CN109385261A - A kind of preparation method from outstanding proppant - Google Patents
A kind of preparation method from outstanding proppant Download PDFInfo
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- CN109385261A CN109385261A CN201811159440.6A CN201811159440A CN109385261A CN 109385261 A CN109385261 A CN 109385261A CN 201811159440 A CN201811159440 A CN 201811159440A CN 109385261 A CN109385261 A CN 109385261A
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- proppant
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
- C09K8/805—Coated proppants
Abstract
The invention belongs to the fluid minerals production technique such as petroleum, natural gas and shale gas fields, a kind of preparation method from outstanding proppant is specifically disclosed, after certainly outstanding proppant is impregnated with organic solvent, filtering, filtering solution is taken to test, the content of the isocyano in solution accounts for the one thousandth of solid content or more；The preparation from outstanding proppant is the following steps are included: it includes outermost resin, outer layer catalyst and outer layer curing agent that (1), which prepares aggregate, inner membrance material and outer membrane material, outer membrane material,；(2) aggregate is heated to 80-160 DEG C, inner membrance material is added, stirring, the revolving speed of stirring is at 50-100 revs/min；(3) temperature drops to 55-110 DEG C, outermost resin and outer layer catalyst is added, stirring, the revolving speed of stirring is at 50-100 revs/min；(4) temperature drops to 40-90 DEG C, outer layer curing agent is added, stirring, for the revolving speed of stirring at 50-100 revs/min, temperature drops to 30-60 DEG C, takes the dish out of the pot.Present invention is mainly used for preparations from outstanding proppant, solves the problems, such as that pure clear water cannot function as pressing crack construction load fluid.
Description
Technical field
The invention belongs to the fluid minerals production technique fields such as petroleum, natural gas and shale gas more particularly to a kind of from outstanding
The preparation method of proppant.
Background technique
In order to develop deep-seated oil, gas well, yield is improved, hydraulic fracturing technology is widely used.Hydraulic fracturing technology is benefit
With the high pressure pump group on ground, the fracturing fluid with viscosity higher is injected constantly into oil well by pit shaft, so that oil well lower part shape
At a kind of technology of high pressure.With the continuous injection of fracturing fluid, pressure is also constantly increased, the formation rock anti-tensile near the borehole wall
When intensity and reservoir stress are less than the pressure that fracturing fluid is formed, the stratum near shaft bottom will just generate crack.When carrying proppant
Fracturing fluid continue injection when, formation fractures can extend forward and be supported agent filling, stop the agent of fracturing work rear support
Play a part of equilibrium strata pressure, make rock seam keep split and have certain flow conductivity, thus reach make oil gas field volume increase,
Extend the purpose of the oil/gas well length of service.
Ideal fracturing propping agent for oil gas well requires have high carrying capacity and high sand ratio, it is therefore desirable to alap
Density and intensity as high as possible.The fracturing propping agents that conventional method is prepared have quartz sand and haydite and their overlay film
Product, outer film coating are solidified at high temperature with phenolic aldehyde or epoxy resin, the amount of curing agent generally in the 5-50% of amount of resin,
Coated temperature is at 230 degree or so, and traditional fracturing propping agents intensity is big, but density is also high, and suspension is poor, is easy precipitating,
It is not easy to be carried into well.The proppant product of existing method preparation is gone back other than coating epoxy resin, phenolic resin film
There is coating urethane resin film, polyurethane resin is a great system, the raw material selected by strict control, raw material
Dosage, condition of reaction etc. can make polyurethane resin have entirely different substance physical property, the existing poly- ammonia for being used to support agent
Ester resin is the polyurethane resin with high rigidity substance physical property, it is ensured that resin film has high-caliber hardness and good resistance to compression
Fragility finally makes proppant have good resistant to breakage ability.But the proppant of the existing urethane resin film of coating produces
Product are still only to meet intensity, hardness requirement, not can solve proppant suspension it is poor, be easy precipitating the problem of.
In order to more effectively make fracturing propping agents reach the target position of well, need to prepare carrying liquid during pressure break.
Carrying liquid is to add water soluble polymer and other additive using water as main carriers to increase the viscosity for carrying liquid,
The frictional resistance for carrying liquid is reduced simultaneously.Fracturing propping agents and carrying liquid mixing in the construction process, in highly viscous carrying liquid,
Fracturing propping agents suspend wherein, thus can pump farther.But it carries macromolecule frozen glue material used in liquid and exists
It is at high cost, serious to reservoir damage, cause serious pollution to the environment, complicated construction technique the disadvantages of.
