CN108276983A - A kind of preparation method of graphene aerogel epoxy resin composite fracturing proppant - Google Patents
A kind of preparation method of graphene aerogel epoxy resin composite fracturing proppant Download PDFInfo
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- CN108276983A CN108276983A CN201810032533.6A CN201810032533A CN108276983A CN 108276983 A CN108276983 A CN 108276983A CN 201810032533 A CN201810032533 A CN 201810032533A CN 108276983 A CN108276983 A CN 108276983A
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- epoxy resin
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
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- C—CHEMISTRY; METALLURGY
- 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
- C09K8/92—Compositions for stimulating production by acting on the underground formation characterised by their form or by the form of their components, e.g. encapsulated material
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Abstract
The invention discloses a kind of preparation methods of graphene aerogel epoxy resin composite fracturing proppant；1, there is formation graphene oxide drop in petroleum ether and methyl-silicone oil mixture by what the instillation of certain density graphene oxide suspension freezed；2, graphene oxide drop is moved into freeze-drying in freeze dryer and obtains graphite oxide aerogel bead；3, graphite oxide aerogel bead high temperature is heat reduced to graphene aerogel bead；4, graphene aerogel bead is imported in epoxy resin and curing agent mixture and vacuumizes compound, be then heating and curing to form graphene epoxy resin composite fracturing proppant；Using the microspheric form fracturing propping agents of graphene aerogel and epoxy resin produced with combination, have the advantages that low-density and high compression-strength, the efficiency of fracturing yield increasing can be significantly improved.
Description
Technical field
The present invention relates to a kind of preparation methods of fracturing propping agents, and in particular to a kind of graphene aerogel epoxy resin is multiple
Close the preparation method of fracturing propping agents
Background technology
Hydraulic fracturing technology has become the major measure of well production increment, is widely used to various oil gas fields at present
Exploitation, wherein proppant work are the piths of hydraulic fracturing.China's oil fracturing propping agents industry development is rapider, market
Scale speedup reaches 20%.2009,4.7 hundred million yuan of the China Petroleum fracturing propping agents trade investment amount of money rose to 6.2 in 2011
Hundred million yuan, average growth rate per annum is 13% or more.Therefore, novel light high-intensity proppant is studied to have very important significance.
Fracturing propping agents can be roughly divided into natural with artificial two major classes.The former using quartz sand as representative, the latter then with
Haydite is representative.But both there is prodigious disadvantage：Quartz sand intensity is relatively low, and it is about 20MPa to start broken pressure, uncomfortable
It closes and is to use in middle high, clossing pressure fractured layer；Although haydite tool high intensity characteristic, its particle relative density compared with
Height reaches 2.7-3.6, and the performance (such as viscosity, rheological characteristic) and pumping conditions (such as discharge capacity, plant capacity) to fracturing fluid are all
More stringent requirements are proposed.
Invention content
In order to solve the above-mentioned problems of the prior art, the purpose of the present invention is to provide a kind of graphene aerogel rings
The preparation method of oxygen resin compounded fracturing propping agents, pressure resistance and the spy that can be molded bead ultralight by graphene aerogel
Point is fabricated to the novel fracturing propping agents with high intensity and extremely-low density, improves proppant with epoxy resin composite molding
Performance.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of graphene aerogel epoxy resin composite fracturing proppant, the preparation method include as follows
Step：
Step 1, petroleum ether is put into freeze drier with the petroleum ether and methyl-silicone oil mixture stirred evenly to be made
Its 20~30min of pre-freeze at -55 DEG C, instills pre-freeze dropwise by certain density graphene oxide suspension with syringe later
Graphene oxide drop is formed in the petroleum ether and methyl-silicone oil mixture crossed；After the completion, petroleum ether and methyl-silicone oil are mixed
Object and graphene oxide drop are put into freeze dryer 15~20min of freezing at -55~-25 DEG C；
Step 2, it is mixed from petroleum ether and methyl-silicone oil after graphene oxide drop is completely solidified into graphene oxide ice hockey
It is filtered in conjunction object and takes out graphene oxide ice hockey, poured into the petroleum ether freezed in advance and clean once, then taking-up is put into cold
The culture dish that froze simultaneously is freeze-dried；After freeze-drying, takes out and obtain graphite oxide aerogel bead, stone will be aoxidized
Black alkene gas gel small ball is put into after ceramic boat and is sent into vacuum tube furnace, so that it is heat-treated under protection of argon gas to get to graphite
Alkene gas gel small ball；
Epoxy resin and curing agent according to mass ratio are 100 by step 3:The ratio of (75~85) is mixed, and is added
Heat, to increase its mobility, is stirred evenly to 40 DEG C~50 DEG C；Graphene aerogel bead well prepared in advance is placed in epoxy
In resin and curing agent mixture, under the dilute strong interaction with epoxy resin of graphite, graphene aerogel bead can be completely
Be immersed into epoxy resin, this is impregnation stage；This stage should keep 40 DEG C~50 DEG C, 1~2h of time；By epoxy resin and
Curing agent mixture and graphene aerogel bead are transferred in freeze drier, and the 3~4h that deaerates at 40 DEG C~50 DEG C；
Step 4 is taken out graphene aerogel bead from epoxy resin and curing agent mixture, is put after the completion of degassing
Onto tinfoil, it is sent into tube furnace and carries out solidification process to get to graphene aerogel epoxy resin composite fracturing proppant bead.
