CN108033710A - A kind of Ultralight overlay film proppant and preparation method thereof - Google Patents
A kind of Ultralight overlay film proppant and preparation method thereof Download PDFInfo
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- CN108033710A CN108033710A CN201711208971.5A CN201711208971A CN108033710A CN 108033710 A CN108033710 A CN 108033710A CN 201711208971 A CN201711208971 A CN 201711208971A CN 108033710 A CN108033710 A CN 108033710A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/12—Condensation polymers of aldehydes or ketones
- C04B26/122—Phenol-formaldehyde condensation polymers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/14—Polyepoxides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/30—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Other silicon-containing organic compounds; Boron-organic compounds
- C04B26/32—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Other silicon-containing organic compounds; Boron-organic compounds containing silicon
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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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
Abstract
The present invention relates to oil, natural gas and shale gas pressure break production technique field, more particularly to a kind of Ultralight overlay film proppant, including aggregate, Special Resin, curing agent, accelerating agent and dispersant, Special Resin includes resin and sub-nanometer inorganic material, the preparation method of Ultralight overlay film proppant is also disclosed, including：1) aggregate is heated to 130~350 DEG C；2) Special Resin is added, after it is wrapped mixing with aggregate stirring, curing agent and accelerating agent is added, stirs and evenly mixs, cured；3) dispersant is added, is stirred and evenly mixed to material dispersion into individual particle shape；4) cool down, is broken, screening, overlay film proppant is made.It is smaller using overlay film proppant volume density and apparent density made from the technical program, can be by long-distance sand transport, and laying process is uniform, helps to improve oil-gas mining amount.
Description
Technical field
The present invention relates to oil, natural gas and shale gas pressure break production technique field, and in particular to a kind of Ultralight overlay film
Proppant and preparation method thereof.
Background technology
Hydraulic fracturing is exactly to utilize ground high-pressure pump, has the fracturing fluid of viscosity higher to oil reservoir squeezing by pit shaft.When
When the speed of injection fracturing fluid exceedes the absorbability of oil reservoir, then very high pressure is formed on the oil reservoir of shaft bottom, when this pressure
More than during the fracture pressure of reservoir rock, oil reservoir will be pressed off and produce crack near shaft bottom.At this moment, on and on to oil reservoir
Fracturing fluid is squeezed, crack will continue to oil reservoir interior expansion.In order to keep the crack pressed off to be in open configuration, then to oil
Layer squeezes into the load fluid with proppant particles, and load fluid enters after crack, and crack on the one hand can be made to continue to extend forward,
On the other hand the crack pressed off can be supported, makes it be not to close.Proppant particles produce permeable passage, possess
Higher flow conductivity, by the passage, oil, gas can be flowed into wellbore, so as to improve oil gas well yield.
Common common proppants have quartz sand, artificial porcelain granule, metallic particles, synthesis organic granular, walnut shell etc..And mesh
Preceding country's fracturing technology is still based on quartz sand and haydite.The pressure break that quartz sand is mainly used in the low clossing pressure well of shallow-layer is made
Industry；Haydite is mainly used in middle-deep well fracturing technology, although haydite solves the problems, such as that quartz sand intensity is low, but due to its density
Greatly, it is of high cost, the factor such as construction risk height, it is difficult to meet the requirement of growing Fracturing Technology.And this kind of support
Agent, can be because be subject to larger impact force and closure stress when more deep fat is applied to, and produces a large amount of fragments and thin
These fragments of powder and fine powder can block crack so as to reduce the flow conductivity in crack, and data shows, common extremely-low density
Percentage of damage 15%~21% of the haydite when clossing pressure is 69MPa, percentage of damage when clossing pressure is 86MPa is 23%~
28%, it is impossible to meet pressing crack construction requirement.For this reason, occur some both at home and abroad in quartz sand, artificial porcelain granule, metal at present
The surface of the proppants such as grain, synthesis organic granular, walnut shell coats the technological innovation of one or more layers resin film, to improve support
The resistant to breakage ability of agent.
United States Patent (USP) US5837656 discloses a kind of application that multi-layer resinous overlay film is used on proppant particles, the U.S.
Patent US3854533, US367986 discloses a kind of application that epoxy resin overlay film is used on proppant particles；Publication No.
The Chinese patent of CN102899019A discloses a kind of using phenolic resin or the proppant of epoxy resin overlay film, Publication No.
