CN109370119A - A kind of high tenacity rubber seal - Google Patents
A kind of high tenacity rubber seal Download PDFInfo
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- CN109370119A CN109370119A CN201811098087.5A CN201811098087A CN109370119A CN 109370119 A CN109370119 A CN 109370119A CN 201811098087 A CN201811098087 A CN 201811098087A CN 109370119 A CN109370119 A CN 109370119A
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- 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
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- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a kind of high tenacity rubber seal, belong to rubber composite material manufacture field.The present invention uses hydrazine hydrate reduction graphene oxide for redox graphene, and it is added in rubber constituent as decentralized medium, most of oxygen-containing functional group can be removed and retain the lamellar structure of graphene oxide, avoid the concentration of stress, whole toughness is improved, added saltcake, ethyl orthosilicate compounding can be in rubber matrix foaming process, the microcellular structure with uniform pore size is formed, the effect of internal mechanical property is improved；The present invention mixes object to tripoli and palygorskite and is modified, acidified, ultrasonic treatment improves surface-active, silane coupling agent and the hydroxyl on its surface act on, while being grafted to form polynary cross-linked network with rubber molecular chain, also the mechanical property after the vulcanization of rubber can be made to be effectively improved.The present invention solves the problems, such as that the toughness of common rubber seal and mechanical property are bad at present.
Description
Technical field
The invention belongs to rubber composite material manufacture fields, and in particular to a kind of high tenacity rubber seal.
Background technique
Sealing ring is the important composition element of rubber product, at present in automobile, electric appliance and electronics, the office big field of instrument three
Using outer, it is also largely used to the high-tech areas such as building, medical treatment, food industry and Aeronautics and Astronautics, the rubber material of different field
The property for needing to have different.
Sealing ring answers resilience height, hardness moderate, and compression set is small；With preferable mechanical property: as stretched
Intensity, determine tensile strength, elongation at break reaches certain standard；With wearability, tear resistance is strong；It is steady with chemical property
It is fixed, it is strong to adapt to working media ability, it is not easy to generate swelling, decompose, hardening；With certain weatherability.
Sealing ring, the circular cowling being made of one or several parts are fixed on a lasso or washer for bearing simultaneously
The narrow labyrinth clearance with another lasso or washer contacts or formation prevents lubricating oil leakage and foreign object intrusion.Sealing ring is a kind of
Section is circular rubber ring, because its section is O-shaped, therefore is called O-ring seal.
Rubber has good comprehensive performance, and metal adhesion, mechanical property, fatigue behaviour, ageing-resistant, heat is low etc.
Performance is all higher.Rubber seal is applied in all trades and professions, and nitrile rubber is by butadiene and acrylonitrile through emulsion polymerization
Made from method, oil resistivity is fabulous, and wearability is higher, and heat resistance is preferable, and bonding force is strong, the use of temperature is typically up to 120 DEG C.With
The development of automobile industry, people vehicle safety, comfort are also required it is higher, therefore to the use temperature of auto parts and components
And service life is also higher and higher, as automobile engine and periphery are related to rubber component heatproof and require to be increased to 150 DEG C.
The circular cowling that rubber seal is made of one or several parts is fixed on the barrier that elasticity is formed in gap,
Play barrier and sealing function.Be divided into liquid sealing and hermetic seal, liquid sealing in oil sealing it is complex.Such as start in vehicle
The rubber seal used on the components such as cylinder, piston on machine will not only realize that obstruction seals act on, simultaneously as institute is close
The medium of envelope is fuel oil or lubricating oil, so rubber seal has to oil resistant, high temperature resistant, fireproof characteristic, current rubber
Glue sealing ring is frequently run onto the bad problems such as heat-resisting, oil resistant, resistance to ozone, tensile strength is low, and the longevity is installed and used in mechanical part
It orders short.Therefore a kind of high tenacity rubber seal that toughness mechanical property is good need to be developed.
Summary of the invention
The technical problems to be solved by the invention: bad for the toughness and mechanical property of current common rubber seal
Problem provides a kind of high tenacity rubber seal.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of high tenacity rubber seal, including following component: 6 ~ 10 parts of dead plasters, 15 ~ 25 parts of fluorubber, 12 ~ 20 parts
Nitrile rubber, 2 ~ 5 parts of auxiliary agents, further includes: 15 ~ 30 parts of composite auxiliary materials, 12 ~ 25 parts of composite modified building stones.
