CN110055041A - A kind of Anti-pressure Foamed water shutoff agent - Google Patents

A kind of Anti-pressure Foamed water shutoff agent Download PDF

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CN110055041A
CN110055041A CN201910181939.5A CN201910181939A CN110055041A CN 110055041 A CN110055041 A CN 110055041A CN 201910181939 A CN201910181939 A CN 201910181939A CN 110055041 A CN110055041 A CN 110055041A
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water shutoff
parts
quality
shutoff agent
foamed water
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陈卓异
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Nanjing Siyu Environmental Protection Technology Co Ltd
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Nanjing Siyu Environmental Protection Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/426Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
    • C09K8/467Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes

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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

The invention discloses a kind of Anti-pressure Foamed water shutoff agents, belong to petrochemistry field.According to parts by weight, it successively weighs: 10~15 parts of solid particles, 5~10 foaming agents, 3~5 parts of polyacrylamides, 5~8 parts of nano particles, 8~15 parts of polyallylamines and 10~18 parts of additives;Polyallylamine and polyacrylamide are mixed in blender, and solid particle is added into blender, foaming agent, nano particle and additive are 30~40 DEG C in temperature, and revolving speed is under conditions of 200~300r/min, after being stirred 30~50min, Anti-pressure Foamed water shutoff agent is obtained.The resulting Anti-pressure Foamed water shutoff agent of the present invention has excellent water plugging effect, and still has preferable water shut-off at elevated pressures.

Description

A kind of Anti-pressure Foamed water shutoff agent
Technical field
The invention discloses a kind of Anti-pressure Foamed water shutoff agents, belong to petrochemistry field.
Background technique
Oil/gas well water outlet is FAQs in oilfield development process, especially the waterflooding extraction later period, since stratum is heterogeneous Property, cause the oil-field aqueous rate of climb fast, the too early water logging of oil reservoir, production decline.Main oilfield comes into High water cut at this stage Phase, widely applied volume increase, well stimulation efficiency are lower and lower under the conditions of original annotation water, and water yield increases considerably, economic benefit Difference.As water content is continuously increased, profile control and water plugging technology is also increasingly taken seriously, and the purpose of profile control and water plugging is water production control layer The flowing of middle water and the flow direction for changing water in water drive try hard to that the water yield in oil field is made to decline whithin a period of time or stablize, To keep oilfield stimulation or stable yields, oil field ultimate recovery is improved.
Water blockoff is carried out with polyacrylamide, is on oil field using most classical, most common technical method.Its conventional method is According to the adsorption property of the polyacrylamide of single high molecular weight.The polymer molecule of absorption forms one hardly on hole wall The layer penetrated effectively limits water flow (wetting phase) in this way, and the center of pore channel keeps oil gas flowing (nonwetting phase) It is unimpeded.The effect of this method is directly with the thickness of adsorption layer in relation to (compared with pore size).For high permeability oil reservoir or split Seam property oil reservoir, water stream channel is more order of magnitude greater than high molecular size, so that this method is nearly unavailable.It is this kind of to handle Situation has had developed several methods with crosslinking agent.Crosslinking agent is usually polyvalent metal ion, can be established in pore channel poly- Polymeric network.Even now processing can water blockoff, but also have and lose selective risk.In fact, due to pore channel center Occupied by polymer network, nonwetting phase --- the flowing of oil gas suffers restraints as water.
Water-plugging technology can be divided into water pack off and chemical water shutoff two major classes.Chemical water shutoff is injected to Thief zone water exit interval Chemical reagent, reagent reduce the water phase permeability of near wellbore zone, reduce oil well High water cut after solidifying or expand in formation pore The water yield of layer, achievees the purpose that water blockoff.The mode difference blocked is formed in oil reservoir according to blocking agent, chemical water shutoff is divided into selection again Property chemical water shutoff and non-selective chemical plugging.Water based foam system is selective water plugging one kind, using water as decentralized medium, gas Body is dispersed phase, and surfactant is foaming agent, and polymer is the dispersion of foam stabilizer, which has the not stifled oil of water blockoff Advantage.
