CN106146722A - Amphion complex microsphere and its preparation method and application - Google Patents
Amphion complex microsphere and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of amphion complex microsphere and its preparation method and application.It includes the component of following weight portion: monomer 10 50 parts, cross-linking agent 0.05 1 parts, 0.2 10 parts of alkali, inserts 0 40 parts, initiator 0.05 1 parts, deionized water 40 70 parts.The amphion complex microsphere of the present invention has resistance to high salinity, the profile-controlling and plugging agent of high temperature resistant formation condition performance as oil field profile control transfer drive, overcome the existing profile-controlling and plugging agent defect in the ground environment stability inferior difference of high temperature and high salt, can be used for high temperature, high salinity oil field profile control and water plugging, improve recovery ratio.
Description
Technical field
The present invention relates to a kind of amphion complex microsphere and its preparation method and application, particularly relate to one
Oil field profile control transfer drive have resistance to high salinity, the amphion complex microsphere of high temperature resistant formation condition performance and
Its preparation method and it is as profile-controlling and plugging agent application in oilfield exploitation.
Background technology
During water flooding, due to anisotropism and the difference of viscosity of oil reservoir vertical and horizontal,
Can cause injecting water to prolong high permeability zone and advance by leaps and bounds, stream less permeable layer, thus formed inject fluid involve less than
Region, even occurs that region of bypassed oil, oil well produced liquid moisture content are increased.It is accomplished by using profile control agent to carry out profile control
Operation.
Oil field at home majority has been enter into development late stage at present, and oil saturation is gradually lowered.Current domestic mainly
Reservoir reserve concentrates on Midwest, such as Tarim Oilfield etc..And the oil field that oil reservoir enriches is due to its high mineralization
Degree, the formation condition of high temperature seriously limit the use of conventional profile control agent.So amphion complex microsphere
Study the most urgent for the oil field profile control of high temperature and high salt.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of simple in construction, low cost, X easy and simple to handle.
For reaching above-mentioned purpose, one amphion complex microsphere of the present invention, including the component system of following weight portion
For forming: monomer 10-50 part, cross-linking agent 0.05-1 part, alkali 1-10 part, inserts 0-40 part, draw
Send out agent 0.05-1 part, deionized water 40-70 part,
Wherein said monomer is selected from acrylic acid, acrylamide, sodium acrylate, methacrylic acid, metering system
Amide, N-[2-(2-methyl-4-oxopentyl), 2-acrylamide-2-methylpro panesulfonic acid, methylacryoyloxyethyl front three
Ammonium chloride, dimethyl diallyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac, N-isopropyl third
Acrylamide, N,N-DMAA, N hydroxymethyl acrylamide, NVP, uncle N-
Butylacrylamide, N-hydroxyethyl acrylamide, hy-droxybutyl, acrylic acid diethyl alcohol ester, methyl-prop
Olefin(e) acid ethylene oxidic ester, one or both of hydroxyethyl methylacrylate and methacrylic acid ethyl acetoacetate
Above with the mixture of arbitrary proportion.
Wherein said cross-linking agent is selected from methene base acrylamide, Ethylene glycol dimethacrylate, trihydroxy methyl
Propane triacrylate, allyl methacrylate, Polyethylene Glycol and acrylate, aluminum chloride and trichlorine
Change one or more of chromium with the mixture of arbitrary proportion.
Wherein said alkali is that one or more of sodium carbonate, sodium bicarbonate and sodium hydroxide are with arbitrary proportion
Mixture.
Wherein said inserts be bentonite, montmorillonite, kieselguhr, clay, Kaolin, ground calcium carbonate,
One or more of precipitated calcium carbonate and modified starch are with the mixture of arbitrary proportion.
Wherein said initiator is potassium peroxydisulfate, sodium peroxydisulfate, sodium sulfite, sodium sulfite, peroxidating
One or more of benzoyl, hydrogen peroxide and azodiisobutyronitrile are with the mixture of arbitrary proportion.
