CN106751695A - A kind of spherical gel particle and preparation method thereof - Google Patents
A kind of spherical gel particle and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of spherical gel particle and preparation method thereof.The spherical gel particle that the present invention is provided is prepared by the raw material including following components：The mass parts of bis-phenol base propane 15~20, the mass parts of epoxychloropropane 20~30, the mass parts of toluene 5~15, the mass parts of alkali compounds 6~8, the mass parts of water 9~12, the mass parts of curing agent 10~15, the mass parts of SILICA FUME 5~15, the mass parts of carbon fiber 2~3, the mass parts of density adjuster 0~50.The present invention prepares material of main part by raw material of bis-phenol base propane, epoxychloropropane, toluene, alkali compounds and water, using SILICA FUME as packing material, using carbon fiber as skeleton bridging materials, the density of spherical gel is adjusted by adding density adjuster, addition curing agent adjustment hardening time, the spherical gel particle for obtaining is water insoluble and oil, hardening time is controllable and solidification after bearing capacity it is high.
Description
Technical field
The present invention relates to oil gas field of engineering technology, more particularly to a kind of spherical gel particle and preparation method thereof.
Background technology
Leakage is the great difficult problem that a kind of restriction drilling well is smoothed out in drilling process, when its time for spending accounts for total drilling well
Between 10% or so, and a series of complex situation such as bit freezing, blowout, well slough can be brought.Particularly in brill chance crack, tomography etc.
During large-scale leakage, drilling fluid is constantly missed in crack or solution cavity, and cannot complete circulation, the phenomenon for " only import but no export " occur,
So that drillng operation cannot continue.Drilling well loss circulation material is essential material during drilling well leak-proof leak-stopping, and drilling well is prevented
The success rate for leaking leak stopping directly depends on the quality of loss circulation material performance.
At present, traditional bridging material and cement injection, but above-mentioned leak stopping material are mainly used for the treatment of conventional leakage
Material is difficult to be stopped in drop ply, is easily influenceed by formation fluid, it is impossible to meet needs；Even material can become under high-temperature and high-pressure conditions
Soft, corrosion, causes leak stopping failure or secondary leakage, it is impossible to fundamentally solve the problems, such as leakage.
Chinese invention patent CN 101353569A disclose a kind of controllable cross-linked gel water blockoff leak stopping for oil gas field
Material, the gel loss circulation material can carry out retarded crosslinking reaction in adding water soluble condensation polymer HPAM solution, obtain motionless strong solidifying
Glue；Chinese invention patent CN 102634325A disclose a kind of parcel high volence metal ion retarded crosslinking gel water-plugging loss circulation material,
The loss circulation material and stabilizer are added in the HPAM aqueous solution, can obtain motionless gel；Chinese invention patent CN 102358771A
Disclose a kind of temperature resistance, without crosslinking, degradable GEL USED FOR PLUGGING WELL LOST CIRCULATION, the sealing agent dissolving after formed shear thinning behavior tie well
Configuration gel.But above-mentioned several loss circulation materials all have certain deficiency and defect, such as water-fast, fuel tolerance capability is weak, plugging strength
It is low, it is impossible to which that solidification or hardening time are whard to control etc..
The content of the invention
It is an object of the invention to provide a kind of spherical gel particle and preparation method thereof.The spherical gel that the present invention is provided
Particle is water insoluble and oil, hardening time is controllable and solidification after bearing capacity it is high.
The invention provides a kind of spherical gel particle, prepared by the raw material including following components：
The mass parts of bis-phenol base propane 15~20；
The mass parts of epoxychloropropane 20~30；
The mass parts of toluene 5~15；
The mass parts of alkali compounds 6~8；
The mass parts of water 9~12；
The mass parts of curing agent 10~15；
The mass parts of SILICA FUME 5~15；
The mass parts of carbon fiber 2~3；
The mass parts of density adjuster 0~50.
Preferably, the curing agent include imidazole curing agent and aromatic amine curing agent in one or two.
Preferably, the imidazole curing agent is including in 2-methylimidazole, 2-ethyl-4-methylimidazole and 2- phenylimidazoles
One kind.
Preferably, the average grain diameter of the SILICA FUME is 0.5~1.5 μm.
