CN110483865A - A kind of rubber material making high-temperature and high-presure resistent packing element and preparation method - Google Patents
A kind of rubber material making high-temperature and high-presure resistent packing element and preparation method Download PDFInfo
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- CN110483865A CN110483865A CN201910931851.0A CN201910931851A CN110483865A CN 110483865 A CN110483865 A CN 110483865A CN 201910931851 A CN201910931851 A CN 201910931851A CN 110483865 A CN110483865 A CN 110483865A
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- packing element
- rubber material
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 121
- 239000005060 rubber Substances 0.000 title claims abstract description 121
- 239000000463 material Substances 0.000 title claims abstract description 83
- 238000012856 packing Methods 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000006229 carbon black Substances 0.000 claims abstract description 41
- 235000019241 carbon black Nutrition 0.000 claims abstract description 41
- 239000002994 raw material Substances 0.000 claims abstract description 41
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 40
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 34
- 239000004014 plasticizer Substances 0.000 claims abstract description 29
- 229920000459 Nitrile rubber Polymers 0.000 claims abstract description 25
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims abstract description 21
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims abstract description 21
- 238000004227 thermal cracking Methods 0.000 claims abstract description 21
- 239000007921 spray Substances 0.000 claims abstract description 18
- 239000004927 clay Substances 0.000 claims abstract description 17
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 16
- 229920003192 poly(bis maleimide) Polymers 0.000 claims abstract description 15
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004073 vulcanization Methods 0.000 claims description 32
- 238000004519 manufacturing process Methods 0.000 claims description 26
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 21
- 239000004033 plastic Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- 239000004636 vulcanized rubber Substances 0.000 claims description 8
- 229910052717 sulfur Inorganic materials 0.000 claims description 7
- 239000011593 sulfur Substances 0.000 claims description 7
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000004808 2-ethylhexylester Substances 0.000 claims description 4
- KRADHMIOFJQKEZ-UHFFFAOYSA-N Tri-2-ethylhexyl trimellitate Chemical compound CCCCC(CC)COC(=O)C1=CC=C(C(=O)OCC(CC)CCCC)C(C(=O)OCC(CC)CCCC)=C1 KRADHMIOFJQKEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005065 mining Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 238000000748 compression moulding Methods 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- -1 0.6% Chemical compound 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 239000000306 component Substances 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 150000008363 butyronitriles Chemical class 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 150000003949 imides Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000008398 formation water Substances 0.000 description 1
- 229920006168 hydrated nitrile rubber Polymers 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 230000008774 maternal effect Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000010057 rubber processing Methods 0.000 description 1
- 238000013040 rubber vulcanization Methods 0.000 description 1
- 238000012163 sequencing technique Methods 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
- C08K5/3415—Five-membered rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Thermal Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Sealing Material Composition (AREA)
Abstract
The present invention provides a kind of rubber material for making high-temperature and high-presure resistent packing element and preparation methods.The rubber material according to the following raw material of mass fraction meter by being prepared: 40~50% hydrogenated nitrile-butadiene rubbers, 12~22% spray carbon blacks, 1~11% thermal cracking carbon black, 4~14% Nano carbon whites, 9~19% clay, 1~9% plasticizer, 0.5~2% anti-aging agent, 0.5~2% dual-tert-butyl peroxy isopropyl base benzene, 1~4%N, N '-penylene bismaleimide.The preparation method can prepare rubber material according to above-mentioned raw materials, and including that will prepare raw material progress, mixing will obtain the rubber material that can be used for making high-temperature and high-presure resistent packing element twice.The beneficial effect comprise that the rubber material being prepared can be resistant to 180 DEG C of high temperature, 105MPa pressure difference, it can effectively meet deep mining to the technical requirements of packing element.
Description
Technical field
The present invention relates to Oil testing fields, and in particular to a kind of rubber material for making high-temperature and high-presure resistent packing element
Material and preparation method.
