CN106221106A - A kind of preparation method of rubber tyre carcass resisting fatigue auxiliary agent - Google Patents
A kind of preparation method of rubber tyre carcass resisting fatigue auxiliary agent Download PDFInfo
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- CN106221106A CN106221106A CN201610636296.5A CN201610636296A CN106221106A CN 106221106 A CN106221106 A CN 106221106A CN 201610636296 A CN201610636296 A CN 201610636296A CN 106221106 A CN106221106 A CN 106221106A
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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
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F293/00—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule
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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
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/06—Copolymers with styrene
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
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Abstract
The invention discloses the preparation method of a kind of rubber tyre carcass resisting fatigue auxiliary agent, belong to rubber production auxiliary agent technical field.The present invention is by molybdenum bisuphide, silicon carbide whiskers etc. carry out oxidation and filter after pulverizing, filtering residue is added excusing from death vibration after methane liquid, collect lower sediment, take 1 octene and MAO again, ethylidene bichloride zirconocene carries out reacting to obtain octene ethylene copolymer equal under high pressure, it is subsequently adding vinylacetate, Ammonium persulfate. stirring reaction, reactant is added deionized water, organic facies carries out decompression and distills to obtain octene ethylene vinyl acetate blocked copolymer, it is added into the stirrings such as paraffin and lower sediment high-speed stirred, cooling, pack to obtain rubber tyre carcass resisting fatigue auxiliary agent.The present invention utilizes silicon carbide whisker preferably high temperature resistant property and good toughness, intensity, defect that the tensile property solving tradition resisting fatigue auxiliary agent is poor, heat aging property is the best etc., is with a wide range of applications.
Description
Technical field
The invention discloses the preparation method of a kind of rubber tyre carcass resisting fatigue auxiliary agent, belong to rubber production auxiliary agent technology
Field.
Background technology
Along with the development of transportation, the travel speed of automobile improves constantly, the tire deformation frequency when actual travel
Rate increases, and carcass heats up very fast, causes rubber to decline with the bonding force of cord, and the shoulder sky phenomenon of tire increases.Only by rubber
It is securely joined with being an entirety with cord, just can make composite normal delivery load when deformation, and be uniformly distributed stress,
Thus it is empty to reduce wheel tire shoulder.Antifatigue is by methyl lemon acid imide, activated form phenolic resin) complexation that forms of binding system
Thing, is mainly used in the cord ply compounds such as chinlon, artificial silk, polyester, can improve the bonding force of sizing material and cord, and can at high temperature protect
Hold bigger bonding force, and be difficult to reduction.Natural rubber products due to aging and lose effect be its in actual use
An inevitable outcome, the fatigue rupture of rubber is also a kind of form in its catabiosis, and it refers to that rubber is being subject to
Under the effect of certain frequency and cyclic stress, the breakoff phenomenon that the molecular structure of elastomeric material changes and occurs.
For elastomeric material, it refer to elastomeric material during repeated deformation, when its local deformation born should
When power exceedes elongation percentage or the limiting range of stress of rubber, fatigue process starts, to such an extent as to finally reaches destruction.This fatigue rupture
Starting point is owing to the inhomogeneities of rubber surface or inside is caused.Use carbon black filled natural rubber vulcanized rubber one
Under constant load during multi-drawing deformation, the physical and mechanical properties of rubber is in fatigue process, and hot strength gradually rose before this,
Beginning to decline after a maximum, the change of tearing strength, the dynamic modulus of elasticity and mechanical loss factor is the most contrary again.
Rubber manufacturing enterprise pays much attention to the research work improving natural rubber anti-fatigue performance and improving always both at home and abroad
Make, the anti-fatigue performance of natural rubber for the damping elastomer element being repeatedly subjected to stress effect be one particularly important
Performance, it is directly connected to vibration-damping function and whether lost efficacy and locomotive, vehicle safety operation conditions.So, natural rubber is resisted
The research of dynamic fatigue property has very important realistic meaning.But tradition rubber tyre carcass resisting fatigue auxiliary agent existence is drawn
Stretch that performance is low, heat aging property is the best, tearing strength and the problem such as rebound value is less.
