CN104152135B - One oil field low-density and high-strength riverfrac treatment proppant and preparation method - Google Patents
One oil field low-density and high-strength riverfrac treatment proppant and preparation method Download PDFInfo
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- CN104152135B CN104152135B CN201410352724.2A CN201410352724A CN104152135B CN 104152135 B CN104152135 B CN 104152135B CN 201410352724 A CN201410352724 A CN 201410352724A CN 104152135 B CN104152135 B CN 104152135B
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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
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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
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
Abstract
A kind of oil field low-density and high-strength riverfrac treatment proppant, it is mainly using benzoyl peroxide, styrene, divinylbenzene, methyl methacrylate as copolymerization system, and added with rare earth oxide, boron-containing compound and modified alginate fibre element additive, suspension polymerization system is formed for dispersant the most again, the product that heated reaction obtains with calcium phosphate, polyethylene alcohol and water.Low-density high temperature resistant of the present invention, anti-high pressure, dimensionally stable, compact structure.
Description
Present disclosure relates to a kind of oil recovery fracturing propping agents and preparation method.
Background technology is compared with high-load oil reservoirs, and low-permeability oil deposit, due to the restriction of self-condition, needs to utilize waterpower
Fracturing technique manufactures effectively support crackle in oil reservoir and is used as the seepage channel of oil reservoir, to increase the flow conductivity of oil, and
It is finally reached the effect of volume increase.
Now widely used proppant is ceramic base proppant and quartz sand class proppant, and they all have the highest pressure
Resistance to spalling, its density is all higher than 1.5g/cm3, belongs to middle-high density proppant.Owing to its density is relatively big, cause its difficulty of transportation,
Fracturing fluid is required the highest, and is difficult to laid at the crack location set.For this problem, research worker is developed ultralow
Density proppant, such as resin-coating quartz sand, walnut shell resin etc., they are being split by laid relatively easily than traditional proppant
In seam, and there is high anti-pressure ability and adaptive capacity to environment.But these super-low-density proppant surface structures are equal
It not spherical, therefore easily block in course of conveying.Have in recent years United States Patent (USP) such as US2009286698, US2009305044 and
US2010319916 proposes a kind of proppant based on polystyrene resin, by polystyrene add white carbon black,
Calcined silica, calcined alumina, CNT, carbon nano-fiber, cellulose nano-fibrous, natural clay, synthesis of clay, powder
The method of coal ash, polyhedral oligomeric silsesquioxane, metal cluster, metal alloy bunch, metal oxide cluster or other mixture obtains
To the spherical proppant with higher-strength.Its weak point is: heatproof, pressure poor performance, apparent consistency are low.
The oil field that summary of the invention it is an object of the invention to provide a kind of heatproof, good pressure-resistant performance, apparent consistency are high is used
Low-density and high-strength riverfrac treatment proppant and preparation method.
The present invention is using benzoyl peroxide, styrene, divinylbenzene, methyl methacrylate as copolymerization system,
And added with rare earth oxide, boron-containing compound and modified alginate fibre element additive, simultaneously again with calcium phosphate, polyethylene alcohol and water
Suspension polymerization system is formed, the product that heated reaction obtains for dispersant.
The preparation method of product of the present invention is as follows:
One, raw material
1, copolymerization system: include benzoyl peroxide, styrene monomer, divinylbenzene and methyl methacrylate, and
And, benzoyl peroxide: styrene monomer: divinylbenzene: methyl methacrylate=0.2-0.4:15.0-25.0:1.0-
15.0:1.0-18.0 (mass ratio).
2, additive: include rare earth oxide, boron-containing compound and modified alginate fibre element, wherein, rare earth oxide bag
Include: cerium oxide, lanthana, Dineodymium trioxide, praseodymium oxide, Disamarium trioxide, Gadolinia., preferably cerium oxide and lanthana；Boracic chemical combination
Thing includes: boron carbide, boron nitride, Borax, sodium borohydride, preferably boron carbide, boron nitride.Wherein, rare earth oxide and containing
The addition of boron compound is the 0.001-1.5% of copolymerization system gross mass, and the addition of modified alginate fibre element is copolymerization
The 1.0-4.0% of system gross mass.Above-mentioned additive is powdery, and its particle diameter is 0.1-0.5 micron.
