CN109535511A - A kind of heat conductive rubber material and preparation method thereof for drilling tool - Google Patents
A kind of heat conductive rubber material and preparation method thereof for drilling tool Download PDFInfo
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Abstract
The heat conductive rubber material and preparation method thereof that the present invention relates to a kind of for drilling tool, the raw material of the heat conductive rubber material forms as follows according to parts by weight: hydrogenated butyronitrile or 90~100 parts of nitrile rubber, 20~70 parts of carbon black, 5~15 parts of amorphous silica, 3~9 parts of activator, 2~20 parts of plasticizer, 2~10 parts of vulcanizing agent, 1~5 part of anti-aging agent, 1~6 part of dispersing agent, 1~50 part of Heat Conduction Material, 10~15 parts of ionic liquid.Rubber material provided by the invention also has excellent heat-conductive characteristic and media isolation other than with excellent physical mechanical property, has lower volume change in mud, can effectively improve the temperature resistant capability of main rubber material.
Description
Technical field
The invention belongs to technical field of function materials, are related to a kind of for the heat conductive rubber material of drilling tool and its preparation
Method.
Background technique
Rubber is as sealing material using more universal in oil drilling tool.Drilling tool is during underground work
Long Term Contact mud medium, mud have rubber certain corrosive power, usual rubber occur after mud acts on swelling,
Molten phenomena such as contracting, soften, being hardened, rubber sealing structure size after swelling or molten contracting because changing, simultaneous rubber object
The reduction of mechanical performance and ageing-resistant performance is managed, the dual variation of size and performance is easy to cause the initial failure of rubber material,
To influence the normal use of drilling tool.
Most commonly used rubber material is nitrile rubber or hydrogenated nitrile-butadiene rubber in drilling tool, generally according to brill
The use temperature of well tool just selects suitable rubber material.Traditional nitrile rubber resistance to extreme temperature generally 120 DEG C~
130 DEG C, hydrogenated nitrile-butadiene rubber resistance to extreme temperature is generally at 175 DEG C~180 DEG C, and drilling tool is as used traditional nitrile rubber and hydrogen
If changing the resistance to extreme temperature that nitrile rubber has been more than basis material aging can lead to seal failure quickly.
The present invention provides a kind of with barrier action and the good rubber material of the capacity of heat transmission, body after impregnating in mud
Product change rate is lower, the huge change of drilling tool size and physical mechanical property caused by capable of effectively avoiding because of swelling or molten contracting
Change, the good capacity of heat transmission of material can also avoid heat from assembling in rubber, delay the aging of rubber, to improve main body
The temperature resistant capability of rubber material.
Summary of the invention
It is a kind of for boring the technical problem to be solved by the present invention is to aiming at the above shortcomings existing in the prior art, provide
Heat conductive rubber material of well tool and preparation method thereof, which has the excellent capacity of heat transmission and obstructing capacity, in mud
Starching has lower volume change in medium, while improving the temperature resistant capability of main rubber material.
In order to solve the above technical problems, present invention provide the technical scheme that
A kind of heat conductive rubber material for drilling tool is provided, the raw material of the heat conductive rubber material is according to parts by weight group
At as follows: hydrogenated butyronitrile or 90~100 parts of nitrile rubber, 20~70 parts of carbon black, 5~15 parts of amorphous silica, activator 3
~9 parts, 2~20 parts of plasticizer, 2~10 parts of vulcanizing agent, 1~5 part of anti-aging agent, 1~6 part of dispersing agent, 1~50 part of Heat Conduction Material,
10~15 parts of ionic liquid.
According to the above scheme, the hydrogenated butyronitrile or nitrile rubber Mooney viscosity value [100 DEG C of ML (1+4)] are 30~60, third
Alkene nitrile content >=30%.
According to the above scheme, the carbon black oil factor (DBP value) is 70~120cm3/ 100g, 30~100nm of partial size.
According to the above scheme, the specific surface area of the amorphous silica is 160~300m2/g。
According to the above scheme, the activator is the combination of one or both of zinc oxide, stearic acid.
