CN106751233A - A kind of cold-resistant sealing ring and preparation method based on Graphene/polymer composites - Google Patents

A kind of cold-resistant sealing ring and preparation method based on Graphene/polymer composites Download PDF

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Publication number
CN106751233A
CN106751233A CN201611003159.4A CN201611003159A CN106751233A CN 106751233 A CN106751233 A CN 106751233A CN 201611003159 A CN201611003159 A CN 201611003159A CN 106751233 A CN106751233 A CN 106751233A
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parts
graphene
sealing ring
cold
resistant sealing
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陈素素
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Nanjing Runqi Electronic Technology Co Ltd
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Nanjing Runqi Electronic Technology Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/7476—Systems, i.e. flow charts or diagrams; Plants
    • B29B7/7495—Systems, i.e. flow charts or diagrams; Plants for mixing rubber
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/002—Methods
    • B29B7/005—Methods for mixing in batches
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
    • B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
    • B29B7/18—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
    • B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
    • B29B7/18—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/183—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft having a casing closely surrounding the rotors, e.g. of Banbury type
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/22—Component parts, details or accessories; Auxiliary operations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/22—Component parts, details or accessories; Auxiliary operations
    • B29B7/28—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
    • B29B7/286—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control measuring properties of the mixture, e.g. temperature, density
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/82—Heating or cooling
    • B29B7/823—Temperature control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B29B7/90—Fillers or reinforcements, e.g. fibres
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2031/00—Other particular articles
    • B29L2031/26—Sealing devices, e.g. packaging for pistons or pipe joints
    • B29L2031/265—Packings, Gaskets
    • 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
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Thermal Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Sealing Material Composition (AREA)

Abstract

The present invention is a kind of cold-resistant sealing ring based on Graphene/polymer composites, and the composite, with Graphene as filler, is comprised the following steps with polymer as matrix：（1）：Take Graphene to pour into alcoholic solution, it is 1 to prepare mass ratio:10‑1:50 suspension, graphene uniform solution is prepared in dissipating machine using ultrasound point system；（2）：By fluorine unpigmented rubber, plasticizer phthalic acid dicyclohexyl maleate etc., abrasive material is carried out in addition material grinder, the abrasive material time is 25 36 hours；（3）：The mixture that abrasive material is obtained is added by step（1）In obtained graphene solution, mixed solution is obtained；（4）：By step（3）In mixed solution kneaded in internal rubber mixer 2 minutes after sequentially add plasticizer phthalic acid dicyclohexyl maleate, antiaging agent octyl group etc., melting temperature is 85 DEG C 105 DEG C, mixing time is 2 hours, then 185 DEG C 200 DEG C are warming up to the speed of 10 DEG C/min, punching press is in blocks, Temperature fall.It is of the invention simply, reasonably to solve the problems, such as by fluorine unpigmented rubber sealing ring as the cold-resistant sealing ring cold resistance that main material is prepared from is poor.

Description

A kind of cold-resistant sealing ring and preparation method based on Graphene/polymer composites
Technical field
It is related to a kind of preparation method of cold-resistant sealing ring the present invention relates to patent, it is more particularly to a kind of to be based on graphite/polymerization The cold-resistant sealing ring and preparation method of thing composite.
Background technology
The cold-resistant sealing of rubber used on current engineering machinery such as diesel engine, the brake apparatus of fuel system engineering machinery Circle needs splendid weatherability, ozone resistance and chemical resistance, and cold resistance is then bad.But the rubber for using at present resists cold close Seal is usually the copolymer of vinyl fluoride and hexafluoropropene.Though salable DOT3 brake fluid, cushion rubber is in bobbin oil Seriously swollen in brake fluid, hardness is reduced, intensity declines, cause cushion rubber early stage because of volumetric expansion, the overproof big, physical property of physical dimension Decline and cause oil leak, lose sealing effectiveness, particularly causing three guarantees product too high using process, customer is very big to this reflection, It is required that rectification.
