CN106674631A - Preparation method of olefin rubber/filler blend vulcanized rubber - Google Patents
Preparation method of olefin rubber/filler blend vulcanized rubber Download PDFInfo
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- CN106674631A CN106674631A CN201611174657.5A CN201611174657A CN106674631A CN 106674631 A CN106674631 A CN 106674631A CN 201611174657 A CN201611174657 A CN 201611174657A CN 106674631 A CN106674631 A CN 106674631A
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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
- C08L7/00—Compositions of natural rubber
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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
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/82—Heating or cooling
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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
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/88—Adding charges, i.e. additives
- B29B7/94—Liquid charges
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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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 a preparation method of olefin rubber/filler blend vulcanized rubber. The method comprises the following steps: preparing a filler predispersion solution; plasticizing unvulcanized natural rubber by a rubber Banbury mixer, mixing with styrene-butadiene rubber and cis-1,4-polybutadiene rubber, increasing the temperature of the Banbury mixer to 110-160 DEG C, adding the filler predispersion solution into the rubber Banbury mixer, compounding, evaporating to remove water, and drying with hot air to obtain an olefin rubber/filler mixture; adding zinc oxide, stearic acid, a vulcanizing agent, an accelerator and an anti-aging agent into a rubber open mill or Banbury mixer, compounding uniformly, discharging, and standing to obtain the olefin rubber/filler compounded rubber; and vulcanizing the olefin rubber/filler compounded rubber on a flat vulcanizing machine to obtain the olefin rubber/filler blend vulcanized rubber. The method has the advantages of simple technique, no solvent pollution and no flying dust, is green and environment-friendly, and can be widely used for mixing multiple fillers and rubber.
Description
Technical field
The present invention relates to olefin rubber, the preparation side of more particularly to a kind of olefin rubber/filler blended vulcanizate
Method, belongs to rubber composite processing and technical field of modification.
Background technology
Traditional rubber internal mixing method is that, using mechanical blending method, the method presence major problem is that the charcoal in mixing process
The fillers such as black, white carbon are flown upward than more serious, easily pollute environment and equipment.Additionally, mass filler in rubber matrix point
Dissipate and be not in good state, cause the mechanical property variation or mechanical property of Blend rubber unstable.In mixing process, the filling of filler
Amount is excessive, causes mixing process heat serious, easily causes gel phenomenon.
Latex coprecipitation method is to mix the pre-dispersed liquid of filler and rubber latex, by adding flocculant by rubber latex and
Filler mixture is flocculated, and is washed out, is dried, and obtains gum filler blend.Although this method can improve filler
Dispersion in rubber, but the step of preparing rubber/filler blends is more, and time-consuming, dry run high energy consumption；Additionally, rubber
The glue latex resting period is short, easily produces rotten and precipitates, and solid rubber is then less there is the resting period and short and rotten etc. ask
Topic.But the method is suitable only for rubber latex, and for some rubber clones, such as fluorubber, does not have fluorubber glue substantially
Breast, then latex coprecipitation method can not be suitable for.It is inefficient and the moisture solution time in latex coprecipitation method later stage is longer.
Prior art latex coprecipitation method is to mix the pre-dispersed liquid of filler and rubber latex, by adding flocculant by rubber
Glue latex and filler mixture are flocculated, and are washed out, are dried, and obtain gum filler blend.Although this method can be with
Improve dispersion of the filler in rubber, but the step of preparing rubber/filler blends is more, and time-consuming, dry run high energy consumption；
Additionally, the rubber latex resting period is short, easily produces rotten and precipitate, and solid rubber is then less, and to there is the resting period short and become
The problems such as matter.
The content of the invention
Present invention aim at solving the deficiencies in the prior art, there is provided a kind of course of processing environmental protection, solid both it had been adapted to
Niggerhead mixes with filler, and dispersion of the filler in rubber matrix is conducive to again, can improve olefin rubber/filler blending sulfur
Change the high temperature moisture evaporation banburying method of glue combination property.
To realize the object of the invention, adopt the following technical scheme that：
The preparation method of a kind of olefin rubber/filler blended vulcanizate, it is characterised in that comprise the following steps：
(1) preparation of filler pre-dispersed liquid
Filler white carbon black and surfactant are added in deionized water, at normal temperatures mechanical agitation, then ultrasonic disperse, obtains
To filler pre-dispersed liquid；Described surfactant is dodecylbenzene sodium sulfonate, sodium lauryl sulphate, cetyl front three
Base ammonium bromide, OPEO, NPE, alkylpolyoxyethylene, polysorbate -60 and
One or more in Polyoxyethylene Sorbitan Monooleate；Described filler white carbon black and the mass ratio of deionized water is 1:5~1:30；With matter
Amount percentages, described surfactant accounts for the 2~10% of the step raw material gross mass；
(2) preparation of olefin rubber/filler mixture
Natural rubber rubber is plasticated using rubber internal mixer, is subsequently adding butadiene-styrene rubber and butadiene rubber, mixing 1
~5min, raises banbury temperature to 110~160 DEG C, and gained filler pre-dispersed liquid is added into rubber internal mixer from charge door
In, charging is finished, and closes charge door, continues to knead 5~15min, treats that moisture evaporation is finished, and is dried using hot-air, and alkene is obtained
Hydrocarbon rubbers/filler mixture；
(3) preparation of olefin rubber/filler blended vulcanizate
By percentage to the quality, 80~95% olefin rubbers/filler mixing is added on rubber internal mixer or mill
Thing, 1~5% Zinc Oxide, 0.8~3% stearic acid, 0.8~3% sulfur, 1~3% accelerator, 1~3% age resistor, mixing is equal
Even, slice parks 12~24h, and olefin rubber/compounded rubber is obtained；Olefin rubber/compounded rubber is in compression molding
Vulcanize on machine, obtain vulcanizate.
