CN105985767A - Proppant and preparation method thereof - Google Patents
Proppant and preparation method thereof Download PDFInfo
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- CN105985767A CN105985767A CN201510058502.4A CN201510058502A CN105985767A CN 105985767 A CN105985767 A CN 105985767A CN 201510058502 A CN201510058502 A CN 201510058502A CN 105985767 A CN105985767 A CN 105985767A
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- proppant
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Abstract
The invention discloses a proppant and a preparation method thereof, and belongs to the technical field of oil and gas exploitation. The proppant comprises an aggregate and at least two layers of resin coated films coated on the aggregate, wherein the weight ratio of the aggregate to the resin coated film is 100:3-100:13; and the aggregate is quartz sand, ceramsite, glass microspheres, sintered bauxite, sintered aluminum oxide, sintered zirconium oxide or a mixture thereof. By virtue of a multilayer film coating technology, the sphericity of the proppant can be improved, the density of the proppant can be reduced, and the chemical inertness and strength can be improved. The proppant disclosed by the invention can be widely applied to oil and gas field exploitation, is beneficial to improvement of the sand ratio, reduces the usage of fracturing fluid, eases the embedding of the proppant, improves the water resistance of the proppant, improves the fracture conductivity, and prolongs the effective fracturing period.
Description
Technical field
The present invention relates to oil gas field field, particularly relate to a kind of proppant and preparation method thereof.
Background technology
In oilfield explorating developing process, the exploration of hypotonic oil gas field the most hypotonic, special and exploitation
In transformation with old Oil/gas Well, pressure break has become as volume increase and improves the Main Means of recovery ratio.
In fracturing process, the effect of proppant is extremely important.The proppant when formation crack, stratum
Addition make crack keep by holding state, proppant defines a medium for supporting crack,
Extraction for oil gas provides conduction pathway.Therefore selecting proppant is the key that oil gas field increases production.
Proppant is brought into by fracturing fluid and is supported in the crack of fracturing stratum, thus effectively by oil gas
Import Oil/gas Well, increase substantially oil and gas production and extend the oil well life-span.Proppant is for having certain grain
Degree and the natural sand of grating or artificial high strength ceramics granule etc., the normal coated with resins of sand grains or haydite surface,
To improve intensity and the guide performance of proppant further.
The most domestic and international proppant used by fracturing technology is mainly haydite, quartz sand and resin coating and props up
Support agent.
Haydite be usually metallic aluminium, the oxide of silicon and other Ore sinter (US4,977,116,
EP0207668A), middle-deep well fracturing technology it is mainly used in.Ceramisite sintered temperature is high, and energy consumption is big,
The poor water resistance when sintering incomplete, and cost is high, density is big, construction risk is high.
Quartz sand refers generally to, from natural silica sand, be mainly used in the pressure break of shallow-layer low clossing pressure well
Operation, profile is similar to spherical, and to make it have certain mobility, quartz sand intensity is relatively low,
Resistant to breakage ability is poor.The most also it is difficult to meet the requirement of growing Fracturing Technology.
Resin coated propping agent refers to that surface coating has the haydite of a lamination resin or quartz sand to carry
The resistant to breakage ability of high proppant.But owing to subsurface environment is extremely complex, the resin molding of proppant surface
Can be corroded and destroyed, cause the burn into of clad to degrade, come off, thus cause formation fractures
Being substantially reduced of flow conductivity.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of proppant and preparation method thereof, can improve
The sphericity of proppant, reduces proppant density, improves chemical inertness and intensity.
For solving above-mentioned technical problem, the present invention provides technical scheme as follows:
Proppant of the present invention, including aggregate and at least 2 layers of resin-coating being coated on aggregate
Film, described aggregate is quartz sand, haydite, precoated sand, glass microsphere, sintered bauxite, sintering oxygen
Change aluminum, sintered zirconia, synthetic resin one or more；Described resin-coating film is by binding resin
Formed with corresponding firming agent.
Proppant of the present invention, multi-layer resinous coating film composition can be identical or different.Described bone
Material is preferably 100:3-100:13 with the weight ratio of resin-coating film.
