CN106675548A - Self-suspension propping agent and preparation method thereof - Google Patents
Self-suspension propping agent and preparation method thereof Download PDFInfo
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- CN106675548A CN106675548A CN201611053034.2A CN201611053034A CN106675548A CN 106675548 A CN106675548 A CN 106675548A CN 201611053034 A CN201611053034 A CN 201611053034A CN 106675548 A CN106675548 A CN 106675548A
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- firming agent
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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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Abstract
A self-suspension propping agent and a preparation method thereof are disclosed. The propping agent comprises the following ingredients: aggregate, reinforced resin, a reinforced resin curing agent, secondary resin, a cross-linking agent, a thickening polymer material, a secondary resin curing agent and a dispersant. The self-suspension propping agent and a gel breaking method thereof realize high reverse discharging rate and cause little damage to stratum. In addition, the preparation is simple and cost is saved.
Description
Technical field
The present invention relates to oil-gas field fracturing exploitation field, particularly a kind of superconduction proppant and preparation method thereof.
Background technology
As China and World's Oil and Gas Resources are day by day exhausted, people have to develop the Low permeable oil and gas reservoirs for being difficult to harvest.
Due to the in-place permeability of oil-gas reservoir it is low, it is necessary to take pressure break means to obtain economic oil (gas) stream, it is necessary to use fracturing fluid
Proppant is brought in stratum to prevent stratum from re-closing.Proppant in prior art, typically by aggregate, binding agent, water
Soluble macromolecular material and firming agent etc. are constituted, and proppant surface does not contain cross-linking agent, only suspends by thickening agent oneself viscosity, is
Suspension effect is reached, a large amount of thickening agents are needed, is unfavorable for the row of returning and filtrate reducing, so as to aggravate formation damage.
The content of the invention
It is an object of the invention to provide one kind after breaking gel liquid viscosity decline rapidly, it is less to formation damage from suspend
Proppant and preparation method thereof.
The technical solution adopted in the present invention is：One kind is provided from suspended prop, the composition of the proppant has：Bone
Material, reinforced resin, reinforced resin firming agent, secondary resin, cross-linking agent, thickening macromolecular material, secondary resin firming agent, dispersion
Agent；The mass ratio of wherein mentioned component is：100:(0.5-3):(0.05-0.6):(0.5-3):(1-8):(0.1-0.5)：
(0.05-0.6)：(0.1-1).
Preferably, aggregate is micro- selected from drift-sand, river sand, sea sand, quartz sand or haydite, precoated sand, overlay film proppant, glass
Ball, sintered bauxite, sintered alumina, sintered zirconia.
Preferably, reinforced resin is epoxy resin or phenolic resin, and secondary resin is also selected from epoxy resin or phenolic aldehyde
Resin.
Preferably, epoxy resin be double A type epoxy resin, epoxide number 0.04-0.54mol/100g；Phenolic resin is heat
Plastic phenolic resin, 80-105 DEG C of softening point, it is 25-100s to gather speed；The firming agent that epoxy resin correspondence is adopted is for modified amine
Firming agent, amine number 200-600mgKOH/g；The firming agent that phenolic resin correspondence is adopted is for hexamethylenamine, paraformaldehyde.
Preferably, the macromolecular material of thickening power include partially hydrolyzed polyacrylamide (PHPA), its molecular weight of 200-1200 ten thousand,
Degree of hydrolysis 25%-40%；For citric acid and alum mixture, both mass ratioes are the macromolecular material firming agent for being adopted
(4-6):1。
Present invention also offers a kind of prepare the above-mentioned method from suspended prop, it is characterised in that：
Hot aggregates is lowered the temperature 10-40 DEG C to after 210-250 DEG C, then adds following composition in mass ratio successively：
Reinforced resin is added, is stirred；
Reinforced resin firming agent is added, is stirred；
Secondary resin is added, is stirred；
Cross-linking agent is added, is stirred；
Add thickening macromolecular material to be stirring evenly and then adding into macromolecular material firming agent, stir；
Dispersant is added, is stirred；
Crushing and screening, from suspended prop.
Preferably, the mixing time of reinforced resin is 5-30s；The mixing time of reinforced resin firming agent is 5-20s；It is secondary
The mixing time of resin is 3-10s；The mixing time of cross-linking agent is 1-5s；The mixing time of thickening macromolecular material is 5-10s；
The mixing time of macromolecular material firming agent is 5-20s；The mixing time of dispersant is 10s.
Preferably, the reinforced resin be double A type epoxy resin, epoxide number 0.04-0.54mol/100g；Or for phenol
Urea formaldehyde is thermoplastic phenolic resin, and 80-105 DEG C of softening point gathers speed for 25-100s；The firming agent that epoxy resin correspondence is adopted
For modified amine curing agent, amine number 200-600mgKOH/g；The firming agent that phenolic resin correspondence is adopted is for hexamethylenamine, poly first
Aldehyde.