Further to realize the object of the invention, it is preferable that described olefin rubber is natural rubber, butadiene-styrene rubber, suitable
One or more in buna.
Preferably, described filler white carbon black be intermediate super abrasion furnace black, high wear-resistant carbon black, fast extrude in carbon black, Universal carbon black, half
One or more in hard carbon black, precipitated silica and gas-phase silica.
Preferably, by percentage to the quality, filler accounts for the 5 of step (1) raw material gross mass in described filler pre-dispersed liquid
~40%.
Preferably, it is described to adopt the temperature that rubber internal mixer is plasticated to natural rubber rubber for 40~80 DEG C, rotor
Rotating speed is 40~80rmin‐1, the time plasticated is 1~5min.
Preferably, described accelerator be dibenzothiazyl disulfide, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, two
One or more in sulfuration tetra methylthiuram, tetraethylthiuram disulfide, (DDC)2Zn；Described
Age resistor be 2,2,4- trimethyls -1,2- dihyaroquinoline polymers (RD), 2-mercaptobenzimidazole (MB), N, N'- dibutyl
One or more in aminodithioformic acid nickel (NBC), N- isopropyls-N'- diphenyl-para-phenylene diamines (4010NA).
Preferably, at normal temperatures the churned mechanically time is 30~180min to step (1), and rotating speed is 400~3000r
min‐1, then 30~180min of ultrasonic disperse under 120~1600w of power.
Preferably, when step (2) described filler water pre-dispersed liquid adds rubber internal mixer, the mixing of rubber internal mixer is controlled
Temperature is 110~160 DEG C, and rotor speed is 40~80rmin‐1, feed time is 5~15min.
Preferably, curing temperature of the olefin rubber/compounded rubber on vulcanizing press is 130~180 DEG C,
Sulfide stress is 8~15MPa, and cure time is 5~60min.
Preferably, the hot-air drying is to dry 1~2h at 100~150 DEG C.
It is pre-dispersed by the way that filler is carried out in water compared to mechanical blending method and latex coprecipitation method, filler can be improved
Dispersion situation in rubber, reinforcer and the interface interaction power of rubber, reduce the temperature of charge in banbury, prevent gel
Change, improve the physical and mechanical propertiess of blended vulcanizate.Further, it is also possible to mitigate filler fly upward, the building ring of neat and tidy is kept
Border.
It is emphasized that in prior art, being typically with dry method is carried out carbon black filler and rubber in banbury
Mixing, and filler should keep drying using before, and moisture evaporation may cause vulcanizate bubbling otherwise in sulfidation.
Therefore, water is typically considered what is should avoided as far as possible in mixing process.However, in existing dry method mixing process, having two big
Subject matter, one is that the carbon black filler of a large amount of additions disperses not enough uniformly, to be susceptible to reunite in rubber matrix, and then is caused
The mechanical properties decrease of vulcanizate；Two is that the filler such as white carbon black flies upward in mixing process, can cause environmental pollution and operator
Respiratory system damage.The present invention breaks through Traditional Thinking, and substantial amounts of water is added in carbon black filler, while being equipped with surfactant
So that filler is uniformly dispersed in water, white carbon black pre-dispersed liquid scattered in water camber is prepared, and then can be easily real
Existing filler is dispersed in final elastomeric compound.Because white carbon black is changed into liquid slurry by initial solid state powder, so
In white carbon black adition process, dust from flying, environmental protection can be completely eliminated.The active control of the present invention heating-up temperature of banbury
(be more than 100 DEG C), when filler water dispersion liquid adds banbury, moisture is set quickly to separate with elastomeric compound in vapour form,
And carbon black filler then continues to stay in elastomeric compound, extend mixing time of the elastomeric compound in banbury, effectively eliminate moisture, and
Further oven drying is carried out to elastomeric compound, the moisture in final elastomeric compound is minimized, so that moisture pair is completely eliminated
The impact of sulfuration bubbling.
