CN103421473A - Emulsifier for novel high-temperature water-in-oil drilling fluid - Google Patents
Emulsifier for novel high-temperature water-in-oil drilling fluid Download PDFInfo
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- CN103421473A CN103421473A CN2013103340833A CN201310334083A CN103421473A CN 103421473 A CN103421473 A CN 103421473A CN 2013103340833 A CN2013103340833 A CN 2013103340833A CN 201310334083 A CN201310334083 A CN 201310334083A CN 103421473 A CN103421473 A CN 103421473A
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Abstract
The invention relates to an emulsifier for a novel high-temperature water-in-oil drilling fluid. The emulsifier comprises the following components in percentage by weight: a main emulsifier DQGC and an auxiliary emulsifier DQNS, wherein the main emulsifier DQGC is a Gemini quaternary ammonium salt surfactant; the auxiliary emulsifier DQNS is an amide surfactant; the molecular structures of the main emulsifier DQGC and the auxiliary emulsifier DQNS are as follows: [(R1CONH(CH2)3N(CH3)2CH2CHOHCH2)2NR2]2+.2Cl-R1CONH(CH2)3N(CH3)2, in the formula, R1 is C17H33, C17H31 and C19H29, and R2 is C12H25. According to the emulsifier, better oleophylic and hydrophilic abilities can be obtained, the emulsifying ability is enhanced, and the stability of the water-in-oil drilling fluid is improved.
Description
Technical field
The present invention relates to a kind of tensio-active agent in the oil drilling technical field, especially a kind of high temperature water-in-oil drilling emulsifying agent.
Background technology
Tensio-active agent can, respectively as defoamer, emulsifying agent, wetting agent, whipping agent and washing composition etc., have a wide range of applications in a lot of fields according to its concrete effect.In field produces, tensio-active agent can be used as oil-water emulsifiers and water-in-oil emulsifier for the oil drilling fluid, and the oil-displacing agent of used for tertiary oil recovery.When tensio-active agent is used for invert oil-emulsion drilling fluid; can significantly reduce oil water interfacial tension; water is scattered in basic oil phase with stable small droplets form; form that a kind of wellbore stability ability is strong, the protection reservoir is effective; can be used for water-sensitive strata, saline bed or high-temperature stratum drilling well, the drilling fluid with excellent oilness and leak-off building capacity.Yet, domestic typical invert mud emulsifying agent be take Span80, stearic acid and oleic acid etc. as main, with the lime effect, forms calcium soap, utilizes phase water droplet in the emulsification of oriented wedge principle, true emulsion, exist surfactivity low, less stable, to the insufficient deficiency that waits of the wetting action of useful solid phase, in on-the-spot drilling process, easily cause drilling fluid viscosity high, the problems such as shear force is low, and large rock-carrying ability is poor, limited the application of invert mud.
Summary of the invention
The invention reside in and overcome the problem existed in background technology, and a kind of novel high temperature water-in-oil drilling emulsifying agent is provided.This novel high temperature water-in-oil drilling emulsifying agent, can obtain the hydrophilic ability of oleophylic preferably, strengthened emulsifying capacity, improved the stability of invert mud.
The present invention solves its problem and can reach by following technical solution: this novel high temperature water-in-oil drilling emulsifying agent, comprise primary emulsion DQGC and co-emulsifier DQNS, wherein DQGC is Gemini gemini quaternary ammonium salt class tensio-active agent, DQNS is amide surfactants, and component DQGC and DQNS molecular structure are as follows respectively:
[(R
1CONH(CH
2)
3N(CH
3)
2CH
2CHOHCH
2)
2NR
2]
2+·2Cl
-……（DQGC）
R
1CONH(CH
2)
3N(CH
3)
2 ……（DQNS）
R in formula
1For C
17H
33, C
17H
31And C
19H
29, R
2For C
12H
25.
Described component DQGC and DQNS mass percent 67:33～75:25.
The synthesis technique of described component DQGC is:
The acid-base neutralisation reaction that the first step is organic acid and organic bases, both mol ratio 1:1.2～1.1:1, wherein organic acid is oleic acid, Yatall MA, sylvic acid or refining Tall oil, organic bases is N, N-dimethylated propyl diethylenetriamine, 140 ℃～170 ℃ of temperature of reaction, reaction times 14h, generate intermediate product I.
The etherification reaction that second step is epoxy chloropropane and organic amine, mol ratio is 2:1～4:1,130 ℃～135 ℃ of temperature of reaction, reaction times 12h～13h, generate intermediate product II.
