CN103824671A - Nano magnetic fluid for monitoring fracturing crack and preparing method of nano magnetic fluid - Google Patents

Nano magnetic fluid for monitoring fracturing crack and preparing method of nano magnetic fluid Download PDF

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CN103824671A
CN103824671A CN201410091172.4A CN201410091172A CN103824671A CN 103824671 A CN103824671 A CN 103824671A CN 201410091172 A CN201410091172 A CN 201410091172A CN 103824671 A CN103824671 A CN 103824671A
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nanometer
nanometer magnetofluid
fracturing fracture
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CN103824671B (en
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罗明良
孙涛
温庆志
刘飞
郭烨
杨国威
吕子龙
李楠
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China University of Petroleum East China
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Abstract

The invention relates to a nano magnetic fluid for monitoring a fracturing crack and a preparing method of the nano magnetic fluid. The nano magnetic fluid is formed by taking Fe3O4 particles modified by a surface modifier as magnetic particles and water as a carrier liquid. The invention also relates to a preparing method of the nano magnetic fluid. The nano magnetic fluid is better in hydration stability, narrow in size distribution, higher in molar susceptibility, low in price of preparing raw materials, simple and easy in preparing process, suitable for industrial production and capable of being used for the field of monitoring on a reservoir layer or crack.

Description

A kind of nanometer magnetofluid for fracturing fracture monitoring and preparation method thereof
Technical field
The present invention relates in a kind of fracturing process, nanometer magnetofluid of monitoring for fracturing fracture and preparation method thereof, belongs to technical field of material.
Background technology
Many large-scale high oil impregnates gas field, the whole world has entered the exploitation later stage, the petroleum resources in low-permeability oil gas field is expected to become the continuous driving force of world's future source of energy and economic development, and oil gas in these compact reservoirs need to can be realized exploitation cost-effectively through fracturing.Oil/gas Well is after fracturing operation, and oil and gas production is effectively promoted.Optimize later fracturing work technique for actual crack state and guidance after assessing fracturing work, operation company need to obtain hydraulic fracture and extend situation, and many information such as geometric shape and size, orientation etc., so Crack Monitoring is a kind of highly effective method.
The existing Main Means for Fracturing Monitoring is micro-seismic technology.What this method was mainly utilized is the seismic wave producing in fracture extension process in pressure break, and the crack data that monitor not are very accurate.For this reason, researcher has carried out extensive work both at home and abroad, is devoted to work out more accurately Crack Monitoring method of one.For example CN103244103A proposes a kind of method of utilizing nanometer magnetofluid to carry out hydraulic fracture Real-Time Monitoring, nanometer magnetofluid and fracturing fluid are mixed to injection crack, utilize transmitting and the receiving device transmitting and receiving signal on down-hole and ground, monitor out the parameter in saturated nanometer magnetofluid crack according to electromagnetic induction principle, as form, size, orientation etc.This method can be determined accurate quantification has good application prospect by fracture parameters.
In existing nanometer magnetofluid preparation method, step complexity, demand HTHP instrument and equipment, output is little, and cost is higher, is not suitable for needing in Crack Monitoring the situations of a large amount of uses.At present, be not specifically designed to the technology of preparing of fracturing fracture monitoring nanometer magnetofluid.Therefore, need a kind of preparation process simple, equipment requirement is simple and easy, and raw material are cheap, the method for large-scale production that what preparation cost was low can be used for.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of nanometer magnetofluid for fracturing fracture monitoring and preparation method thereof.
The technical solution adopted in the present invention is as follows:
For a nanometer magnetofluid for fracturing fracture monitoring, be the Fe modifying with surface modification agent 3o 4particle is magnetic-particle, and water is that carrier fluid forms; Described Fe 3o 4the particle size range of particle is 10～25nm, described Fe 3o 4the molar susceptibility of particle is 290～450cm 3/ mol, described Fe 3o 4the particle concentration of particle is 18～30wt.%; Described coating material is natrium citricum, sodium ethylene diamine tetracetate, enuatrol or lauryl sodium sulfate; Described coating material and Fe 3o 4the mol ratio of particle is (0.1～0.8): 1.