Compared with prior art, the invention has the advantages that and beneficial effect：
1) the high temperature moisture evaporation banburying method that the present invention is adopted, preparation process is simple, does not use any solvent, without the need for carrying out
The washing of intermediate product, water consumption is few, does not produce dust from flying, and non-environmental-pollution, environmental protection, preparation process is few, when being dried
Between it is short, energy consumption is relatively low, it is adaptable to all kind solid block rubber and filler it is compound, can realize filler in rubber matrix
High efficiency dispersion, with very strong application and generalization, easily realizes industrialization.
2) present invention is a kind of high temperature moisture evaporation banburying method, substantially improves dispersion journey of the filler in olefin rubber
Degree, and enhance the effect of the interface cohesion between filler and rubber molecular chain.The present invention is overcoming prior art processing problems
While, the mechanical property such as tensile strength and tearing strength of the olefin rubber/filler blended vulcanizate of preparation is all substantially carried
It is high.
3) olefin rubber/filler blended vulcanizate prepared by the present invention has the drawing higher than traditional mechanical blending method
Stretch the mechanical properties such as intensity, stress at definite elongation, tearing strength, hardness, product excellent combination property.
Specific embodiment
With reference to embodiment, the new preparation side to olefin rubber according to the present invention/filler blended vulcanizate
Method is described further, but embodiment is not as limiting the scope of the invention.
In comparative example and embodiment, the various raw material models for being adopted and manufacturer are as follows respectively.
Natural rubber, 1#Standard rubber, Hainan caoutchouc industry Group Plc；Butadiene-styrene rubber, SBR1502,
Qilu Petrochemical limited company；Butadiene rubber, BR9000, Beijing Yanshan Petrochemical Co.；Intermediate super abrasion furnace black (N220),
High wear-resistant carbon black (N330), Jiangxi Black Cat Carbon Black Co., Ltd.；Fast extrude in carbon black (N550), Universal carbon black (N660), half
Hard carbon black (N774), Longxing Chemical Stock Co., Ltd.；Precipitated silica, TOKUSIL 255, the limited public affairs of south Ji chemical industry
Department；Gas-phase silica, HL-200,200 ± 20m of specific surface area2·g‐1, Guangzhou Science and Technology Ji Sheng Industrial Co；Zinc Oxide,
Stearic acid, accelerator dibenzothiazyl disulfide, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetramethylthiuram disulfide,
Tetraethylthiuram disulfide, (DDC)2Zn, age resistor 2,2,4- trimethyl -1,2- dihyaroquinolines gather
Fit (RD), 2-mercaptobenzimidazole (MB), N, N'- nickel dibutyl dithiocarbamates (NBC), N- isopropyl-N'- phenyl
P-phenylenediamine (4010NA), contains Science and Technology Ltd. and provides by Guangzhou Jinchang.
Comparative example 1
By percentage to the quality, the consumption of each raw material is as follows：
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 40 DEG C, and rotor speed is 40rmin‐1, plasticate
5min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set as into 110 DEG C, and rotor speed is
40r·min‐1, N220 white carbon blacks are added from the charge door of banbury, after white carbon black addition is finished, charge door is closed, continue to knead
5min, discharging, obtains rubber/N220 black stocks.
Rubber/N220 black stocks obtained by adding in rubber mixing mill, and add Zinc Oxide, Hard Fat according to composition of raw materials
Acid, sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N- isopropyl-N'- phenyl are to benzene two
Amine kneads 5min, beats triangle bag 5 times, and control melting temperature is less than 50 DEG C, discharges, and parks 12h.The conditions of vulcanization of elastomeric compound is
150 DEG C × 5min, sulfide stress is 8MPa, and the mechanical property of gained rubber/N220 carbon black vulcanizates is as shown in table 1.It is real
Apply example 1
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N220 white carbon blacks and deionized water is 1 in intermediate super abrasion furnace black (N220) addition deionized water:
5) sodium lauryl sulphate, mechanical agitation 180min, rotating speed 400rmin, are subsequently adding‐1, ultrasound wave dispersion 30min, power
1600w, obtains N220 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 40 DEG C, and rotor speed is 40rmin‐1, plasticate
5min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 110 DEG C, and rotor speed is
40r·min‐1, N220 white carbon black pre-dispersed liquids, plus the angle of incidence are added from the charge door of banbury for 5min, this process banbury
Top has a large amount of vapor to occur, and after the addition of N220 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 5min, directly
To banbury top without any visible vapor, discharging, gained rubber/N220 black stocks air oven is dried,
Condition is 100 DEG C × 1h.