3, dispersant: include polyvinyl alcohol, calcium phosphate and water, and polyvinyl alcohol: calcium phosphate: water=0.002-0.01:
0.006-0.03:100 (mass ratio), the quality of dispersant and copolymerization system mass ratio are 100:22.0-52.4.
4, coloring agent: as product needed can add the coloring agent of 0.05-0.2% copolymerization system gross mass.Such as disperse yellow
6GSL, Lang Sheng EG is red, and Lang Sheng RR is blue, bright Sheng solvent violet 36.
Two, the preparation method of the present invention
1, the process of raw material
Alginate fibre element is powdered substance, needs to use stearic acid to be modified it so that it is have lipophile before using.
Specific practice is as follows: alginate fibre element powder and Stearic acid solids granule that mass ratio is 10:1-100:1 is mixed, pours into pre-
In 50 DEG C of high-speed mixers of heat, control mixing temperature at 50-100 DEG C, mixed at high speed 1 hour, obtain modified alginate fibre element powder
End.
2, preparation method is specific as follows:
(1) in container A, add deionized water, be then heated to 35-50 DEG C.
(2) hot water in container A adds polyvinyl alcohol and calcium phosphate, be slowly stirred, then heat the mixture to 60-
70 DEG C, until being completely dissolved.Mixed liquor is made at room temperature to be slowly cooled to 30-45 DEG C after dissolving.
(3) in another container B, benzoyl peroxide, styrene monomer, divinylbenzene and metering system it are separately added into
Acid methyl ester, adds mixed rare-earth oxide, boron compound and modified alginate fibre element and coloring agent, and stirring is allowed to dissolving becomes oil
Shape liquid i.e. initiator-monomer mixed solution.This initiator-monomer mixed solution is slowly added in container A, the most handy appropriate going
Ionized water washing container B, is then also added to cleaning mixture in container A.Material in stirring container A, mixing speed controls
150-210r/min, until oil phase disperses the microsphere forming certain particle diameter to suspend in water in water.Regulation heater, makes reaction
Liquid temp rises to 70-85 DEG C and in this thermotonus 1-2 hour, then mixing speed is risen to 240-300r/min, anti-at this
Temperature and mixing speed is answered to continue reaction 2-3 hour, until microsphere is hardening.
(4) pour out the milky white liquid on upper strata, obtain transparent microsphere, with hot wash 2-3 time of 90 DEG C, then use room temperature
Water washs 2-3 time.
(5) filtering with centrifugal filtration exsiccator and be dried, the product obtained is product of the present invention.
The present invention compared with prior art has the advantage that
The proppant of the present invention is compared with the similar proppant (being called for short USLB) that Sun Company, Inc. of the U.S. produces: high temperature resistant, anti-
High pressure, dimensionally stable, compact structure, specific as follows:
1, carbon, hydrogen, oxygen three element chemical analysis show, USLB is containing only carbon and two kinds of elements of hydrogen, and the present invention is possibly together with 5-
The oxygen element of 20%, therefore both main polymer compositions are different.
2, according to United States Patent (USP) US7803740, the content that US7803741, US7803742, US7902158 announce, USLB
Heat resistance and the comprcssive strength of product is improved mainly by interpolation white carbon black, and as the content of claim protection.