Background technique
China's deep layer, ultra deep gas reserves account for the 31.23% of natural gas total resources, 15.93% respectively.In routine
Shallow Oil-Gas exploitation enters dry spells, and to meet the needs of to oil gas, marching to deep-seated oil gas reservoir becomes inevitable, is found successively
A large amount of high-quality oil and gas reservoirs of Pisces stone, Jiulong shan Mountain and mill small stream high stone ladder, library the vehicle structural belts such as in front of the mountains.However these reservoirs one
Typical feature is high temperature and pressure even superhigh-temperature and-pressure, brings stern challenge to formation testing completion practice.
Packer is one of the key tool of formation testing completion practice, the weight for undertaking packing oil jacket annulus, ensureing pit shaft safety
Appoint.Packing element is the core component of packer, is the direct executor of sealing function, and high temperature resistant property and intensity in underground are determined
Determine the success or failure of formation testing completion practice.Country's packing element technical level predominantly stays in resistance to 150 DEG C of high temperature, the 70MPa of resistance to pressure difference at present,
It is not able to satisfy the working environment of higher temperatures high pressure.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to solve above-mentioned one existing in the prior art
Or multiple problems.For example, one of the objects of the present invention is to provide a kind of rubber for making high-temperature and high-presure resistent packing element
Material and preparation method, to meet the severe underground work condition of high temperature and pressure.
To achieve the goals above, one aspect of the present invention provides a kind of rubber for making high-temperature and high-presure resistent packing element
Glue material, the packing element may include integrated packing element.
The rubber material can be by being prepared according to the following raw material of mass fraction meter:
40~50% hydrogenated nitrile-butadiene rubbers, 12~22% spray carbon blacks, 1~11% thermal cracking carbon black, 4~14% nanometers it is white
Carbon black, 9~19% clay, 1~9% plasticizer, 0.5~2% anti-aging agent, 0.5~2% dual-tert-butyl peroxy isopropyl base benzene, 1~
4%N, N '-penylene bismaleimide.
In an exemplary embodiment of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention, institute
8% can be smaller than for 36~44%, residual double bonds content by stating acrylonitrile mass fraction in hydrogenated nitrile-butadiene rubber, the hydrogenated butyronitrile
The crude rubber Mooney viscosity ML1+4 (100 DEG C) of rubber can be 50~100.
In an exemplary embodiment of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention, institute
The specific surface area for stating thermal cracking carbon black can be 7~12m2/g。
In an exemplary embodiment of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention, institute
Stating plasticizer may include at least one of DOS plasticizer, DOP plasticizer, TP-95 plasticizer and TOTM plasticizer.
In an exemplary embodiment of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention, institute
Stating anti-aging agent mass fraction shared in rubber material raw material is 1.1~1.9%, the anti-aging agent may include RD anti-aging agent,
At least one of 445 anti-aging agents, ZMTI anti-aging agent and MB anti-aging agent.
In an exemplary embodiment of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention, institute
The effective content for stating dual-tert-butyl peroxy isopropyl base benzene can be not less than 40%.
Another aspect of the present invention provides a kind of preparation side of rubber material for making high-temperature and high-presure resistent packing element
Method.The packing element may include integrated packing element.
Packing element may include integrated packing element, and preparing raw material may include according to mass fraction meter: 40~50% hydrogen
Change nitrile rubber, 12~22% spray carbon blacks, 1~11% thermal cracking carbon black, 4~14% Nano carbon whites, 9~19% clay, 1
~9% plasticizer, 0.5~2% anti-aging agent, 0.5~2% dual-tert-butyl peroxy isopropyl base benzene, 1~4%N, N '-penylene span
Carry out acid imide, the preparation method may include step:
By the hydrogenated nitrile-butadiene rubber prepared in raw material, thermal cracking carbon black, spray carbon black, Nano carbon white, clay, plasticizer
Progress first time mixing, first time plastic emitting in mixing facilities, which are put into, with anti-aging agent obtains rubber master batch；
By rubber master batch, prepare dual-tert-butyl peroxy isopropyl base benzene and N in raw material, N '-penylene bismaleimide investment
It carries out being kneaded for second into mixing facilities, second of plastic emitting obtains rubber material.
