CN102492460A - Preparation method and application of crude oil low-temperature demulsifier - Google Patents
Preparation method and application of crude oil low-temperature demulsifier Download PDFInfo
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Abstract
The invention relates a preparation method of crude oil demulsifier. The preparation method comprises three steps, namely preparation of polyethylene polyamine polyether, preparation of alkylphenol polyether and preparation of demulsifier. The demulsifier provided by the invention has high demulsification dehydration speed at the low temperature of 34-38 DEG C, dehydration rate is more than 90%, heating energy can be saved greatly for an oil field, and demulsification dehydration cost of the crude oil is obviously reduced. Thus, application of the demulsifier has significance to the production, gathering and transportation process of crude oil and environment protection.
Description
Technical field:
The present invention relates to a kind of crude oil low-temperature demulsifying agent preparation method and application thereof.
Background technology:
Along with oil-field development gets into the later stage, the exploitation in domestic many oil fields gets into high water-cut stage, again
Add that steam drives, intensified oil reduction The Application of Technology such as polymer flooding, surfactant flooding and ternary composite driving; Cause the crude oil emulsion water cut to increase severely; Especially the existence of chemical oil displacement agent is become better and better the stability of crude oil emulsion; The breakdown of emulsion difficulty strengthens, and the dehydrating of crude oil difficulty increases, and existing emulsion splitter far can not adapt to the needs of the breaking emulsion and dewatering processing of high water-content crude oil or viscous crude, waxy crude oil.And problem such as each oil field ubiquity breakdown of emulsion temperature is high at present, dosage is big, dewatering speed is undesirable not only causes the huge waste of the energy and remaining high of processing cost; And the long processing period of crude oil; Therefore, make under the crude oil water containing prerequisite up to standard, reducing as much as possible
Dehydration temperaturre and emulsion splitter dosage become the difficult problem that the oil field needs to be resolved hurrily, and the development of low temperature rapid demulsifier is imperative.
The big major cause of conventional emulsion splitter low temperature dewatering difficulty is: the dehydrating of crude oil temperature reduces, and milk sap viscosity increases, and the emulsion splitter molecule is difficult the dispersion in crude oil, and is slack-off to the travelling speed of oil-water interfacial film from oil phase; Originally the paraffin that was dissolved state in the crude oil is when being lower than the crude oil wax precipitation temperature, and crystallization is separated out from crude oil gradually, influence emulsion splitter diffusion and the displacement of the replacement on oil-water interfacial film thereof, thereby the interfacial film that influences milk sap breaks; The profit density difference diminishes during low temperature dewatering, and the drops of water fall down speed of same particle diameter is slack-off, behind the emulsion breakdown oily water separation time longer, form the middle transition band easily.
Therefore, the emulsion splitter that is applicable to the crude oil low temperature dewatering also should possess certain low-temperature demulsification viscosity reduction and suppress the ability that the wax partial crystallization goes out except that should possessing stronger surfactivity, good wettability, very high agglutinating power.
Summary of the invention:
In order to solve problems such as the breakdown of emulsion temperature that prior art exists is high, dosage is big, dewatering speed is undesirable; The objective of the invention is to the defective or the deficiency that exist in the prior art; The breakdown of emulsion temperature that has overcome the current techniques existence is high, dosage is big, dewatering speed waits shortcoming slowly; A kind of preparation technology who is applicable to the low-temperature demulsifying agent of crude oil is provided, and this emulsion splitter has breaking emulsion and dewatering speed faster under 34～38 ℃ of lower temperatures, and dehydration rate reaches more than 90%; Not only can be a large amount of heating energy source of oil field saving, and significantly reduce the breaking emulsion and dewatering cost of crude oil.Therefore, the application of this emulsion splitter is all significant to defeated process of crude production and collection and environment protection.
The present invention is realized by following technical scheme:
(1) preparation of polyethylene polyamine polyethers:
The polyethylene polyamine that in reaction kettle, adds 1.5～6 parts, 3 ~ 5 parts Pottasium Hydroxide starts stirring, heat temperature raising to 120 ℃, finds time, fills nitrogen, then slowly adds 370 ~ 410 parts 125 ~ 145 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; Slowly add 83 ~ 91 parts of oxyethane again behind the reaction 0.5h; 125 ~ 145 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; 0.5h the last propylene oxide that slowly adds 370 ~ 410 parts in back, 125 ~ 145 ℃ of reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains the polyethylene polyamine polyethers.