Conventional water based foam system is divided into two-phase foam, three-phase froth and frothy gel water shutoff agent.Two-phase and three-phase bubble Foam main component is foaming agent and foam stabiliser, configures simple process, but foam stability is poor, is easy to happen gas channeling phenomenon. Frothy gel water shutoff agent can effectively improve foam stability, while system keeps the mechanical strength of Gelling Plugging Agent, but gassiness Rate is lower.Three of the above form requires on the ground to be uniformly mixed various reagents according to a certain percentage, after being sufficiently stirred, then Foam is made up on ground in advance of pressure fan or note nitrogen vehicle, reinjects stratum.Although it is uniform that this method configures foam, employ Equipment is more, at high cost, and frictional resistance is high, injection pressure is big;In addition, by first injecting foaming agent, using underground foaming, bubble efficiency Low, foaming effect is poor.
Therefore a kind of foam quality height is researched and developed, stability is good, and gel cross-linkage is synchronously completed with gas is produced, it can be achieved that efficient envelope Stifled Anti-pressure Foamed water shutoff agent has very vast market prospect.
Summary of the invention
The present invention solves the technical problem of: for traditional Anti-pressure Foamed water shutoff agent since bubble is unstable, and The not high problem for causing water plugging property bad of water blockoff cross-linked network intensity, provides a kind of Anti-pressure Foamed water shutoff agent.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of Anti-pressure Foamed water shutoff agent, is made of the raw material of following parts by weight: 10~15 parts of solid particles, 5~10 hairs Infusion, 3~5 parts of polyacrylamides, 5~8 parts of nano particles, 8~15 parts of polyallylamines and 10~18 parts of additives;
The additive the preparation method comprises the following steps:
Initiator is mixed with ethanol solution 1:220~1:350 in mass ratio, and 110~130 times of initiator quality of benzene is added Vinyl monomer after being stirred to react under nitrogen atmosphere, filters, dry, obtains polystyrene, by polystyrene and water in mass ratio 1: 10~1:15 mixing, and 3~5 times of polystyrene quality of ammonium hydroxide and 3~5 times of polystyrene quality of trimethyl silicane oxygen is added Alkane after being stirred to react, filters, dry, obtains pretreatment microballoon, by pretreatment microballoon and toluene di-isocyanate(TDI) 3:1 in mass ratio ~4:1 mixing, and the organic solvent of 55~60 times of microspheres quality of pretreatment is added, after being stirred to react under nitrogen atmosphere, filtering, Washing, it is dry, modified microballoon is obtained to get additive.
The solid particle is the flyash that mesh number is 150 mesh or mesh number is any one in the yellow mud of 200 mesh.
The foaming agent is alkylbenzene sulfonate, fatty alcohol polyoxyethylene ether sulfate, preferably dodecyl benzene sulfonic acid The mixture of sodium and sodium sulfate of polyethenoxy ether of fatty alcohol.
The nano particle is any one in nano zircite or nano-titanium dioxide.
The initiator is azodiisobutyronitrile, any one in benzoyl peroxide or the different phenylpropyl alcohol of peroxidating two.
The organic solvent is toluene, any one in dimethylbenzene or benzene.
The molecular weight of the polyacrylamide is 100000~1000000.
0.1~0.2 times of additive quality of porous material can be added in the additive, the porous material is by positive silicon Acetoacetic ester is mixed with ethanol solution 1:10~1:12 in mass ratio, and 1~2 times of ethyl orthosilicate quality of polyvinyl pyrrole is added Alkanone and 2~3 times of ethyl orthosilicate quality of ammonium hydroxide after being stirred to react, filter, dry, and calcining obtains porous nanometer titanium dioxide Porous nano silica is mixed with dehydrated alcohol 1:10~1:15 in mass ratio, and porous nano silica is added by silicon 1~2 times of quality of 3- aminopropyl triethoxysilane after being stirred to react, filters, dry, obtains porous material.