The preparation method of the composite auxiliary material, includes the following steps:
(1) in 28 ~ 40 DEG C, take graphene oxide 1:25 in mass ratio ~ 40 that water mixing is added, oxidation stone is added in supersonic oscillations
The hydrazine hydrate of black alkene quality 8 ~ 14%, the ammonium hydroxide of graphene oxide quality 2 ~ 5% are mixed, and are warming up to 80 ~ 95 DEG C, keep the temperature, take out
Filter, takes filter residue to be washed with dehydrated alcohol, dry, obtains pretreating graphite alkene；
(2) according to the mass fraction, 20 ~ 40 parts of pretreating graphite alkene, 3 ~ 7 parts of coupling agent KH-560,6 ~ 10 parts of positive silicic acid are successively taken
Ethyl ester, 4 ~ 8 parts of saltcake, 10 ~ 15 parts of zinc acrylate resins, 6 ~ 10 parts of surfactants, 2 ~ 5 parts of fillers, 50 ~ 70 parts of reagent As, in 30 ~
It 45 DEG C, first takes ethyl orthosilicate, saltcake, zinc acrylate resin, surfactant, reagent A to be mixed, is warming up to 55 ~ 70 DEG C, be added
Coupling agent, pretreating graphite alkene, filler mixing, shearing dispersion obtain dispersion, take dispersion rotary evaporation to get composite auxiliary material.
Surfactant in the step (2): 8:1 ~ 3 take neopelex, laureth in mass ratio
Sodium sulfovinate mixes to get surfactant.
Filler in the step (2): 4 ~ 8:1 in mass ratio takes polyvinylpyrrolidone, microcrystalline wax mixing to get filling out
Material.
Reagent A in the step (2): 3:10 ~ 16 take Dopamine hydrochloride, PBS buffer solution mixing to get examination in mass ratio
Agent A.
The preparation method of the composite modified building stones, includes the following steps:
S1. 5:1 ~ 3 take tripoli, palygorskite to pulverize and sieve in mass ratio, take sieving particle 1:20 in mass ratio ~ 30 that sulfuric acid is added
Solution mixing, ultrasonication are stored at room temperature, and are filtered, and filter residue is taken to be heat-treated in 400 ~ 450 DEG C, and filter residue quality 2 ~ 5% is added
Span-80, the silane resin acceptor kh-550 of filter residue quality 3 ~ 7%, 4 ~ 8 times of filter residue quality of toluene are mixed, in 60 ~ 80 DEG C
7 ~ 10h of back flow reaction, it is cooling, it filters, obtains filter cake, filter cake is taken to be cleaned with ethanol solution, it is dry, obtain modified building stones；
S2. take modified building stones 1:25 in mass ratio ~ 35 be added reagent B be mixed, in 60 ~ 80 DEG C flow back 20 ~ for 24 hours, be added stone
The thiocarbamide mixing for expecting quality 30 ~ 50%, keeps the temperature, thiocarbamide, 15 ~ 30 times of building stones quality of the NaOH that building stones quality 60 ~ 80% is added are molten
Liquid mixing, keeps the temperature, and filtering takes filter residue to be washed with water, and is freeze-dried to get composite modified building stones.
Reagent B in the step S2: 1:12 ~ 18 take epoxy chloroethanes, acetone mixing to get reagent B in mass ratio.
The promotor: Vulcanization accelerator TMTD, captax, any one in promotor ZDMC.
The antiaging agent: antioxidant 4020, anti-aging agent RD, any one in antioxidant NBC.
The auxiliary agent: 1:3 ~ 6:1 in mass ratio takes magnesia, pentaerythrite, zinc oxide mixing to get auxiliary agent.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention uses hydrazine hydrate reduction graphene oxide for redox graphene, and is added to as decentralized medium
In rubber constituent, most of oxygen-containing functional group can be removed and retain the lamellar structure of graphene oxide, so that inside the present invention
Toughness is improved, well dispersed redox graphene to rubber bodies have good reinforcing effect, lamella size with
Rubber molecule ingredient combines, and generates a kind of vitreum layer in interface, strand when stretching in vitreum layer be easy to along
Filler surface occurs reorientation and improves whole toughness, added saltcake, positive silicic acid so as to avoid the concentration of stress
Ethyl ester compounding, can be in rubber matrix foaming process, microcellular structure of the formation with uniform pore size, existing good elasticity, together
When again can to the hole wall of this system carry out reinforcement, make it have enough hardness, the presence of microcellular structure can effectively play dispersion
Stress, mitigate impact friction, improve inside mechanical property effect；
(2) present invention mixes object to tripoli and palygorskite and is modified, and acidified, ultrasonic treatment improves surface-active, and silane is even
The hydroxyl for joining agent and its surface acts on, and then, is associated with thiourea modified raising with the complexing of metal ion, improves the mutual of inside
Active force, in subsequent Vulcanization Process of Rubber, zinc acrylate resin can cooperate composite modified building stones to improve its cross-linking efficiency and be crosslinked close
Degree, while being grafted to form polynary cross-linked network with rubber molecular chain, the mechanical property after capable of also making the vulcanization of rubber obtains effectively
Improve.