The Chinese patent of CN101942296A disclose it is a kind of using phenolic resin, epoxy resin and organic siliconresin etc. as coating
Fiber composite sand control material.The raw material and certain operations step used in these methods, method all drop to a certain extent
The low percentages of damage of proppant particles under stress.
But also there are following defect for existing resin coated propping agent：1st, coating phenolic resin brittleness is larger, compares ring
Oxygen tree fat and organic siliconresin, coating phenolic resin percentage of damage under equal clossing pressure is higher, according to multi-layer resinous overlay film
Or increase amount of resin to improve compression strength, then the thickness of resin mold is accordingly added, so as to influence flow conductivity；2nd, due to
Subsurface environment is extremely complex, phenolic resin coating proppant surface can be subject to oil in rock stratum, gas and water, brine, steam,
The erosion of acid and alkali corrosion liquid, microorganism etc., causes the burn into of clad to degrade, come off, so as to cause formation fractures water conservancy diversion energy
Power substantially reduces；3rd, using the proppant of the resin coatings such as epoxy resin, organic siliconresin, raw material, process costs are relatively
It is high；4th, existing resin coated propping agent bulk density (the proppant quality of unit stacking volume) and apparent density (unit grain
The proppant quality of volume) it is higher, cause resin coated propping agent to carry out short distance conveying in crack, and lay process
Not enough uniformly, sedimentation is fast, reduces oil-gas mining amount, when being applied especially to the fracturing developing of shale gas, the drop of oil-gas mining amount
Low phenomenon is the most obvious.
The content of the invention
It is an object of the invention to provide a kind of Ultralight overlay film proppant and preparation method thereof, obtained overlay film proppant
Bulk density and apparent density are smaller, energy long-distance sand transport, and laying process is uniform, helps to improve oil-gas mining amount.
To reach above-mentioned purpose, base case of the invention is as follows：A kind of Ultralight overlay film proppant, including aggregate, spy
Kind resin, curing agent, accelerating agent and dispersant, Special Resin include resin and sub-nanometer inorganic material；Special Resin and aggregate
Weight ratio be 1~20：100, the weight ratio of curing agent and Special Resin is 3~50：100, the weight of accelerating agent and Special Resin
Amount is than being 0.1~30：100, the weight ratio of dispersant and aggregate is 0.1~10：100.
The operation principle and beneficial effect of above-mentioned technical proposal are：Resin is to pass through used by preparing overlay film proppant
After Subnano-class is inorganic material-modified, so obtained Special Resin has the special performance of sub-nanometer inorganic material, not only
Even if can cause aggregate in the event of high temperatures, it is not easy to soften, and the surface of aggregate can also be dried, is made
Obtaining aggregate has good convergence, and the body shape high molecular polymer that such resin and curing agent are cured reaction generation also can
The surface of aggregate is uniformly coated on, along with sub-nanometer inorganic material itself just has small excellent of bigger than surface, light, density
Gesture, so final obtained overlay film proppant particles are light, bulk density and apparent density are all smaller, suspendability in fracturing fluid
Excellent, when pressing crack construction is applied, this proppant can be by long-distance sand transport into crack, and laying process is uniform, lays
Overlay film support dosage can greatly increase so that crack gap density increase, crack height and seam width increase, crack total cross section
Bigger, oil-gas mining amount are significantly improved.
Preferred solution one：Based on scheme preferred solution, resin include phenolic resin, epoxy resin, organosilicon tree
One or more in fat；Phenolic resin, epoxy resin, the weight ratio of organic siliconresin and sub-nanometer inorganic material for 1~
80：1~100：1~100：0.2~40.
The overlay film proppant strength being made using phenolic resin is higher, and production cost is low, technique is simple, using asphalt mixtures modified by epoxy resin
Overlay film proppant resistant to breakage ability is strong made from fat, and coating technique is good, using overlay film proppant made from organic siliconresin
Temperature tolerance is stronger；And get up to make by phenolic resin, epoxy resin and organic siliconresin combination of two or by three kinds of resin-bondeds
Standby overlay film proppant, then can also realize while the corresponding unique function of various resins all can be combined and preferably prepare work
Skill controllability, the overlay film proppant strength of preparation, resistant to breakage ability and flow conductivity are more excellent, and suspension is more preferable, its is comprehensive
It can show more excellent.
