CN109135721A - A kind of preparation process from suspension covering material - Google Patents
A kind of preparation process from suspension covering material Download PDFInfo
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- CN109135721A CN109135721A CN201811161859.5A CN201811161859A CN109135721A CN 109135721 A CN109135721 A CN 109135721A CN 201811161859 A CN201811161859 A CN 201811161859A CN 109135721 A CN109135721 A CN 109135721A
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/16—Catalysts
- C08G18/22—Catalysts containing metal compounds
- C08G18/24—Catalysts containing metal compounds of tin
- C08G18/242—Catalysts containing metal compounds of tin organometallic compounds containing tin-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/16—Catalysts
- C08G18/22—Catalysts containing metal compounds
- C08G18/26—Catalysts containing metal compounds of lead
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4829—Polyethers containing at least three hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/58—Epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
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 process from suspension covering material, include the following steps, aggregate is heated to 80-230 DEG C by (1), and 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 40-130 DEG C, and the curing agent of catalyst, outermost resin, amines additives and outermost resin is added, and stirring forms outer coat；(4) temperature is down to 35-90 DEG C, stirs after drag reducer is added, and the drag reducer quality is the 0.5-1.5% of aggregate；(5) temperature is down to 30-70 DEG C, takes the dish out of the pot, and controlling from suspension covering material apparent density range is 1.05-2.60g/cm3.From the good guide performance of suspension covering material, reduction frictional resistance good from suspendability made from this preparation process.
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 process of floating covering 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 process from suspension covering material, this preparation process is obtained from outstanding
It is the good guide performance of floating covering material, good from suspendability.
In order to achieve the above object, base case of the invention are as follows: a kind of preparation process from suspension covering material, including
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 coating
Layer；
(3) 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；
(4) temperature is down to 35-90 DEG C, stirs after drag reducer is added, and the drag reducer quality is the 0.5-1.5% of aggregate；
(5) temperature is down to 30-70 DEG C, takes the dish out of the pot, and controlling from suspension covering material apparent density range is 1.05-2.60g/cm3。
The beneficial effect of this base case is: adding drag reducer in step (4), makes to contain on the outermost resin film of production
There is drag reducer, from suspension covering material and clear water mixed process, the part between inner layer resin film and outermost resin film subtracts
Resistance material can dissolve into load fluid rapidly, reduce the frictional resistance of clear water, make also to have in clear water from suspension covering material good
Guide performance reaches corresponding technical requirements, compared with the existing technology for this programme eliminate the auxiliary additives such as slippery water,
Construction cost is reduced, construction technology is simplified, reduces equipment requirement.Since drag reducer addition is in outer layer resin film, such as
The amount of fruit drag reducer add excessively to will lead to other performances such as from suspendability and sphericity by large effect, so
In order to ensure the drag reducing efficiency from suspension covering material, drag reducer quality is the 0.5-1.5% of aggregate, the quality of drag reducer addition with
Addition, compared to decreasing, enables that carrying liquid is followed to reach corresponding destination from suspension covering material in internal layer resin film
While to other performances generate influence it is little.The rate of dissolution from suspension covering material in this programme is fast, in 3-15s
It can be dissolved in clear water, quickly be dissolved in clear water from suspension covering material in construction, huge discharge operation may be implemented, significantly
Improve work efficiency.
Inner layer resin and outermost resin is successively added in step (2) and step (3) in this programme, so that made from this programme
Include internal layer and outer layer two layers of resin film from suspension covering material, aggregate is enable to be coated completely, inner layer resin film can
Guarantee the integral strength from suspension covering material, guarantees the crushing strength from suspension covering material.The outermost resin film of generation
Surface has nanoscale protrusion, these protrusions extend in the surface of proppant particles, and protrusion will increase the buoyancy of proppant, reduces
The volume density and apparent density of proppant entirety, improve proppant from suspendability.
