CN104774602A - High-temperature-resistant blocking agent, and preparation method and application thereof - Google Patents
High-temperature-resistant blocking agent, and preparation method and application thereof Download PDFInfo
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- CN104774602A CN104774602A CN201410017495.9A CN201410017495A CN104774602A CN 104774602 A CN104774602 A CN 104774602A CN 201410017495 A CN201410017495 A CN 201410017495A CN 104774602 A CN104774602 A CN 104774602A
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Abstract
The invention relates to a high-temperature-resistant blocking agent comprising 80-95 wt% of an inorganic solid powder, 5-18 wt% of an organosilicone resin and 0-2 wt% of an emulsifier. The invention also provides a preparation method of the blocking agent, wherein the preparation method includes that with adopting of a fluidized bed processing method, the organosilicone resin and an optionally emulsifier emulsion are uniformly sprayed on the surface of the inorganic solid powder and then dried to obtain the product. The invention further provides an application of the blocking agent, the blocking agent can be directly used in the sealing channeling water blocking construction field, and can also be in cooperative use with a viscosity regulator and a curing regulator; the steam channeling blocking and water blocking construction success rate of the obtained blocking agent system is 100%, and relatively good production-increasing effect is achieved.
Description
Technical field
The present invention relates to a kind of high temperature resistant plugging agent, preparation method and application, belong to field of petroleum exploitation.
Background technology
Due to the continuous increase of energy demand in world wide, the exploitation dynamics of the resources such as oil and gas continues to increase, and routine, shallow-layer reserves are day by day exhausted.The exploitation focus of current hydrocarbon resources has turned to the fields such as heavy crude reservoir, deep-seated oil gas reservoir and unconventional petroleum resources.
Deep-seated oil gas reservoir along with the progress of current exploration engineering, find and success develop proportion increasing.Deep-seated oil gas reservoir is because depth of burial is generally more than 4000 meters, and its lithology is based on the fractured reservoir such as carbonate, volcanics.Its reservoir geology situation is complicated, and Reservoir Heterogeneity is comparatively strong, and crack is generally grown, crack differs more than 100 times with the effective permeability of matrix, therefore cause oil reservoir after exploitation for some time, often cause production fluid High water cut because local water invades, reduce development effectiveness.
Because deep-seated oil gas reservoir has high temperature, high pressure, buries the features such as dark and high angle fracture growth, hole condition is complicated, after oil well produces water, cause plug water construction difficulty very large, up to now, also not having proven technique for using for reference, to need to carry out technological innovation in plugging agent and water-plugging technology to Deep Reservoirs water blockoff at home and abroad, improving water blockoff success ratio.
Viscous crude proportion in crude oil in China output rises year by year.At present, domestic and international expert thinks that the most effective viscous oil recovery method injects high temperature and high pressure steam, reduces Viscosity of Heavy Crude Oil with heat effect, so that exploitation.In steam treatment process, owing to being subject to that reservoir heterogeneity is strong, the impact of steam and the unfavorable factor such as viscous crude mobility ratio difference is large, in heavy crude reservoir, injecting steam generation onlap and fingering phenomenon are very general, and then occur between well, and the vapour between well and Water table alters phenomenon.Serious vapour is altered and will be caused Heavy Oil Reservoir longitudinally upper to inhale vapour uneven, in plane steam alter into, reduce the swept volume of steam, cause heavy crude heat extraction recovery ratio not high, Produced Liquid High water cut, production cost raises.Alter improvement for the vapour in steam injection process, the technical cue taked at present uses chemical plugging agent to alter passage to vapour to carry out shutoff.But what inject due to heavy crude heat extraction is above-critical state steam, and its temperature is generally 200-350 DEG C, pressure is between 8-19MPa, therefore very high request is proposed to the heat resisting and pressure resisting performance of plugging agent and consolidation strength.
At present, conventional heavy crude heat extraction plugging agent has:
1) inorganic solid particles type plugging agent
Inorganic solid particles is the plugging agent commonly used the most, when selecting such plugging agent, first should preferred rational granular size, and make itself and oil reservoir alter hole duct and mate.Because oil reservoir variations in pore size is large, be difficult to prediction, the use success ratio of this plugging agent is lower.When particle size is greater than pore dimension, be difficult to inject fluid-channeling channel; When particle size is less than pore dimension, solid particulate is difficult to be detained at fluid-channeling channel, does not reach envelope and alters object.Have very high intensity after inorganic particle and grout consolidation, but the cement slurry sets time is short, can not carries out indepth plugging, serious to oil layer blocking, construction risk is large.
