CN107459986A - It is a kind of from suspended prop and preparation method thereof - Google Patents

It is a kind of from suspended prop and preparation method thereof Download PDF

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Publication number
CN107459986A
CN107459986A CN201610389988.4A CN201610389988A CN107459986A CN 107459986 A CN107459986 A CN 107459986A CN 201610389988 A CN201610389988 A CN 201610389988A CN 107459986 A CN107459986 A CN 107459986A
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CN
China
Prior art keywords
coupling agent
suspended prop
water
stick type
increasing stick
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CN201610389988.4A
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Chinese (zh)
Inventor
张锁兵
赵梦云
苏长明
苏建政
张汝生
郑承纲
崔佳
刘松
张艳
史爱萍
唐萍
王连生
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China Petroleum and Chemical Corp
Sinopec Exploration and Production Research Institute
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China Petroleum and Chemical Corp
Sinopec Exploration and Production Research Institute
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Priority to CN201610389988.4A priority Critical patent/CN107459986A/en
Publication of CN107459986A publication Critical patent/CN107459986A/en
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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
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/80Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open

Abstract

The invention provides one kind from suspended prop, including:Water-based increasing stick type high polymer material is grafted on through coupling agent modified proppant aggregate.Present invention also offers the above-mentioned preparation method from suspended prop.According to this present invention from suspended prop, with good from suspension function.For hydraulic fracturing, can save conventional pressure break matches somebody with somebody liquid program and equipment, shortens the integral construction time, also reduces due to the injury caused by fracturing fluid recovery (backflow) difference to reservoir and operating cost.Meanwhile it is provided by the invention from suspended prop preparation method, continuous production from suspended prop, there can be the advantages of production efficiency is high, product quality is stable under the conditions of technique for fixing.

Description

It is a kind of from suspended prop and preparation method thereof
Technical field
The present invention relates to field of oil development, and in particular to a kind of from suspension increasing stick type proppant and preparation method thereof.
Background technology
Hydraulic fracturing is the important measures of well production increment, intensified injection of wells, and a large amount of especially as Low permeable oil and gas reservoirs open Hair, hydraulic fracturing technology application are increasingly extensive.The principle of hydraulic fracturing is to utilize the infusion pressure higher than formation fracture pressure, is made Obtain stratum and form man-made fracture, and link up intrinsic fracture, so as to form the flow conductivity higher to formation fluid or entry well fluid, And final significantly lifting oil gas well production or water injection capacity.
In this technique, fracturing propping agents play important work to the high flow conductivity of caused man-made fracture after pressure With.Its action principle is that proppant is carried along into due to man-made fracture caused by pressure break by full-bodied fracturing fluid, is being stopped Only after pressure break infusion, when bottom pressure drops below formation closure pressure, support formation fracture is played by proppant Development status are remained in that, so that pit shaft still keeps preferable connected state with stratum depths, play high flow-guiding channel Effect.
Since 50~sixties of 20th century, successively occur pressing made of the materials such as metal, plastics, walnut shell, glass Proppant is split, but because the defects of its own is unconquerable causes to be eliminated.Proppant used at present is mainly quartz Sand, haydite and overlay film proppant.Quartz sand has that density is relatively low, and is naturally easy to get, the advantage such as cheap, but due to holding The shortcomings such as pressure energy power is poor, easily broken, circularity, sphericity and surface smoothness are low, only make in shallow well, low clossing pressure oil-gas Layer With.For burying deeper oil-gas reservoir, because strata pressure is high, temperature is also higher, mainly using high density, the haydite branch of high intensity Support agent.Particularly at present, it will be that China's oil gas field carries to bury the Low permeable oil and gas reservoirs with abundant reserves deeper, that temperature is higher Rise the main battle ground of yield.This just provides more market demands to the fracturing propping agents of high intensity.
The proppant of high intensity, typically all there is higher density.During deep-well, ultra-deep wells, to carrying branch The fracturing fluid for supportting agent proposes requirements at the higher level, particularly proposes more rigors to the performance of pressure break thickening agent, it is desirable to which it has More preferable heatproof resistant to shearing ability, excellent broken glue effect.This just ultimately results in operating cost and is substantially increased, and due to pressure break Seepage channel caused by liquid returns row's poor performance blocks, and reduces fracturing transformation effect.
