CN102286273A - 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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- CN102286273A CN102286273A CN2011102600251A CN201110260025A CN102286273A CN 102286273 A CN102286273 A CN 102286273A CN 2011102600251 A CN2011102600251 A CN 2011102600251A CN 201110260025 A CN201110260025 A CN 201110260025A CN 102286273 A CN102286273 A CN 102286273A
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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 and solves some low holes, hypotonic, seam hole and grow easy leakage, a 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 treatment 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-balanced drilling, helps liberating hydrocarbon zone, improves the oil gas well productivity; The generation that helps to improve rate of penetration and prevent leakage does not influence electrical measurement and nuclear magnetism 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 an 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 emulsifying effect by emulsifying agent to form oil be that disperse phase, water are the milk sap of external phase.Say that in principle the emulsifying agent of HLB value (hydrophile-lipophile balance value) 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 tensio-active agent is the successful key of decision chemical flooding (surfactant flooding contains the combination flooding of tensio-active agent).Surfactant oil displacement require to reduce that the interfacial tension ability is strong, little in the rock surface adsorptive capacity, 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 sewer oil of generations such as snack bar, restaurant enters rivers,lakes and seas by the drain outlet, causes more serious domestic refuse to pollute to physical environment; If sewer oil flows into snack bar 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 the main raw material(s) of sewer oil, make the reasonable recycling of sewer oil become possibility, effective, a safe solution and an approach can be provided for the processing of sewer oil problem as this product.
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 emulsifying 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, a safe solution and an approach for the processing of sewer oil problem.
High temperature resistance high-performance oil-water emulsifiers, raw material employing sewer oil and tetraethylene pentamine, caustic soda, sewer oil is the various animal-plant oil that restaurant, restaurant reclaim, tetraethylene pentamine is a technical grade.Produce the tetraethylene pentamine of 1 ton of product needed 850-860 kilogram sewer oil and 510-520 kilogram.
A kind of preparation method of oil-in-water emulsifiers is an example to produce 1 ton of product, and its concrete preparation method is:
A. 850-860 kilogram sewer oil is added the enamel reaction still of 2000L, and then add the tetraethylene pentamine 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 is produced in the temperature-rise period;
B. reaction soln comes to life when temperature rises to 180～190 ℃, and produce a large amount of water vapors this moment, reclaims its all cuts;
C. when dry-steam was separated out after reaction for some 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, promptly 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 isopropylcarbinol of 0.5%-0.6% in milk sap.
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 and solve some low holes, hypotonic, seam hole and grow easy leakage, a 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 tensio-active agent of chemical flooding under the high temperature and high salt condition.Simultaneously, can realize reasonable utilization of wastes, avoid harmful sewer oil to flow into fast-food restaurant and hotel, provide the solution of a kind of environmental protection, health, safety for solving the sewer oil problem.
This high temperature resistance is yellow gluing liquid for hgh-performance emulsified dose.Use dosage only 1%～3% just can form water external emulsion, adding isopropylcarbinol emulsifying effectiveness is better in milk sap.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.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Animal-plant oil composition in the raw materials used sewer oil of the present invention changes to some extent, and the amount of adjusting caustic soda soln flexibly can solve, to the effect did not influence.
Raw material employing sewer oil and tetraethylene pentamine, caustic soda, sewer oil is the various animal-plant oil that restaurant, restaurant reclaim, tetraethylene pentamine is a technical grade.
Embodiment 1. adds the enamel reaction still of 2000L with 850 kilograms of sewer oils, and then adds tetraethylene pentamine 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 be produced in the temperature-rise period.Reaction soln comes to life when temperature rises to 180 ℃, and produce a large amount of water vapors 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 ℃, and reacting by heating 30min stops heating then, and 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: in water oil ratio is 20: 80 o'clock.Add 1% mentioned emulsifier and 0.5% isopropylcarbinol respectively according to mass percent, and cooperate 1% organophilic clay, 0.8% wetting agent and 1.5% fluid loss agent just can form true emulsion, this milk sap density is 0.96g/cm
3, funnel viscosity is 40s, (250 ℃, 3.5MPa) filter loss is 12mL to High Temperature High Pressure.
