CN102746470A - Preparation method of efficient deemulsifier for naphthenic extra heavy oil and product thereof - Google Patents
Preparation method of efficient deemulsifier for naphthenic extra heavy oil and product thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of an efficient deemulsifier for naphthenic extra heavy oil and a product thereof, belonging to the technical field of petroleum processing. The efficient deemulsifier is prepared by polymerizing alkylphenol, polyethylene polyamine and formaldehyde to obtain thermoplastic phenol-amine resin as an initiator, polymerizing the initiator with oxirane and epoxypropane to generate polyether blocked copolymer, and then esterifying the polyether blocked copolymer with acrylic acid and other unsaturated acids to generate a modified polyether product by grafting olefine acid. The product prepared by the method has the characteristics of quick dehydration and low dosage. The efficient deemulsifier of the invention is suitable for dehydrating the naphthenic extra heavy oil of Karamay oil fields, meeting the requirements of proper temperature, quick dehydration, high dehydration rate, clear water color, and tidy oil-water interface, and has high efficiency demulsification and dehydration performance.
Description
Technical field
The present invention relates to a kind of special thick oil demulsifier preparation method and product, belong to the Petroleum Processing Technology field.
Background technology
Crude oil because contacting of crude oil and water adds the effect of the naturally occurring emulsifying agent in the crude oil, makes crude oil and water form stable milk sap in recovery process.Make emulsification of crude oil serious.In order to reach the requirement of crude oil exporting, just need carry out breakdown of emulsion to crude oil, make crude oil and water sepn.Along with tertiary oil recovery technology is promoted; A large amount of uses of technology of reservoir sweep such as surfactant flooding, polymer flooding have all caused great influence to crude Treatment; Changed the state of conventional crude extraction liquid; Not only water ratio increase in the emulsion of crude oil, and stability enhancing, the especially output of viscous crude, special viscous crude increase and make the breakdown of emulsion process become complicated.Another unfavorable factor is the energy consumption problem in the breakdown of emulsion process, causes extraction liquid processing cost cumulative year after year, the corresponding processing cost that also increases crude oil extraction liquid.
The emulsion splitter that use at present domestic each oil field is main with polyether type demulsifying agent mainly, and the crude oil characteristics to each oil field improve polyether type demulsifying agent, and its basic line is for changing head, change tail, add bone, transferring and weigh and composite.Disclose a kind of prescription of efficient thick-oil emulsion splitter like Chinese patent CN1037094A, adopted the mixture of a kind of alkylphenol and another kind of phenol and formaldehyde condensation to get resol, with sulfation after oxyethane, the propylene oxide block copolymerization etherificate.Show as bad adaptability for the special viscous crude result of use of naphthenic base, de-emulsification speed is very slow, and it is low finally to deviate from the water yield, and breakdown of emulsion process graded is not obvious.And the emulsion splitter consumption requires shortcomings such as big.
Chinese patent CN1810933A thick oil demulsifier and preparation method thereof, open thick oil demulsifier product are suitable for the special thick oil emulsion breaking in Liaohe Oil Field, are not suitable for the geographic special consistency crude oil breakdown of emulsion in Kelamayi.
The crude oil of the ultra viscous crude heavy oil block of Kelamayi area oil field naphthenic base, oil product have that density is big, viscosity is big, wax content is high, moisture height, intractability are bigger.Use demulsifier product mainly to show as to solve prior art to exist the breakdown of emulsion temperature high problem such as dosage is big, and dewatering speed is undesirable at present.
The present invention has fast, the characteristics of low dosage.Be applicable to the ultra viscous crude field heavy oil dehydration of Kelamayi naphthenic base, it is fast to require temperature to be fit to dehydration, and dehydration rate is high, and water colour is clear, water-oil interface are neat.
Summary of the invention
The purpose of this invention is to provide the high-efficient demulsifier of area, a kind of particularly suitable Kelamayi in the special consistency crude oil of naphthenic base.