For the oil resistivity of cold-resistant sealing ring, it is proposed that a kind of oil resistant fluorine unpigmented rubber sealing ring, fluorine unpigmented rubber sealing ring is put down Average molecular weight 700,000 or so；Canescence is to light yellow bulk or powdery solid, relative density 0.95~1.0；Acrylonitrile content is 26% Tg=-52 DEG C of fluorine unpigmented rubber sealing ring glass transition temperature, Tb=-47 DEG C of brittle temperature, and acrylonitrile content is 40% Tg=-22 DEG C of fluorine unpigmented rubber sealing ring glass transition temperature；Solubility parameter δ=8.9~9.9, fluorine unpigmented rubber sealing ring has Excellent oil resistivity, its oil resistivity is only second to polysulfide rubber and nitrile rubber, and the wearability and air-tightness having.Heat resistance Better than butadiene-styrene rubber, neoprene, can be in 120 DEG C of long-term works；Air-tightness is only second to butyl rubber.Its composition is as follows：Fluorine element 100 parts of rubber；15 parts of activator FT；5 parts of activating agent zinc oxide；3 parts of plasticizer decanedioic acid dibutylester；Antiaging agent is octylatcd 3 parts of diphenylamines；8 parts of reinforcing agent nano-calcium carbonate；10 parts of plasticiser dicyclohexyl phthalate；Diphenylguanidine ETU2 parts；Promote Agent DPG2 parts；0.5 part of sulphur.
Fluorine unpigmented rubber sealing ring is mainly produced using emulsion polymerization at low temperature, and oil resistivity is fabulous, and wearability is higher, heat resistance Preferably, bonding force is strong.But it has the disadvantage that cold resistance is poor, generally require filler to improve, and Graphene be one kind by carbon atom The Novel Carbon Nanomaterials of the individual layer laminated structure of composition, thickness is only 0.35nm.Due to big specific surface area, good Heat endurance and chemical stability, stronger hydrophobicity, it is easy to the advantages of being chemically modified, is expected in high-performance electronic device The fields such as part, composite, field emmision material, gas sensor and energy stores obtain extensive use.And he is miscellaneous by sp2 Change carbon atom close-packed arrays to be formed, it is steady in the presence of its construction unit with unique two-dimension periodic honeycomb lattice structure Determine carbon hexatomic ring and assign its excellent hot property, it is considered to be outstanding heat control material, and with excellent mechanical performance.
The general rubber preparing device for using at present, can only make mixture be tried one's best with bonding agent and be sufficiently mixed, but it cannot be guaranteed that mixed The useless adobe added in the formation of partial particulate, fine powder and bonding agent conglomeration, or refining glue in refining is not fully achieved granularity requirements to be made There is deviation in size distribution, and these factor controllings are bad all to influence stabilized with mixture so as to influence Forming Quality.
The content of the invention
It is cold-resistant the invention provides a kind of high intensity based on Graphene/polymer composites to solve the above problems Sealing ring and preparation method, it is to avoid the defect of cold resistance difference in the prior art, the useless adobe added in refining glue are not fully achieved Granularity requirements make size distribution deviation occur, and these factor controllings are bad all to influence pug stability so as to influence to be molded matter Amount.
In order to overcome deficiency of the prior art, the invention provides a kind of based on Graphene/polymer composites High intensity resists cold sealing ring and preparation method, specific as follows：
A kind of cold-resistant sealing ring based on Graphene/polymer composites, the composite with polymer as matrix, with graphite Alkene is filler, it is characterised in that polymer fraction by weight includes：100 parts of fluorine unpigmented rubber；EO/PO block polyethers 5-12 Part；6-15 parts of activating agent zinc oxide；4-15 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- trimethyl -1, 4-15 parts of 2- dihyaroquinoline condensates, 9-16 parts of reinforcing agent phenolic resin；Plasticiser dicyclohexyl phthalate 12-20 Part；Vulcanization accelerator TMTD 3-10 parts；Accelerant CZ 3-10 parts；Sulphur 0.6-1.2 parts；Graphene is filler, and weight fraction is 0.06- 18 parts.
A kind of preparation method of the cold-resistant sealing ring based on Graphene/polymer composites, comprises the following steps：
Step（1）：Take Graphene to pour into alcoholic solution, it is 1 to prepare mass ratio:10-1:50 suspension, using ultrasound point system Graphene uniform solution is prepared in scattered machine；
Step（2）：By fluorine unpigmented rubber, plasticizer phthalic acid dicyclohexyl maleate, EO/PO block polyethers, activating agent zinc oxide and Sulphur, carries out abrasive material in addition material grinder, the abrasive material time is 25-36 hours；
Step（3）：The mixture that abrasive material is obtained is added by step（1）In obtained graphene solution, mixed solution is obtained；
Step（4）：By step（3）In mixed solution kneaded in internal rubber mixer 2 minutes after to sequentially add plasticizer adjacent Dicyclo-hexyl phthlate, antiaging agent 2,2,4- trimethyl -1,2- dihyaroquinolines condensate, reinforcing agent phenolic resin, modeling Agent dicyclohexyl phthalate, diphenylguanidine ETU and diphenylguanidine PG, melting temperature are 85 DEG C -105 DEG C, and mixing time is 2 Hour, 185 DEG C -200 DEG C then are warming up to the speed of 10 DEG C/min, punching press is in blocks, Temperature fall；
Step（5）：By step（4）In sheet material put mould into, in putting mould into vulcanizer, be warming up to 120-170 DEG C, rise 10-30MPa is depressed into, the duration is 1-2 hours；
Step（6）After release pressure, the demoulding naturally cools to room temperature, carries out deburring treatment, is obtained multiple based on Graphene/polymer The cold-resistant sealing ring of condensation material.