According to the above scheme, the plasticizer is selected from high temperature resistant type plasticizer G-25, TEGMER 812, TP759, NB-4,
TP95。
According to the above scheme, the vulcanizing agent is 2,5- dimethyl -2,5- (di-t-butyl peroxide) hexane, peroxidating diisopropyl
Benzene, the combination of one or more of sulphur.
According to the above scheme, the anti-aging agent be N- isopropyl-N '-diphenyl-para-phenylene diamine, N-N '-diphenyl-p-phenylenediamine,
N- (1,3- dimethylbutyl)-N '-diphenyl-para-phenylene diamine, 4,4 '-bis- (α, α '-dimethyl benzyl) diphenylamines, 2- mercapto benzene
And imidazoles zinc salt, the combination of one or more of 2,2,4- trimethyl -1,2- dihyaroquinoline condensates.
According to the above scheme, the dispersing agent is one of polymeric fatty acid esters emulsion WB212 or WB222 or two
Kind.
According to the above scheme, the ionic liquid is made of cation and anion, wherein cation is imidazole cation,
Selected from 1- methyl -3- butyl imidazolium cations, 1- methyl -3- allyl imidazole cation, 1- propyl -3- methylimidazole sun from
Son；Anion is halide ion, is selected from chloride ion, bromide ion, iodide ion.
According to the above scheme, the Heat Conduction Material is the mixing of carbon nanotubes, thermally conductive carbon fiber, graphene, ball-aluminium oxide
Object, four mass ratioes are 1.5~10:0.1~20:0.1~12:0~10, and longitudinal thermal conductivity of the Heat Conduction Material >=
400W/mK。
According to the above scheme, the multi-walled carbon nanotube that the carbon nanotubes is 12~30nm of internal diameter, length is 3~12 μm, leads
Heating rate >=1200W/mK.
According to the above scheme, the thermally conductive carbon fiber length is 50~250 μm, thermal conductivity >=900W/mK.
According to the above scheme, the graphene number of plies is 1~15 layer, and specific surface area is 40~400m2/ g, thermal conductivity >=
3000W/mK。
According to the above scheme, the ball-aluminium oxide specific surface area is 0.1~1.0m2/ g, Al2O3Content is 99.5% or more.
The present invention also provides the preparation methods of the above-mentioned heat conductive rubber material for drilling tool, the specific steps are as follows:
1) raw material is weighed in proportion, it is spare；
2) Heat Conduction Material carries out pre-dispersed processing: by ionic liquid at 25~80 DEG C high-speed stirred, and in stirring condition
Lower addition part amorphous silica, additional amount account for the 20~60% of amorphous silica gross mass, stir 10~15 points
Heat Conduction Material is added after clock, is sufficiently stirred to obtain functional Heat Conduction Material predispersion；
3) it prepares heat conductive rubber material: will plasticate 1~3 minute in hydrogenated butyronitrile or nitrile rubber investment mixer, then
Activator, anti-aging agent, dispersing agent is added, is kneaded 2~4 minutes, then by carbon black, remaining amorphous silica, plasticizer and step
The rapid functional Heat Conduction Material predispersion of 2) gained is added in two portions, and is kneaded 3~5 minutes after being added every time, is eventually adding sulphur
Agent is kneaded 2~dumping after five minutes, then on a mill it is thin it is 8~10 times logical after bottom sheet, park after at least 16h in plate sulphur
Vulcanization obtains the heat conductive rubber material for drilling tool on change machine.