The raw material of the present invention with the addition of the materials such as alginate fibre element, boron compound, composite rare-earth oxide, be polymerized
Cheng Zhong, the natural polymer subchain of alginate fibre element plays the effect of polymeric skeleton, by the nucleocapsid structure boronation of organic modification
Thing, rare earth oxide complexation product can be tight with the oxygen-containing functional group (not having oxygen-containing functional group in USLB) in polymer network
Close combination, it is uniformly dispersed.Acted on by these, make the polymer of generation have more close cross-linked network, rational interface
Structure, thus significantly improve the thermostability of spherical polyblend, comprcssive strength and toughness.Meanwhile, compound rare-earth oxidation
The existence of thing can substantially eliminate the micro-bubble of profit boundary in polymerization process, improves the light of the spherical Polymer Surface of finished product
Slippery, and reduce the precipitation of polymeric inner free monomer, reduce its dissolubility in polymer, thus significantly improve its profit
Slip energy, comprcssive strength, toughness and compactness.Alginate fibre element, as nucleator, there was added beneficially at the polyreaction initial stage
Accelerate balling-up and control sphere diameter, and Microsphere Density can be improved；There was added of alginate fibre element beneficially saves resource, reduction product simultaneously
Product cost and the internal stress of microsphere, coordinate the contradiction between thermostability and moulding processability, it is achieved that product multi-functional, high
Performance and cost degradation.
3, both main performance correction datas are as follows:
USLB: density 1.05-1.08g/cm3, heatproof 240-250 DEG C, compressive resistance ＞ 57N (40 broken 11), resistance to hydrostatic
Pressure 179.3MPa.
Product of the present invention: density 1.05-1.16g/cm3, heatproof 255-265 DEG C, compressive resistance ＞ 73N (40 broken 3), resistance to
Hydrostatic pressing 193.1MPa.
4, the present invention is the product developed based on China's raw material supply feature, and China is that Rare Earth Production state is big with product boron
State；Alginate fibre element is the side-product of Representing Thomas Energy&Biological Ltd., and therefore raw material comes
Enrich, be easy to get in source.
Detailed description of the invention
Example 1
Note: this example is the example being not added with rare earth oxide, boron compound and modified alginate fibre element for contrast.
Take 5kg deionized water and add reactor, then heat water to 50 DEG C. the hot water in reactor adds 10g
Polyvinyl alcohol and 75g calcium phosphate, be slowly stirred, then heats the mixture to 70 DEG C, until being completely dissolved.Mixed liquor is made after dissolving
At room temperature it is slowly cooled to 45 DEG C.
Another container is separately added into 10g benzoyl peroxide, 750g styrene monomer, 50g divinylbenzene and
200g methyl methacrylate, being allowed to dissolving with Glass rod stirring becomes transparent oily liquid, by this transparent oily liquid slowly
It is added in reactor, with appropriate deionized water wash container, then cleaning mixture is also added in reactor.Open stirring paddle,
Material in stirred autoclave, mixing speed controls at 210r/min, until oil phase disperses to form the micro-of certain particle diameter in water
Ball suspends in water.Regulation heater, makes reacting liquid temperature rise to 85 DEG C and this thermotonus 2 hours, then will stirring speed
Degree rises to 300r/min, continues reaction 3 hours, until microsphere is hardening in this reaction temperature and mixing speed.Pour out the breast on upper strata
White liquid, obtains transparent microsphere, with the hot wash 3 times of 90 DEG C, then washs 3 times with room temperature water.Put into centrifugal filtration to do
Dry device filters and is dried, and the microsphere grader obtaining white separates 200-425um (40-70 mesh), 425-850um (20-40
Mesh), 850-1250um (14-20 mesh).
Example 2
Take 50kg alginate fibre element powder and the mixing of 5kg Stearic acid solids granule, pour the high-speed mixer of preheating 50 DEG C into
In, control mixing temperature 50 DEG C, mixed at high speed 1 hour, obtain alginate fibre element powder, standby.
Take 5kg deionized water and add reactor, then heat water to 30 DEG C. the hot water in reactor adds 20g
Polyvinyl alcohol and 30g calcium phosphate, be slowly stirred, then heats the mixture to 60 DEG C, until being completely dissolved.Mixed liquor is made after dissolving
At room temperature it is slowly cooled to 30 DEG C.