Specific embodiment
Promotor: Vulcanization accelerator TMTD, captax, any one in promotor ZDMC.
Antiaging agent: antioxidant 4020, anti-aging agent RD, any one in antioxidant NBC.
Filler: 4 ~ 8:1 in mass ratio takes polyvinylpyrrolidone, microcrystalline wax mixing to get filler.
Reagent A: the PBS buffer solution that 3:10 ~ 16 take Dopamine hydrochloride in mass ratio, pH is 6.5 ~ 6.8 mixes to get reagent
A。
Reagent B: 1:12 ~ 18 take epoxy chloroethanes, acetone mixing to get reagent B in mass ratio.
Surfactant: 8:1 ~ 3 take neopelex, the mixing of laureth sodium sulfovinate in mass ratio, i.e.,
Obtain surfactant.
Auxiliary agent: 1:3 ~ 6:1 in mass ratio takes magnesia, pentaerythrite, zinc oxide mixing to get auxiliary agent.
The preparation method of composite auxiliary material, includes the following steps:
(1) in 28 ~ 40 DEG C, take graphene oxide 1:25 in mass ratio ~ 40 that water mixing is added, move to supersonic oscillations instrument with 45 ~
55kHz frequency ultrasonic wave vibrates 15 ~ 25min, be added the hydrazine hydrate of graphene oxide quality 8 ~ 14%, graphene oxide quality 2 ~
The ammonium hydroxide of 5% concentration 1mol/L is mixed in reaction kettle, with 450 ~ 800r/min, 30 ~ 50min of magnetic agitation, is warming up to 80 ~ 95
DEG C, 1 ~ 3h is kept the temperature, is filtered, after taking filter residue wash 2 ~ 4 times with dehydrated alcohol, 20 are dried in 65 ~ 80 DEG C of vacuum ovens ~ for 24 hours, it obtains
Pretreating graphite alkene；
(2) according to the mass fraction, successively take 20 ~ 40 parts of pretreating graphite alkene, 3 ~ 7 parts of coupling agents, 6 ~ 10 parts of ethyl orthosilicates, 4 ~
8 parts of saltcake, 10 ~ 15 parts of zinc acrylate resins, 6 ~ 10 parts of surfactants, 2 ~ 5 parts of fillers, 50 ~ 70 parts of reagent As, in 30 ~ 45 DEG C, first
It takes ethyl orthosilicate, saltcake, zinc acrylate resin, surfactant, reagent A to mix in reaction kettle, is stirred with 450 ~ 700r/min magnetic force
35 ~ 60min is mixed, is warming up to 55 ~ 70 DEG C, coupling agent KH-560, pretreating graphite alkene, filler mixing is added, with 2000 ~ 3000r/
Min shearing dispersion 15 ~ 25min, obtain dispersion, take dispersion in 80 ~ 100 DEG C of rotary evaporations to constant weight to get composite auxiliary material.
The preparation method of composite modified building stones, includes the following steps:
S1. 5:1 ~ 3 take tripoli, palygorskite to crushed 120 meshes in pulverizer in mass ratio, take sieving particle in mass ratio 1:
20 ~ 30 be added mass fractions 10% sulfuric acid solutions mixing, move to supersonic oscillations instrument with 45 ~ 55kH frequency ultrasonic wave processing 15 ~
25min is stored at room temperature 1 ~ 3h, filters, takes filter residue after 400 ~ 450 DEG C of 35 ~ 60min of heat treatment, and filter residue quality 2 ~ 5% is added
Span-80, the silane resin acceptor kh-550 of filter residue quality 3 ~ 7%, the mixing of 4 ~ 8 times of filter residue quality of toluene, with 500 ~ 800r/min
After 30 ~ 55min of magnetic agitation, in 60 ~ 80 DEG C of 7 ~ 10h of back flow reaction, cooled to room temperature filters, obtains filter cake, filter cake is taken to use
After the ethanol solution that volume fraction is 60% cleans 3 ~ 5 times, in 80 ~ 100 DEG C of vacuum drying ovens dry 20 ~ for 24 hours, modified building stones are obtained；
S2. take modified building stones 1:25 in mass ratio ~ 35 be added reagent B be mixed, in 60 ~ 80 DEG C flow back 20 ~ for 24 hours after, be added
The thiocarbamide of building stones quality 30 ~ 50% mixes, keep the temperature 5 ~ 8h, be added building stones quality 60 ~ 80% thiocarbamide, 15 ~ 30 times of building stones quality
The NaOH solution of concentration 1mol/L mixes, and keeps the temperature 2 ~ 4h, filtering, after taking filter residue to be washed with water and be neutral to washing lotion, move to -40 DEG C it is cold
Dry 40 ~ the 44h of lyophilizer is to get composite modified building stones.