The 3rd step: be the quaterisation of above-mentioned two-step reaction intermediate product, intermediate product (I) and intermediate product (II) mol ratio 2:1～4:1,160 ℃～175 ℃ of temperature of reaction, reaction times 24h～25h, obtain primary emulsion DQGC.
The synthesis technique of described DQNS is: synthesis material organic acid and organic bases, organic acid and organic bases mol ratio are 1:1.2～1.1:1, wherein organic acid is oleic acid, Yatall MA, sylvic acid or refining Tall oil, organic bases is N, the N-dimethylated propyl diethylenetriamine, 140 ℃～170 ℃ of temperature of reaction, reaction times 14h, obtain co-emulsifier DQNS.
This novel high temperature water-in-oil drilling emulsifying agent has been introduced aromatic ring structure in molecular structure, has finally synthesized anti-200 ℃ of high temperature invert oil-emulsion drilling fluid primary emulsions.Different from conventional emulsifier is that it contains 2～4 oleophylic chains, 2 hydrophilic radicals, by spacer group, many oleophylic chains are coupled together, can effectively solve because the same sex of hydrophilic radical is repelled the poor problem of emulsifying effectiveness that on the water-oil interface that cause, the emulsifying agent arrangement does not closely cause.Simultaneously, such tensio-active agent has special phase behavior, when static, with porous, complicated packing structure, exists, and under shearing, along with rotating speed increases, constantly to level and smooth sheet structure transition, transformation, shows as drilling fluid system and has the rheological property that low sticky height is cut.And the wettability of emulsifying agent makes the solid phase in system less to viscosity influence, can obtain better flow pattern, reduce plastic viscosity, be beneficial to the raising rate of penetration.Coordinate high temperature resistance invert oil-emulsion drilling fluid co-emulsifier, can regulate emulsifier hlb value, obtain the hydrophilic ability of better oleophylic, strengthen emulsifying capacity, improve the stability of invert oil-emulsion drilling fluid.
The present invention compares and can have following beneficial effect with the above-mentioned background technology: this novel high temperature water-in-oil drilling emulsifying agent, in the invert oil-emulsion drilling fluid system, used the Gemini quaternary ammonium salt style tensio-active agent of high temperature resistance as primary emulsion, because it has efficient emulsifying capacity and special phase behavior, and the HLB value suitable with the composite acquisition of co-emulsifier, formed stable milk sap, be used in conjunction with the treatment agents such as high temperature resistance organophilic clay and fluid loss agent simultaneously, still there is stronger spatial grid structure and excellent rheological after making drilling fluids at high temperature aging, in addition, the heat resisting fluid loss reducing agent particle is tightly packed has formed fine and close mud cake, thereby reduction high temperature and high pre ssure filtration.
Embodiment:
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1.
Take Yatall MA 96g and join preheating in magnetic stirring apparatus, add 40g N while being heated to 70 ℃, the N-dimethylated propyl diethylenetriamine, the heated and stirred reactant starts to have elutriation to go out when temperature rises to 140 ℃, shows that reaction starts to carry out, no longer including water after 14h generates, show that reaction finishes, obtain intermediate product (I), put into sample bottle labelled; Get epoxy chloropropane 99g and amino dodecane 50g, the heated and stirred reactant, after 130 ℃ of reaction 13h, remove excessive epoxy chloropropane by underpressure distillation, obtains intermediate product (II), puts into sample bottle labelled; Get 100g intermediate product (I) and 48g intermediate product (II), the heated and stirred reactant, 170 ℃ of reaction 25h carry out quaterisation, obtain the high temperature resistance invert oil-emulsion drilling fluid with primary emulsion DQGC sample 1., put into sample bottle labelled.
Take Yatall MA 96g and join preheating in magnetic stirring apparatus, add 40g N while being heated to 70 ℃, N-dimethylated propyl diethylenetriamine, heated and stirred reactant.When temperature rises to 140 ℃, start to have elutriation to go out, show that reaction starts to carry out, no longer include water after 14h and generate, show that reaction finishes, obtain co-emulsifier DQNS sample 1., put into sample bottle labelled.
24g primary emulsion DQGC sample 1., 1. 8g co-emulsifier DQNS sample be hybridly prepared into emulsifying agent of the present invention.
Embodiment 2.
Take sylvic acid 130g and join preheating in magnetic stirring apparatus, be heated to 130 ℃, add 40gN, N-dimethylated propyl diethylenetriamine, heated and stirred reactant.When temperature rises to 170 ℃, reaction starts, and no longer includes water after 14h and generates, and shows that reaction finishes, and obtains intermediate product (I), puts into sample bottle labelled; Get epoxy chloropropane 108g and tetradecy lamine 100g, the heated and stirred reactant, after 135 ℃ of reaction 12h, remove excessive epoxy chloropropane by underpressure distillation, obtains intermediate product (II), puts into sample bottle labelled; Get 100g intermediate product (I) and 26g intermediate product (II), the heated and stirred reactant, 175 ℃ of reaction 24h carry out quaterisation, obtain the high temperature resistance invert oil-emulsion drilling fluid with primary emulsion DQGC sample 2..