2) foam plugging agent
It is utilize in injecting steam process that foam envelope is altered, and adds tensio-active agent, makes it produce a large amount of foam blocking most permeable zone throat area, and steam turns to other hole due to pressure effect, improves the swept volume of steam, increases the inspiratory capacity of low permeability layer.The advantage of foam plugging agent is that injection is good, and plugging tool is selective.Its shortcoming is that the shut-off capacity sealing fluid-channeling channel is lower, and the foam stabilization time is short, and validity period is short, and construction cost is high.
3) polymer gel plugging agent
Polymer gel plugging agent is the nineties research and development in last century, and current oil field uses the most extensive, the good class plugging agent of net effect.Polymer gel plugging agent has the good feature of injection, but heat-resisting property is poor, if polyacrylamide gellike is after temperature is more than 150 DEG C, loses plugging action completely.
The effect that existing chemical plugging technology alters the field such as shutoff and steam entry profile adjustment, deep-seated oil gas reservoir water blockoff and unconventionaloil pool exploitation water blockoff at heavy crude heat extraction vapour is greatly limited.Its reason is mainly manifested in, flowing property under the resistance to elevated temperatures of existing chemical plugging agent, high temperature and delayed coagulation performance not enough, when applying in above-mentioned hot environment, inject reservoir process in blocking agent and occur multiviscosisty, the unexpected situation such as to solidify, oil deposit deep part can not be injected by design requirements and solidify and the passage of shutoff steam, local water channelling.Therefore, for the technical need in above oil and gas development field, the present invention proposes a kind of high temperature resistant plugging agent and using method, can apply and the field of petroleum exploitation such as heavy crude heat extraction, deep-seated oil gas reservoir, effective shutoff is carried out to injecting steam, local water, improves oil and gas development effect.
Summary of the invention
An object of the present invention is to provide a kind of high temperature resistant plugging agent, alters, technical need that shutoff is carried out in water breakthrough to solve in the production of hydrocarbons field such as heavy crude heat extraction, deep-seated oil gas reservoir to vapour.
Another object of the present invention is to provide the preparation method of described high temperature resistant plugging agent.
Another object of the present invention is to provide the application of described high temperature resistant plugging agent.
One provided by the invention is high temperature resistant plugging agent, comprises following component by weight percentage: inorganic solid phase powder 80 ~ 95wt%, silicone resin 5 ~ 18wt%, emulsifying agent 0 ~ 2wt%.
Described inorganic solid phase powder is calcium carbonate, kaolin or its mixture, and particle size range is 1-50 μm, is preferably 5-20 μm.
In one particular embodiment of the present invention, preferred described inorganic solid phase powder is for containing calcium carbonate 70 ~ 90wt%, and surplus is kaolinic mixture.
Described silicone resin is polysilane and/or polysiloxane, and preferably its molecular weight ranges is 10
4~ 10
6.
In one particular embodiment of the present invention, the chemical formula of described silicone resin is R (CH
2)
nsi (OR ＇)
3, wherein R is the alkyl of C5-C9, as pentyl, heptane base, iso-octyl, octyl group etc.; R ' is methyl, ethyl or propyl group, and n is the integer of 700 ~ 70000.Be specifically as follows octyltri-ethoxysilane and/or heptan alkyl triethoxysilane.
Described emulsifying agent is selected from least one in non-ionic polyoxyethylene ether surfactant, stearate/ester and sulfonated petro-leum, be preferably at least one in calcium stearate, glyceryl monostearate and calcium mahogany sulfonate, be more preferably glyceryl monostearate and/or calcium mahogany sulfonate.Owing to containing a large amount of oxygen in silicone resin, there is natural surfactivity, therefore can not add emulsifying agent when working concentration is lower.
Present invention also offers the preparation method of described high temperature resistant plugging agent, comprise and adopt fluidized-bed working method by silicone resin emulsion even application in inorganic solid phase powder surface, oven dry obtains high temperature resistant plugging agent of the present invention.