Suspended using one kind from suspended prop, i.e. proppant using feature can itself in clear water, without addition The thickener required for load fluid is prepared in conventional fracturing process, while also just eliminates matching somebody with somebody liquid program and setting for conventional pressure break It is standby, the integral construction time is shortened, is also reduced due to the injury caused by fracturing fluid recovery (backflow) difference to reservoir and operating cost.
The process conditions of proppant of the prior art are related to multiple heating, cooling, and auxiliary agent is mostly to be added directly into In aggregate, it is expected that by stirring and reaches uniform state;Meanwhile in order to prevent the caking from suspended prop, agglomeration resistance need to be added Agent, and more auxiliary agents need to be added in order to reach more excellent effect, program is complicated.In addition, the existing production from suspended prop Mode high energy consumption, it is unable to continuous production, product and easily consolidates agglomerating, quality is unstable;And organic substance can be come off from surface it is molten In Xie Shui, Aqueous Solution Viscosity is caused to increase, while temperature has an impact to its sedimentation time, temperature rise, the sedimentation time shortens.
Therefore, still there is larger improvement lifting in for existing at present from suspended prop technology of preparing the problem of, the field Leeway.And optimizing from suspended prop research and development, including formula improvement and preparation process for function admirable, all undoubtedly can be to existing Hydraulic fracturing technology simplifying hydraulic fracturing operations, number of devices, production safety, and the economy and environment finally shown Benefit, it will all produce material impact.
The content of the invention
For existing proppant and from suspended prop technology of preparing exist the shortcomings that, the invention provides a kind of increasing stick type From suspended prop and preparation method.The increasing stick type of the present invention from suspended prop under normal temperature condition, being capable of quick increasing stick (example As 8min cans show preferable suspended state in running water), Stability Analysis of Structures, also have under water in high temperature and high salinity There is good increasing stick effect (for example, under conditions of temperature is higher than 100 DEG C, still to there is good suspending power, and ore deposit in water Change degree is 5.0 × 103Mg/L water sample is smaller from suspension function effect to it).
According to an aspect of the invention, there is provided it is a kind of from suspended prop, including:Through coupling agent modified support Water-based increasing stick type high polymer material is grafted on agent aggregate.
According to the present invention from suspended prop, by the effect of silane coupler, in proppant aggregate and water-based increasing stick Type high polymer material is connected by chemical bond, is connected firmly, in use without departing from and aqueous tackifier high score Sub- material can meet the quick increasing stick of water.According to the present invention from suspended prop, the quick increasing stick of water can be met, from suspending power It is good, Stability Analysis of Structures, in high temperature and the water of high salinity, it can also realize from suspended state.
According to a preferred embodiment of the present invention, the coupling agent is silane coupler, including alkyl silane, amido At least one of silane and methacryloxypropyl silane.Wherein, the alkyl silane includes the ethoxy of isocyanatopropyl three Base silane, dimethoxydiphenylsilane, methyl triacetoxysilane, methyl tributanoximo silane, dimethylformamide dimethyl oxygen Base silane, trimethoxysilane, isobutyl triethoxy silane, phenyltrimethoxysila,e, phenyltriethoxy silane Alkane, n- octyl groups trimethoxy silane, n- octyltri-ethoxysilanes, dodecyl triethoxysilane, dodecyl trimethoxy At least one of base silane and hexadecyl trimethoxy silane etc..The amino silicane coupling agent includes γ-aminopropyl three Ethoxysilane, γ-aminopropyltrimethoxysilane, N- β-aminoethyl-γ-aminopropyltriethoxy dimethoxysilane, N- β-ammonia Ethyl-γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxy diethoxy silane, γ-divinyl triammonium hydroxypropyl methyl two At least one of methoxy silane etc..The methacryloxypropyl silane is γ-(methacryloxypropyl) propyl group trimethoxy Base silane, γ-(methacryloxypropyl) hydroxypropyl methyl dimethoxysilane and γ-methacryloxypropyl triethoxysilicane At least one of alkane etc..In another specific example, the coupling agent dosage is the proppant aggregate dosage 0.1-0.5wt%, such as 0.1-0.2wt%.
