CN105985766A - Proppant and preparation method thereof - Google Patents
Proppant and preparation method thereof Download PDFInfo
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- CN105985766A CN105985766A CN201510058499.6A CN201510058499A CN105985766A CN 105985766 A CN105985766 A CN 105985766A CN 201510058499 A CN201510058499 A CN 201510058499A CN 105985766 A CN105985766 A CN 105985766A
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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, and the size of the aggregate is 10-200 meshes, preferably 20-70 meshes. 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, glass microsphere, sintered bauxite, sintered alumina, burning
Knot zirconium oxide or its mixture, the size of described aggregate is 10-200 mesh, preferably 20-70 mesh, institute
State resin-coating film to be formed by binding resin and corresponding firming agent, described aggregate and resin-coating film
Weight ratio is preferably 100:3-100:13.
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
Epoxy resin and corresponding firming agent thereof are formed, on described aggregate the second layer resin-coating film of cladding by
Phenolic 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, it addition, the organo-silicon compound of active end group
The resistance to water of proppant can also be improved.
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 asphalt mixtures modified by epoxy resin
Fat, its second binding resin is phenolic 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
Preparation method:
Quartz sand 200kg (20-70 mesh) is heated to 250 DEG C, adds phenolic resin 3kg, and stirring is all
Even addition corresponding firming agent crow torr 0.6kg, stirring 80 seconds a period of times of solidification, adds addition phenol
Urea formaldehyde 3kg stirs, and adds firming agent corresponding firming agent crow torr 1kg, and stirring is to being fully cured
(during sand conglomeration), cools down, sieve prepared proppant S1 of the present invention.
Embodiment 2:
Aggregate: 200 parts
Binding resin: 20 parts
Firming agent: 5.33 parts
Preparation method:
Quartz sand 200kg (30-50 mesh) is heated to 180 DEG C and adds phenolic resin 10kg, and stirring is all
Even, add corresponding firming agent crow torr 3.73kg, stirring 50 seconds a period of times of solidification, add asphalt mixtures modified by epoxy resin
Fat 10kg, stirs a period of time, adds corresponding epoxy curing agent (amine curing agent) 1.6kg,
Stirring, to being fully cured (during sand conglomeration), cools down, sieve prepared proppant S2 of the present invention.
Embodiment 3:
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, adds epoxy resin 6kg, and stirring is all
Even, add epoxy curing agent (amine curing agent) 0.67kg, stirring solidification a period of time 60
Second, adding phenolic resin 3kg, stir, add firming agent crow torr 2.7kg, stirring is to completely
Solidification (during sand conglomeration), cools down, sieve prepared proppant S3 of the present invention.
Embodiment 4:
Aggregate: 200 parts
Binding resin: 20 parts
Firming agent: 6.733 parts
Calcium stearate: 1 part
Organo-silicon compound 0.01 part with active end group
Preparation method:
Quartz sand 200kg (20-40 mesh) is heated to 250 DEG C, adds epoxy resin 10kg, stirring
Uniformly, add epoxy curing agent (amine curing agent) 2.233kg, wait 80 seconds certain times,
Add phenolic resin 10kg, stir, add firming agent crow torr 4.5kg, stir to being fully cured,
(during sand conglomeration), adds calcium stearate 1 kilogram, continues stirring 90 seconds, adds and carries active end
The organo-silicon compound of base 0.01 kilogram, stir cooling, prepared support of the present invention of sieving in 90 seconds
Agent S4.
Embodiment 5:
Aggregate: 200 parts
Binding resin: 20 parts
Firming agent: 3 parts
Calcium stearate: 0.5 part
Preparation method:
Quartz sand 200kg (20-40 mesh) is heated to 200 DEG C, adds unsaturated polyester resin 10kg,
Stir, add acyl peroxide class firming agent 1.5kg, stirring 80 seconds certain times of solidification, add
Unsaturated polyester resin 10kg, stirs, and adds acyl peroxide class firming agent 1.5kg, and stirring is extremely
It is fully cured, (during sand conglomeration), adds calcium stearate 0.5 kilogram, continue stirring 180 seconds, cold
But, sieve prepared proppant S5 of the present invention.