Preferably, the macromolecular material of thickening power include partially hydrolyzed polyacrylamide (PHPA), its molecular weight of 200-1200 ten thousand,
Degree of hydrolysis 25%-40%；For citric acid and alum mixture, both mass ratioes are the macromolecular material firming agent for being adopted
(4-6):1。
Preferably, it is characterised in that for blender, and with control module, the time stirred every time exists the equipment for being adopted
It is manually entered before beginning.
The present invention is compared with prior art：The comprcssive strength of proppant itself is increased, while adding in outside functional layer
Polyacrylamide amine crosslinker, produces the higher mixed liquor of viscosity after stirring in water, reach suspension effect, while adding gel breaker
After viscosity of mixed liquid can be down to below 4mpas, reduce formation damage.
Specific embodiment
Proppant of the invention, its composition has：Aggregate, reinforced resin, reinforced resin firming agent, secondary resin, friendship
Connection agent, thickening macromolecular material, secondary resin firming agent, dispersant.
Compared with water-soluble resin used in the prior art, two layers of resin, namely reinforced resin are adopted in the present invention
And secondary resin, one layer is used as to strengthen proppant overall structure with (reinforced resin), and another layer can then improve the suspension of proppant
Property (secondary resin, secondary resin referred to herein refers to the resin of second addition, not with special implication), while can be big
The big consumption for reducing thickening agent in fracturing fluid.This is not the effect for simply adding water-soluble resin at twice and obtaining,
But considered and adopted cooperation between resin, resin amount and resin and aggregate, related firming agent and other reagents
After effect, the technique effect obtained after the improvement of creativeness is carried out to it.In the meantime, in addition it is also necessary to which each reagent is added
Opportunity, mixing time, the main component that stirring condition makes rational adjustment, improvement determination is obtained for entering.
Preferably, through test of many times and improvement, the mass ratio of mentioned component is：100:(0.5-3):(0.05-0.6):
(0.5-3):(1-8):(0.1-0.5)：(0.05-0.6)：(0.1-1).
Aggregate is selected from drift-sand, river sand, sea sand, quartz sand or haydite, precoated sand, overlay film proppant, glass microsphere, sintering
Bauxite, sintered alumina, sintered zirconia, synthetic resin.
Reinforced resin is epoxy resin or phenolic resin, and secondary resin is also selected from epoxy resin or phenolic resin.
Reinforced resin can be with identical or difference with the selection of secondary resin.Preferably, reinforced resin selects to be asphalt mixtures modified by epoxy resin
Fat and secondary resin select to be phenolic resin.
Epoxy resin be double A type epoxy resin, epoxide number 0.04-0.54mol/100g；Phenolic resin is thermoplasticity phenol
Urea formaldehyde, 80-105 DEG C of softening point, it is 25-100s to gather speed；Epoxy resin corresponds to the firming agent for adopting for modified amine curing agent,
Amine number 200-600mgKOH/g；The firming agent that phenolic resin correspondence is adopted is for hexamethylenamine, paraformaldehyde.
The selection of each resin and its related firming agent is not that those skilled in the art can be with usual range
The selection made of meaning, but need the combination effect for resin itself and aggregate, and the bond strength, finally of two layers of resin
The water solublity effect for reaching makes performing creative labour and is just able to what is determined.During present invention research and development, through repeatedly trial, choosing
Epoxy resin and particles of aggregates are selected, thus obtained proppant surface caking property is good, cure shrinkage is low, acidproof alkali salt and water
The superior, solidification process of property does not discharge small molecule, so as to increase the integrity of film；Phenolic resin curing thing rigidity is strong, caking property is good,
Acidproof alkali salt and water are good.
The macromolecular material of thickening power includes partially hydrolyzed polyacrylamide (PHPA), its molecular weight of 200-1200 ten thousand, degree of hydrolysis
25%-40%；For citric acid and alum mixture, both mass ratioes are (4-6) to the macromolecular material firming agent for being adopted:1.
Preferably, 5 are adopted:1 proportioning.
It is of the invention to prepare the above-mentioned method from suspended prop, it is characterised in that：
Hot aggregates is cooled to 10-40 DEG C to 210-250 DEG C, in preferably a kind of scheme, can be heated in aggregate
170 DEG C are cooled to after 210 DEG C, in another preferred version, aggregate 250 DEG C can be heated to, then are cooled to 250 DEG C；Also
After aggregate being heated to into 230 DEG C, 220 DEG C are cooled to.