The mechanical properties such as hardness, tensile strength, the tearing strength of rubber are improved in the present invention using Heat Conduction Material, make rubber
Glue has lower volume change after impregnating in mud, can increase the capacity of heat transmission of rubber, to improve rubber body
The temperature resistant capability of material.Carbon nanotubes can effectively improve the hardness, tensile strength and tearing strength of rubber material, but be added too
More, the Mooney viscosity of sizing material greatly increases, and leads to that the processing performance of rubber compound is too poor, processing cost increases；Thermally conductive carbon fiber energy
The hardness for improving rubber material, it is smaller on the influence of the Mooney viscosity of sizing material, but be added too much, lead to the tensile strength of rubber, tear
Resistance to spalling decline；Graphene has outside reinforcing effect rubber, and layer structure can form barrier action in rubber, can effectively support
Anti- mud to the extraction of the small-molecule substance in rubber and dissolving in for mud small molecular substance, make rubber have in mud compared with
Low volume change, so that rubber has preferable dimensional stability and Physical Mechanical stabilizability as sealing material, but
It is added too much, the Mooney viscosity of sizing material greatly increases, and is unfavorable for processing.The dispersion of carbon nanotubes, grapheme material in rubber
Property it is poor, be easy reunite, handled using ionic liquid and amorphous silica according to the pre-dispersed technique in the present invention
Afterwards, it can be promoted to be uniformly dispersed in rubber.Carbon nanotubes is tubular structure, and thermally conductive carbon fiber is linear structure, and graphene is
Layer structure, ball-aluminium oxide are sphere structure, and every kind of substance is individually largely using there is advantage and disadvantage as described above, if single
Solely a small amount of limited length using due to material itself, individual tubulose, threadiness, stratiform and chondritic, which are hardly formed, mutually to be interconnected
Logical, overlapped network structure.Therefore, the present invention simultaneously using a small amount of different shape and length characteristic material, mechanical property and
Processing performance is complementary；And pre-dispersed processing is carried out so that every kind of heat conduction material to material using ionic liquid and amorphous silica
Material, which can be uniformly dispersed in rubber, forms mutually overlapped three dimentional heat conduction network, further promotes the capacity of heat transmission of rubbery system
With the stabilization of mechanical property.
The beneficial effects of the present invention are: rubber material provided by the invention is in addition to excellent physical mechanical property
Outside, also there is excellent heat-conductive characteristic and media isolation, there is lower volume change in mud, can effectively improve
The temperature resistant capability of main rubber material.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention makees the present invention below with reference to embodiment
It is described in further detail.
Hydrogenated nitrile-butadiene rubber used in the embodiment of the present invention is moral the huge rock AT3404, Mooney viscosity value [ML that A Langxin section produces
100 DEG C of (1+4)] it is 41, acrylonitrile content 36%；Nitrile rubber is the 3945F, Mooney viscosity value [ML that A Langxin section produces
100 DEG C of (1+4)] it is 47, acrylonitrile content 39%；Anti-aging agent is 2 mercapto benzimidazole zinc salt, N- isopropyl-N '-benzene
Base p-phenylenediamine, 2,2,4- trimethyl -1,2- dihyaroquinoline condensates select Grade A and ratings above；Plasticizer
TEGMER 812, molecular weight are about 4000；Plasticizer G-25, molecular weight are about 10000；Carbon black used is Cabot N330, DBP
Value is 98cm3/ 100g, average grain diameter 40.8nm；The specific surface area of amorphous silica used is 188m2/g；Vulcanizing agent used
For cumyl peroxide；Ionic liquid used is 1- methyl -3- butyl imidazole hydrochloride, and colourless transparent liquid, purity is
98%, it is purchased from upper marine origin victory Chemical Co., Ltd.；Carbon nanotubes used is 12~30nm of internal diameter, the multi wall that length is 3~12 μm
Carbon nanotube, thermal conductivity 1200W/mK；Graphene number of plies used is 1~10 layer, and specific surface area is 40~300m2/ g, it is thermally conductive
Rate is 3000W/mK；Thermally conductive carbon fiber used is that length is 150 μm, thermal conductivity 900W/mK；Spherical shape alumina ratio surface used
Product is 0.1~1.0m2/ g, Al2O3Content is 99.5%；Activator is zinc oxide, stearic acid；Dispersing agent is WB222；Nano-sized carbon
Pipe, graphene, thermally conductive carbon fiber, ball-aluminium oxide, zinc oxide, stearic acid, WB222 are commercially available.