Compared to the prior art, the present invention has the following advantages：
(1) graphite of raw material and epoxy resin can be obtained largely in preparation method, relative inexpensiveness.
(2) by preparing graphene aerogel bead, the proppant of controllable size can be obtained.
(3) proppant made of graphene aerogel bead and epoxy resin has the excellent of high intensity and extremely-low density
Point.
Description of the drawings
Fig. 1 is the graphene oxide liquid that the graphene oxide suspension instilled in petroleum ether and methyl-silicone oil mixture is formed
Drop.
Fig. 2 is the graphene aerogel epoxy resin composite proppant finally made.
Specific implementation mode
The present invention is described in further details in the following with reference to the drawings and specific embodiments.
Embodiment 1
A kind of preparation method of graphene aerogel epoxy resin composite fracturing proppant of the present embodiment, including walk as follows
Suddenly,
Step 1, petroleum ether and the petroleum ether stirred evenly, which are put into methyl-silicone oil mixture in freeze drier, makes it
The pre-freeze 20min at -55 DEG C, petroleum ether are 50 with methyl-silicone oil volume ratio:100, it actual state can be adjusted as needed；
The graphene oxide suspension of a concentration of 3mg/ml is instilled to the petroleum ether and methyl-silicone oil mixing that pre-freeze is crossed dropwise with syringe
Graphene oxide drop (as shown in Figure 1) is formed in object, when instillation can mix syringe needle with petroleum ether with methyl-silicone oil
Thing liquid face contacts, and the size of graphene oxide drop is adjusted according to different syringe needle sizes and time of contact；It should ensure that oxidation
At least distance of 0.8~1cm between graphene drop；It can make baffle temperature control with the manual interface of freeze drier when freezing
System is at -55 DEG C, after the completion, by petroleum ether and methyl-silicone oil mixture and graphene oxide drop be slowly put into freeze dryer into
Row freezing 15min；
Step 2 after the complete solidification of graphene oxide drop forms graphene oxide ice hockey, uses filtering spoon filtering to take out
Graphene oxide ice hockey simultaneously pours into the petroleum ether freezed in advance, is cleaned once with the petroleum ether freezed, later will oxidation
Graphene ice hockey is put into the culture dish freezed and is freeze-dried；Temperature is -45 DEG C in freeze drier, by freezing for 24 hours
It is dry to obtain graphite oxide aerogel bead, after freeze-drying, obtained graphite oxide aerogel bead is carefully taken out, is put into
Be sent into vacuum tube furnace after ceramic boat, make its under protection of argon gas 800 DEG C of high temperature thermal reduction 1h to get to graphene aerogel
Bead；
50g E44 (6101) epoxy resin is mixed with 37.5g curing agent (methyl hexahydrophthalic anhydride), and heated by step 3
To 40 DEG C to increase its mobility, stir evenly；Graphene aerogel bead well prepared in advance is placed in epoxy resin and is consolidated
In agent mixture, under the dilute strong interaction with epoxy resin of graphite, graphene aerogel bead can be completely immersed into
In epoxy resin, this is impregnation stage；This stage should keep 40 DEG C, time 1h；By epoxy resin and graphene aerogel bead
It is transferred in freeze drier, and the 3h that deaerates at 50 DEG C；
Step 4 is taken out graphene aerogel bead from epoxy resin and curing agent mixture, is put after the completion of degassing
It onto tinfoil, is sent into tube furnace and is cured, whole process is carried out in three steps, respectively at 80 DEG C, 140 DEG C and 180 DEG C respectively
Solidification is completed to get to graphene aerogel epoxy resin composite fracturing proppant bead such as Fig. 2 institutes after heating 4h, 4h and 3h
Show, diameter is substantially in 2mm or so.