Preferred solution two：Based on scheme preferred solution, sub-nanometer inorganic material includes surface active groups and nothing
Machine oxide.Using containing surface active groups such as-OH ,-NHX ,-COOH ,-CONH- ,-COOR ,-Si-OR ,-OSi-R, nothing
Machine oxide such as silica, aluminium oxide, iron oxide, magnesia, calcium oxide, titanium oxide, manganese oxide, sodium oxide molybdena, potassium oxide etc.
Natural mineral matter or artificial compounded type inorganic particle as sub-nanometer inorganic material, can change well with resin-bonded
Property, obtained overlay film proppant volume density and apparent density smaller, suspension are more preferable.
Preferred solution three：Preferably two preferred solution, sub-nanometer inorganic material is silicon powder, nano-silicon is micro-
One or more in powder, nano alumina powder, glass microballoon, flyash, floating bead powder；The particle diameter of sub-nanometer inorganic material is
1~150um.It is more preferable to the drying effect of aggregate surface using the sub-nanometer inorganic material of this particle size, it is more conducive to drop
The density of low overlay film proppant, and this kind of sub-nanometer inorganic material can be produced by Industrial Stoves, metallurgy, roaster discharge, can be had
Effect reduces proppant cost of manufacture.
Preferred solution four：Based on scheme preferred solution, aggregate be haydite, quartz sand or walnut shell in one kind
Or it is a variety of, and the bulk density of aggregate is less than 1.3g/cm3, the apparent density of aggregate is less than 2.65g/cm3.Using this ultralow close
The aggregate of degree, the proppant volume density and apparent density smaller, suspension being prepared are more preferable.
Preferred solution five：Based on scheme preferred solution, curing agent for paraformaldehyde, hexamethylenetetramine, pregnancy
Epoxide methyl melamine, aliphatic amine, aromatic amine, cycloaliphatic amines, tertiary amine, quaternary amine, imidazoles, acid anhydrides, lewis acid, six methylenes
One or more in urotropine, tetraethoxysilance compound.With Special Resin irreversible cure instead occurs for such curing agent
Should, the cross-linked polymer polymer molecular weight bigger of formation, final obtained overlay film proppant temperature tolerance and intensity are more preferably.
Preferred solution six：Based on scheme preferred solution, accelerating agent is mica powder, CaO, TiO2, oxalic acid acetone are molten
One or more in liquid, organic amine, organo-metallic compound class.Contribute to further improve curing using such accelerating agent
Reaction rate.
Preferred solution seven：Based on scheme preferred solution, dispersant is Tissuemat E, stearic amide, ethylene are double
One or more in stearmide, calcium stearate, zinc stearate, atoleine, amiantuhs ether, silicone oil.Using such point
Powder, which not only facilitates, further prevents occurring phenomena such as particle sedimentation or cohesion in curing reaction, and helps to reduce boundary
Face tension force, promotes mixture to be dispersed into uniform individual particle shape.
Preferred solution eight：Based on scheme, preferred solution one, preferred solution two, preferred solution three, preferred solution four,
The preferred solution of preferred solution five, preferred solution six or preferred solution seven, a kind of preparation method of Ultralight overlay film proppant, bag
Include following steps：
1) aggregate is heated to 130~350 DEG C；
2) Special Resin is added, after it is wrapped mixing with aggregate stirring, adds curing agent and accelerating agent, stirring is mixed
It is even, cured；
3) dispersant is added, is stirred and evenly mixed to material dispersion into individual particle shape；
4) cool down, is broken, screening, overlay film proppant is made.
The operation principle and beneficial effect of above-mentioned technical proposal are：Special Resin is cured under the action of curing agent
The raw webbed high molecular polymer of reaction, and under the action of accelerating agent, reaction rate is faster；Meanwhile extraordinary tree used
Fat has the special performance of sub-nanometer inorganic material, can not only cause aggregate under 350 DEG C of high-temperature condition, to be not easy to
Soften, and the surface of aggregate can also be dried so that aggregate has good convergence, such high molecular polymerization
Thing can equably film be in aggregate surface, and obtained overlay film proppant is light, suspension is good, and apparent density and bulk density are small,
This proppant can be by long-distance sand transport into crack, and laying process is uniform, and the overlay film support dosage of laying can greatly increase,
So that the increase of crack gap density, crack height and seam width increase, crack total cross section bigger, oil-gas mining measures significant
Improve.
