CN103881693A - Inverse emulsion drag reduction agent for fracturing shale gas by using quick water and preparation method thereof - Google Patents
Inverse emulsion drag reduction agent for fracturing shale gas by using quick water and preparation method thereof Download PDFInfo
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- C09K8/62—Compositions for forming crevices or fractures
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- C09K8/84—Compositions based on water or polar solvents
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Abstract
The invention discloses an inverse emulsion drag reduction agent for fracturing a shale gas by using quick water and a preparation method thereof, and relates to the technical field of petroleum engineering. The inverse emulsion drag reduction agent is a macromolecular water soluble polymer which is prepared from acrylamide, sodium acrylate and dodecyl methacrylate copolymerized in an inverse emulsion, and azo diisobutyl hydrochloride and sodium hydrogen sulfite as complex initiation systems. A long-chain hydrophobic monomer is introduced into the drag reduction agent, so that the shear resistance of the drag reduction agent in a high displacement pump injection process is improved, meanwhile, the drag reduction agent is prepared from the inverse emulsion in a polymerization manner, the product is a liquor and instant, the liquor demands of a continuous mixed construction technology for fracturing the shale gas are met, the dosage for field use is 0.06-0.8% of mass of clean water, and the drag reduction rate can be up to 73%.
Description
Technical field
The present invention relates to petroleum engineering technical field, be specifically related to a kind of shale gas slippery water pressure break reversed-phase emulsion friction reducer and preparation method thereof.
Background technology
As the shale gas of unconventional petroleum resources, its reservoir reconstruction technique and conventional gas and oil resource have a great difference.In order to link up to greatest extent or to open the Fracture System in reservoir, shale gas reservoir volume increase transformation adopts large liquid measure, large discharge capacity fracturing technique.For shale gas volume increase transformation demand, reduce the energy waste that fracturing liquid fluid causes because of high infusion pressure influence generation turbulent flow in pumping procedure, improve infusion discharge capacity and the liquid injection rate under identical infusion discharge capacity particularly important.
Publication number is CN1487985A, the Chinese patent literature that open day is on April 7th, 2004 discloses a kind of surfactant-based friction reducer, relates to zwitterionics and ether sulfate or ether carboxylate tensio-active agent and is combined in the application as flow improver in aqueous based systems.But this class flow improver need to reach the micelle-forming concentration of tensio-active agent could be used above, and working concentration is high, is not suitable for shale gas low cost development demand.
Publication number is CN103333672A, within open day, be that the Chinese patent literature on October 2nd, 2013 discloses the application that made by acrylamide and propenyl tri alkyl ammomium chloride or alkyl acrylamide base tri alkyl ammomium chloride or the polymerization of dialkyl diallyl aqueous ammonium chloride solution and the sodium salt friction reducer of shale gas reservoir, friction reducer prepared by the method is pulvis, and pulvis is not suitable in the extensive shale gas pressing crack construction that adopts continuous mixture construction technology.
Publication number is CN102977877A, the Chinese patent literature that open day is on March 20th, 2013 discloses shale gas pressure break flow improver being made by acrylamide, sodium acrylate and 2-acrylamide-2 methyl propane sulfonic acid sodium and preparation method thereof, the method needs first to prepare stablizer by aqueous solution polymerization, prepare flow improver by dispersion polymerization again, in preparation process, need logical nitrogen deoxygenation and preparation time long (total reaction time is more than 20h) simultaneously, complex manufacturing, be unfavorable for suitability for industrialized production, this friction reducer solid content is low simultaneously, and dosage is larger in use.
Summary of the invention
The present invention is intended to for the existing defect of above-mentioned prior art and deficiency, a kind of shale gas slippery water pressure break reversed-phase emulsion friction reducer is provided, adopt the present invention, structural stability and resistance-reducing performance under high infusion discharge capacity are improved, this friction reducer is product emulsion simultaneously, be easy to dosing, be applicable to the extensive shale gas pressing crack construction of continuous mixture construction technology.
