CN102746470B - 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 Petroleum Processing Technology field.
Background technology
Crude oil, in recovery process, due to contacting of crude oil and water, adds the effect of the naturally occurring emulsifying agent in crude oil, makes crude oil and water form stable milk sap.Make emulsification of crude oil serious.In order to reach the requirement of crude oil exporting, just need to carry out breakdown of emulsion to crude oil, crude oil is separated with water.Along with tertiary oil recovery technology is promoted, a large amount of uses of the technology of reservoir sweep such as surfactant flooding, polymer flooding have all caused great impact to crude Treatment, change the state of conventional crude Produced Liquid, in emulsion of crude oil, not only water ratio increases, and stability enhancing, the especially output of viscous crude, special viscous crude increase and make breakdown of emulsion process become complicated.Another unfavorable factor is the energy consumption problem in breakdown of emulsion process, causes Produced Liquid processing cost cumulative year after year, the corresponding processing cost that also increases crude oil Produced Liquid.
The emulsion splitter that at present domestic each oil field is used, mainly taking polyether type demulsifying agent as main, for the crude oil feature in each oil field, improves polyether type demulsifying agent, its basic line for changing head, change tail, add bone, adjust and weigh and composite.As Chinese patent CN1037094A discloses a kind of formula of efficient thick-oil emulsion splitter, adopt the mixture of a kind of alkylphenol and another kind of phenol and formaldehyde condensation to obtain resol, with sulfation after oxyethane, propylene oxide block copolymerization etherificate.Show as bad adaptability for the special viscous crude result of use of cycloalkyl, de-emulsification speed is very slow, finally deviates from the water yield low, and breakdown of emulsion process graded is not obvious.And emulsion splitter consumption requires the shortcomings such as large.
Chinese patent CN1810933A thick oil demulsifier and preparation method thereof, open thick oil demulsifier product is suitable for the special thick oil emulsion breaking in Liaohe Oil Field, is not suitable for the special consistency crude oil breakdown of emulsion of Karamy area.
The crude oil of the super viscous crude heavy oil block of Oil Field In Karamay Area cycloalkyl, oil product has that density is large, viscosity is large, wax content is high, moisture height, intractability are larger.Now use demulsifier product main manifestations to have the problems such as breakdown of emulsion temperature is high, and dosage is large, and dewatering speed is undesirable for solving prior art.
That the present invention has is quick, the feature of low dosage.Be applicable to the super viscous crude field heavy oil dehydration of Kelamayi cycloalkyl, require temperature to be applicable to dehydration fast, dehydration rate is high, and water colour is clear, water-oil interface are neat.
Summary of the invention
The object of this invention is to provide a kind of particularly suitable Karamy area in the high-efficient demulsifier of the special consistency crude oil of cycloalkyl.
Technical scheme of the present invention is as follows:
The special thick oil demulsifier of a kind of cycloalkyl, it is characterized in that it is taking modification phenol-amine resin as initiator, under catalyst action, carry out after block polymerization again the multilayer shape obtaining with 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 comprises the following steps:
1, phenol-amine resin is synthetic
Alkylphenol or dihydroxyphenyl propane, polyethylene polyamine and dimethylbenzene are joined in the reactor with whipping appts, be warming up to 50～90 DEG C, then drip formaldehyde solution, maintain the temperature at polyreaction under 65～115 DEG C of conditions, then rise to 110～185 DEG C and dewater and obtain reddish-brown phenol-amine resin under reduced pressure.Wherein the middle amount proportioning of aryl phenol, the formaldehyde solution of polyethylene polyamine taking weight percent concentration as 37% calculating as: 1: 0.5～20: 0.1～5
Described aromatic ring phenol comprises phenol, dihydroxyphenyl propane
Described alkylphenol comprises nonyl phenol, octyl phenol
Described polyethylene polyamine comprises triethylene tetramine, tetraethylene pentamine, five ethene hexamines
2, block polyether is synthetic
Gained phenol-amine resin and catalyzer in step 1 are joined in the reactor of airtight nitrogen protection; stir; be warming up to 130～140 DEG C; adjusting pressure range is 0.2～0.5MPa; add successively propylene oxide and oxyethane to carry out polyreaction, container inner pressure no longer changes to be considered 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: potassium hydroxide, Potassium ethanoate, calcium hydroxide, an acidic catalyst comprises citric acid, glacial acetic acid, tartrate.Catalyst levels for the two part by weight be 1: 1.