Binding resin of the present invention is phenolic resin, epoxy resin, furane resins, unsaturated polyester (UP)
One or more of the macromolecular materials such as resin, vinylite, organic siliconresin；Described bonding tree
When fat is phenolic resin, its corresponding firming agent be crow torr, paraformaldehyde, the one of hexamethylenetetramine
Plant or several；When described binding resin is epoxy resin, its corresponding firming agent is amine curing agent
One or more；When described binding resin is furane resins, its corresponding firming agent is benzenesulfonic acid, first
Benzenesulfonic acid, xylene monosulfonic acid one or more；When described binding resin is unsaturated polyester resin,
Its corresponding firming agent be acyl peroxide class, peroxyesters one or more；Described binding resin
During for vinylite, its corresponding firming agent is acyl peroxide class, the one of peroxyesters or several
Kind.
Proppant of the present invention, it is preferred that on its aggregate cladding ground floor resin-coating film by
Phenolic resin and corresponding firming agent thereof are formed, on described aggregate the second layer resin-coating film of cladding by
Epoxy resin and corresponding firming agent thereof are formed.
Proppant of the present invention, goes back the organosilicon of the active end group of clad strip on resin-coating film
Compound or calcium stearate.Organo-silicon compound or the calcium stearate of the active end group added play lubrication
The effect of agent, it is ensured that the integrity of overlay film proppant.
Proppant of the present invention is preferably dimensioned to be 10-100 mesh, is shaped as spherical or approximation ball
Shape；The size of described aggregate is 10-100 mesh.Further, the size of described proppant is 20-70
Mesh, the size of described aggregate is 20-70 mesh.
The preparation method of proppant of the present invention, including:
Step 1: aggregate is heated to 150～400 DEG C, is then cooled to 160～250 DEG C；
Step 2: add the first binding resin, be stirred, adds corresponding firming agent afterwards, carries out
Mixing time a；
Step 3: add the second binding resin, be stirred, adds corresponding firming agent afterwards, enters
Row mixing time.
The preparation method of proppant of the present invention, it is also possible to include step 4: add the 3rd bonding
Resin, is stirred, and adds corresponding firming agent afterwards, is stirred.
The preparation method of proppant of the present invention, it is preferred that its first binding resin is phenolic aldehyde tree
Fat, its second binding resin is epoxy resin.
The preparation method of proppant of the present invention, it is preferred that the mixing time of described step 2 is
The 5-10 second.Preferably, adding the mixing time after the second binding resin in described step 3 is 15-90
Second, adding the mixing time after corresponding firming agent is the 10-120 second.
The method have the advantages that
1) sphericity of proppant is improved
Multilayer coating film can make this effect more preferable, and multilayer coating film can be in the more tree of aggregate surface overlay film
Fat, the rough place of aggregate surface is padded more round, and interparticle porosity is higher, has more
High flow conductivity.
2) density of proppant is reduced
Resin coating rear support agent density reduces, and amount of resin is the biggest, and density is the lowest.
3) chemical-resistance is more stable
Film covered resin amount is the highest, and film is the thickest, and the ability such as acid resistance, alkali resistance, resistance to water is greatly improved.
4) intensity is higher
Film covered resin amount is the highest, and film is the thickest, and particle surface stress disperses evenly, and spheroid can bear more
High load and do not crush, favourable to flow conductivity.
5) durability is longer
Resin coating is the most, and film is the thickest, even if aggregate is crushed, the chip of generation is preferably wrapped by
The migration of chip, fine powder, the beneficially flow conductivity of proppant will not be produced in resin shell.
6), when preparing proppant, aggregate is used first to heat the method being stirred for Temperature fall, stirred
Journey carries out heat exchange, makes aggregate temperature uniformity.
7) using same resin demand, multilayer coating film proppant and one layer of overlay film proppant are compared,
Its resin molding bonding is more firmly, overlay film rate is higher, resin molding more completely, more closely knit, have higher
Intensity, acid solubility etc..
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the preparation method of the proppant of the present invention.
Detailed description of the invention
For making the solving the technical problem that of the present invention, technical scheme and advantage clearer, below will
It is described in detail in conjunction with the drawings and the specific embodiments.
Embodiment 1:
Proppant of the present invention is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 6 parts
Firming agent: 1.6 parts
Organo-silicon compound: 0.01 part
Preparation method:
Quartz sand 200kg (20-40 mesh) is heated to 300 DEG C, then cools to 250 DEG C, adds phenol
Urea formaldehyde 3kg, waits that 50 seconds certain times added corresponding firming agent crow torr 1.12kg, waits certain
10 seconds time, add epoxy resin 3kg, wait 15 seconds certain times, add respective rings epoxy resins
Firming agent (amine curing agent) 0.48kg, waits 80 seconds certain times (during sand conglomeration), adds
Organo-silicon compound 10g, continuation stirring cools down for 100 seconds, sieve prepared proppant of the present invention.