Technical scheme of the present invention is following:
The special thick oil demulsifier of a kind of naphthenic base; It is characterized in that it is is initiator with the modification phenol-amine resin, under catalyst action, carry out after the block polymerization again the multilayer shape that obtains with the unsaturated acid esterification graft modification, the modified polyether emulsion splitter monomer of many aromatic rings tridimensional network with propylene oxide and oxyethane.The preparation method of this emulsion splitter may further comprise the steps:
1, phenol-amine resin is synthetic
Alkylphenol or dihydroxyphenyl propane, polyethylene polyamine and YLENE are joined in the reactor drum of band whipping appts; Be warming up to 50～90 ℃; Drip formaldehyde solution then; Maintain the temperature at polyreaction under 65～115 ℃ of conditions, rise to then 110～185 ℃ under reduced pressure dehydration obtain the reddish-brown phenol-amine resin.Wherein aryl phenol, polyethylene polyamine are that the middle amount proportioning of 37% formaldehyde solution calculated is with weight percent concentration: 1: 0.5～20: 0.1～5
Described aromatic ring phenol comprises phenol, dihydroxyphenyl propane
Described alkylphenol comprises NP, octyl phenol
Described polyethylene polyamine comprises triethylene tetramine, TEPA, five ethene hexamines
2, block polyether is synthetic
Gained phenol-amine resin and catalyzer in the step 1 are joined in the reactor drum of airtight nitrogen protection; Stir; Be warming up to 130～140 ℃; The adjusting pressure range is 0.2～0.5MPa, adds propylene oxide and oxyethane successively and carries out polyreaction, and container inner pressure no longer changes promptly to be regarded as reacting and finishes.Obtain block polyether, wherein the weight ratio of phenol-amine resin, propylene oxide and oxyethane is: 1: 80～140: 20～50.
Described polymerisation catalysts is the compound of basic catalyst and an acidic catalyst, and wherein basic catalyst comprises: Pottasium Hydroxide, Potassium ethanoate, calcium hydroxide, an acidic catalyst comprise Hydrocerol A, glacial acetic acid, tartrate.Catalyst levels is 1: 1 for the two part by weight.
Described an acidic catalyst comprises glacial acetic acid, oxalic acid, tartrate.
3, graft esterification reaction
Synthetic even collecting process two processes by unsaturated acid such as vinylformic acid and block polyether esterification process and high fat thing of graft esterification modification are formed; Specifically synthesis step is following: unsaturated acid such as block polyether, vinylformic acid, Catalyzed by p-Toluenesulfonic Acid agent are added in the reactor drum, and stirring heats up 40～150 ℃ refluxed 30～60 minutes, divided till the dried up no longer increase; Be cooled to 40～80 ℃; Add a certain amount of vinylformic acid, add quantitative initiator Lucidol after stirring again, be warming up to 120～180 ℃; React and accomplished esterification in 2～8 hours, promptly obtain modified polyether monomer demulsifier product.
Weight proportion is: catalyzer: unsaturated acid such as vinylformic acid: block polyether=0.5: 1～30: 30～100.
The initiator Lucidol accounts for 7～12% of unsaturated acid such as vinylformic acid batching gross weight
Described unsaturated acid comprises one or more of unsaturated acid such as vinylformic acid, methylacrylic acid, maleic anhydride, toxilic acid and fumaric acid.
Beneficial effect of the present invention is that this emulsion splitter is the modified polyether emulsion splitter monomer with multilayer shape, many aromatic rings tridimensional network, and this emulsion splitter reaches water-oil interface rapidly in special viscous crude, fall greatly
2, block polyether is synthetic
Gained phenol-amine resin and catalyzer in the step 1 are joined in the reactor drum of airtight nitrogen protection; Stir; Be warming up to 130～140 ℃; The adjusting pressure range is 0.2～0.5MPa, adds propylene oxide and oxyethane successively and carries out polyreaction, and container inner pressure no longer changes promptly to be regarded as reacting and finishes.Obtain block polyether, wherein the weight ratio of phenol-amine resin, propylene oxide and oxyethane is: 1: 80～140: 20～50.