Embodiment 6:
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 S6 of the present invention.
Embodiment 7:
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 (20-70 mesh) is heated to 350 DEG C, then cools to
250 DEG C, add epoxy resin 10kg, stir 120 seconds certain times, add epoxy curing agent
(amine curing agent) 1.8kg, stirring 5 seconds certain times of solidification, adds epoxy resin 10kg, etc.
Treat certain time 25 seconds, add firming agent epoxy curing agent (amine curing agent) 1.8kg, etc.
Treat certain time 120 seconds, add the organo-silicon compound 0.05kg with active end group and stearic acid
Calcium 1kg, continuation stirring cools down for 180 seconds, sieve prepared proppant S7 of the present invention.
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: 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 ring
Epoxy resins 3kg, stirs, and adds corresponding epoxy curing agent (amine curing agent) 0.48kg, stirs
Mix solidification 8 seconds, add phenolic resin 3kg, stir 14 seconds certain times, add corresponding firming agent crow
Torr 1.12kg, stirring 60 seconds certain times of solidification, there was added organic silicon compound 10g, continues stirring
180 seconds, cool down, sieve prepared proppant S8.
Embodiment 9:
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
Calcium stearate 0.5 part
The organo-silicon compound of active end group: 0.01 part
Preparation method:
Quartz sand 200kg (40-60 mesh) is heated to 200 DEG C, then cools to 180 DEG C, adds ring
Epoxy resins 5kg, stirs, and adds corresponding epoxy curing agent (amine curing agent) 1.2kg,
Stirring solidification 10 seconds, adds phenolic resin 4kg, stirs 15 seconds, add corresponding firming agent crow torr
0.8kg, stirring solidification 40 seconds, add the organo-silicon compound 10g of active end group, stir 60 seconds,
Add calcium stearate 0.5kg, stir 100 seconds, cool down, sieve prepared proppant S9.
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 250 DEG C, adds phenolic resin 6kg, waits one
Fix time 50 seconds and add corresponding firming agent crow torr 1.6kg, wait that 80 seconds certain times, (sand was tied
During group), there was added organic silicon compound 10g, continuation stirring cools down for 100 seconds, sieve prepared proppant
D1。
Comparative example 2:
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 parts
Calcium stearate: 0.5 part
Preparation method:
Quartz sand 200kg (20-40 mesh) is heated to 200 DEG C, adds unsaturated polyester resin 20kg,
Stirring, add acyl peroxide class firming agent 3kg, stirring solidification 80 seconds certain times stirring is to complete
All solidstate, (during sand conglomeration), add calcium stearate 0.5 kilogram, continue stirring 180 seconds, cool down,
Sieve prepared proppant D2.
Comparative example 3:
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 the prepared present invention
Described proppant D3.
According to standard SY/T5108-2006 to above-described embodiment 1～9 gained proppant S1～S9, and contrast
Proppant D1～D3 of example 1～3 gained carries out performance detection, and testing result is shown in Table 1:
Table 1 embodiment 1～9 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 1S1 | 0.78 | 75 | 2.5 |
| Embodiment 2S2 | 0.80 | 81 | 1.5 |
| Embodiment 3S3 | 0.78 | 81 | 1.8 |
| Embodiment 4S4 | 0.80 | 78 | 1.6 |
| Embodiment 5S5 | 0.81 | 73 | 2.3 |
| Embodiment 6S6 | 0.82 | 74 | 1.7 |
| Embodiment 7S7 | 0.81 | 80 | 1.1 |
| Embodiment 8S8 | 0.85 | 84 | 1.2 |
| Embodiment 9S9 | 0.85 | 85 | 1.0 |
| Comparative example 1D1 | 0.70 | 70 | 5.4 |
| Comparative example 2D2 | 0.72 | 75 | 3.9 |
| Comparative example 3D3 | 0.65 | 70 | 4.8 |
Above-mentioned result of the test fully shows, proppant S1～S9 obtained by the present invention prepares with comparative example
Proppant D1～D3 compare, possess preferable performance parameter, be embodied in outward appearance, intensity,
The many aspects such as percentage of damage.