The beneficial effects of the present invention are:
(1) additive is added when preparing Anti-pressure Foamed water shutoff agent in the present invention, firstly, containing polymethyl siloxane in additive Microballoon can be filled in the hole of product cross-linked network after being added in product, so that the water plugging property of product is improved, and And since polymethsiloxane microspheres remained on surface has hydroxyl, hydrogen bond can be generated with the hydroxyl of the nano grain surface of addition and made With so that the cohesive force of product be made to improve, and then improving the water shut-off of product, secondly, the polymethyl siloxane in additive After modification, polymethyl siloxane surface grafting toluene di-isocyanate(TDI) makes dimethyl silicone polymer surface have cyano, Carbon dioxide gas is generated to which after product is contacted with water, cyano can be reacted with water, the carbon dioxide gas of generation is on the one hand It can be used as crosslinking agent, the polyallylamine being added in product promoted to be crosslinked, to form cross-linked network in interiors of products, make product Water plugging property further increases, and on the other hand, the carbon dioxide of generation can form three-phase froth with foaming agent and solid particle, and And the nano particle being added can be used as foam stabilizer, to make three-phase froth is uniform and stable to be adsorbed in cross-linked network, and then make The water plugging property of product further increases, furthermore, since in product use process, portions additive is when not in contact with water, still With the cyano compared with high reaction activity, cross-linked network abundant can be formed in interiors of products, and then make product under high pressure, Still there is preferable water plugging property;
(2) porous material can be added when preparing Anti-pressure Foamed water shutoff agent by the present invention, and the addition of porous material not only can crop Fixed-site after bubble generates further increases the water shut-off of product to play the role of foam stabilizing, moreover, porous material Nano silica has excellent hydrophobic performance after treatment in material, and then after being added in product, can densify While product, further increase the hydrophobic performance of product, simultaneously because nano-silica surface after treatment contains There is amino, therefore, complicated crosslinked network can be formed together with other substances in product in product use process, and then make to produce Foam in product improves water blockoff ability of the product under high-pressure situations by stable fixation.
Specific embodiment
Initiator and ethanol solution 1:220~1:350 in mass ratio are mixed in flask, and is added and causes into flask The styrene monomer that 110~130 times of agent quality, the rate into flask with 18~35mL/min are passed through nitrogen, it is bubbled 30~ It is 70~75 DEG C in temperature, under conditions of revolving speed is 300~350r/min, after being stirred to react 2~4h, filtering is obtained after 40min Polystyrene blank obtains polystyrene under conditions of being 70~75 DEG C in temperature by polystyrene blank after dry 1~2h, will Polystyrene and water 1:10~1:15 in mass ratio are mixed in three-necked flask, and polystyrene quality is added into three-necked flask 3~5 times of mass fraction be 18~22% ammonium hydroxide and 3~5 times of polystyrene quality of trimethicone, in temperature be 45 ~60 DEG C, under conditions of revolving speed is 300~320r/min, after being stirred to react 2~5h, filtering must pre-process microballoon blank, will be pre- Under conditions of processing microballoon blank is 60~70 DEG C in temperature after dry 1~2h, pretreatment microballoon is obtained, it will pretreatment microballoon and first Phenylene diisocyanate 3:1~4:1 in mass ratio is mixed in four-hole boiling flask, and pretreatment microspheres quality is added into four-hole boiling flask 55~60 times of organic solvent, then nitrogen is passed through with the rate of 30~35mL/min into four-hole boiling flask, in temperature be 60~65 DEG C, under conditions of revolving speed is 200~400r/min, after being stirred to react 4~6h, filtering obtains modified microballoon blank, by modified microballoon After blank washs 5~8 times with toluene, then with acetone washing 5~8 times, and by the modification microballoon blank after washing in temperature be 70 Under conditions of~85 DEG C after dry 1~2h, modified microballoon is obtained to get additive;According to parts by weight, it successively weighs: 10~15 Part solid particle, 5~10 foaming agents, 3~5 parts of polyacrylamides, 5~8 parts of nano particles, 8~15 parts of polyallylamines and 10~ 18 parts of additives;Polyallylamine and polyacrylamide are mixed in blender, and solid particle is added into blender, is foamed Agent, nano particle and additive are 30~40 DEG C in temperature, under conditions of revolving speed is 200~300r/min, it is stirred 30~ After 50min, Anti-pressure Foamed water shutoff agent is obtained.The solid particle is the flyash that mesh number is 150 mesh or the Huang that mesh number is 200 mesh Any one in mud.The foaming agent is alkylbenzene sulfonate, fatty alcohol polyoxyethylene ether sulfate, preferably detergent alkylate The mixture of sodium sulfonate and sodium sulfate of polyethenoxy ether of fatty alcohol.The nano particle is nano zircite or nano-titanium dioxide In any one.The initiator is azodiisobutyronitrile, any one in benzoyl peroxide or the different phenylpropyl alcohol of peroxidating two.Institute Stating organic solvent is toluene, any one in dimethylbenzene or benzene.The molecular weight of the polyacrylamide be 100000~ 1000000.0.1~0.2 times of additive quality of porous material can be added in the additive, the porous material is by positive silicon Acetoacetic ester is mixed with ethanol solution 1:10~1:12 in mass ratio, and 1~2 times of ethyl orthosilicate quality of polyvinyl pyrrole is added Alkanone and 2~3 times of ethyl orthosilicate quality of ammonium hydroxide after being stirred to react, filter, dry, and calcining obtains porous nanometer titanium dioxide Porous nano silica is mixed with dehydrated alcohol 1:10~1:15 in mass ratio, and porous nano silica is added by silicon 1~2 times of quality of 3- aminopropyl triethoxysilane after being stirred to react, filters, dry, obtains porous material.