Another container is separately added into 12g benzoyl peroxide, 850g styrene monomer, 200g divinylbenzene and
50g methyl methacrylate, 0.5g disperse yellow, (0.002g cerium oxide, 0.002g aoxidizes to add 0.01g mixed rare-earth oxide
Lanthanum, 0.002g Dineodymium trioxide, 0.002g praseodymium oxide, 0002g Disamarium trioxide), 0.5g boron carbide and 0.5g boron nitride and 44.5g modified
Alginate fibre element, being allowed to dissolving with Glass rod stirring becomes transparent oily liquid, and this transparent oily liquid is slowly added to reaction
In still, with appropriate deionized water wash container, then cleaning mixture is also added in reactor.Open stirring paddle, stirring reaction
Material in still, mixing speed controls at 180r/min, until oil phase disperses the microsphere forming certain particle diameter to be suspended in water
In water.Regulation heater, makes reacting liquid temperature rise to 75 DEG C and this thermotonus 1.5 hours, then mixing speed is risen to
280r/min, continues reaction 2.5 hours, until microsphere is hardening in this reaction temperature and mixing speed.Pour out the milky on upper strata
Liquid, obtains transparent microsphere, with the hot wash 3 times of 90 DEG C, then washs 3 times with room temperature water.Put into centrifugal filtration exsiccator
Filtering and be dried, the microsphere grader obtaining yellow separates 200-425um (40-70 mesh), 425-850um (20-40 mesh),
850-1250um (14-20 mesh), is product of the present invention.
Example 3
Take 5kg deionized water and add reactor, then heat water to 45 DEG C. the hot water in reactor adds 40g
Polyvinyl alcohol and 150g calcium phosphate, be slowly stirred, then heats the mixture to 65 DEG C, until being completely dissolved.Mixing is made after dissolving
Liquid is at room temperature slowly cooled to 35 DEG C.
Another container is separately added into 18g benzoyl peroxide, 1250g styrene monomer, 750g divinylbenzene and
700g methyl methacrylate, 5.4g Lang Sheng EG are red, and (0.22g cerium oxide, 0.22g aoxidizes to add 1.1g mixed rare-earth oxide
Lanthanum, 0.22g Dineodymium trioxide, 0.22g praseodymium oxide, 0.22g Disamarium trioxide), 0.005g Borax and 0.005g sodium borohydride compound and
27.2g modification alginate fibre element (example 2 preparation), being allowed to dissolving with Glass rod stirring becomes transparent oily liquid, and this is transparent
Oily liquids is slowly added in reactor, with appropriate deionized water wash container, is then also added in reactor by cleaning mixture.
Opening stirring paddle, the material in stirred autoclave, mixing speed controls at 200r/min, until oil phase disperses formation one in water
The microsphere determining particle diameter suspends in water.Regulation heater, makes reacting liquid temperature rise to 80 DEG C and this thermotonus 1 hour, so
After mixing speed is risen to 240r/min, continue reaction 3 hours in this reaction temperature and mixing speed, until microsphere is hardening.Incline
Go out the milky white liquid on upper strata, obtain transparent microsphere, with the hot wash 2 times of 90 DEG C, then wash 2 times with room temperature water.Put into
Centrifugal filtration exsiccator filters and is dried, and obtains peach microsphere grader and separates 200-425um (40-70 mesh), 425-
850um (20-40 mesh), 850-1250um (14-20 mesh), be product of the present invention.
Example 4
Take 5kg deionized water and add reactor, then heat water to 40 DEG C. the hot water in reactor adds 50g
Polyvinyl alcohol and 100g calcium phosphate, be slowly stirred, then heats the mixture to 70 DEG C, until being completely dissolved.Mixing is made after dissolving
Liquid is at room temperature slowly cooled to 40 DEG C.
