CN107501656B - A kind of preparation method of the wear-resisting nitrile rubber of conduction - Google Patents
A kind of preparation method of the wear-resisting nitrile rubber of conduction Download PDFInfo
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- CN107501656B CN107501656B CN201710961369.2A CN201710961369A CN107501656B CN 107501656 B CN107501656 B CN 107501656B CN 201710961369 A CN201710961369 A CN 201710961369A CN 107501656 B CN107501656 B CN 107501656B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
Abstract
The present invention relates to field of rubber technology, and in particular to a kind of preparation method of the wear-resisting nitrile rubber of conduction.Graphite microwave treatment is obtained into expanded graphite in the present invention, and it is ultrasonically treated, expanded graphite, which is shaken, is dispersed into nano-graphite lamella, nano-graphite lamella is copolymerized with acrylonitrile and butadiene, under emulsion blending, autovulcanization occurs for nano-graphite lamella active site and rubber molecule, forms conductive network, to achieve the effect that improve poorly conductive.Due to the polar interaction between group, the mobility of nitrile rubber segment is greatly reduced.Modified alta-mud is added during plasticating, biggish hysteresis loss can be generated in friction, the sizing material of friction surface forms abrasive grain after being destroyed, these abrasive grains can be improved sizing material to the adhesion strength in the face of rubbing, to achieve the purpose that improve wear resistance.
Description
Technical field
The present invention relates to technical field of rubber preparation, and in particular to a kind of preparation side of the wear-resisting nitrile rubber of conduction
Method.
Background technique
Raw rubber is the material of main part of rubber product manufacture.Rubber is a kind of flexible polymer, according to mode is made
Difference, rubber can be divided into two class of synthetic rubber and natural rubber.Natural rubber is mainly derived from para ruber, when this rubber
When the epidermis of gum is cut open, milky juice, referred to as latex will flow out, latex is through cohesion, washing, molding, drying
Obtain natural rubber.Synthetic rubber is can to synthesize variety classes using different raw materials as prepared by artificial synthesis
Rubber, such as butadiene rubber, neoprene, butadiene-styrene rubber, nitrile rubber.
Nitrile rubber is as butadiene and acrylonitrile through containing unsaturated double-bond in strand made from emulsion polymerization
With polar group-CN, thus has outstanding lubricating oil resistance energy.In addition rubber itself has cross-linked structure and
The high resiliency of acquisition, thus there is fabulous oil resistance and excellent physical mechanical property, it is widely used in industrial production
In.It is mainly used for making oil-resistant article, such as oil-resistant pipe, adhesive tape, diaphragm of rubber and large-scale oil sac, is usually used in making all kinds of oil resistants
Molded article, such as O-ring, oil sealing, leather cup, diaphragm, valve, bellows are also used for production offset plate and wear part.But fourth
The intensity of nitrile rubber material is not high, weather resistance is bad, be prone to wear, electrical property is inferior, elasticity is slightly lower etc..In actual production often
These disadvantages are made up with modified method.
Therefore it provides the nitrile rubber of a kind of high conductivity, excelling in abrasion resistance is current urgent problem to be solved.
Summary of the invention
Present invention mainly solves the technical issues of, for rubber poorly conductive, the defect being prone to wear, provide one kind and lead
The preparation method of the wear-resisting nitrile rubber of electricity.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of the wear-resisting nitrile rubber of conduction, it is characterised in that specific preparation step are as follows:
(1) it weighs 20~30g expansible graphite to be placed in a vacuum drying oven, 100~120g is put into vacuum oven
Phosphorus pentoxide, it is dry, the expansible graphite after drying is put into beaker, then beaker is placed under microwave and is handled, takes out and burn
Cup is cooled to room temperature, and is expanded expansible graphite, is obtained expanded graphite;
(2) lauryl sodium sulfate of 20~25g is mixed with 200~220mL deionized water, stirs, obtains emulsion,
10~15g expanded graphite is immersed in emulsion, mixing suspension is obtained, mixing suspension is ultrasonically treated, ultrasound
The water slurry of nano-graphite lamella is obtained after processing;
(3) 100~110g acrylonitrile and 90~100g butadiene are added to the three-necked flask for having blender and thermometer
In, 100~120mL sodium hydroxide solution, 30~40g polyvinyl alcohol, 100~110mL nano-graphite are added into three-necked flask
The aqueous suspension body fluid of lamella starts blender, after stirring and emulsifying, 1~3g potassium peroxydisulfate, heat temperature raising is added, insulation reaction obtains
Enhance nitrile rubber to nanometer;
(4) 40~45g acrylic acid and maleic anhydride acid copolymer are added in the beaker equipped with 100~120mL acetone soln,
Heat temperature raising is added 60~70g bentonite to beaker, is cooled to room temperature and obtains bentonite suspension, bentonite suspension is set
In supercentrifuge, centrifugation removes upper liquid, obtains lamella bentonite, lamella bentonite is placed in baking oven, and heating rises
Temperature, it is dry, obtain modified alta-mud;
(5) nanometer enhancing nitrile rubber is placed in double roll mill and is plasticated, then nanometer is added into double roll mill and increases
Modified alta-mud, the 20~25g white carbon black of strong nitrile rubber quality 5~8%, mixing plasticate, discharge, and obtain conductive wear-resisting butyronitrile
Rubber material.