Described polymerisation catalysts is the compound of basic catalyst and an acidic catalyst, and wherein basic catalyst comprises: Pottasium Hydroxide, Potassium ethanoate, calcium hydroxide, an acidic catalyst comprise Hydrocerol A, glacial acetic acid, tartrate.Catalyst levels is 1: 1 for the two part by weight.
Described an acidic catalyst comprises glacial acetic acid, oxalic acid, tartrate.
3, graft esterification reaction
Synthetic even collecting process two processes by unsaturated acid such as vinylformic acid and block polyether esterification process and high fat thing of graft esterification modification are formed; Specifically synthesis step is following: unsaturated acid such as block polyether, vinylformic acid, Catalyzed by p-Toluenesulfonic Acid agent are added in the reactor drum, and stirring heats up 40～150 ℃ refluxed 30～60 minutes, divided till the dried up no longer increase; Be cooled to 40～80 ℃; Add a certain amount of vinylformic acid, add quantitative initiator Lucidol after stirring again, be warming up to 120～180 ℃; React and accomplished esterification in 2～8 hours, promptly obtain modified polyether monomer demulsifier product.
Weight proportion is: catalyzer: unsaturated acid such as vinylformic acid: block polyether=0.5: 1～30: 30～100.
The initiator Lucidol accounts for 7～12% of unsaturated acid such as vinylformic acid batching gross weight
Described unsaturated acid comprises one or more of unsaturated acid such as vinylformic acid, methylacrylic acid, maleic anhydride, toxilic acid and fumaric acid.
Beneficial effect of the present invention is that this emulsion splitter is the modified polyether emulsion splitter monomer with multilayer shape, many aromatic rings tridimensional network; This emulsion splitter reaches water-oil interface rapidly in special viscous crude; Reduce the elasticity and the viscosity of interfacial film greatly; Quicken the gathering of drop, reach the purpose of efficient fast emulsion breaking.The special thick oil demulsifier of the naphthenic base that provides has that synthesis technique is simple, and operational condition is gentle, and tooling cost is low, is convenient to suitability for industrialized production, to advantages such as the special thick oil emulsion breaking in area, Kelamayi are effective.
Embodiment
Embodiment 1
With phenol 100kg, TEPA 550kg, YLENE 200kg; Drop in the reaction kettle, be warming up to 60 ℃ under stirring, slowly drip 37% formaldehyde solution 210kg; Continue heating and maintain the temperature at 90～95 ℃; After the reaction to terminal, be-0.08 in 120 ℃ of vacuum tightnesss of temperature～-dewater under the 0.09MPa, make phenol-amine resin.In autoclave, add 50kg phenol-amine resin, 15kg catalyzer by Pottasium Hydroxide and glacial acetic acid according to by 1: 1 composite forming of weight ratio; Adding propylene oxide 750kg temperature control to 135～155 ℃; Adding oxyethane 200kg temperature control is 0.2～0.4MPa at 120 ℃ of following control still pressure, and polymerization obtains the block polyether macromolecular compound.To synthesize in block polyether 700kg, vinylformic acid 200kg, the catalyzer tosic acid 5kg input reaction kettle, and stir and heat up 130～145 ℃, divide till the dried up no longer increase to refluxing 40～60 minutes; Be cooled to 50～75 ℃, add vinylformic acid 50kg, the initiator Lucidol 25kg that adds again after stirring; Be warming up to 145～180 ℃; React and accomplished esterification in 4～6 hours, promptly obtain the graft esterification demulsifier product, be numbered the ultra thick oil demulsifier of 1#.