Described silicone resin emulsion is the aqueous emulsion of aforementioned organic silicon resin and optional emulsifying agent, and preferably it comprises following component by weight percentage:
A) silicone resin of 5 ~ 60wt%;
B) emulsifying agent of 0 ~ 5wt%; And
C) surplus is water.
Described emulsion is prepared by method well known in the art.Such as: in the distilled water of metering or other dosing water, add emulsifying agent under agitation condition, slowly add silicone resin after a small amount of foam to be generated, namely react after described silicone resin and water dilute, the emulsion obtained needed finished using the same day.
In one particular embodiment of the present invention, described emulsion is commerical prod, can be selected from SMK1311, SMK2100 or SMK550 that the production of (China) company limited is digested by Germany watt, optimum with SMK1311.The DOW that Dow Corning Corporation produces can also be selected
q2-7523, and the model that An Zhi Electron Material Co., Ltd produces is the polysiloxane of S05.
After ultrafine inorganic powder surface-coated silicone resin, prepared plugging agent can inject that the vapour of heavy crude reservoir is altered, water breakthrough passage easily, and under the high temperature action of thermal recovery injecting steam, between silicone resin, and will bonding reaction be there is between silicone resin and powder, form spacial framework and rapidly solidified.Meanwhile, under the solidification modulator effect that plugging agent adds when preparing, its set time and solidification intensity are all adjustable.
In one particular embodiment of the present invention, the preparation method of described high temperature resistant plugging agent comprises:
1) inorganic solid phase powder is loaded in fluidized-bed reactor, open blower fan and the heating unit of fluidized-bed reactor, make the inorganic solid phase powder in fluidized-bed reactor keep boiling flowing;
2) described emulsion is sprayed in fluidized-bed reactor, make emulsion that inorganic solid phase powder coated is completed granulation, obtain described high temperature resistant plugging agent.
Preferably in step 1), fan delivery is 150 ~ 200m
3/ min, Heating temperature is 55 DEG C ~ 65 DEG C.
Preferably in step 2) in, when the air outlet temperature of fluidized-bed reactor and the blast inlet temperature difference are less than 2.0 DEG C, be that described emulsion sprays in fluidized-bed reactor with the flow velocity of 20 ~ 100ml/min by the pressurized air of 0.6-0.8MPa with pressure, after emulsion has been sprayed, Heating temperature is set as 100 DEG C ~ 105 DEG C, adjustment fan delivery is 200 ~ 300m
3/ min, boiling constant temperature reacted end after 10 ~ 20 minutes.
The mass ratio of preferred described inorganic solid phase powder and described emulsion is 4 ~ 19:1.
In chemistry and petroleum industry, when curable materials such as particle or powder surface coated with resins, traditional method adopts to stir cladding process or spin coating method.Paddling process is placed in stirring tank by particle or powder, after being heated to certain temperature, slowly adding coated material and stir, then obtain finished product through mixing, the process such as broken and dry; Spin coating method is placed in tilt rotary furnace by particle or powder, after being heated to certain temperature, under certain rotation speed, adds coated material, then obtain finished product through mixing, the process such as broken and dry; There is more problem in these two kinds of coating methods, as: use oil phase solvent to have potential safety hazard in production, product hardens in production unit, coating uniformity is poor, coat-thickness is difficult to control, product aftertreatment technology is complicated and tooling cost is high.
The present invention adopts aqueous phase silicone resin, applies ultra-thin silicone resin coating with fluidization at inorganic solid phase powder surface, and prepared high temperature resistant plugging agent is the breakthrough of traditional plugging agent technology of preparing.By the optimization to silicone resin emulsion formula, base material and fluidized bed coating process technique, overlay thickness can be formed at plugging agent particle surface and be less than the continuous coated of traditional way, thus make the chemical resistant properties of plugging agent, resistance to elevated temperatures and consolidation rate, induration mechanical property is all better than plugging agent prepared by conventional art.Thus effectively reduce silicone resin consumption, while significantly reducing costs, promote sealing characteristics.
Invention further provides the application of described high temperature resistant plugging agent.Described high temperature resistant plugging agent can be directly used in envelope and alter plug water construction field, also can with viscosity-controlling agent and solidify conditioning agent with the use of, enhancing plugging effect.