In work progress, the reserved group in outermost resin film can react rapidly a large amount of small point of gas of generation after meeting water
Son, these gas molecules or is enclosed in resin film to expand against resin membrane body stage and thicken and increases covering material particle
The equivalent diameter of body, or be attached to the extension of covering material surface stage or be gathered in what covering material resin film was contacted with water body
The gas blanket of one layer of package covering material granule, this gas blanket formation stages between covering material granule are formed on interface
Property be connected to and the result closed causes simple grain covering material to form more loose cotton wadding in water body to gather shape, thus significantly
Reduce the relative density of covering material in water, so as to make covering material suspend in water, realization use clear water as
Carry liquid (carry liquid certainly and be also not only limited to clear water, can also be the carrying liquid added with thickener).Covering material moves in water
When, the protrusion of the curved surface on covering material resin film can reduce the covering material rate of settling in water；Part is settled down to water body bottom
The covering material of portion's accumulation reduces the degree of packing of covering material settled layer, particle because of the more protrusion of its surface resin film
Between water body amount it is more compared with conventional particle stack, and then when water body even if with very little fluidity can more easily push away
The separation of its congeries and movement are moved, realizes that covering material preferably suspends in water, meets the covering material in this programme
While the basic pressure break of industry requires, the thickeners such as addition guar gum are not needed in fracturing process, greatly reduce cost, essence
Letter fracturing unit and technique reduce the pollution to environment, and huge discharge operation may be implemented using clear water as liquid is carried,
Improve working efficiency.
Apparent density range is 1.05-2.60g/cm3Comprehensive accumulation can be formed in pure clear water from suspension covering material
Density is in 0.6~1.3g/cm3Solid-liquid mixing, when such solid-liquid mixing is applied certain mechanical stirring momentum,
It can more be evenly distributed in clear water from suspension covering material, can make in mixed liquor when mixed liquor reaches certain flow rate
It, and can be compared to tradition from suspension covering material with from the reservoir fracture that suspended state carries out under long distance delivery to recovery well
Reach slot height distribution support of totally cleaving from suspension covering material, improves the rate of growth of petroleum etc..
Further, the drag reducer preparation step in step (4) is as follows, and the water of 85-93%, 5- are added as mass fraction
10% acrylamide and acrylamide derivative, the acrylic acid and methacrylic acid of 0.5-2%, the 2- acrylamide-of 1-5%
The methylpropene sodium sulfonate of 2- methyl propane sulfonic acid and 0.5-3% stirs 150-220rpm, and is warming up to 40-70 DEG C, is added above-mentioned
The initiator of gross mass 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, so that there is also isocyanate groups in urethane resin film at this time, when covering for this programme
Membrane material isocyanate groups remaining when meeting water react with water and can be in the microcosmic small spaces that the chain element of resin film surrounds
Gas is generated in vivo, and this small quantity gas is gradually increased volume under the promotion of reaction energy and forms bubble, and pushes resin film
Increase in the radial dimension of covering material particle, reaches the dilation for coating layer surface most preferably, covered to further reduced
The apparent density and volume density of membrane material, 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 from suspension covering 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, catalysis time is short, can accelerate solidification rate and the intensity performance of coat.
Further, amines additives be one of diethylenetriamine, triethylamine, ethamine, triethylene tetramine, ethylenediamine or
Person is a variety of.Cheap, the excellent catalytic effect of these types of amines additives is conducive to the formation of protrusion.
Detailed description of the invention
Fig. 1 is in embodiment 1 from the electron-microscope scanning figure of suspension covering material.
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 film is polyalcohols resin, epoxy resin and phenolic resin
It is one or more.
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, be alkyls tin and alkyl ekalead compound, preferably dibutyl tin dilaurate, tributyl tin,
One of 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 0.5-1.5% of aggregate, and the amines additives quality is the 1/100-20/100 of outermost resin quality, is urged
Agent quality is the 1/1000-1/100 of polyalcohols resin quality.
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 80-90 DEG C, and two laurels of 2 parts of glycol polymers and 0.02 part are added
Sour dibutyl tin stirring；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, is added 0.8 part
Toluene di-isocyanate(TDI) stirring；Temperature is down to 50-60 DEG C, adds 0.8 part of drag reducer mixing；Temperature is down to 40-50 DEG C and 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；Glycerine polymerization
Object, 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, there is nanoscale protrusion from suspension covering material outer surface.
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 120-130 DEG C, and 4 parts of glycerine polymer and the stirring of 0.02 part of isooctyl acid lead are added；Temperature
Degree 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 it is different that 1 part of methylenediphenyl two is added
Cyanate stirring；Temperature is down to 80-90 DEG C, adds 1.2 parts of drag reducer mixing；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 40/70,80-90 DEG C is heated to, by the haydite of heating
It pours into inside bowl-type mulling pot, 2 parts of ethylene glycol and the stirring of 0.02 part of tributyl tin is then added；Temperature is down to 75-85 DEG C, adds
Enter 0.6 part of isophorone diisocyanate and stirs；Temperature is down to 55-65 DEG C, and 4 parts of glycerine polymer and 0.02 part is added
The stirring of isooctyl acid lead；Temperature is down to 45-55 DEG C, and 0.2 part of triethylamine stirring is added；Temperature is down to 40-50 DEG C, and 1 part of methylene is added
The stirring of base diphenyl diisocyanate；Temperature is down to 35-45 DEG C, adds 1.6 parts of drag reducer mixing；Temperature is down to 30-40 DEG C
It takes the dish out of the pot.