Summary of the invention
The technical problem that present invention mainly solves: there is draftability for tradition rubber tyre carcass resisting fatigue auxiliary agent at present
The defects such as energy is low, heat aging property is the best, it is provided that the preparation method of a kind of rubber tyre carcass resisting fatigue auxiliary agent.The present invention
Carry out oxidation after molybdenum bisuphide, silicon carbide whisker etc. being pulverized to filter, filtering residue is added excusing from death vibration after methane liquid, collects lower floor
Precipitation, then take 1-octene and MAO, ethylidene bichloride zirconocene carries out reacting to obtain octene ethylene copolymer equal under high pressure
Thing, is subsequently adding vinylacetate, Ammonium persulfate. stirring reaction, reactant adds deionized water, and organic facies carries out decompression distillation
Octene-ethylene-vinylacetate blocked copolymer, be added into the stirrings such as paraffin and lower sediment high-speed stirred, cooling,
Pack to obtain rubber tyre carcass resisting fatigue auxiliary agent.The present invention utilizes silicon carbide whisker preferably high temperature resistant property and good tough
Property, intensity, defect that the tensile property solving tradition resisting fatigue auxiliary agent is poor, heat aging property is the best etc., have widely
Using value.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) 10～20g molybdenum bisuphide, 10～20g precipitated silica, 5～8g silicon carbide whisker, 6～8g glass fibre are weighed
Join in pulverizer and pulverize, cross 80～100 mesh sieves, obtain mixed-powder, mixed-powder is joined in beaker, to burning
Adding 200～300mL mass concentrations in Bei is 28～30% hydrogen peroxide, and stirring reaction 12～14h is filtered, obtained filtering residue, will filter
Slag joins in conical flask, adds 200～300mL methane liquids, is placed in supersonic oscillations instrument carrying out with 20～30W power
Vibration, 35～45 DEG C of sonic oscillations 3～4 days, then heats to 90～100 DEG C, vibrates 10～20min, stand 10～
20min, discards upper strata impurity, obtains lower sediment, standby；
(2) weigh 8～10g1-octenes and join in autoclave, sequentially add 100～200mL dehydrated alcohol, 2～4g
MAO, 3～5g ethylidene bichloride zirconocene, controlling pressure is 2～5MPa, and temperature is 60～80 DEG C, insulated and stirred 20
～30min, then in reactor, it is passed through 2～4L ethylene, stirring reaction 12～14h with the speed of 1～3L/min, obtain octene second
Alkene copolymer；
(3) adding 10～20g vinylacetates in above-mentioned octene ethylene copolymer, control temperature, at 90～100 DEG C, stirs 5
～10min, add 3～5g Ammonium persulfate .s, stirring reaction 3～4h, be cooled to room temperature, pressure release, reactant is discharged to beaker
In, in beaker, add 200～300mL deionized waters, stand, discard upper strata aqueous phase, organic facies is carried out decompression distillation, obtains
Octene-ethylene-vinylacetate blocked copolymer；
(4) joining in blender by above-mentioned blocked copolymer, arranging rotating speed is 6000～8000r/min, controls temperature and exists
50～60 DEG C, sequentially add 3～5g paraffin, 5～8g glycerol, 1～3g monoalkoxytitanates, high-speed stirred 30～40min,
Add lower sediment standby in above-mentioned steps (1), high-speed stirred reaction 5～6h, by greenhouse cooling to room temperature, material is entered
Row packaging, obtains rubber tyre carcass resisting fatigue auxiliary agent.
The application process of the present invention is: count by weight, adds the rubber tyre carcass that 3～4 parts of present invention prepare and resists
Tired auxiliary agent, 1～2 part of dodecylbenzene sodium sulfonate, 2～4 parts of p-phenylenediamine, 8～10 parts of butadiene-styrene rubber are in elastomer casting machine
In, it is heated to 120～130 DEG C, deaeration 15～30min, it is evacuated to 0.2～0.3MPa, depanning after keeping 30～60min, will
Having poured into a mould the tire of tyre surface and be placed in 70～80 DEG C of baking ovens process 12～24h, get product tire, hot strength reach 22～
24MPa, tearing strength reaches 108～120kN m-1, Life of Tyre extends 7～9 years.