Take sylvic acid 130g and join preheating in magnetic stirring apparatus, be heated to 130 ℃, add 40gN, N-dimethylated propyl diethylenetriamine, heated and stirred reactant.When temperature rises to 170 ℃, reaction starts, and no longer includes water after 14h and generates, and shows that 2. reaction finishes, obtain co-emulsifier DQNS sample.
26g primary emulsion DQGC sample 2., 2. 9.2g co-emulsifier DQNS sample be hybridly prepared into emulsifying agent of the present invention.
Embodiment 3.
Take Yatall MA 96g and join preheating in magnetic stirring apparatus, add 40g N while being heated to 70 ℃, N-dimethylated propyl diethylenetriamine, heated and stirred reactant.When temperature rises to 140 ℃, start to have elutriation to go out, show that reaction starts to carry out, no longer include water after 14h and generate, show that reaction finishes, obtain intermediate product (I), put into sample bottle labelled; Get epoxy chloropropane 75g and amino dodecane 50g, the heated and stirred reactant, after 130 ℃ of reaction 12h,, obtain intermediate product (II), put into sample bottle labelled; Get 100g intermediate product (I) and 33g intermediate product (II), the heated and stirred reactant, 160 ℃ of reaction 24h carry out quaterisation, obtain high temperature water-in-oil drilling with primary emulsion DQGC sample 3..
Take Yatall MA 96g and join preheating in magnetic stirring apparatus, add 40g N while being heated to 70 ℃, N-dimethylated propyl diethylenetriamine, heated and stirred reactant.When temperature rises to 140 ℃, start to have elutriation to go out, show that reaction starts to carry out, no longer include water after 14h and generate, show that 3. reaction finishes, obtain co-emulsifier DQNS sample.
28g primary emulsion DQGC sample 3., 3. 14g co-emulsifier DQNS sample be hybridly prepared into emulsifying agent of the present invention.
With reference to oil and gas industry standard SY/T6615-2005 " drilling fluid emulsifying agent assessment process ", synthetic emulsifying agent sample is estimated.The milk sap water oil ratio is 70:30, add respectively 2.1% primary emulsion, 2.1% and 0.7% major-minor newborn composite emulsifier, add while stirring 2% organophilic clay, 12000r/min adds calcium chloride brine after stirring 10min, be mixed with water-in-oil emulsion after continuing to stir at the same rate 30min, in the high temp roller process furnace, after 200 ℃ of aging 16h, the electricity consumption stability meter is measured the emulsion-breaking voltage ES of milk sap.Experimental result sees the following form 1.
Table 1 high temperature resistance emulsifying agent sample is estimated
After table 1 is found out 200 ℃ of aging 16h of synthetic emulsifying agent preparation milk sap, emulsion-breaking voltage still is greater than 400V, and stability is better, can temperature resistance 200 ℃.
The novel high temperature resistance invert oil-emulsion drilling fluid that uses the present invention to develop has made the low sticky height of novel high temperature resistance with primary emulsion DQGC and co-emulsifier DQNS and has cut invert oil-emulsion drilling fluid, formula consists of formula A: water oil ratio 90:10, primary emulsion DQGC6.0～7.0%+ co-emulsifier DQNS2.0～3.5%+ organophilic clay BS-1C4.0%+ lime 1.5～3.0%+ fluid loss agent DQHA6.0%; The formula composition reaches, with domestic traditional invert oil-emulsion drilling fluid system performance, contrast simultaneously, the formula of domestic traditional invert oil-emulsion drilling fluid consists of formula B: water oil ratio 85:15, primary emulsion Span804.0～6.0%+ co-emulsifier cycloalkanoimide 4.0～6.0%+ wetting agent oleic acid 2.0～3.0%+ organophilic clay BS-1C4.0～6.0%+ lime 3.0～5.0%+ potassium hydroxide 0.5%+ fluid loss agent sulfonated gilsonite 2.0～3.5%+ fluid loss agent oxidized bitumen 2.0～3.5%.The low sticky height of both novel high temperature resistances is cut the traditional performance contrast of invert oil-emulsion drilling fluid and domestic traditional invert oil-emulsion drilling fluid in Table 2.