Preferably, the filament diameter of the carbon fiber is 5~10 μm, and the length of carbon fiber is 0.6~1.5mm.
Preferably, the density adjuster is in blanc fixe, agstone, Iron Ore Powder, ilmenite powder and galena powder
One or two.
Present invention also offers the preparation method of spherical gel particle described in above-mentioned technical proposal, comprise the following steps：
(1) bis-phenol base propane, epoxychloropropane, toluene, alkali compounds and water are mixed, polycondensation reaction obtains forerunner
Body；
(2) presoma for obtaining the step (1) is mediated with SILICA FUME, carbon fiber, density adjuster and curing agent, is obtained
To mixed material；
(3) the mixed material granulation for obtaining the step (2), obtains spherical gel particle.
Preferably, the temperature of polycondensation reaction is 55~85 DEG C in the step (1), and the time of polycondensation reaction is 4~8h.
Preferably, the temperature mediated in the step (2) is 60~70 DEG C, and the time of kneading is 20~30min.
Preferably, the granulation in the step (3) is mist projection granulating.
The invention provides a kind of spherical gel particle, prepared by the raw material including following components：Bis-phenol base propane
15~20 mass parts, the mass parts of epoxychloropropane 20~30, the mass parts of toluene 5~15, the mass parts of alkali compounds 6~8, water 9
~12 mass parts, the mass parts of curing agent 10~15, the mass parts of SILICA FUME 5~15, the mass parts of carbon fiber 2~3, density adjuster 0
~50 mass parts.The present invention prepares main body material by raw material of bis-phenol base propane, epoxychloropropane, toluene, alkali compounds and water
Material, using SILICA FUME as packing material, using carbon fiber as skeleton bridging materials, adjusts spherical solidifying by adding density adjuster
The density of glue, addition curing agent adjustment hardening time, the spherical gel particle for obtaining is water insoluble and oil, will not be by mud or ground
Layer fluid invades dirt, will not also pollute wellbore fluids；Under temperature pressure function, intensity gradually strengthens the spherical gel particle,
Until solidification, hardening time it is controllable and solidification after bearing capacity it is high.Test result indicate that, the spherical gel particle that the present invention is provided
4~10h is curable, and bearing capacity is up to 12MPa after solidification.
The spherical gel particle raw material sources that the present invention is provided are wide, and preparation method is simple, cost economy, it is adaptable to big rule
Mould industrial production.
Brief description of the drawings
Fig. 1 is hardening time and strength development tendency chart of the spherical gel particle at 80 DEG C in embodiment 1~5；
Fig. 2 is spherical gel particle hardening time at different temperatures and strength development tendency chart in embodiment 3；
Fig. 3 is hardening time and strength development tendency chart of the spherical gel particle at 80 DEG C in embodiment 6~10；
Fig. 4 is spherical gel particle hardening time at different temperatures and strength development tendency chart in embodiment 8.
Specific embodiment
The invention provides a kind of spherical gel particle, prepared by the raw material including following components：
The mass parts of bis-phenol base propane 15~20；
The mass parts of epoxychloropropane 20~30；
The mass parts of toluene 5~15；
The mass parts of alkali compounds 6~8；
The mass parts of water 9~12；
The mass parts of curing agent 10~15；
The mass parts of SILICA FUME 5~15；
The mass parts of carbon fiber 2~3；
The mass parts of density adjuster 0~50.
In the present invention, the raw material for preparing spherical gel particle includes the mass parts of bis-phenol base propane 15~20, preferably 16
~18 mass parts.
In the present invention, the raw material for preparing spherical gel particle includes the mass parts of epoxychloropropane 20~30, preferably 24
~26 mass parts.
In the present invention, the raw material for preparing spherical gel particle includes the mass parts of toluene 5~15, preferably 8~12 mass
Part.
The present invention originates without special restriction to the bis-phenol base propane, epoxychloropropane and toluene, using ability
Commercially available prod known to field technique personnel.In the present invention, the bis-phenol base propane, epoxychloropropane and toluene are preparation
The primary raw material of spherical gel particle presoma.