Described an acidic catalyst comprises glacial acetic acid, oxalic acid, tartrate.
3, graft esterification reaction
Graft esterification modification is synthetic to be made up of even collecting process two processes of the unsaturated acid such as vinylformic acid and block polyether esterification process and high fat thing, concrete synthesis step is as follows: by block polyether, the unsaturated acid such as vinylformic acid, Catalyzed by p-Toluenesulfonic Acid agent adds in reactor, stirring heats up 40～150 DEG C refluxes 30～60 minutes, till Separation of Water no longer increases, be cooled to 40～80 DEG C, add a certain amount of vinylformic acid, after stirring, add again quantitative initiator benzoyl peroxide, be warming up to 120～180 DEG C, react and within 2～8 hours, complete esterification, obtain modified polyether monomer demulsifier product.
Weight proportion is: catalyzer: the unsaturated acid such as vinylformic acid: block polyether=0.5: 1～30: 30～100.
Initiator benzoyl peroxide accounts for 7～12% of the unsaturated acid batching gross weights such as vinylformic acid
Described unsaturated acid comprises one or more of the unsaturated acid such as vinylformic acid, methacrylic 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 rapidly water-oil interface in special viscous crude, greatly falls
2, block polyether is synthetic
Gained phenol-amine resin and catalyzer in step 1 are joined in the reactor of airtight nitrogen protection; stir; be warming up to 130～140 DEG C; adjusting pressure range is 0.2～0.5MPa; add successively propylene oxide and oxyethane to carry out polyreaction, container inner pressure no longer changes to be considered 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: potassium hydroxide, Potassium ethanoate, calcium hydroxide, an acidic catalyst comprises citric acid, glacial acetic acid, tartrate.Catalyst levels for the two part by weight be 1: 1.
Described an acidic catalyst comprises glacial acetic acid, oxalic acid, tartrate.
3, graft esterification reaction
Graft esterification modification is synthetic to be made up of even collecting process two processes of the unsaturated acid such as vinylformic acid and block polyether esterification process and high fat thing, concrete synthesis step is as follows: by block polyether, the unsaturated acid such as vinylformic acid, Catalyzed by p-Toluenesulfonic Acid agent adds in reactor, stirring heats up 40～150 DEG C refluxes 30～60 minutes, till Separation of Water no longer increases, be cooled to 40～80 DEG C, add a certain amount of vinylformic acid, after stirring, add again quantitative initiator benzoyl peroxide, be warming up to 120～180 DEG C, react and within 2～8 hours, complete esterification, obtain modified polyether monomer demulsifier product.
Weight proportion is: catalyzer: the unsaturated acid such as vinylformic acid: block polyether=0.5: 1～30: 30～100.
Initiator benzoyl peroxide accounts for 7～12% of the unsaturated acid batching gross weights such as vinylformic acid
Described unsaturated acid comprises one or more of the unsaturated acid such as vinylformic acid, methacrylic 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 rapidly water-oil interface in special viscous crude, greatly reduce elasticity and the viscosity of interfacial film, accelerate the gathering of drop, reach the object of efficient fast emulsion breaking.It is simple that the special thick oil demulsifier of the cycloalkyl that provides has synthesis technique, operational condition gentleness, and tooling cost is low, is convenient to suitability for industrialized production, to advantages such as the special thick oil emulsion breaking in Karamy area are effective.