Preferred solution nine：Preferably eight preferred solution, the preparation method of Special Resin comprise the following steps：Will
Resin and sub-nanometer inorganic material are heated to 80~200 DEG C, mix 1~10min.Resin and the heating of sub-nanometer inorganic material is mixed
After Special Resin is made in conjunction, then with aggregate, curing agent etc. overlay film proppant is mixed with, there is following beneficial effect：1st, contribute to
The process that sub-nanometer inorganic material, resin are mixed with aggregate is allowed to be more prone to, mixing uniformity is also more preferable, so obtained overlay film
Proppant uniformity higher, performance are also more excellent；2nd, sub-nanometer inorganic material is first mixed with resin, again property input aggregate
In, not only more accurate to the weight weighing of each material, especially sub-nanometer inorganic material, so each substance reaction ratio is more
Accurately, and operation is also more convenient, it is thus also avoided that sub-nanometer inorganic material other techniques such as dust from flying brought that kick the beam are asked
Topic.
Embodiment
Below by embodiment, the present invention is described in further detail：
Embodiment 1
1) 100kg aggregates are heated to 350 DEG C；Wherein aggregate be haydite, quartz sand either one kind in walnut shell or
It is a variety of, the preferred haydite of the present embodiment, particle diameter preferably 40/70 mesh of haydite, the preferred 1.3g/cm of bulk density3, apparent density is preferred
2.65g/cm3。
2) 20kg Special Resins are added, after it is wrapped mixing with aggregate stirring, 10kg curing agent is added and 6kg promotes
Agent, stirs and evenly mixs, and is cured.
The production method of wherein Special Resin is：Resin and sub-nanometer inorganic material are heated to 200 DEG C, mix 10min；
Resin includes phenolic resin, epoxy resin and organic siliconresin, and phenolic resin, epoxy resin, organic siliconresin and sub-nanometer
The quality of inorganic material is respectively 5kg, 6.25kg, 6.25kg, 2.5kg.Sub-nanometer inorganic material is silicon powder, nano-silicon is micro-
One or more in powder, nano alumina powder, glass microballoon, flyash, floating bead powder, and the particle diameter of sub-nanometer inorganic material
For 1~150um, the silicon powder of the preferred 150um of the present embodiment.
Curing agent is paraformaldehyde, hexamethylenetetramine, hexamethoxymethyl melamine, aliphatic amine, aromatic amine, fat
Ring race amine, tertiary amine, quaternary amine, imidazoles, acid anhydrides, lewis acid, hexa, one kind in tetraethoxysilance compound or more
Kind, the mixture of the preferred hexamethylenetetramine of the present embodiment, tertiary amine and imidazoles, corresponding quality is respectively 2kg, 4kg, 4kg.
Accelerating agent is one in mica powder, CaO, TiO2, oxalic acid acetone soln, organic amine, organo-metallic compound class
Kind or a variety of, the preferred CaO of the present embodiment.
3) 10kg dispersants are added when group has been started in step 2), stirred and evenly mixed to material dispersion into individual particle
Shape；Dispersant is Tissuemat E, stearic amide, ethylene bis stearamide, calcium stearate, zinc stearate, atoleine, advanced
One or more in petroleum ether, silicone oil, the preferred calcium stearate of the present embodiment.
4) cool down, is broken, screening, overlay film proppant is made.
Particularly, the preferred sand mixer of device of step 2) and the middle various materials of stirring of step 3).
Embodiment 2
1) after 100kg aggregates being heated to 130 DEG C；The wherein preferred haydite of aggregate, particle diameter preferably 40/70 mesh of haydite, body
The preferred 1.3g/cm of product density3, the preferred 2.65g/cm of apparent density3。
2) 1kg Special Resins are added, after making it stirring wrapping mixing with aggregate, add 0.003kg curing agent and
0.001kg accelerating agents, stir and evenly mix, and are cured.
The production method of wherein Special Resin is：Resin and sub-nanometer inorganic material are heated to 80 DEG C, mix 1min；Tree
Fat includes phenolic resin, epoxy resin and organic siliconresin, and phenolic resin, epoxy resin, organic siliconresin and sub-nanometer without
The quality of machine material is respectively 0.2kg, 0.4kg, 0.3kg, 0.1kg.Sub-nanometer inorganic material for silicon powder, nano silicon micronization,
One or more in nano alumina powder, glass microballoon, flyash, floating bead powder, and the particle diameter of sub-nanometer inorganic material is
1um, the preferred silicon powder of the present embodiment.