In one particular embodiment of the present invention, provide a kind of high temperature resistant water base temperature-sensitive solidification blocking agent system, comprise the following component be calculated in mass percent:
I) viscosity-controlling agent 1 ~ 5wt%;
Ii) high temperature resistant plugging agent 5 ~ 35wt%;
Iii) conditioning agent 2.5 ~ 12.5wt% is solidified; And
Iiii) surplus is water.
Described viscosity-controlling agent and high temperature resistant plugging agent are well known in the art.Described viscosity-controlling agent is preferably partially hydrolyzed polyacrylamide and/or treated starch, is preferably treated starch.Described partially hydrolyzed polyacrylamide (HPAM) is prepared by basic hydrolysis methacrylamide homopolymer, and degree of hydrolysis is 10 ~ 25%, molecular weight is 6,000,000 ~ 12,000,000; Described treated starch is prepared through etherification modified by native starch, and granularity is less than 350 microns, viscosity 500 ~ 1000mPa.s (determination of aqueous solution of 1wt%);
Described solidification conditioning agent is preferably at least one in organic amine, silicon nitrogen resin and silica resin, as at least one in diethylenetriamine, triethylene tetramine, tetraethylene pentamine, poly-methylsilazane and PSI, is preferably tetraethylene pentamine.The molecular weight of preferred described poly-methylsilazane and PSI is within 10,000 ~ 200,000.
The preparation of described high temperature resistant water base temperature-sensitive solidification blocking agent system, be under whipped state, viscosity-controlling agent is added to the water, be stirred to after fully dissolving and add high temperature resistant plugging agent, be stirred to dispersed after, add solidification conditioning agent again, after stirring, can plugging construction be carried out.
In one particular embodiment of the present invention, under the condition of fully circulation or stirring, in water, slowly, in batches add viscosity-controlling agent, circulation stirring more than 1 hour is to dissolving completely.Then add high temperature resistant plugging agent in batches, be stirred to dispersed after, then add solidification conditioning agent in batches, add to stir after terminating and form uniform and stable mixed solution in more than 0.5 hour, plugging construction can be carried out under Injection Well.
Described high temperature resistant water base temperature-sensitive solidification blocking agent system be low glutinous, high thixotropic fluid at normal temperatures, fast setting more than 150 DEG C, the induration that formation heatproof is greater than 350 DEG C, can alter, water breakthrough passage carries out permanent shutoff to the vapour of thick oil thermal extraction.There is high temperature resistant, the feature such as sealing ratiod is high, voltage endurance capability is strong, good stability, meet the process specifications of heavy oil thermal recovery fleeing proof water blockoff and deep-seated oil gas reservoir water blockoff completely.This blocking agent system has all carried out test in place at the steam flood steam injection well of Shengli Oil Field heavy crude heat extraction block, steam stimulation horizontal well, shutoff vapour alter with water blockoff be constructed into power 100%, obtain good effect of increasing production.
Accompanying drawing explanation
Fig. 1 is in an embodiment of plugging agent preparation method of the present invention, the schematic diagram of the fluidizer of use.
Wherein, 1-air compressor, 2-emulsion volume pump, 3-air intake well heater, 4-fluidized-bed main body, 5-exhaust air filter, 6-LS head, 7-aerofoil fan, 8-finished product travelling belt, 9-finished product discharge port, 10-fluidized-bed filter screen.
Embodiment
In the present invention, as follows the various performance index of high temperature resistant water base temperature-sensitive solidification blocking agent system are tested:
1. viscosity test: sample is loaded in the dull and stereotyped test macro of RS-6000 type rotational viscosimeter, the shearing rate of test slab is adjusted to 100s
-1after measure, after stable, record data are sample viscosity.
2. consolidation temperature (temperature of sample generation consolidation reaction) test: sample is loaded in the dull and stereotyped test macro of RS-6000 type rotational viscosimeter, at heat-up rate 2 DEG C/min, shearing rate 20s
-1by sample viscosity curve, the viscosity B coefficent of lower record sample, occurs that inflection temperature when significantly rising is designated as consolidation temperature.
3. consolidation time (completing the time to losing flowability from sample preparation) test: sample is loaded the dull and stereotyped test macro of RS-6000 type rotational viscosimeter, be warming up to the consolidation temperature of sample, at shearing rate 20s
-1under condition, record sample viscosity reaches the time of 1000mPa.s, is consolidation time.