A kind of high tenacity rubber seal, according to the mass fraction, including following component: 6 ~ 10 parts of dead plasters, 15 ~ 25
Part fluorubber, 12 ~ 20 parts of nitrile rubbers, 2 ~ 5 parts of auxiliary agents, 15 ~ 30 parts of composite auxiliary materials, 12 ~ 25 parts of composite modified building stones.
A kind of preparation method of high tenacity rubber seal, includes the following steps:
(1) according to the mass fraction, take 6 ~ 10 parts of dead plasters, 15 ~ 25 parts of fluorubber, 12 ~ 20 parts of nitrile rubbers, 2 ~ 5 parts help
Agent, 15 ~ 30 parts of composite auxiliary materials, 12 ~ 25 parts of composite modified building stones；
(2) in 35 ~ 50 DEG C, dead plaster, fluorubber, nitrile rubber, composite auxiliary material is first taken to mix in batch mixer, with 400 ~
600r/min 40 ~ 60min of magnetic agitation, add composite modified building stones, auxiliary agent mixing, with 1000 ~ 15000r/min stirring 1 ~
After 3h, mixer is put into, in 105 ~ 115 DEG C of 6 ~ 10min that plasticate, must plasticate material, then through calender calendering formation, obtain blank, take
Blank is in vulcanizing press, and under 175 ~ 190 DEG C, 40 ~ 50MPa pressure condition, 2 ~ 5h of hot-press vulcanization discharges to get high tenacity
Rubber seal.
Embodiment 1
Promotor: Vulcanization accelerator TMTD.
Antiaging agent: antioxidant 4020.
Filler: 4:1 in mass ratio takes polyvinylpyrrolidone, microcrystalline wax mixing to get filler.
Reagent A: the PBS buffer solution that 3:10 in mass ratio takes Dopamine hydrochloride, pH is 6.5 ~ 6.8 mixes to get reagent A.
Reagent B: 1:12 in mass ratio takes epoxy chloroethanes, acetone mixing to get reagent B.
Surfactant: 8:1 in mass ratio take neopelex, laureth sodium sulfovinate mixing to get
Surfactant.
Auxiliary agent: 1:3:1 in mass ratio takes magnesia, pentaerythrite, zinc oxide mixing to get auxiliary agent.
The preparation method of composite auxiliary material, includes the following steps:
(1) it in 28 DEG C, takes graphene oxide 1:25 in mass ratio that water mixing is added, moves to supersonic oscillations instrument with 45kHz frequency
The ammonia of the hydrazine hydrate of graphene oxide quality 8%, the concentration 1mol/L of graphene oxide quality 2% is added in supersonic oscillations 15min
Water is mixed in reaction kettle, with 450r/min magnetic agitation 30min, is warming up to 80 DEG C, is kept the temperature 1h, filters, take filter residue with anhydrous second
After alcohol washs 2 times, in the dry 20h of 65 DEG C of vacuum ovens, pretreating graphite alkene is obtained；
(2) according to the mass fraction, 20 parts of pretreating graphite alkene, 3 parts of coupling agents, 6 parts of ethyl orthosilicates, 4 parts of saltcake, 10 are successively taken
Part zinc acrylate resin, 6 parts of surfactants, 2 parts of fillers, 50 parts of reagent As first take ethyl orthosilicate, saltcake, acrylic acid in 30 DEG C
Zinc, surfactant, reagent A are mixed in reaction kettle, with 450r/min magnetic agitation 35min, are warming up to 55 DEG C, coupling agent is added
KH-560, pretreating graphite alkene, filler mixing shear dispersion 15min with 2000r/min, obtain dispersion, take dispersion in 80 DEG C
Rotary evaporation is to constant weight to get composite auxiliary material.
