CN107501656A - 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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- CN107501656A CN107501656A CN201710961369.2A CN201710961369A CN107501656A CN 107501656 A CN107501656 A CN 107501656A CN 201710961369 A CN201710961369 A CN 201710961369A CN 107501656 A CN107501656 A CN 107501656A
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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, with rubber molecule autovulcanization occurs for nano-graphite lamella active site, forms conductive network, so as to reach the effect for improving 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, larger hysteresis loss can be produced in friction, forms abrasive particle after the sizing material of friction surface is destroyed, these abrasive particles can improve adhesion strength of the sizing material to the face of rubbing, so as to reach the purpose for improving 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 technology
Rubber is the material of main part of rubber manufacture.Rubber is a kind of flexible polymer, according to mode is made
Difference, rubber can be divided into synthetic rubber and the class of natural rubber two.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 condensing, washing, being molded, drying i.e.
Obtain natural rubber.Prepared by synthetic rubber is by artificial synthesis, variety classes can be synthesized using different raw materials
Rubber, such as butadiene rubber, neoprene, butadiene-styrene rubber, nitrile rubber.
Nitrile rubber is as made from butadiene and acrylonitrile through emulsion polymerization, contains unsaturated double-bond in its strand
With polar group-CN, thus possesses outstanding lubricating oil resistance energy.In addition rubber itself possessed cross-linked structure and
The high resiliency of acquisition, thus there is fabulous oil resistance and excellent physical and mechanical properties, it is widely used in industrial production
In.It is mainly used in 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
Pressing, such as O-ring, oil sealing, leather cup, diaphragm, valve, bellows, it is also used for making offset plate and wear part.But fourth
The intensity of nitrile rubber material is not high, weather resistance is bad, easy abrasion, electrical property is inferior, elasticity is slightly lower etc..In actual production often
These shortcomings 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.
The content of the invention
Present invention mainly solves technical problem, for rubber poorly conductive, easily wear the defects of, there is provided one kind is led
The preparation method of the wear-resisting nitrile rubber of electricity.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of the wear-resisting nitrile rubber of conduction, it is characterised in that specifically preparation process is：
（1）Weigh 20~30g expansible graphites to be placed in vacuum drying chamber, the oxygen of 100~120g five is put into vacuum drying chamber
Change two phosphorus, dry, dried expansible graphite is put into beaker, then beaker is placed under microwave and handled, it is cold to take out beaker
But to room temperature, expansible graphite is expanded, obtains expanded graphite；
（2）20~25g lauryl sodium sulfate is mixed with 200~220mL deionized waters, stirs, emulsion is obtained, by 10
~15g expanded graphites are immersed in emulsion, obtain mixing suspension, mixing suspension is ultrasonically treated, and are ultrasonically treated
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 agitator and thermometer, to
100~120mL sodium hydroxide solutions, 30~40g polyvinyl alcohol, 100~110mL nano-graphite lamellas are added in three-necked flask
Aqueous suspension body fluid, start agitator, after stirring and emulsifying, add 1~3g potassium peroxydisulfates, heat temperature raising, insulation reaction, obtain nanometer
Strengthen nitrile rubber；
（4）40~45g acrylic acid and maleic anhydride acid copolymer are added in the beaker equipped with 100~120mL acetone solns, heating
Heating, 60~70g bentonites are added to beaker, room temperature is cooled to and obtains bentonite suspension, bentonite suspension is placed in height
In fast centrifuge, centrifugation, upper liquid is removed, lamella bentonite is obtained, lamella bentonite is placed in baking oven, heat temperature raising, done
It is dry, obtain modified alta-mud；
（5）Nanometer enhancing nitrile rubber is placed in double roll mill and plasticated, then nanometer enhancing fourth is added into double roll mill
Modified alta-mud, the 20~25g white carbons of nitrile rubber quality 5~8%, mixing are plasticated, discharging, obtain conductive wear-resisting nitrile rubber
Material.
Step（1）Described sets vacuum drying chamber temperature as 100~110 DEG C, and 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.
Step（2）Described mixing time is 10~15min, sets ultrasonic frequency as 30~32KHz.
Step（3）The mass fraction of described sodium hydroxide solution is 5%, and speed of agitator is 80~90r/min, stirring breast
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.