Curing agent is paraformaldehyde, hexamethylenetetramine, hexamethoxymethyl melamine, aliphatic amine, aromatic amine, fat
Ring race amine, tertiary amine, quaternary amine, imidazoles, acid anhydrides, lewis acid, hexa, one kind in tetraethoxysilance compound or more
Kind, the mixture of the preferred hexamethylenetetramine of the present embodiment, tertiary amine and imidazoles, corresponding quality be respectively 0.001kg,
0.001kg、0.001kg。
Accelerating agent is one in mica powder, CaO, TiO2, oxalic acid acetone soln, organic amine, organo-metallic compound class
Kind or a variety of, the preferred CaO of the present embodiment.
3) dispersant is added when group has been started in step 2), stirred and evenly mixed to material dispersion into individual particle shape；Its
The quality of middle dispersant is 1kg；Dispersant is Tissuemat E, stearic amide, ethylene bis stearamide, calcium stearate, tristearin
One or more in sour zinc, atoleine, amiantuhs ether, silicone oil, the preferred calcium stearate of the present embodiment.
4) cool down, is broken, screening, overlay film proppant is made.
Particularly, the preferred sand mixer of device of step 2) and the middle various materials of stirring of step 3).
Embodiment 3
1) 100kg aggregates are heated to 300 DEG C；The wherein preferred haydite of aggregate, particle diameter preferably 40/70 mesh of haydite, volume
The preferred 1.3g/cm of density3, the preferred 2.65g/cm of apparent density3。
2) 4.5kg Special Resins are added, after it is wrapped mixing with aggregate stirring, add 2.0kg curing agent and 0.8kg
Accelerating agent, stirs and evenly mixs, and is cured.
The production method of wherein Special Resin is：Resin and sub-nanometer inorganic material are heated to 100 DEG C, mix 5min；
Resin includes phenolic resin, epoxy resin and organic siliconresin, and phenolic resin, epoxy resin, organic siliconresin and sub-nanometer
The quality of inorganic material is respectively 1kg, 1.5kg, 1.5kg, 0.5kg.Sub-nanometer inorganic material for silicon powder, nano silicon micronization,
One or more in nano alumina powder, glass microballoon, flyash, floating bead powder, and the particle diameter of sub-nanometer inorganic material is
5um, the preferred silicon powder of the present embodiment.
Curing agent is paraformaldehyde, hexamethylenetetramine, hexamethoxymethyl melamine, aliphatic amine, aromatic amine, fat
Ring race amine, tertiary amine, quaternary amine, imidazoles, acid anhydrides, lewis acid, hexa, one kind in tetraethoxysilance compound or more
Kind, the mixture of the preferred hexamethylenetetramine of the present embodiment, tertiary amine and imidazoles, corresponding quality be respectively 0.4kg, 0.8kg,
0.8kg。
Accelerating agent is one in mica powder, CaO, TiO2, oxalic acid acetone soln, organic amine, organo-metallic compound class
Kind or a variety of, the preferred CaO of the present embodiment.
3) dispersant is added when group has been started in step 2), stirred and evenly mixed to material dispersion into individual particle shape；Its
The quality of middle dispersant is 0.8kg；Dispersant is Tissuemat E, stearic amide, ethylene bis stearamide, calcium stearate, hard
One or more in resin acid zinc, atoleine, amiantuhs ether, silicone oil, the preferred calcium stearate of the present embodiment.
4) cool down, is broken, screening, overlay film proppant is made.
Particularly, the preferred sand mixer of device of step 2) and the middle various materials of stirring of step 3).
Embodiment 4
1) 100kg aggregates are heated to 300 DEG C；The wherein preferred haydite of aggregate, particle diameter preferably 40/70 mesh of haydite, volume
The preferred 1.3g/cm of density3, the preferred 2.65g/cm of apparent density3。
2) 4.5kg Special Resins are added, after it is wrapped mixing with aggregate stirring, add 2.0kg curing agent and 0.8kg
Accelerating agent, stirs and evenly mixs, and is cured.