A kind of method preparing described amphion complex microsphere, comprises the following steps: by described deionization
Water, described alkali mix homogeneously, temperature reduces to less than 20 DEG C, adds described monomer, and temperature remains at 20
Below DEG C, adding described cross-linking agent, described inserts, mix homogeneously, add described initiator, stirring is all
Even, make system solidify under the conditions of system is positioned over 45 DEG C, after reacting completely, place in 65 DEG C of environment old
Changing 1h-4h, polyreaction i.e. completes, and dries and pulverizes and get final product.
Wherein said amphion complex microsphere is as profile-controlling and plugging agent application in oilfield exploitation.
The present invention is that the amphion complex microsphere of the present invention contains approrpiate wts proportioning unlike the prior art
Each components by weight percent, which overcoming original profile control agent can not the formation condition of resisting high temperature, high salt, it is impossible to for height
The shortcoming in temperature high salt oil field；Amphion complex microsphere of the present invention is owing to utilizing zwitterionic monomer to be polymerized
Space net structure, and introduced the group of heat-resistant salt-resistant, there is the characteristic of heat-resistant salt-resistant after polymerisation.
It is steady under the ground environment of high temperature and high salt that the amphion complex microsphere of the present invention overcomes existing profile-controlling and plugging agent
The defect of qualitative difference, can be used for high temperature, high salinity oil field profile control and water plugging, improves recovery ratio.
Accompanying drawing explanation
Fig. 1 is that the present invention increases multiple and time curve mensuration figure with common micro-ball mean diameter.
Detailed description of the invention
Below in conjunction with embodiment, to the present invention, above-mentioned and other technical characteristic and advantage are made in more detail
Bright.
Embodiment 1
By deionized water 57kg, sodium hydroxide 3.7kg mix homogeneously, temperature is reduced to less than 20 DEG C, is added single
Body acrylic acid 5kg, 2-acrylamide-2-methylpro panesulfonic acid 5kg, acrylyl oxy-ethyl-trimethyl salmiac 7
Kg, N hydroxymethyl acrylamide 2kg, temperature remains at less than 20 DEG C, adds cross-linking agent methene base
Acrylamide 0.1kg, filler bentonite 20kg, mix homogeneously, add initiator potassium persulfate 0.1kg,
Anhydrous sodium sulfite 0.1kg, stirs.Make system solidify under the conditions of system is placed on 45 DEG C, treat completely
After reaction, placing aging 2h in 65 DEG C of environment, polyreaction i.e. completes, and dries and pulverizes and get final product.
Embodiment 2
By deionized water 50kg, sodium carbonate 5.5kg mix homogeneously, temperature is reduced to less than 20 DEG C, is added monomer
Acrylamide 2kg, acrylic acid 8kg, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 5kg, N, N-dimethyl
Acrylamide 4kg, temperature remains at less than 20 DEG C, adds cross-linking agent methene base acrylamide 0.2kg,
Filler height territory 25kg, mix homogeneously, add initiator ammonium persulfate 0.2kg, anhydrous sodium sulfite
0.1kg, stirs.Make system solidify under the conditions of system is placed on 45 DEG C, after reacting completely, place
Aging 2h in 65 DEG C of environment, polyreaction i.e. completes, and dries and pulverizes and get final product.
Embodiment 3
By deionized water 50kg, sodium hydroxide 3.5kg mix homogeneously, temperature is reduced to less than 20 DEG C, is added single
Body acrylamide 4kg, 2-acrylamide-2-methylpro panesulfonic acid 10kg, acrylyl oxy-ethyl-trimethyl chlorination
Ammonium 3kg, N-hydroxyethyl acrylamide 2kg, temperature remains at less than 20 DEG C, adds cross-linking agent first
Base allyl acrylate 0.2kg, filler triple superphosphate 27kg, mix homogeneously, add initiator ammonium persulfate 0.2
Kg, anhydrous sodium sulfite 0.1kg, stir.Make system solidify under the conditions of system is placed on 45 DEG C, treat
Completely after reaction, placing aging 2h in 65 DEG C of environment, polyreaction i.e. completes, and dries and pulverizes and get final product.