Another aspect of the present invention additionally provides a kind of preparation of rubber material for making high-temperature and high-presure resistent packing element
Method.
Packing element may include integrated packing element, and preparing raw material may include according to mass fraction meter: 40~50% hydrogen
Change nitrile rubber, 12~22% spray carbon blacks, 1~11% thermal cracking carbon black, 4~14% Nano carbon whites, 9~19% clay, 1
~9% plasticizer, 0.5~2% anti-aging agent, 0.5~2% dual-tert-butyl peroxy isopropyl base benzene, 1~4%N, N '-penylene span
Carry out acid imide, the preparation method may include step:
By the hydrogenated nitrile-butadiene rubber prepared in raw material, thermal cracking carbon black, spray carbon black, Nano carbon white, clay, plasticizer
Progress first time mixing, first time plastic emitting in mixing facilities, which are put into, with anti-aging agent obtains rubber master batch；
By rubber master batch, prepare dual-tert-butyl peroxy isopropyl base benzene and N in raw material, N '-penylene bismaleimide investment
It carries out being kneaded for second into mixing facilities, second of plastic emitting is obtained to vulcanized rubber material；
It will be dried to vulcanized rubber material；
Material after the drying is subjected to primary vulcanization, obtains the first sulfur product；
First sulfur product is carried out second to vulcanize, obtains rubber material.
In the one or more of the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention
In exemplary embodiment, before second of the progress is kneaded, the method may further comprise the step of: the rubber master batch in room temperature
Lower placement 8h or more.
In the one or more of the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention
In exemplary embodiment, the rotor speed for the mixing facilities that the first time is kneaded can be 70~80rpm, the temperature of first time plastic emitting
Degree can be 90~100 DEG C, and the time can be 10~15min.
In the one or more of the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention
In exemplary embodiment, the rotor speed of second of mixer being kneaded can be 50~70rpm, the temperature of second of plastic emitting
It can be 100~120 DEG C, the time can be 3~5min.
One in the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention is exemplary
In embodiment, before the progress primary vulcanization, the method may further comprise the step of: by vulcanized rubber material in room temperature
Lower placement 8h or more.
One in the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention is exemplary
In embodiment, the temperature condition of the primary vulcanization can be 145~155 DEG C, and the time can be 42~48min.
One in the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production of the invention is exemplary
In embodiment, the temperature condition of second of vulcanization can be 145~155 DEG C, and the time can be 3~5h.
Compared with prior art, beneficial effects of the present invention can include: the rubber material being prepared can be resistant to 180 DEG C of height
Temperature, 105MPa pressure difference, can effectively meet deep mining to the technical requirements of packing element.
Specific embodiment
Hereinafter, the high-temperature and high-presure resistent packer rubber of production of the invention will be described in detail in conjunction with exemplary embodiment
The rubber material and preparation method of cylinder, what is occurred in the present invention first and second does not indicate sequencing, is only used for being mutually distinguishable.
One aspect of the present invention provides a kind of rubber material for making high-temperature and high-presure resistent packing element.The packer
Packing element includes integrated packing element, i.e. the packing element has a kind of rubber material to be prepared.The packer may include sealing
Partially, anchor portion, righting part, setting section, lock portion and unsealed portions, wherein setting section may include packer
Packing element.