Also occur some proppants that can be suspended certainly in water, the existing proppant master that can be suspended certainly in water at present
There are two class technologies, first is that in aggregate quartz sand or haydite surface coating layer of material, this material is mainly some water-soluble
Property high molecular material, such as polyacrylamide, carboxymethyl cellulose, polyacrylic acid, guar gum, natural plant gum.These materials meet water
It can expand rapidly, and the viscosity that can dissolve into increase water in water achievees the purpose that suspension.This technology from suspended prop not
There is the technology for fundamentally changing suspension, thickener overlay film is not only solved environmental issue on aggregate, without real
Realization reduce cost, increase production and improve productivity.Another technology is to change the apparent density of aggregate, makes the haydite of extremely-low density, or
Resin beads.Such product is able to achieve really half to suspend in water, reduces the rate of settling of proppant in water, but due to wanting
Apparent density is greatly lowered, production cost greatly increases, and the performance of proppant, such as broken, sour molten, water conservancy diversion performance meeting
It is substantially reduced.And the production efficiency of resin beads is low, it is at high cost the defects of, also limit its popularization and use.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method from outstanding proppant, it is prepared with to solve conventional method
Fracturing propping agents density is high, suspension is poor, it is not easy to be carried into the problems in well.
In order to achieve the above object, base case of the invention are as follows: a kind of preparation method from outstanding proppant, from outstanding support
After agent is impregnated with organic solvent, filtering, take filtering solution to test, the content of the isocyano in solution account for solid content thousand/
One or more；The preparation from outstanding proppant the following steps are included:
(1) preparing aggregate, inner membrance material and outer membrane material, outer membrane material includes outermost resin, outer layer catalyst and outer layer
Curing agent；
(2) aggregate is heated to 80-160 DEG C, inner membrance material is added, stirring, the revolving speed of stirring is at 50-100 revs/min；
(3) temperature drops to 55-110 DEG C, outermost resin and outer layer catalyst is added, stirring, the revolving speed of stirring is in 50-100
Rev/min；
(4) temperature drops to 40-90 DEG C, outer layer curing agent is added, stirring, at 50-100 revs/min, temperature drops the revolving speed of stirring
It to 30-60 DEG C, takes the dish out of the pot, obtains from outstanding proppant.
The beneficial effect of this base case is:
1, applicant studies for a long period of time discovery, and after being impregnated with organic solvent from outstanding proppant, filtering takes filtering solution to test,
When more than the one thousandth that the content of the isocyano in solution accounts for solid content, proppant can suspend in clear water, and
Suspension time is greater than 4 hours, suspends than being greater than 10%, the effect of suspension is preferable.
2, the proppant that the present patent application is prepared can suspend in water, therefore directly achieve that height using clear water
Prop-carrying capacity, without changing the density of water.During exploiting oil gas, traditional pressure break branch is replaced using riverfrac treatment proppant
Agent is supportted, traditional fracturing fluid is replaced using clear water, realizes zero addition of load fluid thickener in fracturing work, and then save conventional pressure
What is split matches liquid process and equipment.Meanwhile the removal of thickener also reduces injury and pressure break cost of the pressure break to reservoir.
3, the proppant being prepared using the present patent application, construction fracturing fluid not only can be used clear water, also can be used ground
Recycling can be recycled after instead arranging in layer water and multi-purpose station sewage, fracturing fluid, and Saline Water is more advantageous to the use of the product, reduces
Fracturing fluid cost.
4, the Applicable temperature range of proppant of the invention in pressing crack construction is 5 DEG C -145 DEG C, proppant Applicable temperature
Range is wide, and the stability in this temperature range is good, using effect is good.
Further, inner membrance material includes the first resin and the first curing agent, and the first resin quality number is aggregate quality part
Several 0.5-9%, the first curing agent mass fraction are the 10-50% of the first resin quality number；In step (2), by aggregate plus
Heat arrives 80-160 DEG C, the first resin is added, stirring, the revolving speed of stirring is at 50-100 revs/min；Temperature drops to 65-130 DEG C, is added
First curing agent, stirring, the revolving speed of stirring is at 50-100 revs/min.