Simultaneously, the present invention also provides the preparation method of shale gas slippery water pressure break reversed-phase emulsion friction reducer, the method adopts super dense inverse emulsion polymerization, water accounts for system 70%～80%, solid content is high, and gained friction reducer just can reach good resistance reducing effect under low dosage condition, and in the time producing, one-step polymerization obtains product simultaneously, without logical nitrogen deoxygenation, production time section, greatly simplify production technique.
The present invention is by adopting following technical proposals to realize:
A kind of shale gas slippery water pressure break reversed-phase emulsion friction reducer, is characterized in that: by percentage to the quality, the proportioning of each component is as follows:
High molecular weight water soluble polymer 30%～37.5%;
Non-polar solvent 20%～25%;
Oil-soluble emulsifier 2.5%～2.75%;
Solubility promoter 0.2%～0.3%;
All the other are water.
Described high molecular weight water soluble polymer is the multipolymer of acrylamide, sodium acrylate and three kinds of monomers of methacrylic dodecyl gallate, in high molecular weight water soluble polymer, the mass percent of described acrylamide is 65%～70%, and the mass percent of described sodium acrylate is 29%～33%; The mass percent of described water beetle base dodecyl acrylate is 1%～2%; Initiator in high molecular weight water soluble polymer is azo diisobutyl amidine hydrochloride and sodium bisulfite composite initiator, wherein, azo diisobutyl amidine hydrochloride accounts for 0.1%～0.3% of described three kinds of monomer total masses, and sodium bisulfite accounts for 0.1%～0.4% of described three kinds of monomer total masses.
Described non-polar solvent is 15# white oil.
Described oil-soluble emulsifier is sorbitan mono-oleic acid ester and SPAN85 compound emulsifying agent, and wherein the mass ratio of sorbitan mono-oleic acid ester and SPAN85 is 8～9:1～2.
Described solubility promoter is sodium bicarbonate.
A preparation method for reversed-phase emulsion friction reducer for shale gas slippery water pressure break, is characterized in that step is as follows:
1) prepare acrylamide, sodium acrylate and three kinds of monomers of methacrylic dodecyl gallate, first by soluble in water the sodium acrylate that accounts for three kinds of monomer total masses 23%～29%, add again account for three kinds of monomer total masses 70%～75% acrylamide, account for three kinds of monomer total masses, 0.1%～0.3% initiator azo diisobutyl amidine hydrochloride and account for the solubility promoter sodium bicarbonate of prepared friction reducer total mass 0.2%～0.3%, stirring and dissolving obtains aqueous phase solution;
2) in the 15# white oil that accounts for prepared friction reducer total mass 20%～25%, add the emulsifier sorbitol acid anhydride monoleate and the SPAN85 that account for prepared friction reducer total mass 2.5%～2.75%, wherein: the mass ratio of sorbitan mono-oleic acid ester and SPAN85 is 8～9:1～2; In described 15# white oil, add again the methacrylic dodecyl gallate that accounts for three kinds of monomer total masses 1%～2%, stir and obtain oil phase;
3) by above-mentioned 1) aqueous phase solution that obtains in step is added dropwise to above-mentioned 2 under continuously stirring state) in the oil phase that obtains of step, dropwise rear emulsification 30min and obtain reversed-phase emulsion;
4) under 15～25 ℃, continuously stirring state to above-mentioned 3) drip the aqueous solution of sodium bisulfite that accounts for three kinds of monomer total masses 0.1%～0.4% in the reversed-phase emulsion that obtains of step, after dropwising, stop stirring when also standing and reacting to system temperature rises to 35 ℃ and start and stir, be continuously stirring to and when temperature no longer changes, stop stirring and leave standstill insulation after 4 hours, naturally be cooled to blowing after envrionment temperature, obtain reversed-phase emulsion friction reducer.
In described step 1), acrylamide selects acrylamide performance prepared by microbial method more.