According to the present invention, preferred, described Fe 3o 4the particle size range of particle is 12～15nm.
According to the present invention, preferred, described Fe 3o 4the molar susceptibility of particle is 420～450cm 3/ mol.
According to the present invention, preferred, described Fe 3o 4the particle concentration of particle is 20～22wt.%.
A preparation method for the nanometer magnetofluid of monitoring for fracturing fracture, comprises that step is as follows:
(1) press Fe 2+/ Fe 3+molar ratio is 0.6～0.8 by divalent iron salt and trivalent iron salt even, the described Fe that is dissolved in deionized water for stirring 3+concentration be 0.15～0.25mol/L;
(2) under stirring condition, press OH -/ Fe 3+mol ratio is 4.2～4.6 to add aqueous slkali to precipitate, and 40～50 ℃ of reaction 20～40min, regulate pH to 5～7, obtain Fe 3o 4particle;
(3) press coating material/Fe 3o 4particle mol ratio is (0.1～0.8): 1 adds finishing agent solution, 80～90 ℃ of slaking 0.5～2h, and described coating material is natrium citricum, sodium ethylene diamine tetracetate, enuatrol or lauryl sodium sulfate; Magnetic separation goes out solid phase particles, removes supernatant, by being dispersed in deionized water after the washing of solid phase particles deionized water, stirs, and obtains the nanometer magnetofluid for fracturing fracture monitoring.
According to the present invention, preferred, the Fe described in step (1) 2+/ Fe 3+molar ratio is 0.7, described Fe 3+concentration be 0.2mol/L, described divalent iron salt is ferrous sulfate, frerrous chloride or iron ammonium sulfate, described trivalent iron salt is iron chloride, ferric sulfate, described aqueous slkali is sodium hydroxide solution, potassium hydroxide solution or ammoniacal liquor.
According to the present invention, preferred, the OH described in step (2) -/ Fe 3+mol ratio is 4.4, and reaction temperature is 50 ℃, and stir speed (S.S.) is 800r/min.
According to the present invention, preferred, the coating material/Fe described in step (3) 3o 4particle mol ratio is (0.2～0.4): 1,85 ℃ of slaking 1h;
Preferred, magnetic separation magnetic nanometer, with deionized water washing magnetic nanometer 3～5 times, is that 20wt.% is dispersed in deionized water by the concentration of magnetic nanometer, obtains the nanometer magnetofluid for fracturing fracture monitoring.
Nanometer magnetofluid of the present invention is monitored for fracturing fracture as contrast agent.
Nanometer magnetofluid of the present invention injects reservoir or crack can strengthen the susceptibility of nanometer magnetofluid overlay area greatly, series of features as a kind of contrast agent for characterize reservoir or crack, comprise reservoir parameter, interlayer heterogeneity, the features such as flaw size, shape, trend.The effect of coating material is by being adsorbed onto Fe 3o 4particle surface, on coating material, institute is electrically charged because of electrostatic repulsion maintenance Fe 3o 4stablizing of particle.
The preparation principle of nanometer magnetofluid:
By soluble in water to reactant divalent iron salt and trivalent iron salt, maintain at a certain temperature.Slowly add precipitation reagent, under certain stir speed (S.S.), guarantee that the magnetic particle particle diameter generating maintains in a narrower distribution.After reacting completely, add the modifying surface of coating material to magnetic particle, make it have strongly hydrophilic and good stability.
Nanometer Fe 3o 4the fundamental equation of chemical coprecipitation reaction is:
2Fe 3++Fe 2++8OH -=Fe 3O 4↓+4H 2O
Nanometer magnetofluid is as the principle of contrast agent:
Nanometer magnetofluid is injected to stratum or crack, can strengthen the relative permeability of overlay area, more easily externally-applied magnetic field is responded.
As hour (<5%) of solid volume fraction of nanometer magnetofluid, for easy calculating can be ignored the interaction between particle.The susceptibility of nanometer magnetofluid can calculate with Langevin formula,
&chi; = &pi;&phi; &mu; 0 M d 2 d 3 18 kT
In above formula, the solid volume fraction that φ is nanometer magnetofluid; μ 0for permeability of vacuum, 4 π × 10 -7n/A 2; M dfor the saturation magnetization of magnetic-particle, the A/m of unit; D is the average grain diameter of solid phase particles, the m of unit; K is Boltzmann constant, 1.38065 × 10 -23j/K; T is absolute temperature, unit K.