Further, inner membrance material includes the second resin, the second curing agent and internal layer catalyst, and the second resin quality number is
The 0.5-9% of aggregate quality number, the second curing agent mass fraction are the 40-80% of the second resin quality number, internal layer catalysis
Agent mass fraction is the 0.1-1% of the second resin quality number；In step (2), aggregate is heated to 80-160 DEG C, is added second
Resin and internal layer catalyst, stirring, the revolving speed of stirring is at 50-100 revs/min；Temperature drops to 65-130 DEG C, and the second solidification is added
Agent, stirring, the revolving speed of stirring is at 50-100 revs/min.
Further, the outer layer curing agent, the second curing agent are isocyanates.Select isocyanates as solidification
Agent, resin cured effect of being heated are preferable.
Further, the outer layer catalyst, internal layer catalyst are the organo-metallic compound and/or alkyl of alkyls tin
One or more of organo-metallic compound of ekalead.The organo-metallic compound of alkyls tin and alkyl ekalead is as catalysis
Agent, the effect for being catalyzed reaction are preferable.
Further, the outermost resin, the second resin are polyalcohols resin；The equivalent of outermost resin hydroxyl is 60-
300, the mass fraction of outer layer curing agent is the 40-80% of outermost resin mass fraction.Polyalcohols resin energy and isocyanates
Reaction generate polyurethane resin, we application in by the dosage of strict control outer layer curing agent make isocyanates with it is more
First alcohols resin reaction still has residue after generating polyurethane resin.Proppant is put into water, when proppant and water contact, table
The isocyanates in face can react rapidly with water releases gas molecules, these gas molecules or is enclosed in swollen in theca externa
It is swollen, it pushes theca externa stage to thicken and increases the equivalent diameter of proppant particles body, or be attached to proppant surface stage
The gas blanket that one layer of package proppant particles body is formed on the interface that proppant coating layer is contacted with water body is extended or is gathered in, this
Kind of gas blanket formation stages between proppant particles body are connected to and the result closed cause simple grain proppant formed in water body compared with
Gather shape for loose cotton wadding, is greatly lowered the relative density of proppant in water in this way, the suspension of proppant can be made
Performance is more preferably.
Further, outermost resin mass fraction is the 0.5-9% of aggregate quality number, and outer layer catalyst mass fraction is outer
The 0.1-1% of layer resin quality number.Catalyst in the range, is not only able to achieve outermost resin and solidifies well, and advantageous
It is swelled in generating, not only can increase the resistant to breakage ability of proppant in this way, but also can increase suspension.Applicant is by repeatedly research hair
It is existing, using the raw material production of above-mentioned mass fraction from outstanding proppant, be prepared from outstanding proppant suspension effect and its
His better performances.
Further, outer membrane material further includes aminated compounds, and the mass fraction of aminated compounds is outermost resin mass parts
Several 10-20%.Polyalcohols resin reacts the isocyanates for having some residual with isocyanates, remaining isocyanates with
Aminated compounds reaction, during this, can generate the gases such as nitrogen, nitric oxide, carbon monoxide, portion gas is closed in
In not yet fully hardened urethane resin film, a large amount of protuberance is formed, the diameter of protuberance is 100-500nm, and protuberance quantity exists
Every square millimeter 4 × 107More than a, these protuberances facilitate proppant and suspend.What strict control aminated compounds was added
Amount, it is ensured that suitable gas is generated in reaction process, guarantees that the protuberance size generated controls in suitable range, it is not too big
And it is formed and wears stomata.Aminated compounds there remains the isocyanates of part after reacting with isocyanates, proppant is put into water
Afterwards, remaining isocyano can act on water and generate gas in proppant, and portion gas evolution, portion gas is closed in protuberance
In, the volume further expansion of protuberance makes resin membrane swelling, can make the suspendability of proppant more preferably.
Further, the preparation from outstanding proppant the following steps are included:
(1) prepare aggregate, inner membrance material and outer membrane material, outer membrane material includes that outermost resin, outer layer catalyst, outer layer are solid
Agent and aminated compounds；
(2) aggregate is heated to 80-160 DEG C, inner membrance material is added, stirring, the revolving speed of stirring is at 50-100 revs/min；
(3) temperature drops to 55-110 DEG C, outermost resin and outer layer catalyst is added, stirring, the revolving speed of stirring is in 50-100
Rev/min；
(4) temperature drops to 50-100 DEG C, and aminated compounds is added, is stirred 10-20 seconds；
(5) temperature drops to 40-90 DEG C, outer layer curing agent is added, stirring, at 50-100 revs/min, temperature drops the revolving speed of stirring
It to 30-60 DEG C, takes the dish out of the pot, obtains from outstanding proppant.