Step（4）The mass fraction of described acetone soln is 30~40%, and temperature is 80~85 DEG C after heat temperature raising, from
Scheming rotating speed is 3200~3400r/min, and centrifugation time is 15~17min, and temperature is 80~90 DEG C after heat temperature raising, when drying
Between be 3~4h.
Step（5）Described condition of plasticating：Preceding roll temperature be 55~60 DEG C, rear roll temperature be 50~55 DEG C, roll spacing be 6~
8mm, number of plasticating are 1~3 time, and mixing plasticates number as 2~3 times.
The beneficial effects of the invention are as follows：
（1）By expansible graphite microwave treatment in the present invention, heat expandable graphite obtains expanded graphite, then expanded graphite is put
It is ultrasonically treated in surface activating solution, expanded graphite, which is shaken, is dispersed into nano-graphite lamella, and nano-graphite lamella is in propylene
Nitrile is with that during butadiene copolymer, because nano-graphite lamella there may be some active reaction points, can trigger the friendship of rubber
Connection reaction, under emulsion blending, graphite flake layer has reached nano-dispersed, while also certain intercalation configuration in rubber matrix
In the presence of, on nano-graphite lamella potential active site and rubber molecule there occurs sufficiently contacting and thus there occurs autovulcanization,
Cause nano-graphite lamella fully dispersed in rubber, and the insulation crystalline region of rubber can be destroyed, form conductive network, so as to rise
To the effect for improving nitrile rubber electric conductivity；
（2）Due between the polar functional group and the group of rubber in the fine dispersion and graphite flake layer of nano-graphite in the present invention
Polar interaction, cause interface cohesion strong between graphite and matrix, greatly reduce the activity of nitrile rubber segment
Ability, rubber will not produce large deformation in friction is worn surface, and modified alta-mud is added during plasticating to be inserted
Layer can produce larger hysteresis loss into rubber in friction, and abrasive particle is formed after the sizing material of friction surface is destroyed, these
Abrasive particle can improve adhesion strength of the sizing material to the face of rubbing, so as to reach the purpose for improving wear resistance, before having wide application
Scape.
Embodiment
Weigh 20~30g expansible graphites to be placed in vacuum drying chamber, set vacuum drying chamber temperature as 100~110 DEG C,
100~120g phosphorus pentoxides are put into vacuum drying chamber, 8~10h is dried, dried expansible graphite is put into beaker
In, then beaker is placed under microwave and is cooled to room temperature with 700~800W 40~45s of Power Processing, taking-up beaker, makes may expand
Graphite expands, and such microwave treatment heating expands 3~5 times, obtains expanded graphite；By 20~25g dodecyl sulphate
Sodium mixes with 200~220mL deionized waters, stirs 10~15min, obtains emulsion, 10~15g expanded graphites are immersed in into breast
Change in liquid, obtain mixing suspension, mixing suspension is ultrasonically treated, set ultrasonic frequency as 30~32KHz, ultrasound
The water slurry of nano-graphite lamella is obtained after processing；100~110g acrylonitrile and 90~100g butadiene are added to carry and stirred
In the three-necked flask for mixing device and thermometer, it is molten that the sodium hydroxide that 100~120mL mass fractions are 5% is added into three-necked flask
Liquid, 30~40g polyvinyl alcohol, the aqueous suspension body fluid of 100~110mL nano-graphite lamellas, start agitator, with 80~90r/
After 10~15min of min rotating speed stirring and emulsifyings, 1~3g potassium peroxydisulfates are added, are heated to 45~48 DEG C, insulation reaction 3~
4h, obtain nanometer enhancing nitrile rubber；40~45g acrylic acid and maleic anhydride acid copolymer are added 100~120mL mass is housed
Fraction adds 60~70g bentonites, cooling in the beaker of 30~40% acetone solns, to be heated to 80~85 DEG C, to beaker
Bentonite suspension is obtained to room temperature, bentonite suspension is placed in supercentrifuge, with 3200~3400r/min rotating speed
15~17min is centrifuged, upper liquid is removed, obtains lamella bentonite, lamella bentonite is placed in baking oven, it is heated to 80~
90 DEG C, 3~4h is dried, 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 carbons of nanometer enhancing nitrile rubber quality 5~8%, mixing is plasticated 2~3 times, discharges, obtain
To conductive wear-resisting nitrile rubber.