Embodiment 3 amphion complex microsphere increases the mensuration of multiple with common micro-ball mean diameter
1 instrument
Steel cylinder: stainless steel, heatproof 120 DEG C, pressure 1.5MPa, internal diameter × interior height=30mm × 120mm,
Rustless, dirty, buchner funnel, calorstat in bottle: room temperature to 200 DEG C, temperature waviness is not more than 2 DEG C, electronics
Balance: scale division value 0.0001g, spoon, test tube: internal diameter × interior height=15mm × 100mm, bottle,suction: 500ml,
Vacuum pump: the American-European gram LS-pop6 type of (0～0.1MPa), laser particle size analyzer；Grain diameter measurement scope:
0.2-500μm；Repeatability error: ＜ 3%；Data sampling persistent period: 1s～100s；Shading ratio requires:
8%～12%, measuring cup: 100ml, beaker: 250ml, volumetric flask: 1000ml, qualitative filter paper, absorbent cotton,
Salt: sodium chloride, anhydrous calcium chloride, Magnesium dichloride hexahydrate, is analytical pure, distilled water.
2 determination steps
2.1 saline
Weigh sodium chloride 200.00g (all claiming accurate to 0.01g), be respectively placed in beaker, add distilled water and dissolve,
Then solution is all proceeded in 1000ml volumetric flask, with distilled water diluting to scale, shake up.Above-mentioned saline
Salinity is 200000mg/kg.
Mensuration 2.2.1 of 2.2 initial mean particle size, by Particle Size Analyzer and computer line, opens computer.
Open Particle Size Analyzer on and off switch, preheat half an hour, with stable laser output.By in laser beam
The heart is adjusted to consistent with the center of annular photodetector, runs laser particle size analyzer program, arranges corresponding system
System parameter.
2.2.2 weigh 0.07g sample (accurately to 0.01g), measure 50ml kerosene, do dispersion with kerosene and be situated between
Matter, joins in measuring cup by sample and disperse medium, seals dust-proof, put into by measuring cup in ultrasonic washing unit,
Make the liquid level in rinse bath reach 1/2nd of measuring cup total height, open ultrasonic waves for cleaning electromechanical source, vibration
2min, after being uniformly dispersed, turns off ultrasonic waves for cleaning electromechanical source, takes out measuring cup.
2.2.3 sample cell kerosene cleans up, it is ensured that its surface is without dirt.
2.2.4 after above-mentioned preparation completes, start circulating pump, be measured behaviour according to instrument using method
Make.Test result shows with particle size distribution data table, profile shape, prints and takes passages related data.
2.2.5 resolve grading curve, read its initial particle scope, take its volume average particle size, be denoted as
R0。
The mensuration of the mean diameter of sample after 2.3 expansions
2.3.1 on electronic balance, weigh the sample (accurately to 0.01g) of about 1.0g, sample is put into examination
Simulation water corresponding for Guan Zhongyong fills test tube, clogs test tube mouth with absorbent cotton, is placed in steel cylinder by test tube, examination
Pipe and steel cylinder gap are also injected into identical saline, keep the water surface less than test tube mouth.After steel cylinder is sealed with lid
Uprightly put in calorstat, constant temperature 24h.In calorstat, controlling temperature is (120 ± 2) DEG C.
2.3.2 connect vacuum pump, bottle,suction, buchner funnel, buchner funnel is installed double-deck qualitative filter paper.
From calorstat, steel cylinder is taken out, as in water bath with thermostatic control, temperature control (90 ± 2) DEG C, constant temperature 30min, from
Water-bath is taken out steel cylinder, opens lid, the sample expanded in test tube is poured in buchner funnel (residual
Sample expanded washes out with corresponding saline), sucking filtration, no longer having drop to ooze to buchner funnel bottom.
2.3.3 weigh the sample after 0.25g (accurately to 0.01g) sucking filtration, then weigh 50ml distilled water (point
Dispersion media), sample and disperse medium are added sequentially in measuring cup, measuring cup is put into ultrasonic washing unit,
Make the liquid level in rinse bath be positioned at the 1/2 of measuring cup total height, open ultrasonic waves for cleaning electromechanical source, vibrate 2min
After being uniformly dispersed, turn off ultrasonic waves for cleaning electromechanical source, take out measuring cup.