In an exemplary embodiment of the rubber material of the packing element of production high temperature resistant elegance of the invention, institute
State rubber material can be by being prepared according to the following raw material of mass fraction meter:
40~50% hydrogenated nitrile-butadiene rubbers, for example, 41.1%, 44.5%, 45.1%, 49.9% etc.；
12~22% spray carbon blacks, such as 12.1%, 16.9%, 17.1%, 20.5%, 21.9% etc.；
1~11% thermal cracking carbon black, for example, 1.1%, 2.5%, 2.9%, 3.1%, 5.9%, 6.1%, 7.9%,
8.1%, 10.9% etc.；
4~14% Nano carbon whites, for example, 4.1%, 4.4%, 4.6%, 5.9%, 6.1%, 8.9%, 9.1%,
13.9% etc.；
9~19% clay, for example, such as 9.1%, 11.5%, 13.9%, 14.1%, 15.9%, 16.1%, 18.9%
Deng；
1~9% plasticizer, such as 1.1%, 4.9%, 5.1%, 7.5%, 8.9% etc.；
0.5~2% anti-aging agent, such as 0.6%, 0.9%, 1.2%, 1.5%, 1.8% etc.；
0.5~2% dual-tert-butyl peroxy isopropyl base benzene, such as 0.6%, 0.9%, 1.1%, 1.9% etc.；
1~4%N, N '-penylene bismaleimide, such as 1.1%, 1.9%, 2.1%, 2.9%, 3.1%, 3.9%
Deng.
In the present embodiment, hydrogenated nitrile-butadiene rubber can select A Langxin section HNBR3607, HNBR3907, HNBR4307,
HNBR4367, hydrogenated nitrile-butadiene rubber HNBR have excellent oil resistant solvent resistance and keep preferable high-low temperature resistant balance, institute
Stating the acrylonitrile mass fraction in hydrogenated nitrile-butadiene rubber to be can be 36~44%, and residual double bonds content is less than 8%, hydrogenated butyronitrile
The crude rubber Mooney viscosity ML1+4 (100 DEG C) of rubber can be 50~100.
It can be prepared when the mass fraction of the acrylonitrile in the hydrogenated nitrile-butadiene rubber of selection is 36~44%
Rubber material can take into account the performance and good compression set characteristic of heat-resisting, oil resistant, resistance to hydrogen sulfide.Test envelope
Require packing element that there is good recovery after the completion of test every device packing element, acrylonitrile content is higher, and the recovery of packing element is poorer,
The test packing element being prepared for the rubber material is after the completion of test by good recovery, the matter of acrylonitrile
Measuring score should not be high again.
When the residual double bonds content in the hydrogenated nitrile-butadiene rubber of selection is less than 8%, it is ensured that can be generated when vulcanization
More cross-bonds can be improved the three-dimensional net structure of rubber, is conducive to rubber and resists higher pressure under oil/gas well.
When range of the crude rubber Mooney viscosity of the hydrogenated nitrile-butadiene rubber of selection 50~100, it can guarantee rubber material
Has good processability during refining glue and vulcanization.
In the present embodiment, spray carbon black, thermal cracking carbon black and Nano carbon white are used as and improve as combination supporting material
Respectively exclusive advantage is played while the magnitude mechanical performance of rubber again respectively to fight underground high temperature ageing, dynamic load sheet
The adverse circumstances such as body failure, high extruding tearing.Wherein, rubber later period ageing-resistant performance also can be improved in spray carbon black；Thermal cracking
Carbon black has maximum particle size (average diameter can be 240~320nm) in carbon black, but its specific surface area is minimum, can
For 7~12m2/ g, thermal cracking carbon black can reduce rubber compression set, improve dynamic and sealing performance；Gao Bibiao
Nano carbon white (the specific surface area 250m of area2/ g), primary partical diameter is less than 100nm, can greatly improve rubber
Tear resistance and wear-resisting property under high temperature and high pressure environment.
In the present embodiment, clay can be improved the hard of rubber as filler under the premise of not influencing processing performance
Degree and acid resistance can make the situation that rubber processing is difficult, yield rate is low to avoid carbon black class reinforcing agent is excessively used.