4. penetration degree test: be a kind of universal method evaluating blocking agent concretion body strength, have the detecting instrument of standard to sell.Its detection method adopts standard weights test prong (load-carrying 50 grams) freely to fall from 15 cm heights, and reading test prong enters the degree of depth in induration, and namely represent the intensity of induration, unit is 1/10 millimeter.The larger expression induration of penetration degree is softer, otherwise then represents that induration is harder.
5. durability test: preparation blocking agent after constant temperature makes it solidify under consolidation temperature, testing needle in-degree, as the initial penetration degree of sample.To be positioned over constant temperature in 200 DEG C of baking ovens aging by airtight for sample, and regularly take out test intensity, and when recording penetration degree and being less than 90% of initial penetration degree, record digestion time is as durability index.
6. plugging strength test: preparation blocking agent injects the fill out sand tube of simulation core flow-through appt, closes fill out sand tube two ends, under consolidation temperature after isothermal curing, the aqueous phase breakthrough pressure of test fill out sand tube, represents plugging strength with the pressure gradient broken through.
Below in conjunction with drawings and Examples, the present invention is described in detail.
As shown in Figure 1, in fluidizer of the present invention, the air outlet of aerofoil fan 7 is connected with fluidized-bed main body 4 top by exhaust air filter 5, air intake well heater 3 is connected with bottom fluidized-bed main body 4, is connected with emulsion volume pump 2 for the air compressor 1 emulsion sprayed into the LS head 6 being positioned at fluidized-bed main body 4 inside.
The preparation method of described high temperature resistant plugging agent comprises:
Inorganic solid phase powder is positioned on the filter screen 10 in fluidized-bed main body 4, open the aerofoil fan 7 and exhaust air filter 5 that are connected successively with fluidized-bed main body 4 top, and with the air intake well heater 3 be connected bottom fluidized-bed main body 4, make inorganic solid phase powder in fluidized-bed main body 4 keep boiling flow state; Then air compressor 1 and emulsion volume pump 2 is opened, with pressurized air silicone resin emulsion be pumped to LS head 6 and spray in fluidized-bed main body 4, make emulsion that inorganic solid phase powder coated is completed granulation, boiling constant temperature stopping device after 10 ~ 20 minutes, from the finished product discharge port 9 of fluidized-bed main body 4, discharging is to finished product travelling belt 8, obtains described high temperature resistant plugging agent.
Preferably in step 1), the air quantity of aerofoil fan 7 is 150 ~ 200m
3/ min, the air outlet temperature of air intake well heater 3 is 55 DEG C ~ 65 DEG C.
Preferably in step 2) in, when air intake well heater 3 temperature out and the exhaust air filter 5 import temperature difference are less than 2.0 DEG C, air compressor 1 operating pressure is set as 0.6-0.8MPa, the flow set of emulsion volume pump 2 is 20 ~ 100ml/min, with pressurized air, silicone resin emulsion is sprayed in fluidized-bed main body 4, after emulsion has been sprayed, raise the power of air intake well heater 3, be 100 DEG C ~ 105 DEG C to its temperature out, regulating shaft flow fan 7 air quantity is 200 ~ 300m
3/ min, completes granulation.
The preparation of embodiment 1-6 is high temperature resistant plugging agent
Take a certain amount of inorganic solid phase powder (particle diameter is 1-50 μm) to load in fluidized-bed, open blower fan and the heating unit of fluidized-bed, adjustment fan delivery is 150m
3/ min makes the inorganic solid phase powder in fluidized-bed keep fully seething with excitement flowing, and hot blast temperature is set as 60 DEG C; When air outlet temperature and intake air temperature difference are less than 2.0 DEG C, by the consumption of table 1, spray pressure is set as 0.8MPa, with pressurized air, silicone resin emulsion is sprayed in fluidized-bed with the flow velocity of 25ml/min, after emulsion has been sprayed, hot blast temperature is set as 105 DEG C, adjustment fan delivery is 300m
3/ min, boiling constant temperature is after 15 minutes, and closure systems, takes out and be coated high temperature resistant plugging agent.
Calculate by the high temperature resistant plugging agent of preparation 1000g, the raw material usage of different ingredients is in table 1.