From test result it can be seen that proppant S1～S9 has good sphericity and intensity, anti-
Breaking capacity is strong, proppant S3 S4 S8 S9 be the first binding resin be epoxy resin, the second bonding
Resin is phenolic resin, has good sphericity, individual seed strength and resistant to breakage ability, this is because
(physics of phenolic resin and epoxy resin itself is special for the resin molding that both on aggregate is the most different
Property causes), the feature of intensity and toughness can be taken into account, reach more preferable effect.Particularly embodiment
The proppant S8 of 8～9 gained S9, there is more excellent intensity and resistant to breakage ability.In embodiment
In the preparation process of 8～9, step 2 is after adding the first knot resin and corresponding firming agent thereof, rapidly
Add the second binding resin.Now, the first binding resin is not yet fully hardened, the second bonding of addition
Resin can form, with the first binding resin, the transition structure being cross-linked with each other at interlayer.The mistake of this crosslinking
Crossing structure and can improve the sphericity of proppant, intensity and durability, resistant to breakage ability is strong, leads for a long time
Flow 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 (7)
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, and described aggregate is 100:3-100:13 with the weight ratio of resin-coating film, described aggregate
A size of 10-200 mesh.
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 2, it is characterised in that cladding on described aggregate
Ground floor resin-coating film is formed by epoxy resin and corresponding firming agent thereof, cladding on described aggregate
Second layer resin-coating film is formed by phenolic resin and corresponding firming agent thereof.
4. the preparation method of the arbitrary described proppant of claims 1 to 3, it is characterised in that bag
Include:
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 4, it is characterised in that described first bonding tree
Fat is epoxy resin, and described second binding resin is phenolic resin.
Preparation method the most according to claim 4, it is characterised in that add in described step 2
Mixing time after corresponding firming agent is the 5-10 second.
Preparation method the most according to claim 6, it is characterised in that add in described step 3
Entering the mixing time after the second binding resin is the 15-90 second, stirring after adding corresponding firming agent
The time of mixing is the 10-120 second.
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| CN106701056A (en) * | 2016-12-28 | 2017-05-24 | 中国建材国际工程集团有限公司 | Method for preparing low-density fracturing proppant by utilizing sinking beads of hollow glass beads |
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| CN109575907B (en) * | 2017-09-28 | 2021-01-01 | 中国石油天然气股份有限公司 | Proppant and preparation method thereof |
| CN108751915A (en) * | 2018-06-28 | 2018-11-06 | 中国石油天然气股份有限公司 | A kind of bottom water reservoir water blockoff pressure break overlay film proppant and preparation method |
| CN108751915B (en) * | 2018-06-28 | 2022-02-01 | 中国石油天然气股份有限公司 | Water plugging fracturing tectorial membrane proppant for bottom water reservoir and preparation method |
| CN111334274A (en) * | 2020-02-19 | 2020-06-26 | 北京昆仑隆源石油开采技术有限公司 | Low-temperature consolidated sand and preparation method thereof |
| CN113308237A (en) * | 2021-04-21 | 2021-08-27 | 四川省帕提科斯能源科技有限公司 | High-strength propping agent for fracturing and preparation method thereof |
| CN113174244A (en) * | 2021-05-13 | 2021-07-27 | 北京昆仑隆源石油开采技术有限公司 | Tectorial membrane proppant and preparation method thereof |
| CN114479823A (en) * | 2021-12-31 | 2022-05-13 | 宁波锋成先进能源材料研究院有限公司 | Fracturing propping agent and preparation method and application thereof |
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