CN102286273B - Oil-in-water emulsifier as well as preparation and use methods thereof - Google Patents
Oil-in-water emulsifier as well as preparation and use methods thereof Download PDFInfo
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- CN102286273B CN102286273B CN201110260025.1A CN201110260025A CN102286273B CN 102286273 B CN102286273 B CN 102286273B CN 201110260025 A CN201110260025 A CN 201110260025A CN 102286273 B CN102286273 B CN 102286273B
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Abstract
The invention discloses a high temperature resistant oil-in-water emulsifier with high performance. The oil-in-water emulsifier is prepared through the following steps: adding 850-860kg of illegal cooking oil into a 2000L enamel reactor, then adding 510-520kg of tetraethylenepentamine and 25-30kg of 20% sodium hydroxide aqueous solution, introducing steam by a jacket for heating and starting up stirring; in the process of raising the temperature, recovering water generated by reaction by a condensing reflux water division device, and beginning to boil a reaction material when the temperature is raised to 180-190 DEG C, continuously raising the temperature, keeping the temperature at 230-250 DEG C to heat for 40min, then stopping heating, and reducing the temperature by introducing cooling water through the jacket; and cooling the reaction material to the room temperature, and then discharging and barreling. The reasonable utilization of wastes is realized, the illegal cooking oil harmful to human bodies is prevented from entering fast-food restaurants and wineshops, and an environment-friendly, healthy and safe solution is provided for solving the illegal cooking oil problem.
Description
Technical field
The present invention relates to drilling well and oil recovery technique field, particularly a kind of preparation method and using method of high temperature resistance high-performance oil-water emulsifiers.
Background technology
Oil-in-water emulsion drilling fluid system is mainly used in solving some low holes, hypotonic, seam hole and grows easy leakage, drilling well reservoir protection problem and a deep-well under-balanced drilling technology difficult problem that reservoir pressure coefficient is low.It is made up of water, oil phase, emulsifying agent and other inorganic agent, and wherein water is the foreign minister, and oil phase is interior phase.Its advantage is as follows: the system stable performance, and the temperature resistance ability is strong, good fluidity, filter loss is low, and the stabilizing borehole ability is stronger; Its density is lower than common drilling fluid system, and is minimum to formation damage during under balance pressure drilling, is conducive to liberate oil-gas Layer, improves the oil gas well capacity; The generation that helps to improve rate of penetration and prevent leakage does not influence electrical measurement and nuclear magnetic resonance log.The oil-in-water emulsion drilling fluid belongs to a kind of thermodynamic unstable system, and the main factor that influences its stability is oil-in-water emulsifiers, is the stable key of emulsion system.The main effect of oil-in-water emulsifiers be exactly with oil and two kinds of immiscible liquid of water the emulsification by emulsifying agent to form oil be that decentralized photo, water are the emulsion of continuous phase.Say that in principle the emulsifying agent of HLB value (hydrophilic lipophilic balance) in 8～18 scopes all can be used as the emulsifying agent of oil-in-water emulsion drilling fluid.But the emulsifying effectiveness of at present domestic oil-water emulsifiers is undesirable, and high temperature resistant property is poor, is difficult to satisfy the requirement of deep-well oil-in-water emulsion drilling fluid, therefore is necessary to develop a kind of high temperature-resisting oil-in-water type emulsifying agent.
Simultaneously, China's waterflooding oil field (its reserves and output all account for the whole nation more than 80%) method of improving recovery ratio is mainly chemical flooding (alkali drives, polymer flooding, surfactant flooding etc.).In recent ten years, combination flooding (alkali, surfactant and polymer compound) is shown one's talent from chemical flooding, becomes one of method of tool application prospect.And the performance of surfactant is to determine the successful key of chemical flooding (surfactant flooding contains the combination flooding of surfactant).Surfactant oil displacement require to reduce that the interfacial tension ability is strong, little in the rock surface adsorbance, price is low, can adapt to the high temperature on stratum and hypersaline environment etc., also must in indoor physical simulation, show the ability of higher raising recovery ratio on this basis, therefore also be necessary to develop a kind of environment-friendly type high performance emulsifying agent of heat and salinity tolerance.
In recent years, because the fast development of catering trade, the waste oil of generations such as fast food restaurant, restaurant enters rivers,lakes and seas by the drain outlet, causes more serious house refuse to pollute to natural environment; If waste oil flows into fast food restaurant and hotel by back door, will have a strong impact on people's safe diet, become an outstanding problem of harm society at present.Select waste oil as the main raw material(s) of this product, make the reasonable recycling of waste oil become possibility, effective, safe solution and an approach can be provided for the processing of waste oil problem.
Summary of the invention
The main purpose of the present invention is to address the above problem, and a kind of oil-in-water emulsifiers and preparation method thereof and using method are provided, and makes oil-in-water emulsion drilling fluid system have good emulsion stability, heat-resisting property and reservoir protection performance.Simultaneously also can be used as surfactant oil displacement, can reduce oil water interfacial tension significantly, have good heat and salinity tolerance performance.In addition, can provide effective, safe solution and an approach for the processing of waste oil problem.