Embodiment 2
A kind of preparation method of graphene aerogel epoxy resin composite fracturing proppant of the present embodiment, including walk as follows
Suddenly,
Step 1, petroleum ether and the petroleum ether stirred evenly, which are put into methyl-silicone oil mixture in freeze drier, makes it
The pre-freeze 25min at -55 DEG C, petroleum ether are 65 with methyl-silicone oil volume ratio:100, it actual state can be adjusted as needed；
The graphene oxide suspension of a concentration of 8mg/ml is instilled to the petroleum ether and methyl-silicone oil mixing that pre-freeze is crossed dropwise with syringe
Graphene oxide drop (as shown in Figure 1) is formed in object, when instillation can mix syringe needle with petroleum ether with methyl-silicone oil
Thing liquid face contacts, and the size of graphene oxide drop is adjusted according to different syringe needle sizes and time of contact；It should ensure that oxidation
At least distance of 0.8~1cm between graphene drop；It can make baffle temperature control with the manual interface of freeze drier when freezing
System is at -50 DEG C, after the completion, by petroleum ether and methyl-silicone oil mixture and graphene oxide drop be slowly put into freeze dryer into
Row freezing 18min；
Step 2 after the complete solidification of graphene oxide drop forms graphene oxide ice hockey, uses filtering spoon filtering to take out
Graphene oxide ice hockey simultaneously pours into the petroleum ether freezed in advance, is cleaned once with the petroleum ether freezed, later will oxidation
Graphene ice hockey is put into the culture dish freezed and is freeze-dried；Temperature is -45 DEG C in freeze drier, by freezing for 24 hours
It is dry to obtain graphite oxide aerogel bead, after freeze-drying, obtained graphite oxide aerogel bead is carefully taken out, is put into
Be sent into vacuum tube furnace after ceramic boat, make its under protection of argon gas 800 DEG C of high temperature thermal reduction 1h to get to graphene aerogel
Bead；
50g E44 (6101) epoxy resin is mixed with 40g curing agent (methyl hexahydrophthalic anhydride), and is heated to by step 3
45 DEG C, to increase its mobility, stir evenly；Graphene aerogel bead well prepared in advance is placed in epoxy resin and solidification
In agent composition, under the dilute strong interaction with epoxy resin of graphite, graphene aerogel bead can completely be immersed into ring
In oxygen resin, this is impregnation stage；This stage should keep 45 DEG C, time 1h；Epoxy resin and graphene aerogel bead are turned
It moves in freeze drier, and the 3h that deaerates at 45 DEG C；
Step 4 is taken out graphene aerogel bead from epoxy resin and curing agent mixture, is put after the completion of degassing
It onto tinfoil, is sent into tube furnace and is cured, whole process is carried out in three steps, respectively at 80 DEG C, 140 DEG C and 180 DEG C respectively
Solidification is completed to get to graphene aerogel epoxy resin composite fracturing proppant bead such as Fig. 2 institutes after heating 4h, 4h and 3h
Show, diameter is substantially in 2mm or so.
Embodiment 3
Step 1, petroleum ether and the petroleum ether stirred evenly, which are put into methyl-silicone oil mixture in freeze drier, makes it
The pre-freeze 30min at -55 DEG C, petroleum ether are 80 with methyl-silicone oil volume ratio:100, it actual state can be adjusted as needed；
It will be a concentration of
The graphene oxide suspension of 15mg/ml instills the petroleum ether that pre-freeze is crossed and methyl-silicone oil mixing with syringe dropwise
Graphene oxide drop (as shown in Figure 1) is formed in object, when instillation can mix syringe needle with petroleum ether with methyl-silicone oil
Thing liquid face contacts, and the size of graphene oxide drop is adjusted according to different syringe needle sizes and time of contact；It should ensure that oxidation
At least distance of 0.8~1cm between graphene drop；It can make baffle temperature control with the manual interface of freeze drier when freezing
System is at -55 DEG C, after the completion, by petroleum ether and methyl-silicone oil mixture and graphene oxide drop be slowly put into freeze dryer into
Row freezing 20min；
Step 2 after the complete solidification of graphene oxide drop forms graphene oxide ice hockey, uses filtering spoon filtering to take out
Graphene oxide ice hockey simultaneously pours into the petroleum ether freezed in advance, is cleaned once with the petroleum ether freezed, later will oxidation
Graphene ice hockey is put into the culture dish freezed and is freeze-dried；Temperature is -45 DEG C in freeze drier, by freezing for 24 hours
It is dry to obtain graphite oxide aerogel bead, after freeze-drying, obtained graphite oxide aerogel bead is carefully taken out, is put into
Be sent into vacuum tube furnace after ceramic boat, make its under protection of argon gas 800 DEG C of high temperature thermal reduction 1h to get to graphene aerogel
Bead；
50g E44 (6101) epoxy resin is mixed with 42.5g curing agent (methyl hexahydrophthalic anhydride), and heated by step 3
To 40 DEG C to increase its mobility, stir evenly；Graphene aerogel bead well prepared in advance is placed in epoxy resin and is consolidated
In agent mixture, under the dilute strong interaction with epoxy resin of graphite, graphene aerogel bead can be completely immersed into
In epoxy resin, this is impregnation stage；This stage should keep 50 DEG C, time 1h；By epoxy resin and graphene aerogel bead
It is transferred in freeze drier, and the 3h that deaerates at 50 DEG C；
Step 4 is taken out graphene aerogel bead from epoxy resin and curing agent mixture, is put after the completion of degassing
It onto tinfoil, is sent into tube furnace and is cured, whole process is carried out in three steps, respectively at 80 DEG C, 140 DEG C and 180 DEG C respectively
Solidification is completed to get to graphene aerogel epoxy resin composite fracturing proppant bead such as Fig. 2 institutes after heating 4h, 4h and 3h
Show, diameter is substantially in 2mm or so.
