CN109181675A - A kind of preparation method of overlay film backing material - Google Patents
A kind of preparation method of overlay film backing material Download PDFInfo
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- CN109181675A CN109181675A CN201811161723.4A CN201811161723A CN109181675A CN 109181675 A CN109181675 A CN 109181675A CN 201811161723 A CN201811161723 A CN 201811161723A CN 109181675 A CN109181675 A CN 109181675A
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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
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Abstract
The invention belongs to the fluid minerals production technique such as petroleum, natural gas and shale gas fields, specifically disclose a kind of preparation method of overlay film backing material, include the following steps, aggregate is heated to 180-230 DEG C by (1), and the aggregate after heating is stirred mixing；(2) temperature is down to 75-200 DEG C, and inner layer resin stirring is added, adds the curing agent of inner layer resin, and stir, and forms interior coat；(3) temperature is down to 65-190 DEG C, stirs after drag reducer is added, and drag reducer quality is the 0.8-2% of aggregate；(4) temperature is down to 40-130 DEG C, and the curing agent of catalyst, outermost resin, amines additives and outermost resin is added, and stirring forms outer coat；(5) temperature is down to 30-70 DEG C, takes the dish out of the pot, and control low-density overlay film backing material apparent density range is 1.05-2.60g/cm3.The good guide performance of overlay film backing material made from this preparation method, good from suspendability, frictional resistance is low.
Description
Technical field
The invention belongs to the fluid minerals production technique field such as petroleum, natural gas and shale gas more particularly to a kind of overlay films
The preparation method of backing material.
Background technique
Hydraulic fracturing technology at home and abroad comparative maturity, petroleum fracturing propping agent is as essential in fracturing process
One of article, performance superiority and inferiority will directly influence fracturing effect, and apparent density is to evaluate the important finger of proppant performance
One of mark, apparent density is lower, and it is lower relative to the relative density of fracturing fluid, after proppant is mixed with pressure break carrying liquid, depending on
The lower density the easier to suspend in fracturing fluid, to greatly reduce the rate of settling.It will pump farther in pumping procedure.
High pumping pressure pumps fluid into well, while rock stratum of splitting is to allow hydrocarbons preferably to pass through.However, removing non-pressure
It keeps, the aperture otherwise newly formed is closed.In order to open and keep path, support is injected simultaneously during pumping fluid
Agent, support needed for keeping aperture with generation.When forming crack, biography when proppant passes through release hydraulic pressure in the slurry
It passs, proppant forms the filling or support for staying open crack herein.
With the development that domestic petroleum fracturing propping agents produce, miscellaneous proppant emerges one after another, such as covers
Film proppant.And for domestic fracturing technology mainly based on quartz sand and haydite, quartz sand is mainly used in the low closure of shallow-layer at present
The fracturing work of pressure well, haydite is mainly used in middle-deep well fracturing technology, but the resistant to breakage ability of quartz sand and haydite is equal
It is limited, it is difficult to adapt to hyperbaric environment.And overlay film proppant is by enhancing the intensity of proppant in aggregate surface overlay film, to improve
Proppant resists broken ability.Currently, the coating film of overlay film proppant common are phenolic resin film, epoxy resin film at present
With urethane resin film etc..
Present aggregate surface cladding phenolic resin film, epoxy resin film and urethane resin film etc. are primarily to improve branch
The intensity of agent is supportted, so substantially to consider how that improving resin film (covers phenolic resin film, epoxy resin film and poly- ammonia at present
Ester resin film etc.) intensity, but the suspendability of proppant is not improved, is applied using this kind of overlay film proppant pressure break
Working hour usually requires preparing the carrying liquid with viscoelasticity, and traditional carrying liquid making method is that a large amount of increase is added in water
The viscoelasticity that thick dose (substances such as guar gum) increase its own enables overlay film proppant to suspend in carrying liquid, but its disadvantage
It is that will lead to that pressure break higher cost, reservoir damage are serious, pollute the environment after addition thickener, therefore be badly in need of one now
The proppant that kind can suspend in clear water.
