CN103254888A - Clean-water carrying fracturing supporting agent and preparation method - Google Patents
Clean-water carrying fracturing supporting agent and preparation method Download PDFInfo
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- CN103254888A CN103254888A CN2013101897804A CN201310189780A CN103254888A CN 103254888 A CN103254888 A CN 103254888A CN 2013101897804 A CN2013101897804 A CN 2013101897804A CN 201310189780 A CN201310189780 A CN 201310189780A CN 103254888 A CN103254888 A CN 103254888A
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Abstract
The invention provides a clean-water carrying fracturing supporting agent. The supporting agent is prepared by coating and modifying macromolecule polymer particles. A monomer solution, a crosslink agent, an initiator and rock ore material powder are synthesized in an aqueous solution with dissolved dispersing agent to obtain the macromolecule polymer particles. The invention also provides a method for preparing the supporting agent. The breaking rate of the clean-water carrying fracturing supporting agent is less than 2 percent under the pressure of 52MPa, the volume density is 0.61 to 0.68 g/cm<3>, the apparent density is 1.02 to 1.25 g/cm<3>, the density is close to that of the water, and water or salted water can be used as a sand carrying liquid in the application process of the supporting agent, so that the fracturing construction cost can be greatly reduced, the energy conservation and emission reduction can be achieved, the macromolecule assistant such as guar gum can be avoided, and the environmental pollution can be reduced.
Description
Technical field
The invention provides a kind of clear water and carry fracturing propping agents, the preparation method of above-mentioned propping agent also is provided simultaneously, belong to oil, gasser pressure break exploitation field.
Background technology
In order to develop deep-seated oil, gas well, improve output, fracturing technology is widely used.In order to ensure effectively strutting of underground deep layer pressure-break, the proper supporting agent is necessary, and it can increase the flow conductivity on stratum, improves the output of oil or gas, is the important factor that fracturing technology is used quality.
Desirable well fracturing propping agent requires to have high carrying capacity and high sand ratio, therefore needs alap density and high as far as possible intensity.Existing propping agent is mainly high-density, middle density and three kinds of propping agents of low density, and in order to satisfy the requirement of intensity, the density of existing propping agent is bigger, and its suspension is poor, and precipitation is not easy to be carried in the well easily, and cost of winning is big.
Though present stage be applied to fracturing propping agents in the pressure break oil recovery technique can both be aspect intensity to a certain degree satisfy pressure break requirement, the characteristics that ubiquity density is higher.In order to make these propping agents effectively along with fracturing liquid arrives the crack, this just need use high viscosity or highdensity fracturing liquid.And traditional fracturing liquid main component is guanidine glue, and guanidine glue is a kind of organic polymer material.Its a large amount of uses cause very big injury to the stratum, cause the perviousness on stratum itself to reduce, and cause groundwater pollution, and reduce the crude oil taste.In view of there is unavoidable drawback in traditional fracturing technique, just need look for another way to improve the usefulness of pressure break, since can't find cheap high density fracturing liquid, can set about from reducing propping agent density.Part fracturing propping agents density and water approach even are lower than the density of water, they in use only need just can satisfy requirement---the riverfrac treatment technology that pressure break is recovered the oil as sand-carrying agent with tap water or salt solution, and the propping agent that riverfrac treatment uses just is the riverfrac treatment propping agent.Thus, research and develop a kind of high strength, low-density clear water carries propping agent, for improving crude oil in China output and sampling most important; In addition, it is applied to can not bring secondary environmental pollution in the pressure break oil recovery technique, will has tangible environment demonstration benefit, and meet China's strategy of sustainable development requirement.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of intensity height, density fracturing propping agents that can be carried by water close to water and preparation method thereof are provided.
Realize that the technical scheme that above-mentioned purpose of the present invention adopts is:
A kind of clear water carries fracturing propping agents, this propping agent is made behind the overlay film modified technique by the high molecular polymerization composition granule, described high molecular polymerization composition granule is polymerized in being dissolved with the aqueous solution of dispersion agent by monomer solution, linking agent, initiator and rock forming mineral material powder, and wherein the mass ratio between distilled water, dispersion agent, nano mineral materials powder, monomer solution, linking agent and the initiator is 100:0.5～1.5:0.5～15:15～30:1.0～3.0:0.05～0.25.