In the present embodiment, the mobility of material in a mold when processing performance and vulcanization in order to improve rubber, can be with
Plasticizer is added in preparing raw material, plasticizer can select DOS plasticizer, DOP plasticizer, TP-95 plasticizer and TOTM to increase
At least one of agent is moulded, it is possible to further be two of them, wherein rubber high temperature resistance, DOS can be improved in TOTM
The cryogenic property of rubber can be improved.
In the present embodiment, shared mass fraction can be 1.1~1.9% to anti-aging agent in the feed, and anti-aging agent can be with
At least one of RD anti-aging agent, 445 anti-aging agents, ZMTI anti-aging agent and MB anti-aging agent are selected, it is possible to further be wherein two
Kind, anti-aging agent can slow down the aging speed of rubber, improve the service life of rubber, wherein anti-aging agent RD and MB and with good
Good synergistic effect, anti-aging agent 445 and ZMTI and with good cooperative ability.
In the present embodiment, using dual-tert-butyl peroxy isopropyl base benzene, since dual-tert-butyl peroxy isopropyl base benzene is peroxide
Compound forms C-C key in vulcanization crosslinking, and intensity is higher than the S -- S formed when sulfur cross-linking, is conducive to increase rubber molecular chain
Structural strength when vulcanization crosslinking reticulates occurs, and heatproof, hydrogen sulfide corrosion-resistant performance are more preferable, realize better rubber body
Structural strength.The effective content of the dual-tert-butyl peroxy isopropyl base benzene can be not less than 40%, such as 60%.
In the present embodiment, N, N '-penylene bismaleimide can cooperate with peroxide, accelerate hydrogenated nitrile-butadiene rubber
Vulcanization form higher cross-linked network structure and crosslink density, to extend sealability and time.Because resistance to pressure difference performance reaches
The packing time needed when to 105MPa is longer, i.e., at least insulates under the conditions of 177 DEG C for 24 hours, suitable crosslinking accelerator can produce
Raw optimal mechanical property.
Another aspect of the present invention provides a kind of preparation side of rubber material for making high-temperature and high-presure resistent packing element
Method.The packing element may include integrated packing element.
An exemplary reality of the preparation method of the rubber material of high-temperature and high-presure resistent packing element is made in the present invention
It applies in example, the preparation method may include above-mentioned raw material, such as according to mass fraction meter: 40~50% hydrogenated butyronitrile rubbers
Glue, 12~22% spray carbon blacks, 1~11% thermal cracking carbon black, 4~14% Nano carbon whites, 9~19% clay, 1~9% increase
Mould agent, 0.5~2% anti-aging agent, 0.5~2% dual-tert-butyl peroxy isopropyl base benzene, 1~4%N, N '-penylene bismaleimide
Amine, the preparation method may comprise steps of:
It is kneaded for the first time: following components successively being put into mixing machinery:
Prepare the hydrogenated nitrile-butadiene rubber in raw material；
Prepare the thermal cracking carbon black in raw material；
Prepare the spray carbon black in raw material；
Prepare the Nano carbon white in raw material；
Prepare the clay and plasticizer in raw material；
Provide the anti-aging agent in raw material for oneself；
Rubber master batch is obtained after first time is kneaded, rubber master batch is parked into 8h or more, such as 10h at room temperature.Wherein, kneading machine
The rotor speed of device can be 70~80rpm, and it is possible to further be 75rpm, being kneaded total time can be 10~15min, into
One step, it can be 10min, the requirement being kneaded for the first time to temperature may include plastic emitting under the conditions of 90~100 DEG C of temperature, into
One step, it can be 100 DEG C.It rubber master batch is parked to 8h or more at room temperature can eliminate and leave in rubber master batch first time mixing process
Internal stress, additionally it is possible to promote the dispersion of internal raw material, while improve reinforcement.
