CN103086472B - High-temperature sewage treatment reverse demulsifier of ultra-heavy oil - Google Patents
High-temperature sewage treatment reverse demulsifier of ultra-heavy oil Download PDFInfo
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Abstract
The invention discloses a high-temperature sewage treatment reverse demulsifier of ultra-heavy oil. The method comprises the following steps of preparing chlorinated polyether by taking propanetriol and epichlorohydrin as materials and boron trifluoride ether solution as an initiator; preparing cationic poly ether by placing the chlorinated polyether and trimethylamine in a high-pressure reactor; by taking carbinol as a solvent, and boron trifluoride diethyl etherate as the initiator, repeatedly and alternatively carrying out Michael addition reaction and amidation by ethanediamine, methyl acrylate and the like to prepare 3.0-generation dendritic macromolecule polyamide-amine; by taking polyethylene glycol and poly propylene glycol as materials, and potassium hydroxide powder as a catalyst, adding polypropylene glycol to prepare non-ionic polyether after the polyethylene glycol reacts a period of time; finally by taking 3.0-generation polyamide-amine as a cross-linking agent, preparing the modified composite polyamide-amine-polyether high-temperature sewage treatment reverse demulsifier of the ultra-heavy oil by compounding cationic polyether and non-ionic polyether.
Description
Technical field
The present invention relates to the technical field of petroleum chemistry treatment agent, the reverse-phase emulsifier providing is particularly useful for the processing of super Heavy Oil High Temperature sewage.
Background technology
The key character that super viscous crude is different from other class petroleum resources is that its bituminous matter, gum level are very high, cause that its viscosity is high, density is large, super heavy oil recovery adopts steam thermal recovery more, high-temperature produced liquid there is following characteristic: (1) super viscous crude density is high, because resin and asphalt content is high, cause the density variation of crude oil and water little, the mean density of viscous crude is 900kg/m
3, the density of special super viscous crude is at 990kg/m
3above; (2) super viscous crude Produced Liquid has more impurity, and oil-contg and solid suspension content be up to more than 10000mg/L, and contains the Multiple components such as petroleum-type, suspended solid, dispersed oil and oil slick, oil in water emulsion and chemical agent; (3) because colloid and pitch have natural emulsified character, oil droplet cohesion is added to the difficulties, and adds to the difficulties to the breakdown of emulsion of super viscous crude Produced Liquid, and emulsification is serious; (4) there is larger viscosity, particularly more remarkable when water temperature is low; (5) water temperature is high, often temperature will be brought up to more than 90 ℃ on stream in order to reduce viscosity of crude; (6) in super viscous crude Produced Liquid, contain a large amount of positively charged ion (Na
+, Ca
2+deng) and negatively charged ion (Cl
-, SO
4 2-deng), they can affect surge capability, saltiness and the fouling tendency of viscous crude Produced Liquid; In addition, super viscous crude Produced Liquid is in dehydration during sedimentation, and the chemical agents such as the emulsion splitter using can remain in sewage in a large number, and the emulsion's stability that sewage is formed is extremely strong, is one of the most unmanageable oil extraction waste water.
Patent for reverse-phase emulsifier discloses: the U.S. has announced a kind of quaternary ammonium salt reverse-phase emulsifier (US387017); The U.S. has announced a kind of allylic reverse-phase emulsifier (US4614593); European publication a kind of amine macromolecular compound emulsion splitter (EP0331323A2) that is applicable to crude oil development; China has announced a kind of reverse-phase emulsifier and preparation method thereof (CN102559246A), for cationic polyamide-amine, Hydrin quaternary ammonium salt, polyacrylamide oxy-ethyl-trimethyl salmiac and water mix and obtains described reverse-phase emulsifier.China has announced a kind of preparation method (CN101357992) of stellate poly quaternary ammonium salt high efficient reverse-phase emulsifier, first with the organic amines such as secondary amine, tertiary amine and epoxy chloropropane ring-opening polymerization, make linear polyquaternium, take polyamide-amide as linking agent again, finally make stellate poly quaternary ammonium salt reverse-phase emulsifier.China has also announced a kind of highly efficient anti-phase emulsion breaker for thick oil pollution water processing (CN1966138), using propylene glycol as initiator, under the effect of catalyzer, carry out propoxylation reaction, then carry out addition polymerization with oxyethane, using nonyl phenol as initiator, under the effect of catalyzer, generate nonyl phenol ethoxylate with reacting ethylene oxide, then carry out addition polymerization with propylene oxide, generate alkylphenol polyoxyethylene; The mixture of propylene glycol polyethers and alkylphenol polyoxyethylene and vinylformic acid are carried out to esterification under acidic conditions, under the effect of initiator, carry out radical polymerization, generate carboxylate; With toxilic acid, carry out esterification more partially end-blocked, generate acrylic acid modified high molecular weight demulsifier.