(2) preparation of alkyl phenol polyether:
The alkylphenol that in reaction kettle, adds 21～29 parts, 3 ~ 5 parts Pottasium Hydroxide starts stirring, heat temperature raising to 120 ℃, finds time, fills nitrogen, then slowly adds 436 ~ 501 parts 125 ~ 145 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; Slowly add 290 ~ 310 parts of oxyethane again behind the reaction 0.5h; 125 ~ 145 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains alkyl phenol polyether.
(3) preparation of low-temperature demulsifying agent:
With weight percent is that 35 ~ 45% water adds enamel and is mixed in the still; Start stirring, be warming up to 50 ℃; And then weight percent is 12 ~ 18% polyethylene polyamine polyethers, 21 ~ 27% alkyl phenol polyethers, adds enamel and be mixed in the still add 15 ~ 25% methyl alcohol again after stirring 30 min, adding weight ratio at last is 0.3 ~ 0.5% pour point depressant; Stir 30～60min, cooling discharge obtains low-temperature demulsifying agent.
The invention has the beneficial effects as follows: the cryogenic dewatering demulsifier of crude-oil extract that adopts present method preparation; The dehydrating of crude oil temperature is in the time of 34～38 ℃, and dosage is in 30 ~ 50mg/L scope, and it is moisture less than 0.2% that crude oil takes off the back; Sewage with oil reaches the crude oil exporting standard less than 500mg/L.
Embodiment:
Below in conjunction with specific examples the present invention is described further.
Embodiment 1,
(1) preparation of polyethylene polyamine polyethers:
The triethylene tetramine that in reaction kettle, adds 3.7 kilograms, 5 kilograms Pottasium Hydroxide starts stirrings, heat temperature raising to 120 ℃, finds time, fills nitrogen, 125 ~ 130 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, the temperature of reaction of then slowly 387 kilograms of addings; Slowly add 84 kilograms of oxyethane again behind the reaction 0.5h; 125 ~ 130 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; 0.5h the last propylene oxide that slowly adds 387 kilograms in back, 125 ~ 145 ℃ of reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains the triethylene tetramine polyethers.
(2) preparation of alkyl phenol polyether:
The NP that in reaction kettle, adds 23 kilograms, 3 kilograms Pottasium Hydroxide starts stirrings, heat temperature raising to 120 ℃, finds time, fills nitrogen, 130 ~ 135 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, the temperature of reaction of then slowly 439 kilograms of addings; Slowly add 297 kilograms of oxyethane again behind the reaction 0.5h; 125 ~ 130 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains the NP polyethers.
(3) preparation of low-temperature demulsifying agent:
With weight percent is that 45% water adds enamel and is mixed in the still; Start stirring, be warming up to 50 ℃; And then weight percent is 17.5% triethylene tetramine polyethers, 22% NP polyethers, adds enamel and be mixed in the still add 15% methyl alcohol again after stirring 30 min, adding weight ratio at last is 0.5% polyethylene vinyl acetate ester pour point depressant; Stir 50min, cooling discharge obtains low-temperature demulsifying agent.
Embodiment 2
(1) preparation of polyethylene polyamine polyethers:
The diethylenetriamine that in reaction kettle, adds 2.8 kilograms, 3.5 kilograms Pottasium Hydroxide starts stirrings, heat temperature raising to 120 ℃, finds time, fills nitrogen, 125 ~ 130 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, the temperature of reaction of then slowly 379 kilograms of addings; Slowly add 84 kilograms of oxyethane again behind the reaction 0.5h; 130 ~ 135 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; 0.5h the last propylene oxide that slowly adds 379 kilograms in back, 125 ~ 145 ℃ of reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains the diethylenetriamine polyethers.
(2) preparation of alkyl phenol polyether:
The octyl phenol that in reaction kettle, adds 24 kilograms, 3.4 kilograms Pottasium Hydroxide starts stirrings, heat temperature raising to 120 ℃, finds time, fills nitrogen, 130 ~ 135 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, the temperature of reaction of then slowly 457 kilograms of addings; Slowly add 301 kilograms of oxyethane again behind the reaction 0.5h; 125 ~ 130 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains the octyl phenol polyethers.
(3) preparation of low-temperature demulsifying agent:
With weight percent is that 41% water adds enamel and is mixed in the still; Start stirring, be warming up to 50 ℃; And then weight percent is 15.6% diethylenetriamine polyethers, 23% octyl phenol polyethers, adds enamel and be mixed in the still add 20% methyl alcohol again after stirring 30 min, adding weight ratio at last is 0.4% polyethylene vinyl acetate ester pour point depressant; Stir 60min, cooling discharge obtains low-temperature demulsifying agent.