In the present invention, prepare spherical gel particle raw material include the mass parts of alkali compounds 6~8, preferably 6.5~
7.5 mass parts.The present invention does not have special restriction to the species of the alkali compounds, using well known to those skilled in the art
Alkali compounds is provided.In the present invention, the alkali compounds is preferably hydroxide, more preferably alkali metal hydrogen-oxygen
Compound, most preferably NaOH and/or potassium hydroxide.
In the present invention, the raw material for preparing spherical gel particle includes the mass parts of water 9~12, preferably 10~11 mass
Part.
In the present invention, the alkali compounds and water provide alkaline environment to prepare spherical gel particle presoma.It is excellent
Choosing, the alkaline solution being mixed to get with alkali compounds and water of the invention is as raw material, and the mass concentration of the alkaline solution is excellent
Elect 5~15% as；The mass fraction of the alkaline solution is preferably 15~20 parts.
In the present invention, the raw material for preparing spherical gel particle includes the mass parts of curing agent 10~15, preferably 12~14
Mass parts.In the present invention, the curing agent preferably include one kind in imidazole curing agent and aromatic amine curing agent or
Two kinds；The imidazole curing agent preferably includes in 2-methylimidazole, 2-ethyl-4-methylimidazole and 2- phenylimidazoles
Kind；The aromatic amine curing agent is preferably the methanediamine of isophthalic two.
In the present invention, the raw material for preparing spherical gel particle includes the mass parts of SILICA FUME 5~15, preferably 8~12 matter
Amount part.In the present invention, the average grain diameter of the SILICA FUME is preferably 0.5~1.5 μm, more preferably 0.8~1.2 μm.At this
In invention, the SILICA FUME is preferably industrial furnace during high melt industrial silicon and ferrosilicon, is produced in ore-smelting electric furnace
Go out the very strong SiO of a large amount of volatility2With Si gases, formed with air rapid oxidation condensation precipitation after gas discharge, main component
It is SiO2.The present invention originates without special restriction to the SILICA FUME, using well known to those skilled in the art commercially available micro-
Silica flour.In the present invention, the SILICA FUME is preferably Sai Pusen reinforcing oil well SILICA FUMEs.In the present invention, it is described micro-
Silica flour is the packing material of spherical gel particle.
In the present invention, prepare spherical gel particle raw material include the mass parts of carbon fiber 2~3, more preferably 2.2~
2.6 mass parts.In the present invention, the filament diameter of the carbon fiber is preferably 5~10 μm, more preferably 6~8 μm；The carbon
The length of fiber is preferably 0.6~1.5mm, more preferably 0.8~1.2mm.In the present invention, the carbon fiber is preferably carbon containing
Amount is piled up along fiber axial direction by organic fibers such as flake graphites and formed more than 94%, through carbonization and graphitization
Soft outside but hard inside microcrystalline graphite material obtained from treatment.The present invention, without special restriction, is adopted to the source of the carbon fiber
With commercially available carbon fiber well known to those skilled in the art.In the present invention, the carbon fiber is preferably Weihai and expands fiber
The chopped carbon fiber of Co., Ltd.In the present invention, the carbon fiber is the skeleton bridging materials of spherical gel particle.
In the present invention, prepare spherical gel particle raw material include the mass parts of density adjuster 0~50, preferably 5~
30 mass parts, more preferably 10~20 mass parts.In the present invention, the density adjuster is preferably blanc fixe, lime stone
One or two in powder, Iron Ore Powder, ilmenite powder and galena powder.In the present invention, the density adjuster can be adjusted
The density of spherical gel particle, realizes that the density of spherical gel particle is controllable.In the present invention, the density adjuster can make
The Auto-regulating System of Density of Heavy Medium of spherical gel particle to consistent with the mud density of site of deployment, make the dosage of spherical gel particle 20~
In the drilling fluid for when between 40wt%, also can uniformly suspend, disperseing at the scene or in other leak stopping slurry base fluid, can be with leak stopping
Agent base fluid is pumped into drop ply section, and leakage channel is entered using conventional crowded stifled method agent, blocks drop ply.
In the present invention, the particle diameter of the spherical gel particle can be specially 0.5~2mm, 2~5mm, 5~10mm, 10~
20mm or 20~30mm.In the present invention, the width according to lost-circulation zone crack selects the particle diameter of the spherical gel particle.