Another container is separately added into 20g benzoyl peroxide, 1100g styrene monomer, 500g divinylbenzene and
900g methyl methacrylate, 3.8g bright Sheng RR is blue, adds 40.8g mixed rare-earth oxide (20.4g Dineodymium trioxide, 20.4g oxygen
Change praseodymium), 40.8g boron carbide and 30.2g modification alginate fibre element (example 2 preparation), being allowed to dissolving with Glass rod stirring becomes
Bright oily liquids, is slowly added to this transparent oily liquid in reactor, with appropriate deionized water wash container, then will wash
Wash liquid to be also added in reactor.Opening stirring paddle, the material in stirred autoclave, mixing speed controls at 150r/min, until
Oil phase disperses the microsphere forming certain particle diameter to suspend in water in water.Regulation heater, makes reacting liquid temperature rise to 70 DEG C also
This thermotonus 2 hours, then mixing speed is risen to 290r/min, continue reaction 2 in this reaction temperature and mixing speed
Hour, until microsphere is hardening.Pour out the milky white liquid on upper strata, obtain transparent microsphere, with the hot wash 3 times of 90 DEG C, then
Wash 2 times with room temperature water.Putting into centrifugal filtration exsiccator to filter and be dried, the microsphere grader obtaining blueness separates 200-
425um (40-70 mesh), 425-850um (20-40 mesh), 850-1250um (14-20 mesh), be product of the present invention.
Example 5
Take 5kg deionized water and add reactor, then heat water to 50 DEG C. the hot water in reactor adds 30g
Polyvinyl alcohol and 50g calcium phosphate, be slowly stirred, then heats the mixture to 70 DEG C, until being completely dissolved.Mixed liquor is made after dissolving
At room temperature it is slowly cooled to 45 DEG C.
Another container is separately added into 15g benzoyl peroxide, 1050g styrene monomer, 450g divinylbenzene and
400g methyl methacrylate, 2.3g bright Sheng solvent violet 36, then add 25.2g mixed rare-earth oxide (12.6g cerium oxide, 12.6g
Lanthana), 20.2g boron nitride and 37.8g modification alginate fibre element (example 2 preparation), being allowed to dissolving with Glass rod stirring becomes
Transparent oily liquid, is slowly added to this transparent oily liquid in reactor, with appropriate deionized water wash container, then will
Cleaning mixture is also added in reactor.Opening stirring paddle, the material in stirred autoclave, mixing speed controls at 210r/min, directly
The microsphere forming certain particle diameter is disperseed to suspend in water in water to oil phase.Regulation heater, makes reacting liquid temperature rise to 85 DEG C
And this thermotonus 2 hours, then mixing speed is risen to 300r/min, continue reaction in this reaction temperature and mixing speed
3 hours, until microsphere is hardening.Pour out the milky white liquid on upper strata, obtain transparent microsphere, with the hot wash 3 times of 90 DEG C, then
Wash 3 times with room temperature water.Putting into centrifugal filtration exsiccator to filter and be dried, the microsphere grader obtaining purple separates 200-
425um (40-70 mesh), 425-850um (20-40 mesh), 850-1250um (14-20 mesh), be product of the present invention.
Products obtained therefrom in embodiment is carried out performance test, the results are shown in Table 1 and table 2.
Under the different clossing pressure of table 1., all kinds of proppant flow conductivities compare
Experimental condition: API refluence room, waits mass method；Laid concentration is 5kg/m2, temperature 20～23 DEG C, Experimental Flowing Object is
Distilled water, the test period: short-term.
Table 2. low-density macromolecule composite proppant compares with American side like product percentage of damage
Claims (6)
1. an oil field low-density and high-strength riverfrac treatment proppant, it is characterised in that: it is with mass ratio as 0.2-0.4:
15.0-25.0:1.0-15.0:1.0-18.0 benzoyl peroxide, styrene, divinylbenzene, methyl methacrylate make
For copolymerization system, and added be the rare earth oxide of this copolymerization system gross mass 0.001-1.5% and boron-containing compound respectively with
And be that copolymerization system gross mass 1.0-4.0% is by the plain modification made with stearic acid of the alginate fibre that mass ratio is 10:1-100:1
Alginate fibre element additive, simultaneously copolymerization system again with the calcium phosphate that mass ratio is 0.002-0.01:0.006-0.03:100, poly-
The dispersant of ethylene alcohol and water forms suspension polymerization system with mass ratio 22-52.4:100, the product that heated reaction obtains, institute
The modified alginate fibre element additive stated is alginate fibre element powder and Stearic acid solids granule to be mixed, and pours preheating 50 DEG C high into
Speed mixer in, control mixing temperature at 50-100 DEG C, mixed at high speed 1 hour, the modified alginate fibre element powder obtained.