Vacuum oven temperature is set described in step (1) as 100~110 DEG C, drying time is 8~10h, microwave power
For 700~800W, microwave treatment time is 40~45s, and microwave treatment heating expansion number is 3~5 times.
Mixing time described in step (2) is 10~15min, sets ultrasonic frequency as 30~32KHz.
The mass fraction of sodium hydroxide solution described in step (3) is 5%, and speed of agitator is 80~90r/min, stirring cream
The change time is 10~15min, and temperature is 45~48 DEG C after heat temperature raising, and the insulation reaction time is 3~4h.
The mass fraction of acetone soln described in step (4) is 30~40%, and temperature is 80~85 DEG C after heat temperature raising, from
Scheming revolving speed is 3200~3400r/min, and centrifugation time is 15~17min, and temperature is 80~90 DEG C after heat temperature raising, when dry
Between be 3~4h.
Plasticate described in step (5) condition: preceding roll temperature is 55~60 DEG C, and rear roll temperature is 50~55 DEG C, roll spacing is 6~
8mm, number of plasticating are 1~3 time, and mixing number of plasticating is 2~3 times.
The beneficial effects of the present invention are:
(1) by expansible graphite microwave treatment in the present invention, heat expandable graphite obtains expanded graphite, then will expand stone
Ink is placed in surface activating solution and is ultrasonically treated, and expanded graphite, which is shaken, is dispersed into nano-graphite lamella, and nano-graphite lamella exists
During acrylonitrile and butadiene copolymer, since nano-graphite lamella is there may be some active reaction points, rubber can trigger
Cross-linking reaction, under emulsion blending, graphite flake layer has reached nano-dispersed in rubber matrix, while there are also certain intercalations
Structure exists, and potential active site has occurred with rubber molecule on nano-graphite lamella adequately contacts and bin cure thus has occurred
Change, cause nano-graphite lamella fully dispersed in rubber, and the insulation crystalline region of rubber can be destroyed, forms conductive network, from
And play the role of improving nitrile rubber electric conductivity;
(2) due to the base of polar functional group and rubber in the fine dispersion and graphite flake layer of nano-graphite in the present invention
Polar interaction between group causes interface cohesion strong between graphite and matrix, greatly reduces nitrile rubber segment
Mobility, rubber, which will not generate big deformation in friction, is worn surface, and modified alta-mud energy is added during plasticating
It being enough intercalation into rubber, biggish hysteresis loss can be generated in friction, the sizing material of friction surface forms abrasive grain after being destroyed,
These abrasive grains can be improved sizing material to the adhesion strength in the face of rubbing, to achieve the purpose that improve wear resistance, have wide answer
Use prospect.