Embodiment 2:
Proppant of the present invention is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 20 parts
Firming agent: 5.33 parts
Organo-silicon compound: 0.05 part
Preparation method:
Quartz sand 200kg (30-50 mesh) is heated to 180 DEG C, then cools to 160 DEG C, adds phenol
Urea formaldehyde 10kg, when waiting 90 seconds certain times, adds corresponding firming agent crow torr 3.73kg, waits
5 seconds certain times, add epoxy resin 10kg, wait 50 seconds certain times, add corresponding epoxy
Resin curing agent (amine curing agent) 1.6kg, waits 20 seconds certain times (during sand conglomeration), adds
Entering organo-silicon compound 50g, continuation stirring cools down for 180 seconds, sieve prepared proppant of the present invention.
Embodiment 3:
Proppant of the present invention is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 9 parts
Firming agent: 3.37 parts
Calcium stearate: 0.075 part
Preparation method:
Quartz sand 200kg (40-60 mesh) is heated to 200 DEG C, then cools to 160 DEG C, adds phenol
Urea formaldehyde 6kg, when waiting 40 seconds certain times, adds firming agent crow torr 2.7kg, waits a timing
Between 8 seconds, add epoxy resin 3kg, wait 45 seconds certain times, add epoxy curing agent (amine
Class firming agent) 0.67kg, wait 120 seconds certain times (during sand conglomeration), add calcium stearate
0.075 part, continue stirring 40 seconds, cool down, sieve prepared proppant of the present invention.
Embodiment 4:
Proppant of the present invention is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 20 parts
Firming agent: 6.733 parts
Calcium stearate: 1 part
Preparation method:
Quartz sand 200kg (50-100 mesh) is heated to 250 DEG C, then cools to 180 DEG C, adds
Phenolic resin 10kg, waits 80 seconds certain times, adds firming agent crow torr 4.5kg, waits certain
15 seconds time, add epoxy resin 10kg, wait 40 seconds certain times, add epoxy resin cure
Agent (amine curing agent) 2.233kg, waits 30 seconds certain times (during sand conglomeration), adds hard
Fat acid calcium 1 part, continues stirring 180 seconds, cools down, sieve prepared proppant of the present invention.
Embodiment 5:
Proppant of the present invention is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 8 parts
Firming agent: 1.44 parts
Organo-silicon compound 0.005 part with active end group
Preparation method:
Quartz sand 200kg (40-60 mesh) is heated to 400 DEG C, then cools to 250 DEG C, adds ring
Epoxy resins 4kg, waits 90 seconds certain times, adds epoxy curing agent (amine curing agent)
0.72kg, waits 90 seconds certain times, adds epoxy resin 4kg, waits 45 seconds certain times,
Add firming agent epoxy curing agent (amine curing agent) 0.72kg, wait 120 seconds certain times,
Add the organo-silicon compound 0.005kg with active end group, continue stirring cooling in 80 seconds, cross sieve series
Obtain proppant of the present invention.
Embodiment 6:
Proppant of the present invention is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 20 parts
Firming agent: 3.6 parts
Organo-silicon compound with active end group: 0.05 part
Calcium stearate: 1 part
Preparation method:
Quartz sand heats, and quartz sand 200kg (80-100 mesh) is heated to 350 DEG C, then cools to
250 DEG C, add epoxy resin 10kg, wait 120 seconds certain times, add epoxy curing agent
(amine curing agent) 1.8kg, waits 14 seconds certain times, adds epoxy resin 10kg, waits one
Fix time 25 seconds, add firming agent epoxy curing agent (amine curing agent) 1.8kg, wait one
Fix time 120 seconds, add organo-silicon compound 0.05kg and calcium stearate 1kg with active end group,
Continue stirring cooling in 180 seconds, sieve prepared proppant of the present invention.
Embodiment 7:
Proppant of the present invention is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 6 parts
Firming agent: 1.6 parts
Organo-silicon compound: 0.01 part
Preparation method:
Quartz sand 200kg (40-60 mesh) is heated to 200 DEG C, then cools to 180 DEG C, adds phenol
Urea formaldehyde 3kg, waits 90 seconds certain times, adds corresponding firming agent crow torr 1.12kg, waits one
Fix time 60 seconds, add epoxy resin 3kg, wait 14 seconds certain times, add respective rings oxygen tree
Fat firming agent (amine curing agent) 0.48kg, waits 60 seconds certain times, there was added organic silicon compound
10g, continues stirring 180 seconds, cools down, sieve prepared proppant.