Oil field the most according to claim 1 low-density and high-strength riverfrac treatment proppant, it is characterised in that: add
The coloring agent of 0.05-0.2% copolymerization system gross mass.
Oil field the most according to claim 1 low-density and high-strength riverfrac treatment proppant, it is characterised in that: additive bag
Including rare earth oxide, boron-containing compound and modified alginate fibre element, wherein, rare earth oxide is: cerium oxide, lanthana, oxidation
One of neodymium, praseodymium oxide, Disamarium trioxide, Gadolinia.；Boron-containing compound is: one of boron carbide, boron nitride, Borax, sodium borohydride.
Oil field the most according to claim 3 low-density and high-strength riverfrac treatment proppant, it is characterised in that: above-mentioned interpolation
Agent is powdery, and its particle diameter is 0.1-0.5 micron.
5. according to the low-density and high-strength riverfrac treatment proppant of the oil field described in claim 3 or 4, it is characterised in that: rare earth
Oxide is cerium oxide and lanthana, and boron-containing compound is Borax, sodium borohydride and boron carbide.
6. the oil field of claim 1 low-density and high-strength riverfrac treatment proppant production method, it is characterised in that: preparation method
Specific as follows:
(1) in container A, add deionized water, be then heated to 35-50 DEG C,
(2) hot water in container A adds polyvinyl alcohol and calcium phosphate, be slowly stirred, then heat the mixture to 60-70
DEG C, until being completely dissolved, after dissolving, make mixed liquor at room temperature be slowly cooled to 30-45 DEG C,
(3) in another container B, benzoyl peroxide, styrene monomer, divinylbenzene and methyl methacrylate it are separately added into
Ester, adds mixed rare-earth oxide, boron compound and modified alginate fibre element and coloring agent, and stirring is allowed to dissolving becomes oily liquid
Body i.e. initiator-monomer mixed solution, is slowly added to this initiator-monomer mixed solution in container A, the material in stirring container A,
Mixing speed controls at 150-210r/min, until oil phase disperses the microsphere forming certain particle diameter to suspend in water in water, adjusts
Joint heater, makes reacting liquid temperature rise to 70-85 DEG C and in this thermotonus 1-2 hour, then mixing speed is risen to 240-
300r/min, continues reaction 2-3 hour in this reaction temperature and mixing speed, until microsphere is hardening,
(4) pour out the milky white liquid on upper strata, obtain transparent microsphere, with hot wash 2-3 time of 90 DEG C, then wash by room temperature
Wash 2-3 time,
(5) filter with centrifugal filtration exsiccator and be dried.
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| CN105837720A (en) * | 2016-04-01 | 2016-08-10 | 孙安顺 | Resin filler for fracturing and its preparation method |
| CN106833601A (en) * | 2017-01-17 | 2017-06-13 | 中国地质大学（武汉） | Modified super-low-density proppant of a kind of Graphene and preparation method thereof |
| CN106893575A (en) * | 2017-02-16 | 2017-06-27 | 青岛科凯达橡塑有限公司 | A kind of natural gas extraction molten overlay film proppant of gas and its preparation method and application |
| CN106832081B (en) * | 2017-02-16 | 2019-08-13 | 青岛科凯达橡塑有限公司 | A kind of oil exploitation oil-soluble resin and its preparation method and application |
| CN106987243A (en) * | 2017-04-21 | 2017-07-28 | 合肥智慧殿投资管理有限公司 | A kind of fracturing propping agents additive, fracturing propping agents and preparation method |
| CN113278210B (en) * | 2021-05-19 | 2022-07-26 | 山东高速集团有限公司创新研究院 | Rubber-plastic alloy for modified asphalt mixture and preparation method thereof |
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