2.3.4 sample cell distilled water is cleaned, is dried, it is ensured that its surface cleaning.
2.3.5 after above-mentioned preparation completes, run laser particle size analyzer program, start circulating pump, press
It is measured operation according to instrument using method.Test result shows with particle size distribution data table, profile shape
Show, print and take passages related data.Read its volume average particle size, be R1。
3 calculate mean diameter increases multiple by formula (1) calculating:
δ=(R1-R0)/R0 (1)
In formula
The mean diameter of δ sample increases multiple；
R0The initial mean particle size of sample, μm；
R1The mean diameter of sample, μm after expansion.
The mean diameter of amphion complex microsphere of the present invention and common micro-ball increase multiple measurement result be shown in Table 1,
Table 2 and Fig. 1.
Table 1 amphion complex microsphere mean diameter increases multiple
| Time/sky | Initial bubble particle diameter/D4,3 | Finally expand particle diameter/D4,3 | Mean diameter increase multiple/times |
| 1 | 44.05 | 212.7 | 3.83 |
| 3 | 44.05 | 214.78 | 3.88 |
| 7 | 44.05 | 213.14 | 3.84 |
| 15 | 44.05 | 215.89 | 3.90 |
| 30 | 44.05 | 215.37 | 3.89 |
| 60 | 44.05 | 216.61 | 3.92 |
| 90 | 44.05 | 216.63 | 3.92 |
| 120 | 44.05 | 215.16 | 3.88 |
| 180 | 44.05 | 215.64 | 3.90 |
| 240 | 44.05 | 216.43 | 3.91 |
| 270 | 44.05 | 216.99 | 3.93 |
| 300 | 44.05 | 214.67 | 3.87 |
| 330 | 44.05 | 215.91 | 3.90 |
| 360 | 44.05 | 214.87 | 3.88 |
| 390 | 44.05 | 214.18 | 3.86 |
| 420 | 44.05 | 214.98 | 3.88 |
Table 2 common micro-ball mean diameter increases multiple
| Time/sky | Initial bubble particle diameter/D4,3 | Finally expand particle diameter/D4,3 | Mean diameter increase multiple/times |
| 1 | 40.32 | 201.37 | 3.99 |
| 3 | 40.32 | 18361 | 3.55 |
| 7 | 40.32 | 219.91 | 4.45 |
| 15 | 40.32 | 206.58 | 4.12 |
| 30 | 40.32 | 73.29 | 0.82 |
| 60 | 40.32 | 65.47 | 0.62 |
| 90 | 40.32 | 46.91 | 0.16 |
Learnt by Tables 1 and 2,120 DEG C, under the conditions of 200000mg/kg salinity, common micro-ball exists
Occur when 30 days that mean diameter increases the phenomenon that strongly reduces of multiple, and the average particle of amphion complex microsphere
Footpath increases multiple value and can stablize more than 1 year.Amphion complex microsphere relatively common micro-ball the most of the present invention is more
There is the performance of heatproof, salt tolerant.
Embodiment described above is only to be described the preferred embodiment of the present invention, not to this
Bright scope is defined, on the premise of designing spirit without departing from the present invention, and those of ordinary skill in the art
The various deformation making technical scheme and improvement, all should fall into claims of the present invention and determine
Protection domain in.
Claims (7)
1. an amphion complex microsphere, it is characterised in that include that the component of following weight portion is prepared from:
Monomer 10-50 part, cross-linking agent 0.05-1 part, alkali 1-10 part, inserts 0-40 part, initiator 0.05-1
Part, deionized water 40-70 part,
Wherein said monomer is selected from acrylic acid, acrylamide, sodium acrylate, methacrylic acid, metering system
Amide, N-[2-(2-methyl-4-oxopentyl), 2-acrylamide-2-methylpro panesulfonic acid, methylacryoyloxyethyl front three
Ammonium chloride, dimethyl diallyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac, N-isopropyl third
Acrylamide, N,N-DMAA, N hydroxymethyl acrylamide, NVP, uncle N-
Butylacrylamide, N-hydroxyethyl acrylamide, hy-droxybutyl, acrylic acid diethyl alcohol ester, methyl-prop
Olefin(e) acid ethylene oxidic ester, one or both of hydroxyethyl methylacrylate and methacrylic acid ethyl acetoacetate
Above with the mixture of arbitrary proportion.