Described monomer solution is methyl methacrylate, Jia Jibingxisuanyizhi or butyl methacrylate; Described nano mineral materials powder is one or more the mixture in nano kaoline, nano-attapulgite stone, nano montmorillonite and the nano silicon; Described linking agent is Vinylstyrene; Initiator is benzoyl peroxide; Dispersion agent is gelatin or polyvinyl alcohol.
This clear water carries that percentage of damage is less than 2.0% under the fracturing propping agents 52MPa pressure, and its volume density is 0.61～0.68g/cm
3, volume density is 1.02～1.25g/cm
3
The present invention also provides above-mentioned clear water to carry the preparation method of fracturing propping agents simultaneously, may further comprise the steps: (1), under 40～60 ℃ condition, add dispersion agent in the container that distilled water is housed and fully stir and make its dissolving, more than in container, adding rock forming mineral material powder then and stirring 10min with the speed that is not less than 300r/min it is fully disperseed, again with linking agent, initiator and monomer solution add in the container, then the temperature in the container is warming up to 55～65 ℃ and allow the solution in the container under this temperature, react 0.5～1h, then the temperature in the container is warming up to 68～78 ℃ and allow the solution in the container under this temperature, react 0.5～2h, then the temperature in the container is warming up to 80～95 ℃ and allow the solution in the container under this temperature, react 0.5～2h, so far precipitation is finished and is generated in reaction, with drying after the washing of precipitate and crossing 10～60 mesh sieves, namely make the high molecular polymerization composition granule;
(2), will go up the high molecular polymerization composition granule for preparing in the step joins and is stirred and heated to 100～150 ℃ in the resin sand mill, add coupling agent, resol, Resins, epoxy and toughner in the whipping process, add solidifying agent and dispersion agent then successively, 10～60 mesh sieves namely make clear water and carry fracturing propping agents excessively at last.
Described monomer solution is methyl methacrylate, Jia Jibingxisuanyizhi or butyl methacrylate; Described nano mineral materials powder is one or more the mixture in nano kaoline, nano-attapulgite stone, nano montmorillonite and the nano silicon; Described linking agent is Vinylstyrene; Initiator is benzoyl peroxide; Dispersion agent is gelatin or polyvinyl alcohol.
In the step (1) in the process of temperature reaction, with the speed of 300r/min to the solution stirring in the container.
Resol described in the step (2) is novolac resin, and described coupling agent is silane coupling agent, as amine propyl-triethoxysilicane, epoxypropyl triethoxyl silane, anilinomethyl triethoxysilane etc.; Described Resins, epoxy is E44, E51 series of loops epoxy resins, described toughner is adjacent benzene type dicarboxylic acid esters, as dimethyl phthalate, dibutyl phthalate, dimixo-octyl phthalate, described solidifying agent is Paraformaldehyde 96 or vulkacit H, and described dispersion agent is calcium stearate or Zinic stearas.
Described container is there-necked flask.
Clear water provided by the present invention carries fracturing propping agents, and percentage of damage is less than 2.0% under 52MPa pressure, and its volume density is 0.61～0.68g/cm
3, volume density is 1.02～1.25g/cm
3, density is close to water, in use can water or salt solution serve as sand-carrying agent, thereby can significantly reduce the pressing crack construction cost, and energy-saving and emission-reduction avoid using polymer auxiliary agents such as guar gum, reduce the pollution to environment.In addition, the present invention improves polymer strength and durothermic purpose by adding a certain amount of mineral material in the building-up process of high molecular polymerization composition granule, can reaching in preparation process, thereby is applicable to that deep well fracturing uses.Simultaneously, clear water of the present invention carries the fracturing propping agents preparation method and simply can carry out suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment the present invention is done detailed specific description; but following examples only are used for explanation technical scheme of the present invention but not limiting the scope of the invention; the modification that those of ordinary skill in the art carries out according to following examples or be equal to replacement all drops within protection scope of the present invention.
Employed container is there-necked flask in following examples, in the mouth of there-necked flask thermometer, agitator and condenser is housed respectively; Heating process in preparation process all adopts heating in water bath.
Embodiment 1
The clear water that provides in the present embodiment carries fracturing propping agents and adopts following method preparation: add 600ml distilled water in there-necked flask, the 3g gelatin is added in the there-necked flask, be warmed up to 55 ℃ and mechanical stirring and make its dissolving, add 3g8000 order kaolin then, speed mechanical dispersed with stirring 30min with 300r/min fully disperses it.