The preparation method of composite modified building stones, includes the following steps:
S1. 5:1 in mass ratio takes tripoli, palygorskite to crushed 120 meshes in pulverizer, takes sieving particle 1:20 in mass ratio
The sulfuric acid solution mixing of mass fraction 10% is added, moves to supersonic oscillations instrument with 45kH frequency ultrasonic wave and handles 15min, room temperature
1h is stood, filters, takes filter residue after 400 DEG C of heat treatment 35min, the Span-80 of filter residue quality 2%, the silicon of filter residue quality 3% is added
Alkane coupling agent KH-550, the mixing of 4 times of filter residue quality of toluene, after 500r/min magnetic agitation 30min, in 60 DEG C of back flow reactions
7h, cooled to room temperature filter, obtain filter cake, after taking filter cake to clean 3 times with the ethanol solution that volume fraction is 60%, in 80 DEG C
Vacuum drying oven dries 20h, obtains modified building stones；
S2. it takes modified building stones 1:25 in mass ratio that reagent B is added to be mixed, after 60 DEG C of reflux 20h, building stones quality is added
30% thiocarbamide mixing, keeps the temperature 5h, and the thiocarbamide of building stones quality 60%, the NaOH solution of 15 times of building stones quality of concentration 1mol/L is added
Mixing, keeps the temperature 2h, filtering, after taking filter residue to be washed with water and be neutral to washing lotion, moves to the dry 40h of -40 DEG C of freeze driers to get multiple
Close modified building stones.
A kind of high tenacity rubber seal, according to the mass fraction, including following component: 6 parts of dead plasters, 15 parts of fluorine rubbers
Glue, 12 parts of nitrile rubbers, 2 parts of auxiliary agents, 15 parts of composite auxiliary materials, 12 parts of composite modified building stones.
A kind of preparation method of high tenacity rubber seal, includes the following steps:
(1) according to the mass fraction, take 6 parts of dead plasters, 15 parts of fluorubber, 12 parts of nitrile rubbers, 2 parts of auxiliary agents, 15 parts it is compound
Auxiliary material, 12 parts of composite modified building stones；
(2) in 35 DEG C, dead plaster, fluorubber, nitrile rubber, composite auxiliary material is taken to mix in batch mixer, first with 400r/min
Magnetic agitation 40min adds composite modified building stones, auxiliary agent mixing, after stirring 1h with 1000r/min, puts into mixer, in
105 DEG C of 6min that plasticate, must plasticate material, then through calender calendering formation, obtain blank, take blank in vulcanizing press, in 175 DEG C,
Under 40MPa pressure condition, hot-press vulcanization 2h discharges to get high tenacity rubber seal.
Embodiment 2
Promotor: captax.
Antiaging agent: anti-aging agent RD.
Filler: 6:1 in mass ratio takes polyvinylpyrrolidone, microcrystalline wax mixing to get filler.
Reagent A: the PBS buffer solution that 3:13 in mass ratio takes Dopamine hydrochloride, pH is 6.7 mixes to get reagent A.
Reagent B: 1:16 in mass ratio takes epoxy chloroethanes, acetone mixing to get reagent B.
Surfactant: 8:2 in mass ratio take neopelex, laureth sodium sulfovinate mixing to get
Surfactant.
Auxiliary agent: 1:5:1 in mass ratio takes magnesia, pentaerythrite, zinc oxide mixing to get auxiliary agent.
The preparation method of composite auxiliary material, includes the following steps:
(1) it in 35 DEG C, takes graphene oxide 1:35 in mass ratio that water mixing is added, moves to supersonic oscillations instrument with 50kHz frequency
The concentration 1mol/L of the hydrazine hydrate of graphene oxide quality 12%, graphene oxide quality 4% is added in supersonic oscillations 20min
Ammonium hydroxide is mixed in reaction kettle, with 600r/min magnetic agitation 40min, is warming up to 85 DEG C, is kept the temperature 2h, filters, and takes filter residue with anhydrous
After ethanol washing 3 times, in the dry 22h of 70 DEG C of vacuum ovens, pretreating graphite alkene is obtained；
(2) according to the mass fraction, 30 parts of pretreating graphite alkene, 5 parts of coupling agents, 8 parts of ethyl orthosilicates, 6 parts of saltcake, 13 are successively taken
Part zinc acrylate resin, 8 parts of surfactants, 4 parts of fillers, 60 parts of reagent As first take ethyl orthosilicate, saltcake, acrylic acid in 40 DEG C
Zinc, surfactant, reagent A are mixed in reaction kettle, with 600r/min magnetic agitation 50min, are warming up to 60 DEG C, coupling agent is added
KH-560, pretreating graphite alkene, filler mixing shear dispersion 20min with 2500r/min, obtain dispersion, take dispersion in 90 DEG C
Rotary evaporation is to constant weight to get composite auxiliary material.