Reverse-phase emulsifier kind is more at present, there is stronger specific aim, mainly contain mineral-type macromolecular compound and organic cationic polymers, but when being applied to the rp demulsification of super viscous crude Produced Liquid, effect is undesirable, complexity day by day along with super Heavy Oil High Temperature sewage quality, high temperature sewage changes O/W type or W/O/W type into by the w/o type of initial stage of development, oil-water emulsion stability is extremely strong, therefore traditional reverse-phase emulsifier has been difficult to meet the demands, and the exploitation of the super Heavy Oil High Temperature Produced Liquid reverse-phase emulsifier of high temperature resistant, excellent performance seems particularly urgent.
The present invention carries out copolymerization by polyamide-amide and polyethers and non-ionic polyalcohol and obtains new modified reverse-phase emulsifier, belong to water miscible polymkeric substance, the water external emulsion of super Heavy Oil High Temperature sewage is had to excellent demulsification, with performances such as electrical neutralization, absorption, bridge formations, add 10-30ppm and can effectively remove the pollutents such as oil in high oily(waste)water, suspended substance.
Summary of the invention
The object of the invention is to: the super Heavy Oil High Temperature sewage disposal high efficient reverse-phase emulsifier providing, can efficiently process super Heavy Oil High Temperature sewage, there is oily water separation speed fast, improve the beneficial effect of the universality of product and the economic benefit of product.
The object of the present invention is achieved like this: a kind of super Heavy Oil High Temperature sewage disposal reverse-phase emulsifier, the modified composite reverse-phase emulsifier obtaining take cation polyether and nonionic polyoxyalkylene as raw material, the 3.0G dendroid polyamide-amide of take be linking agent, implementation step is as follows:
Wherein cation polyether is synthetic:
The glycerol that adds 0.020-0.030mol in the four-hole boiling flask that agitator, prolong, thermometer are housed, then add 2.10-2.17g boron trifluoride diethyl etherate, temperature control 45-55 ℃ under agitation, slowly drip again epoxy chloropropane 38-42g, time for adding 4-6min, dropwises, and is warming up to 75 ℃, reaction 5-7h, obtains the thick terminal hydroxy group chloro polyethers of brown; By 90-110g terminal hydroxy group chloro polyethers and 182-202g trimethylamine aqueous solution, be placed in clean reactor, pass into nitrogen excluding air, temperature control 70-80 ℃, reaction 4-6h, continues to be warming up to 120-130 ℃, reaction 6-8h, obtains the water miscible cation polyether of brown; Wherein the ratio of quality and the number of copies of epoxy chloropropane, glycerol, Trimethylamine 99 is 40-60:1:40-60, and the consumption of initiator boron trifluoride diethyl etherate liquid is epoxy chloropropane 1%;
Wherein 3.0G PAMAM's is synthetic:
1) 0.5G polyamide-amide is synthetic: under the protection of nitrogen, to being equipped with in the four-hole boiling flask of stirring rod, thermometer, prolong, add quadrol 30.6g, methyl alcohol 96.2g, with ice-water bath, be cooled to after 0 ℃, slowly drip methyl acrylate 174.0g, stir lower temperature control 22-27 ℃, continue reaction 22-26h, the weak yellow liquid obtaining, under 45 ℃ of conditions, carry out underpressure distillation, obtain flaxen 0.5G polyamide-amide product;
2) 1.0G polyamide-amide is synthetic: with methyl alcohol 120g, dissolve 1.0G polyamide-amide 270g, join in four-hole boiling flask, ice-water bath is cooled to after 0 ℃, slowly drip quadrol, stir lower temperature control 23-28 ℃, time for adding 1-1.5h, dropwise and continue reaction 24h, the weak yellow liquid obtaining carries out underpressure distillation under 70 ℃ of conditions, obtains faint yellow 1.0G polyamide-amide product;