Initiator and ethanol solution 1:350 in mass ratio are mixed in flask, and initiator quality is added into flask 130 times of styrene monomer, the rate into flask with 35mL/min are passed through nitrogen, after being bubbled 40min, in temperature be 75 DEG C, Under conditions of revolving speed is 350r/min, after being stirred to react 4h, filtering obtains polystyrene blank, by polystyrene blank in temperature Under conditions of being 75 DEG C after dry 2h, polystyrene is obtained, polystyrene and water 1:15 in mass ratio are mixed in three-necked flask, And the mass fraction that 5 times of polystyrene quality are added into three-necked flask is 22% ammonium hydroxide and 5 times of polystyrene quality of front three Radical siloxane is 60 DEG C in temperature, and under conditions of revolving speed is 320r/min, after being stirred to react 5h, filtering must pre-process microballoon base Material obtains pretreatment microballoon, by pretreatment microballoon and first under conditions of being 70 DEG C in temperature by pretreatment microballoon blank after dry 2h Phenylene diisocyanate 4:1 in mass ratio is mixed in four-hole boiling flask, and 60 times of microspheres quality of pretreatment is added into four-hole boiling flask Organic solvent, then nitrogen is passed through with the rate of 35mL/min into four-hole boiling flask, in temperature be 65 DEG C, revolving speed 400r/min Under conditions of, after being stirred to react 6h, filtering obtains modified microballoon blank, after modified microballoon blank is washed 8 times with toluene, then uses Acetone washing 8 times, and by the modification microballoon blank after washing be 85 DEG C in temperature under conditions of after dry 2h, obtain modified microballoon, Up to additive;According to parts by weight, it successively weighs: 15 parts of solid particles, 10 foaming agents, 5 parts of polyacrylamides, 8 parts of nanometers Particle, 15 parts of polyallylamines and 18 parts of additives;Polyallylamine and polyacrylamide are mixed in blender, and to blender Middle addition solid particle, foaming agent, nano particle and additive are 40 DEG C in temperature, under conditions of revolving speed is 300r/min, stir After mixing mixing 50min, Anti-pressure Foamed water shutoff agent is obtained.The solid particle is the flyash that mesh number is 150 mesh.The foaming agent The preferably mixture of neopelex and sodium sulfate of polyethenoxy ether of fatty alcohol.The nano particle is nano oxidized Zirconium.The initiator is azodiisobutyronitrile.The organic solvent is toluene.The molecular weight of the polyacrylamide is 100000.0.2 times of additive quality of porous material can be added in the additive, the porous material is by ethyl orthosilicate Mixed with ethanol solution 1:12 in mass ratio, and be added 2 times of ethyl orthosilicate quality polyvinylpyrrolidone and positive silicic acid second The ammonium hydroxide that 3 times of ester quality after being stirred to react, filters, dry, and calcining obtains porous nano silica, by porous nano titanium dioxide Silicon is mixed with dehydrated alcohol 1:15 in mass ratio, and 2 times of porous nano silica quality of 3- aminopropyl-triethoxy is added Silane after being stirred to react, filters, dry, obtains porous material.