The invention has the beneficial effects as follows:
(1) rubber resisting fatigue auxiliary agent of the present invention can improve the dynamic fatigue resistance energy of carcass, and hot strength is obviously enhanced
Reaching 22～24MPa, tearing strength reaches 108～120kN m-1, the distance travelled of tire significantly improves；
(2) antifatigue that the present invention prepares makes extend 7～9 years the service life of rubber tyre carcass.
Detailed description of the invention
First 10～20g molybdenum bisuphide, 10～20g precipitated silica, 5～8g silicon carbide whisker, 6～8g glass are weighed
Fiber joins in pulverizer and pulverizes, and crosses 80～100 mesh sieves, obtains mixed-powder, joined by mixed-powder in beaker,
Adding 200～300mL mass concentrations in beaker is 28～30% hydrogen peroxide, and stirring reaction 12～14h is filtered, obtained filtering residue,
Filtering residue is joined in conical flask, add 200～300mL methane liquids, be placed in supersonic oscillations instrument with 20～30W power
Vibrate, 35～45 DEG C of sonic oscillations 3～4 days, then heat to 90～100 DEG C, vibrate 10～20min, stand 10～
20min, discards upper strata impurity, obtains lower sediment, standby；Weigh 8～10g1-octenes to join in autoclave, then depend on
Secondary addition 100～200mL dehydrated alcohol, 2～4g MAO, 3～5g ethylidene bichloride zirconocene, control pressure be 2～
5MPa, temperature is 60～80 DEG C, insulated and stirred 20～30min, then is passed through 2～4L in reactor with the speed of 1～3L/min
Ethylene, stirring reaction 12～14h, obtain octene ethylene copolymer；10～20g acetic acid are added in above-mentioned octene ethylene copolymer
Vinyl acetate, control temperature, at 90～100 DEG C, stirs 5～10min, adds 3～5g Ammonium persulfate .s, stirring reaction 3～4h, fall
Warm to room temperature, pressure release, reactant is discharged in beaker, in beaker, add 200～300mL deionized waters, stand, discard
Layer aqueous phase, carries out organic facies decompression distillation, obtains octene-ethylene-vinylacetate blocked copolymer；By above-mentioned blocked
Copolymer joins in blender, and arranging rotating speed is 6000～8000r/min, and control temperature, at 50～60 DEG C, sequentially adds 3
～5g paraffin, 5～8g glycerol, 1～3g monoalkoxytitanates, high-speed stirred 30～40min, add above-mentioned standby lower floor
Precipitation, high-speed stirred reaction 5～6h, by greenhouse cooling to room temperature, material is packed, obtain rubber tyre carcass resisting fatigue
Auxiliary agent.
Example 1
First weigh 10g molybdenum bisuphide, 10g precipitated silica, 5g silicon carbide whisker, 6g glass fibre join in pulverizer
Pulverize, cross 80 mesh sieves, obtain mixed-powder, mixed-powder is joined in beaker, in beaker, add 200mL mass dense
Degree is 28% hydrogen peroxide, stirring reaction 12h, filters, obtains filtering residue, joined by filtering residue in conical flask, add 200mL biogas
Liquid, is placed in supersonic oscillations instrument vibrating with 20W power, 35 DEG C of sonic oscillations 3 days, then heats to 90 DEG C, shakes
Swing 10min, stand 10min, discard upper strata impurity, obtain lower sediment, standby；Weigh 8g1-octene and join autoclave
In, sequentially adding 100mL dehydrated alcohol, 2g MAO, 3g ethylidene bichloride zirconocene, control pressure is 2MPa, temperature
Degree is 60 DEG C, insulated and stirred 20min, then is passed through 2L ethylene, stirring reaction 12h in reactor with the speed of 1L/min, obtains
Octene ethylene copolymer；Adding 10g vinylacetate in above-mentioned octene ethylene copolymer, control temperature, at 90 DEG C, stirs
5min, adds 3g Ammonium persulfate., stirring reaction 3h, is cooled to room temperature, pressure release, is discharged in beaker by reactant, to beaker
Middle addition 200mL deionized water, stands, discards upper strata aqueous phase, organic facies carries out decompression distillation, obtains octene-ethylene-acetic acid
Vinyl acetate blocked copolymer；Above-mentioned blocked copolymer is joined in 6000r/min blender, control temperature at 50 DEG C,
Sequentially add 3g paraffin, 5g glycerol, 1g monoalkoxytitanates, high-speed stirred 30min, add above-mentioned standby lower floor and sink
Form sediment, high-speed stirred reaction 5h, by greenhouse cooling to room temperature, packs material, obtains rubber tyre carcass resisting fatigue auxiliary agent.