Example 1
Weigh 20g expansible graphites to be placed in vacuum drying chamber, vacuum drying chamber temperature is set as 100 DEG C, to vacuum drying chamber
In be put into 100g phosphorus pentoxides, dry 8h, dried expansible graphite be put into beaker, then beaker is placed under microwave
With 700W Power Processing 40s, take out beaker and be cooled to room temperature, expand expansible graphite, such microwave treatment heating
Expansion 3 times, obtains expanded graphite；20g lauryl sodium sulfate is mixed with 200mL deionized waters, 10min is stirred, obtains
Emulsion, 10g expanded graphites are immersed in emulsion, obtain mixing suspension, mixing suspension is ultrasonically treated, if
It is 30KHz to determine ultrasonic frequency, and the water slurry of nano-graphite lamella is obtained after supersound process；By 100g acrylonitrile and 90g fourths
Diene is added in the three-necked flask with agitator and thermometer, and the hydrogen that 100mL mass fractions are 5% is added into three-necked flask
Sodium hydroxide solution, 30g polyvinyl alcohol, the aqueous suspension body fluid of 100mL nano-graphite lamellas, start agitator, with 80r/min rotating speeds
After stirring and emulsifying 10min, 1g potassium peroxydisulfates are added, are heated to 45 DEG C, insulation reaction 3h, obtain nanometer enhancing butyronitrile rubber
Glue；40g acrylic acid and maleic anhydride acid copolymer are added 100mL mass fractions are housed in the beaker of 30% acetone soln, to heat
80 DEG C are warming up to, 60g bentonites is added to beaker, is cooled to room temperature and obtains bentonite suspension, bentonite suspension is placed in
In supercentrifuge, 15min is centrifuged with 3200r/min rotating speed, upper liquid is removed, lamella bentonite is obtained, by lamella swelling
Soil is placed in baking oven, is heated to 80 DEG C, is dried 3h, is obtained modified alta-mud；Nanometer enhancing nitrile rubber is placed in double roller
It it is 55 DEG C in preceding roll temperature in kneading machine, rear roll temperature is 50 DEG C, and roll spacing is plasticated 1 time under conditions of being 6mm, then is mixed to double roller
Modified alta-mud, the 20g white carbons of nanometer enhancing nitrile rubber quality 5% are added in mill, mixing is plasticated 2 times, discharges, obtain
Conductive wear-resisting nitrile rubber.
Example 2
Weigh 25g expansible graphites to be placed in vacuum drying chamber, vacuum drying chamber temperature is set as 105 DEG C, to vacuum drying chamber
In be put into 110g phosphorus pentoxides, dry 9h, dried expansible graphite be put into beaker, then beaker is placed under microwave
With 750W Power Processing 42s, take out beaker and be cooled to room temperature, expand expansible graphite, such microwave treatment heating
Expansion 4 times, obtains expanded graphite；23g lauryl sodium sulfate is mixed with 210mL deionized waters, 13min is stirred, obtains
Emulsion, 13g expanded graphites are immersed in emulsion, obtain mixing suspension, mixing suspension is ultrasonically treated, if
It is 31KHz to determine ultrasonic frequency, and the water slurry of nano-graphite lamella is obtained after supersound process；By 105g acrylonitrile and 95g fourths
Diene is added in the three-necked flask with agitator and thermometer, and the hydrogen that 110mL mass fractions are 5% is added into three-necked flask
Sodium hydroxide solution, 35g polyvinyl alcohol, the aqueous suspension body fluid of 105mL nano-graphite lamellas, start agitator, with 85r/min rotating speeds
After stirring and emulsifying 12min, 2g potassium peroxydisulfates are added, are heated to 46 DEG C, insulation reaction 3.5h, obtain nanometer enhancing butyronitrile rubber
Glue；42g acrylic acid and maleic anhydride acid copolymer are added 110mL mass fractions are housed in the beaker of 35% acetone soln, to heat
82 DEG C are warming up to, 65g bentonites is added to beaker, is cooled to room temperature and obtains bentonite suspension, bentonite suspension is placed in
In supercentrifuge, 16min is centrifuged with 3300r/min rotating speed, upper liquid is removed, lamella bentonite is obtained, by lamella swelling
Soil is placed in baking oven, is heated to 85 DEG C, is dried 3.5h, is obtained modified alta-mud；Nanometer enhancing nitrile rubber is placed in double
It is 57 DEG C in preceding roll temperature in roller kneading machine, rear roll temperature is 52 DEG C, and roll spacing is plasticated 2 times under conditions of being 7mm, then to double roller
Modified alta-mud, the 23g white carbons of nanometer enhancing nitrile rubber quality 6% are added in kneading machine, mixing is plasticated 2 times, discharges, obtain
To conductive wear-resisting nitrile rubber.