Existing proppant can be in water from there are two main classes the technology of suspension, first is that on aggregate quartz sand or haydite surface
Overlay film layer of material, this material are mainly some water-soluble high-molecular materials, such as polyacrylamide, carboxymethyl cellulose, are gathered
Acrylic acid, guar gum, natural plant gum etc..These materials are met water energy and are expanded rapidly, and the viscosity that can dissolve into increase water in water reaches outstanding
Floating purpose.The technology for not changing suspension fundamentally from suspended prop of this technology, only thickener overlay film
On aggregate, environmental issue is not solved, cost is reduced without really realizing, increases production and improves productivity.Another technology is to change
The apparent density of aggregate makes the haydite or resin beads of extremely-low density.Such product is able to achieve really half to suspend in water,
The rate of settling of proppant in water is reduced, but since apparent density to be greatly lowered, production cost is greatly increased, and
The performance of proppant, such as broken, sour molten, water conservancy diversion performance can be substantially reduced.And the production efficiency of resin beads is low, it is at high cost etc.
Defect also limits its popularization and use.And although above-mentioned proppant can be realized from suspension in water, but carry the frictional resistance of liquid
It is enhanced, so that proppant could be pumped into corresponding position by applying the higher pump pressure of man-hour requirement, improves
Construction cost.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of overlay film backing material, overlay film branch made from this preparation method
It is the good guide performance of timbering material, good from suspendability.
In order to achieve the above object, base case of the invention are as follows: a kind of preparation method of overlay film backing material, including with
Lower step,
(1) aggregate is heated to 80-230 DEG C, the aggregate after heating is stirred mixing；
(2) temperature is down to 75-200 DEG C, and the curing agent of inner layer resin and inner layer resin is added, and stirs, and forms interior coating
Layer；
(3) temperature is down to 65-190 DEG C, stirs after drag reducer is added, and drag reducer quality is the 0.8-2% of aggregate；
(4) temperature is down to 40-130 DEG C, and the curing agent of catalyst, outermost resin, amines additives and outermost resin is added,
Stirring forms outer coat；
(5) temperature is down to 30-70 DEG C, takes the dish out of the pot, and control low-density overlay film backing material apparent density range is 1.05-2.60g/
cm3。
The beneficial effect of this base case is: adding drag reducer in step (3), makes overlay film backing material Surface Creation
Inner layer resin film and outermost resin film between contain drag reducer, in overlay film backing material and clear water mixed process, internal layer tree
Part draft reduction material between adipose membrane and outermost resin film can dissolve into load fluid rapidly, reduce the frictional resistance of clear water, make overlay film branch
Timbering material in clear water also have good guide performance, reach corresponding technical requirements, compared with the existing technology for we
Case eliminates the auxiliary additives such as slippery water, reduces construction cost, simplifies construction technology, reduces equipment requirement.Due to
Drag reducer adds in internal layer resin film, such as not too large from the variation of other performances such as suspendability and sphericity, and in order to
Ensure the drag reducing efficiency of overlay film backing material, institute's drag reducer quality is the 0.8-2% of aggregate, and the quality of drag reducer addition and addition exist
Overlay film backing material surface enables overlay film backing material to follow and carries the corresponding destination of liquid arrival compared to being increased.Together
When this programme in overlay film backing material rate of dissolution it is fast, can be dissolved in clear water in 3-15s, construction when overlay film branch
Timbering material is quickly dissolved in clear water, and huge discharge operation may be implemented, greatly improve working efficiency.
Inner layer resin and outermost resin is successively added in step (2) and step (4) in this programme, so that made from this programme
Overlay film backing material includes internal layer and outer layer two layers of resin film, and aggregate is enable to be coated completely, and inner layer resin film can be protected
The integral strength of overlay film backing material is demonstrate,proved, guarantees the resistant to breakage rate of overlay film backing material.The outermost resin film surface of generation has
Nanoscale protrusion, these protrusions extend in the surface of proppant particles, and protrusion will increase the buoyancy of proppant, reduce proppant
Whole volume density and apparent density, improve proppant from suspendability.
In work progress, the reserved group in the resin film on backing material surface can react rapidly generation largely after meeting water
Gas molecules, these gas molecules or are enclosed in resin film to expand against resin membrane body stage and thicken and increase support
The equivalent diameter of material granule body, or be attached to the extension of backing material surface stage or be gathered in backing material resin film and water
The gas blanket of one layer of package backing material granule is formed on the interface of body contact, this gas blanket is between backing material granule
Formation stages are connected to and the result closed causes simple grain backing material to form more loose cotton wadding in water body to gather shape, this
Sample is greatly lowered the relative density of backing material in water, so as to make backing material suspend in water, realizes and uses
Clear water (carries liquid certainly and is also not only limited to clear water, can also be the carrying liquid added with thickener) as carrying liquid.Backing material exists
When moving in water, the protrusion of the curved surface on backing material resin film can reduce the backing material rate of settling in water；Part settles
The backing material accumulated to water bottom reduces the tight of backing material settled layer because of the more protrusion of its surface resin film
Solidity, intergranular water body amount is more compared with conventional particle stack, and then when water body can be more the fluidity with very little
Add and easily push the separation of its congeries and movement, realizes that backing material preferably suspends in water, make the support in this programme
While material meets the basic pressure break of industry and requires, the thickeners such as addition guar gum are not needed in fracturing process, are dropped significantly
Low cost has simplified fracturing unit and technique, reduces the pollution to environment, and may be implemented using clear water as carrying liquid
Huge discharge operation, improves working efficiency.