3) reverse-phase emulsifier: proceed Michael addition reaction with above-mentioned 1.0G polyamide-amide, obtain 1.5G polyamide-amide, then carry out amidate action, obtain 2.0G polyamide-amide, carry out successively Michael addition reaction and amidate action, obtain the polyamide-amide of corresponding algebraically;
Wherein nonionic polyoxyalkylene is synthetic:
In there-necked flask, add 90-110g potassium hydroxide powder and 900-1100ml methylene dichloride, mix and blend under room temperature, then drip 600-polyoxyethylene glycol 230-270g, the potassium hydroxide powder that adds respectively 4-6g when 1.0h, 2.0h, 3.0h, wherein in the centre that adds potassium hydroxide powder, add 20g polypropylene glycol, continue to obtain crude product after reaction 20h, after methylene dichloride is evaporated completely, with the toluene 400-500ml of heating, dissolve, after standing, get potassium hydroxide precipitation, with the toluene 400-500ml of heating, dissolve once again, obtain polyoxyethylene propylene oxide;
Wherein modified composite reverse-phase emulsifier is synthetic: in the aqueous solution that is 800-1200g in gross weight, add successively the dendroid polyamide-amide 150-400g in cation polyether 100-250g, 3.0 generations, nonionic polyoxyalkylene 50-100g; At 35-45 ℃, stir 2-3h, obtain modified composite reverse-phase emulsifier, be super Heavy Oil High Temperature sewage disposal reverse-phase emulsifier.
Described reverse-phase emulsifier, adopts the super Heavy Oil High Temperature sewage of this product treatment, and its oleaginousness drops to below 10mg/L from 6250mg/L.
Effect of the present invention and mechanism: the synthesis mechanism of multichain section cation polyether-glycerol chloro polyethers: using glycerol as initiator, boron trifluoride diethyl etherate liquid is initiator, cause epoxy chloropropane and carry out positively charged ion ring-opening polymerization, generate terminal hydroxy group chloro polyethers; Active chlorine atom in terminal hydroxy group chloro polyethers and Trimethylamine 99 carry out the alkylated reaction of amine, generate the polycation polyethers with positive charge.The synthesis mechanism of polyamide-amide: hocket Michael addition and amidate action, can obtain for 1.5 generations, 2.0 generations, 2.5 generations, 3.0 generation PAMAM.
The method of reverse-phase emulsifier prepared by the present invention, comprises the synthetic of cation polyether, 3.0 PAMAMs synthetic, nonionic polyoxyalkylene synthetic, polyamide-amide-polyether-type--modified composite reverse-phase emulsifier synthetic, its technological line is simple, reaction conditions is gentle, dewatering speed is fast, and breakdown of emulsion efficiency is high, produces practical function splendid, the product innovation providing, reduced production cost, Ye Wei enterprise energy-saving and cost-reducing made demonstration, shows technical progress.
Embodiment
The present invention is described further in conjunction with the embodiments.
Embodiment
1) cation polyether is synthetic:
Be equipped with agitator, prolong, thermometer four-hole boiling flask in add the glycerol of 0.025mol as initiator, then add 2.13g (being about 1%) boron trifluoride diethyl etherate liquid, under agitation condition, temperature control is 50 ℃, slowly drip epoxy chloropropane, time for adding 5min, after be warming up to 75 ℃ reaction 6h, obtain the thick terminal hydroxy group chloro polyethers of brown; 100g terminal hydroxy group chloro polyethers and 191.3g trimethylamine aqueous solution (amino and chlorine atom equivalent) are placed in clean reactor, pass into nitrogen excluding air, 75 ℃ of temperature controls, reaction 5h, continue to be warmed up to 125 ℃, reaction 7h, obtains the water miscible cation polyether of brown; Wherein the ratio of quality and the number of copies of epoxy chloropropane, glycerol, Trimethylamine 99 is 40:1:40 or 60:1:60, and epoxy chloropropane and Trimethylamine 99 equivalent be take boron trifluoride diethyl etherate liquid as initiator, and its consumption is epoxy chloropropane 1%.