The contrast of table 2 drilling fluid traditional performance
By the contrast of the traditional performance in table 2, can find out, novel high temperature water-in-oil drilling of the present invention can maintain drilling fluid stability preferably under the condition lower at dosage with emulsifying agent, and rheological has the characteristic that low sticky height is cut, and obviously is better than state's internal emulsifying agent performance.
The low sticky height of the novel high temperature resistance of the present invention's preparation is cut the invert oil-emulsion drilling fluid system and carried out test in place and application in ancient dark 3 wells of Daqing oil field, flat 4 wells of Xu Shen 9-and Song Shen 9H well etc.Wherein, ancient dark 3 wells are the prospect pits of a bite high temperature risk, design well depth 4920m, and Average geothermal gradient is up to 4.07 ℃/100m, and bottom temperature can reach 200 ℃.Three spud in meets and to step on Lou Ku group and battalion's city group.Step on the Lou Ku group and be mainly mud stone, pelitic siltstone and mud stone and siltstone alternating layers, its characteristics are that shale index is high, and clay mineral be take illite and illite/smectite mixed layer as main, meet water the flake-off piece easily occurs; The inner possibility of battalion's city group volcanics mature fault, lithology is mainly tuff, andesite and basalt, and wherein tuff is loose, easy aquation, the inner microfracture of andesite is grown, and basalt hardness is high, and drillability is poor.Real brill data shows, this block stratum abrasive property is strong, single headway per drill bit is few, drilling period is long, Daqing oil field was successively disposed and the probing task of the 2 mouthfuls of high temperature deep wells of constructing at Gulong area in the past, all occurred that reaming in various degree, the borehole wall peel off, bit freezing, hole drift angle exceed standard, high temperature resistant drilling fluids can not meet construction requirement, the problem that the complex accident rate is high.For above complexcase, use the low sticky height of novel high temperature resistance to cut invert oil-emulsion drilling fluid three spud sections are crept into, on-the-spot property of drilling fluid is as shown in table 3 below.
The on-the-spot property of drilling fluid of ancient dark 3 wells of table 3
The low sticky height of novel high temperature resistance is cut invert oil-emulsion drilling fluid under the hot environment of nearly 2 months as can be seen from Table 3, property of drilling fluid is stable, the temperature resistance ability is strong, the minimum 1308V of emulsion-breaking voltage ES, viscosity and shear force change steadily, funnel viscosity FV50～68s, and ratio of dynamic shear force/yield value to plastic viscosity YP/PV is greater than 0.4Pa/mPas all the time, show good low sticky height and cut rheological, high temperature and high pre ssure filtration FLHTHP7.2mL.The down-hole complexity does not occur in drilling process, the well rule, diameter enlargement ratio is only 5.83%, three drive chi 531m into, 642.5h during brill, and average rate of penetration is up to 0.83m/h, refreshed the record of this block with rate of penetration under geologic condition, the high-quality and efficient job task that has completed this well.
Claims (5)
1. a novel high temperature water-in-oil drilling emulsifying agent, comprise primary emulsion DQGC and co-emulsifier DQNS, wherein DQGC is Gemini gemini quaternary ammonium salt class tensio-active agent, and DQNS is amide surfactants, and component DQGC and DQNS molecular structure are as follows respectively:
[(R
1CONH(CH
2)
3N(CH
3)
2CH
2CHOHCH
2)
2NR
2]
2+·2Cl
-
R
1CONH(CH
2)
3N(CH
3)
2
R in formula
1For C
17H
33, C
17H
31And C
19H
29, R
2For C
12H
25.
2. a kind of novel high temperature water-in-oil drilling emulsifying agent according to claim 1, is characterized in that: described component DQGC and DQNS mass percent 67:33 ~ 75:25.
3. a kind of novel high temperature water-in-oil drilling emulsifying agent according to claim 1 and 2, it is characterized in that: the synthesis technique of described component DQGC is:
The acid-base neutralisation reaction that the first step is organic acid and organic bases, both mol ratio 1:1.2 ~ 1.1:1, wherein organic acid is oleic acid, Yatall MA, sylvic acid or refining Tall oil, organic bases is N, N-dimethylated propyl diethylenetriamine, 140 ℃ ~ 170 ℃ of temperature of reaction, reaction times 14h, generate intermediate product
The etherification reaction that second step is epoxy chloropropane and organic amine, mol ratio is 2:1 ~ 4:1,130 ℃ ~ 135 ℃ of temperature of reaction, reaction times 12h ~ 13h, generate intermediate product
The 3rd step: be the quaterisation of above-mentioned two-step reaction intermediate product, intermediate product (
) and intermediate product (
) mol ratio 2:1 ~ 4:1,160 ℃ ~ 175 ℃ of temperature of reaction, reaction times 24h ~ 25h, obtain primary emulsion DQGC.