Other takes by weighing 90g methyl methacrylate, 6g Vinylstyrene, 0.70g benzoyl peroxide, add in the there-necked flask behind the stirring and evenly mixing, the rotating speed of regulating agitator in the there-necked flask is 300r/min, then the temperature in the there-necked flask is warming up to 60 ℃, reaction 1h, then temperature is warming up to 70 ℃, reaction 2h, temperature is warming up to 80 ℃ then, reaction 1h, so far precipitation is finished and is generated in reaction, will precipitate suction filtration, the oven dry of washing back and cross 10～60 mesh sieves, namely makes the polymethylmethacrylate ball;
The polymethylmethacrylate ball that prepared in the last step is taken by weighing 500g to join and is stirred and heated to 150 ℃ in the resin sand mill, drip 0.5ml coupling agent KH-550 successively, add 20g resol, 10gE-44 Resins, epoxy and 2.5ml dimethyl phthalate, continue to stir and to add 2.4g vulkacit H solidifying agent behind the 60s and stir and when the sign of dispersion is arranged, add 1.5g calcium stearate dispersion agent and disperse, cross 10～60 mesh sieves and namely obtain clear water and carry fracturing propping agents.
Embodiment 2
The clear water that provides in the present embodiment carries fracturing propping agents and adopts following method preparation: add 600ml distilled water in there-necked flask, the 6g gelatin is added in the there-necked flask, be warmed up to 55 ℃ and mechanical stirring and make its dissolving, add 6g8000 order kaolin then, speed mechanical dispersed with stirring 25min with 310r/min,, it is fully disperseed.
Other takes by weighing 180g Jia Jibingxisuanyizhi, 7.5g Vinylstyrene, 0.30g benzoyl peroxide, add in the there-necked flask behind the stirring and evenly mixing, the rotating speed of regulating agitator in the there-necked flask is 300r/min, then the temperature in the there-necked flask is warming up to 60 ℃, reaction 1h, then temperature is warming up to 70 ℃, reaction 2h, temperature is warming up to 80 ℃ then, reaction 1h, so far precipitation is finished and is generated in reaction, will precipitate suction filtration, the oven dry of washing back and cross 10～60 mesh sieves, namely makes the polyethyl methacrylate ball;
The polyethyl methacrylate ball that prepared in the last step is taken by weighing 500g to join and is stirred and heated to 150 ℃ in the resin sand mill, drip 0.5ml coupling agent KH-550 successively, add 20g resol, 10gE-51 Resins, epoxy and 5ml dibutyl phthalate, continue to stir and to add 2.4g Paraformaldehyde 96 amine hardener behind the 60s and stir and when the sign of dispersion is arranged, add 1.5g calcium stearate dispersion agent and disperse, cross 10～60 mesh sieves and namely obtain clear water and carry fracturing propping agents.
Embodiment 3
The clear water that provides in the present embodiment carries fracturing propping agents and adopts following method preparation: add 600ml distilled water in there-necked flask, the 9g polyvinyl alcohol is added in the there-necked flask, be warmed up to 55 ℃ and mechanical stirring and make its dissolving, add 9g8000 order Attapulgite then, speed mechanical dispersed with stirring 23min with 320r/min fully disperses it.
Other takes by weighing 120g butyl methacrylate, 10g Vinylstyrene, 0.80g benzoyl peroxide, add in the there-necked flask behind the stirring and evenly mixing, the rotating speed of regulating agitator in the there-necked flask is 300r/min, then the temperature in the there-necked flask is warming up to 60 ℃, reaction 1h, then temperature is warming up to 70 ℃, reaction 2h, temperature is warming up to 80 ℃ then, reaction 1h, so far precipitation is finished and is generated in reaction, will precipitate suction filtration, the oven dry of washing back and cross 10～60 mesh sieves, namely makes the poly-n-butyl methacrylate ball;
The poly-n-butyl methacrylate ball that prepared in the last step is taken by weighing 500g to join and is stirred and heated to 150 ℃ in the resin sand mill, drip 0.5ml coupling agent KH-560 successively, add 20g resol, 10g Resins, epoxy and 2.5ml dimixo-octyl phthalate, continue to stir and to add 2.4g vulkacit H solidifying agent behind the 60s and stir and when the sign of dispersion is arranged, add 1.5g Zinic stearas dispersion agent and disperse, cross 10～60 mesh sieves and namely obtain clear water and carry fracturing propping agents.