Present invention also offers the preparation method of spherical gel particle described in above-mentioned technical proposal, comprise the following steps：
(1) bis-phenol base propane, epoxychloropropane, toluene, alkali compounds and water are mixed, polycondensation reaction obtains forerunner
Body；
(2) presoma for obtaining the step (1) is mediated with SILICA FUME, carbon fiber, density adjuster and curing agent, is obtained
To mixed material；
(3) the mixed material granulation for obtaining the step (2), obtains spherical gel particle.
The present invention mixes bis-phenol base propane, epoxychloropropane, toluene, alkali compounds and water, before polycondensation reaction is obtained
Drive body.In the present invention, it is preferred to bis-phenol base propane is mixed with alkali compounds and water, polycondensation reaction temperature is heated to, then
Mix with epoxychloropropane and toluene, polycondensation reaction obtains presoma.The present invention is to the side for being heated to polycondensation reaction temperature
Formula does not have special restriction, the technical scheme heated using solution well known to those skilled in the art.In the present invention, institute
The heating rate for stating heating is preferably 4~6 DEG C/min.
In the present invention, the temperature of the polycondensation reaction is preferably 55~85 DEG C, more preferably 60~80 DEG C, most preferably
65~75 DEG C；The time of the polycondensation reaction is preferably 4~8h, most preferably more preferably 5~7h, 5.5~6.5h.In this hair
In bright, the pH value of the polycondensation reaction is preferably 8~10.In the present invention, in the polycondensation process, bis-phenol base propane,
Epoxychloropropane and the reacted generation resinae of toluene.
The present invention is post-processed polycondensation product preferably after the completion of the polycondensation reaction, obtains presoma.
In the present invention, the post processing preferably includes washing and vacuum distillation.In the present invention, the detergent of the washing is preferably
Water；The temperature of the water is preferably 90~100 DEG C, more preferably 96~99 DEG C.In the present invention, the number of times of the washing is preferred
It is 10~15 times, more preferably 12~14 times.
The present invention collects organic phase vacuum distillation preferably by the product stratification after the washing.In the present invention, institute
The temperature for stating vacuum distillation is preferably 35~40 DEG C；The pressure of the vacuum distillation is preferably 48~52mmHg；The decompression is steamed
The time for evaporating is preferably 15~20min.
After obtaining presoma, the present invention pinches the presoma with SILICA FUME, carbon fiber, density adjuster and curing agent
Close, obtain mixed material.In the present invention, the kneading is preferably carried out under conditions of speed is preferably 25~35rpm, more excellent
Elect 28~32rpm as；The temperature of the kneading is preferably 60~70 DEG C, more preferably 63~66 DEG C；The time of the kneading is excellent
Elect 20~30min, more preferably 22~26min as.
Be heated to for the presoma first preferably to mediate temperature by the present invention, with SILICA FUME, carbon fiber and density adjuster
The first kneading is carried out, then is mixed with curing agent and is carried out the second kneading.In the present invention, it is described first mediate time be preferably 20
~25min；Described second time mediated was preferably 2~3min.
After obtaining mixed material, mixed material granulation is obtained spherical gel particle by the present invention.The present invention is to described
The method of granulation does not have special restriction, using prilling process well known to those skilled in the art.In the present invention, it is described
Granulation is preferably mist projection granulating.In the present invention, the mist projection granulating parameter is preferably：120~125 DEG C of EAT, air-out
85~90 DEG C of temperature, 150~240ml/h of charging rate.In the present invention, by controlling charging rate and nozzle diameter control ball
The particle diameter of shape gel particle.
The present invention does not have special restriction to the particle diameter for granulating the spherical gel particle for obtaining, and is entered according to required particle diameter
Row granulation.In the present invention, the particle diameter of the spherical gel particle can be specially 0.5~2mm, 2~5mm, 5~10mm,
10~20mm or 20~30mm.
In order to further illustrate the present invention, the spherical gel particle to present invention offer and its preparation with reference to embodiment
Method is described in detail, but they can not be interpreted as into limiting the scope of the present invention.