Compared with prior art, the beneficial effect that the present invention reaches is as follows:
1, select " high molecular weight water soluble polymer 30%～37.5%; Non-polar solvent 20%～25%; Oil-soluble emulsifier 2.5%～2.75%; Solubility promoter 0.2%～0.3%; All the other are water " friction reducer of specific like this proportioning, improve structural stability and resistance-reducing performance under high infusion discharge capacity, this friction reducer is product emulsion simultaneously, is easy to dosing, is applicable to the extensive shale gas pressing crack construction of continuous mixture construction technology
2, through overtesting, when recording this reversed-phase emulsion friction reducer and dissolving in water, tackify rapidly, in 3min, solution apparent viscosity can reach stable viscosity more than 90%.Therefore in the extensive fracturing reform process of shale gas, can adopt continuous mixture technique to carry out dosing construction, liquid friction reducer product can directly pump into manifold by metering with proportioning pump, reduces greatly construction dosing workload, improves operating efficiency.
3, to have adopted the hydrophobic methacrylic dodecyl gallate of long-chain be function monomer to reversed-phase emulsion friction reducer provided by the invention, utilizes hydrophobic association effect to strengthen friction reducer molecule (5～16 m under the high infusion discharge capacity of pressing crack construction at the scene
3/ min) there is good molecular structure stabilized.
4, reversed-phase emulsion friction reducer provided by the invention only need obtain product by one-step polymerization in process of production, and can reach product application performance without passing into nitrogen deoxygenation in production process, production time short (6h left and right), greatly simplify production process, reduced production cost.
5, to fall dosage low for reversed-phase emulsion friction reducer provided by the invention, and resistance reducing effect is good, and in shale gas slippery water pressing crack construction, under 0.05%～0.1% friction reducer dosage condition, its resistance-reducing yield can reach more than 70% at the scene.
6, providing following contrast experiment's data, illustrate in this preparation method the 4th with this) selection of the parameters of step has specific reason:
| Comparative example | The temperature of reversed-phase emulsion (℃) | After aqueous solution of sodium bisulfite dropwises, start stir time system temperature (℃) | Standing soaking time (hour) | Comparing result |
| 1 | 15～25 | 35 | 4 | Polymerization is steady, and product is placed stable, and resistance-reducing yield can reach more than 70% |
| 2 | 25～30 | 35 | 4 | Polymerization is steady, and product shelf-stability is poor, very easily after blowing, occurs and breakdown of emulsion caking sudden and violent gathering in 24 hours |
| 3 | 15～25 | 25～30 | 4 | Polymerization is steady, and product is poor at non-lucifuge place shelf-stability, and in 2 days, autohemagglutination caking, place and stablize, but resistance-reducing yield is only 30% left and right at lucifuge place |
| 4 | 15～25 | More than 40 | 4 | Polymerization in early stage is steady, and after temperature rises to more than 40 ℃, polymerization temperature climbing speed is sharply accelerated, then drives agitator and water coolant is also difficult to control rising sharply of temperature, and material sudden and violent coalescence in reactor is lumpd |
| 5 | 15～25 | 35 | 1～3 | Polymerization is steady, and product has autohemagglutination exothermic phenomenon while placement at non-lucifuge place, but does not occur breakdown of emulsion caking, places and stablizes at lucifuge place, and resistance-reducing yield is in 50% left and right |
Accompanying drawing explanation
Below in conjunction with specification drawings and specific embodiments, the present invention is described in further detail, wherein:
Fig. 1 is the friction test graphic representation under the coiled tubing, 700 type fracturing truck infusions, 0.1% reversed-phase emulsion friction reducer dosage condition of the long internal diameter 25.4mm of 375m.
Fig. 2 is the frictional resistance graphic representation of the relative clear water of the friction reducer aqueous solution under different displacements under above-mentioned test condition.