Embodiment 4
Taking apparent density is 2.65g/cm3, granularity be 100 parts of haydite of 70/140,150-160 DEG C is heated to, by heating
Haydite pours into inside bowl-type mulling pot, and 2 parts of ethylene glycol and the stirring of 0.02 part of tributyl tin are then added；Temperature is down to 130-
140 DEG C, 0.6 part of isophorone diisocyanate is added and stirs；Temperature is down to 100-110 DEG C, and 4 parts of glycerine polymer are added
Isooctyl acid lead with 0.02 part stirs；Temperature is down to 90-100 DEG C, and 0.2 part of triethylamine stirring is added；Temperature is down to 80-90 DEG C,
1 part of methylenediphenyl diisocyanates stirring is added；Temperature is down to 70-80 DEG C, adds 2 parts of drag reducer mixing；Temperature drop
It takes the dish out of the pot to 50-60 DEG C.
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 DEG C, and 0.2 part of modified aromatic amine is added
Curing agent (T31) simultaneously stirs；Temperature is down to 80-90 DEG C, and 2 parts of epoxy resin stirrings are added；Temperature is down to 70-80 DEG C, is added 0.2
Part ethylenediamine stirring；Temperature is down to 60-70 DEG C, and 0.2 part of modified aromatic amine curing agent (T31) stirring is added；Temperature is down to 50-
60 DEG C, add 0.8 part of drag reducer mixing；Temperature, which is down to 40-50 DEG C and takes the dish out of the pot, (obtains the inner layer resin from suspension covering material
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 120-130 DEG C, and 4 parts of phenolic resin stirrings are added；Temperature is down to 100-110 DEG C, is added
0.2 part of triethylamine stirring；Temperature is down to 90-100 DEG C, and 0.8 part of hexamethylenetetramine is added and stirs；Temperature is down to 80-90 DEG C,
Add 1.2 parts of drag reducer mixing；Temperature be down to 60-70 DEG C take the dish out of the pot (obtain from the inner layer resin film of suspension covering material 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 0.3.
Comparative example 6
The difference of this comparative example and embodiment 1 is only that the mass fraction of drag reducer is 1.8.
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 3.4 parts
Raw material parts is mass fraction in above embodiments and comparative example.
Above-mentioned main performance index and measuring method from suspension covering 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.
Simultaneously by above-described embodiment and comparative example do mattress height from suspension covering material, suspend ratio and suspension time
Test.
1. suspension ratio
It suspends than being to evaluate that suspension amount in upper layer accounts for total percentage from suspension covering material in water from suspension covering material
Than.
We use from the mass ratio of suspension covering material and water and evaluate for the case where 1:4 in test.Experimental method
It is to measure 200ml water in the wide-mouth bottle of 300ml with graduated cylinder and pour into wide-mouth bottle, precise 50g falls from suspension covering material
Enter to have filled in the wide-mouth bottle of water, close the lid, up and down firmly shake 30 times, it is static after ten minutes, after the same method up and down
It firmly shakes 30 times, filters out weighing from suspension covering material, after drying for upper layer suspension with filter paper after static and filter out
It is m (g) from the quality of suspension covering material, b=m/50*100% is compared in suspension.
2. mattress height
Mattress height is lower layer height of the 20g from suspension covering 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 is poured into from suspension covering material and filled water
Graduated cylinder 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
The method of sample is reversed 10 times up and down, has vernier caliper to measure bed height of the lower layer from suspension covering material after static.
3. suspension time
Suspension time refers to the maximum duration that can freely suspend in water.
We use from the mass ratio of suspension covering material and water and evaluate for the case where 1:4 in test.Experimental method
It is to measure 200ml water in the wide-mouth bottle of 300ml with graduated cylinder and pour into wide-mouth bottle, precise 50g falls from suspension covering material
Enter to have filled in the wide-mouth bottle of water, close the lid, up and down firmly shake 30 times, it is static after ten minutes, after the same method up and down
Firmly shake 30 times, then by the static placement of wide-mouth bottle, the longest that timing measuring freely suspends in water from suspension covering material
Time.