The application process of the present invention is: count by weight, and the rubber tyre carcass resisting fatigue that the addition present invention prepares helps
Agent 3 parts, 1 part of dodecylbenzene sodium sulfonate, 2 parts of p-phenylenediamine, 8 parts of butadiene-styrene rubber, in elastomer casting machine, are heated to 120
DEG C, deaeration 15min, it is evacuated to 0.2MPa, keeps depanning after 30min, the tire of the tyre surface poured into a mould is placed in 70 DEG C of baking ovens
Middle process 12h, get product tire, and hot strength reaches 22MPa, and tearing strength reaches 108kN m-1, Life of Tyre extends 7
Year.
Example 2
First weigh 15g molybdenum bisuphide, 15g precipitated silica, 7g silicon carbide whisker, 7g glass fibre join in pulverizer
Pulverize, cross 90 mesh sieves, obtain mixed-powder, mixed-powder is joined in beaker, in beaker, add 250mL mass dense
Degree is 29% hydrogen peroxide, stirring reaction 13h, filters, obtains filtering residue, joined by filtering residue in conical flask, add 250mL biogas
Liquid, is placed in supersonic oscillations instrument vibrating with 25W power, 40 DEG C of sonic oscillations 3.5 days, then heats to 95 DEG C,
Vibration 15min, stands 15min, discards upper strata impurity, obtain lower sediment, standby；Weigh 9g1-octene and join reaction under high pressure
In still, sequentially adding 150mL dehydrated alcohol, 3g MAO, 4g ethylidene bichloride zirconocene, control pressure is 3MPa,
Temperature is 70 DEG C, insulated and stirred 25min, then is passed through 3L ethylene, stirring reaction 13h in reactor with the speed of 2L/min, obtains
To octene ethylene copolymer；Adding 15g vinylacetate in above-mentioned octene ethylene copolymer, control temperature, at 95 DEG C, stirs
7min, adds 4g Ammonium persulfate., stirring reaction 3.5h, is cooled to room temperature, pressure release, is discharged in beaker by reactant, to burning
Add 250mL deionized water in Bei, stand, discard upper strata aqueous phase, organic facies is carried out decompression distillation, obtains octene-ethylene-vinegar
Vinyl acetate blocked copolymer；Above-mentioned blocked copolymer is joined in 7000r/min blender, controls temperature 55
DEG C, sequentially add 4g paraffin, 7g glycerol, 2g monoalkoxytitanates, high-speed stirred 35min, add above-mentioned standby under
Layer precipitation, high-speed stirred reaction 5.5h, by greenhouse cooling to room temperature, packs material, obtains rubber tyre carcass and resist tired
Labor auxiliary agent.
The application process of the present invention is: count by weight, and the rubber tyre carcass resisting fatigue that the addition present invention prepares helps
Agent 3.5 parts, 2 parts of dodecylbenzene sodium sulfonate, 3 parts of p-phenylenediamine, 9 parts of butadiene-styrene rubber, in elastomer casting machine, are heated to 125
DEG C, deaeration 25min, it is evacuated to 0.25MPa, keeps depanning after 50min, the tire of the tyre surface poured into a mould is placed in 75 DEG C of baking ovens
Middle process 18h, get product tire, and hot strength reaches 23MPa, and tearing strength reaches 109kN m-1, Life of Tyre extends 8
Year.