Amphion complex microsphere the most according to claim 1, it is characterised in that: described cross-linking agent selects
From methene base acrylamide, Ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate, methyl
Allyl acrylate, Polyethylene Glycol and acrylate, one or more of aluminum chloride and chromium trichloride
Mixture with arbitrary proportion.
Amphion complex microsphere the most according to claim 1, it is characterised in that: described alkali is carbonic acid
One or more of sodium, sodium bicarbonate and sodium hydroxide are with the mixture of arbitrary proportion.
Amphion complex microsphere the most according to claim 1, it is characterised in that: described inserts is
Bentonite, montmorillonite, kieselguhr, clay, Kaolin, ground calcium carbonate, precipitated calcium carbonate and modified shallow lake
One or more of powder are with the mixture of arbitrary proportion.
Amphion complex microsphere the most according to claim 1, it is characterised in that: described initiator is
Potassium peroxydisulfate, sodium peroxydisulfate, sodium sulfite, sodium sulfite, benzoyl peroxide, hydrogen peroxide and idol
One or more of nitrogen bis-isobutyronitrile are with the mixture of arbitrary proportion.
6. the method preparing amphion complex microsphere as according to any one of claim 1-5, its
Be characterised by comprising the following steps: by described deionized water, described alkali mix homogeneously, temperature reduce to 20 DEG C with
Under, adding described monomer, temperature remains at less than 20 DEG C, adds described cross-linking agent, described inserts,
Mix homogeneously, adds described initiator, stirs, and makes system solidify under the conditions of system is positioned over 45 DEG C,
After reacting completely, placing aging 1h-4h in 65 DEG C of environment, polyreaction i.e. completes, and dries and pulverizes and get final product.
7. according to amphion complex microsphere according to any one of claim 1-5 as profile-controlling and plugging agent at oil
Application in the exploitation of field.
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| CN106867488A (en) * | 2017-03-28 | 2017-06-20 | 四川光亚聚合物化工有限公司 | One kind physical crosslinking gel-like profile control and water plugging system and its application |
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| CN110204653A (en) * | 2019-06-17 | 2019-09-06 | 黑龙江益瑞化工有限公司 | A kind of oilfield chemistry oil recovery profile-controlling and plugging agent amphoteric ion polymer particle |
| CN110819324A (en) * | 2019-10-24 | 2020-02-21 | 白成才 | Profile control water shutoff agent and preparation method thereof |
| CN111234790A (en) * | 2020-02-19 | 2020-06-05 | 中国石油大学(华东) | Gel particles suitable for low-permeability fractured carbon dioxide flooding oil reservoir, profile control agent, preparation method and application |
| CN111320974A (en) * | 2020-04-20 | 2020-06-23 | 大庆市新万通科技开发有限公司 | Acidizing temporary plugging agent and preparation method and application thereof |
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| CN109233769A (en) * | 2018-09-07 | 2019-01-18 | 中国石油化工股份有限公司 | A kind of pre-crosslinked gel particle and preparation method thereof for low-temperature reservoir profile control |
| CN110204653A (en) * | 2019-06-17 | 2019-09-06 | 黑龙江益瑞化工有限公司 | A kind of oilfield chemistry oil recovery profile-controlling and plugging agent amphoteric ion polymer particle |
| CN110819324A (en) * | 2019-10-24 | 2020-02-21 | 白成才 | Profile control water shutoff agent and preparation method thereof |
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| CN111320974B (en) * | 2020-04-20 | 2021-03-23 | 大庆市新万通科技开发有限公司 | Acidizing temporary plugging agent and preparation method and application thereof |
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