Embodiment 8:
Proppant of the present invention is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 9 parts
Firming agent: 2 parts
Organo-silicon compound: 0.01 part
Preparation method:
Quartz sand 200kg (40-60 mesh) is heated to 200 DEG C, then cools to 180 DEG C, adds phenol
Urea formaldehyde 4kg, waits 90 seconds certain times, adds corresponding firming agent crow torr 0.8kg, waits certain
40 seconds time, add epoxy resin 5kg, wait 60 seconds certain times, add respective rings epoxy resins
Firming agent (amine curing agent) 1.2kg, waits 100 seconds certain times, there was added organic silicon compound
10g, continues stirring 180 seconds, cools down, sieve prepared proppant.
Comparative example 1:
Proppant is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 6 parts
Firming agent: 1.6 parts
Organo-silicon compound: 0.01 part
Preparation method:
Quartz sand 200kg (20-40 mesh) is heated to 300 DEG C, then cools to 250 DEG C, adds phenol
Urea formaldehyde 6kg, waits that 50 seconds certain times added corresponding firming agent crow torr 1.6kg, waits a timing
Between 80 seconds (during sand conglomeration), there was added organic silicon compound 10g, continue stirring 100 seconds, cooling,
Sieve prepared proppant.
Comparative example 2:
Proppant is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 9 parts
Firming agent: 2 parts
Organo-silicon compound: 0.01 part
Quartz sand 200kg (40-60 mesh) is heated to 200 DEG C, then cools to 180 DEG C, adds phenol
Urea formaldehyde 9kg, waits 90 seconds certain times, adds corresponding firming agent crow torr 2kg, waits a timing
Between 60 seconds, there was added organic silicon compound 10g, continue stirring 180 seconds, cool down, sieving to prepare supports
Agent.
Comparative example 3:
Proppant is made up of by ratio of weight and the number of copies following component:
Aggregate: 200 parts
Binding resin: 20 parts
Firming agent: 3.6 parts
Organo-silicon compound with active end group: 0.05 part
Calcium stearate: 1 part
Preparation method:
Quartz sand heats, and quartz sand 200kg (80-100 mesh) is heated to 350 DEG C, then cools to
250 DEG C, add epoxy resin 20kg, wait 120 seconds certain times, add epoxy curing agent
(amine curing agent) 3.6kg, waits 120 seconds certain times, adds organic with active end group
Silicon compound 0.05kg and calcium stearate 1kg, continuation stirring cools down for 180 seconds, sieve prepared proppant.
According to standard SY/T5108-2006 to above-described embodiment 1～8 and the support for preparing of comparative example 1～3
Agent carries out performance detection, and testing result is shown in Table 1:
Table 1 embodiment 1～8 and the proppant for preparing of comparative example 1～3 carry out performance detection
| Project | Sphericity | Single particle strength, N | Percentage of damage (%) (69MPa) |
| Embodiment 1 | 0.81 | 79 | 1.1 |
| Embodiment 2 | 0.80 | 81 | 1.5 |
| Embodiment 3 | 0.78 | 81 | 1.1 |
| Embodiment 4 | 0.80 | 78 | 1.6 |
| Embodiment 5 | 0.81 | 73 | 2.3 |
| Embodiment 6 | 0.82 | 74 | 2.2 |
| Embodiment 7 | 0.81 | 78 | 1.5 |
| Embodiment 8 | 0.75 | 79 | 1.8 |
| Comparative example 1 | 0.70 | 70 | 5.4 |
| Comparative example 2 | 0.65 | 65 | 4.3 |
| Comparative example 3 | 0.65 | 70 | 4.8 |
Above-mentioned result of the test fully shows, the proppant (embodiment 1～8) obtained by the present invention and contrast
Proppant obtained by example 1～3 is compared, and possesses preferable performance parameter, is embodied in outward appearance, strong
The many aspects such as degree, percentage of damage.