4. a kind of novel high temperature water-in-oil drilling emulsifying agent according to claim 3, it is characterized in that: described organic amine is amino dodecane, tetradecy lamine or cetylamine.
5. a kind of novel high temperature water-in-oil drilling emulsifying agent according to claim 1 and 2, it is characterized in that: the synthesis technique of described DQNS is: synthesis material organic acid and organic bases, organic acid and organic bases mol ratio are 1:1.2 ~ 1.1:1, wherein organic acid is oleic acid, Yatall MA, sylvic acid or refining Tall oil, organic bases is N, N-dimethylated propyl diethylenetriamine, 140 ℃ ~ 170 ℃ of temperature of reaction, reaction times 14h, obtain co-emulsifier DQNS.
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| CN103965861A (en) * | 2014-05-21 | 2014-08-06 | 中国石油化工股份有限公司 | High temperature resistant Gemini cationic viscoelastic surfactant (VES) and synthetic method thereof |
| CN105062448A (en) * | 2015-07-28 | 2015-11-18 | 中国石油集团渤海钻探工程有限公司 | Water soluble ultra-thick crude oil emulsifying and viscosity-reducing agent and preparation method thereof |
| CN105419751A (en) * | 2015-10-30 | 2016-03-23 | 中国石油天然气集团公司 | Highly thixotropic emulsifier for anti-high-temperature oil-in-water drilling fluid |
| CN112607826A (en) * | 2021-03-02 | 2021-04-06 | 烟台垚磊信息技术有限公司 | Oily emulsification effluent treatment plant |
| CN114524736A (en) * | 2021-12-30 | 2022-05-24 | 福州大学 | Asymmetric Gemini cationic surfactant and preparation method thereof |
| CN115418207A (en) * | 2022-09-20 | 2022-12-02 | 四川捷贝通能源科技有限公司 | Temperature-resistant salt-tolerant foamed gel system and preparation method thereof |
| CN116790232A (en) * | 2023-06-30 | 2023-09-22 | 中石化胜利石油工程有限公司难动用项目管理中心 | Composite brine oil-in-water invert emulsion drilling fluid system and preparation method thereof |
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| CN103756652A (en) * | 2014-01-20 | 2014-04-30 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | Emulsifier for oil-based drilling fluid and preparation method thereof |
| CN103756652B (en) * | 2014-01-20 | 2016-05-25 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | A kind of emulsifying agent and preparation method thereof for oil base drilling fluid |
| CN103965861A (en) * | 2014-05-21 | 2014-08-06 | 中国石油化工股份有限公司 | High temperature resistant Gemini cationic viscoelastic surfactant (VES) and synthetic method thereof |
| CN103965861B (en) * | 2014-05-21 | 2016-08-17 | 中国石油化工股份有限公司 | A kind of high temperature resistance Gemini cationic viscoelastic surfactants and synthetic method thereof |
| CN105062448A (en) * | 2015-07-28 | 2015-11-18 | 中国石油集团渤海钻探工程有限公司 | Water soluble ultra-thick crude oil emulsifying and viscosity-reducing agent and preparation method thereof |
| CN105419751A (en) * | 2015-10-30 | 2016-03-23 | 中国石油天然气集团公司 | Highly thixotropic emulsifier for anti-high-temperature oil-in-water drilling fluid |
| CN112607826A (en) * | 2021-03-02 | 2021-04-06 | 烟台垚磊信息技术有限公司 | Oily emulsification effluent treatment plant |
| CN112607826B (en) * | 2021-03-02 | 2021-05-07 | 烟台垚磊信息技术有限公司 | Oily emulsification effluent treatment plant |
| CN114524736A (en) * | 2021-12-30 | 2022-05-24 | 福州大学 | Asymmetric Gemini cationic surfactant and preparation method thereof |
| CN115418207A (en) * | 2022-09-20 | 2022-12-02 | 四川捷贝通能源科技有限公司 | Temperature-resistant salt-tolerant foamed gel system and preparation method thereof |
| CN116790232A (en) * | 2023-06-30 | 2023-09-22 | 中石化胜利石油工程有限公司难动用项目管理中心 | Composite brine oil-in-water invert emulsion drilling fluid system and preparation method thereof |
| CN116790232B (en) * | 2023-06-30 | 2024-06-07 | 中石化胜利石油工程有限公司难动用项目管理中心 | Composite brine oil-in-water invert emulsion drilling fluid system and preparation method thereof |
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Application publication date: 20131204 |