Second of mixing: following components is successively put into mixing machinery:
Rubber master batch；
Prepare dual-tert-butyl peroxy isopropyl base benzene and the N in raw material, N '-penylene bismaleimide；
Plastic emitting under the conditions of 100~120 DEG C of temperature, such as 110 DEG C.Then thin on the open mill of 0.5~1mm roll spacing
Logical to beat triangle bag 3~5 times, end rubber material can be obtained in last uniform slice.Wherein, the rotor speed of mixing machinery can
Think 50~70rpm, it is possible to further be 65rpm, be kneaded total time can be 3~5min, it is possible to further for
4min。
In another exemplary embodiment of the preparation method of high-temperature and high-presure resistent rubber material of the invention, the system
The raw material for preparing of Preparation Method may include above-mentioned raw material, such as according to mass fraction meter: 40~50% hydrogenated nitrile-butadiene rubbers,
12~22% spray carbon blacks, 1~11% thermal cracking carbon black, 4~14% Nano carbon whites, 9~19% clay, 1~9% plasticising
Agent, 0.5~2% anti-aging agent, 0.5~2% dual-tert-butyl peroxy isopropyl base benzene, 1~4%N, N '-penylene bismaleimide,
The preparation method may comprise steps of:
S01: it is kneaded for the first time: following components successively being put into mixing machinery:
Prepare the hydrogenated nitrile-butadiene rubber in raw material；
Prepare the thermal cracking carbon black in raw material；
Prepare the spray carbon black in raw material；
Prepare the Nano carbon white in raw material；
Prepare the clay and plasticizer in raw material；
Provide the anti-aging agent in raw material for oneself；
Rubber master batch is obtained after first time is kneaded, rubber master batch is parked into 8h or more, such as 10h at room temperature, rubber master batch is parked
Be conducive to eliminate the internal stress left during milling maternal rubber.Wherein, the rotor speed of mixing machinery can for 70~
80rpm, it is possible to further be 75rpm, being kneaded total time can be 10~15min, it is possible to further be 10min, the
The primary requirement being kneaded to temperature may include plastic emitting under the conditions of 90~100 DEG C of temperature, it is possible to further be 100 DEG C.It will
Rubber master batch parks 8h or more at room temperature can eliminate the internal stress left in rubber master batch first time mixing process, additionally it is possible in promotion
The dispersion of portion's raw material, while improving reinforcement.The step can be kneaded phase with the first time in a kind of upper preparation of end rubber material
Together.
S02: second is kneaded: following components is successively put into mixing machinery:
Rubber master batch；
Prepare dual-tert-butyl peroxy isopropyl base benzene and the N in raw material, N '-penylene bismaleimide；
Plastic emitting under the conditions of 100~120 DEG C of temperature, such as 110 DEG C.Then thin on the open mill of 0.5~1mm roll spacing
It is logical to beat triangle bag 3~5 times, last uniform slice, can be obtained end packing element to vulcanized rubber material.Wherein, mixing machinery
Rotor speed can be 50~70rpm, it is possible to further be 65rpm, be kneaded total time can be 3~5min, further
Ground can be 4min.The step can be identical as second of mixing in a kind of upper preparation of end rubber material.
S03: will park at room temperature 8h or more to vulcanized rubber material, then in 50~65 DEG C of hot blast drying box
Then 1.5~2.5h of preliminary drying provides the environment of 90~100 DEG C of temperature, 20~25MPa pressure with vulcanizing press, in a mold
Rubber compression moulding.
In the present embodiment, rubber material to be vulcanized is parked at room temperature is to make the crosslinking accelerator in raw material
In the material diffusion uniformly, be conducive to the later period vulcanized after rubber material stability.
Preliminary drying can make that rubber is internal, external reaches a higher temperature: can rubber be softened first, increase
Mobility is conducive to later period compression moulding, while also avoiding excessively high so that rubber sulphur with internal difference in temperature outside the vulcanization initial stage
Change unevenly, further, the temperature of preliminary drying can be 60 DEG C, and the time can be 2h.And vulcanizing press is in vulcanization machine
One kind, the vulcanization environment condition of rubber material can be not only provided, the temperature of rubber compression moulding in a mold can also be provided
Degree and pressure condition, further, the temperature of compression moulding can be 100 DEG C, and pressure can be 25MPa.