Initiator and ethanol solution 1:350 in mass ratio are mixed in flask, and initiator quality is added into flask 130 times of styrene monomer, the rate into flask with 35mL/min are passed through nitrogen, after being bubbled 40min, in temperature be 75 DEG C, Under conditions of revolving speed is 350r/min, after being stirred to react 4h, filtering obtains polystyrene blank, by polystyrene blank in temperature Under conditions of being 75 DEG C after dry 2h, polystyrene is obtained, polystyrene and water 1:15 in mass ratio are mixed in three-necked flask, And the mass fraction that 5 times of polystyrene quality are added into three-necked flask is 22% ammonium hydroxide and 5 times of polystyrene quality of front three Radical siloxane is 60 DEG C in temperature, and under conditions of revolving speed is 320r/min, after being stirred to react 5h, filtering must pre-process microballoon base Material obtains pretreatment microballoon, by pretreatment microballoon and first under conditions of being 70 DEG C in temperature by pretreatment microballoon blank after dry 2h Phenylene diisocyanate 4:1 in mass ratio is mixed in four-hole boiling flask, and 60 times of microspheres quality of pretreatment is added into four-hole boiling flask Organic solvent, then nitrogen is passed through with the rate of 35mL/min into four-hole boiling flask, in temperature be 65 DEG C, revolving speed 400r/min Under conditions of, after being stirred to react 6h, filtering obtains modified microballoon blank, after modified microballoon blank is washed 8 times with toluene, then uses Acetone washing 8 times, and by the modification microballoon blank after washing be 85 DEG C in temperature under conditions of after dry 2h, obtain modified microballoon, Up to additive;According to parts by weight, it successively weighs: 15 parts of solid particles, 10 foaming agents, 5 parts of polyacrylamides, 8 parts of nanometers Particle and 18 parts of additives;Polyacrylamide is added in blender, and solid particle is added into blender, foaming agent is received Rice grain and additive are 40 DEG C in temperature, under conditions of revolving speed is 300r/min, after being stirred 50min, obtain Anti-pressure bubble Foam water shutoff agent.The solid particle is the flyash that mesh number is 150 mesh.The foaming agent be preferably neopelex and The mixture of sodium sulfate of polyethenoxy ether of fatty alcohol.The nano particle is nano zircite.The initiator is that azo two is different Butyronitrile.The organic solvent is toluene.The molecular weight of the polyacrylamide is 100000.Addition can be added in the additive The porous material that 0.2 times of agent quality, the porous material be ethyl orthosilicate is mixed with ethanol solution 1:12 in mass ratio, and 2 times of ethyl orthosilicate quality of polyvinylpyrrolidone and 3 times of ethyl orthosilicate quality of ammonium hydroxide, after being stirred to react, mistake is added Filter, dry, calcining obtains porous nano silica, porous nano silica is mixed with dehydrated alcohol 1:15 in mass ratio, And 2 times of porous nano silica quality of 3- aminopropyl triethoxysilane is added, and after being stirred to react, filter, it is dry, much Porous materials.
Initiator and ethanol solution 1:350 in mass ratio are mixed in flask, and initiator quality is added into flask 130 times of styrene monomer, the rate into flask with 35mL/min are passed through nitrogen, after being bubbled 40min, in temperature be 75 DEG C, Under conditions of revolving speed is 350r/min, after being stirred to react 4h, filtering obtains polystyrene blank, by polystyrene blank in temperature Under conditions of being 75 DEG C after dry 2h, polystyrene is obtained, polystyrene and water 1:15 in mass ratio are mixed in three-necked flask, And the mass fraction that 5 times of polystyrene quality are added into three-necked flask is 22% ammonium hydroxide and 5 times of polystyrene quality of front three Radical siloxane is 60 DEG C in temperature, and under conditions of revolving speed is 320r/min, after being stirred to react 5h, filtering must pre-process microballoon base Material obtains pretreatment microballoon, will pre-process microballoon first under conditions of being 70 DEG C in temperature by pretreatment microballoon blank after dry 2h After benzene washs 8 times, then with acetone washing 8 times, and by the pretreatment microballoon after washing be 85 DEG C in temperature under conditions of dry 2h Afterwards, additive is obtained;According to parts by weight, it successively weighs: 15 parts of solid particles, 10 foaming agents, 5 parts of polyacrylamides, 8 parts of nanometers Particle, 15 parts of polyallylamines and 18 parts of additives;Polyallylamine and polyacrylamide are mixed in blender, and to blender Middle addition solid particle, foaming agent, nano particle and additive are 40 DEG C in temperature, under conditions of revolving speed is 300r/min, stir After mixing mixing 50min, Anti-pressure Foamed water shutoff agent is obtained.The solid particle is the flyash that mesh number is 150 mesh.The foaming agent The preferably mixture of neopelex and sodium sulfate of polyethenoxy ether of fatty alcohol.The nano particle is nano oxidized Zirconium.The initiator is azodiisobutyronitrile.The organic solvent is toluene.The molecular weight of the polyacrylamide is 100000.0.2 times of additive quality of porous material can be added in the additive, the porous material is by ethyl orthosilicate Mixed with ethanol solution 1:12 in mass ratio, and be added 2 times of ethyl orthosilicate quality polyvinylpyrrolidone and positive silicic acid second The ammonium hydroxide that 3 times of ester quality after being stirred to react, filters, dry, and calcining obtains porous nano silica, by porous nano titanium dioxide Silicon is mixed with dehydrated alcohol 1:15 in mass ratio, and 2 times of porous nano silica quality of 3- aminopropyl-triethoxy is added Silane after being stirred to react, filters, dry, obtains porous material.