The production method of wherein Special Resin is：Resin and sub-nanometer inorganic material are heated to 100 DEG C, mix 5min；
Resin is phenolic resin, and the quality of phenolic resin and sub-nanometer inorganic material is respectively 4kg, 0.5kg.Sub-nanometer inorganic material
For the one or more in silicon powder, nano silicon micronization, nano alumina powder, glass microballoon, flyash, floating bead powder, and it is sub-
The particle diameter of nano inorganic material is 5um, the preferred silicon powder of the present embodiment.
Curing agent is paraformaldehyde, hexamethylenetetramine, hexamethoxymethyl melamine, aliphatic amine, aromatic amine, fat
Ring race amine, tertiary amine, quaternary amine, imidazoles, acid anhydrides, lewis acid, hexa, one kind in tetraethoxysilance compound or more
Kind, the preferred hexamethylenetetramine of the present embodiment.
Accelerating agent is one in mica powder, CaO, TiO2, oxalic acid acetone soln, organic amine, organo-metallic compound class
Kind or a variety of, the preferred CaO of the present embodiment.
3) dispersant is added when group has been started in step 2), stirred and evenly mixed to material dispersion into individual particle shape；Its
The quality of middle dispersant is 0.8kg；Dispersant is Tissuemat E, stearic amide, ethylene bis stearamide, calcium stearate, hard
One or more in resin acid zinc, atoleine, amiantuhs ether, silicone oil, the preferred calcium stearate of the present embodiment.
4) cool down, is broken, screening, overlay film proppant is made.
Particularly, the preferred sand mixer of device of step 2) and the middle various materials of stirring of step 3).
Embodiment 5
1) 100kg aggregates are heated to 300 DEG C；The wherein preferred haydite of aggregate, particle diameter preferably 40/70 mesh of haydite, volume
The preferred 1.3g/cm of density3, the preferred 2.65g/cm of apparent density3。
2) 4.5kg Special Resins are added, after it is wrapped mixing with aggregate stirring, add 2.0kg curing agent and 0.8kg
Accelerating agent, stirs and evenly mixs, and is cured.
The production method of wherein Special Resin is：Resin and sub-nanometer inorganic material are heated to 100 DEG C, mix 5min；
Resin is epoxy resin, and the quality of epoxy resin and sub-nanometer inorganic material is respectively 4kg, 0.5kg.Sub-nanometer inorganic material
For the one or more in silicon powder, nano silicon micronization, nano alumina powder, glass microballoon, flyash, floating bead powder, and it is sub-
The particle diameter of nano inorganic material is 5um, the preferred silicon powder of the present embodiment.
Curing agent is paraformaldehyde, hexamethylenetetramine, hexamethoxymethyl melamine, aliphatic amine, aromatic amine, fat
Ring race amine, tertiary amine, quaternary amine, imidazoles, acid anhydrides, lewis acid, hexa, one kind in tetraethoxysilance compound or more
Kind, the present embodiment preferred tertiary amine.
Accelerating agent is one in mica powder, CaO, TiO2, oxalic acid acetone soln, organic amine, organo-metallic compound class
Kind or a variety of, the preferred CaO of the present embodiment.
3) dispersant is added when group has been started in step 2), stirred and evenly mixed to material dispersion into individual particle shape；Its
The quality of middle dispersant is 0.8kg；Dispersant is Tissuemat E, stearic amide, ethylene bis stearamide, calcium stearate, hard
One or more in resin acid zinc, atoleine, amiantuhs ether, silicone oil, the preferred calcium stearate of the present embodiment.
4) cool down, is broken, screening, overlay film proppant is made.
Particularly, the preferred sand mixer of device of step 2) and the middle various materials of stirring of step 3).
Comparative example 1
1) after 100kg aggregates being heated to 300 DEG C, it is put into sand mixer；Wherein the preferred haydite of aggregate, the particle diameter of haydite are excellent
Select 40/70 mesh, the preferred 1.3g/cm of bulk density3, the preferred 2.65g/cm of apparent density3。
2) 4.5kg phenolic resin is added into sand mixer, after it is wrapped mixing with aggregate stirring, adds 2.0kg six
Methine tetramine and 0.8kgCaO, stir and evenly mix, and are cured.
3) 0.8kg calcium stearates are added when group has been started in step 2), stirred and evenly mixed to material dispersion into single
It is granular.
4) cool down, is broken, screening, overlay film proppant is made.