Relative permeability μ requal χ and add 1.
μ r=χ+1
The reservoir of saturated nanometer magnetofluid or the effective permeability in crack can calculate with Effective medium is theoretical, and the present invention uses implicit expression Bruggeman equation.
( 1 - ( 1 - S or ) &phi; ) &mu; f - &mu; e &mu; f + 2 &mu; e + ( 1 - S or ) &phi; &mu; m - &mu; e &mu; m + 2 &mu; e = 0
μ in above formula efor the relative permeability of saturated magnetic fluid medium, μ ffor the relative permeability of nanometer magnetofluid, μ mfor the relative permeability of rock or fracture matrix, φ is the effecive porosity in reservoir or crack, S orfor the residual oil porosity of reservoir, suppose that crude oil magnetic permeability is zero here.
Nanometer magnetofluid is injected to stratum or fracture medium, a transmitting coil is installed in down-hole, transmitting alternating magnetic field.Alternating magnetic field, through reservoir or fracture medium, under the effect of nanometer magnetofluid, produces secondary magnetic field in medium.Collect field signal by the recipient that is arranged in ground or offset well, then solve through computer inversion algorithm, can obtain the relevant parameter in target zone or crack.The monitoring principle schematic diagram of nanometer magnetofluid is referring to Fig. 2.
Compared with prior art, the invention has the beneficial effects as follows:
1. nanometer magnetofluid of the present invention has stronger hydrophily and stability, can be soluble in water arbitrarily, place one month without obviously layering.
2. nanometer magnetofluid of the present invention has higher molar susceptibility, nanometer Fe 3o 4granulated magnetic coefficient is 420～450cm 3/ g, under magnetic fields the response time short, can realize the object of quick Crack Monitoring.
3. Fe of the present invention 3o 4the toxicity of particle and coating material is little, and good biocompatibility is little on the impact of environment.
Raw material of the present invention be easy to get cheap, method simple possible, the reaction time is short, is suitable for suitability for industrialized production, effective for Crack Monitoring.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of magnetic nano particle stably dispersing in the aqueous solution in the nanometer magnetofluid prepared of the embodiment of the present invention 1.
Fig. 2 is the principle schematic that the present invention's nanometer magnetofluid carries out Crack Monitoring; Wherein, 1, crack, 2, nano particle, 3, payzone, 4, transmitting coil.
Fig. 3 be in the nanometer magnetofluid prepared of the embodiment of the present invention 1 surface modification agent modify after Fe 3o 4the transmission electron microscope photo (TEM) of nano particle.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but the present invention's scope required for protection is not limited to the related scope of embodiment.
Embodiment 1
A preparation method for the nanometer magnetofluid of monitoring for fracturing fracture, comprises that step is as follows:
(1) by 8.1gFeCl 36H 2o and 5.8gFeSO 47H 2o is dissolved in 75ml deionized water, is loaded in the three-necked bottle with heating water bath, and with mechanical separator speed, 800r/min stirs;
(2) water-bath is heated to 50 ℃, slowly add in three-necked bottle in 5.3gNaOH being dissolved in to 75ml deionized water under mechanical separator speed 800r/min stirring condition, keep 30min; After reacting completely, with salt acid for adjusting pH to 5;
(3) add 20ml to be dissolved with the deionized water of 2.55g bis-hydration trisodium citrates, be warming up to 85 ℃, keep 1h, make the further slaking of particle;
(4) with permanent magnet, magnetic nanoparticle is drawn to bottom, removes supernatant liquor, add deionized water washing, repeat 3 times; Add 23ml deionized water as carrier fluid, dispersed with stirring is even, obtains the nanometer magnetofluid for fracturing fracture monitoring.