Applicant is by repeatedly the study found that being made by the above method from outstanding proppant, what is be prepared supports from outstanding
Agent suspension effect and other better performances.
Further, polyalcohols resin selects one of polymer such as ethyl alcohol, ethylene glycol, propylene glycol, glycerine, propyl alcohol
Or it is several.Application experiment discovery, selects above-mentioned specific resin, the proppant material resultant effect being prepared is preferable.
Further, isocyanates selects toluene di-isocyanate(TDI), methylenediphenyl diisocyanates, isophorone two
One of isocyanates, methyl diphenylene diisocyanate are several.By applicant's the study found that selecting above-mentioned
For raw material as curing agent, resin cured effect of being heated is preferable.
Further, the organo-metallic compound of alkyls tin specifically selects dibutyl tin dilaurate, tributyl tin, alkyl
The organo-metallic compound of ekalead specifically selects lead tetraethide, isooctyl acid lead.By applicant's the study found that selecting above-mentioned
For raw material as catalyst, the effect for being catalyzed reaction is preferable.
Further, the aminated compounds is diethylenetriamine, triethylamine, ethamine, triethylene tetramine, one in ethylenediamine
Kind is several.Applicant has found by test of many times, selects above-mentioned raw material as aminated compounds, can make proppant material
The effect for generating protuberance is more preferable.
Further, in first resinous molecular structure at least containing epoxy group, phenolic hydroxyl group, carbonyl, amide groups, amino,
The average molecular weight of the organic macromolecule material of two or more groups in isocyanate group, the first resin is greater than 100.Applicant
It is found by test of many times, selects above-mentioned material as the first resin, the theca interna intensity being prepared is preferable.
Further, the aggregate selects quartz sand, haydite, Artificial Ceramic matter sand, organic synthesis sand or organo-mineral complexing
Material sand.The aggregate of proppant material need to meet index in certain performances, and above-mentioned aggregate can preferably meet use demand.
Detailed description of the invention
Fig. 1 is the electron-microscope scanning figure from outstanding proppant being prepared in embodiment 1.
Specific embodiment
Raw material selection is illustrated below, and the present invention is described in further detail by specific embodiment:
Outer layer curing agent, the second curing agent in the present embodiment are isocyanates, select toluene di-isocyanate(TDI), methylene
One of base diphenyl diisocyanate, isophorone diisocyanate, methyl diphenylene diisocyanate are several.
Aminated compounds in the present embodiment is diethylenetriamine, in triethylamine, ethamine, triethylene tetramine, ethylenediamine
It is one or several kinds of.
Outer layer catalyst, internal layer catalyst in the present embodiment are the organo-metallic compound and/or alkane of alkyls tin
One or more of the organo-metallic compound of base class lead, the organo-metallic compound of alkyls tin specifically select tin dilaurate
Dibutyl tin, tributyl tin, the organo-metallic compound of alkyl ekalead specifically select lead tetraethide, isooctyl acid lead.
Outermost resin, the second resin in the present embodiment are polyalcohols resin, select ethyl alcohol, ethylene glycol, propylene glycol,
One of polymer such as glycerine, propyl alcohol are several.
At least containing in epoxy group, phenolic hydroxyl group, carbonyl, amide groups, amino, isocyanate group in first resinous molecular structure
Two or more groups organic macromolecule material, the average molecular weight of the first resin is greater than 100.
Embodiment 1
A kind of preparation method from outstanding proppant, comprising the following steps:
(1) prepare the raw material of following mass fraction: 100 parts of aggregate, 1.8 parts of outermost resin, 2 parts of the first resin, first are consolidated
0.8 part of agent, 1.3 parts of outer layer curing agent, 0.005 part of outer layer catalyst, 0.2 part of aminated compounds.Wherein aggregate selects 20/40
Quartz sand, outermost resin select alcohol polymer, the first resin to select epoxy resin, and the first curing agent selects T31, outer layer solidification
Isophorone diisocyanate is selected in agent, and outer layer catalyst selects isooctyl acid lead, and aminated compounds selects triethylamine.