The constituent based on Graphene/polymer composites includes：100 parts of fluorine unpigmented rubber；EO/PO blocks gather Ether 8-10 parts；8-12 parts of activating agent zinc oxide；6-12 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- tri- Methyl isophthalic acid, 6-12 parts of 2- dihyaroquinoline condensates, 12-14 parts of reinforcing agent phenolic resin；Plasticiser dicyclohexyl Ester 14-18 parts；Diphenylguanidine ETU5-8 parts；Diphenylguanidine PG5-8 parts；Sulphur 0.8-1.0 parts；Graphene 0.5-12 parts.
The constituent based on Graphene/polymer composites includes：100 parts of fluorine unpigmented rubber；EO/PO blocks gather 9 parts of ether；10 parts of activating agent zinc oxide；10 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- trimethyl -1, 11 parts of 2- dihyaroquinolines condensate, 13 parts of reinforcing agent phenolic resin；16 parts of plasticiser dicyclohexyl phthalate；Accelerator DETU7 parts；Diphenylguanidine PG7 parts；0.9 part of sulphur；4 parts of Graphene.
Stating internal rubber mixer includes support and refining glue room, and feed box, the pan feeding are provided with the top of the refining glue room The both sides of case are provided with feeding mouth；Pressure-applying unit is provided with above the refining glue room；The refining glue chamber interior be provided with turn rod and under Turn rod, it is described on turn rod and under turn rod and be provided with hobboing cutter, above turn rod and under turn rod relative motion；The bottom of the refining glue room is provided with Discharging opening, the discharging opening is extended to outside support.
The discharge outlet is equipped with filter screen by screw, and formation is detachably connected.
The pressure-applying unit includes that turbine increases device, and the turbocharger is connected by worm screw with floating weight, upper top Bolt is located at the surface of refining glue room, top bolt under being arranged right below of refining glue room.
Also include temperature sensor in the refining glue room, the side of refining glue room is provided with dedusting cabin, the bottom of the dedusting cabin Upper surface with support is connected by screw.
The bottom of the dedusting cabin is provided with reservoir.
Beneficial effect：The present invention provides new formula, and simple, rational solving by fluorine unpigmented rubber sealing ring is main material The problem of the sealing ring cold resistance difference that material is prepared from；Effectively mixture is screened, it is ensured that the size of mixture, increase mixed The stability of compound, improves the quality of shaped article.
Brief description of the drawings
Fig. 1 is the structural representation of the rubber mixing machine in inventive embodiments.
Fig. 1's is respectively labeled as：1 support, 2 refining glue rooms, 3 feed box, 4 feeding mouths turn to turn rod under rod, 6,7 hobboing cutters on 5, and 8 go out Material mouth, 9 turbines increase device, 10 worm screws, 11 floating weights, 12 times top bolts, 13 temperature sensors, 14 dedusting cabins, 15 reservoirs.
Specific embodiment
To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawing and tool Body embodiment is described in detail.
Embodiment 1
A kind of cold-resistant sealing ring based on Graphene/polymer composites, the composite with polymer as matrix, with graphite Alkene is filler, it is characterised in that polymer fraction by weight includes：100 parts of fluorine unpigmented rubber；5 parts of EO/PO block polyethers； 15 parts of activating agent zinc oxide；4 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- trimethyl -1,2- dihydros 15 parts of quinoline condensate, 9 parts of reinforcing agent phenolic resin；20 parts of plasticiser dicyclohexyl phthalate；Diphenylguanidine ETU3 parts； Diphenylguanidine PG10 parts；0.6 part of sulphur；With Graphene as filler, weight fraction is 18 parts.