Rubber/N220 black stocks obtained by adding in rubber mixing mill, and add Zinc Oxide, Hard Fat according to composition of raw materials
Acid, sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N- isopropyl-N'- phenyl are to benzene two
Amine kneads 5min, beats triangle bag 5 times, and control melting temperature is less than 50 DEG C, discharges, and parks 12h.The conditions of vulcanization of elastomeric compound is
150 DEG C × 5min, sulfide stress is 8MPa, and the mechanical property of gained rubber/N220 carbon black vulcanizates is as shown in table 1.It is real
Apply example 2
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N220 white carbon blacks and deionized water is 1 in intermediate super abrasion furnace black (N220) addition deionized water:
30) sodium lauryl sulphate, mechanical agitation 30min, rotating speed 3000rmin, are subsequently adding‐1, ultrasound wave dispersion 180min, work(
Rate 120w, obtains N220 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 40 DEG C, and rotor speed is 40rmin‐1, plasticate
5min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 110 DEG C, and rotor speed is
40r·min‐1, N220 white carbon black pre-dispersed liquids, plus the angle of incidence are added from the charge door of banbury for 10min, this process banbury
Top has a large amount of vapor to occur, and after the addition of N220 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 10min, directly
To banbury top without any visible vapor, discharging, gained rubber/N220 black stocks air oven is dried,
Condition is 150 DEG C × 1h.
Rubber mixing mill add rubber/N220 black stocks, according still further to composition of raw materials add Zinc Oxide, stearic acid,
Sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N- isopropyl-N'- diphenyl-para-phenylene diamines
Mixing 5min, beats triangle bag 5 times, and control melting temperature is less than 50 DEG C, discharges, and parks 12h.The conditions of vulcanization of elastomeric compound is 150
DEG C × 5min, sulfide stress is 8MPa, and the mechanical property of gained rubber/N220 carbon black vulcanizates is as shown in table 1.
Embodiment 3
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N220 white carbon blacks and deionized water is 1 in intermediate super abrasion furnace black (N220) addition deionized water:
30) surfactant OPEO, mechanical agitation 30min, rotating speed 3000rmin, are added‐1, ultrasound wave dispersion
180min, power 120w, obtain N220 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 40 DEG C, and rotor speed is 40rmin‐1, plasticate
5min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 110 DEG C, and rotor speed is
40r·min‐1, N220 white carbon black pre-dispersed liquids are added from charge door, plus the angle of incidence is 15min, this process banbury top has big
Amount vapor occurs, and after the addition of N220 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 10min, until banbury
Top is dried without any visible vapor, discharging, gained rubber/N220 black stocks air oven, and condition is 150
℃×1h。
Rubber/N220 black stocks obtained by adding in rubber mixing mill, according still further to composition of raw materials Zinc Oxide, Hard Fat are added
Acid, sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N- isopropyl-N'- phenyl are to benzene two
Amine kneads 5min, and control melting temperature is less than 100 DEG C, and 12h is parked in discharging.The conditions of vulcanization of elastomeric compound is 150 DEG C × 5min,
Sulfide stress is 8MPa, and the mechanical property of gained rubber/N220 carbon black vulcanizates is as shown in table 1.
Embodiment 4
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N220 white carbon blacks and deionized water is 1 in intermediate super abrasion furnace black (N220) addition deionized water:
30) dodecylbenzene sodium sulfonate, mechanical agitation 30min, rotating speed 3000rmin, are subsequently adding‐1, ultrasound wave dispersion 180min,
Power 120w, obtains N220 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 40 DEG C, and rotor speed is 40rmin‐1, plasticate
5min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 160 DEG C, and rotor speed is
80r·min‐1, N220 white carbon black pre-dispersed liquids, plus the angle of incidence are added from the charge door of banbury for 5min, this process banbury
Top has a large amount of vapor to occur, and after the addition of N220 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 5min, directly
To banbury top without any visible vapor, discharging, gained rubber/N220 black stocks air oven is dried,
Condition is 100 DEG C × 1h.
Rubber/N220 black stocks obtained by adding in rubber mixing mill, according still further to composition of raw materials Zinc Oxide, Hard Fat are added
Acid, sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N- isopropyl-N'- phenyl are to benzene two
Amine kneads 5min, beats triangle bag 5 times, and control melting temperature is less than 100 DEG C, discharges, and parks 12h.The conditions of vulcanization of elastomeric compound is
150 DEG C × 5min, sulfide stress is 8MPa, and the mechanical property of gained rubber/N220 carbon black vulcanizates is as shown in table 1.
Embodiment 5
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N220 white carbon blacks and deionized water is 1 in intermediate super abrasion furnace black (N220) addition deionized water:
30) dodecylbenzene sodium sulfonate, mechanical agitation 30min, rotating speed 3000rmin, are subsequently adding‐1, ultrasound wave dispersion 180min,
Power 120w, obtains N220 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 40 DEG C, and rotor speed is 40rmin‐1, plasticate
5min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 160 DEG C, and rotor speed is
80r·min‐1, N220 white carbon black pre-dispersed liquids, plus the angle of incidence are added from the charge door of banbury for 15min, this process banbury
Top has a large amount of vapor to occur, and after the addition of N220 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 5min, directly
To banbury top without any visible vapor, discharging, gained rubber/N220 black stocks air oven is dried,
Condition is 100 DEG C × 1h.