(2) aggregate is heated to be put into sand mixer after 140 DEG C, the first resin is added, stirred, 50 revs/min of sand mixer revolving speed；
(3) temperature drops to 110 DEG C, and the first curing agent is added, and stirs, 50 revs/min of sand mixer revolving speed；
(4) temperature drops to 95 DEG C, and outermost resin and outer layer catalyst is added, and stirs, 50 revs/min of sand mixer revolving speed；
(5) temperature drops to 85 DEG C, and aminated compounds is added, and stirs 10 seconds, 55 revs/min of sand mixer revolving speed；
(6) temperature drops to 75 DEG C, and outer layer curing agent is added, and stirs, 55 revs/min of sand mixer revolving speed；Temperature drops to 55 DEG C, out
Pot is obtained from outstanding proppant.
In the present embodiment, after which is impregnated with organic solvent, filtering takes filtering solution to test, in solution
The content of isocyano account for the 1/900 of solid content.
Embodiment 2
A kind of preparation method from outstanding proppant, comprising the following steps:
(1) prepare the raw material of following mass fraction: 100 parts of aggregate, 1 part of outermost resin, 1 part of the first resin, the first solidification
0.6 part of agent, 0.8 part of outer layer curing agent, 0.008 part of outer layer catalyst, 0.3 part of aminated compounds.Wherein aggregate selects 30/50 stone
Sand, outermost resin select glycerine polymer, the first resin to select epoxy resin, and the first curing agent selects 113D, outer layer solid
Agent selects methylenediphenyl diisocyanates, and outer layer catalyst selects tributyl tin, and aminated compounds selects ethylenediamine.
(2) aggregate is heated to be put into sand mixer after 120 DEG C, the first resin is added, stirred 15 seconds, sand mixer revolving speed 55
Rev/min；
(3) temperature drops to 100 DEG C, and the first curing agent is added, and stirs, 55 revs/min of sand mixer revolving speed；
(4) temperature drops to 90 DEG C, and outermost resin and outer layer catalyst is added, and stirs 15s, and 55 revs/min of sand mixer revolving speed；
(5) temperature drops to 80 DEG C, and aminated compounds is added, and stirs, 55 revs/min of sand mixer revolving speed；
(6) temperature drops to 70 DEG C, and outer layer curing agent is added, and stirs, 55 revs/min of sand mixer revolving speed；Temperature drops to 50 DEG C, out
Pot is obtained from outstanding proppant.
In the present embodiment, after which is impregnated with organic solvent, filtering takes filtering solution to test, in solution
The content of isocyano account for the 1/680 of solid content.
Embodiment 3
A kind of preparation method from outstanding proppant, comprising the following steps:
(1) prepare the raw material of following mass fraction: 100 parts of aggregate, 1.2 parts of outermost resin, 1.5 parts of the first resin, first
0.5 part of curing agent, 0.8 part of outer layer curing agent, 0.01 part of outer layer catalyst, 0.3 part of aminated compounds.Wherein aggregate selects 40/
70 quartz sands, outermost resin select ethylene glycol polymer, the first resin to select phenolic aldehyde tree, and the first curing agent selects six methines four
Amine, outer layer curing agent select toluene di-isocyanate(TDI), and outer layer catalyst selects tributyl tin, and aminated compounds selects triethylene four
Amine.
(2) aggregate is heated to be put into sand mixer after 150 DEG C, the first resin is added, stirred, 60 revs/min of sand mixer revolving speed；
(3) temperature drops to 130 DEG C, and the first curing agent is added, and stirs, 60 revs/min of sand mixer revolving speed；
(4) temperature drops to 110 DEG C, and outermost resin and outer layer catalyst is added, and stirs, 60 revs/min of sand mixer revolving speed；
(5) temperature drops to 95 DEG C, and aminated compounds is added, and stirs, 60 revs/min of sand mixer revolving speed；
(6) temperature drops to 80 DEG C, and outer layer curing agent is added, and stirs, 60 revs/min of sand mixer revolving speed；Temperature drops to 50 DEG C, out
Pot is obtained from outstanding proppant.
In the present embodiment, after which is impregnated with organic solvent, filtering takes filtering solution to test, in solution
The content of isocyano account for the 1/860 of solid content.
Embodiment 4
A kind of preparation method from outstanding proppant, comprising the following steps:
(2) prepare the raw material of following mass fraction: 100 parts of aggregate, 2 parts of outermost resin, 1.5 parts of the first resin, first are consolidated
0.7 part of agent, 1.5 parts of outer layer curing agent, 0.015 part of outer layer catalyst, 0.2 part of aminated compounds.Wherein aggregate selects 40/70
Quartz sand, outermost resin selection ethyl alcohol polymer, the first resin selection phenolic aldehyde tree, the first curing agent selection hexamethylenetetramine,
Outer layer curing agent selects toluene di-isocyanate(TDI), and outer layer catalyst selects dibutyl tin dilaurate, and aminated compounds selects three
Ethamine.