Example 3
First weigh 20g molybdenum bisuphide, 20g precipitated silica, 8g silicon carbide whisker, 8g glass fibre join in pulverizer
Pulverize, cross 100 mesh sieves, obtain mixed-powder, mixed-powder is joined in beaker, in beaker, add 300mL mass
Concentration is 28～30% hydrogen peroxide, stirring reaction 14h, filters, obtains filtering residue, joined by filtering residue in conical flask, add
300mL methane liquid, is placed in supersonic oscillations instrument vibrating with 30W power, 45 DEG C of sonic oscillations 4 days, then heats up
To 100 DEG C, vibrate 20min, stands 20min, discards upper strata impurity, obtain lower sediment, standby；Weigh 10g1-octene to add
In autoclave, sequentially add 200mL dehydrated alcohol, 4g MAO, 5g ethylidene bichloride zirconocene, control pressure
Power is 5MPa, and temperature is 80 DEG C, insulated and stirred 30min, then is passed through 4L ethylene in reactor with the speed of 3L/min, and stirring is anti-
Answer 14h, obtain octene ethylene copolymer；In above-mentioned octene ethylene copolymer, add 20g vinylacetate, control temperature and exist
100 DEG C, stir 10min, add 5g Ammonium persulfate., stirring reaction 4h, be cooled to room temperature, pressure release, be discharged to reactant burn
In Bei, in beaker, add 300mL deionized water, stand, discard upper strata aqueous phase, organic facies is carried out decompression distillation, obtains pungent
Alkene-ethylene-vinyl acetate blocked copolymer；Above-mentioned blocked copolymer is joined in 8000r/min blender, controls
Temperature, at 60 DEG C, sequentially adds 5g paraffin, 8g glycerol, 3g monoalkoxytitanates, high-speed stirred 40min, adds above-mentioned
Standby lower sediment, high-speed stirred reaction 6h, by greenhouse cooling to room temperature, packs material, obtains rubber tyre tire
Body resisting fatigue auxiliary agent.
The application process of the present invention is: count by weight, and the rubber tyre carcass resisting fatigue that the addition present invention prepares helps
Agent 4 parts, 2 parts of dodecylbenzene sodium sulfonate, 4 parts of p-phenylenediamine, 10 parts of butadiene-styrene rubber, in elastomer casting machine, are heated to 130
DEG C, deaeration 30min, it is evacuated to 0.3MPa, keeps depanning after 60min, the tire of the tyre surface poured into a mould is placed in 80 DEG C of baking ovens
Middle process 24h, get product tire, and hot strength reaches 24MPa, and tearing strength reaches 120kN m-1, Life of Tyre extends 9
Year.
Claims (1)
1. the preparation method of a rubber tyre carcass resisting fatigue auxiliary agent, it is characterised in that concrete preparation process is:
(1) 10～20g molybdenum bisuphide, 10～20g precipitated silica, 5～8g silicon carbide whisker, 6～8g glass fibre are weighed
Join in pulverizer and pulverize, cross 80～100 mesh sieves, obtain mixed-powder, mixed-powder is joined in beaker, to burning
Adding 200～300mL mass concentrations in Bei is 28～30% hydrogen peroxide, and stirring reaction 12～14h is filtered, obtained filtering residue, will filter
Slag joins in conical flask, adds 200～300mL methane liquids, is placed in supersonic oscillations instrument carrying out with 20～30W power
Vibration, 35～45 DEG C of sonic oscillations 3～4 days, then heats to 90～100 DEG C, vibrates 10～20min, stand 10～
20min, collects lower sediment, standby；
(2) weigh 8～10g1-octenes and join in autoclave, sequentially add 100～200mL dehydrated alcohol, 2～4g
MAO, 3～5g ethylidene bichloride zirconocene, controlling pressure is 2～5MPa, and temperature is 60～80 DEG C, insulated and stirred 20
～30min, then in reactor, it is passed through 2～4L ethylene, stirring reaction 12～14h with the speed of 1～3L/min, obtain octene second
Alkene copolymer；
(3) adding 10～20g vinylacetates in above-mentioned octene ethylene copolymer, control temperature, at 90～100 DEG C, stirs 5
～10min, add 3～5g Ammonium persulfate .s, stirring reaction 3～4h, be cooled to room temperature, pressure release, reactant is discharged to beaker
In, in beaker, add 200～300mL deionized waters, stand, discard upper strata aqueous phase, organic facies is carried out decompression distillation, obtains
Octene-ethylene-vinylacetate blocked copolymer；
(4) joining in blender by above-mentioned blocked copolymer, arranging rotating speed is 6000～8000r/min, controls temperature and exists
50～60 DEG C, sequentially add 3～5g paraffin, 5～8g glycerol, 1～3g monoalkoxytitanates, high-speed stirred 30～40min,
Add lower sediment standby in above-mentioned steps (1), high-speed stirred reaction 5～6h, by greenhouse cooling to room temperature, material is entered
Row packaging, obtains rubber tyre carcass resisting fatigue auxiliary agent.
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