High temperature resistance high-performance oil-water emulsifiers, raw material employing waste oil and TEPA, caustic soda, waste oil is the various animal and plant fats that restaurant, restaurant reclaim, TEPA is technical grade.Produce the TEPA of 1 ton of product needed 850-860 kilogram waste oil and 510-520 kilogram.
A kind of preparation method of oil-in-water emulsifiers is example to produce 1 ton of product, and its concrete preparation method is:
A. 850-860 kilogram waste oil is added the enamel reaction still of 2000L, and then add TEPA and 25-30 kilogram 20% caustic-soda aqueous solution of 510-520 kilogram, the logical Steam Heating of enamel reaction still chuck is also started stirring; Adopt the condensing reflux division box to reclaim the moisture that reaction produces in the temperature-rise period;
B. reaction solution comes to life when temperature rises to 180～190 ℃, and produce a large amount of water vapours this moment, reclaims its all cuts;
C. when dry-steam was separated out after reaction a period of time, temperature began to continue to raise; Temperature is remained on 230～250 ℃ of heating 30min, stop heating then, the enamel reaction still chuck leads to cooling water temperature;
D. reaction mass is cooled to room temperature, namely obtains high temperature resistance high-performance oil-water emulsifiers.
Described emulsifying agent using method, by mass percentage, described emulsifying agent dosage is 1%～3%.
Described emulsifying agent using method by mass percentage, also adds the isobutanol of 0.5%-0.6% in emulsion.
This emulsifying agent high temperature resistant property reaches 250 ℃; can be used in the high temperature deep well oil-in-water emulsion drilling fluid system, be mainly used in solving some low holes, hypotonic, seam hole and grow easy leakage, drilling well reservoir protection problem and a deep-well under-balanced drilling technology difficult problem that reservoir pressure coefficient is low.In addition, this emulsifying agent salt-resisting high-temperature-resisting can be as the surfactant of chemical flooding under the high temperature and high salt condition.Simultaneously, can realize reasonable utilization of wastes, avoid harmful waste oil to flow into fast-food restaurant and hotel, provide the solution of a kind of environmental protection, health, safety for solving the waste oil problem.
This high temperature resistance is yellow gluing liquid for hgh-performance emulsified dose.Use dosage only 1%～3% just can form oil-in-water emulsion, adding isobutanol emulsifying effectiveness is better in emulsion.Oil-water emulsifiers of the present invention has better emulsifying effectiveness, high temperature resistant property than general oil-water emulsifiers and better reduces the effect of interfacial tension.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Animal and plant fat composition in the raw materials used waste oil of the present invention changes to some extent, and the amount of adjusting soda bath flexibly can solve, to the effect did not influence.
Raw material employing waste oil and TEPA, caustic soda, waste oil is the various animal and plant fats that restaurant, restaurant reclaim, TEPA is technical grade.
Embodiment 1. adds the enamel reaction still of 2000L with 850 kilograms of waste oils, and then adds TEPA and 25 kilogram of 20% (mass percent concentration) caustic-soda aqueous solution of 510 kilograms, and the logical Steam Heating of the chuck of enamel reaction still is also started stirring.The moisture (this part moisture is not back to reactor) that adopts condensing reflux division box separating reaction to produce in the temperature-rise period.Reaction solution comes to life when temperature rises to 180 ℃, and produce a large amount of water vapours this moment, reclaims its all cuts (can not be back to reactor), as the raw material of other products.When dry-steam was separated out behind the reaction 40min, temperature began to continue to raise; Temperature is remained on 230 ℃, add thermal response 30min, stop heating then, the logical water quench of chuck is to room temperature, and surplus materials is high temperature resistance high-performance oil-water emulsifiers of the present invention in the enamel reaction still.
Evaluation experimental: be 20: 80 o'clock in oil-water ratio.Add 1% mentioned emulsifier and 0.5% isobutanol respectively according to mass percent, and cooperate 1% organoclay, 0.8% wetting agent and 1.5% fluid loss additive just can form stable emulsion, this emulsion density is 0.96g/cm
3, funnel viscosity is 40s, (250 ℃, 3.5MPa) filter loss is 12mL to HTHP.
Embodiment 2. adds the enamel reaction still of 2000L with 855 kilograms of waste oils, and then adds TEPA and 28 kilogram of 20% (mass percent concentration) caustic-soda aqueous solution of 515 kilograms, and the logical Steam Heating of the chuck of enamel reaction still is also started stirring.The moisture (this part moisture is not back to reactor) that adopts condensing reflux division box separating reaction to produce in the temperature-rise period.Reaction solution comes to life when temperature rises to 180 ℃, and produce a large amount of water vapours this moment, reclaims its all cuts (can not be back to reactor), as the raw material of other products.When dry-steam was separated out behind the reaction 45min, temperature began to continue to raise; Temperature is remained on 230 ℃, add thermal response 30min, stop heating then, the logical water quench of chuck is to room temperature, and surplus materials is high temperature resistance high-performance oil-water emulsifiers of the present invention in the enamel reaction still.