Apparent density range is 1.05-2.60g/cm3Overlay film backing material comprehensive bulk density can be formed in clear water
In 0.6~1.3g/cm3Solid-liquid mixing, when such solid-liquid mixing is applied certain mechanical stirring momentum, overlay film
Backing material can be more evenly distributed in clear water, and the overlay film branch in mixed liquor can be made when mixed liquor reaches certain flow rate
Timbering material compared to traditional overlay film and can support from the reservoir fracture that suspended state carries out under long distance delivery to recovery well
Material reaches slot height distribution support of totally cleaving, and improves the rate of growth of petroleum etc..
Further, the drag reducer preparation step is as follows, as mass fraction the water of addition 85-93%, and the third of 5-10%
Acrylamide and acrylamide derivative, the acrylic acid and methacrylic acid of 0.5-2%, the 2- acrylamide -2- methyl-prop of 1-5%
The methylpropene sodium sulfonate of sulfonic acid and 0.5-3% stirs 150-220rpm, and is warming up to 40-70 DEG C, and above-mentioned gross mass is added
The initiator of 0.3-2%, reacts through 3-40min, is down to room temperature.
Further, the mass fraction of raw material is respectively 100 parts of aggregate, and 0.25-5 parts of inner layer resin, outermost resin 0.25-5
Part, the amines additives quality is the 1/100-20/100 of outermost resin quality, and catalyst quality is outermost resin quality
1/1000-1/100。
Further, the inner layer resin is the one or more of polyalcohols resin, epoxy resin and phenolic resin, described
Outermost resin is polyalcohols resin, and the equivalent of polyalcohols resin hydroxyl is 60-300, and the curing agent of outermost resin is isocyanide
Esters of gallic acid curing agent, Isocyanates curing agent quality are the 40-80% of polyalcohols resin.Applicant is in long-term practice
It was found that the control of polyalcohols resin, isocyanates produces the performance entirely different with current material performance in above range,
Firstly, polyalcohols resin reacts the urethane resin film for generating and having micro protrusion with isocyanate groups, due to further including
Amines additives, polyalcohols resin can be to the anti-of isocyanate groups with amines additives in isocyanate groups reaction process
Facilitation should be played, makes to generate a large amount of mutually isolated bubbles inside urethane resin film, bubble is closed in polyurethane tree
Inside adipose membrane, so that bubble forms a large amount of protrusion in polyurethane resin film surface, bump sizes are between 100~500nm, protrusion
In coating layer surface random distribution, there is the random distribution of heterogencity in the surface resin film of single particle body, it is equal for converting
The surface of every 100 square micron has 1~40 or so protrusion under one distribution, reduces apparent density and volume density, improves
It is from suspendability.Simultaneously because the equivalent of polyalcohols resin hydroxyl is 60-300, isocyanate is at least polyalcohol
The 40% of resinoid also remains part after isocyanates and whole polyalcohols resin reaction generation urethane resin films
Isocyanate groups are not reacted, low when this programme so that there is also isocyanate groups in urethane resin film at this time
Remaining isocyanate groups are reacted with water and can be surrounded in the chain element of resin film microcosmic small when density proppant meets water
Gas is generated in space body, this small quantity gas is gradually increased volume under the promotion of reaction energy and forms bubble, and pushes tree
Adipose membrane increases in the radial dimension of proppant particles, reaches the dilation for coating layer surface most preferably, to further reduced
The apparent density and volume density of proppant, while isocyanate is at most the 80% of polyalcohols resin, makes the bubble generated
Volume be unlikely to too big and bubble caused to be easy breakage etc., and make the quantity of the bubble generated will not be excessive, make a large amount of gas
It being all mutually isolated between bubble, causing air bubble intensity to reduce without there are problems that bubble contacts with each other.