Embodiment 1:
(1) 45 parts of bis-phenol base propane are first dissolved in the sodium hydroxide solution that 15 parts of mass concentrations are 10% by mass fraction
In, it is added in 25 parts of epoxychloropropane and in 8 parts of toluene, it is placed in closed reactor, polycondensation reaction 8h at a temperature of 55 DEG C；
(2) boiling water is washed 10 times, 38 DEG C, 50mmHg, the presoma obtained after vacuum distillation 15min；
(3) presoma is heated to 65 DEG C, adds 10 parts of SILICA FUMEs, 3 parts of carbon fibers, 25 parts of density adjusters to mediate 20min,
Plus 15 parts of curing agent mediates 2min.
(4) mist projection granulating is used, mist projection granulating parameter is set to：125 DEG C of EAT, 90 DEG C of leaving air temp, charging speed
Degree 200ml/h, selects 2mm nozzles；Sub-sieve obtains the spherical gel particle of 0.5~2mm particle diameters.
Embodiment 2:
According to the methods described of embodiment 1, mist projection granulating, mist projection granulating parameter is set to：125 DEG C of EAT, goes out wind-warm syndrome
90 DEG C of degree, charging rate 170ml/h selects 5mm nozzles；Sub-sieve obtains the spherical gel particle of 2~5mm particle diameters.
Embodiment 3:
According to the methods described of embodiment 1, mist projection granulating, mist projection granulating parameter is set to：125 DEG C of EAT, goes out wind-warm syndrome
90 DEG C of degree, charging rate 190ml/h selects 10mm nozzles；Sub-sieve obtains the spherical gel particle of 5~10mm particle diameters.
The spherical gel particle obtained to the present embodiment hardening time at different temperatures and strength development are tested,
Result is as shown in Figure 2.Figure it is seen that be in solid-state under the spherical gel particle normal temperature of the present embodiment offer, in formation temperature
Softening gel can be formed after more than 40 DEG C and clamp-ons drop ply solidify afterwards, temperature is higher, and the gel solidification reaction time is shorter.
Embodiment 4:
According to the methods described of embodiment 1, mist projection granulating, mist projection granulating parameter is set to：125 DEG C of EAT, goes out wind-warm syndrome
90 DEG C of degree, charging rate 210ml/h selects 20mm nozzles；Sub-sieve obtains the spherical gel particle of 10~20mm particle diameters.
Embodiment 5:
According to the methods described of embodiment 1, mist projection granulating, mist projection granulating parameter is set to：125 DEG C of EAT, goes out wind-warm syndrome
90 DEG C of degree, charging rate 240ml/h selects 30mm nozzles；Sub-sieve obtains the spherical gel particle of 20~30mm particle diameters.
Hardening time and strength development at 80 DEG C of the spherical gel particle that testing example 1~5 is obtained, as a result such as Fig. 1
It is shown.It will be seen from figure 1 that its particle diameter of spherical gel particle bigger hardening time that the present invention is provided is more long.
Embodiment 6:
(1) 45 parts of bis-phenol base propane are first dissolved in the sodium hydroxide solution that 15 parts of mass concentrations are 10% by mass fraction
In, it is added in 25 parts of epoxychloropropane and in 8 parts of toluene, it is placed in closed reactor, polycondensation reaction 4h at a temperature of 85 DEG C；
(2) boiling water is washed 15 times, 38 DEG C, 50mmHg, the presoma obtained after vacuum distillation 20min；
(3) presoma is heated to 60 DEG C, adds 10 parts of SILICA FUMEs, 3 parts of carbon fibers, 35 parts of density adjusters to mediate 20min,
Plus 10 parts of curing agent mediates 2min.
(4) mist projection granulating, mist projection granulating parameter is set to：125 DEG C of EAT, 90 DEG C of leaving air temp, charging rate
150ml/h；Sub-sieve obtains the spherical gel particle of 0.5~2mm particle diameters.
Embodiment 7:
According to the methods described of embodiment 6, mist projection granulating, mist projection granulating parameter is set to：125 DEG C of EAT, goes out wind-warm syndrome
90 DEG C of degree, charging rate 170ml/h selects 5mm nozzles；Sub-sieve obtains the spherical gel particle of 2~5mm particle diameters.
Embodiment 8:
According to the methods described of embodiment 6, mist projection granulating, mist projection granulating parameter is set to：125 DEG C of EAT, goes out wind-warm syndrome
90 DEG C of degree, charging rate 190ml/h selects 10mm nozzles；Sub-sieve obtains the spherical gel particle of 5~10mm particle diameters.