Add following composition in mass ratio successively afterwards：
Reinforced resin is added, is stirred；
Reinforced resin firming agent is added, is stirred；
Secondary resin is added, is stirred；
Cross-linking agent is added, is stirred；
Add thickening macromolecular material to be stirring evenly and then adding into macromolecular material firming agent, stir；
Dispersant is added, is stirred；
Crushing and screening, from suspended prop.Preferably, the proppant particle diameter 1180-600 μm, 600-425 μm, m,
It is optimal in 425-212 μ ms.Different geological conditions, can select the proppant of different-grain diameter.It is this in crushing and screening
During, need grading system successively for the proppant particles of different-grain diameter, different crushing and screenings can be used in this case
Equipment is carried out.And due to the less proppant of particle diameter, its crushing and screening duration is longer, and produced heat is bigger, in proppant
Can there is certain impact in the performance of resin, therefore, during crushing and screening, should also sense the screening in crusberscreen
Temperature, when temperature is higher than 100 DEG C during crushing and screening, time-out is sized to screening machine, opens air-blast cooling system, to screening temperature
After spending for 40 DEG C, proceed screening, until it reaches predetermined particle size range.This is usually ignored in proppant manufacture process
One sport technique segment.
Preferably, the mixing time of reinforced resin is 5-30s；The mixing time of reinforced resin firming agent is 5-20s；It is secondary
The mixing time of resin is 3-10s；The mixing time of cross-linking agent is 1-5s；The mixing time of thickening macromolecular material is 5-10s；
The mixing time of macromolecular material firming agent is 5-20s；The mixing time of dispersant is 10s.Above-mentioned mixing time is not
The conventional selection that those skilled in the art make according to practical situation.But various matching somebody with somebody is being carried out to various mixing time sections
Than, and the final prioritization scheme obtained after the proppant particles to being formed are verified in multiple oil recovery practice.
Reinforced resin be double A type epoxy resin, epoxide number 0.04-0.54mol/100g；Or for phenolic resin for heat
Plastic phenolic resin, 80-105 DEG C of softening point, it is 25-100s to gather speed；The firming agent that epoxy resin correspondence is adopted is for modified amine
Firming agent, amine number 200-600mgKOH/g；The firming agent that phenolic resin correspondence is adopted is for hexamethylenamine, paraformaldehyde.
The macromolecular material of thickening power includes partially hydrolyzed polyacrylamide (PHPA), its molecular weight of 200-1200 ten thousand, degree of hydrolysis
25%-40%；For citric acid and alum mixture, both mass ratioes are (4-6) to the macromolecular material firming agent for being adopted:1,
Preferably, the mass ratio of citric acid and Alumen is 5:1.
For blender, and with control module, the time stirred every time is manually entered before proceeding the equipment for being adopted.
Embodiment
Aggregate is heated to into 210-250 DEG C, is lowered the temperature 40 DEG C, add reinforced resin layer, stir 5-30s, be subsequently adding supporting
Firming agent continues to stir 5-20s, second addition resin agitating 3-10s, adds cross-linking agent stirring 1-5s, adds with thickening
Complete curing agent is added after the macromolecular material 5-10s of effect, 5-20s is stirred for, dispersant stirring 10s is added, crushing and screening,
It is available from suspended prop.
Preferably, the aggregate for being adopted include but is not limited to drift-sand, river sand, sea sand, quartz sand, haydite, precoated sand,
Overlay film proppant, glass microsphere, sintered bauxite, sintered alumina, sintered zirconia, synthetic resin.
For blender, and with control module, the time stirred every time is manually entered before proceeding the equipment for being adopted.
Sedimentation experiment is carried out from suspended prop according to the application, resulting result is：Will from suspended prop with
Water 20-50 by volume:100 mixing, stir 1min, and proppant is in suspended state, and 1h is not settled；
In broken glue by according to the application from suspended prop and water 20-50 by volume:100 mixing, stir 1min,
Proppant is in suspended state, is subsequently adding 70 DEG C of heating 10min of Ammonium persulfate., and proppant sedimentation, test liquid viscosity is 4-
10 centipoises, broken glue works well.
The above, patent only of the present invention preferably specific embodiment, but the protection domain of patent of the present invention is not
This is confined to, any those familiar with the art can readily occur in the technical scope of patent diselosesll of the present invention
Change or replacement, all should cover within the protection domain of patent of the present invention.
Claims (9)
1. one kind is from suspended prop, it is characterised in that the composition of the proppant has：Aggregate, reinforced resin, reinforced resin are solid
Agent, secondary resin, cross-linking agent, thickening macromolecular material, secondary resin firming agent, dispersant；The wherein quality of mentioned component
Than for：100:(0.5-3):(0.05-0.6):(0.5-3):(1-8):(0.1-0.5)：(0.05-0.6)：(0.1-1).
