactor mixing solutions of fatty alcohol polyoxypropylene Soxylat A 25-7 and toluene or dimethylbenzene again; (c) constant temperature is 30~80 ℃, stirs 50~70 rev/mins and reacts 3 hours down;
(3) preparation target compound: with intermediate II oil: sour acid amides is with 724~881: the ratio of 50-130 mass ratio under 50~70 rev/mins agitation condition and normal temperature, mixes intermediate II and amine hydroxybenzene and gets final product in reactor.
CN200910016000XA 2009-06-10 2009-06-10 Polymer flooding oil-water separating agent and preparation method thereof Expired - Fee Related CN101633837B (en)

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Application Number Priority Date Filing Date Title
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CN101633837A true CN101633837A (en) 2010-01-27
CN101633837B CN101633837B (en) 2012-05-02

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103923634A (en) * 2014-05-07 2014-07-16 淮南华俊新材料科技有限公司 Micro emulsion mutual solvent used for oil well acidization

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103923634A (en) * 2014-05-07 2014-07-16 淮南华俊新材料科技有限公司 Micro emulsion mutual solvent used for oil well acidization
CN103923634B (en) * 2014-05-07 2016-04-06 淮南华俊新材料科技有限公司 A kind of microemulsion mutual solvent for oil well acidation

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