Further, the polyalcohols resin is the polymer one or several kinds of ethylene glycol, propylene glycol, glycerine.
Further, Isocyanates curing agent is toluene di-isocyanate(TDI), methylenediphenyl diisocyanates, different Fo Er
One or more of ketone diisocyanate, methyl diphenylene diisocyanate.Polyalcohols resin and above-mentioned several solidifications
Dosage form generating polyurethane resin film is coated on the surface of aggregate, and the surface of the urethane resin film generated has several nanoscales
Protrusion, the volume density and apparent density of overlay film backing material can be reduced.
Further, the catalyst is one or more of alkyls tin compound and/or alkyls lead compound
Mixture.
Further, alkyls tin compound is one of dibutyl tin dilaurate, tributyl tin or several mixed
Object is closed, alkyls lead compound is one of lead tetraethide, isooctyl acid lead or several mixtures.Above-mentioned several catalyst
Cost performance it is high, solidification rate and the intensity performance of coat can be accelerated.
Further, amines additives be one of diethylenetriamine, triethylamine, ethamine, triethylene tetramine, ethylenediamine or
Person is a variety of.These types of amines additives facilitation effect is good, is conducive to the formation of protrusion.
Detailed description of the invention
Fig. 1 is the electron-microscope scanning figure of overlay film backing material in embodiment 1.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail:
Raw material is selected:
Aggregate selects the one or more of haydite, quartz sand, selects haydite as an example, haydite in present embodiment
Apparent density is 1.05~2.65g/cm3, circularity >=0.7, sphericity >=0.7, resistant to breakage rate≤3% (86mpa), acid solubility≤
5%, granularity is 20~140 mesh.
Outermost resin is polyalcohols resin, and inner layer resin is the one of polyalcohols resin, epoxy resin and phenolic resin
Kind is a variety of.
Polyalcohols resin is the polymer one or several kinds of ethylene glycol, propylene glycol, glycerine, polyalcohols resin hydroxyl
The equivalent of base is 60-300.
The curing agent of polyalcohols resin is Isocyanates curing agent, preferably toluene di-isocyanate(TDI), methylene two
One or more of phenyl diisocyanate, isophorone diisocyanate, methyl diphenylene diisocyanate.
The curing agent of epoxy resin is modified aromatic amine curing agent (T31), and the curing agent of phenolic resin is six methines
Tetramine.
Catalyst is the mixture of one or more of alkyls tin compound and/or alkyls lead compound, preferably
For one of dibutyl tin dilaurate, tributyl tin, lead tetraethide, isooctyl acid lead or several mixtures.
Amines additives select one of diethylenetriamine, triethylamine, ethamine, triethylene tetramine, ethylenediamine or more
Kind.
The mass fraction of raw material is respectively 100 parts of aggregate, 0.25-5 parts of inner layer resin, 0.25-5 parts of outermost resin, described
Drag reducer quality is the 0.8-2% of aggregate, and the amines additives quality is the 1/100-20/100 of outermost resin quality, catalysis
Agent quality is the 1/1000-1/100 of polyalcohols resin quality, and Isocyanates curing agent quality is outermost resin quality
40-80%.
Drag reducer, as mass fraction be added 85-93% water, the acrylamide and acrylamide derivative of 5-10%,
The acrylic acid and methacrylic acid of 0.5-2%, the 2- acrylamide-2-methyl propane sulfonic of 1-5% and the metering system of 0.5-3%
Sodium sulfonate stirs 150-220rpm, and is warming up to 40-70 DEG C, the initiator of above-mentioned gross mass 0.3-2% is added, through 3-40min
Reaction, is down to room temperature and obtains required drag reducer.Wherein initiator includes azo diisobutyl amidine hydrochloride, two isobutyl imidazoles of azo
Quinoline hydrochloride, azo dicyano valeric acid, azo dicyclohexyl formonitrile HCN one or more.