1000g plugging agent prepared by table 1, and each formula uses additive amount table
Annotation: CG ratio is calcium carbonate and kaolinic mass ratio in mixture
The preparation of water base temperature-sensitive solidification blocking agent system that embodiment 7-12 is high temperature resistant and performance evaluation
One, the preparation of high temperature resistant water base temperature-sensitive solidification blocking agent system
Calculate by the high temperature resistant water base temperature-sensitive solidification blocking agent system of preparation 1000g, the raw material usage of different ingredients is in table 2.
1000g finished product prepared by table 2, and each formula uses additive amount table
Wherein, partially hydrolyzed polyacrylamide is that Beijing Xitao Development Tech Co., Ltd. produces, model YT-550, molecular weight 8,000,000, degree of hydrolysis 18%.
Treated starch is that Shanghai Xiang Hu Industrial Co., Ltd. produces, model HR-30, pH=10, the viscosity 1200mPa.s(5wt% aqueous solution).
Poly-methylsilazane is that An Zhi Electron Material Co., Ltd produces, model NN-120, hot setting type, molecular weight 150,000.
PSI is the silicone product that An Zhi Electron Material Co., Ltd produces, model S05 series, specific inductivity K < 3.0.
By table 2 consumption, the high temperature resistant water base temperature-sensitive solidification blocking agent system of preparation embodiment 7-12.
According to the dosage requirement of different additive in table 2, under the state of fully circulation or stirring, in water, add the viscosity-controlling agent of metering slowly, in batches, after adding, keep circulation stirring more than 1 hour, dissolve completely to viscosity-controlling agent and be distributed in water.And then under abundant recurrent state, slow in aqueous phase, to be sequentially added into metering high temperature resistant plugging agent and solidification conditioning agent, then after stirring 0.5 hour, form uniform and stable mixed solution.
Two, the performance evaluation of high temperature resistant water base temperature-sensitive solidification blocking agent system
The index of water base temperature-sensitive that usual sign is high temperature resistant solidification blocking agent system performance has: viscosity, consolidation temperature, consolidation time, penetration degree, the index such as weather resistance, plugging strength at 200 DEG C.
After the high temperature resistant water base temperature-sensitive solidification blocking agent system newly prepared is placed 1h, stir, then test performance, the results are shown in following table 3.Wherein, comparative example is removed plugging agent and is adopted existing method for making, and namely inorganic solid phase powder+oil-phase resin is prepared in revolving pan, and other raw material and proportioning are with embodiment 8.Wherein, inorganic solid phase powder is calcium carbonate, silicon-dioxide, calcium sulfate etc., and oil-phase resin is that soluble phenolic resin is dissolved in medium-boiling solvent oil, is formulated as 10-25% strength solution and uses.
The performance of water base temperature-sensitive solidification blocking agent that table 3 is high temperature resistant
Test result shows, formula with high temperature resistant water base temperature-sensitive solidification blocking agent system is different, prepare the viscosity of blocking agent, consolidation temperature, consolidation time, penetration degree, the index such as weather resistance, plugging strength changes to some extent at 200 DEG C, particularly resistance to gentle ageing-resistant performance is given prominence to, and the high temperature resistant envelope that the properties of blocking agent meets the field of petroleum exploitation such as heavy crude heat extraction, deep-seated oil gas reservoir completely alters water-plugging technique requirement.And consolidation time, penetration degree, weather resistance, plugging strength are prepared far above existing method at 200 DEG C plugging agent.
It should be noted that above-described embodiment only for explaining the present invention, not forming any limitation of the invention.By referring to exemplary embodiments, invention has been described, but to should be understood to word wherein used be descriptive and explanatory vocabulary, instead of limited vocabulary.Can modify the present invention by the scope being defined in the claims in the present invention, and the present invention be revised not deviating from scope and spirit of the present invention.Although the present invention wherein described relates to specific method, material and embodiment, and do not mean that the present invention is limited to particular case disclosed in it, on the contrary, easily extensible of the present invention is to other all methods and applications with identical function.
Claims (10)
1. a high temperature resistant plugging agent, comprising: inorganic solid phase powder 80 ~ 95wt%, silicone resin 5 ~ 18wt% and emulsifying agent 0 ~ 2wt%.
2. plugging agent according to claim 1, it is characterized in that, described inorganic solid phase powder is particle size range 1-50 μm, is preferably the calcium carbonate of 5-20 μm, kaolin or its mixture, more preferably described inorganic solid phase powder is for containing calcium carbonate 70 ~ 90wt%, and surplus is kaolinic mixture.