According to a preferred embodiment of the present invention, the dosage of the water-based increasing stick type high polymer material is the support The 0.5-10wt% of agent aggregate dosage, such as such as 0.5-5wt%, 0.5-0.6wt%.The water-based increasing stick type high polymer material is chance The high-molecular organic material of the quick increasing stick of water, it is artificial synthesized high polymer material.In a specific example, water-based increasing stick type High polymer material is selected from acrylic polymer, acrylic polymer, 2- acrylamido -2- methyl-propanesulfonic acid esters Birds of the same feather flock together at least one of compound, acrylic acid/2- acrylamido -2- methyl-propanesulfonic acid ester copolymers.The acrylic compounds Polymer includes acrylate copolymer and its derivative, such as polyacrylic acid-acrylamide.The acrylic polymer is such as PMA, polyethyl acrylate, polymethyl methacrylate etc..2- acrylamidos -2- methyl-propan the sulphurs Esters of gallic acid polymer includes 2- acrylamidos -2- methyl-propanesulfonic acids ester polymer and its derivative etc., such as 2- acryloyls Amido -2- methyl-propanesulfonic acid ethyl esters.The acrylic acid/2- acrylamido -2- methyl-propanesulfonic acid ester copolymers, such as Acrylic acid -2- acrylamido -2- methyl-propanesulfonic acid ethyl esters.
According to the another embodiment of the present invention, the proppant aggregate is quartz sand and/or haydite.Such as water / quartz sand or haydite of pickling are washed, the pressure break quartz sand by processing procedures such as washing, classifications can be selected or pressure break sinters Haydite.In an instantiation, the particle size range of the proppant aggregate is 6-140 mesh (109~3350 μm), more preferably grain Footpath scope is 20-70 mesh (212~830 μm).
, being capable of quick increasing stick (such as 8min cans under normal temperature condition according to provided by the invention from suspended prop Preferable suspended state is shown in running water), Stability Analysis of Structures, also there is good increasing stick under water in high temperature and high salinity Effect (for example, under conditions of temperature is higher than 100 DEG C, still there is good suspending power in water, and salinity for 5.0 × 103Mg/L water sample is smaller from suspension function effect to it).The increasing stick type of the present invention utilizes proppant aggregate from suspended prop The chance water increasing stick group of surface modification (grafting), adds aqueous phase viscosity around proppant particles, achieves oneself in water Suspended state, thickener required for load fluid is prepared in conventional fracturing process without additionally adding, while also just saved Conventional pressure break matches somebody with somebody liquid program and equipment, shortens the integral construction time, also reduces due to caused by fracturing fluid recovery (backflow) difference Injury and operating cost to reservoir.
According to another aspect of the present invention, additionally provide it is a kind of prepare the above-mentioned method from suspended prop, including:
At a certain temperature, the solution of coupling agent is ejected into the surface of proppant aggregate, the coupling agent and proppant First reaction occurs for aggregate, obtains coupling agent modified proppant aggregate;Then by the breast of property of water-bearing increasing stick type high polymer material Liquid is ejected on the proppant aggregate of the modification, the water-based increasing stick type high polymer material and the proppant aggregate of the modification Second reaction, obtain described from suspended prop.
According to method provided by the invention, coupling agent alcoholic solution is ejected into proppant aggregate surface, solvent heated fast Evaporation, and the surface of coupling agent and proppant aggregate is reacted rapidly, is formed and can further be reacted in proppant aggregate surface Coupling molecule, namely by first reaction coupling agent and proppant aggregate is bonded.Then injection will be carried out again contain water Property the high molecular emulsion of increasing stick type, solvent heated fast evaporation, and the proppant of water-based increasing stick type macromolecule and coupling modifier Surface is reacted rapidly, the certainly outstanding proppant of the increasing stick type for being made described.Namely by the second reaction, using coupling agent by proppant bone Material and aqueous tackifier macromolecule are bonded.
According to the method provided by the present invention preferred embodiment, the certain temperature is 105-150 DEG C, preferably 120- 150℃;And/or the reaction time of first reaction is 5-15min, preferably 10min, the reaction time of second reaction is 15-30min, preferably 20min.
According to the method provided by the present invention preferred embodiment, the solution of the coupling agent is molten for the alcohol of coupling agent Liquid.It is preferred that in the solution of the coupling agent, the concentration of coupling agent is 2-10wt%, preferably 5-10wt%.The coupling agent Hydrolytic accelerating agent can be contained in solution, such as acid, such as acetic acid, formic acid etc..