Rubber mixing mill add rubber/N220 black stocks, according still further to composition of raw materials add Zinc Oxide, stearic acid,
Sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N- isopropyl-N'- diphenyl-para-phenylene diamines
Mixing 5min, beats triangle bag 5 times, and control melting temperature is less than 100 DEG C, discharges, and parks 12h.The conditions of vulcanization of elastomeric compound is 150
DEG C × 5min, sulfide stress is 8MPa, and the mechanical property of gained rubber/N220 carbon black vulcanizates is as shown in table 1.Embodiment
6
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N220 white carbon blacks and deionized water is 1 in intermediate super abrasion furnace black (N220) addition deionized water:
30) dodecylbenzene sodium sulfonate, mechanical agitation 30min, rotating speed 3000rmin, are subsequently adding‐1, ultrasound wave dispersion 180min,
Power 1600w, obtains N220 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 40 DEG C, and rotor speed is 40rmin‐1, plasticate
5min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 160 DEG C, and rotor speed is
80r·min‐1, N220 white carbon black pre-dispersed liquids, plus the angle of incidence are added from the charge door of banbury for 15min, this process banbury
Top has a large amount of vapor to occur, and after the addition of N220 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 5min, directly
To banbury top without any visible vapor, discharging, gained rubber/N220 black stocks air oven is dried,
Condition is 100 DEG C × 1h.
Rubber mixing mill add rubber/N220 black stocks, according still further to composition of raw materials add Zinc Oxide, stearic acid,
Sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N- isopropyl-N'- diphenyl-para-phenylene diamines
Mixing 5min, beats triangle bag 5 times, and control melting temperature is less than 100 DEG C, discharges, and parks 12h.The conditions of vulcanization of elastomeric compound is 150
DEG C × 5min, sulfide stress is 8MPa, and the mechanical property of gained rubber/N220 carbon black vulcanizates is as shown in table 1.
Embodiment 7
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N220 white carbon blacks and deionized water is 1 in intermediate super abrasion furnace black (N220) addition deionized water:
30) dodecylbenzene sodium sulfonate, mechanical agitation 30min, rotating speed 3000rmin, are subsequently adding‐1, ultrasound wave dispersion 30min, work(
Rate 1600w, obtains N220 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 40 DEG C, and rotor speed is 40rmin‐1, plasticate
5min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 160 DEG C, and rotor speed is
80r·min‐1, N220 white carbon black pre-dispersed liquids, plus the angle of incidence are added from the charge door of banbury for 5min, this process banbury
Top has a large amount of vapor to occur, and after the addition of N220 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 5min, directly
To banbury top without any visible vapor, discharging, gained rubber/N220 black stocks air oven is dried,
Condition is 100 DEG C × 1h.
Rubber mixing mill add rubber/N220 black stocks, according still further to composition of raw materials add Zinc Oxide, stearic acid,
Sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N- isopropyl-N'- diphenyl-para-phenylene diamines
Mixing 5min, beats triangle bag 5 times, and control melting temperature is less than 100 DEG C, discharges, and parks 12h.The conditions of vulcanization of elastomeric compound is 150
DEG C × 5min, sulfide stress is 8MPa, and the mechanical property of gained rubber/N220 carbon black vulcanizates is as shown in table 1.
Embodiment 8
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N330 white carbon blacks and deionized water is 1 in high wear-resistant carbon black (N330) addition deionized water:30),
Add surfactant cetyl trimethylammonium bromide, mechanical agitation 30min, rotating speed 3000rmin‐1, ultrasound wave dispersion
180min, power 120w, obtain N330 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 50 DEG C, and rotor speed is 80rmin‐1, plasticate
1min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 160 DEG C, and rotor speed is
80r·min‐1, N330 white carbon black pre-dispersed liquids are added from charge door, plus the angle of incidence is 10min, this process banbury top has big
Amount vapor occurs, and after the addition of N330 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 5min, until banbury
Top is dried without any visible vapor, discharging, gained rubber/N330 black stocks air oven, and condition is 100
℃×2h。
Rubber mixing mill add rubber/N330 black stocks, according still further to composition of raw materials add Zinc Oxide, stearic acid,
Sulfur, dibenzothiazyl disulfide, tetramethylthiuram disulfide, 2,2,4- trimethyl -1,2- dihyaroquinolines polymer are mixed
Refining 5min, beats triangle bag 5 times, and control melting temperature is less than 80 DEG C, discharges, and parks 24h.The conditions of vulcanization of elastomeric compound is 180 DEG C
× 5min, sulfide stress is 8MPa, and the mechanical property of gained rubber/N330 carbon black vulcanizates is as shown in table 1.