Embodiment 1
Taking apparent density is 1.05g/cm3, granularity be 100 parts of haydite of 20/40,175-185 DEG C is heated to, by the pottery of heating
Grain pours into inside bowl-type mulling pot, and 2 parts of epoxy resin stirrings are then added；Temperature is down to 150-160 DEG C, and 0.2 part of modification is added
Aromatic amine curing agent (T31) simultaneously stirs；Temperature is down to 140-150 DEG C, and 0.8 portion of drag reducer is added and is mixed；Temperature is down to
80-90 DEG C, 2 parts of glycol polymers and the stirring of 0.02 part of dibutyl tin dilaurate are added；Temperature is down to 70-80 DEG C, adds
Enter 0.2 part of ethylenediamine stirring；Temperature is down to 60-70 DEG C, and 0.8 part of toluene di-isocyanate(TDI) stirring is added；Temperature is down to 40-50 DEG C
It takes the dish out of the pot.Epoxy resin and modified aromatic amine curing agent generate inner layer resin film, and inner layer resin film is epoxy resin film；The third three
Alcohol, dibutyl tin dilaurate, diethylenetriamine and toluene di-isocyanate(TDI) generate outermost resin film, and outermost resin film is poly- ammonia
Ester resin film, as shown in Figure 1, overlay film backing material outer surface has nanoscale protrusion.
Embodiment 2
Taking apparent density is 1.65g/cm3, granularity be 100 parts of haydite of 30/50,220-230 DEG C is heated to, by the pottery of heating
Grain pours into inside bowl-type mulling pot, and 3 parts of phenolic resin stirrings are then added；Temperature is down to 190-200 DEG C, be added 0.6 part six times
Tetramine simultaneously stirs；Temperature is down to 180-190 DEG C, adds 1.2 parts of drag reducer mixing；Temperature is down to 120-130 DEG C, is added
4 parts of glycerine polymer and the stirring of 0.02 part of isooctyl acid lead；Temperature is down to 100-110 DEG C, and 0.2 part of triethylamine stirring is added；
Temperature is down to 90-100 DEG C, and 2 parts of methylenediphenyl diisocyanates stirrings are added；Temperature is down to 60-70 DEG C and takes the dish out of the pot.
Embodiment 3
Taking apparent density is 2.05g/cm3, granularity be 100 parts of haydite of 40/70, the haydite of heating is poured into bowl-type mulling pot
Then 2 parts of ethylene glycol polymers and the stirring of 0.02 part of tributyl tin are added in the inside；Temperature is down to 75-85 DEG C, is added 0.6 part
Isophorone diisocyanate simultaneously stirs；Temperature is down to 65-75 DEG C, adds 1.6 parts of drag reducer mixing；Temperature is down to 55-65
DEG C, 4 parts of glycerine polymer and the stirring of 0.02 part of isooctyl acid lead are added；Temperature is down to 45-55 DEG C, and 0.2 part of triethylamine is added
Stirring；Temperature is down to 35-45 DEG C, and 2.4 parts of methylenediphenyl diisocyanates stirrings are added；Temperature is down to 30-40 DEG C and takes the dish out of the pot.
Embodiment 4
Taking apparent density is 2.65g/cm3, granularity be 100 parts of haydite of 70/140, the haydite of heating is poured into bowl-type mulling
Then 2 parts of ethylene glycol polymers and the stirring of 0.02 part of tributyl tin are added in pot the inside；Temperature is down to 130-140 DEG C, is added
0.6 part of isophorone diisocyanate simultaneously stirs；Temperature is down to 120-130 DEG C, adds 2 parts of drag reducer mixing；Temperature is down to
100-110 DEG C, 4 parts of glycerine polymer and the stirring of 0.02 part of isooctyl acid lead are added；Temperature is down to 90-100 DEG C, is added 0.2
Part triethylamine stirring；Temperature is down to 80-90 DEG C, and 3.2 parts of methylenediphenyl diisocyanates stirrings are added；Temperature is down to 50-
60 DEG C take the dish out of the pot.
Comparative example 1
Taking apparent density is 1.05g/cm3, granularity be 100 parts of haydite of 20/40,175-185 DEG C is heated to, by the pottery of heating
Grain pours into inside bowl-type mulling pot, and 2 parts of epoxy resin stirrings are then added；Temperature is down to 150-160 DEG C, and 0.2 part of modification is added
Aromatic amine curing agent (T31) simultaneously stirs；Temperature is down to 140-150 DEG C, adds 0.8 part of drag reducer mixing；Temperature is down to 80-
90 DEG C, 2 parts of epoxy resin stirrings are added；Temperature is down to 70-80 DEG C, and 0.2 part of ethylenediamine stirring is added；Temperature is down to 60-70 DEG C,
0.2 part of modified aromatic amine curing agent (T31) stirring is added；Temperature, which is down to 40-50 DEG C and takes the dish out of the pot, (obtains overlay film backing material
Inner layer resin film and outermost resin film are epoxy resin film).