2. it is as claimed in claim 1 from suspended prop, it is characterised in that aggregate is selected from drift-sand, river sand, sea sand, quartz sand
Or haydite, precoated sand, overlay film proppant, glass microsphere, sintered bauxite, sintered alumina, sintered zirconia.
3. as claimed in claim 2 from suspended prop, it is characterised in that：Reinforced resin is epoxy resin or phenolic aldehyde tree
Fat, secondary resin is also selected from epoxy resin or phenolic resin.
4. it is as claimed in claim 3 from suspended prop, it is characterised in that epoxy resin is double A type epoxy resin, epoxy
Value 0.04-0.54mol/100g；Phenolic resin is thermoplastic phenolic resin, and 80-105 DEG C of softening point gathers speed for 25-100s；Ring
Oxygen tree fat corresponds to the firming agent for adopting for modified amine curing agent, amine number 200-600mgKOH/g；Phenolic resin correspondence is adopted
Firming agent is hexamethylenamine, paraformaldehyde.
5. it is as claimed in claim 3 from suspended prop, it is characterised in that the macromolecular material of thickening power includes part water
Solution polyacrylamide, its molecular weight of 200-1200 ten thousand, degree of hydrolysis 25%-40%；The macromolecular material firming agent for being adopted is for lemon
Lemon acid and alum mixture, both mass ratioes are (4-6):1.
6. a kind of method from suspended prop prepared as described in claim 1-5, it is characterised in that：
Hot aggregates is lowered the temperature 10-40 DEG C to after 210-250 DEG C, then adds following composition in mass ratio successively：
Reinforced resin is added, is stirred；
Reinforced resin firming agent is added, is stirred；
Secondary resin is added, is stirred；
Cross-linking agent is added, is stirred；
Add thickening macromolecular material to be stirring evenly and then adding into macromolecular material firming agent, stir；
Dispersant is added, is stirred；
Crushing and screening, obtains from suspended prop.
7. the preparation method of superconduction proppant according to claim 6, it is characterised in that：The mixing time of reinforced resin is
5-30s；The mixing time of reinforced resin firming agent is 5-20s；The mixing time of secondary resin is 3-10s；The stirring of cross-linking agent
Time is 1-5s；The mixing time of thickening macromolecular material is 5-10s；The mixing time of macromolecular material firming agent is 5-20s；
The mixing time of dispersant is 10s.
8. the preparation method of superconduction proppant according to claim 7, it is characterised in that：The reinforced resin is double A
Type epoxy resin, epoxide number 0.04-0.54mol/100g；Or for phenolic resin be thermoplastic phenolic resin, softening point 80-
105 DEG C, it is 25-100s to gather speed；Epoxy resin corresponds to the firming agent for adopting for modified amine curing agent, amine number 200-
600mgKOH/g；The firming agent that phenolic resin correspondence is adopted is for hexamethylenamine, paraformaldehyde.
9. the preparation method of superconduction proppant according to claim 8, it is characterised in that the macromolecular material of thickening power
Comprising partially hydrolyzed polyacrylamide (PHPA), its molecular weight of 200-1200 ten thousand, degree of hydrolysis 25%-40%；The macromolecular material for being adopted
Firming agent is citric acid and alum mixture, and both mass ratioes are (4-6):1.
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| CN201611053034.2A CN106675548A (en) | 2016-11-25 | 2016-11-25 | Self-suspension propping agent and preparation method thereof |
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Cited By (5)
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| CN108795404A (en) * | 2017-04-27 | 2018-11-13 | 关中原 | It is a kind of for riverfrac treatment from suspended prop and preparation method thereof |
| CN111303858A (en) * | 2020-03-30 | 2020-06-19 | 北京昆仑隆源石油开采技术有限公司 | Quartz sand proppant and preparation method and preparation device thereof |
| CN111621284A (en) * | 2020-06-05 | 2020-09-04 | 西南石油大学 | Water-control scale-inhibition coated proppant and preparation method thereof |
| CN114891492A (en) * | 2022-05-24 | 2022-08-12 | 中国地质科学院勘探技术研究所 | Low-temperature self-suspension solidified sand and preparation method thereof |
| CN115873588A (en) * | 2022-11-30 | 2023-03-31 | 北京昆仑隆源石油开采技术有限公司 | Proppant and preparation method thereof |
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| CN111303858A (en) * | 2020-03-30 | 2020-06-19 | 北京昆仑隆源石油开采技术有限公司 | Quartz sand proppant and preparation method and preparation device thereof |
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| CN114891492A (en) * | 2022-05-24 | 2022-08-12 | 中国地质科学院勘探技术研究所 | Low-temperature self-suspension solidified sand and preparation method thereof |
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