Embodiment 9
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N550 white carbon blacks and deionized water is 1 in fast extrude in carbon black (N550) addition deionized water:30),
Add surfactant OPEO, mechanical agitation 30min, rotating speed 3000rmin‐1, ultrasound wave dispersion
180min, power 120w, obtain N550 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 50 DEG C, and rotor speed is 80rmin‐1, plasticate
1min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 160 DEG C, and rotor speed is 80r
min‐1, N550 white carbon black pre-dispersed liquids are added from charge door, feed time is 10min, and this process banbury top has a large amount of water to steam
Gas occurs, and after the addition of N550 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 5min, until banbury top does not have
Any visible vapor, discharging, gained rubber/N550 black stocks air oven is dried, and condition is 100 DEG C × 2h.
Rubber/N550 black stocks obtained by adding in rubber mixing mill, according still further to composition of raw materials Zinc Oxide, Hard Fat are added
Acid, sulfur, (DDC)2Zn, tetraethylthiuram disulfide, N- isopropyl-N'- diphenyl-para-phenylene diamines are mixed
Refining 5min, beats triangle bag 5 times, and control melting temperature is less than 80 DEG C, discharges, and parks 24h.The conditions of vulcanization of elastomeric compound is 130 DEG C
× 60min, sulfide stress is 15MPa, and the mechanical property of gained rubber/N550 carbon black vulcanizates is as shown in table 1.
Embodiment 10
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N660 white carbon blacks and deionized water is 1 in Universal carbon black (N660) addition deionized water:30), then
Add surfactant sodium dodecyl base polyoxyethylene ether, mechanical agitation 30min, rotating speed 3000rmin‐1, ultrasound wave dispersion
180min, power 120w, obtain N660 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 50 DEG C, and rotor speed is 80rmin‐1, plasticate
1min, adds butadiene-styrene rubber and butadiene rubber, mixes 1min, and the temperature of rubber internal mixer is set to into 160 DEG C, and rotor speed is
80r·min‐1, N660 white carbon black pre-dispersed liquids are added from charge door, plus the angle of incidence is 10min, this process banbury top has big
Amount vapor occurs, and after the addition of N660 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 5min, until banbury
Top is dried without any visible vapor, discharging, gained rubber/N660 black stocks air oven, and condition is 100
℃×2h。
Rubber mixing mill add rubber/N660 black stocks, according still further to composition of raw materials add Zinc Oxide, stearic acid,
Sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, 2-mercaptobenzimidazole mixing 5min, beat
Triangle bag 5 times, control melting temperature is less than 80 DEG C, and 24h is parked in discharging.The conditions of vulcanization of elastomeric compound be 150 DEG C × 5min, sulfur
Change pressure is 8MPa, and the mechanical property of gained rubber/N660 carbon black vulcanizates is as shown in table 1.
Embodiment 11
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of N774 white carbon blacks and deionized water is 1 in semi-reinforcing hydrocarbon black (N774) addition deionized water:30),
It is subsequently adding dodecylbenzene sodium sulfonate, mechanical agitation 30min, rotating speed 3000rmin‐1, ultrasound wave dispersion 180min, power
120w, obtains N774 white carbon black pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 40 DEG C, and rotor speed is 40rmin‐1, plasticate
5min, adds butadiene rubber and butadiene-styrene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 160 DEG C, and rotor speed is
80r·min‐1, N774 white carbon black pre-dispersed liquids, plus the angle of incidence are added from the charge door of banbury for 5min, this process banbury
Top has a large amount of vapor to occur, and after the addition of N774 white carbon blacks pre-dispersed liquid is finished, closes charge door, continues to knead 5min, directly
To banbury top without any visible vapor, discharging, gained rubber/N774 black stocks air oven is dried,
Condition is 100 DEG C × 1h.
Rubber mixing mill add rubber/N774 black stocks, according still further to composition of raw materials add Zinc Oxide, stearic acid,
Sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N- isopropyl-N'- diphenyl-para-phenylene diamines
Mixing 5min, beats triangle bag 5 times, and control melting temperature is less than 100 DEG C, discharges, and parks 12h.The conditions of vulcanization of elastomeric compound is 150
DEG C × 5min, sulfide stress is 8MPa, and the mechanical property of gained rubber/N774 carbon black vulcanizates is as shown in table 1.
Embodiment 12
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of T255 white carbon blacks and deionized water is 1 in precipitated silica (T255) addition deionized water:30),
Add surfactant Polysorbate -60, mechanical agitation 30min, rotating speed 3000rmin‐1, ultrasound wave dispersion 180min,
Power 120w, obtains T255 white carbon pre-dispersed liquids.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 50 DEG C, and rotor speed is 80rmin‐1, plasticate
1min, adds butadiene-styrene rubber and butadiene rubber, mixes 5min, and the temperature of rubber internal mixer is set to into 160 DEG C, and rotor speed is
80r·min‐1, T255 white carbon pre-dispersed liquids are added from charge door, plus the angle of incidence is 10min, this process banbury top has
A large amount of vapor occur, and after the addition of T255 white carbons pre-dispersed liquid is finished, close charge door, continue to knead 5min, Zhi Daomi
Mill top is dried without any visible vapor, discharging, gained rubber/T255 white carbons mixture air oven, bar
Part is 100 DEG C × 2h.