Comparative example 2
Taking apparent density is 1.65g/cm3, granularity be 100 parts of haydite of 30/50,220-230 DEG C is heated to, by the pottery of heating
Grain pours into inside bowl-type mulling pot, and 3 parts of phenolic resin stirrings are then added；Temperature is down to 190-200 DEG C, be added 0.6 part six times
Tetramine simultaneously stirs；Temperature is down to 180-190 DEG C, adds 0.8 part of drag reducer mixing；Temperature is down to 120-130 DEG C, is added
4 parts of phenolic resin stirrings；Temperature is down to 100-110 DEG C, and 0.2 part of triethylamine stirring is added；Temperature is down to 90-100 DEG C, is added
0.8 part of hexamethylenetetramine simultaneously stirs；Temperature be down to 60-70 DEG C take the dish out of the pot (obtain overlay film backing material inner layer resin film and
Outermost resin film is phenolic resin film).
Comparative example 3
The difference of this comparative example and embodiment 1, which is only that, is added without ethylenediamine (amines additives).
Comparative example 4
The difference of this comparative example and embodiment 1, which is only that, is added without drag reducer.
Comparative example 5
The difference of this comparative example and embodiment 1 is only that the mass fraction of drag reducer is 0.5.
Comparative example 6
The difference of this comparative example and embodiment 1 is only that the mass fraction of drag reducer is 2.5.
Comparative example 7
It buys from the ceramsite propping agent of 20/40 specification of Luoyang Zhong Tai Industrial Co., Ltd. and is tested for the property.
Comparative example 8
The difference of this comparative example and embodiment 1 is only that the mass fraction of toluene di-isocyanate(TDI) is 0.7 part.
Comparative example 9
The difference of this comparative example and embodiment 4 is only that the mass fraction of methylenediphenyl diisocyanates is 3.6 parts.
Raw material parts is mass fraction in above embodiments and comparative example.
The main performance index and measuring method of above-mentioned overlay film backing material:
Examination criteria: molten about apparent density, bulk density, circle/sphericity, percentage of damage and acid in above-described embodiment and comparative example
The test of Xie Du according to " SY/T 5108-2014 hydraulic fracturing and gravel packing operations proppant performance test methods " into
Row test.
The overlay film backing material of above-described embodiment and comparative example is done to the survey of mattress height, suspend ratio and suspension time simultaneously
Examination.
1. suspension ratio
It suspends than being that suspension amount in upper layer accounts for the percentage of total overlay film backing material to evaluation overlay film backing material in water.
We use the mass ratio of overlay film backing material and water to evaluate for the case where 1:4 in test.Experimental method is
In the wide-mouth bottle of 300ml, 200ml water is measured with graduated cylinder and is poured into wide-mouth bottle, precise 50g overlay film backing material pours into dress
In the wide-mouth bottle of water, close the lid, firmly shake up and down for 30 times, it is static after ten minutes, exert oneself up and down after the same method
It shakes 30 times, filters out the overlay film backing material of upper layer suspension after static with filter paper, the overlay film branch filtered out is weighed after drying
The quality of timbering material is m (g), and b=m/50*100% is compared in suspension.
2. mattress height
Mattress height is lower layer height of the 20g overlay film backing material 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 overlay film backing material, which pours into, has filled water
In graduated cylinder, 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
Method up and down reverse 10 times, there is vernier caliper to measure the bed height of lower layer's overlay film backing material after static.
3. suspension time
Suspension time refers to the maximum duration that can freely suspend in water.
We use the mass ratio of overlay film backing material and water to evaluate for the case where 1:4 in test.Experimental method is
In the wide-mouth bottle of 300ml, 200ml water is measured with graduated cylinder and is poured into wide-mouth bottle, precise 50g overlay film backing material pours into dress
In the wide-mouth bottle of water, close the lid, firmly shake up and down for 30 times, it is static after ten minutes, exert oneself up and down after the same method
It shakes 30 times, the maximum duration that then the static placement of wide-mouth bottle, timing measuring overlay film backing material freely suspend in water.
Embodiment 1- embodiment 4, the Example Test Data of comparative example 1- comparative example 9 are as follows:
" certainly outstanding composite index " is the overall target for evaluating overlay film backing material suspendability in clear water in upper table, by sinking
Bed height and the ratio that suspends codetermine, and engineering significance is practical bulk density of the overlay film backing material in clear water, and value is got over
The small relative density being equivalent in water is with regard to smaller, then the suspension of overlay film backing material is better, suspension time is longer.