A kind of preparation method of the cold-resistant sealing ring based on Graphene/polymer composites, comprises the following steps：
Step（1）：Take Graphene to pour into alcoholic solution, it is 1 to prepare mass ratio:10 suspension, machine is dissipated using ultrasound point system In prepare graphene uniform solution；
Step（2）：By fluorine unpigmented rubber, plasticizer phthalic acid dicyclohexyl maleate, EO/PO block polyethers, activating agent zinc oxide and Sulphur, carries out abrasive material in addition material grinder, the abrasive material time is 25 hours；
Step（3）：The mixture that abrasive material is obtained is added by step（1）In obtained graphene solution, mixed solution is obtained；
Step（4）：By step（3）In mixed solution kneaded in internal rubber mixer 2 minutes after to sequentially add plasticizer adjacent Dicyclo-hexyl phthlate, antiaging agent 2,2,4- trimethyl -1,2- dihyaroquinolines condensate, reinforcing agent phenolic resin, modeling Agent dicyclohexyl phthalate, diphenylguanidine ETU and diphenylguanidine PG, melting temperature are 85 DEG C, and mixing time is 2 hours, Then 185 DEG C are warming up to the speed of 10 DEG C/min, punching press is in blocks, Temperature fall；
Step（5）：By step（4）In sheet material put mould into, in putting mould into vulcanizer, be warming up to 120 DEG C, boost to 10MPa, the duration is 1 hour；
Step（6）After release pressure, the demoulding naturally cools to room temperature, carries out deburring treatment, is obtained multiple based on Graphene/polymer The cold-resistant sealing ring of condensation material.
The internal rubber mixer includes support 1 and refining glue room 2, and the top of the refining glue room 2 is provided with feed box 3, institute The both sides for stating feed box 3 are provided with feeding mouth 4；The top of the refining glue room 2 is provided with pressure-applying unit；The pressure-applying unit includes turbine Increase device 9, the turbocharger 9 is connected by worm screw 10 with floating weight 11, floating weight 11 is located at just going up for refining glue room 2 Side, pushes up bolt 12 under being arranged right below of refining glue room.
Be provided with inside the refining glue room 2 turn rod 5 and under turn rod 6, it is described on turn rod 5 and under turn rod 6 and be provided with hobboing cutter 7, On turn rod 5 and under turn the relative motion of rod 6；The bottom of the refining glue room 2 is provided with discharging opening 8, and the discharging opening 8 extends to support Outward；Filter screen is equipped with by screw at the discharging opening 8, formation is detachably connected.
Also include temperature sensor 13 in the refining glue room 2, the side of refining glue room 2 is provided with dedusting cabin 14, the dedusting cabin 14 bottom is connected by screw with the upper surface of support 1；The bottom of the dedusting cabin 14 is provided with reservoir 15.
Embodiment 2
A kind of cold-resistant sealing ring based on Graphene/polymer composites, the composite with polymer as matrix, with graphite Alkene is filler, it is characterised in that polymer fraction by weight includes：100 parts of fluorine unpigmented rubber；12 parts of EO/PO block polyethers； 6 parts of activating agent zinc oxide；15 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- trimethyl -1,2- dihydros 4 parts of quinoline condensate, 16 parts of reinforcing agent phenolic resin；12 parts of plasticiser dicyclohexyl phthalate；Diphenylguanidine ETU10 parts； Diphenylguanidine PG3 parts；1.2 parts of sulphur；With Graphene as filler, weight fraction is 0.06 part.
A kind of preparation method of the cold-resistant sealing ring based on Graphene/polymer composites, comprises the following steps：
Step（1）：Take Graphene to pour into alcoholic solution, it is 1 to prepare mass ratio:50 suspension, machine is dissipated using ultrasound point system In prepare graphene uniform solution；
Step（2）：By fluorine unpigmented rubber, plasticizer phthalic acid dicyclohexyl maleate, EO/PO block polyethers, activating agent zinc oxide and Sulphur, carries out abrasive material in addition material grinder, the abrasive material time is 36 hours；
Step（3）：The mixture that abrasive material is obtained is added by step（1）In obtained graphene solution, mixed solution is obtained；
Step（4）：By step（3）In mixed solution kneaded in internal rubber mixer 2 minutes after to sequentially add plasticizer adjacent Dicyclo-hexyl phthlate, antiaging agent 2,2,4- trimethyl -1,2- dihyaroquinolines condensate, reinforcing agent phenolic resin, modeling Agent dicyclohexyl phthalate, diphenylguanidine ETU and diphenylguanidine PG, melting temperature are 105 DEG C, and mixing time is 2 hours, Then 200 DEG C are warming up to the speed of 10 DEG C/min, punching press is in blocks, Temperature fall；
Step（5）：By step（4）In sheet material put mould into, in putting mould into vulcanizer, be warming up to 170 DEG C, boost to 30MPa, the duration is 2 hours；
Step（6）After release pressure, the demoulding naturally cools to room temperature, carries out deburring treatment, is obtained multiple based on Graphene/polymer The cold-resistant sealing ring of condensation material.