Embodiment 2
With dihydroxyphenyl propane 150kg, triethylene tetramine 650kg, YLENE 300kg; Be warming up to 65 ℃ under stirring; Slowly drip 36.5% formaldehyde solution 300kg, continue heating and maintain the temperature at 90～105 ℃, after the reaction to terminal; Be-0.08 in 120 ℃ of vacuum tightnesss of temperature～-0.09MPa under dehydration, make phenol-amine resin.In autoclave, add the 70kg phenol-amine resin; 18.5kg catalyzer by 1: 1 composite forming of weight ratio, is warming up to 140 ℃ by calcium hydroxide and sodium acetate, the adjusting pressure range is 0.2～0.5MPa; Add propylene oxide 800kg; 120 ℃ add oxyethane 350kg down, and it is 0.2～0.4MPa at 120 ℃ of following control still pressure that polymerization gets block polyether high score adding oxyethane 290kg temperature control, and polymerization obtains the block polyether macromolecular compound.To synthesize in block polyether 900kg, fumaric acid 260kg, the catalyzer tosic acid 5kg input reaction kettle, and stir and heat up 140～150 ℃, divide till the dried up no longer increase to refluxing 50～60 minutes; Be cooled to 60～70 ℃, add fumaric acid 100kg, the initiator Lucidol 40kg that adds again after stirring; Be warming up to 170～180 ℃; React and accomplished esterification in 7～8 hours, promptly obtain the graft esterification demulsifier product, be numbered the ultra thick oil demulsifier of 4#.
Embodiment 5
With dihydroxyphenyl propane 1500kg, TEPA 600kg, YLENE 600kg; Drop in the reaction kettle, be warming up to 70 ℃ under stirring, slowly drip 37% formaldehyde solution 160kg; Continue heating and maintain the temperature at 90～95 ℃; After the reaction to terminal, be-0.08 in 120 ℃ of vacuum tightnesss of temperature～-dewater under the 0.09MPa, make phenol-amine resin.Adding 100kg phenol-amine resin, 18kg catalyzer are pressed 1: 1 weight ratio mixture by calcium hydroxide and glacial acetic acid in autoclave; Adding propylene oxide 900kg temperature control to 135～155 ℃; Adding oxyethane 200kg temperature control is 0.2～0.4MPa at 120 ℃ of following control still pressure, and polymerization obtains the block polyether macromolecular compound.To synthesize in block polyether 800kg, methylacrylic acid 260kg, the catalyzer tosic acid 5kg input reaction kettle, and stir and heat up 140～150 ℃, divide till the dried up no longer increase to refluxing 50～60 minutes; Be cooled to 60～70 ℃, add methylacrylic acid 80kg, the initiator Lucidol 36kg that adds again after stirring; Be warming up to 170～180 ℃; React and accomplished esterification in 7～8 hours, promptly obtain the graft esterification demulsifier product, be numbered the ultra thick oil demulsifier of 5#.
More than the product index of five kinds of ultra thick oil demulsifiers see table 1
The special thick oil demulsifier product index of table 1
Embodiment 6 surpasses the experiment of thick oil demulsifier demulsification
Experimentize with oil as emulsion splitter experiment of the present invention with the special viscous crude of Karamay oilfield, the trade names of using with the oil field simultaneously are reference example as KH-1 (certain University of Petroleum produces) and trade names as the emulsion splitter of KN-5 (Kelamayi chemical assistant factory product).The weight percent of crude oil water containing is 76%, and demulsifier concentration is 500ppm in the crude oil, and dehydration temperaturre is at 85～90 ℃.
With reference to the oil and gas industry standard SY/T5281-2000 of the People's Republic of China " crude oil demulsifier use properties detection method (bottle examination method) "; The special viscous crude in Kelamayi is carried out the test of bottle examination method breaking emulsion and dewatering under differing temps, the concussion method of dehydration trial jar adopts artificial concussion method in the test.
Concrete steps are following:
The crude oil emulsion sample is poured in the 100mL tool plug graduated cylinder (self-control dehydration trial jar) into water bath with thermostatic control heating 30min.In the dehydration trial jar, add a certain amount of crude oil demulsification agent solution with transfer pipet.Adopt the artificial hand shaking to swing method, amplitude is greater than 20cm, and the concussion number of times is 200 times, fully behind the mixing, becomes flexible bottle cap, and the trial jar that will dewater places the water bath with thermostatic control standing sedimentation again.The dehydrating amount of range estimation record different time, when stopping sedimentation, observational data sewage color and water-oil interface situation.