Embodiment 2
A preparation method for the nanometer magnetofluid of monitoring for fracturing fracture, comprises that step is as follows:
(1) by 6.1gFeCl 36H 2o and 2.7gFeCl 24H 2o is dissolved in 75ml deionized water, is loaded in the three-necked bottle with heating water bath, and with mechanical separator speed, 800r/min stirs;
(2) water-bath is heated to 50 ℃, slowly add in three-necked bottle in 3.78gNaOH being dissolved in to 75ml deionized water under mechanical separator speed 800r/min stirring condition, keep 30min; After reacting completely, with salt acid for adjusting pH to 5;
(3) add 20ml to be dissolved with the deionized water of 1.1g enuatrol, be warming up to 85 ℃, keep 1h, make the further slaking of particle;
(4) with permanent magnet, magnetic nanoparticle is drawn to bottom, removes supernatant liquor, add deionized water washing, repeat 3 times; Add 16ml deionized water as carrier fluid, dispersed with stirring is even, obtains the nanometer magnetofluid for fracturing fracture monitoring.
Embodiment 3
A preparation method for the nanometer magnetofluid of monitoring for fracturing fracture, comprises that step is as follows:
(1) by 8.1gFeCl 36H 2o and 5.8gFeSO 47H 2o is dissolved in 75ml deionized water, is loaded in the three-necked bottle with heating water bath, and with mechanical separator speed, 800r/min stirs;
(2) water-bath is heated to 50 ℃, under mechanical separator speed 800r/min stirring condition, add 25～28wt% ammoniacal liquor 7.3ml, keep 30min; After reacting completely, with salt acid for adjusting pH to 5;
(3) add 20ml to be dissolved with the deionized water of 1.76g bis-hydration trisodium citrates, be warming up to 85 ℃, keep 1h, make the further slaking of particle;
(4) with permanent magnet, magnetic nanoparticle is drawn to bottom, removes supernatant liquor, add deionized water washing, repeat 3 times; Add 23ml deionized water as carrier fluid, dispersed with stirring is even, obtains the nanometer magnetofluid for fracturing fracture monitoring.
Embodiment 4
For a preparation method for the nanometer magnetofluid of fracturing fracture monitoring, step is with embodiment 1, and the heating-up temperature that different is in step (2) is 40 ℃; Curing temperature in step (3) is 90 ℃.
Embodiment 5
A preparation method for the nanometer magnetofluid of monitoring for fracturing fracture, comprises that step is as follows:
(1) by 8.1gFeCl 36H 2o and 5gFeSO 47H 2it is even that O is dissolved in 75ml deionized water for stirring, adds in the there-necked flask with heating water bath, and with rotating speed, 800r/min stirs;
(2) under stirring condition, 7.39gKOH is dissolved in to 75ml deionized water, adds reaction system, 45 ℃ of reaction 20min, regulate pH to 6;
(3) 1.75g sodium ethylene diamine tetracetate is dissolved in to 20ml deionized water, is warming up to 80 ℃, keep 2h, make the further slaking of particle;
(4) with permanent magnet, nano magnetic particle is drawn to bottom, removes supernatant liquor, add deionized water washing, repeat 3 times; Add 22ml deionized water as carrier fluid, dispersed with stirring is even, obtains the nanometer magnetofluid for fracturing fracture monitoring.
Embodiment 6
A preparation method for the nanometer magnetofluid of monitoring for fracturing fracture, comprises that step is as follows:
(1) by 8.1gFeCl 36H 2o and 6.7gFeSO 47H 2o is dissolved in 75ml deionized water, adds in the three-necked bottle with heating water bath, and with rotating speed, 800r/min stirs;
(2) water-bath is heated to 50 ℃, 5.5gNaOH is dissolved in 75ml deionized water, slowly add in three-necked bottle, keep 30min, with salt acid for adjusting pH to 5;
(3) 1.3g lauryl sodium sulfate is dissolved in to solution in 20ml deionized water, adds reaction system, be warming up to 85 ℃, keep 1h, make the further slaking of particle;
(4) with permanent magnet, nano magnetic particle is drawn to bottom, removes supernatant liquor, add deionized water washing, repeat 3 times; Add 22ml deionized water as carrier fluid, dispersed with stirring is even, obtains the nanometer magnetofluid for fracturing fracture monitoring.