According to the method provided by the present invention preferred embodiment, in the breast of the property of water-bearing increasing stick type high polymer material In liquid, the content of water-based increasing stick type high polymer material is 5-20wt%, preferably 10-20wt%.In a specific embodiment, In the emulsion of the property of water-bearing increasing stick type high polymer material, can also it contain emulsifying agent to improve emulsifying effectiveness, and/or contain water Solve accelerator, such as acid, such as acetic acid, formic acid etc..The emulsion can be that water is solvent or alcohols such as methanol, ethanol or isopropanol Deng for solvent.The emulsifying agent is conventional emulsifying agent, such as polyethylene oxide alkyl ethers, polyoxyalkyl ester.
According to the method for the invention preferred embodiment, methods described specifically comprises the following steps:
(1) proppant aggregate is placed in fluid bed, at 105-150 DEG C, at preferably 120-150 DEG C, makes proppant aggregate Into fluidized state;
(2) fluid bed and then by the solution of the coupling agent from the bottom of fluid bed is sprayed into, carries out the first reaction;
(3) and then by the emulsion of the property of water-bearing increasing stick type high polymer material from the tangent line mouth of fluid bed fluid bed is sprayed into It is interior, constant temperature is kept, under fluidized state, carries out the second reaction, is finally obtained described from suspended prop.
According to the present invention, the use of fluid bed, the contact area of proppant particles and reactant is added, and at the moment In motion state, hot-spot is avoided, improves reaction speed, and the particle flowed is easy to add and taken out, and does not influence Reaction is carried out, and can be made process continuous, be improved production efficiency.
It is of the present invention from suspended prop preparation method, can under the conditions of technique for fixing continuous production from suspension support Agent, there is the advantages of production efficiency is high, product quality is stable.
It is according to the method for the invention preferred embodiment, the coupling agent alcoholic solution prepared is empty using compression Gas, under high pressure (for example, it is preferable to the pressure of compressed air is 0.5-1.0MPa) by bottom pressure spray process (using compressed air by institute The solution for stating coupling agent sprays into fluid bed from the bottom of fluid bed) proppant aggregate surface is ejected into, solvent heated fast steams Hair, and coupling agent is reacted rapidly with proppant surface, and the coupling point that can be further reacted is formed in proppant aggregate surface Son;Again to the modification proppant surface fully reacted, carry out injection again by tangential jet technique and contain increasing stick type high score The solution of son, the evaporation of solvent heated fast, and the proppant surface of increasing stick type macromolecule and coupling modifier is reacted rapidly, is made The certainly outstanding proppant of described increasing stick type.
In a specific embodiment, methods described includes:(1) coupling agent alcoholic solution and water-soluble increasing stick type have been configured High molecular emulsion;(2) fluid bed is opened, adjusts aspiration pressure and EAT, hot blast temperature is set as 120~150 DEG C, pressure Power finally reaches " boiling " fluidized state depending on proppant;(3) atomizing pressure is adjusted after heating is preheating to designated value With certain value, coupling agent alcoholic solution is sprayed into fluid bed from fluidized-bed bottom with compressed air;The pressure of compressed air be 0.5~ 1.0MPa, react 10min;(4) water-soluble increasing stick type high molecular alcohol solution or the aqueous solution are sprayed into fluid bed from tangent line mouth again; (5) after the injection completely of water-soluble increasing stick type high molecular alcohol solution, constant temperature is kept, " boiling " fluidized state is still presented in proppant, Water-soluble increasing stick type functional membrane is formed in proppant aggregate surface, is made described from suspension increasing stick type proppant;Constant temperature time with The reaction completely of increasing stick type high polymer material is advisable, and is usually no more than 30min.
Heretofore described fluid bed, be it is a kind of apply more mature equipment with industrial circle, can be used for be granulated, Coating etc..Routinely composition includes for it:Air filtration heater, bed body, gas distributor, cyclone separator, dipleg, heat exchanger, If the stem portions such as expanding reach are formed.Air after purification is blown at a high speed from bottom by heating, makes proppant particles in bed body In fluidized state, after coupling agent and the high molecular solution atomization of water-soluble increasing stick type are sprayed into, reacted with proppant surface, together When due to continuous drying of the hot-air to proppant, make rapid solvent evaporation, reactant fast reaction.Of the thermal current in suspension Intergranular is by carrying out heat exchange, taking away moisture, make (super-hydrophobic) emulsion for being sprayed on proppant aggregate surface fast under dynamic condition Speed reaction and drying and forming-film.