Specific embodiment
It weighs 20~30g expansible graphite to be placed in a vacuum drying oven, sets vacuum oven temperature as 100~110 DEG C,
100~120g phosphorus pentoxide is put into vacuum oven, the expansible graphite after drying is put into beaker by dry 8~10h
In, then beaker is placed on 40~45s of Power Processing under microwave with 700~800W, it takes out beaker and is cooled to room temperature, make may expand
Graphite expands, and such microwave treatment heating expansion 3~5 times obtains expanded graphite;By the dodecyl sulphate of 20~25g
Sodium is mixed with 200~220mL deionized water, is stirred 10~15min, is obtained emulsion, 10~15g expanded graphite is immersed in cream
Change in liquid, obtain mixing suspension, mixing suspension is ultrasonically treated, set ultrasonic frequency as 30~32KHz, it is ultrasonic
The water slurry of nano-graphite lamella is obtained after processing;100~110g acrylonitrile and 90~100g butadiene are added to have and stirred
In the three-necked flask for mixing device and thermometer, it is molten that the sodium hydroxide that 100~120mL mass fraction is 5% is added into three-necked flask
Liquid, 30~40g polyvinyl alcohol, 100~110mL nano-graphite lamella aqueous suspension body fluid, start blender, with 80~90r/
After 10~15min of min revolving speed stirring and emulsifying, 1~3g potassium peroxydisulfate is added, is heated to 45~48 DEG C, insulation reaction 3~
4h obtains nanometer enhancing nitrile rubber;40~45g acrylic acid and maleic anhydride acid copolymer are added, 100~120mL mass is housed
Score is to be heated to 80~85 DEG C in the beaker of 30~40% acetone solns, and 60~70g bentonite, cooling is added to beaker
Bentonite suspension is obtained to room temperature, bentonite suspension is placed in supercentrifuge, with the revolving speed of 3200~3400r/min
It is centrifuged 15~17min, upper liquid is removed, obtains lamella bentonite, lamella bentonite is placed in baking oven, it is heated to 80~
90 DEG C, dry 3~4h obtains modified alta-mud;Nanometer enhancing nitrile rubber is placed in double roll mill, is in preceding roll temperature
55~60 DEG C, rear roll temperature is 50~55 DEG C, and roll spacing is plasticated 1~3 time under conditions of being 6~8mm, then is added into double roll mill
Enter modified alta-mud, the 20~25g white carbon black of nanometer enhancing nitrile rubber quality 5~8%, mixing is plasticated 2~3 times, is discharged, is obtained
To conductive wear-resisting nitrile rubber.
Example 1
It weighs 20g expansible graphite to be placed in a vacuum drying oven, sets vacuum oven temperature as 100 DEG C, done to vacuum
It is put into 100g phosphorus pentoxide in dry case, the expansible graphite after drying is put into beaker by dry 8h, then beaker is placed on micro-
With the Power Processing 40s of 700W under wave, takes out beaker and be cooled to room temperature, expand expansible graphite, such microwave treatment
Heating expansion 3 times, obtains expanded graphite;The lauryl sodium sulfate of 20g is mixed with 200mL deionized water, stirs 10min,
Emulsion is obtained, 10g expanded graphite is immersed in emulsion, mixing suspension is obtained, mixing suspension is carried out at ultrasound
Reason, sets ultrasonic frequency as 30KHz, the water slurry of nano-graphite lamella is obtained after ultrasonic treatment;By 100g acrylonitrile and
90g butadiene is added in the three-necked flask with blender and thermometer, and it is 5% that 100mL mass fraction is added into three-necked flask
Sodium hydroxide solution, 30g polyvinyl alcohol, 100mL nano-graphite lamella aqueous suspension body fluid, start blender, with 80r/min
After revolving speed stirring and emulsifying 10min, 1g potassium peroxydisulfate is added, is heated to 45 DEG C, insulation reaction 3h, obtains nanometer enhancing butyronitrile
Rubber;It is to add in the beaker of 30% acetone soln equipped with 100mL mass fraction that 40g acrylic acid and maleic anhydride acid copolymer, which are added,
Heat is warming up to 80 DEG C, and 60g bentonite is added to beaker, is cooled to room temperature and obtains bentonite suspension, bentonite suspension is set
In supercentrifuge, 15min is centrifuged with the revolving speed of 3200r/min, upper liquid is removed, obtains lamella bentonite, lamella is swollen
Profit soil is placed in baking oven, is heated to 80 DEG C, and dry 3h obtains modified alta-mud;Nanometer enhancing nitrile rubber is placed in double
It is 55 DEG C in preceding roll temperature in roller kneading machine, rear roll temperature is 50 DEG C, and roll spacing is plasticated 1 time under conditions of being 6mm, then to double roller
Modified alta-mud, the 20g white carbon black of nanometer enhancing nitrile rubber quality 5% are added in kneading machine, mixing is plasticated 2 times, is discharged, is obtained
To conductive wear-resisting nitrile rubber.