From test result it can be seen that the proppant of embodiment 1～8 all has good sphericity with strong
Degree, resistant to breakage ability is strong, embodiment 1～4 and embodiment 7～8 be the first binding resin be phenolic resin,
Second binding resin is epoxy resin, has good sphericity, individual seed strength and resistant to breakage ability,
This is because resin molding (phenolic resin and epoxy resin itself that both on aggregate is the most different
Physical characteristic cause), the feature of intensity and toughness can be taken into account, reach more preferable effect.Especially
It is the proppant of embodiment 1～3 gained, there is more excellent intensity and resistant to breakage ability.Implementing
In the preparation process of example 1～3, step 2 is after adding the first knot resin and corresponding firming agent thereof, fast
Speed adds the second binding resin.Now, the first binding resin is not yet fully hardened, and the second of addition is glued
Knot resin can form, with the first binding resin, the transition structure being cross-linked with each other at interlayer.This crosslinking
Transition structure can improve the sphericity of proppant, intensity and durability, and resistant to breakage ability is strong, for a long time
Water conservancy diversion is effective.
The above is the preferred embodiment of the present invention, it is noted that general for the art
For logical technical staff, on the premise of without departing from principle of the present invention, it is also possible to make some changing
Entering and retouch, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a proppant, it is characterised in that include aggregate and at least 2 layers be coated on aggregate
Resin-coating film, described aggregate is quartz sand, haydite, glass microsphere, sintered bauxite, sintering oxygen
Change aluminum, sintered zirconia or its mixture；Described resin-coating film is by binding resin and corresponding solidification
Agent is formed.
Proppant the most according to claim 1, it is characterised in that described aggregate and resin bag
The weight ratio of overlay film is 100:3-100:13.
Proppant the most according to claim 1, it is characterised in that described binding resin is phenol
Urea formaldehyde, epoxy resin, furane resins, unsaturated polyester resin, vinylite, organosilicon tree
One or more of the macromolecular materials such as fat；When described binding resin is phenolic resin, it is solid accordingly
Agent be crow torr, paraformaldehyde, hexamethylenetetramine one or more；Described binding resin is ring
During epoxy resins, its corresponding firming agent is one or more of amine curing agent；Described binding resin is
During furane resins, its corresponding firming agent be benzenesulfonic acid, toluenesulfonic acid, the one of xylene monosulfonic acid or
Several；When described binding resin is unsaturated polyester resin, its corresponding firming agent be acyl peroxide class,
One or more of peroxyesters；When described binding resin is vinylite, it solidifies accordingly
Agent be acyl peroxide class, peroxyesters one or more.
Proppant the most according to claim 3, it is characterised in that cladding on described aggregate
Ground floor resin-coating film is formed by phenolic resin and corresponding firming agent thereof, cladding on described aggregate
Second layer resin-coating film is formed by epoxy resin and corresponding firming agent thereof.
5. according to the proppant described in any claim in Claims 1-4, it is characterised in that
The size of described proppant is 10-200 mesh, is shaped as spherical or almost spherical；The chi of described aggregate
Very little for 10-200 mesh.
Proppant the most according to claim 5, it is characterised in that the size of described proppant is
20-40 mesh, the size of described aggregate is 20-70 mesh.
7. the preparation method of the proppant described in claim 1, it is characterised in that including:
Step 1: aggregate is heated to 150～400 DEG C, is then cooled to 160～250 DEG C；
Step 2: add the first binding resin, be stirred, adds corresponding firming agent afterwards, enters
Row stirring；
Step 3: add the second binding resin, be stirred, adds corresponding firming agent afterwards, enters
Row stirring.
Preparation method the most according to claim 7, it is characterised in that described first bonding tree
Fat is phenolic resin, and described second binding resin is epoxy resin.
9. according to the preparation method described in claim 7 or 8, it is characterised in that described step 2
Mixing time after the corresponding firming agent of middle addition is the 5-10 second.
10. according to the preparation method described in claim 7 or 8, it is characterised in that described step 3
Mixing time after middle addition the second binding resin is the 15-90 second, after adding corresponding firming agent
Mixing time be the 10-120 second.
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| CN111621284A (en) * | 2020-06-05 | 2020-09-04 | 西南石油大学 | Water-control scale-inhibition coated proppant and preparation method thereof |
| CN117181990A (en) * | 2023-10-07 | 2023-12-08 | 胜利油田金岛实业有限责任公司 | High-temperature-resistant precoated sand and preparation method thereof |
| CN117181990B (en) * | 2023-10-07 | 2024-03-19 | 胜利油田金岛实业有限责任公司 | High-temperature-resistant precoated sand and preparation method thereof |
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