The preparation method of composite modified building stones, includes the following steps:
S1. 5:2 in mass ratio takes tripoli, palygorskite to crushed 120 meshes in pulverizer, takes sieving particle 1:25 in mass ratio
The sulfuric acid solution mixing of mass fraction 10% is added, moves to supersonic oscillations instrument with 50kH frequency ultrasonic wave and handles 20min, room temperature
2h is stood, filters, takes filter residue after 425 DEG C of heat treatment 50min, the Span-80 of filter residue quality 4%, the silicon of filter residue quality 5% is added
Alkane coupling agent KH-550, the mixing of 6 times of filter residue quality of toluene, after 700r/min magnetic agitation 45min, in 70 DEG C of back flow reactions
9h, cooled to room temperature filter, obtain filter cake, after taking filter cake to clean 4 times with the ethanol solution that volume fraction is 60%, in 90 DEG C
Vacuum drying oven dries 22h, obtains modified building stones；
S2. it takes modified building stones 1:30 in mass ratio that reagent B is added to be mixed, after 70 DEG C of reflux 22h, building stones quality is added
40% thiocarbamide mixing, keeps the temperature 6h, and the thiocarbamide of building stones quality 70%, the NaOH solution of 20 times of building stones quality of concentration 1mol/L is added
Mixing, keeps the temperature 3h, filtering, after taking filter residue to be washed with water and be neutral to washing lotion, moves to the dry 42h of -40 DEG C of freeze driers to get multiple
Close modified building stones.
A kind of high tenacity rubber seal, according to the mass fraction, including following component: 8 parts of dead plasters, 20 parts of fluorine rubbers
Glue, 18 parts of nitrile rubbers, 4 parts of auxiliary agents, 25 parts of composite auxiliary materials, 20 parts of composite modified building stones.
A kind of preparation method of high tenacity rubber seal, includes the following steps:
(1) according to the mass fraction, take 8 parts of dead plasters, 20 parts of fluorubber, 18 parts of nitrile rubbers, 4 parts of auxiliary agents, 20 parts it is compound
Auxiliary material, 20 parts of composite modified building stones；
(2) in 40 DEG C, dead plaster, fluorubber, nitrile rubber, composite auxiliary material is taken to mix in batch mixer, first with 500r/min
Magnetic agitation 50min adds composite modified building stones, auxiliary agent mixing, after stirring 2h with 1250r/min, puts into mixer, in
110 DEG C of 8min that plasticate, must plasticate material, then through calender calendering formation, obtain blank, take blank in vulcanizing press, in 180 DEG C,
Under 45MPa pressure condition, hot-press vulcanization 4h discharges to get high tenacity rubber seal.
Embodiment 3
Promotor: promotor ZDMC.
Antiaging agent: antioxidant NBC.
Filler: 8:1 in mass ratio takes polyvinylpyrrolidone, microcrystalline wax mixing to get filler.
Reagent A: the PBS buffer solution that 3:16 in mass ratio takes Dopamine hydrochloride, pH is 6.8 mixes to get reagent A.
Reagent B: 1:18 in mass ratio takes epoxy chloroethanes, acetone mixing to get reagent B.
Surfactant: 8:3 in mass ratio take neopelex, laureth sodium sulfovinate mixing to get
Surfactant.
Auxiliary agent: 1:6:1 in mass ratio takes magnesia, pentaerythrite, zinc oxide mixing to get auxiliary agent.
The preparation method of composite auxiliary material, includes the following steps:
(1) it in 40 DEG C, takes graphene oxide 1:40 in mass ratio that water mixing is added, moves to supersonic oscillations instrument with 55kHz frequency
The concentration 1mol/L of the hydrazine hydrate of graphene oxide quality 14%, graphene oxide quality 5% is added in supersonic oscillations 25min
Ammonium hydroxide is mixed in reaction kettle, with 800r/min magnetic agitation 50min, is warming up to 95 DEG C, is kept the temperature 1 ~ 3h, filters, take filter residue nothing
It is dry for 24 hours in 80 DEG C of vacuum ovens after water-ethanol washs 4 times, obtain pretreating graphite alkene；
(2) according to the mass fraction, successively take 40 parts of pretreating graphite alkene, 7 parts of coupling agents, 10 parts of ethyl orthosilicates, 8 parts of saltcake,
15 parts of zinc acrylate resins, 10 parts of surfactants, 5 parts of fillers, 70 parts of reagent As first take ethyl orthosilicate, saltcake, propylene in 45 DEG C
Sour zinc, surfactant, reagent A are mixed in reaction kettle, with 700r/min magnetic agitation 60min, are warming up to 70 DEG C, coupling is added
Agent KH-560, pretreating graphite alkene, filler mixing, with 3000r/min shear dispersion 25min, obtain dispersion, take dispersion in