Example 2
It weighs 25g expansible graphite to be placed in a vacuum drying oven, sets vacuum oven temperature as 105 DEG C, done to vacuum
It is put into 110g phosphorus pentoxide in dry case, the expansible graphite after drying is put into beaker by dry 9h, then beaker is placed on micro-
With the Power Processing 42s of 750W under wave, takes out beaker and be cooled to room temperature, expand expansible graphite, such microwave treatment
Heating expansion 4 times, obtains expanded graphite;The lauryl sodium sulfate of 23g is mixed with 210mL deionized water, stirs 13min,
Emulsion is obtained, 13g expanded graphite is immersed in emulsion, mixing suspension is obtained, mixing suspension is carried out at ultrasound
Reason, sets ultrasonic frequency as 31KHz, the water slurry of nano-graphite lamella is obtained after ultrasonic treatment;By 105g acrylonitrile and
95g butadiene is added in the three-necked flask with blender and thermometer, and it is 5% that 110mL mass fraction is added into three-necked flask
Sodium hydroxide solution, 35g polyvinyl alcohol, 105mL nano-graphite lamella aqueous suspension body fluid, start blender, with 85r/min
After revolving speed stirring and emulsifying 12min, 2g potassium peroxydisulfate is added, is heated to 46 DEG C, insulation reaction 3.5h, obtains nanometer enhancing fourth
Nitrile rubber;42g acrylic acid and maleic anhydride acid copolymer are added and are equipped in the beaker that 110mL mass fraction is 35% acetone soln,
82 DEG C are heated to, 65g bentonite is added to beaker, is cooled to room temperature and obtains bentonite suspension, by bentonite suspension
It is placed in supercentrifuge, 16min is centrifuged with the revolving speed of 3300r/min, upper liquid is removed, lamella bentonite is obtained, by lamella
Bentonite is placed in baking oven, is heated to 85 DEG C, and dry 3.5h obtains modified alta-mud;Nanometer enhancing nitrile rubber is set
It is 57 DEG C in preceding roll temperature in double roll mill, rear roll temperature is 52 DEG C, and roll spacing is plasticated 2 times under conditions of being 7mm, then to
Modified alta-mud, the 23g white carbon black of nanometer enhancing nitrile rubber quality 6% are added in double roll mill, mixing is plasticated 2 times, out
Material obtains conductive wear-resisting nitrile rubber.
Example 3
It weighs 30g expansible graphite to be placed in a vacuum drying oven, sets vacuum oven temperature as 110 DEG C, done to vacuum
120g phosphorus pentoxide is put into dry case, the expansible graphite after drying is put into beaker, then beaker is placed on by dry 10h
With the Power Processing 45s of 800W under microwave, takes out beaker and be cooled to room temperature, expand expansible graphite, at such microwave
Reason heating expansion 5 times, obtain expanded graphite;The lauryl sodium sulfate of 25g is mixed with 220mL deionized water, is stirred
15min obtains emulsion, and 15g expanded graphite is immersed in emulsion, mixing suspension is obtained, and carries out to mixing suspension
Ultrasonic treatment, sets ultrasonic frequency as 32KHz, the water slurry of nano-graphite lamella is obtained after ultrasonic treatment;By 110g third
Alkene nitrile and 100g butadiene are added in the three-necked flask with blender and thermometer, and 120mL mass is added into three-necked flask
Score be 5% sodium hydroxide solution, 40g polyvinyl alcohol, 110mL nano-graphite lamella aqueous suspension body fluid, start blender,
After 90r/min revolving speed stirring and emulsifying 15min, 3g potassium peroxydisulfate is added, is heated to 48 DEG C, insulation reaction 4h is received
Meter Zeng Qiang nitrile rubber;It is 40% acetone soln that 45g acrylic acid and maleic anhydride acid copolymer, which are added equipped with 120mL mass fraction,
Beaker in, be heated to 85 DEG C, to beaker be added 70g bentonite, be cooled to room temperature and obtain bentonite suspension, by swelling
Native suspension is placed in supercentrifuge, is centrifuged 17min with the revolving speed of 3400r/min, is removed upper liquid, obtain lamella swelling
Lamella bentonite is placed in baking oven by soil, is heated to 90 DEG C, and dry 4h obtains modified alta-mud;Nanometer is enhanced into butyronitrile
Rubber is placed in double roll mill, is 60 DEG C in preceding roll temperature, and rear roll temperature is 55 DEG C, and roll spacing plasticates 3 under conditions of being 8mm
It is secondary, then modified alta-mud, the 25g white carbon black of nanometer enhancing nitrile rubber quality 8% is added into double roll mill, mixing plasticates 3
Secondary, discharging obtains conductive wear-resisting nitrile rubber.
The nitrile rubber material that comparative example is produced with company, Xuancheng City is as a comparison case to conduction produced by the present invention
Nitrile rubber material in wear-resisting nitrile rubber and comparative example is detected, and testing result is as shown in table 1: 1, test side
Method
Abrasion resistance is detected using Akron abrasion machine by the regulation of GB/T1689-2014.
Using example 1-3 produced by the present invention and comparative example product, the identical (15cm of 4 blocks product is taken on product respectively
× 15cm × 0.2cm) test block.Under the conditions of 25 DEG C, the constant temperature and humidity that relative humidity is 55%, applies 500V voltage, utilize superelevation
Resistance/Weak current tester measures resistivity.