S04: the rubber material after compression moulding is subjected to primary vulcanization, obtains the first sulfur product.Primary vulcanization
The curing temperature of processing can control at 145~155 DEG C, and vulcanization time can control in 42~48min, further, vulcanization
Temperature can be 150 DEG C, the time can be 45min.The purpose of primary vulcanization be in order to guarantee the rubber overwhelming majority all by
Vulcanization forms the high reticular structure of rubber internal intensity, increases rubber manufacturing machinery intensity.
S05: the first sulfur product is carried out second and is vulcanized, the rubber material of packer end packing element is obtained.Second
Vulcanization can carry out in heat aging test chamber, and the temperature of second vulcanization can control at 145~155 DEG C, the time of vulcanization
It can control in 3~5h, further, the temperature of vulcanization can be 150 DEG C, and the time can be 4h.The purpose of second of vulcanization
It is further to vulcanize, keeps vulcanization more thorough, due to preventing that the vulcanization effect of old case is not so good as vulcanizer, thus it is time-consuming long, still
Since primary vulcanization completed substantially by vulcanization, to further increase vulcanization effect, sexual valence is relatively high.
Rubber material described in first exemplary embodiment of the invention can be by second exemplary implementation of the invention
Preparation method in example and third exemplary embodiment, which is prepared into, to be come.
In conclusion the advantages of rubber material and preparation method of the high-temperature and high-presure resistent packing element of production of the invention
Can include:
(1) rubber material provided by the invention, which is used as, prepares packing element, can be with resistance to 177 DEG C of high temperature, resistance to pressure difference
105MPa.Deep-well, ultradeep well, exploitation effectively are met to the technical requirements of packing element, are conducive to China's deep-well, ultradeep well
The independence of oil gas well mining, breaks external monopolization, also advantageously reduces the technical difficulty of China's deep-well, ultradeep well oil-gas mining
And cost, application prospect are good.
(2) rubber material provided by the invention can be in H2S content reaches 40% or more, pit shaft acid strength and reaches 20%
Above, formation water salinity reaches in the adverse circumstances of 80000mg/L or more and uses.
Although those skilled in the art should be clear above by combining exemplary embodiment to describe the present invention
Chu can carry out exemplary embodiment of the present invention each without departing from the spirit and scope defined by the claims
Kind modifications and changes.
Claims (14)
1. a kind of rubber material for making high-temperature and high-presure resistent packing element, which is characterized in that the packing element includes
Integrated packing element, the rubber material according to the following raw material of mass fraction meter by being prepared:
40~50% hydrogenated nitrile-butadiene rubbers, 12~22% spray carbon blacks, 1~11% thermal cracking carbon black, 4~14% nanometers of hard charcoals
Black, 9~19% clay, 1~9% plasticizer, 0.5~2% anti-aging agent, 0.5~2% dual-tert-butyl peroxy isopropyl base benzene, 1~
4%N, N '-penylene bismaleimide.
2. the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 1, which is characterized in that described
Acrylonitrile mass fraction is 36~44%, residual double bonds content less than 8% in hydrogenated nitrile-butadiene rubber, the hydrogenated nitrile-butadiene rubber
(100 DEG C) of crude rubber Mooney viscosity ML1+4 are 50~100.
3. the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 1, which is characterized in that described
The specific surface area of thermal cracking carbon black is 7~12m2/g。
4. the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 1, which is characterized in that described
Plasticizer includes at least one of DOS plasticizer, DOP plasticizer, TP-95 plasticizer and TOTM plasticizer.