Embodiment 4
The clear water that provides in the present embodiment carries fracturing propping agents and adopts following method preparation: add 600ml distilled water in there-necked flask, the 6g gelatin is added in the there-necked flask, be warmed up to 55 ℃ and mechanical stirring and make its dissolving, add 3g8000 order kaolin then, speed mechanical dispersed with stirring 20min with 350r/min fully disperses it.
Other takes by weighing 100g methyl methacrylate, 7.5g Vinylstyrene, 0.70g benzoyl peroxide, add in the there-necked flask behind the stirring and evenly mixing, the rotating speed of regulating agitator in the there-necked flask is 300r/min, then the temperature in the there-necked flask is warming up to 60 ℃, reaction 1h, then temperature is warming up to 70 ℃, reaction 2h, temperature is warming up to 80 ℃ then, reaction 1h, so far precipitation is finished and is generated in reaction, will precipitate suction filtration, the oven dry of washing back and cross 10～60 mesh sieves, namely makes the polymethylmethacrylate ball;
The polymethylmethacrylate ball that prepared in the last step is taken by weighing 500g to join and is stirred and heated to 150 ℃ in the resin sand mill, drip 0.5ml coupling agent KH-550 successively, add 20g resol, 10g Resins, epoxy and 2.5ml dimethyl phthalate, continue to stir and to add 2.4g vulkacit H solidifying agent behind the 60s and stir and when the sign of dispersion is arranged, add 1.5g calcium stearate dispersion agent and disperse, cross 10～60 mesh sieves and namely obtain clear water and carry fracturing propping agents.
Embodiment 5
The clear water that provides in the present embodiment carries fracturing propping agents and adopts following method preparation: add 600ml distilled water in there-necked flask, the 6g gelatin is added in the there-necked flask, be warmed up to 55 ℃ and mechanical stirring and make its dissolving, add the 5g nano silicon then, speed mechanical dispersed with stirring 20min with 350r/min,, it is fully disperseed.
Other takes by weighing 100g methyl methacrylate, 15g Vinylstyrene, 1.2g benzoyl peroxide, add in the there-necked flask behind the stirring and evenly mixing, the rotating speed of regulating agitator in the there-necked flask is 300r/min, then the temperature in the there-necked flask is warming up to 60 ℃, reaction 1h, then temperature is warming up to 70 ℃, reaction 2h, temperature is warming up to 80 ℃ then, reaction 1h, so far precipitation is finished and is generated in reaction, will precipitate suction filtration, the oven dry of washing back and cross 10～60 mesh sieves, namely makes the polymethylmethacrylate ball;
The polymethylmethacrylate ball that prepared in the last step is taken by weighing 500g to join and is stirred and heated to 150 ℃ in the resin sand mill, drip 1ml coupling agent KH-550 successively, add 15g resol, 15g Resins, epoxy and 2.5ml dimethyl phthalate, continue to stir and to add 3.0g vulkacit H solidifying agent behind the 60s and stir and when the sign of dispersion is arranged, add 1.5g calcium stearate dispersion agent and disperse, cross 10～60 mesh sieves and namely obtain clear water and carry fracturing propping agents.
Embodiment 6
The clear water that provides in the present embodiment carries fracturing propping agents and adopts following method preparation: add 600ml distilled water in there-necked flask, the 3g gelatin is added in the there-necked flask, be warmed up to 55 ℃ and mechanical stirring and make its dissolving, add the polynite of 1g8000 order then, speed mechanical dispersed with stirring 18min with 340r/min fully disperses it.
Other takes by weighing 100g methyl methacrylate, 7.5g Vinylstyrene, 1.5g benzoyl peroxide, add in the there-necked flask behind the stirring and evenly mixing, the rotating speed of regulating agitator in the there-necked flask is 315r/min, then the temperature in the there-necked flask is warming up to 60 ℃, reaction 1h, then temperature is warming up to 70 ℃, reaction 2h, temperature is warming up to 80 ℃ then, reaction 1h, so far precipitation is finished and is generated in reaction, will precipitate suction filtration, the oven dry of washing back and cross 10～60 mesh sieves, namely makes the polymethylmethacrylate ball;
The polymethylmethacrylate ball that prepared in the last step is taken by weighing 500g to join and is stirred and heated to 150 ℃ in the resin sand mill, drip 1ml coupling agent anilinomethyl triethoxysilane successively, add 15g resol, 15g Resins, epoxy and 2.5ml dimethyl phthalate, continue to stir and to add 2.4g vulkacit H solidifying agent behind the 60s and stir and when the sign of dispersion is arranged, add 1.5g calcium stearate dispersion agent and disperse, cross 10～60 mesh sieves and namely obtain clear water and carry fracturing propping agents.