Embodiment
embodiment 1(presses 400kg and produces)
In reactor, add 121.7kg clear water, add the anionic monomer acrylic acid of 30kg, add the sodium hydroxide solution of 16.7kg sodium hydroxide and the preparation of 25kg clear water, regulate pH value in 6.5 left and right, add the solubility promoter sodium bicarbonate of non-ionic monomer microbial method acrylamide, 0.3kg initiator azo diisobutyl amidine hydrochloride and the 1kg of 98.5kg, be stirred to completely and dissolve and obtain aqueous phase solution; The oil-soluble monomer methacrylic dodecyl gallate that adds 9kg sorbitan mono-oleic acid ester and 1kg SPAN85 and 1.5kg in the 15# of 90kg white oil, stirs and obtains oil phase; Above-mentioned aqueous phase solution is added dropwise in oil phase under continuously stirring state, dropwises rear emulsify at a high speed 30min and obtain stable reversed-phase emulsion system; With 5kg clear water dissolving 0.3kg sodium bisulfite, under 20 ℃, continuously stirring state, in reversed-phase emulsion system obtained above, drip this aqueous solution of sodium bisulfite, when stopping to stir standing and reacting to system temperature after dropwising and rising to 35 ℃, start and stir, be continuously stirring to stop stirring when temperature no longer changes and leave standstill insulation and after 4 hours, be naturally cooled to blowing after envrionment temperature, obtain homogeneous, stable reversed-phase emulsion friction reducer.Get 10kg friction reducer and add 10m
3in clear water (friction reducer mass percentage concentration is 0.1%), adopt the coiled tubing of the long internal diameter 25.4mm of 375m, with 700 type fracturing truck infusion friction reducer solution, record resistance-reducing yield and can reach 70.7%.
embodiment 2(presses 400kg and produces)
In reactor, add 121.6kg clear water, add the anionic monomer acrylic acid of 32kg, add the sodium hydroxide solution of 17.8kg sodium hydroxide and the preparation of 25kg clear water, regulate pH value in 6.5 left and right, add the solubility promoter sodium bicarbonate of non-ionic monomer microbial method acrylamide, 0.15kg initiator azo diisobutyl amidine hydrochloride and the 1kg of 96kg, be stirred to completely and dissolve and obtain aqueous phase solution; The oil-soluble monomer methacrylic dodecyl gallate that adds 9kg sorbitan mono-oleic acid ester and 1kg SPAN85 and 2kg in the 15# of 90kg white oil, stirs and obtains oil phase; Above-mentioned aqueous phase solution is added dropwise in oil phase under continuously stirring state, dropwises rear emulsify at a high speed 30min and obtain stable reversed-phase emulsion system; With 5kg clear water dissolving 0.45kg sodium bisulfite, under 20 ℃, continuously stirring state, in reversed-phase emulsion system obtained above, drip this aqueous solution of sodium bisulfite, when stopping to stir standing and reacting to system temperature after dropwising and rising to 35 ℃, start and stir, be continuously stirring to stop stirring when temperature no longer changes and leave standstill insulation and after 4 hours, be naturally cooled to blowing after envrionment temperature, obtain homogeneous, stable reversed-phase emulsion friction reducer.Get 10kg friction reducer and add 10m
3in clear water (friction reducer mass percentage concentration is 0.1%), adopt the coiled tubing of the long internal diameter 25.4mm of 375m, with 700 type fracturing truck infusion friction reducer solution, record resistance-reducing yield and can reach 70.2%.
embodiment 3(presses 400kg and produces)
In reactor, add 116.6kg clear water, add the anionic monomer acrylic acid of 35kg, add the sodium hydroxide solution of 19.5kg sodium hydroxide and the preparation of 25kg clear water, regulate pH value in 6.5 left and right, add the solubility promoter sodium bicarbonate of non-ionic monomer microbial method acrylamide, 0.3kg initiator azo diisobutyl amidine hydrochloride and the 1kg of 95kg, be stirred to completely and dissolve and obtain aqueous phase solution; The oil-soluble monomer methacrylic dodecyl gallate that adds 8.5kg sorbitan mono-oleic acid ester and 1.5kg SPAN85 and 2kg in the 15# of 90kg white oil, stirs and obtains oil phase; Above-mentioned aqueous phase solution is added dropwise in oil phase under continuously stirring state, dropwises rear emulsify at a high speed 30min and obtain stable reversed-phase emulsion system; With 5kg clear water dissolving 0.6kg sodium bisulfite, under 20 ℃, continuously stirring state, in reversed-phase emulsion system obtained above, drip this aqueous solution of sodium bisulfite, when stopping to stir standing and reacting to system temperature after dropwising and rising to 35 ℃, start and stir, be continuously stirring to stop stirring when temperature no longer changes and leave standstill insulation and after 4 hours, be naturally cooled to blowing after envrionment temperature, obtain homogeneous, stable reversed-phase emulsion friction reducer.Get 10kg friction reducer and add 10m
3in clear water (friction reducer mass percentage concentration is 0.1%), adopt the coiled tubing of the long internal diameter 25.4mm of 375m, with 700 type fracturing truck infusion friction reducer solution, record resistance-reducing yield and can reach 68.7%.