According to preparation method provided by the invention, preferably in fluid bed, will prepare first containing the molten of coupling agent Liquid, it is injected in using bottom pressure spray process technology from the proppant aggregate of feed bin release, treats that it is fully contacted instead with proppant aggregate Ying Hou, then the Polymer Solution body containing increasing stick type functional group prepared using tangential jet technology from side injection System, after the system is heated, rapid solvent evaporation, and chemistry occurs for increasing stick type high polymer material and the proppant aggregate surface of coupling React and dry rapidly.
According to the present invention, continuous production from suspended prop, can have production efficiency height, product under the conditions of technique for fixing The advantages of steady quality.Meanwhile the increasing stick type of the invention of production from suspended prop under normal temperature condition, being capable of quick increasing stick (such as 8min cans show preferable suspended state in running water), Stability Analysis of Structures are underwater in high temperature and high salinity Also have good increasing stick effect (for example, under conditions of temperature is higher than 100 DEG C, still there is good suspending power in water, And salinity is 5.0 × 103Mg/L water sample is smaller from suspension function effect to it).
According to another aspect of the present invention, additionally provide above-mentioned from oneself of suspended prop or above method preparation Application of the suspended prop in hydraulic fracturing.
, can quickly (such as 8min can for increasing stick under normal temperature condition according to the increasing stick type of the present invention from suspended prop To show preferable suspended state in running water), Stability Analysis of Structures, also there is good increasing under water in high temperature and high salinity Glutinous effect (for example, under conditions of temperature is higher than 100 DEG C, still has good suspending power, and salinity is 5.0 in water ×103Mg/L water sample is smaller from suspension function effect to it).The present invention's is used for hydraulic fracturing from suspended prop, can The thickener prepared in conventional fracturing process required for load fluid need not be added by realizing, (be connect using the modification of proppant aggregate surface Branch) chance water increasing stick group, add aqueous phase viscosity around proppant particles, achieve in water from suspended state, together When also just eliminate conventional pressure break match somebody with somebody liquid program and equipment, shorten the integral construction time, also reduce because fracturing fluid returns Injury to reservoir and operating cost caused by row's difference.
As oilfield prospecting developing degree is deepened, hypotonic in new discovery oil gas field, special hypotonic oil gas field accounting is larger, then Plus hypotonic, the extra-low permeability oil gas field with abundant reserves for being difficult to employ in the past, it will be that China's petroleum resources supplies Important guarantee, and the oil gas in these compact reservoirs needs that by hydraulic fracturing the economic exploitation can be realized.Proppant conduct The critical material that hydraulic fracturing technology is effectively implemented, the breakthrough of its technology are undoubtedly significant.According to the support of the present invention Agent is used for hydraulic fracturing, has broad application prospects.
Embodiment
The present invention is further described with reference to specific embodiment, but the scope of the present invention is not limited to this.
Tested from suspending power:Measure respectively 200mL running water or mineralized water (with potassium chloride prepare salinity be 5.0 × 103Mg/L water sample) it is placed in 6 beakers, 60g is then poured into respectively from suspended prop, with agitator (500r/m) difference Stop stirring after stirring 2min, 4min, 6min, 8min, 30min, 60min, be then poured into 250mL glass cylinders, see Examine its in water from suspending power.
Temperature resistant capability is tested:With running water and mineralized water, (it is 5.0 × 10 to prepare salinity with potassium chloride3Mg/L water) Sample, 100mL then being measured respectively and is poured into beaker, then pour into 30g from suspended prop, 8min is stirred with agitator (500r/m) After be fitted into blue lid bottle, after being placed on 100 DEG C of baking oven constant temperature 3h, take out observe its sinking speed.
Embodiment 1:
Coupling agent alcoholic solution is prepared:Measure absolute ethyl alcohol 900mL, trimethoxysilane 50g, hydrolytic accelerating agent second Sour 10mL, it is standby after being stirred 10 minutes with 400r/min speed.