The prepared product of above embodiment that provides among the present invention is carried out performance index measures, to the test of its volume density, volume density, degree of sphericity, percentage of damage and flow conductivity all according to the oil and gas industry standard SY/T 5108-2006 of the People's Republic of China (PRC) " fracturing propping agents and performance index and test recommend method ".The results are shown in following table:
Claims (8)
1. a clear water carries fracturing propping agents, it is characterized in that: this propping agent is made behind the overlay film modified technique by the high molecular polymerization composition granule, described high molecular polymerization composition granule is polymerized in being dissolved with the aqueous solution of dispersion agent by monomer solution, linking agent, initiator and rock forming mineral material powder, and wherein the mass ratio between distilled water, dispersion agent, nano mineral materials powder, monomer solution, linking agent and the initiator is 100:0.5～1.5:0.5～15:15～30:1.0～3.0:0.05～0.25.
2. clear water according to claim 1 carries fracturing propping agents, it is characterized in that: described monomer solution is methyl methacrylate, Jia Jibingxisuanyizhi or butyl methacrylate; Described nano mineral materials powder is one or more the mixture in nano kaoline, nano-attapulgite stone, nano montmorillonite and the nano silicon; Described linking agent is Vinylstyrene; Initiator is benzoyl peroxide; Dispersion agent is gelatin or polyvinyl alcohol.
3. clear water according to claim 1 carries fracturing propping agents, it is characterized in that: this clear water carries that percentage of damage is less than 2.0% under the fracturing propping agents 52MPa pressure, and its volume density is 0.61～0.68g/cm
3, volume density is 1.02～1.25g/cm
3
4. clear water as claimed in claim 1 carries the preparation method of fracturing propping agents, it is characterized in that may further comprise the steps: (1), under 40～60 ℃ condition, add dispersion agent in the container that distilled water is housed and fully stir and make its dissolving, more than in container, adding rock forming mineral material powder then and stirring 10min with the speed that is not less than 300r/min it is fully disperseed, again with linking agent, initiator and monomer solution add in the container, then the temperature in the container is warming up to 55～65 ℃ and allow the solution in the container under this temperature, react 0.5～1h, then the temperature in the container is warming up to 68～78 ℃ and allow the solution in the container under this temperature, react 0.5～2h, then the temperature in the container is warming up to 80～95 ℃ and allow the solution in the container under this temperature, react 0.5～2h, so far precipitation is finished and is generated in reaction, with drying after the washing of precipitate and crossing 10～60 mesh sieves, namely make the high molecular polymerization composition granule;
(2), will go up the high molecular polymerization composition granule for preparing in the step joins and is stirred and heated to 100～150 ℃ in the resin sand mill, add coupling agent, resol, Resins, epoxy and toughner in the whipping process, add solidifying agent and dispersion agent then successively, 10～60 mesh sieves namely make clear water and carry fracturing propping agents excessively at last.
5. clear water according to claim 4 carries the preparation method of fracturing propping agents, it is characterized in that: described monomer solution is methyl methacrylate, Jia Jibingxisuanyizhi or butyl methacrylate; Described nano mineral materials powder is one or more the mixture in nano kaoline, nano-attapulgite stone, nano montmorillonite and the nano silicon; Described linking agent is Vinylstyrene; Initiator is benzoyl peroxide; Dispersion agent is gelatin or polyvinyl alcohol.
6. clear water according to claim 4 carries the preparation method of fracturing propping agents, it is characterized in that: in the step (1) in the process of temperature reaction, with the speed of 300r/min to the solution stirring in the container.
7. clear water according to claim 4 carries the preparation method of fracturing propping agents, it is characterized in that: the resol described in the step (2) is novolac resin, described coupling agent is silane coupling agent, as amine propyl-triethoxysilicane, epoxypropyl triethoxyl silane, anilinomethyl triethoxysilane etc.; Described Resins, epoxy is E44, E51 series of loops epoxy resins, described toughner is adjacent benzene type dicarboxylic acid esters, as dimethyl phthalate, dibutyl phthalate, dimixo-octyl phthalate, described solidifying agent is Paraformaldehyde 96 or vulkacit H, and described dispersion agent is calcium stearate or Zinic stearas.
8. clear water according to claim 4 carries the preparation method of fracturing propping agents, it is characterized in that: described container is there-necked flask.
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