Embodiment
Raw material quality part of the embodiment of the present invention 1~2 and comparative example 1~4 proportion is shown in Table 1, all using nitrile rubber
Material based on material, wherein comparative example 1 is not added with Heat Conduction Material, and comparative example 2 is added to nano-sized carbon on the basis of comparative example 1
Pipe；Comparative example 3 is added to thermally conductive carbon fiber on the basis of comparative example 1；Comparative example 4 is added on the basis of comparative example 1
Graphene；Embodiment 1 is that carbon nanotubes, thermally conductive carbon fiber, graphene are added on the basis of comparative example 1；Embodiment 2 be
Ball-aluminium oxide is added on the basis of embodiment 1.
Table 1
The pretreating process of Heat Conduction Material is according to following progress in above embodiments 1~2 and comparative example 2~4: by ionic liquid
Body is added 5 parts of amorphous silica under 60 DEG C of heating temperature, high-speed stirred, stirs 15 minutes；Further according to need successively plus
Enter graphene, carbon nanotubes, thermally conductive carbon fiber, ball-aluminium oxide, it is every a kind of substance is added after stir 3h, obtaining final product is
Functional Heat Conduction Material predispersion.
The calendering process of 1~4 rubber of above embodiments 1~2 and comparative example is according to following progress: first putting into nitrile rubber
It plasticates in mixer 2 minutes, zinc oxide, stearic acid, N- isopropyl-N '-diphenyl-para-phenylene diamine, 2,2,4- front threes is then added
Base -1,2- dihyaroquinoline condensate, WB222, mixing time are 2 minutes, then by carbon black N330, remaining unformed titanium dioxide
Silicon, plasticizer TEGMER 812, plasticizer G-25, functional Heat Conduction Material predispersion (Heat Conduction Material is not added in comparative example 1) point
It is added twice, mixing time is 3 minutes after being added every time, is eventually adding vulcanizing agent cumyl peroxide and is kneaded 3 minutes heel row
Glue, then bottom sheet after thin logical 10 times on a mill, vulcanizes on vulcanizing press after parking for 24 hours.
Examples 1 to 2 and comparative example 1~4 in table 1 are pre-dispersed according to process above, be kneaded and vulcanization after carry out room temperature
Mechanical property, 150 DEG C of water-base muds impregnate 240h performance evaluation, thermal conductivity measurement, and measurement result is shown in Table 2.
Table 2
As shown in Table 2, compared with comparative example 1, it has been separately added into carbon nanotubes in comparative example 2~4 and Examples 1 to 2, has led
The Heat Conduction Material that hot carbon fiber, graphene, ball-aluminium oxide different ratio obtain, the rubber of comparative example 2~4 and Examples 1 to 2
The thermal conductivity of material has different degrees of raising, again while increasing the hardness and tearing strength of rubber.By at 150 DEG C
After impregnating 240h in water-base mud, serious aging is had occurred in the common nitrile rubber of comparative example 1, and common nitrile rubber does not tolerate
150 DEG C of superheated waters.Compared with comparative example 1, comparative example 2~4 and Examples 1 to 2 firmness change are smaller, show excellent resistance to
The ability of 150 DEG C of water-base muds, wherein comparative example 4, in Examples 1 to 2 with the addition of graphene, the volume change of rubber
Reduce, illustrates that the rubber containing graphene has preferable barriering effect to mud medium.From the point of view of thermal conductivity, comparative example 2~4 and
For Examples 1 to 2 compared with comparative example 1, thermal conductivity has different degrees of raising, wherein the thermal conductivity highest of embodiment 2, explanation
Carbon nanotubes, thermally conductive carbon fiber, graphene, ball-aluminium oxide and use and using ionic liquid and amorphous silica into
The pre-dispersed processing of row, which can effectively facilitate Heat Conduction Material and mutually overlap, forms three dimentional heat conduction network, and promotion is thermally conductive.
Raw material quality part of the embodiment of the present invention 3~4 and comparative example 6~8 proportion is shown in Table 3, and not add Heat Conduction Material
It is comparative example 5.Embodiment 3~4 and comparative example 5~8 are all made of hydrogenated butyronitrile raw rubber as basis material.