Embodiment 2. adds the enamel reaction still of 2000L with 855 kilograms of sewer oils, and then adds tetraethylene pentamine 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 be produced in the temperature-rise period.Reaction soln comes to life when temperature rises to 180 ℃, and produce a large amount of water vapors 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 ℃, and reacting by heating 30min stops heating then, and 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: in water oil ratio is 40: 60 o'clock.Add 1.5% mentioned emulsifier and 0.5% isopropylcarbinol respectively according to weight percent, and cooperate 1% organophilic clay, 0.5% wetting agent and 1.5% fluid loss agent just can form true emulsion, this milk sap density is 0.93g/cm
3, funnel viscosity is 50s, (250 ℃, 3.5MPa) filter loss is 10mL to High Temperature High Pressure.
Embodiment 3. adds the enamel reaction still of 2000L with 860 kilograms of sewer oils, and then adds tetraethylene pentamine 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 is produced in the temperature-rise period.Reaction soln comes to life when temperature rises to 180 ℃, and produce a large amount of water vapors 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 ℃, and reacting by heating 30min stops heating then, and 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: in water oil ratio is 50: 50 o'clock.Add 1.8% mentioned emulsifier and 0.6% isopropylcarbinol respectively according to weight percent, and cooperate 1% organophilic clay, 0.5% wetting agent and 1.0% fluid loss agent just can form true emulsion, this milk sap density is 0.90g/cm
3, funnel viscosity is 54s, (250 ℃, 3.5MPa) filter loss is 8mL to High Temperature High Pressure.
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. the preparation method of an oil-in-water emulsifiers is characterized in that, is example to produce 1 ton of product, and its concrete preparation method is:
A. 850-860 kilogram sewer oil is added the enamel reaction still of 2000L, and then add the tetraethylene pentamine 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 is produced in the temperature-rise period;
B. reaction soln comes to life when temperature rises to 180～190 ℃, and produce a large amount of water vapors this moment, reclaims its all cuts;
C. when dry-steam began to separate out after reaction for some 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, promptly 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 described emulsifying agent using method of claim 2 is characterized in that, by mass percentage, described emulsifying agent dosage is 1%～3%.
4. the described emulsifying agent using method of claim 2 is characterized in that, by mass percentage, also adds the isopropylcarbinol of 0.5%-0.6% in milk sap.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104140792A (en) * | 2014-04-23 | 2014-11-12 | 中国石油化工股份有限公司 | Emulsifier for oil-based drilling fluid as well as preparation method and application thereof |
| US10385254B2 (en) | 2017-07-27 | 2019-08-20 | Saudi Arabian Oil Company | Ecofriendly emulsifier synthesis from esterified waste vegetable oil for wellbore drilling fluids |
| CN110157403A (en) * | 2019-05-08 | 2019-08-23 | 中国石油大学(北京) | A kind of low-permeability oil deposit 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 |
|---|---|---|---|---|
| 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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2011
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Patent Citations (2)
| 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 |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104140792A (en) * | 2014-04-23 | 2014-11-12 | 中国石油化工股份有限公司 | Emulsifier for oil-based drilling fluid as well as preparation method and application thereof |
| 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 |
| US10808161B2 (en) | 2017-07-27 | 2020-10-20 | Saudi Arabian Oil Company | Ecofriendly emulsifier synthesis from esterified waste vegetable oil for wellbore drilling fluids |
| CN110157403A (en) * | 2019-05-08 | 2019-08-23 | 中国石油大学(北京) | A kind of low-permeability oil deposit 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 |
| US11072736B2 (en) | 2019-07-11 | 2021-07-27 | 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 |
| US11739249B2 (en) | 2020-08-12 | 2023-08-29 | Saudi Arabian Oil Company | Lost circulation material for reservoir section |
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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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