Comparative example 2
1) after 100kg aggregates being heated to 300 DEG C, it is put into sand mixer；Wherein the preferred haydite of aggregate, the particle diameter of haydite are excellent
Select 40/70 mesh, the preferred 1.3g/cm of bulk density3, the preferred 2.65g/cm of apparent density3。
2) 4.5kg epoxy resin is added into sand mixer, after it is wrapped mixing with aggregate stirring, adds uncle 2.0kg
Amine and 0.8kgCaO, stir and evenly mix, and are cured.
3) 0.8kg calcium stearates are added when group has been started in step 2), stirred and evenly mixed to material dispersion into single
It is granular.
4) cool down, is broken, screening, overlay film proppant is made.
By made from embodiment 1~5 and comparative example 1~2 overlay film proppant carry out bulk density, apparent density, acid solubility,
The test and comparison of turbidity, percentage of damage and short-term flow conductivity.Wherein：
Bulk density：The proppant quality of unit stacking volume.10.3.3 section volumes according to SY/T5108-2014 standards
Density measurement method detects sample bulk density.
Apparent density：The proppant quality of unit grain volume.10.4.2 section apparent densities according to SY/T5108-2014 standards
Test method detects sample apparent density.
Acid solubility：Under defined calculation solution and reaction condition, the proppant of certain mass by the quality of acid dissolving with
The percentage of total proppant quality.Acid according to 8.4 section acid solubility experimental method detection samples of SY/T5108-2014 standards
Solubility.
Turbidity：The proppant of certain mass is added in the distilled water of prescribed volume, through shaking and placing after a certain period of time
The muddy degree of liquid.Turbidity according to 9.5 section turbidimetry detection samples of SY/T5108-2014 standards.
Percentage of damage：The percentage that proppant crushes under the conditions of clossing pressure is provided.According to SY/T5108-2014 standards
The percentage of damage of 11.5 section proppant percentage of damage test method detection samples.
Short-term flow conductivity：The ability that i.e. proppant passes through crack；Short-term water conservancy diversion energy according to SY/T6302-2009 standards
Force test method monitors the short-term flow conductivity of sample.(the linear diversion chamber of API, test fluid are distilled water, laying concentration is
10kg/cm3) test result see the table below：
Following derivation can be drawn from upper table：
1st, the bulk density of embodiment 1~5 is respectively less than the bulk density of comparative example 1~2, and the apparent density of embodiment 1~5 is equal
Less than the apparent density of comparative example 1~2；By contrasting it can be found that having in common that for each embodiment all employs extraordinary tree
Fat, and each comparative example has in common that the ordinary resin all used；Meanwhile can be with by comparative example 4 and comparative example 1
It was found that both differs only in：Embodiment employs Special Resin, and comparative example employs ordinary resin；Implementation is contrasted again
Example 5 and comparative example 2 are also such；And the bulk density of overlay film proppant made from Special Resin is used all than using ordinary resin
The bulk density of obtained overlay film proppant is small (apparent density is also such), therefore it may be concluded that is formulated using this preparation
Contribute to reduce the bulk density and apparent density of overlay film proppant with method；And bulk density and apparent density are reduced, help to prop up
Agent is supportted in fracturing process by long-distance sand transport, ensures that overlay film proppant lays the uniformity of process, crack openings section is big, oil
Gas yield bigger.
2nd, by comparative example 4, comparative example 1 or embodiment 5, comparative example 2 it is also found that being made using the present invention
Overlay film proppant its acid solubility, turbidity, percentage of damage and short-term flow conductivity be not much different with comparative example, and bulk density
It is intended to apparent density smaller, illustrates not only more light using overlay film proppant made from the technical program, but also can also meet to press
Split remaining performance requirement to proppant.
3rd, can be seen that embodiment 3 when Special Resin is prepared from the percentage of damage of embodiment 3 and embodiment 4 is to adopt
With what phenolic resin, epoxy resin, organic siliconresin and sub-nanometer inorganic material were mixed to prepare, embodiment 4 be only with
What phenolic resin and sub-nanometer inorganic material were mixed to prepare, and every test index of overlay film proppant made from embodiment 3 is all
Every test index than the overlay film proppant of embodiment 4 is more excellent, illustrates when Special Resin is prepared, by phenolic resin,
The Special Resin performance that epoxy resin, three kinds of resins of organic siliconresin and sub-nanometer inorganic material are mixed to prepare is more preferably.