Embodiment 3,
(1) preparation of polyethylene polyamine polyethers:
The TEPA that in reaction kettle, adds 5.1 kilograms, 5 kilograms Pottasium Hydroxide starts stirrings, heat temperature raising to 120 ℃, finds time, fills nitrogen, 135 ~ 140 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, the temperature of reaction of then slowly 407 kilograms of addings; Slowly add 87 kilograms of oxyethane again behind the reaction 0.5h; 130 ~ 135 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; 0.5h the last propylene oxide that slowly adds 407 kilograms in back, 135 ~ 140 ℃ of reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains the TEPA polyethers.
(2) preparation of alkyl phenol polyether:
The NP that in reaction kettle, adds 27 kilograms, 3 kilograms Pottasium Hydroxide starts stirrings, heat temperature raising to 120 ℃, finds time, fills nitrogen, 130 ~ 135 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, the temperature of reaction of then slowly 486 kilograms of addings; Slowly add 310 kilograms of oxyethane again behind the reaction 0.5h; 125 ~ 130 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains the NP polyethers.
(3) preparation of low-temperature demulsifying agent:
With weight percent is that 41% water adds enamel and is mixed in the still; Start stirring, be warming up to 50 ℃; And then weight percent is 12% TEPA polyethers, 21.7% NP polyethers, adds enamel and be mixed in the still add 25% methyl alcohol again after stirring 30 min, adding weight ratio at last is 0.3% pour point depressant; Stir 30min, cooling discharge obtains low-temperature demulsifying agent.
Embodiment 4,
(1) preparation of polyethylene polyamine polyethers:
The diethylenetriamine that in reaction kettle, adds 2.7 kilograms, 3 kilograms Pottasium Hydroxide starts stirrings, heat temperature raising to 120 ℃, finds time, fills nitrogen, 125 ~ 130 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, the temperature of reaction of then slowly 391 kilograms of addings; Slowly add 89 parts of oxyethane again behind the reaction 0.5h; 130 ~ 135 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; 0.5h the last propylene oxide that slowly adds 391 kilograms in back, 125 ~ 145 ℃ of reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains divinyl three polyethers.
(2) preparation of alkyl phenol polyether:
The two NPs that in reaction kettle, add 29 kilograms, 5 kilograms Pottasium Hydroxide starts stirrings, heat temperature raising to 120 ℃, finds time, fills nitrogen, 125 ~ 145 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, temperature of reaction that then slow adding is 501 kilograms; Slowly add 307 kilograms of oxyethane again behind the reaction 0.5h; 140 ~ 145 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains two NP polyethers.
(3) preparation of low-temperature demulsifying agent:
With weight percent is that 43.7% water adds enamel and is mixed in the still; Start stirring, be warming up to 50 ℃; And then weight percent is 13% diethylenetriamine polyethers, the 23% pair of NP polyethers, adds enamel and be mixed in the still add 20% methyl alcohol again after stirring 30 min, adding weight ratio at last is 0.3% phenylethylene-maleic anhydride-Yodo Sol GH 28 pour point depressant; Stir 60min, cooling discharge obtains low-temperature demulsifying agent.
Embodiment 5,
(1) preparation of polyethylene polyamine polyethers:
The triethylene tetramine that in reaction kettle, adds 5.7 kilograms, 4.1 kilograms Pottasium Hydroxide starts stirrings, heat temperature raising to 120 ℃, finds time, fills nitrogen, 135 ~ 140 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, the temperature of reaction of then slowly 407 kilograms of addings; Slowly add 88 kilograms of oxyethane again behind the reaction 0.5h; 125 ~ 145 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; 0.5h the last propylene oxide that slowly adds 407 kilograms in back, 135 ~ 140 ℃ of reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains the triethylene tetramine polyethers.
(2) preparation of alkyl phenol polyether:
The octyl phenol that in reaction kettle, adds 26.7 kilograms, 3.9 kilograms Pottasium Hydroxide starts stirrings, heat temperature raising to 120 ℃, finds time, fills nitrogen, 135 ~ 140 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, the temperature of reaction of then slowly 493 kilograms of addings; Slowly add 298 kilograms of oxyethane again behind the reaction 0.5h; 140 ~ 145 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains the octyl phenol polyethers.
(3) preparation of low-temperature demulsifying agent:
With weight percent is that 36.7% water adds enamel and is mixed in the still; Start stirring, be warming up to 50 ℃; And then weight percent is 14% triethylene tetramine polyethers, 24% octyl phenol polyethers, adds enamel and be mixed in the still add 25% methyl alcohol again after stirring 30 min, adding weight ratio at last is 0.3% pour point depressant; Stir 40min, cooling discharge obtains low-temperature demulsifying agent.