Embodiment
Embodiment 1
By phenol 100kg, tetraethylene pentamine 550kg, dimethylbenzene 200kg, drop in reactor, under stirring, be warming up to 60 DEG C, slowly drip 37% formaldehyde solution 210kg, continue heating and maintain the temperature at 90～95 DEG C, after reaction to terminal, be to dewater under-0.08～-0.09MPa in 120 DEG C of vacuum tightnesss of temperature, make phenol-amine resin.To add in autoclave 50kg phenol-amine resin, 15kg catalyzer by potassium hydroxide and glacial acetic acid according to by 1: 1 composite forming of weight ratio, add propylene oxide 750kg temperature control to 135～155 DEG C, adding oxyethane 200kg temperature control at 120 DEG C, to control still pressure is 0.2～0.4MPa, and polymerization obtains block polyether macromolecular compound.To synthesize in block polyether 700kg, vinylformic acid 200kg, catalyzer tosic acid 5kg input reactor, stir and heat up 130～145 DEG C to refluxing 40～60 minutes, till Separation of Water no longer increases, be cooled to 50～75 DEG C, add vinylformic acid 50kg, the initiator benzoyl peroxide 25kg adding again after stirring, be warming up to 145～180 DEG C, react and within 4～6 hours, complete esterification, obtain graft esterification demulsifier product, be numbered the super thick oil demulsifier of 1#.
Embodiment 2
By dihydroxyphenyl propane 150kg, triethylene tetramine 650kg, dimethylbenzene 300kg, under stirring, be warming up to 65 DEG C, slowly drip 36.5% formaldehyde solution 300kg, continue heating and maintain the temperature at 90～105 DEG C, after reaction to terminal, be to dewater under-0.08～-0.09MPa in 120 DEG C of vacuum tightnesss of temperature, make phenol-amine resin.In autoclave, add 70kg phenol-amine resin, 18.5kg catalyzer by calcium hydroxide and sodium acetate by 1: 1 composite forming of weight ratio, be warming up to 140 DEG C, adjusting pressure range is 0.2～0.5MPa, add propylene oxide 800kg, at 120 DEG C, add oxyethane 350kg, polymerization obtains block polyether high score, and to add oxyethane 290kg temperature control at 120 DEG C, to control still pressure be 0.2～0.4MPa, and polymerization obtains block polyether macromolecular compound.To synthesize in block polyether 900kg, fumaric acid 260kg, catalyzer tosic acid 5kg input reactor, stir and heat up 140～150 DEG C to refluxing 50～60 minutes, till Separation of Water no longer increases, be cooled to 60～70 DEG C, add fumaric acid 100kg, the initiator benzoyl peroxide 40kg adding again after stirring, be warming up to 170～180 DEG C, react and within 7～8 hours, complete esterification, obtain graft esterification demulsifier product, be numbered the super thick oil demulsifier of 4#.
Embodiment 5
By dihydroxyphenyl propane 1500kg, tetraethylene pentamine 600kg, dimethylbenzene 600kg, drop in reactor, under stirring, be warming up to 70 DEG C, slowly drip 37% formaldehyde solution 160kg, continue heating and maintain the temperature at 90～95 DEG C, after reaction to terminal, be to dewater under-0.08～-0.09MPa in 120 DEG C of vacuum tightnesss of temperature, make phenol-amine resin.To add in autoclave 100kg phenol-amine resin, 18kg catalyzer by calcium hydroxide and glacial acetic acid by 1: 1 weight ratio mixture, add propylene oxide 900kg temperature control to 135～155 DEG C, adding oxyethane 200kg temperature control at 120 DEG C, to control still pressure is 0.2～0.4MPa, and polymerization obtains block polyether macromolecular compound.To synthesize in block polyether 800kg, methacrylic acid 260kg, catalyzer tosic acid 5kg input reactor, stir and heat up 140～150 DEG C to refluxing 50～60 minutes, till Separation of Water no longer increases, be cooled to 60～70 DEG C, add methacrylic acid 80kg, the initiator benzoyl peroxide 36kg adding again after stirring, be warming up to 170～180 DEG C, react and within 7～8 hours, complete esterification, obtain graft esterification demulsifier product, be numbered the super thick oil demulsifier of 5#.
The product index of above five kinds of super thick oil demulsifiers is in table 1
The special thick oil demulsifier product index of table 1
Embodiment 6 surpasses the experiment of thick oil demulsifier demulsification
Test with oil as emulsion splitter experiment of the present invention using the special viscous crude of Karamay oilfield, the trade names that using taking oil field 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) simultaneously.The weight percent of crude oil water containing is 76%, and in crude oil, demulsifier concentration is 500ppm, and dehydration temperaturre is at 85～90 DEG C.