Rubber/T255 white carbon mixture obtained by adding in rubber mixing mill, according still further to composition of raw materials addition Zinc Oxide, firmly
Fat acid, sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N, N'- dibutyl dithio ammonia
Base nickel formate kneads 5min, beats triangle bag 5 times, and control melting temperature is less than 80 DEG C, discharges, and parks 12h.The sulfuration bar of elastomeric compound
Part is 180 DEG C × 5min, and sulfide stress is 8MPa, the mechanical property such as institute of table 1 of gained rubber/T255 white carbon blended vulcanizates
Show.
Embodiment 13
By percentage to the quality, the consumption of each raw material is as follows：
First by (mass ratio of gas-phase silica and deionized water is 1 in gas-phase silica addition deionized water:30), then add
Enter surfactant Polysorbate -80, mechanical agitation 30min, rotating speed 3000rmin‐1, ultrasound wave dispersion 180min, power
120w, obtains gas-phase silica pre-dispersed liquid.
Natural rubber rubber is plasticated using rubber internal mixer, temperature is 50 DEG C, and rotor speed is 80rmin‐1, plasticate
1min, adds butadiene-styrene rubber and butadiene rubber, mixes 2min, and the temperature of rubber internal mixer is set to into 160 DEG C, and rotor speed is
80r·min‐1, gas-phase silica pre-dispersed liquid is added from charge door, plus the angle of incidence is 10min, this process banbury top has
A large amount of vapor occur, and after the addition of gas-phase silica aqueous dispersions is finished, close charge door, continue to knead 5min, Zhi Daomi
Mill top is dried without any visible vapor, discharging, gained rubber/gas-phase silica mixture air oven, bar
Part is 100 DEG C × 2h.
Rubber/gas-phase silica mixture obtained by adding in rubber mixing mill, according still further to composition of raw materials addition Zinc Oxide, firmly
Fat acid, sulfur, N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetraethylthiuram disulfide, N- isopropyl-N'- phenyl are to benzene
Diamidogen kneads 5min, beats triangle bag 5 times, and control melting temperature is less than 80 DEG C, discharges, and parks 24h.The conditions of vulcanization of elastomeric compound is
150 DEG C × 5min, sulfide stress is 8MPa, and the mechanical property of gained rubber/gas-phase silica blended vulcanizate is as shown in table 1.
The mechanical property of the different embodiment correspondence olefin rubber/filler blended vulcanizates of table 1
As it can be seen from table 1 the mechanics of the gum filler mixture prepared using traditional mechanical blending method (comparative example 1)
Performance is relatively low.Mechanical blending method is compared, the present invention adopts the blended vulcanizate of high temperature moisture evaporation banburying method (embodiment 1-13)
Tensile strength and tearing strength have and improve to some extent.When the present invention is using high temperature moisture evaporation banburying method, by filler
Carry out effectively pre-dispersed very crucial, the proportioning (embodiment 2) of increase deionized water and filler, or Raised rubber mixing temperature
The feed time (embodiment 5) of (embodiment 4) or proper extension filler pre-dispersed liquid, change ultrasonic disperse condition (embodiment 6),
Or increase emulsifier (embodiment 7), filler can be better dispersed in rubber matrix, so as to improve blended vulcanizate
Mechanical property.The present invention adopts the various different fillers and rubber mixed (example 8-13) of the preparation of high temperature moisture evaporation
With good mechanical property.
The present invention is simultaneously real during rubber processing due to being mixed in banbury with rubber using filler pre-dispersed liquid
Filler dispersion and the step such as moisture drying are showed, simultaneously because the cooling effect of moisture evaporation, also in effective control banbury
Portion is rapidly heated, so as to reduce rubber internal mixing during gel content, it is ensured that blended vulcanizate has preferable power
Learn performance.
Embodiments of the present invention are not limited by above-described embodiment, and in the range of the technology design of the present invention, others are appointed
What without departing from the present invention spirit and the change, modification, replacement made under principle, combine, simplification, should be equivalent and put
Mode is changed, protection scope of the present invention is belonged to.