Comparative example: initiator and ethanol solution 1:350 in mass ratio are mixed in flask, and are added and are caused into flask The styrene monomer that 130 times of agent quality, the rate into flask with 35mL/min are passed through nitrogen, after being bubbled 40min, are in temperature 75 DEG C, revolving speed be 350r/min under conditions of, after being stirred to react 4h, filtering, obtain polystyrene blank, by polystyrene blank in Temperature after dry 2h, obtains polystyrene under conditions of being 75 DEG C, and polystyrene and water 1:15 in mass ratio are mixed in three mouthfuls of burnings In bottle, and 5 times of polystyrene quality of mass fraction is added as 22% ammonium hydroxide and 5 times of polystyrene quality into three-necked flask Trimethicone, in temperature be 60 DEG C, revolving speed be 320r/min under conditions of, after being stirred to react 5h, filtering, must pre-process Microballoon blank obtains pretreatment microballoon, will pre-process micro- under conditions of being 70 DEG C in temperature by pretreatment microballoon blank after dry 2h After ball washs 8 times with toluene, then with acetone washing 8 times, and by the pretreatment microballoon after washing under conditions of temperature is 85 DEG C After dry 2h, additive is obtained;According to parts by weight, it successively weighs: 15 parts of solid particles, 10 foaming agents, 5 parts of polyacrylamides, 8 Part nano particle and 18 parts of additives;Polyacrylamide is added in blender, and solid particle is added into blender, is foamed Agent, nano particle and additive are 40 DEG C in temperature, under conditions of revolving speed is 300r/min, after being stirred 50min, obtain anti- Die mould Foamed water shutoff agent.The solid particle is the flyash that mesh number is 150 mesh.The foaming agent is preferably detergent alkylate sulphur The mixture of sour sodium and sodium sulfate of polyethenoxy ether of fatty alcohol.The nano particle is nano zircite.The initiator is even Nitrogen bis-isobutyronitrile.The organic solvent is toluene.The molecular weight of the polyacrylamide is 100000.It can add in the additive Enter 0.2 times of additive quality of porous material, the porous material is by ethyl orthosilicate and ethanol solution 1:12 in mass ratio Mixing, and 2 times of ethyl orthosilicate quality of polyvinylpyrrolidone and 3 times of ethyl orthosilicate quality of ammonium hydroxide is added, stirring is anti- Ying Hou is filtered, dry, and calcining obtains porous nano silica, by porous nano silica and dehydrated alcohol in mass ratio 1: 15 mixing, and 2 times of porous nano silica quality of 3- aminopropyl triethoxysilane is added, it after being stirred to react, filters, does It is dry, obtain porous material.
1 to 3 gained Anti-pressure Foamed water shutoff agent of example and comparative example product are subjected to performance detection, specific detection method is such as Under:
1. leak rate: by 1 to 3 gained Anti-pressure Foamed water shutoff agent of example and comparative example product respectively with soil 1:50 in mass ratio Mixing, and the water of 10cm high is added, after standing 3h, test leak rate;
2. crushing resistance: by 1 to 3 gained Anti-pressure Foamed water shutoff agent of example and comparative example product respectively with soil 1:50 in mass ratio Mixing, and the water of 20cm high is added, after standing 3h, test leak rate;
Specific testing result is as shown in table 1:
Table 1: leak rate and crushing resistance performance detection table
Detection content Example 1 Example 2 Example 3 Example 4
Leak rate/% when the high 10cm of water 4.0 5.0 5.8 10.5
Leak rate/% when the high 20cm of water 4.8 5.5 6.8 18.6
By 1 testing result of table it is found that the resulting Anti-pressure Foamed water shutoff agent of the present invention has excellent water plugging effect, and higher Still there is preferable water shut-off under pressure.