The internal rubber mixer includes support 1 and refining glue room 2, and the top of the refining glue room 2 is provided with feed box 3, institute The both sides for stating feed box 3 are provided with feeding mouth 4；The top of the refining glue room 2 is provided with pressure-applying unit；The pressure-applying unit includes turbine Increase device 9, the turbocharger 9 is connected by worm screw 10 with floating weight 11, floating weight 11 is located at just going up for refining glue room 2 Side, pushes up bolt 12 under being arranged right below of refining glue room.
Be provided with inside the refining glue room 2 turn rod 5 and under turn rod 6, it is described on turn rod 5 and under turn rod 6 and be provided with hobboing cutter 7, On turn rod 5 and under turn the relative motion of rod 6；The bottom of the refining glue room 2 is provided with discharging opening 8, and the discharging opening 8 extends to support Outward；Filter screen is equipped with by screw at the discharging opening 8, formation is detachably connected.
Also include temperature sensor 13 in the refining glue room 2, the side of refining glue room 2 is provided with dedusting cabin 14, the dedusting cabin 14 bottom is connected by screw with the upper surface of support 1；The bottom of the dedusting cabin 14 is provided with reservoir 15.
Embodiment 3
A kind of cold-resistant sealing ring based on Graphene/polymer composites, the composite with polymer as matrix, with graphite Alkene is filler, it is characterised in that polymer fraction by weight includes：100 parts of fluorine unpigmented rubber；8 parts of EO/PO block polyethers； 12 parts of activating agent zinc oxide；6 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- trimethyl -1,2- dihydros 12 parts of quinoline condensate, 12 parts of reinforcing agent phenolic resin；18 parts of plasticiser dicyclohexyl phthalate；Diphenylguanidine ETU5 parts； Diphenylguanidine PG8 parts；0.8 part of sulphur；With Graphene as filler, weight fraction is 12 parts.
A kind of preparation method of the cold-resistant sealing ring based on Graphene/polymer composites, comprises the following steps：
Step（1）：Take Graphene to pour into alcoholic solution, it is 1 to prepare mass ratio:10 suspension, machine is dissipated using ultrasound point system In prepare graphene uniform solution；
Step（2）：By fluorine unpigmented rubber, plasticizer phthalic acid dicyclohexyl maleate, EO/PO block polyethers, activating agent zinc oxide and Sulphur, carries out abrasive material in addition material grinder, the abrasive material time is 27 hours；
Step（3）：The mixture that abrasive material is obtained is added by step（1）In obtained graphene solution, mixed solution is obtained；
Step（4）：By step（3）In mixed solution kneaded in internal rubber mixer 2 minutes after to sequentially add plasticizer adjacent Dicyclo-hexyl phthlate, antiaging agent 2,2,4- trimethyl -1,2- dihyaroquinolines condensate, reinforcing agent phenolic resin, modeling Agent dicyclohexyl phthalate, diphenylguanidine ETU and diphenylguanidine PG, melting temperature are 90 DEG C, and mixing time is 2 hours, Then 190 DEG C are warming up to the speed of 10 DEG C/min, punching press is in blocks, Temperature fall；
Step（5）：By step（4）In sheet material put mould into, in putting mould into vulcanizer, be warming up to 150 DEG C, boost to 25MPa, the duration is 1 hour；
Step（6）After release pressure, the demoulding naturally cools to room temperature, carries out deburring treatment, is obtained multiple based on Graphene/polymer The cold-resistant sealing ring of condensation material.
The internal rubber mixer includes support 1 and refining glue room 2, and the top of the refining glue room 2 is provided with feed box 3, institute The both sides for stating feed box 3 are provided with feeding mouth 4；The top of the refining glue room 2 is provided with pressure-applying unit；The pressure-applying unit includes turbine Increase device 9, the turbocharger 9 is connected by worm screw 10 with floating weight 11, floating weight 11 is located at just going up for refining glue room 2 Side, pushes up bolt 12 under being arranged right below of refining glue room.
Be provided with inside the refining glue room 2 turn rod 5 and under turn rod 6, it is described on turn rod 5 and under turn rod 6 and be provided with hobboing cutter 7, On turn rod 5 and under turn the relative motion of rod 6；The bottom of the refining glue room 2 is provided with discharging opening 8, and the discharging opening 8 extends to support Outward；Filter screen is equipped with by screw at the discharging opening 8, formation is detachably connected.
Also include temperature sensor 13 in the refining glue room 2, the side of refining glue room 2 is provided with dedusting cabin 14, the dedusting cabin 14 bottom is connected by screw with the upper surface of support 1；The bottom of the dedusting cabin 14 is provided with reservoir 15.