Water-soluble increasing stick type macromolecule emulsion liquid is prepared:Weigh 250g polyacrylic acid acetoacetic ester (weight average molecular weight 3,000,000, Mw/Mn is 2.56) high polymer material, 10g emulsifier op-10s, measures 30mL acetic acid as hydrolytic accelerating agent, is poured into successively It is standby after being stirred 10 minutes with 1000r/min speed in 1500mL water.
Prepared from suspended prop:A certain amount of 50kg ceramsite propping agents (particle diameter 40-70 mesh) are weighed, are loaded in fluid bed; The blower fan and heater of fluid bed are opened, fan delivery can make the proppant in fluid bed keep fully boiling flowing, heat Air temperature is set as 150 DEG C;When temperature is constant in bed, with the compressed air that pressure is 0.5MPa by the coupling agent alcoholic solution of preparation Spray in fluidized bed, isothermal reaction 10min;Again with the compressed air that pressure is 0.5MPa by the increasing stick type macromolecule of preparation In emulsion injection fluidized bed, isothermal reaction 30min can be taken off obtained from suspended prop.
Obtained from suspended prop will test from suspending power and temperature resistant capability, data are shown in Tables 1 and 2.
Embodiment 2 (contrast):
Water-soluble increasing stick type macromolecule emulsion liquid is prepared with embodiment 1.
Prepared from suspended prop:A certain amount of 50kg ceramsite propping agents (particle diameter 40-70 mesh) are weighed, it is standby to load container; The increasing stick type macromolecule emulsion liquid of preparation is added in container, stirred, after the mixture of gained is spontaneously dried, screening, It is made from suspended prop.See Tables 1 and 2 from suspending power and temperature resistant capability test data.
Suspending power of the table 1 from suspended prop
Table 2 tests (100 DEG C) from suspended prop temperature resistant capability
Embodiment 3:
Coupling agent alcoholic solution is prepared:Measure absolute ethyl alcohol 1700mL, dodecyltrimethoxysilane 100g, acetic acid 50mL, it is standby after being stirred 10 minutes with 400r/min speed.
Water-soluble increasing stick type macromolecule emulsion liquid is prepared:Weigh the poly- 2- acrylamidos -2- methyl-propanesulfonic acid second of 300g Ester (weight average molecular weight 6,000,000, Mw/Mn 1.75) high polymer material, emulsifier op-10 20g, measure 50mL acetolysis rush Enter agent, pour into successively in 2000mL water, it is standby after being stirred 10 minutes with 1000r/min speed.
Prepared from suspended prop:A certain amount of 50kg ceramsite propping agents (particle diameter 40-70 mesh) are weighed, are loaded in fluid bed; The blower fan and heater of fluid bed are opened, fan delivery can make the proppant in fluid bed keep fully boiling flowing, heat Air temperature is set as 150 DEG C;When temperature is constant in bed, with the compressed air that pressure is 0.5MPa by the coupling agent alcoholic solution of preparation Spray in fluidized bed, isothermal reaction 10min;Again with the compressed air that pressure is 0.5MPa by the increasing stick type macromolecule of preparation In emulsion injection fluidized bed, isothermal reaction 30min can be taken off obtained from suspended prop.
Tested obtained from suspended prop from suspending power and temperature resistant capability, the results are shown in Table 3 and table 4.
Embodiment 4 (comparative example):
Water-soluble increasing stick type macromolecule emulsion liquid is prepared with embodiment 3.
Prepared from suspended prop:A certain amount of 50kg ceramsite propping agents (particle diameter 40-70 mesh) are weighed, it is standby to load container; The increasing stick type macromolecule emulsion liquid of preparation is added in container, stirred, after the mixture of gained is spontaneously dried, screening, It is made from suspended prop.3 and table 4 are shown in Table from suspending power and temperature resistant capability test data.
Suspending power of the table 3 from suspended prop
Table 4 tests (100 DEG C) from suspended prop temperature resistant capability
Embodiment 5:
(1) coupling agent alcoholic solution is prepared:Measure absolute ethyl alcohol 800mL, γ-(methacryloxypropyl) propyl trimethoxy silicon Alkane 50g, acetic acid 20mL, it is standby after being stirred 10 minutes with 400r/min speed.