Table 3
The pretreating process of Heat Conduction Material is according to following progress in the above comparative example 6~8 and embodiment 3~4: by ionic liquid
Body is added 5 parts of amorphous silica under 60 DEG C of heating temperature, high-speed stirred, stirs 15 minutes；Further according to need successively plus
Enter graphene, carbon nanotubes, thermally conductive carbon fiber, ball-aluminium oxide, it is every a kind of substance is added after stir 3h, obtaining final product is
Functional Heat Conduction Material predispersion.
The calendering process of 3~4 rubber of the above comparative example 5~8 and embodiment is according to following progress: first putting into hydrogenated butyronitrile
It plasticates in mixer 2 minutes, zinc oxide, stearic acid, 2 mercapto benzimidazole zinc salt, WB222 is then added, mixing time is
3 minutes, then carbon black, remaining amorphous silica, plasticizer TEGMER 812, functional Heat Conduction Material predispersion is (right
Heat Conduction Material is not added in ratio 5) it is added in two portions, each mixing time is 4 minutes, is eventually adding vulcanizing agent and is kneaded 3 minutes heel row
Glue, then bottom sheet after thin logical 10 times on a mill, vulcanizes on vulcanizing press after parking for 24 hours.
Comparative example 5~8 and embodiment 3~4 in table 3 are pre-dispersed according to process above, be kneaded and vulcanization after carry out room temperature
Mechanical property, 205 DEG C of water-base muds impregnate 168h performance evaluation, thermal conductivity measurement, and measurement result is shown in Table 4.
Table 4
As shown in Table 4, compared with comparative example 5, carbon nanotubes has been separately added into comparative example 6~8 and embodiment 3~4, has been led
The Heat Conduction Material that hot carbon fiber, graphene, ball-aluminium oxide different ratio obtain, the thermal conductivity of rubber material have in various degree
Raising, again while increasing the hardness and tearing strength of rubber.After impregnating 168h in 205 DEG C of water-base muds, with
Comparative example 5 is compared, and comparative example 6~8 and 3~4 firmness change of embodiment are smaller, shows excellent high temperature resistant water-base mud
Ability, wherein comparative example 8, in embodiment 3~4 with the addition of graphene, the volume change of rubber reduces, illustrates containing stone
The rubber of black alkene has preferable barriering effect to mud medium.From the point of view of thermal conductivity, comparative example 6~8 and embodiment 3~4 with it is right
Ratio 5 is compared, and thermal conductivity has different degrees of raising, wherein the thermal conductivity highest of embodiment 4, illustrates a meter carbon pipe, thermally conductive carbon
Fiber, graphene, ball-aluminium oxide and carry out pre-dispersed processing energy with and using ionic liquid and amorphous silica
It effectively facilitates Heat Conduction Material and mutually overlaps and form three dimentional heat conduction network.
By above-described embodiment and test data it can be seen that the rubber material that the present invention obtains has excellent Physical Mechanical
Can be outer, also there is excellent heat-conductive characteristic and mud medium barrier property, there is lower volume change in mud, can have
Effect improves the temperature resistant capability of main rubber material.The present invention program has excellent performance, has significant progress.
Above embodiments are preferred embodiment of the invention, but embodiment of the present invention is not by above-mentioned case study on implementation
Limitation.Therefore all any modifications and supplement made within the scope of the present invention, it is within the scope of the present invention.
Claims (10)
1. a kind of heat conductive rubber material for drilling tool, which is characterized in that the raw material of the heat conductive rubber material is according to weight
It is as follows to measure part composition: hydrogenated butyronitrile or 90~100 parts of nitrile rubber, 20~70 parts of carbon black, 5~15 parts of amorphous silica,
3~9 parts of activator, 2~20 parts of plasticizer, 2~10 parts of vulcanizing agent, 1~5 part of anti-aging agent, 1~6 part of dispersing agent, Heat Conduction Material 1
~50 parts, 10~15 parts of ionic liquid.
2. the heat conductive rubber material according to claim 1 for drilling tool, which is characterized in that the hydrogenated butyronitrile or
Nitrile rubber Mooney viscosity value is 30~60, acrylonitrile content >=30%.