Embodiment 4
A kind of cold-resistant sealing ring based on Graphene/polymer composites, the composite with polymer as matrix, with graphite Alkene is filler, it is characterised in that polymer fraction by weight includes：100 parts of fluorine unpigmented rubber；10 parts of EO/PO block polyethers； 8 parts of activating agent zinc oxide；12 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- trimethyl -1,2- dihydros 6 parts of quinoline condensate, 14 parts of reinforcing agent phenolic resin；14 parts of plasticiser dicyclohexyl phthalate；Diphenylguanidine ETU8 parts； Diphenylguanidine PG5 parts；1.0 parts of sulphur；Characterized in that, with Graphene as filler, weight fraction is 0.5 part.
A kind of preparation method of the cold-resistant sealing ring based on Graphene/polymer composites, comprises the following steps：
Step（1）：Take Graphene to pour into alcoholic solution, it is 1 to prepare mass ratio:30 suspension, machine is dissipated using ultrasound point system In prepare graphene uniform solution；
Step（2）：By fluorine unpigmented rubber, plasticizer phthalic acid dicyclohexyl maleate, EO/PO block polyethers, activating agent zinc oxide and Sulphur, carries out abrasive material in addition material grinder, the abrasive material time is 25 hours；
Step（3）：The mixture that abrasive material is obtained is added by step（1）In obtained graphene solution, mixed solution is obtained；
Step（4）：By step（3）In mixed solution kneaded in internal rubber mixer 2 minutes after to sequentially add plasticizer adjacent Dicyclo-hexyl phthlate, antiaging agent 2,2,4- trimethyl -1,2- dihyaroquinolines condensate, reinforcing agent phenolic resin, modeling Agent dicyclohexyl phthalate, diphenylguanidine ETU and diphenylguanidine PG, melting temperature are 85 DEG C, and mixing time is 2 hours, Then 185 DEG C are warming up to the speed of 10 DEG C/min, punching press is in blocks, Temperature fall；
Step（5）：By step（4）In sheet material put mould into, in putting mould into vulcanizer, be warming up to 160 DEG C, boost to 25MPa, the duration is 1 hour；
Step（6）After release pressure, the demoulding naturally cools to room temperature, carries out deburring treatment, is obtained multiple based on Graphene/polymer The cold-resistant sealing ring of condensation material.
The internal rubber mixer includes support 1 and refining glue room 2, and the top of the refining glue room 2 is provided with feed box 3, institute The both sides for stating feed box 3 are provided with feeding mouth 4；The top of the refining glue room 2 is provided with pressure-applying unit；The pressure-applying unit includes turbine Increase device 9, the turbocharger 9 is connected by worm screw 10 with floating weight 11, floating weight 11 is located at just going up for refining glue room 2 Side, pushes up bolt 12 under being arranged right below of refining glue room.
Be provided with inside the refining glue room 2 turn rod 5 and under turn rod 6, it is described on turn rod 5 and under turn rod 6 and be provided with hobboing cutter 7, On turn rod 5 and under turn the relative motion of rod 6；The bottom of the refining glue room 2 is provided with discharging opening 8, and the discharging opening 8 extends to support Outward；Filter screen is equipped with by screw at the discharging opening 8, formation is detachably connected.
Also include temperature sensor 13 in the refining glue room 2, the side of refining glue room 2 is provided with dedusting cabin 14, the dedusting cabin 14 bottom is connected by screw with the upper surface of support 1；The bottom of the dedusting cabin 14 is provided with reservoir 15.
Embodiment 5
A kind of cold-resistant sealing ring based on Graphene/polymer composites, the composite with polymer as matrix, with graphite Alkene is filler, it is characterised in that polymer fraction by weight includes：100 parts of fluorine unpigmented rubber；9 parts of EO/PO block polyethers； 10 parts of activating agent zinc oxide；10 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- trimethyl -1,2- dihydros 11 parts of quinoline condensate, 13 parts of reinforcing agent phenolic resin；16 parts of plasticiser dicyclohexyl phthalate；Diphenylguanidine ETU7 parts； Diphenylguanidine PG7 parts；0.9 part of sulphur；With Graphene as filler, weight fraction is 4 parts.