The spherical gel particle obtained to the present embodiment hardening time at different temperatures and strength development are tested,
Result is as shown in Figure 4.From fig. 4, it can be seen that be in solid-state under the spherical gel particle normal temperature of the present embodiment offer, in formation temperature
Softening gel can be formed after more than 40 DEG C and clamp-ons drop ply solidify afterwards, temperature is higher, and the gel solidification reaction time is shorter.
Embodiment 9:
According to the methods described of embodiment 6, mist projection granulating, mist projection granulating parameter is set to：125 DEG C of EAT, goes out wind-warm syndrome
90 DEG C of degree, charging rate 210ml/h selects 20mm nozzles；Sub-sieve obtains the spherical gel particle of 10~20mm particle diameters.
Embodiment 10:
According to the methods described of embodiment 6, mist projection granulating, mist projection granulating parameter is set to：125 DEG C of EAT, goes out wind-warm syndrome
90 DEG C of degree, charging rate 240ml/h selects 30mm nozzles；Obtain the spherical gel particle of 20~30mm particle diameters.
Hardening time and strength development at 80 DEG C of the spherical gel particle that testing example 6~10 is obtained, as a result such as Fig. 3
It is shown.From figure 3, it can be seen that its particle diameter of spherical gel particle bigger hardening time that the present invention is provided is more long.
As can be seen from the above embodiments, it is in solid-state under the spherical gel particle normal temperature that the present invention is provided, in formation temperature
Softening gel can be formed after more than 40 DEG C and clamp-ons drop ply solidify afterwards, its particle diameter is bigger, and hardening time is more long, temperature gel higher
The curing reaction time is shorter, and the gel solidification time can be adjusted by the dosage of adjustment curing agent, meets construction condition
Requirement.
The above is only the preferred embodiment of the present invention, and any formal limitation is not made to the present invention.Should
Point out, for those skilled in the art, under the premise without departing from the principles of the invention, if can also make
Dry improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of spherical gel particle, is prepared by the raw material including following components：
The mass parts of bis-phenol base propane 15~20；
The mass parts of epoxychloropropane 20~30；
The mass parts of toluene 5~15；
The mass parts of alkali compounds 6~8；
The mass parts of water 9~12
The mass parts of curing agent 10~15；
The mass parts of SILICA FUME 5~15；
The mass parts of carbon fiber 2~3；
The mass parts of density adjuster 0~50.
2. spherical gel particle according to claim 1, it is characterised in that the curing agent include imidazole curing agent and
One or two in aromatic amine curing agent.
3. spherical gel particle according to claim 2, it is characterised in that the imidazole curing agent includes 2- methyl miaows
One kind in azoles, 2-ethyl-4-methylimidazole and 2- phenylimidazoles.
4. spherical gel particle according to claim 1, it is characterised in that the average grain diameter of the SILICA FUME is 0.5~
1.5μm。
5. spherical gel particle according to claim 1, it is characterised in that the filament diameter of the carbon fiber is 5~10 μ
M, the length of carbon fiber is 0.6~1.5mm.
6. spherical gel particle according to claim 1, it is characterised in that the density adjuster is blanc fixe, stone
One or two in limestone flour, Iron Ore Powder, ilmenite powder and galena powder.
7. the preparation method of spherical gel particle described in claim 1~6 any one, comprises the following steps：
(1) bis-phenol base propane, epoxychloropropane, toluene, alkali compounds and water are mixed, polycondensation reaction obtains presoma；
(2) presoma for obtaining the step (1) is mediated with SILICA FUME, carbon fiber, density adjuster and curing agent, is mixed
Compound material；
(3) the mixed material granulation for obtaining the step (2), obtains spherical gel particle.
8. preparation method according to claim 7, it is characterised in that the temperature of polycondensation reaction is 55 in the step (1)
~85 DEG C, the time of polycondensation reaction is 4~8h.
9. preparation method according to claim 7, it is characterised in that the temperature mediated in the step (2) is 60~70
DEG C, the time of kneading is 20~30min.
10. preparation method according to claim 7, it is characterised in that the granulation in the step (3) is mist projection granulating.
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