Evaluation experimental: be 40: 60 o'clock in oil-water ratio.Add 1.5% mentioned emulsifier and 0.5% isobutanol respectively according to percentage by weight, and cooperate 1% organoclay, 0.5% wetting agent and 1.5% fluid loss additive just can form stable emulsion, this emulsion density is 0.93g/cm
3, funnel viscosity is 50s, (250 ℃, 3.5MPa) filter loss is 10mL to HTHP.
Embodiment 3. adds the enamel reaction still of 2000L with 860 kilograms of waste oils, and then adds TEPA and 30 kilogram of 20% (mass percent concentration) caustic-soda aqueous solution of 520 kilograms, and the logical Steam Heating of the chuck of enamel reaction still is also started stirring.Adopt the condensing reflux division box to reclaim the moisture (this part moisture is not back to reactor) that reaction produces in the temperature-rise period.Reaction solution comes to life when temperature rises to 180 ℃, and produce a large amount of water vapours this moment, reclaims its all cuts (can not be back to reactor), as the raw material of other products.When dry-steam was separated out behind the reaction 50min, temperature began to continue to raise; Temperature is remained on 230 ℃, add thermal response 30min, stop heating then, the logical water quench of chuck is to room temperature, and surplus materials is high temperature resistance high-performance oil-water emulsifiers of the present invention in the enamel reaction still.
Evaluation experimental: be 50: 50 o'clock in oil-water ratio.Add 1.8% mentioned emulsifier and 0.6% isobutanol respectively according to percentage by weight, and cooperate 1% organoclay, 0.5% wetting agent and 1.0% fluid loss additive just can form stable emulsion, this emulsion density is 0.90g/cm
3, funnel viscosity is 54s, (250 ℃, 3.5MPa) filter loss is 8mL to HTHP.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (4)
1. a preparation method who is used in the oil-in-water emulsifiers in the high temperature deep well oil-in-water emulsion drilling fluid system is characterized in that, is example to produce 1 ton of product, and its concrete preparation method is:
A. 850-860 kilogram waste oil is added the enamel reaction still of 2000L, and then add TEPA and 25-30 kilogram 20% caustic-soda aqueous solution of 510-520 kilogram, the logical Steam Heating of enamel reaction still chuck is also started stirring; Adopt the condensing reflux division box to reclaim the moisture that reaction produces in the temperature-rise period; Waste oil is the various animal and plant fats that restaurant, restaurant reclaim;
B. reaction solution comes to life when temperature rises to 180～190 ℃, and produce a large amount of water vapours this moment, reclaims its all cuts;
C. when dry-steam began to separate out after reaction a period of time, temperature began to continue to raise; Temperature is remained on 230～250 ℃ of heating 30min, stop heating then, the enamel reaction still chuck leads to cooling water temperature;
D. reaction mass is cooled to room temperature, namely obtains high temperature resistance high-performance oil-water emulsifiers.
2. the emulsifying agent that makes according to the described method of claim 1.
3. the using method of emulsifying agent described in the claim 2 is characterized in that, by mass percentage, described emulsifying agent dosage is 1%～3%.
4. emulsifying agent makes described in the claim 2 uses method, it is characterized in that, by mass percentage, also adds the isobutanol of 0.5%-0.6% in emulsion.
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| CN104140792B (en) * | 2014-04-23 | 2018-03-30 | 中国石油化工股份有限公司 | A kind of oil base drilling fluid emulsifying agent and its preparation method and application |
| US10385254B2 (en) | 2017-07-27 | 2019-08-20 | Saudi Arabian Oil Company | Ecofriendly emulsifier synthesis from esterified waste vegetable oil for wellbore drilling fluids |
| CN110157403B (en) * | 2019-05-08 | 2020-09-29 | 中国石油大学(北京) | Low-permeability oil reservoir oil displacement agent |
| US10858568B1 (en) | 2019-07-11 | 2020-12-08 | Saudi Arabian Oil Company | Rheology modifier for organoclay-free invert emulsion drilling fluid systems |
| US11352545B2 (en) | 2020-08-12 | 2022-06-07 | Saudi Arabian Oil Company | Lost circulation material for reservoir section |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101157850A (en) * | 2007-11-20 | 2008-04-09 | 孝英 | Preparation of high temperature resistant lubricant for drilling liquid by animal plant oil |
| CN101411970A (en) * | 2007-10-19 | 2009-04-22 | 天津市环境保护科学研究院 | Method for preparing fuel oil emulsifier using trench oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101411970A (en) * | 2007-10-19 | 2009-04-22 | 天津市环境保护科学研究院 | Method for preparing fuel oil emulsifier using trench oil |
| CN101157850A (en) * | 2007-11-20 | 2008-04-09 | 孝英 | Preparation of high temperature resistant lubricant for drilling liquid by animal plant oil |
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Address after: Shaanxi Xi'an high tech Zone Technology Road 710065 No. 30 Cheshire Heli building A block 10 layer Applicant after: China Petroleum University (East China) Address before: 266555 Qingdao economic and Technological Development Zone, Changjiang Road, No. 66, Shandong Applicant before: China Petroleum University (East China) |
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