With reference to the oil and gas industry standard SY/T5281-2000 of the People's Republic of China (PRC) " crude oil demulsifier use properties detection method (bottle examination method) ", the special viscous crude in Kelamayi is carried out to the test of bottle examination method breaking emulsion and dewatering under differing temps, and in test, the concussion method of dehydration test bottle adopts artificial concussion method.
Concrete steps are as follows:
Crude oil emulsion sample is poured in 100mL tool plug graduated cylinder (self-control dehydration test bottle) into water bath with thermostatic control heating 30min.In dehydration test bottle, add a certain amount of crude oil demulsification agent solution with transfer pipet.Adopt artificial hand shaking to swing method, amplitude is greater than 20cm, and concussion number of times is 200 times, and after fully mixing, loosening bottle cap, is placed in water bath with thermostatic control standing sedimentation again by dehydration test bottle.The dehydrating amount of different time is recorded in range estimation, while stopping sedimentation, and observational data sewage color and water-oil interface situation.
Special thick oil demulsifier demulsification is tested in table 2, table 3
90 DEG C, table 2 dehydration test to the special viscous crude in Kelamayi
80 DEG C, table 3 dehydration test to the special viscous crude in Kelamayi
As can be seen from the above table, emulsion splitter prepared by the present invention has good breaking emulsion and dewatering performance, especially emulsion splitter to the special viscous crude in Kelamayi, and temperature is 90 DEG C, and when chemical feeding quantity is 500ppm, its maximum dehydration rate can reach more than 90%.
Claims (1)
1. a preparation method for the special thick oil demulsifier of cycloalkyl, is characterized in that taking following steps:
By dihydroxyphenyl propane 1500kg, tetraethylene pentamine 600kg, dimethylbenzene 600kg, drop in reactor, under stirring, be warming up to 70 DEG C, slowly drip 37% formaldehyde solution 160kg, continue heating and maintain the temperature at 90～95 DEG C, after reaction to terminal, be to dewater under-0.08～-0.09MPa in 120 DEG C of vacuum tightnesss of temperature, make phenol-amine resin; To add in autoclave 100kg phenol-amine resin, 18kg catalyzer by calcium hydroxide and glacial acetic acid by 1: 1 weight ratio mixture, add propylene oxide 900kg temperature control to 135～155 DEG C, adding oxyethane 200kg temperature control at 120 DEG C, to control still pressure is 0.2～0.4MPa, and polymerization obtains block polyether macromolecular compound; To synthesize in block polyether 800kg, methacrylic acid 260kg, catalyzer tosic acid 5kg input reactor, stir and heat up 140～150 DEG C to refluxing 50～60 minutes, till Separation of Water no longer increases, be cooled to 60～70 DEG C, add methacrylic acid 80kg, the initiator benzoyl peroxide 36kg adding again after stirring, be warming up to 170～180 DEG C, react and within 7～8 hours, complete esterification, obtain graft esterification demulsifier product, super thick oil demulsifier.
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Inventor after: Wang Mingxian Inventor after: Liu Li Inventor after: Shen Nana Inventor after: Wang Xinlong Inventor after: Xu Haitao Inventor after: Li Yujun Inventor after: Yang Li Inventor after: Wu Weilong Inventor after: Li Qionghong Inventor before: Wang Mingxian Inventor before: Wang Xinlong Inventor before: Xu Haitao Inventor before: Li Yujun Inventor before: Yang Li Inventor before: Wu Weilong |
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Free format text: CORRECT: INVENTOR; FROM: WANG MINGXIAN WANG XINLONG XU HAITAO LI YUJUN YANG LI WU WEILONG TO: WANG MINGXIAN LIU LI SHEN NANA WANG XINLONG XU HAITAO LI YUJUN YANG LI WU WEILONG LI QIONGHONG |
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Owner name: KARAMAY TIANMING CHEMICAL CO., LTD. Free format text: FORMER NAME: KARAMAY AOKE CHEMICAL CO., LTD. |
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Address after: The three town Jianshe Road Karamay city the Xinjiang Uygur Autonomous Region 834007 white base No. 88 Patentee after: KARAMAY TIANMING CHEMICAL CO., LTD. Address before: The three town Jianshe Road Karamay city the Xinjiang Uygur Autonomous Region 834007 white base No. 88 Patentee before: Karamay Aoke Chemical Co., Ltd. |