Claims (10)
1. the preparation method of a kind of olefin rubber/filler blended vulcanizate, it is characterised in that comprise the following steps：
(1) preparation of filler pre-dispersed liquid
Filler white carbon black and surfactant are added in deionized water, at normal temperatures mechanical agitation, then ultrasonic disperse, is filled out
Material pre-dispersed liquid；Described surfactant is dodecylbenzene sodium sulfonate, sodium lauryl sulphate, cetyl trimethyl bromine
Change ammonium, OPEO, NPE, alkylpolyoxyethylene, polysorbate -60 and poly- mountain
One or more in pears alcohol ester -80；Described filler white carbon black and the mass ratio of deionized water is 1:5~1:30；With quality hundred
Divide than meter, described surfactant accounts for the 2~10% of the step raw material gross mass；
(2) preparation of olefin rubber/filler mixture
Natural rubber rubber is plasticated using rubber internal mixer, is subsequently adding butadiene-styrene rubber and butadiene rubber, mixing 1~
5min, raises banbury temperature to 110~160 DEG C, and gained filler pre-dispersed liquid is added in rubber internal mixer from charge door,
Charging is finished, and closes charge door, continues to knead 5~15min, treats that moisture evaporation is finished, and is dried using hot-air, and olefines is obtained
Rubber/filler mixture；
(3) preparation of olefin rubber/filler blended vulcanizate
By percentage to the quality, on rubber internal mixer or mill add 80~95% olefin rubbers/filler mixture, 1
~5% Zinc Oxide, 0.8~3% stearic acid, 0.8~3% sulfur, 1~3% accelerator, 1~3% age resistor, mixing is uniform, goes out
Piece, parks 12~24h, and olefin rubber/compounded rubber is obtained；Olefin rubber/compounded rubber is on vulcanizing press
Sulfuration, obtains vulcanizate.
2. preparation method according to claim 1, it is characterised in that：Described olefin rubber is natural rubber, butylbenzene
One or more in rubber, butadiene rubber.
3. preparation method according to claim 1, it is characterised in that：Described filler white carbon black is intermediate super abrasion furnace black, height
One or more in abrasion resistant carbon black, fast extrude in carbon black, Universal carbon black, semi-reinforcing hydrocarbon black, precipitated silica and gas-phase silica.
4. preparation method according to claim 1, it is characterised in that：By percentage to the quality, described filler is pre-dispersed
Filler accounts for the 5~40% of step (1) raw material gross mass in liquid.
5. preparation method according to claim 1, it is characterised in that：The employing rubber internal mixer is to natural rubber rubber
The temperature plasticated is 40~80 DEG C, and rotor speed is 40~80rmin‐1, the time plasticated is 1~5min.
6. preparation method according to claim 1, it is characterised in that：Described accelerator be dibenzothiazyl disulfide,
N- cyclohexyls -2-[4-morpholinodithio sulfenamide, tetramethylthiuram disulfide, tetraethylthiuram disulfide, the sulfur of diethyl two
For one or more in carbaminate；Described age resistor is 2,2,4- trimethyl -1,2- dihyaroquinoline polymers, 2- mercaptos
Base benzimidazole, N, one or more in N'- nickel dibutyl dithiocarbamates, N- isopropyl-N'- diphenyl-para-phenylene diamines.
7. preparation method according to claim 1, it is characterised in that：At normal temperatures the churned mechanically time is step (1)
30~180min, rotating speed is 400~3000rmin‐1, then 30~180min of ultrasonic disperse under 120~1600w of power.
8. preparation method according to claim 1, it is characterised in that：Step (2) described filler water pre-dispersed liquid adds rubber
During glue banbury, the melting temperature for controlling rubber internal mixer is 110~160 DEG C, and rotor speed is 40~80rmin‐1, charging
Time is 5~15min.
9. preparation method according to claim 1, it is characterised in that：Olefin rubber/the compounded rubber is in flat board
Curing temperature on vulcanizer is 130~180 DEG C, and sulfide stress is 8~15MPa, and cure time is 5~60min.
10. preparation method according to claim 1, it is characterised in that：The hot-air drying is to dry 1 at 100~150 DEG C
~2h.
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| CN110591174A (en) * | 2019-09-29 | 2019-12-20 | 华南理工大学 | High-mechanical-property, high-conductivity and light-weight rubber composition and preparation method thereof |
| CN110591175A (en) * | 2019-09-29 | 2019-12-20 | 华南理工大学 | Non-filled rubber composition with high mechanical property and low hysteresis loss and preparation method thereof |
| WO2020247663A1 (en) * | 2019-06-05 | 2020-12-10 | Beyond Lotus Llc | Methods of preparing a composite having elastomer and filler |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108276619A (en) * | 2017-12-18 | 2018-07-13 | 黄燕 | High intensity vulcanized rubber preparation method |
| WO2020247663A1 (en) * | 2019-06-05 | 2020-12-10 | Beyond Lotus Llc | Methods of preparing a composite having elastomer and filler |
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| CN110591174A (en) * | 2019-09-29 | 2019-12-20 | 华南理工大学 | High-mechanical-property, high-conductivity and light-weight rubber composition and preparation method thereof |
| CN110591175A (en) * | 2019-09-29 | 2019-12-20 | 华南理工大学 | Non-filled rubber composition with high mechanical property and low hysteresis loss and preparation method thereof |
| CN110591175B (en) * | 2019-09-29 | 2021-11-02 | 华南理工大学 | Non-filled rubber composition with high mechanical property and low hysteresis loss and preparation method thereof |
| CN110591174B (en) * | 2019-09-29 | 2021-11-02 | 华南理工大学 | High-mechanical-property, high-conductivity and light-weight rubber composition and preparation method thereof |
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