embodiment 4
As a preferred embodiments of the present invention, its shale gas slippery water pressure break reversed-phase emulsion friction reducer, by percentage to the quality, the proportioning of each component is as follows: high molecular weight water soluble polymer 35%; Non-polar solvent 23%; Oil-soluble emulsifier 2.5%; Solubility promoter 0.25%; All the other are water.Described high molecular weight water soluble polymer is the multipolymer of acrylamide, sodium acrylate and three kinds of monomers of methacrylic dodecyl gallate, in high molecular weight water soluble polymer, the mass percent of described acrylamide is 70%, and the mass percent of described sodium acrylate is 29%; The mass percent of described water beetle base dodecyl acrylate is 1%; Initiator in high molecular weight water soluble polymer is azo diisobutyl amidine hydrochloride and sodium bisulfite composite initiator, wherein, azo diisobutyl amidine hydrochloride accounts for 0.2% of described three kinds of monomer total masses, and sodium bisulfite accounts for 0.3% of described three kinds of monomer total masses.Described non-polar solvent is 15# white oil.Described oil-soluble emulsifier is sorbitan mono-oleic acid ester and SPAN85 compound emulsifying agent, and wherein the mass ratio of sorbitan mono-oleic acid ester and SPAN85 is 8～9:1～2.Described solubility promoter is sodium bicarbonate.
Claims (7)
1. a shale gas slippery water pressure break reversed-phase emulsion friction reducer, is characterized in that: by percentage to the quality, the proportioning of each component is as follows:
High molecular weight water soluble polymer 30%～37.5%;
Non-polar solvent 20%～25%;
Oil-soluble emulsifier 2.5%～2.75%;
Solubility promoter 0.2%～0.3%;
All the other are water.
2. described shale gas slippery water pressure break reversed-phase emulsion friction reducer according to claim 1, it is characterized in that: high molecular weight water soluble polymer is the multipolymer of acrylamide, sodium acrylate and three kinds of monomers of methacrylic dodecyl gallate, in high molecular weight water soluble polymer, the mass percent of described acrylamide is 65%～70%, and the mass percent of described sodium acrylate is 29%～33%; The mass percent of described water beetle base dodecyl acrylate is 1%～2%; Initiator in high molecular weight water soluble polymer is azo diisobutyl amidine hydrochloride and sodium bisulfite composite initiator, wherein, azo diisobutyl amidine hydrochloride accounts for 0.1%～0.3% of described three kinds of monomer total masses, and sodium bisulfite accounts for 0.1%～0.4% of described three kinds of monomer total masses.
3. described shale gas slippery water pressure break reversed-phase emulsion friction reducer according to claim 1, is characterized in that: described non-polar solvent is 15# white oil.
4. described shale gas slippery water pressure break reversed-phase emulsion friction reducer according to claim 1, it is characterized in that: described oil-soluble emulsifier is sorbitan mono-oleic acid ester and SPAN85 compound emulsifying agent, and wherein the mass ratio of sorbitan mono-oleic acid ester and SPAN85 is 8～9:1～2.
5. described shale gas slippery water pressure break reversed-phase emulsion friction reducer according to claim 1, is characterized in that: described solubility promoter is sodium bicarbonate.