A kind of preparation method of the cold-resistant sealing ring based on Graphene/polymer composites, comprises the following steps：
Step（1）：Take Graphene to pour into alcoholic solution, it is 1 to prepare mass ratio:35 suspension, machine is dissipated using ultrasound point system In prepare graphene uniform solution；
Step（2）：By fluorine unpigmented rubber, plasticizer phthalic acid dicyclohexyl maleate, EO/PO block polyethers, activating agent zinc oxide and Sulphur, carries out abrasive material in addition material grinder, the abrasive material time is 25 hours；
Step（3）：The mixture that abrasive material is obtained is added by step（1）In obtained graphene solution, mixed solution is obtained；
Step（4）：By step（3）In mixed solution kneaded in internal rubber mixer 2 minutes after to sequentially add plasticizer adjacent Dicyclo-hexyl phthlate, antiaging agent 2,2,4- trimethyl -1,2- dihyaroquinolines condensate, reinforcing agent phenolic resin, modeling Agent dicyclohexyl phthalate, diphenylguanidine ETU and diphenylguanidine PG, melting temperature are 85 DEG C, and mixing time is 2 hours, Then 185 DEG C are warming up to the speed of 10 DEG C/min, punching press is in blocks, Temperature fall；
Step（5）：By step（4）In sheet material put mould into, in putting mould into vulcanizer, be warming up to 160 DEG C, boost to 20MPa, the duration is 1 hour；
Step（6）After release pressure, the demoulding naturally cools to room temperature, carries out deburring treatment, is obtained multiple based on Graphene/polymer The cold-resistant sealing ring of condensation material.
The internal rubber mixer includes support 1 and refining glue room 2, and the top of the refining glue room 2 is provided with feed box 3, institute The both sides for stating feed box 3 are provided with feeding mouth 4；The top of the refining glue room 2 is provided with pressure-applying unit；The pressure-applying unit includes turbine Increase device 9, the turbocharger 9 is connected by worm screw 10 with floating weight 11, floating weight 11 is located at just going up for refining glue room 2 Side, pushes up bolt 12 under being arranged right below of refining glue room.
Be provided with inside the refining glue room 2 turn rod 5 and under turn rod 6, it is described on turn rod 5 and under turn rod 6 and be provided with hobboing cutter 7, On turn rod 5 and under turn the relative motion of rod 6；The bottom of the refining glue room 2 is provided with discharging opening 8, and the discharging opening 8 extends to support Outward；Filter screen is equipped with by screw at the discharging opening 8, formation is detachably connected.
Also include temperature sensor 13 in the refining glue room 2, the side of refining glue room 2 is provided with dedusting cabin 14, the dedusting cabin 14 bottom is connected by screw with the upper surface of support 1；The bottom of the dedusting cabin 14 is provided with reservoir 15.
When rubber mixing machine works, above turn rod 5 and under turn that rod 6 is relative to turn round, the material in feed box 3 is clamped and brings roll gap receipts into To the extruding and shearing of roller, through roll gap after with it is lower top bolt touch, the top of roll gap is returned along the gap of roller, therefore Material is crushed because of the shearing for receiving.
Sum it up, the present invention provides new formula, simple, rational solving by fluorine unpigmented rubber sealing ring is main material The problem of the sealing ring cold resistance difference that material is prepared from；Effectively mixture is screened, it is ensured that the size of mixture, increase mixed The stability of compound, improves the quality of shaped article.

Claims (9)

1. a kind of cold-resistant sealing ring based on Graphene/polymer composites, the composite with polymer as matrix, with stone Black alkene is filler, it is characterised in that polymer fraction by weight includes：100 parts of fluorine unpigmented rubber；EO/PO block polyethers 5- 12 parts；6-15 parts of activating agent zinc oxide；4-15 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- trimethyls- 1,2- 4-15 parts of dihyaroquinoline condensate, 9-16 parts of reinforcing agent phenolic resin；Plasticiser dicyclohexyl phthalate 12-20 Part；Diphenylguanidine ETU3-10 parts；Diphenylguanidine PG3-10 parts；Sulphur 0.6-1.2 parts；Characterized in that, with Graphene as filler, Weight fraction is 0.06-18 parts.
2. the preparation method of the cold-resistant sealing ring based on Graphene/polymer composites described in a kind of claim 1, it is special Levy and be, comprise the following steps：
Step（1）：Take Graphene to pour into alcoholic solution, it is 1 to prepare mass ratio:10-1:50 suspension, using ultrasound point system Graphene uniform solution is prepared in scattered machine；
Step（2）：By fluorine unpigmented rubber, plasticizer phthalic acid dicyclohexyl maleate, EO/PO block polyethers, activating agent zinc oxide and Sulphur, carries out abrasive material in addition material grinder, the abrasive material time is 25-36 hours；
Step（3）：The mixture that abrasive material is obtained is added by step（1）In obtained graphene solution, mixed solution is obtained；
Step（4）：By step（3）In mixed solution kneaded in internal rubber mixer 2 minutes after to sequentially add plasticizer adjacent Dicyclo-hexyl phthlate, antiaging agent 2,2,4- trimethyl -1,2- dihyaroquinolines condensate, reinforcing agent phenolic resin, modeling Agent dicyclohexyl phthalate, diphenylguanidine ETU and diphenylguanidine PG, melting temperature are 85 DEG C -105 DEG C, and mixing time is 2 Hour, 185 DEG C -200 DEG C then are warming up to the speed of 10 DEG C/min, punching press is in blocks, Temperature fall；
Step（5）：By step（4）In sheet material put mould into, in putting mould into vulcanizer, be warming up to 120-170 DEG C, rise 10-30MPa is depressed into, the duration is 1-2 hours；
Step（6）After release pressure, the demoulding naturally cools to room temperature, carries out deburring treatment, is obtained multiple based on Graphene/polymer The cold-resistant sealing ring of condensation material.