Specific embodiments of the present invention are described above, it should be pointed out that for the common of the art
For technical staff, various improvements and modifications may be made without departing from the principle of the present invention, these are improved and profit
Decorations also should be protection scope of the present invention.
Claims (6)
1. a kind of preparation method of graphene aerogel epoxy resin composite fracturing proppant, it is characterised in that：The preparation side
Method includes the following steps：
Step 1, petroleum ether and the petroleum ether stirred evenly and methyl-silicone oil mixture, which are put into freeze drier, makes it
20~30min of pre-freeze at -55 DEG C, instills pre-freeze mistake with syringe dropwise by certain density graphene oxide suspension later
Petroleum ether and methyl-silicone oil mixture in formed graphene oxide drop；After the completion, by petroleum ether and methyl-silicone oil mixture
15~20min of freezing at -55~-25 DEG C is put into freeze dryer with graphene oxide drop；
Step 2, after graphene oxide drop is completely solidified into graphene oxide ice hockey, from petroleum ether and methyl-silicone oil mixture
Graphene oxide ice hockey is taken out in middle filtering, pours into the petroleum ether freezed in advance and cleans once, and then taking-up, which is put into, freezed
Culture dish and be freeze-dried；After freeze-drying, takes out and obtain graphite oxide aerogel bead, by graphene oxide
Gas gel small ball is put into after ceramic boat and is sent into vacuum tube furnace, so that it is heat-treated under protection of argon gas to get to graphene gas
Gelled pill；
Epoxy resin and curing agent according to mass ratio are 100 by step 3:The ratio of (75~85) is mixed, and is heated to
40 DEG C~50 DEG C, to increase its mobility, stir evenly；Graphene aerogel bead well prepared in advance is placed in epoxy resin
In curing agent mixture, under the dilute strong interaction with epoxy resin of graphite, graphene aerogel bead can completely soak
It is less than in epoxy resin, this is impregnation stage；This stage should keep 40 DEG C~50 DEG C, 1~2h of time；By epoxy resin and solidification
Agent composition and graphene aerogel bead are transferred in freeze drier, and the 3~4h that deaerates at 40 DEG C~50 DEG C；
Step 4 takes out graphene aerogel bead from epoxy resin and curing agent mixture, is put into tin after the completion of degassing
On paper, it is sent into tube furnace and carries out solidification process to get to graphene aerogel epoxy resin composite fracturing proppant bead.
2. the preparation method of graphene aerogel epoxy resin composite fracturing proppant according to claim 1, feature
It is：Petroleum ether described in step 1 is (50~80) with methyl-silicone oil volume ratio:100.
3. the preparation method of graphene aerogel epoxy resin composite fracturing proppant according to claim 1, feature
It is：A concentration of 3~15mg/ml of graphene oxide suspension described in step 1.
4. the preparation method of graphene aerogel epoxy resin composite fracturing proppant according to claim 1, feature
It is：The temperature being freeze-dried described in step 2 is -45 DEG C, and the time is for 24 hours.
5. the preparation method of graphene aerogel epoxy resin composite fracturing proppant according to claim 1, feature
It is：The temperature heat-treated described in step 2 is 800 DEG C, recovery time 1h.
6. the preparation method of graphene aerogel epoxy resin composite fracturing proppant according to claim 1, feature
It is：Solidification process described in step 4 is carried out in three steps, and heats 4h respectively at 80 DEG C, 140 DEG C and 180 DEG C respectively, 4h and
Solidification is completed after 3h.
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