100 DEG C of rotary evaporations are to constant weight to get composite auxiliary material.
The preparation method of composite modified building stones, includes the following steps:
S1. 5:3 in mass ratio takes tripoli, palygorskite to crushed 120 meshes in pulverizer, takes sieving particle 1:30 in mass ratio
The sulfuric acid solution mixing of mass fraction 10% is added, moves to supersonic oscillations instrument with 55kH frequency ultrasonic wave and handles 25min, room temperature
3h is stood, filters, takes filter residue after 450 DEG C of heat treatment 60min, the Span-80 of filter residue quality 5%, the silicon of filter residue quality 7% is added
Alkane coupling agent KH-550, the mixing of 8 times of filter residue quality of toluene, after 800r/min magnetic agitation 55min, in 80 DEG C of back flow reactions
10h, cooled to room temperature filter, obtain filter cake, after taking filter cake to clean 5 times with the ethanol solution that volume fraction is 60%, in 100
DEG C vacuum drying oven is dry for 24 hours, obtains modified building stones；
S2. it takes modified building stones 1:35 in mass ratio that reagent B is added to be mixed, after 80 DEG C of reflux for 24 hours, building stones quality is added
50% thiocarbamide mixing, keeps the temperature 8h, and the thiocarbamide of building stones quality 80%, the NaOH solution of 30 times of building stones quality of concentration 1mol/L is added
Mixing, keeps the temperature 4h, filtering, after taking filter residue to be washed with water and be neutral to washing lotion, moves to the dry 44h of -40 DEG C of freeze driers to get multiple
Close modified building stones.
A kind of high tenacity rubber seal, according to the mass fraction, including following component: 10 parts of dead plasters, 25 parts of fluorine
Rubber, 20 parts of nitrile rubbers, 5 parts of auxiliary agents, 30 parts of composite auxiliary materials, 25 parts of composite modified building stones.
A kind of preparation method of high tenacity rubber seal, includes the following steps:
(1) according to the mass fraction, take 10 parts of dead plasters, 25 parts of fluorubber, 20 parts of nitrile rubbers, 5 parts of auxiliary agents, 30 parts it is compound
Auxiliary material, 25 parts of composite modified building stones；
(2) in 50 DEG C, dead plaster, fluorubber, nitrile rubber, composite auxiliary material is taken to mix in batch mixer, first with 600r/min
Magnetic agitation 60min adds composite modified building stones, auxiliary agent mixing, after stirring 3h with 15000r/min, puts into mixer, in
115 DEG C of 10min that plasticate, must plasticate material, then through calender calendering formation, obtain blank, take blank in vulcanizing press, in 190 DEG C,
Under 50MPa pressure condition, hot-press vulcanization 5h discharges to get high tenacity rubber seal.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking auxiliary agent.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking composite modified building stones.
Comparative example 3: the high tenacity rubber seal of Taicang company production.
Embodiment is tested with high tenacity rubber seal obtained by comparative example according to HG/T2579-94 standard, is tested
The results are shown in Table 1.
Table 1
In summary, high tenacity rubber seal of the invention is more preferable compared to commercial product effect, is worth promoting.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of high tenacity rubber seal, according to the mass fraction, including following component: 6 ~ 10 parts of dead plasters, 15 ~ 25 parts
Fluorubber, 12 ~ 20 parts of nitrile rubbers, 2 ~ 5 parts of auxiliary agents, which is characterized in that further include: 15 ~ 30 parts of composite auxiliary materials, 12 ~ 25 parts it is multiple
Close modified building stones.