Table 1
According to data in table 1 it is found that the wear-resisting nitrile rubber of conduction produced by the present invention, wear hardness are significantly larger than state
Family's standard, wear-resisting property is prominent and electric conductivity is excellent, which has very high popularization and application and wide prospect of the application.
Claims (6)
1. a kind of preparation method of the wear-resisting nitrile rubber of conduction, it is characterised in that specific preparation step are as follows:
(1) it weighs 20~30g expansible graphite to be placed in a vacuum drying oven, 100~120g, five oxygen is put into vacuum oven
Change two phosphorus, it is dry, the expansible graphite after drying is put into beaker, then beaker is placed under microwave and is handled, it is cold to take out beaker
But to room temperature, expansible graphite is expanded, obtains expanded graphite;
(2) lauryl sodium sulfate of 20~25g is mixed with 200~220mL deionized water, stirs, emulsion is obtained, by 10
~15g expanded graphite is immersed in emulsion, is obtained mixing suspension, is ultrasonically treated to mixing suspension, ultrasonic treatment
The water slurry of nano-graphite lamella is obtained afterwards;
(3) 100~110g acrylonitrile and 90~100g butadiene are added in the three-necked flask with blender and thermometer, to
100~120mL sodium hydroxide solution, 30~40g polyvinyl alcohol, 100~110mL nano-graphite lamella are added in three-necked flask
Aqueous suspension body fluid starts blender, after stirring and emulsifying, 1~3g potassium peroxydisulfate, heat temperature raising is added, insulation reaction obtains nanometer
Enhance nitrile rubber;
(4) 40~45g acrylic acid and copolymer-maleic anhydride are added in the beaker equipped with 100~120mL acetone soln, are added
Heat heating is added 60~70g bentonite to beaker, is cooled to room temperature and obtains bentonite suspension, bentonite suspension is placed in
In supercentrifuge, centrifugation removes upper liquid, obtains lamella bentonite, lamella bentonite is placed in baking oven, heat temperature raising,
It is dry, obtain modified alta-mud;
(5) nanometer enhancing nitrile rubber is placed in double roll mill and is plasticated, then nanometer is added into double roll mill to enhance fourth
Modified alta-mud, the 20~25g white carbon black of nitrile rubber quality 5~8%, mixing are plasticated, discharging, obtain conductive wear-resisting nitrile rubber
Material.
2. a kind of preparation method of wear-resisting nitrile rubber of conduction according to claim 1, it is characterised in that: step
(1) the vacuum oven temperature described in is set as 100~110 DEG C, and drying time is 8~10h, and microwave power is 700~800W,
Microwave treatment time is 40~45s, and microwave treatment heating expansion number is 3~5 times.
3. a kind of preparation method of wear-resisting nitrile rubber of conduction according to claim 1, it is characterised in that:
Mixing time described in step (2) is 10~15min, sets ultrasonic frequency as 30~32KHz.
4. a kind of preparation method of wear-resisting nitrile rubber of conduction according to claim 1, it is characterised in that:
The mass fraction of sodium hydroxide solution described in step (3) is 5%, and speed of agitator is 80~90r/min, when stirring and emulsifying
Between be 10~15min, temperature is 45~48 DEG C after heat temperature raising, and the insulation reaction time is 3~4h.
5. a kind of preparation method of wear-resisting nitrile rubber of conduction according to claim 1, it is characterised in that:
The mass fraction of acetone soln described in step (4) is 30~40%, and temperature is 80~85 DEG C after heat temperature raising, centrifuge
Revolving speed is 3200~3400r/min, and centrifugation time is 15~17min, and temperature is 80~90 DEG C after heat temperature raising, and drying time is
3~4h.
6. a kind of preparation method of wear-resisting nitrile rubber of conduction according to claim 1, it is characterised in that: step
(5) condition of plasticating described in: preceding roll temperature is 55~60 DEG C, and rear roll temperature is 50~55 DEG C, and roll spacing is 6~8mm, number of plasticating
It is 1~3 time, mixing number of plasticating is 2~3 times.
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CN1401679A (en) * | 2002-08-27 | 2003-03-12 | 珠海公牛高性能复合材料股份有限公司 | Rubber/lamellar silicate composite nanomaterial and mfg. method thereof |
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CN101463149B (en) * | 2007-12-19 | 2011-11-09 | 北京化工大学 | Preparation of wear resistant rubber composite material |
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