(2) aggregate is heated to be put into sand mixer after 130 DEG C, the first resin is added, stirred, 58 revs/min of sand mixer revolving speed；
(3) temperature drops to 110 DEG C, and the first curing agent is added, and stirs, 58 revs/min of sand mixer revolving speed；
(4) temperature drops to 90 DEG C, and outermost resin and outer layer catalyst is added, and stirs, 58 revs/min of sand mixer revolving speed；
(5) temperature drops to 80 DEG C, and aminated compounds is added, and stirs, 58 revs/min of sand mixer revolving speed；
(6) temperature drops to 70 DEG C, and outer layer curing agent is added, and stirs, 58 revs/min of sand mixer revolving speed；Temperature drops to 45 DEG C, out
Pot is obtained from outstanding proppant.
In the present embodiment, after which is impregnated with organic solvent, filtering takes filtering solution to test, in solution
The content of isocyano account for the 1/750 of solid content.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that: in this comparative example outer layer catalyst be added amount be 0.05 part.It should
After being impregnated with organic solvent from outstanding proppant, filtering takes filtering solution to test, the content of the isocyano in solution accounts for solid content
1/1660.
Comparative example 2
Comparative example 1 the difference from embodiment 1 is that: in this comparative example outer layer curing agent be added amount be 0.5 part (for outer layer
The 28% of resin quality number).Certainly after the outstanding proppant is impregnated with organic solvent, filtering takes filtering solution to test, in solution
The content of isocyano account for the 1/2880 of solid content.
Riverfrac treatment proppant in embodiment 1-4, comparative example 1,2 is tested, the performance of this proppant measured
Index is as shown in table 1:
Table 1
It illustrates:
1, suspension time refers to the maximum duration that proppant can freely suspend in water.
2, suspend than be evaluation proppant upper layer suspension amount Zhan total proppant in water percentage.
We use the mass ratio of proppant and water to evaluate for the case where 1:4 in test.Experimental method is in 300ml
Wide-mouth bottle in, with graduated cylinder measure 200ml water pour into wide-mouth bottle, precise 50g proppant pours into the wide-mouth bottle for having filled water
In, it closes the lid, firmly shakes 30 times up and down, it is static firmly to shake 30 times up and down after the same method after ten minutes, it is static
The proppant for filtering out upper layer suspension with filter paper afterwards, the quality that the proppant filtered out is weighed after drying is m (g), and b is compared in suspension
=m/50*100%.
3, mattress height is lower layer height of the 20g proppant in the 100ml graduated cylinder equipped with 100ml clear water.
Since laboratory can only do static suspension test, so the mattress height of lower layer is also evaluate suspendability one
Item important indicator.The amount of plastic wound packages 100ml water of 100ml is used in experiment, precise 20g proppant pours into the graduated cylinder for having filled water
In, tightly cover graduated cylinder mouth with the right hand, left hand is picked up graduated cylinder and is gently reversed 10 times up and down, it is static after ten minutes, according to same side
Method is reversed 10 times up and down, has vernier caliper to measure the bed height of lower layer support agent after static.
It 4, is to evaluate the overall target of proppant suspendability in clear water from outstanding composite index, by mattress height and suspension
Than codetermining, engineering significance is practical bulk density of the proppant in clear water, is worth the smaller phase being equivalent in water
To density with regard to smaller, then the suspension of proppant is better, suspension time is longer.
(b is suspension ratio, h is mattress height)
5, the test of apparent density, bulk density, percentage of damage and acid solubility is according to " SY/T 5108-2014 hydraulic fracturing
With gravel packing operations proppant performance test methods " it is tested.
Conclusion:
(1) come as can be seen from Table 1, after being impregnated from outstanding proppant with organic solvent, filtering takes filtering solution to survey
It tries, when the content of the isocyano in solution accounts for 1/1000 of solid content or more, what embodiment 1-4 was prepared hangs proppant certainly
Suspension ratio be all larger than 10%, suspension time and be both greater than 4 hours, suspendability is good, and the pressure break that can preferably meet deep-well is wanted
It asks.