2) 3.0GPAMAM's is synthetic
(1) 0.5G polyamide-amide is synthetic: under the protection of nitrogen; in the four-hole boiling flask with stirring rod, thermometer, prolong, add quadrol 30.6g, methyl alcohol 96.2g; with ice-water bath, be cooled to 0 ℃; slowly drip methyl acrylate; stir 25 ℃ of lower temperature controls, the complete continuation reaction of time for adding 1h 24h, the weak yellow liquid obtaining; under 45 ℃ of conditions, carry out underpressure distillation, obtain the light yellow product of 0.5G polyamide-amide.
(2) 1.0G polyamide-amide is synthetic: the 1.0G polyamide-amide of separating with dissolve with methanol, join in four-hole boiling flask, ice-water bath is cooled to 0 ℃, slowly drip quadrol, stir 25 ℃ of lower temperature controls, time for adding 1-1.5h continues reaction 24h, the weak yellow liquid obtaining, under 70 ℃ of conditions, carry out underpressure distillation, obtain the light yellow product of 1.0G polyamide-amide.
Reverse-phase emulsifier (3) is proceeded Michael addition reaction with 1.0G polyamide-amide obtained above, can obtain 1.5G polyamide-amide, then carry out amidate action, obtain 2.0G polyamide-amide, carry out successively Michael addition reaction and amidate action, obtain the polyamide-amide of corresponding algebraically.
3) nonionic polyoxyalkylene is synthetic
In there-necked flask, add 100g potassium hydroxide powder and 1000ml methylene dichloride, mix and blend under room temperature, then drip 250g polyoxyethylene glycol-600, the potassium hydroxide powder that adds respectively 5g while being 1.0h, 2.0h, 3.0h, and when 2.0h, drip 20g polypropylene glycol, continue to obtain crude product after reaction 20h, after methylene dichloride is evaporated completely, with hot toluene 400-500ml, dissolve, the standing unreacted potassium hydroxide precipitation of removing, the toluene 400-500ml dissolution precipitation of reusable heat once, obtains the product of polyoxyethylene propylene oxide.
4) modified composite reverse-phase emulsifier is synthetic
Cation polyether is mixed with nonionic polyoxyalkylene, 3.0G polyamide-amide is linking agent, in the aqueous solution that is 1000g in gross weight, cation polyether be 100 or 250g, the dendroid polyamide-amide in 3.0 generations be 150 or 400g, nonionic polyoxyalkylene is 50 or 100g; At 40 ℃, stir 2h, obtain final product modified composite reverse-phase emulsifier, be i.e. super Heavy Oil High Temperature sewage disposal reverse-phase emulsifier.
Reverse-phase emulsifier of the present invention is synthesis type medicament, and at 85 ℃, pH:7.0 or 8.0, under the condition that dosage is 30mg/L, can drop to the oleaginousness of super Heavy Oil High Temperature sewage below 10mg/L from 6249.3mg/L, and evaluation result sees the following form:
Reverse-phase emulsifier of the present invention, possesses very strong close electric charge ability, is enough to the negative charge that balance emulsifying agent forms; Have very strong surfactivity, can destroy the interfacial energy of milk sap, oil removal rate is greater than 98%; This reverse-phase emulsifier is not stratified, without caking, machinery-free impurity, good water solubility, have oily water separation speed soon, the low feature of oleaginousness in water.
The present invention obtains modified composite reverse-phase emulsifier, and super Heavy Oil High Temperature sewage disposal reverse-phase emulsifier product meets company standard.
The manufacturer of the glycerol that the present invention selects is Shanghai Jin Rui Chemicals company limited; Boron trifluoride diethyl etherate manufacturer is Chemical Reagent Co., Ltd., Sinopharm Group; Epoxy chloropropane manufacturer is Qilu Petrochemical Company; Terminal hydroxy group chloro polyethers is self-control; Trimethylamine 99 manufacturer is Changzhou Ju Feng Chemical Co., Ltd.; Potassium hydroxide powder production producer is Jinan Jin Hao Chemical Co., Ltd.; The manufacturer of polypropylene glycol is Jiangsu Hai'an Petrochemical Plant.