Table 2, table 3 are seen in special thick oil demulsifier demulsification experiment
90 ℃ of dehydration tests of table 2 to the special viscous crude in Kelamayi
80 ℃ of dehydration tests of table 3 to the special viscous crude in Kelamayi
Can find out that from last table the emulsion splitter of the present invention preparation has breaking emulsion and dewatering performance, especially emulsion splitter preferably to the special viscous crude in Kelamayi, temperature is 90 ℃, and when adding dose and being 500ppm, its maximum dehydration rate can reach more than 90%.
Claims (1)
1. the preparation method of the special thick oil demulsifier of a naphthenic base is characterized in that taking following steps:
1, the special thick oil demulsifier of a kind of naphthenic base; It is characterized in that it is is initiator with the modification phenol-amine resin, under catalyst action, carry out after the block polymerization again the multilayer shape that obtains with the unsaturated acid esterification graft modification, the modified polyether emulsion splitter monomer of many aromatic rings tridimensional network with propylene oxide and oxyethane.
2, the special thick oil demulsifier of naphthenic base according to claim 1 is characterized in that unsaturated acid comprises: one or more of unsaturated acid such as vinylformic acid, methylacrylic acid, maleic anhydride, toxilic acid and fumaric acid.
3, the special thick oil demulsifier preparation method of the said naphthenic base of claim 1, it is characterized in that this preparation process through the initiator phenol-amine resin synthetic, block polyether is synthetic, three steps of graft esterification reaction accomplish, concrete steps are following:
(1) phenol-amine resin is synthetic
Alkylphenol or dihydroxyphenyl propane, polyethylene polyamine and YLENE are joined in the reactor drum of band whipping appts; Be warming up to 50～90 ℃; Drip formaldehyde solution then, maintain the temperature at polyreaction under 65～115 ℃ of conditions, rise to 110～185 ℃ then and under reduced pressure, obtain the reddish-brown phenol-amine resin.Wherein aryl phenol, polyethylene polyamine are that the middle amount proportioning of 37% formaldehyde solution calculated is with weight percent concentration: 1: 0.5～20: 0.1～5
(2) block polyether is synthetic
Gained phenol-amine resin in the step (1) and catalyzer are joined in the reactor drum of airtight nitrogen protection; Stir; Be warming up to 120～150 ℃, the adjusting pressure range is 0.2～0.5MPa, adds propylene oxide and oxyethane successively and carries out polyreaction; Container inner pressure no longer changes promptly to be regarded as reacting and finishes, and obtains block polyether.Wherein the mass ratio of phenol-amine resin, propylene oxide and oxyethane is: 1: 80～140: 20～50.
(3) graft esterification reaction
Synthetic even collecting process two processes by unsaturated acid such as vinylformic acid and block polyether esterification process and high fat thing of graft esterification modification are formed; Specifically synthesis step is following: unsaturated acid such as block polyether, vinylformic acid, Catalyzed by p-Toluenesulfonic Acid agent are added in the reactor drum, stir the 30～60min that reflux that heat up 40～150 ℃, divide till the dried up no longer increase; Be cooled to 40～80 ℃; Add insatiable hunger acid such as quantitative vinylformic acid, add a certain amount of initiator Lucidol after stirring again, be warming up to 120～180 ℃; React and accomplished esterification in 2～8 hours, promptly obtain modified polyether monomer demulsifier product.
The weight proportion that feeds intake is: catalyzer: unsaturated acid such as vinylformic acid: block polyether=0.5: 1～30: 30～100
Said initiator Lucidol accounts for 7～12% of unsaturated acid such as vinylformic acid batching gross weight.
Described unsaturated acid comprises one or more of unsaturated acid such as vinylformic acid, methylacrylic acid, maleic anhydride, toxilic acid and fumaric acid.
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