(2) it can be seen that come from the data in table 1, when static, the certainly outstanding proppant in embodiment 1-4 is on upper layer
There is a certain amount of proppant that left floating.
(3) in general, the roughing sand of different size, original pottery and their mattress height all < from outstanding proppant
30mm；And in embodiment 1-4, the mattress height of proppant all > 30mm, therefore in static state, in fact from outstanding proppant
It is that the state to suspend with a kind of half is deposited in liquid bottom, once liquid flows, these proppants can suspend.
(4) as can be seen from Table 1, existing pressure break branch can be met or exceeded from outstanding proppant in embodiment 1-4
The indices for supportting agent, can meet use demand.
(5) embodiment 1 and comparative example 1, comparative example 2 are compared, it was therefore concluded that: it is soaked from outstanding proppant with organic solvent
After bubble, filtering takes filtering solution to test, when the content of the isocyano in solution accounts for 1/1000 or less solid content, proppant
Suspension ratio, suspension time be substantially reduced, the decline of the suspendability of proppant.
Claims (15)
1. a kind of preparation method from outstanding proppant, it is characterised in that: after certainly outstanding proppant is impregnated with organic solvent, filtering is taken
Filtering solution is tested, and the content of the isocyano in solution accounts for the one thousandth of solid content or more；The system from outstanding proppant
It is standby the following steps are included:
(1) prepare aggregate, inner membrance material and outer membrane material, outer membrane material includes outermost resin, outer layer catalyst and outer layer solidification
Agent；
(2) aggregate is heated to 80-160 DEG C, inner membrance material is added, stirring, the revolving speed of stirring is at 50-100 revs/min；
(3) temperature drops to 55-110 DEG C, is added outermost resin and outer layer catalyst, stirring, and the revolving speed of stirring turns in 50-100/
Point；
(4) temperature drops to 40-90 DEG C, outer layer curing agent is added, stirring, at 50-100 revs/min, temperature drops to the revolving speed of stirring
It 30-60 DEG C, takes the dish out of the pot, obtains from outstanding proppant.
2. a kind of preparation method from outstanding proppant according to claim 1, it is characterised in that: inner membrance material includes first
Resin and the first curing agent, the first resin quality number are the 0.5-9% of aggregate quality number, and the first curing agent mass fraction is
The 10-50% of first resin quality number；In step (2), aggregate is heated to 80-160 DEG C, the first resin is added, stirring is stirred
The revolving speed mixed is at 50-100 revs/min；Temperature drops to 65-130 DEG C, the first curing agent is added, stirring, the revolving speed of stirring is in 50-100
Rev/min.
3. a kind of preparation method from outstanding proppant according to claim 1, it is characterised in that: inner membrance material includes second
Resin, the second curing agent and internal layer catalyst, the second resin quality number are the 0.5-9% of aggregate quality number, the second solidification
Agent mass fraction is the 40-80% of the second resin quality number, and internal layer catalyst mass fraction is the second resin quality number
0.1-1%；In step (2), aggregate is heated to 80-160 DEG C, the second resin and internal layer catalyst, stirring is added, stirring turns
Speed is at 50-100 revs/min；Temperature drops to 65-130 DEG C, the second curing agent is added, stirring, the revolving speed of stirring is at 50-100 revs/min.
4. a kind of preparation method from outstanding proppant according to claim 3, it is characterised in that: the outer layer curing agent,
Second curing agent is isocyanates.
5. a kind of preparation method from outstanding proppant according to claim 3, it is characterised in that: the outer layer catalyst,
Internal layer catalyst be one of the organo-metallic compound of alkyls tin and/or the organo-metallic compound of alkyl ekalead or
It is several.
6. according to a kind of described in any item preparation methods from outstanding proppant of claim 3-5, it is characterised in that: the outer layer
Resin, the second resin are polyalcohols resin；The equivalent of outermost resin hydroxyl is 60-300, the mass fraction of outer layer curing agent
For the 40-80% of outermost resin mass fraction.
7. a kind of preparation method from outstanding proppant according to claim 6, it is characterised in that: outermost resin mass fraction
For the 0.5-9% of aggregate quality number, outer layer catalyst mass fraction is the 0.1-1% of outermost resin mass fraction.
8. a kind of preparation method from outstanding proppant according to claim 7, it is characterised in that: outer membrane material further includes amine
Class compound, the mass fraction of aminated compounds are the 10-20% of outermost resin mass fraction.