(2) water-soluble increasing stick type macromolecule emulsion liquid is prepared:Weigh acrylic acid -2- acrylamido -2- methyl-propan sulphurs Acetoacetic ester copolymer (weight average molecular weight 3,000,000, the mass ratio of acrylic acid and 2- acrylamido -2- methyl-propanesulfonic acid ethyl esters For 8/5, Mw/Mn 1.27) 300g, emulsifier op-10 20g, it is added in 1500mL absolute ethyl alcohols, with 800r/min speed Degree is standby after stirring 10 minutes.
(3) prepared from suspended prop:A certain amount of 50kg ceramsite propping agents (particle diameter 30-50 mesh) are weighed, load fluid bed It is interior;The blower fan and heater of fluid bed are opened, fan delivery can make the proppant in fluid bed keep fully boiling flowing, Hot blast temperature is set as 150 DEG C;When temperature is constant in bed, it will be prepared with the compressed air that pressure is 0.5MPa in step (1) In coupling agent alcoholic solution injection fluidized bed, isothermal reaction 10min;Again with the compressed air that pressure is 0.5MPa by step (2) in the middle increasing stick type macromolecule emulsion liquid injection fluidized bed prepared, isothermal reaction 30min can be taken off obtained from suspension Proppant.
Tested obtained from suspended prop from suspending power and temperature resistant capability, the results are shown in Table 5 and table 6.
Embodiment 6 (comparative example):
Water-soluble increasing stick type macromolecule emulsion liquid is prepared with embodiment 5.
Prepared from suspended prop:A certain amount of 50kg ceramsite propping agents (particle diameter 40-70 mesh) are weighed, it is standby to load container; The increasing stick type macromolecule emulsion liquid of preparation is added in container, stirred, after the mixture of gained is spontaneously dried, screening, It is made from suspended prop.5 and table 6 are shown in Table from suspending power and temperature resistant capability test data.
Suspending power of the table 5 from suspended prop
Table 6 tests (100 DEG C) from suspended prop temperature resistant capability
According to the present invention, continuous production from suspended prop, can have production efficiency height, product under the conditions of technique for fixing The advantages of steady quality.Meanwhile the increasing stick type of the invention of production from suspended prop under normal temperature condition, being capable of quick increasing stick (such as 8min cans show preferable suspended state in running water), Stability Analysis of Structures are underwater in high temperature and high salinity Also there is good increasing stick effect.
Any numerical value mentioned in the present invention, if simply having two between any minimum and any of the highest value The interval of unit, then include all values of one unit of each increase from minimum to peak.For example, if statement is a kind of The amount of component, or the value of the state-variable such as temperature, pressure, time is 50-90, it is in this manual it means that specific List 51-89,52-88 ... and the numerical value such as 69-71 and 70-71.For the value of non-integer, can with due regard to 0.1st, 0.01,0.001 or 0.0001 is a unit.This is only some special examples indicated.In this application, with similar side Formula, the combination that is possible to of the numerical value between cited minimum and peak are considered to disclose.
It should be noted that embodiment described above is only used for explaining the present invention, do not form to any of the present invention Limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that word wherein used is descriptive With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it relates to And specific method, material and embodiment, it is not intended that the present invention is limited to wherein disclosed particular case, on the contrary, this hair It is bright to can be extended to other all methods and applications with identical function.

Claims (10)

1. it is a kind of from suspended prop, including:Water-based increasing stick type macromolecule is grafted on through coupling agent modified proppant aggregate Material.
It is 2. according to claim 1 from suspended prop, it is characterised in that the coupling agent is silane coupler, including At least one of alkyl silane, amino containing silane and methacryloxypropyl silane;It is preferred that the coupling agent dosage is described The 0.1-0.5wt% of proppant aggregate dosage, preferably 0.1-0.2wt%.
It is 3. according to claim 1 or 2 from suspended prop, it is characterised in that the water-based increasing stick type high polymer material Dosage be the proppant aggregate dosage 0.5-10wt%, more preferably preferably 0.5-5wt%, 0.5-0.6wt%;And/or
Water-based increasing stick type high polymer material is selected from acrylic polymer, acrylic polymer, 2- acrylamido -2- first At least one in base-propane sulfonic acid esters polymer, acrylic acid/2- acrylamido -2- methyl-propanesulfonic acid ester copolymers Kind.
4. according to any one in claim 1-3 from suspended prop, it is characterised in that the proppant aggregate is Quartz sand and/or haydite;It is preferred that the particle size range of the proppant aggregate is 6-140 mesh, more preferably particle size range is 20-70 Mesh.