Particle diameter, mole susceptibility and stability and the particle concentration of the nanometer magnetofluid magnetic nanoparticle for fracturing fracture monitoring prepared by embodiment 1-6 are investigated, and result is as shown in table 1 below.
Table 1
Figure BDA0000476071960000061

Claims (10)

1. for a nanometer magnetofluid for fracturing fracture monitoring, it is characterized in that this nanometer magnetofluid is the Fe modifying with surface modification agent 3o 4particle is magnetic-particle, and water is that carrier fluid forms; Described Fe 3o 4the particle size range of particle is 10～25nm, described Fe 3o 4the molar susceptibility of particle is 290～450cm 3/ mol, described Fe 3o 4the particle concentration of particle is 18～30wt.%; Described coating material is natrium citricum, sodium ethylene diamine tetracetate, enuatrol or lauryl sodium sulfate; Described coating material and Fe 3o 4the mol ratio of particle is (0.1～0.8): 1.
2. the nanometer magnetofluid for fracturing fracture monitoring according to claim 1, is characterized in that described Fe 3o 4the particle size range of particle is 12～15nm.
3. the nanometer magnetofluid for fracturing fracture monitoring according to claim 1, is characterized in that described Fe 3o 4the molar susceptibility of particle is 420～450cm 3/ mol.
4. the nanometer magnetofluid for fracturing fracture monitoring according to claim 1, is characterized in that described Fe 3o 4the particle concentration of particle is 20～22wt.%.
5. a preparation method for the nanometer magnetofluid for fracturing fracture monitoring described in claim 1～4 any one, comprises that step is as follows:
(1) press Fe 2+/ Fe 3+molar ratio is 0.6～0.8 by divalent iron salt and trivalent iron salt even, the described Fe that is dissolved in deionized water for stirring 3+concentration be 0.15～0.25mol/L;
(2) under stirring condition, press OH -/ Fe 3+mol ratio is 4.2～4.6 to add aqueous slkali to precipitate, and 40～50 ℃ of reaction 20～40min, regulate pH to 5～7, obtain Fe 3o 4particle;
(3) press coating material/Fe 3o 4particle mol ratio is (0.1～0.8): 1 adds finishing agent solution, 80～90 ℃ of slaking 0.5～2h, and described coating material is natrium citricum, sodium ethylene diamine tetracetate, enuatrol or lauryl sodium sulfate; Magnetic separation goes out solid phase particles, removes supernatant, by being dispersed in deionized water after the washing of solid phase particles deionized water, stirs, and obtains the nanometer magnetofluid for fracturing fracture monitoring.
6. the preparation method of the nanometer magnetofluid for fracturing fracture monitoring according to claim 5, is characterized in that the Fe described in step (1) 2+/ Fe 3+molar ratio is 0.7, described Fe 3+concentration be 0.2mol/L, described divalent iron salt is ferrous sulfate, frerrous chloride or iron ammonium sulfate, described trivalent iron salt is iron chloride, ferric sulfate, described aqueous slkali is sodium hydroxide solution, potassium hydroxide solution or ammoniacal liquor.
7. the preparation method of the nanometer magnetofluid for fracturing fracture monitoring according to claim 5, is characterized in that the OH described in step (2) -/ Fe 3+mol ratio is 4.4, and reaction temperature is 50 ℃, and stir speed (S.S.) is 800r/min.
8. the preparation method of the nanometer magnetofluid for fracturing fracture monitoring according to claim 5, is characterized in that the coating material/Fe described in step (3) 3o 4particle mol ratio is (0.2～0.4): 1,85 ℃ of slaking 1h.
9. the preparation method of the nanometer magnetofluid for fracturing fracture monitoring according to claim 5, it is characterized in that after the middle magnetic separation magnetic nanometer of step (3), with deionized water washing magnetic nanometer 3～5 times, be that 20wt.% is dispersed in deionized water by the concentration of magnetic nanometer, obtain the nanometer magnetofluid for fracturing fracture monitoring.
10. the nanometer magnetofluid described in claim 1～4 any one is monitored for fracturing fracture as contrast agent.
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CN108676109B (en) * 2018-05-08 2021-02-09 中国石油大学(华东) Nanofluid for interwell tracing and preparation method and application thereof

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