9. a kind of preparation method from outstanding proppant according to claim 8, it is characterised in that: the certainly outstanding proppant
Preparation the following steps are included:
(1) preparing aggregate, inner membrance material and outer membrane material, outer membrane material includes outermost resin, outer layer catalyst, outer layer curing agent
And aminated compounds；
(2) aggregate is heated to 80-160 DEG C, inner membrance material is added, stirring, the revolving speed of stirring is at 50-100 revs/min；
(3) temperature drops to 55-110 DEG C, is added outermost resin and outer layer catalyst, stirring, and the revolving speed of stirring turns in 50-100/
Point；
(4) temperature drops to 50-100 DEG C, and aminated compounds is added, is stirred 10-20 seconds；
(5) temperature drops to 40-90 DEG C, outer layer curing agent is added, stirring, at 50-100 revs/min, temperature drops to the revolving speed of stirring
It 30-60 DEG C, takes the dish out of the pot, obtains from outstanding proppant.
10. a kind of preparation method from outstanding proppant according to claim 6, it is characterised in that: the choosing of polyalcohols resin
With one of polymer such as ethyl alcohol, ethylene glycol, propylene glycol, glycerine, propyl alcohol or several.
11. a kind of preparation method from outstanding proppant according to claim 4, it is characterised in that: isocyanates is selected
Toluene di-isocyanate(TDI), methylenediphenyl diisocyanates, isophorone diisocyanate, methyl diphenylene diisocyanate
One of or it is several.
12. a kind of preparation method from outstanding proppant according to claim 5, it is characterised in that: alkyls tin it is organic
Metallic compound specifically selects dibutyl tin dilaurate, tributyl tin, and the organo-metallic compound of alkyl ekalead is specifically selected
Lead tetraethide, isooctyl acid lead.
13. a kind of preparation method from outstanding proppant according to claim 8 or claim 9, it is characterised in that: the amine chemical combination
Object is one of diethylenetriamine, triethylamine, ethamine, triethylene tetramine, ethylenediamine or several.
14. a kind of preparation method from outstanding proppant according to claim 2, it is characterised in that: first resin point
At least having containing the two or more groups in epoxy group, phenolic hydroxyl group, carbonyl, amide groups, amino, isocyanate group in minor structure
The average molecular weight of machine macromolecular substances, the first resin is greater than 100.
15. a kind of preparation method from outstanding proppant according to claim 1-5, it is characterised in that: the bone
Material selects quartz sand, haydite, Artificial Ceramic matter sand, organic synthesis sand or organo-mineral complexing material sand.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811159440.6A CN109385261A (en) | 2018-09-30 | 2018-09-30 | A kind of preparation method from outstanding proppant |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811159440.6A CN109385261A (en) | 2018-09-30 | 2018-09-30 | A kind of preparation method from outstanding proppant |
Publications (1)
| Publication Number | Publication Date |
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Family
ID=65419177
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111004619A (en) * | 2019-11-22 | 2020-04-14 | 中国石油天然气股份有限公司 | Self-heating and self-generating proppant and preparation method and application method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104797681A (en) * | 2012-09-25 | 2015-07-22 | 优选技术有限责任公司 | Coated and cured proppants |
| US20160333259A1 (en) * | 2015-05-13 | 2016-11-17 | Preferred Technology, Llc | High performance proppants |
| US20170058190A1 (en) * | 2009-10-20 | 2017-03-02 | Self-Suspending Proppant Llc | Proppants for hydraulic fracturing technologies |
-
2018
- 2018-09-30 CN CN201811159440.6A patent/CN109385261A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170058190A1 (en) * | 2009-10-20 | 2017-03-02 | Self-Suspending Proppant Llc | Proppants for hydraulic fracturing technologies |
| CN104797681A (en) * | 2012-09-25 | 2015-07-22 | 优选技术有限责任公司 | Coated and cured proppants |
| US20160333259A1 (en) * | 2015-05-13 | 2016-11-17 | Preferred Technology, Llc | High performance proppants |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111004619A (en) * | 2019-11-22 | 2020-04-14 | 中国石油天然气股份有限公司 | Self-heating and self-generating proppant and preparation method and application method thereof |
| CN111004619B (en) * | 2019-11-22 | 2022-02-01 | 中国石油天然气股份有限公司 | Self-heating and self-generating proppant and preparation method and application method thereof |
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Application publication date: 20190226 |