5. a kind of method prepared in claim 1-4 described in any one from suspended prop, including:
At a certain temperature, the solution of coupling agent is ejected into the surface of proppant aggregate, the coupling agent and proppant aggregate The first reaction occurs, obtains coupling agent modified proppant aggregate;Then the emulsion of property of water-bearing increasing stick type high polymer material is sprayed It is mapped on the proppant aggregate of the modification, the water-based increasing stick type high polymer material and the proppant aggregate second of the modification Reaction, obtain described from suspended prop.
6. according to the method for claim 5, it is characterised in that the certain temperature is 105-150 DEG C, preferably 120-150 ℃;And/or the reaction time of first reaction is 5-15min, preferably 10-15min, the reaction time of second reaction is 15-30min, preferably 20-30min.
7. the method according to claim 5 or 6, it is characterised in that the solution of the coupling agent is the alcoholic solution of coupling agent; It is preferred that in the solution of the coupling agent, the concentration of coupling agent is 2-10wt%, preferably 5-10wt%;Or
In the emulsion of the property of water-bearing increasing stick type high polymer material, the content of water-based increasing stick type high polymer material is 5- 20wt%, preferably 10-20wt%.
8. according to the method described in any one in claim 5-7, it is characterised in that methods described includes:
(1) proppant aggregate is placed in fluid bed, at 105-150 DEG C, at preferably 120-150 DEG C, makes proppant aggregate into stream Change state;
(2) fluid bed and then by the solution of the coupling agent from the bottom of fluid bed is sprayed into, carries out the first reaction;
(3) and then by the emulsion of the property of water-bearing increasing stick type high polymer material from the tangent line mouth of fluid bed spray into fluid bed, protect Constant temperature is held, under fluidized state, carries out the second reaction, is finally obtained described from suspended prop.
9. according to the method for claim 8, it is characterised in that using compressed air by the solution of the coupling agent from fluidisation The bottom of bed sprays into fluid bed, and the pressure of preferred compressed air is 0.5-1.0MPa.
10. according to any one in claim 1-4 from described in any one in suspended prop or claim 5-9 Application from suspended prop in hydraulic fracturing prepared by method.
CN201610389988.4A 2016-06-03 2016-06-03 It is a kind of from suspended prop and preparation method thereof Pending CN107459986A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109281645A (en) * 2018-09-30 2019-01-29 重庆长江造型材料(集团)股份有限公司 Using the construction method from suspension riverfrac treatment proppant
CN111187609A (en) * 2020-03-18 2020-05-22 大关华欣矿业有限公司 Self-suspending quartz sand used as fracturing propping agent
CN112282722A (en) * 2020-06-05 2021-01-29 中国海洋石油集团有限公司 Low-density organic water-control proppant and preparation method thereof

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CN104379697A (en) * 2012-04-19 2015-02-25 自悬浮支撑有限公司 Self-suspending proppants for hydraulic fracturing
CN104946234A (en) * 2014-03-28 2015-09-30 北京仁创科技集团有限公司 Self-suspended propping agent and preparation method thereof
US20160333258A1 (en) * 2015-05-13 2016-11-17 Preferred Technology, Llc Hydrophobic Coating of Particulates for Enhanced Well Productivity

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN104379697A (en) * 2012-04-19 2015-02-25 自悬浮支撑有限公司 Self-suspending proppants for hydraulic fracturing
CN104946234A (en) * 2014-03-28 2015-09-30 北京仁创科技集团有限公司 Self-suspended propping agent and preparation method thereof
US20160333258A1 (en) * 2015-05-13 2016-11-17 Preferred Technology, Llc Hydrophobic Coating of Particulates for Enhanced Well Productivity

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109281645A (en) * 2018-09-30 2019-01-29 重庆长江造型材料(集团)股份有限公司 Using the construction method from suspension riverfrac treatment proppant
CN111187609A (en) * 2020-03-18 2020-05-22 大关华欣矿业有限公司 Self-suspending quartz sand used as fracturing propping agent
CN112282722A (en) * 2020-06-05 2021-01-29 中国海洋石油集团有限公司 Low-density organic water-control proppant and preparation method thereof

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Application publication date: 20171212