Claims (9)

1. a kind of Anti-pressure Foamed water shutoff agent, which is characterized in that be made of the raw material of following parts by weight: 10~15 parts of solids Particle, 5~10 foaming agents, 3~5 parts of polyacrylamides, 5~8 parts of nano particles, 8~15 parts of polyallylamines and 10~18 parts add Add agent;
The additive the preparation method comprises the following steps:
Initiator is mixed with ethanol solution 1:220~1:350 in mass ratio, and 110~130 times of initiator quality of benzene is added Vinyl monomer after being stirred to react under nitrogen atmosphere, filters, dry, obtains polystyrene, by polystyrene and water in mass ratio 1: 10~1:15 mixing, and 3~5 times of polystyrene quality of ammonium hydroxide and 3~5 times of polystyrene quality of trimethyl silicane oxygen is added Alkane after being stirred to react, filters, dry, obtains pretreatment microballoon, by pretreatment microballoon and toluene di-isocyanate(TDI) 3:1 in mass ratio ~4:1 mixing, and the organic solvent of 55~60 times of microspheres quality of pretreatment is added, after being stirred to react under nitrogen atmosphere, filtering, Washing, it is dry, modified microballoon is obtained to get additive.
2. a kind of Anti-pressure Foamed water shutoff agent according to claim 1, it is characterised in that: the solid particle is that mesh number is The flyash or mesh number of 150 mesh are any one in the yellow mud of 200 mesh.
3. a kind of Anti-pressure Foamed water shutoff agent according to claim 1, it is characterised in that: the foaming agent is benzene sulfonamide Hydrochlorate, fatty alcohol polyoxyethylene ether sulfate, preferably neopelex and sodium sulfate of polyethenoxy ether of fatty alcohol Mixture.
4. a kind of Anti-pressure Foamed water shutoff agent according to claim 1, it is characterised in that: the nano particle is nano oxygen Change any one in zirconium or nano-titanium dioxide.
5. a kind of Anti-pressure Foamed water shutoff agent according to claim 1, it is characterised in that: the initiator is that azo two is different Any one in butyronitrile, benzoyl peroxide or the different phenylpropyl alcohol of peroxidating two.
6. a kind of Anti-pressure Foamed water shutoff agent according to claim 1, it is characterised in that: the organic solvent is toluene, Any one in dimethylbenzene or benzene.
7. a kind of Anti-pressure Foamed water shutoff agent according to claim 1, it is characterised in that: the molecule of the polyacrylamide Amount is 100000~1000000.
8. a kind of Anti-pressure Foamed water shutoff agent according to claim 1, it is characterised in that: the Anti-pressure Foamed water shutoff agent Application method be Anti-pressure Foamed water shutoff agent is mixed with water 1:4~1:10 in mass ratio, obtain Anti-pressure Foamed water shutoff agent divide Anti-pressure foam water plugging agent dispersing liquid is sprayed at required position, the use of Anti-pressure Foamed water shutoff agent can be completed by dispersion liquid.
9. a kind of Anti-pressure Foamed water shutoff agent according to claim 1, it is characterised in that: can be added and add in the additive Add 0.1~0.2 times of agent quality of porous material, the porous material is by ethyl orthosilicate and ethanol solution 1:10 in mass ratio ~1:12 mixing, and be added 1~2 times of ethyl orthosilicate quality polyvinylpyrrolidone and 2~3 times of ethyl orthosilicate quality Ammonium hydroxide after being stirred to react, filters, dry, and calcining obtains porous nano silica, by porous nano silica and anhydrous second Alcohol 1:10~1:15 in mass ratio mixing, and 1~2 times of porous nano silica quality of 3- aminopropyl-triethoxy silicon is added Alkane after being stirred to react, filters, dry, obtains porous material.
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