Above-described is only the embodiment of the present invention, and the general knowledge such as known concrete structure and characteristic is not made herein in scheme
Excessive description., 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 should also be considered as protection scope of the present invention, these are implemented all without the influence present invention
Effect and practical applicability.The scope of protection required by this application should be based on the content of the claims, in specification
The records such as embodiment can be used for the content for explaining claim.
Claims (10)
1. a kind of Ultralight overlay film proppant, it is characterised in that including aggregate, Special Resin, curing agent, accelerating agent and disperse
Agent, the Special Resin include resin and sub-nanometer inorganic material；The weight ratio of the Special Resin and the aggregate for 1~
20：100, the weight ratio of the curing agent and the Special Resin is 3~50：100, the accelerating agent and the Special Resin
Weight ratio is 0.1~30：100, the weight ratio of the dispersant and the aggregate is 0.1~10：100.
2. a kind of Ultralight overlay film proppant according to claim 1, it is characterised in that the resin includes phenolic aldehyde tree
One or more in fat, epoxy resin, organic siliconresin；The phenolic resin, epoxy resin, organic siliconresin and Ya Na
The weight ratio of rice inorganic material is 1~80：1~100：1~100：0.2~40.
A kind of 3. Ultralight overlay film proppant according to claim 1, it is characterised in that the sub-nanometer inorganic material bag
Containing surface active groups and inorganic oxide.
4. a kind of Ultralight overlay film proppant according to claim 3, it is characterised in that the sub-nanometer inorganic material is
One or more in silicon powder, nano silicon micronization, nano alumina powder, glass microballoon, flyash, floating bead powder；The Asia
The particle diameter of nano inorganic material is 1~150um.
5. a kind of Ultralight overlay film proppant according to claim 1, it is characterised in that the aggregate is haydite, quartz
One or more in sand or walnut shell, and the bulk density of the aggregate is less than 1.3g/cm3, the apparent density of aggregate is low
In 2.65g/cm3。
6. a kind of Ultralight overlay film proppant according to claim 1, it is characterised in that the curing agent is poly first
Aldehyde, hexamethylenetetramine, hexamethoxymethyl melamine, aliphatic amine, aromatic amine, cycloaliphatic amines, tertiary amine, quaternary amine, imidazoles,
One or more in acid anhydrides, lewis acid, hexa, tetraethoxysilance compound.
A kind of 7. Ultralight overlay film proppant according to claim 1, it is characterised in that the accelerating agent for mica powder,
One or more in CaO, TiO2, oxalic acid acetone soln, organic amine, organo-metallic compound class.
8. a kind of Ultralight overlay film proppant according to claim 1, it is characterised in that the dispersant is polyethylene
One in wax, stearic amide, ethylene bis stearamide, calcium stearate, zinc stearate, atoleine, amiantuhs ether, silicone oil
Kind is a variety of.
9. the preparation method of Ultralight overlay film proppant according to any one of claim 1 to 8, it is characterised in that bag
Include following steps：
1) aggregate is heated to 130~350 DEG C；
2) Special Resin is added, after it is wrapped mixing with aggregate stirring, curing agent and accelerating agent is added, stirs and evenly mixs, into
Row cures；
3) dispersant is added, is stirred and evenly mixed to material dispersion into individual particle shape；
4) cool down, is broken, screening, overlay film proppant is made.
10. the preparation method of Ultralight overlay film proppant according to claim 9, it is characterised in that the Special Resin
Preparation method comprise the following steps：Resin and sub-nanometer inorganic material are heated to 80~200 DEG C, mix 1~10min.
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| CN109281645A (en) * | 2018-09-30 | 2019-01-29 | 重庆长江造型材料（集团）股份有限公司 | Using the construction method from suspension riverfrac treatment proppant |
| CN109385263A (en) * | 2018-12-13 | 2019-02-26 | 中国石油大学(华东) | A kind of low-density film-coated ceramisite proppant and preparation method thereof |
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| CN110157405A (en) * | 2019-04-23 | 2019-08-23 | 中国石油大学(北京) | For the overlay film proppant of unconventional reservoir hydraulic fracturing and preparation and application |
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| CN108929667A (en) * | 2018-09-08 | 2018-12-04 | 佛山市禅城区诺高环保科技有限公司 | A kind of preparation method of thermostable type oil field sand-fixating agent |
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