Claims (2)
1. a super Heavy Oil High Temperature sewage disposal reverse-phase emulsifier, is characterized in that: implement step by step:
1) cation polyether is synthetic:
In the four-hole boiling flask that agitator, prolong, thermometer are housed, add the glycerol of 0.025mol as initiator, then add 2.13 g boron trifluoride diethyl etherate liquid, under agitation condition, temperature control is 50 ℃, slowly drip epoxy chloropropane, time for adding 5min, after be warming up to 75 ℃ reaction 6h, obtain the thick terminal hydroxy group chloro polyethers of brown; By 100g terminal hydroxy group chloro polyethers and 191.3 g trimethylamine aqueous solutions
,be placed in clean reactor, pass into nitrogen excluding air, 75 ℃ of temperature controls, reaction 5h, continues to be warmed up to 125 ℃, and reaction 7h, obtains the water miscible cation polyether of brown; Wherein the ratio of quality and the number of copies of epoxy chloropropane, glycerol, Trimethylamine 99 is 40:1:40 or 60:1:60, and the quality such as epoxy chloropropane and Trimethylamine 99 be take boron trifluoride diethyl etherate liquid as initiator, and its consumption is epoxy chloropropane 1%;
2) 3.0GPAMAM's is synthetic:
(1) 0.5G polyamide-amide is synthetic: under the protection of nitrogen, in the four-hole boiling flask with stirring rod, thermometer, prolong, add quadrol 30.6g, methyl alcohol 96.2g, with ice-water bath, be cooled to 0 ℃, slowly drip methyl acrylate, stir 25 ℃ of lower temperature controls, the complete continuation reaction of time for adding 1h 24h, the weak yellow liquid obtaining, under 45 ℃ of conditions, carry out underpressure distillation, obtain the light yellow product of 0.5G polyamide-amide;
(2) 1.0G polyamide-amide is synthetic: the 0.5G polyamide-amide of separating with dissolve with methanol, join in four-hole boiling flask, ice-water bath is cooled to 0 ℃, slowly drip quadrol, stir 25 ℃ of lower temperature controls, time for adding 1-1.5h continues reaction 24h, the weak yellow liquid obtaining, under 70 ℃ of conditions, carry out underpressure distillation, obtain the light yellow product of 1.0G polyamide-amide;
(3) with 1.0G polyamide-amide obtained above, proceed Michael addition reaction, obtain 1.5G polyamide-amide, then carry out amidate action, obtain 2.0G polyamide-amide, carry out successively Michael addition reaction and amidate action, obtain the polyamide-amide of corresponding algebraically;
3) nonionic polyoxyalkylene is synthetic:
In there-necked flask, add 100g potassium hydroxide powder and 1000mL methylene dichloride, mix and blend under room temperature, then drip 250g polyoxyethylene glycol-600, the potassium hydroxide powder that adds respectively 5g while being 1.0h, 2.0h, 3.0h, and when 2.0h, drip 20g polypropylene glycol, continue to obtain crude product after reaction 20h, after methylene dichloride is evaporated completely, with hot toluene 400-500mL, dissolve, the standing unreacted potassium hydroxide precipitation of removing, the toluene 400-500mL dissolution precipitation of reusable heat once, obtains the product of polyoxyethylene propylene oxide;
4) modified composite reverse-phase emulsifier is synthetic:
Cation polyether is mixed with nonionic polyoxyalkylene, and 3.0G polyamide-amide is linking agent, and in the aqueous solution that is 1000g in gross weight, cation polyether is that 100-250g, 3.0G polyamide-amide are 150-400g, and nonionic polyoxyalkylene is 50-100g; At 40 ℃, stir 2h, obtain final product modified composite reverse-phase emulsifier, must surpass Heavy Oil High Temperature sewage disposal reverse-phase emulsifier.
2. according to reverse-phase emulsifier described in claim 1, it is characterized in that: adopt the super Heavy Oil High Temperature sewage of this product treatment, its oleaginousness drops to below 10mg/L from 6250mg/L.
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