2. a kind of high tenacity rubber seal according to claim 1, which is characterized in that the preparation side of the composite auxiliary material
Method includes the following steps:
(1) in 28 ~ 40 DEG C, take graphene oxide 1:25 in mass ratio ~ 40 that water mixing is added, oxidation stone is added in supersonic oscillations
The hydrazine hydrate of black alkene quality 8 ~ 14%, the ammonium hydroxide of graphene oxide quality 2 ~ 5% are mixed, and are warming up to 80 ~ 95 DEG C, keep the temperature, take out
Filter, takes filter residue to be washed with dehydrated alcohol, dry, obtains pretreating graphite alkene；
(2) according to the mass fraction, 20 ~ 40 parts of pretreating graphite alkene, 3 ~ 7 parts of coupling agent KH-560,6 ~ 10 parts of positive silicic acid are successively taken
Ethyl ester, 4 ~ 8 parts of saltcake, 10 ~ 15 parts of zinc acrylate resins, 6 ~ 10 parts of surfactants, 2 ~ 5 parts of fillers, 50 ~ 70 parts of reagent As, in 30 ~
It 45 DEG C, first takes ethyl orthosilicate, saltcake, zinc acrylate resin, surfactant, reagent A to be mixed, is warming up to 55 ~ 70 DEG C, be added
Coupling agent, pretreating graphite alkene, filler mixing, shearing dispersion obtain dispersion, take dispersion rotary evaporation to get composite auxiliary material.
3. a kind of high tenacity rubber seal according to claim 2, which is characterized in that the surface in the step (2) is living
Property agent: in mass ratio 8:1 ~ 3 take neopelex, laureth sodium sulfovinate mixing to get surfactant.
4. a kind of high tenacity rubber seal according to claim 2, which is characterized in that the filler in the step (2): press
4 ~ 8:1 of mass ratio takes polyvinylpyrrolidone, microcrystalline wax mixing to get filler.
5. a kind of high tenacity rubber seal according to claim 2, which is characterized in that the reagent A in the step (2):
3:10 ~ 16 take Dopamine hydrochloride, PBS buffer solution mixing to get reagent A in mass ratio.
6. a kind of high tenacity rubber seal according to claim 1, which is characterized in that the preparation of the composite modified building stones
Method includes the following steps:
S1. 5:1 ~ 3 take tripoli, palygorskite to pulverize and sieve in mass ratio, take sieving particle 1:20 in mass ratio ~ 30 that sulfuric acid is added
Solution mixing, ultrasonication are stored at room temperature, and are filtered, and filter residue is taken to be heat-treated in 400 ~ 450 DEG C, and filter residue quality 2 ~ 5% is added
Span-80, the silane resin acceptor kh-550 of filter residue quality 3 ~ 7%, 4 ~ 8 times of filter residue quality of toluene are mixed, in 60 ~ 80 DEG C
7 ~ 10h of back flow reaction, it is cooling, it filters, obtains filter cake, filter cake is taken to be cleaned with ethanol solution, it is dry, obtain modified building stones；
S2. take modified building stones 1:25 in mass ratio ~ 35 be added reagent B be mixed, in 60 ~ 80 DEG C flow back 20 ~ for 24 hours, be added stone
The thiocarbamide mixing for expecting quality 30 ~ 50%, keeps the temperature, thiocarbamide, 15 ~ 30 times of building stones quality of the NaOH that building stones quality 60 ~ 80% is added are molten
Liquid mixing, keeps the temperature, and filtering takes filter residue to be washed with water, and is freeze-dried to get composite modified building stones.
7. a kind of high tenacity rubber seal according to claim 6, which is characterized in that the reagent B in the step S2: press
Mass ratio 1:12 ~ 18 take epoxy chloroethanes, acetone mixing to get reagent B.
8. a kind of high tenacity rubber seal according to claim 1, which is characterized in that the promotor: Vulcanization accelerator TMTD,
Any one in captax, promotor ZDMC.
9. a kind of high tenacity rubber seal according to claim 1, which is characterized in that the antiaging agent: anti-aging agent
4020, anti-aging agent RD, any one in antioxidant NBC.
10. a kind of high tenacity rubber seal according to claim 1, which is characterized in that the auxiliary agent: 1:3 in mass ratio ~
6:1 takes magnesia, pentaerythrite, zinc oxide mixing to get auxiliary agent.
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| CN110527159A (en) * | 2019-08-30 | 2019-12-03 | 北京化工大学 | A kind of original position hydrorubber graphene elastomer and preparation method |
| CN113440290A (en) * | 2021-07-09 | 2021-09-28 | 上海驻净电子科技有限公司 | Gland sealing piece for tooth flushing device and manufacturing method thereof |
| WO2022037060A1 (en) * | 2020-08-19 | 2022-02-24 | 吴立中 | Preparation method for reduced graphene oxide nitrile rubber and for tooth block without tooth marks |
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