(b is suspension ratio, h is mattress height)
Embodiment 1 and comparative example 1 are compared, embodiment 2 and comparative example 2 compare, and wherein embodiment 1 and embodiment 2 is outer
Layer resin film is urethane resin film, and the outermost resin film of comparative example 1 and comparative example 2 is not urethane resin film, root
According to upper table, can release, the suspension time of embodiment 1 and embodiment 2 is respectively higher than the suspension time of comparative example 1 and comparative example 2,
The certainly outstanding composite index of embodiment 1 and embodiment 2 is respectively smaller than comparative example 1 and comparative example 2, that is, embodiment 1 and 1 phase of comparative example
More preferable than from suspendability, embodiment 2 is more preferable from suspendability compared with comparative example 2, it can be seen that, urethane resin film can
Improve overlay film backing material from suspendability, it is specific for during the preparation process, polyurethane resin film surface can generate several
Protrusion, the isocyanates root (Isocyanates curing agent offer) when meeting water in urethane resin film can also react life with water
At bubble, so improve overlay film backing material from suspendability.
According to upper table, compared with comparative example 7, suspension time and the ratio that suspends are significantly increased embodiment 1, from outstanding composite index
It is substantially reduced, i.e., this programme greatly improves for conventional proppants from suspendability.
Embodiment 1 is only in outermost resin film compared with comparative example 3 containing ethylenediamine (amines additives), according to upper table,
Concluding that overlay film backing material is compared with comparative example 3 made from embodiment 1, suspension time and the ratio that suspends are significantly increased, from
Outstanding composite index is substantially reduced, i.e. overlay film backing material is significantly improved from suspendability, illustrates overlay film branch made from embodiment 1
Supportting material surface has more protrusions, and can release amines additives has the formation of overlay film backing material surface bulge
Preferable facilitation makes greatly improving from suspendability for overlay film backing material by amines additives.
Embodiment 1 and comparative example 4 are compared, it was therefore concluded that: after being added to drag reducer from suspension covering material
Drag reducing efficiency is substantially better than the drag reducing efficiency from suspension covering material for being not added with drag reducer, can be substantially reduced by adding drag reducer
From the frictional resistance of suspension covering material, its guide performance is promoted.
Embodiment 1 and comparative example 5 are compared, it was therefore concluded that: the overlay film branch when the mass fraction of drag reducer is less than 0.8
The drag reducing efficiency of timbering material substantially reduces, and corresponding technique requirement is not achieved.
Embodiment 1 and comparative example 6 are compared, it was therefore concluded that: when the mass fraction of drag reducer is greater than 2, overlay film is supported
The resistant to breakage of material, which is filtered, and acid is molten is all increased, and reduces the performance of overlay film backing material product, while suspension can also be deteriorated,
Reduce overlay film backing material from suspendability.
Comparative example 8 is distinguished compared with Example 1 is that the mass fraction of toluene di-isocyanate(TDI) is 0.7 part, in comparative example 8
Toluene di-isocyanate(TDI) (isocyanates) and the quality accounting of glycerine polymer (polyalcohols resin) areThe quality accounting of isocyanates and polyalcohols resin in embodiment 1 is
The quality of isocyanates is less than the 40% of polyalcohols resin quality i.e. in comparative example 8, according to upper table, it can be deduced that comparative example 8
The suspension time of backing material and suspension are decreased obviously than, are significantly improved from outstanding composite index, i.e., comparative example 8 compares embodiment
It is substantially reduced for 1 from suspendability, when illustrating that the quality of isocyanates is less than the 40% of polyalcohols resin quality, fid
Material is substantially reduced from suspendability.
Comparative example 9 is distinguished compared with Example 4 is that the mass fraction of toluene di-isocyanate(TDI) is 3.6 parts, in comparative example 9
Methylenediphenyl diisocyanates (isocyanates) and the quality accounting of glycerine polymer (polyalcohols resin) areThe quality accounting of isocyanates and polyalcohols resin in embodiment 4 is
The quality of isocyanates is greater than the 80% of polyalcohols resin quality i.e. in comparative example 9, according to upper table, it can be deduced that comparative example 9
The suspension time of backing material and suspension are decreased obviously than, are significantly improved from outstanding composite index, i.e., comparative example 9 compares embodiment
It is substantially reduced for 4 from suspendability, when illustrating that the quality of isocyanates is greater than the 80% of polyalcohols resin quality, fid
Material is substantially reduced from suspendability.