The low-temperature demulsifying agent dehydrating effect is estimated:
Experiment uses crude oil to be grand celebration six factory's loudspeakers, the two joint station crude oil that recover the oil.
Accepted standard:
GB/T 8929 detecting crude oil water content method distillation method
SY/T 5281 emulsion splitter use properties detection method bottles examination method
SY/T 5329 petroclastic rock oil-bearing stratum flooding water quality are recommended index and analytical procedure
Table 1 low-temperature demulsifying agent testing data:
Claims (5)
1. the preparation method of a crude oil demulsifier, this method was accomplished through preparation, the preparation of alkyl phenol polyether, three steps of emulsion splitter preparation of polyethylene polyamine polyethers, and concrete preparation process is following:
(1) preparation of polyethylene polyamine polyethers:
The polyethylene polyamine that in reaction kettle, adds 1.5～6 parts, 3 ~ 5 parts Pottasium Hydroxide starts stirring, heat temperature raising to 120 ℃, finds time, fills nitrogen, then slowly adds 370 ~ 410 parts 125 ~ 145 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; Slowly add 83 ~ 91 parts of oxyethane again behind the reaction 0.5h; 125 ~ 145 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; 0.5h the last propylene oxide that slowly adds 370 ~ 410 parts in back, 125 ~ 145 ℃ of reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains the polyethylene polyamine polyethers;
(2) preparation of alkyl phenol polyether:
The alkylphenol that in reaction kettle, adds 21～29 parts, 3 ~ 5 parts Pottasium Hydroxide starts stirring, heat temperature raising to 120 ℃, finds time, fills nitrogen, then slowly adds 436 ~ 501 parts 125 ~ 145 ℃ of propylene oxide reaction pressure 0.25 ~ 0.3MPa, temperature of reaction; Slowly add 290 ~ 310 parts of oxyethane again behind the reaction 0.5h; 125 ~ 145 ℃ of reaction pressure 0.2 ~ 0.25MPa, temperature of reaction; React after 1 hour question response still internal pressure reduces to zero, cooling discharge obtains alkyl phenol polyether;
(3) preparation of emulsion splitter:
With weight percent is that 35 ~ 45% water adds enamel and is mixed in the still; Start stirring, be warming up to 50 ℃; And then weight percent is 12 ~ 18% polyethylene polyamine polyethers, 21 ~ 27% alkyl phenol polyethers, adds enamel and be mixed in the still add 15 ~ 25% methyl alcohol again after stirring 30 min, adding weight ratio at last is 0.3 ~ 0.5% pour point depressant; Stir 30～60min, cooling discharge obtains emulsion splitter; Above-mentioned each raw material by weight ratio.
2. the preparation method of crude oil demulsifier according to claim 1, it is characterized in that: polyethylene polyamine is one or more mixtures in quadrol, diethylenetriamine, triethylene tetramine, TEPA and the five ethene hexamines.
3. the preparation method of crude oil demulsifier according to claim 1, it is characterized in that: alkylphenol is one or more mixtures in octyl phenol, NP and the two NP.
4. according to the preparation method of the described crude oil demulsifier of claim l, it is characterized in that: pour point depressant is one or more in polyethylene vinyl acetate ester, phenylethylene-maleic anhydride-Yodo Sol GH 28 and the maleic acid anhydride-propenoic acid ester copolymer.
5. the alkyl benzene amine carboxylate anion tensio-active agent of the described method of claim l preparation, the low-temperature demulsifying agent that oily water separation is used as crude oil low temperature.
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| CN112159679A (en) * | 2020-10-20 | 2021-01-01 | 克拉玛依新科澳石油天然气技术股份有限公司 | Demulsifier for dehydrating foam-containing crude oil and preparation method thereof |
| CN113717750A (en) * | 2021-01-20 | 2021-11-30 | 万达集团股份有限公司 | Demulsifier suitable for crude oil with high wax content |
| CN113003633A (en) * | 2021-04-30 | 2021-06-22 | 西南石油大学 | Dendritic water clarifier for polymer-containing oily sewage treatment and preparation method thereof |
| CN115746901A (en) * | 2022-10-26 | 2023-03-07 | 中石化石油工程技术服务有限公司 | Compound demulsifier and application thereof, and method for treating polymer-containing produced liquid in oil field through physicochemical coupling |
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Application publication date: 20120613 |