3. the cold-resistant sealing ring based on Graphene/polymer composites according to claim 1 and 2, it is characterised in that The constituent based on Graphene/polymer composites includes：100 parts of fluorine unpigmented rubber；EO/PO block polyethers 8-10 Part；8-12 parts of activating agent zinc oxide；6-12 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- trimethyl -1, 6-12 parts of 2- dihyaroquinoline condensates, 12-14 parts of reinforcing agent phenolic resin；Plasticiser dicyclohexyl phthalate 14-18 Part；Diphenylguanidine ETU5-8 parts；Diphenylguanidine PG5-8 parts；Sulphur 0.8-1.0 parts；Graphene 0.5-12 parts.
4. the cold-resistant sealing ring based on Graphene/polymer composites according to claim 1 and 2, it is characterised in that The constituent based on Graphene/polymer composites includes：100 parts of fluorine unpigmented rubber；9 parts of EO/PO block polyethers；It is living 10 parts of property agent zinc oxide；10 parts of plasticizer phthalic acid dicyclohexyl maleate, antiaging agent 2,2,4- trimethyl -1,2- dihydros 11 parts of quinoline condensate, 13 parts of reinforcing agent phenolic resin；16 parts of plasticiser dicyclohexyl phthalate；Diphenylguanidine ETU7 parts； Diphenylguanidine PG7 parts；0.9 part of sulphur；4 parts of Graphene.
5. the preparation method of the cold-resistant sealing ring based on Graphene/polymer composites according to claim 2, it is special Levy and be, the internal rubber mixer includes support and refining glue room, and feed box, the pan feeding are provided with the top of the refining glue room The both sides of case are provided with feeding mouth；Pressure-applying unit is provided with above the refining glue room；The refining glue chamber interior be provided with turn rod and under Turn rod, it is described on turn rod and under turn rod and be provided with hobboing cutter, above turn rod and under turn rod relative motion；The bottom of the refining glue room is provided with Discharging opening, the discharging opening is extended to outside support.
6. the preparation method of the cold-resistant sealing ring based on Graphene/polymer composites according to claim 5, it is special Levy and be, the discharge outlet is equipped with filter screen by screw, formation is detachably connected.
7. the preparation method of the cold-resistant sealing ring based on Graphene/polymer composites according to claim 5, it is special Levy and be, the pressure-applying unit includes that turbine increases device, and the turbocharger is connected by worm screw with floating weight, floating weight The top bolt under the surface of refining glue room, being arranged right below of refining glue room.
8. the preparation method of the cold-resistant sealing ring based on Graphene/polymer composites according to claim 5, it is special Levy and be, also include temperature sensor in the refining glue room, the side of refining glue room is provided with dedusting cabin, the bottom of the dedusting cabin with The upper surface of support is connected by screw.
9. the preparation method of the cold-resistant sealing ring based on Graphene/polymer composites according to claim 8, it is special Levy and be, the bottom of the dedusting cabin is provided with reservoir.
CN201611003159.4A 2016-11-15 2016-11-15 A kind of cold-resistant sealing ring and preparation method based on Graphene/polymer composites Pending CN106751233A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021243866A1 (en) * 2020-06-02 2021-12-09 鄂州市兴方磨具有限公司 Resin liquid weighing device for rice milling emery roll
CN114851449A (en) * 2022-04-29 2022-08-05 四川大学 Polymer aging acceleration processing device and processing method
CN115448673A (en) * 2022-10-24 2022-12-09 上海镎素工业技术有限公司 Cement-based material with strong stability and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021243866A1 (en) * 2020-06-02 2021-12-09 鄂州市兴方磨具有限公司 Resin liquid weighing device for rice milling emery roll
CN114851449A (en) * 2022-04-29 2022-08-05 四川大学 Polymer aging acceleration processing device and processing method
CN114851449B (en) * 2022-04-29 2023-05-26 四川大学 Polymer aging acceleration treatment device and treatment method
CN115448673A (en) * 2022-10-24 2022-12-09 上海镎素工业技术有限公司 Cement-based material with strong stability and preparation method thereof

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