To sum up, the quality of isocyanates is controlled in the range of polyalcohols resin quality 40%-80% in this programme
When, overlay film backing material all has preferably from suspendability, meets overlay film backing material in clear water from the requirement to suspend.And
When the quality of isocyanates is lower than polyalcohols resin quality less than 40% or greater than 80%, overlay film backing material suspends certainly
Performance is decreased obviously, it is difficult to meet the requirement to suspend in clear water.
What has been described above is only an embodiment of the present invention, and the common sense such as well known specific structure and characteristic are not made herein in scheme
Excessive description.It, without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these also should be considered as protection scope of the present invention, these all will not influence what the present invention was implemented
Effect and patent practicability.The scope of protection required by this application should be based on the content of the claims, in specification
The records such as specific embodiment can be used for explaining the content of claim.
Claims (9)
1. a kind of preparation method of overlay film backing material, it is characterised in that: include the following steps,
(1) aggregate is heated to 80-230 DEG C, the aggregate after heating is stirred mixing；
(2) temperature is down to 75-200 DEG C, and the curing agent of inner layer resin and inner layer resin is added, and stirs, and forms interior coat；
(3) temperature is down to 65-190 DEG C, stirs after drag reducer is added, and drag reducer quality is the 0.8-2% of aggregate；
(4) temperature is down to 40-130 DEG C, and the curing agent of catalyst, outermost resin, amines additives and outermost resin is added, stirs
It mixes, forms outer coat；
(5) temperature is down to 30-70 DEG C, takes the dish out of the pot, and control low-density overlay film backing material apparent density range is 1.05-2.60g/cm3。
2. a kind of preparation method of overlay film backing material according to claim 1, it is characterised in that: the drag reducer preparation
Steps are as follows, and the water of 85-93%, the acrylamide and acrylamide derivative of 5-10%, 0.5-2% are added as mass fraction
Acrylic acid and methacrylic acid, the 2- acrylamide-2-methyl propane sulfonic of 1-5% and the methylpropene sodium sulfonate of 0.5-3%,
150-220rpm is stirred, and is warming up to 40-70 DEG C, the initiator of above-mentioned gross mass 0.3-2% is added, is reacted through 3-40min, is dropped
To room temperature.
3. a kind of preparation method of overlay film backing material according to claim 1, it is characterised in that: the mass fraction of raw material
Respectively 100 parts of aggregate, 0.25-5 parts of inner layer resin, 0.25-5 parts of outermost resin, the amines additives quality is outer layer tree
The 1/100-20/100 of lipid amount, catalyst quality are the 1/1000-1/100 of outermost resin quality.
4. a kind of preparation method of overlay film backing material according to claim 1, it is characterised in that: the inner layer resin is
Polyalcohols resin, epoxy resin and phenolic resin it is one or more, the outermost resin is polyalcohols resin, polyalcohol
The equivalent of resinoid hydroxyl is 60-300, and the curing agent of outermost resin is Isocyanates curing agent, Isocyanates curing agent
Quality is the 40-80% of polyalcohols resin.
5. a kind of preparation method of overlay film backing material according to claim 4, it is characterised in that: the polyalcohols tree
Rouge is the polymer one or several kinds of ethylene glycol, propylene glycol, glycerine.
6. a kind of preparation method of overlay film backing material according to claim 4, it is characterised in that: isocyanates solidification
Agent is toluene di-isocyanate(TDI), methylenediphenyl diisocyanates, isophorone diisocyanate, two isocyanide of diphenyl methane
One or more of acid esters.
7. a kind of preparation method of overlay film backing material according to claim 1, it is characterised in that: the catalyst is alkane
The mixture of one or more of base class tin compound and/or alkyls lead compound.
8. a kind of preparation method of overlay film backing material according to claim 7, it is characterised in that: alkyls tin compound
For one of dibutyl tin dilaurate, tributyl tin or several mixtures, alkyls lead compound be lead tetraethide,
One of isooctyl acid lead or several mixtures.
9. a kind of preparation method of overlay film backing material according to claim 1, it is characterised in that: amines additives two
One or more of ethylene triamine, triethylamine, ethamine, triethylene tetramine, ethylenediamine.
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| CN201811161723.4A CN109181675A (en) | 2018-09-30 | 2018-09-30 | A kind of preparation method of overlay film backing material |
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| CN201811161723.4A CN109181675A (en) | 2018-09-30 | 2018-09-30 | A kind of preparation method of overlay film backing material |
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