6. a preparation method for reversed-phase emulsion friction reducer for shale gas slippery water pressure break, is characterized in that step is as follows:
1) prepare acrylamide, sodium acrylate and three kinds of monomers of methacrylic dodecyl gallate, first by soluble in water the sodium acrylate that accounts for three kinds of monomer total masses 23%～29%, add again account for three kinds of monomer total masses 70%～75% acrylamide, account for three kinds of monomer total masses, 0.1%～0.3% initiator azo diisobutyl amidine hydrochloride and account for the solubility promoter sodium bicarbonate of prepared friction reducer total mass 0.2%～0.3%, stirring and dissolving obtains aqueous phase solution;
2) in the 15# white oil that accounts for prepared friction reducer total mass 20%～25%, add the emulsifier sorbitol acid anhydride monoleate and the SPAN85 that account for prepared friction reducer total mass 2.5%～2.75%, wherein: the mass ratio of sorbitan mono-oleic acid ester and SPAN85 is 8～9:1～2; In described 15# white oil, add again the methacrylic dodecyl gallate that accounts for three kinds of monomer total masses 1%～2%, stir and obtain oil phase;
3) by above-mentioned 1) aqueous phase solution that obtains in step is added dropwise to above-mentioned 2 under continuously stirring state) in the oil phase that obtains of step, dropwise rear emulsification 30min and obtain reversed-phase emulsion;
4) under 15～25 ℃, continuously stirring state to above-mentioned 3) drip the aqueous solution of sodium bisulfite that accounts for three kinds of monomer total masses 0.1%～0.4% in the reversed-phase emulsion that obtains of step, after dropwising, stop stirring when also standing and reacting to system temperature rises to 35 ℃ and start and stir, be continuously stirring to and when temperature no longer changes, stop stirring and leave standstill insulation after 4 hours, naturally be cooled to blowing after envrionment temperature, obtain reversed-phase emulsion friction reducer.
7. described shale gas slippery water pressure break reversed-phase emulsion friction reducer according to claim 6, is characterized in that: in described step 1), acrylamide selects acrylamide performance prepared by microbial method more.
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| CN104744630A (en) * | 2015-03-26 | 2015-07-01 | 长江大学 | Drag reducer for low-damage hydraulic fracture of hydrophobic modified oil-based inverse emulsion |
| CN105384868A (en) * | 2014-09-05 | 2016-03-09 | 中国石油化工股份有限公司 | Drag reducing agent composition for fracturing, preparation method of drag reducing agent for fracturing, and drag reducing agent for fracturing |
| CN105418840A (en) * | 2015-12-04 | 2016-03-23 | 中国石油大学(华东) | Preparation method of hydrophobically associating polymer inverse emulsion |
| CN106661441A (en) * | 2014-07-15 | 2017-05-10 | 索尔维美国有限公司 | Salt tolerant friction reducer |
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| CN109135687A (en) * | 2018-08-01 | 2019-01-04 | 四川省威沃敦化工有限公司 | A kind of shale gas fracturing fluid Instant suspension salt resistance friction reducer and preparation method thereof |
| CN109265605A (en) * | 2018-11-26 | 2019-01-25 | 西南石油大学 | A kind of low adsorption salt tolerant friction reducer suitable for shale reservoir fracturing reform |
| CN111748332A (en) * | 2020-07-16 | 2020-10-09 | 陕西万朗石油工程技术服务有限公司 | Multifunctional online emulsified self-crosslinking fracturing fluid and preparation method thereof |
| CN111763511A (en) * | 2020-06-28 | 2020-10-13 | 中国石油集团长城钻探工程有限公司压裂公司 | Preparation and liquid preparation method of integrated self-crosslinking thickener modified polymer for fracturing |
| CN112029491A (en) * | 2020-09-15 | 2020-12-04 | 郑州德融科技有限公司 | Drag reducer for fracturing and production process thereof |
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| CN103146372A (en) * | 2013-02-28 | 2013-06-12 | 中国石油化工股份有限公司 | Inverse emulsion polymer thickener for fracturing fluid and preparation method thereof |
| CN103627380A (en) * | 2013-11-08 | 2014-03-12 | 中国石油天然气股份有限公司 | Water-soluble drag reducer as well as preparation method and application thereof |
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