3. plugging agent according to claim 1, is characterized in that, described silicone resin is polysilane and/or polysiloxane, and preferably its molecular weight ranges is 10
4~ 10
6; Described emulsifying agent is selected from least one in non-ionic polyoxyethylene ether surfactant, stearate/ester and sulfonated petro-leum, be preferably at least one in calcium stearate, glyceryl monostearate and calcium mahogany sulfonate, be more preferably glyceryl monostearate and/or calcium mahogany sulfonate.
4. the preparation method of plugging agent according to any one of claims 1 to 3, comprise and adopt fluidized-bed working method by the emulsion even application containing described silicone resin and optional emulsifying agent in inorganic solid phase powder surface, oven dry obtains described high temperature resistant plugging agent.
5. method according to claim 4, is characterized in that, comprising:
1) inorganic solid phase powder is loaded in fluidized-bed reactor, open blower fan and the heating unit of fluidized-bed reactor, make the inorganic solid phase powder in fluidized-bed reactor keep boiling flowing;
2) described emulsion is sprayed in fluidized-bed reactor, make emulsion that inorganic solid phase powder coated is completed granulation, obtain described high temperature resistant plugging agent.
6. method according to claim 5, is characterized in that, in step 1), fan delivery is 150 ~ 200m
3/ min, Heating temperature is 55 DEG C ~ 65 DEG C.
7. method according to claim 5, it is characterized in that, in step 2) in, when the air outlet temperature of fluidized-bed reactor and the blast inlet temperature difference are less than 2.0 DEG C, be that described emulsion sprays in fluidized-bed reactor with the flow velocity of 20 ~ 100ml/min by the pressurized air of 0.6-0.8MPa with pressure, after emulsion has been sprayed, Heating temperature is set as 100 DEG C ~ 105 DEG C, adjustment fan delivery is 200 ~ 300m
3/ min, boiling constant temperature reacted end after 10 ~ 20 minutes.
8. the method according to any one of claim 5 to 7, is characterized in that, the mass ratio of described inorganic solid phase powder and described emulsion is 4 ~ 19:1.
9. according to any one of claims 1 to 3, plugging agent is sealing the application of altering in plug water construction field.
10. a high temperature resistant water base temperature-sensitive solidification blocking agent system, comprises the following component be calculated in mass percent:
I) viscosity-controlling agent, 1 ~ 5wt%;
Ii) plugging agent produced of method described in plugging agent described in any one of claims 1 to 3 or any one of claim 4 to 7,5 ~ 35wt%;
Iii) conditioning agent is solidified, 2.5 ~ 12.5wt%;
Iiii) surplus is water;
Described viscosity-controlling agent is preferably partially hydrolyzed polyacrylamide and/or treated starch, is more preferably treated starch;
Described solidification conditioning agent is preferably at least one in organic amine, silicon nitrogen resin and silica resin, be more preferably at least one in diethylenetriamine, triethylene tetramine, tetraethylene pentamine, poly-methylsilazane and PSI, most preferably be tetraethylene pentamine.
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| CN108084983B (en) * | 2017-11-28 | 2020-10-23 | 中国石油大学(华东) | Temporary plugging agent and preparation method thereof |
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| CN111484833B (en) * | 2020-03-27 | 2022-08-12 | 中国石油天然气集团有限公司 | Low-friction film-forming plugging agent for high-temperature oil-based drilling fluid and preparation method and application thereof |
| CN111995995A (en) * | 2020-09-03 | 2020-11-27 | 西南石油大学 | Bulk-expanded particle heterogeneous crack plugging effect improving agent and preparation method thereof |
| CN111995995B (en) * | 2020-09-03 | 2021-04-30 | 西南石油大学 | Bulk-expanded particle heterogeneous crack plugging effect improving agent and preparation method thereof |
| CN113122217A (en) * | 2021-04-23 | 2021-07-16 | 西南石油大学 | Carbon-based amphiphilic nano-flow for oil displacement and preparation method thereof |
| CN113122217B (en) * | 2021-04-23 | 2022-07-05 | 西南石油大学 | Carbon-based amphiphilic nano-flow for oil displacement and preparation method thereof |
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