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 evaluated from suspension covering material suspendability in clear water in upper table, by
Mattress height and the ratio that suspends codetermine, and engineering significance is the practical bulk density from suspension covering material in clear water,
It is worth the smaller relative density being equivalent in water with regard to smaller, then the suspension from suspension covering material is better, suspension time
It 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
It improves from suspension covering material from suspendability, specific is during the preparation process, if polyurethane resin film surface can generate
Dry protrusion, the isocyanates root (Isocyanates curing agent offer) when meeting water in urethane resin film can also react with water
Bubble is generated, and then is improved from suspension covering material from suspendability.
According to upper table, embodiment 1 suspension time and the ratio that suspends compared with comparative example 7 are significantly increased, i.e., this programme is compared
It is greatly improved 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,
It concluding that made from embodiment 1 from suspension covering material compared with comparative example 3, suspension time and the ratio that suspends are significantly increased,
That is significantly improving from suspendability from suspension covering material, illustrate that embodiment 1 is obtained has from suspension covering material surface
More protrusions, can release amines additives there is preferable promotion to make the formation from suspension covering material surface bulge
With making greatly improving from suspendability from suspension covering 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: when the mass fraction of drag reducer is less than 0.5 from suspension
The drag reducing efficiency of covering 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 1.5 from suspension
The drag reducing efficiency of covering material substantially reduces, and suspension time is also declined, and reduces from suspension covering material from suspension
Energy.
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 covering 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, overlay film material
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 3.4 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 covering 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, overlay film material
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, covering material all has preferably from suspendability, meets covering material in clear water from the requirement to suspend.And work as isocyanic acid
The quality of ester lower than polyalcohols resin quality less than 40% or when being greater than 80%, covering material from suspendability it is obvious under
Drop, 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 process from suspension covering 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 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；
(4) temperature is down to 35-90 DEG C, stirs after drag reducer is added, and the drag reducer quality is the 0.5-1.5% of aggregate；
(5) temperature is down to 30-70 DEG C, takes the dish out of the pot, and controlling from suspension covering material apparent density range is 1.05-2.60g/cm3。
2. a kind of preparation process from suspension covering material according to claim 1, it is characterised in that: in step (4)
Drag reducer preparation step is as follows, and the water of 85-93% is added as mass fraction, and the acrylamide and acrylamide of 5-10% is derivative
Object, the acrylic acid and methacrylic acid of 0.5-2%, the 2- acrylamide-2-methyl propane sulfonic of 1-5% and the methyl of 0.5-3%
Sodium allylsulfonate 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.
3. a kind of preparation process from suspension covering material according to claim 1, it is characterised in that: the mass parts of raw material
Number is respectively 100 parts of aggregate, and 0.25-5 parts of inner layer resin, 0.25-5 parts of outermost resin, the amines additives quality is outer layer
The 1/100-20/100 of resin quality, catalyst quality are the 1/1000-1/100 of outermost resin quality.
4. a kind of preparation process from suspension covering material according to claim 1, it is characterised in that: the inner layer resin
For the one or more of polyalcohols resin, epoxy resin and phenolic resin, the outermost resin is polyalcohols resin, polynary
The equivalent of alcohol resinoid hydroxyl is 60-300, and the curing agent of outermost resin is Isocyanates curing agent, isocyanates solidification
Agent quality is the 40-80% of polyalcohols resin.
5. a kind of preparation process from suspension covering material according to claim 4, it is characterised in that: the polyalcohols
Resin is the polymer one or several kinds of ethylene glycol, propylene glycol, glycerine.
6. a kind of preparation process from suspension covering material according to claim 4, it is characterised in that: isocyanates is solid
Agent is that toluene di-isocyanate(TDI), methylenediphenyl diisocyanates, isophorone diisocyanate, diphenyl methane two are different
One or more of cyanate.
7. a kind of preparation process from suspension covering material according to claim 1, it is characterised in that: the catalyst is
The mixture of one or more of alkyls tin compound and/or alkyls lead compound.
8. a kind of preparation process from suspension covering material according to claim 7, it is characterised in that: alkyls tin chemical combination
Object is one of dibutyl tin dilaurate, tributyl tin or several mixtures, and alkyls lead compound is tetraethyl
One of lead, isooctyl acid lead or several mixtures.
9. a kind of preparation process from suspension covering material according to claim 1, it is characterised in that: amines additives are
One or more of diethylenetriamine, triethylamine, ethamine, triethylene tetramine, ethylenediamine.
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| CN201811161859.5A CN109135721A (en) | 2018-09-30 | 2018-09-30 | A kind of preparation process from suspension covering material |
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