5. the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 1, which is characterized in that described
Anti-aging agent mass fraction shared in rubber material raw material is 1.1~1.9%, and the anti-aging agent includes RD anti-aging agent, 445 anti-
At least one of old agent, ZMTI anti-aging agent and MB anti-aging agent.
6. the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 1, which is characterized in that described
The effective content of dual-tert-butyl peroxy isopropyl base benzene is not less than 40%.
7. a kind of preparation method for the rubber material for making high-temperature and high-presure resistent packing element, which is characterized in that the packing
Device packing element includes integrated packing element, and preparing raw material includes according to mass fraction meter: 40~50% hydrogenated nitrile-butadiene rubbers, 12~
22% spray carbon black, 1~11% thermal cracking carbon black, 4~14% Nano carbon whites, 9~19% clay, 1~9% plasticizer, 0.5
~2% anti-aging agent, 0.5~2% dual-tert-butyl peroxy isopropyl base benzene, 1~4%N, N '-penylene bismaleimide, the system
Preparation Method comprising steps of
By the hydrogenated nitrile-butadiene rubber prepared in raw material, thermal cracking carbon black, spray carbon black, Nano carbon white, clay, plasticizer and prevent
Old agent puts into progress first time mixing, first time plastic emitting in mixing facilities and obtains rubber master batch；
By rubber master batch, dual-tert-butyl peroxy isopropyl base benzene and N in raw material are prepared, N '-penylene bismaleimide is put into mixed
It refines and carries out second of mixing in equipment, second of plastic emitting obtains high-temperature and high-presure resistent rubber material.
8. a kind of preparation method for the rubber material for making high-temperature and high-presure resistent packing element, which is characterized in that the packing
Device packing element includes integrated packing element, and preparing raw material includes according to mass fraction meter: 40~50% hydrogenated nitrile-butadiene rubbers, 12~
22% spray carbon black, 1~11% thermal cracking carbon black, 4~14% Nano carbon whites, 9~19% clay, 1~9% plasticizer, 0.5
~2% anti-aging agent, 0.5~2% dual-tert-butyl peroxy isopropyl base benzene, 1~4%N, N '-penylene bismaleimide, the system
Preparation Method comprising steps of
By the hydrogenated nitrile-butadiene rubber prepared in raw material, thermal cracking carbon black, spray carbon black, Nano carbon white, clay, plasticizer and prevent
Old agent puts into progress first time mixing, first time plastic emitting in mixing facilities and obtains rubber master batch；
By rubber master batch, dual-tert-butyl peroxy isopropyl base benzene and N in raw material are prepared, N '-penylene bismaleimide is put into mixed
It refines and carries out second of mixing in equipment, second of plastic emitting is obtained to vulcanized rubber material；
It will be dried to vulcanized rubber material；
Material after the drying is subjected to primary vulcanization, obtains the first sulfur product；
First sulfur product is carried out second to vulcanize, obtains high-temperature and high-presure resistent rubber material.
9. the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 7 or 8,
It is characterized in that, before second of the progress is kneaded, the method also includes steps: the rubber master batch is placed 8h at room temperature
More than.
10. the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 7 or 8,
It is characterized in that, the rotor speed of the mixing facilities of the first time mixing is 70~80rpm, the temperature of first time plastic emitting is 90
~100 DEG C, the time is 10~15min.
11. the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 7 or 8,
It is characterized in that, the rotor speed of second of mixer being kneaded is 50~70rpm, the temperature of second of plastic emitting is 100
~120 DEG C, the time is 3~5min.
12. the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 8, special
Sign is that before the progress primary vulcanization, the method also includes steps: will put at room temperature to vulcanized rubber material
Set 8h or more.
13. the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 8, special
Sign is that the temperature condition of the primary vulcanization is 145~155 DEG C, and the time is 42~48min.
14. the preparation method of the rubber material of the high-temperature and high-presure resistent packing element of production according to claim 8, special
Sign is that the temperature condition of second of vulcanization is 145~155 DEG C, and the time is 3~5h.
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