3. the heat conductive rubber material according to claim 1 for drilling tool, which is characterized in that the carbon black oil factor
For 70~120cm3/ 100g, 30~100nm of partial size；The specific surface area of the amorphous silica is 160~300m2/g。
4. the heat conductive rubber material according to claim 1 for drilling tool, which is characterized in that the activator is oxygen
Change the combination of one or both of zinc, stearic acid.
5. the heat conductive rubber material according to claim 1 for drilling tool, which is characterized in that the plasticizer is selected from
High temperature resistant type plasticizer G-25, TEGMER 812, TP759, NB-4, TP95.
6. the heat conductive rubber material according to claim 1 for drilling tool, which is characterized in that the vulcanizing agent is 2,
5- dimethyl -2,5- (di-t-butyl peroxide) hexane, cumyl peroxide, the combination of one or more of sulphur.
7. the heat conductive rubber material according to claim 1 for drilling tool, which is characterized in that the anti-aging agent is N-
Isopropyl-N '-diphenyl-para-phenylene diamine, N-N '-diphenyl-p-phenylenediamine, N- (1,3- dimethylbutyl)-N '-phenyl is to benzene two
Amine, 4,4 '-bis- (α, α '-dimethyl benzyl) diphenylamines, 2 mercapto benzimidazole zinc salt, 2,2,4- trimethyl -1,2- dihydros
Change the combination of one or more of quinoline condensate.
8. the heat conductive rubber material according to claim 1 for drilling tool, which is characterized in that the dispersing agent is height
One or both of molecular fat acid esters emulsion WB212 or WB222；The ionic liquid is by cation and anion group
At wherein cation is imidazole cation, selected from 1- methyl -3- butyl imidazolium cations, 1- methyl -3- allyl imidazole sun
Ion, 1- propyl -3- methyl imidazolium cation；Anion is halide ion, is selected from chloride ion, bromide ion, iodide ion.
9. the heat conductive rubber material according to claim 1 for drilling tool, which is characterized in that the Heat Conduction Material is
Carbon nanotubes, thermally conductive carbon fiber, graphene, ball-aluminium oxide mixture, four mass ratioes be 1.5~10:0.1~20:0.1
~12:0~10, and longitudinal thermal conductivity >=400W/mK of the Heat Conduction Material；
The multi-walled carbon nanotube that the carbon nanotubes is 12~30nm of internal diameter, length is 3~12 μm, thermal conductivity >=1200W/mK；
The thermally conductive carbon fiber length is 50~250 μm, thermal conductivity >=900W/mK；The graphene number of plies is 1~15 layer, specific surface
Product is 40~400m2/ g, thermal conductivity >=3000W/mK；The ball-aluminium oxide specific surface area is 0.1~1.0m2/ g, Al2O3Contain
Amount is 99.5% or more.
10. a kind of preparation method of any heat conductive rubber material for drilling tool of claim 1-9, feature exist
In, the specific steps are as follows:
1) raw material is weighed in proportion, it is spare；
2) Heat Conduction Material carries out pre-dispersed processing: by ionic liquid at 25~80 DEG C high-speed stirred, and under agitation plus
Enter part amorphous silica, additional amount accounts for the 20~60% of amorphous silica gross mass, after stirring 10~15 minutes
Heat Conduction Material is added, is sufficiently stirred to obtain functional Heat Conduction Material predispersion；
3) it prepares heat conductive rubber material: will plasticate 1~3 minute in hydrogenated butyronitrile or nitrile rubber investment mixer, be then added
Activator, anti-aging agent, dispersing agent are kneaded 2~4 minutes, then by carbon black, remaining amorphous silica, plasticizer and step 2)
Gained functionality Heat Conduction Material predispersion is added in two portions, and is kneaded 3~5 minutes after being added every time, is eventually adding vulcanizing agent
Be kneaded 2~dumping after five minutes, then on a mill it is thin it is 8~10 times logical after bottom sheet, park after at least 16h in vulcanizing press
Upper vulcanization obtains the heat conductive rubber material for drilling tool.
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