Example 3
Weigh 30g expansible graphites to be placed in vacuum drying chamber, vacuum drying chamber temperature is set as 110 DEG C, to vacuum drying chamber
In be put into 120g phosphorus pentoxides, dry 10h, dried expansible graphite be put into beaker, then beaker is placed on microwave
Under with 800W Power Processing 45s, take out beaker and be cooled to room temperature, expand expansible graphite, such microwave treatment adds
Thermal expansion 5 times, obtains expanded graphite；25g lauryl sodium sulfate is mixed with 220mL deionized waters, 15min is stirred, obtains
To emulsions, 15g expanded graphites are immersed in emulsion, obtain mixing suspension, mixing suspension is ultrasonically treated,
Ultrasonic frequency is set as 32KHz, the water slurry of nano-graphite lamella is obtained after supersound process；By 110g acrylonitrile and 100g
Butadiene is added in the three-necked flask with agitator and thermometer, and it is 5% that 120mL mass fractions are added into three-necked flask
Sodium hydroxide solution, 40g polyvinyl alcohol, the aqueous suspension body fluid of 110mL nano-graphite lamellas, start agitator, turned with 90r/min
After fast stirring and emulsifying 15min, 3g potassium peroxydisulfates are added, are heated to 48 DEG C, insulation reaction 4h, obtain nanometer enhancing butyronitrile rubber
Glue；45g acrylic acid and maleic anhydride acid copolymer are added 120mL mass fractions are housed in the beaker of 40% acetone soln, to heat
85 DEG C are warming up to, 70g bentonites is added to beaker, is cooled to room temperature and obtains bentonite suspension, bentonite suspension is placed in
In supercentrifuge, 17min is centrifuged with 3400r/min rotating speed, upper liquid is removed, lamella bentonite is obtained, by lamella swelling
Soil is placed in baking oven, is heated to 90 DEG C, is dried 4h, is obtained modified alta-mud；Nanometer enhancing nitrile rubber is placed in double roller
It it is 60 DEG C in preceding roll temperature in kneading machine, rear roll temperature is 55 DEG C, and roll spacing is plasticated 3 times under conditions of being 8mm, then is mixed to double roller
Modified alta-mud, the 25g white carbons of nanometer enhancing nitrile rubber quality 8% are added in mill, mixing is plasticated 3 times, discharges, obtain
Conductive wear-resisting nitrile rubber.
The nitrile rubber material that comparative example is produced with company of 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 1：1st, test side
Method
Abrasion resistance is detected using Akron abrasion machine by GB/T1689-2014 regulation.
Using example 1-3 produced by the present invention and comparative example product, 4 blocks are taken to accumulate identical on product respectively（15cm
×15cm×0.2cm）Test block.Under the conditions of 25 DEG C, the constant temperature and humidity that relative humidity is 55%, apply 500V voltages, utilize superelevation
Resistance/Weak current tester measure resistivity.
Table 1
It can be seen from data in table 1, the wear-resisting nitrile rubber of conduction produced by the present invention, wear hardness is significantly larger than country's mark
Standard, anti-wear performance is prominent and electric conductivity is excellent, and the product 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 specifically preparation process is：
（1）Weigh 20~30g expansible graphites to be placed in vacuum drying chamber, the oxygen of 100~120g five is put into vacuum drying chamber
Change two phosphorus, dry, dried expansible graphite is put into beaker, then beaker is placed under microwave and handled, it is cold to take out beaker
But to room temperature, expansible graphite is expanded, obtains expanded graphite；
（2）20~25g lauryl sodium sulfate is mixed with 200~220mL deionized waters, stirs, emulsion is obtained, by 10
~15g expanded graphites are immersed in emulsion, obtain mixing suspension, mixing suspension is ultrasonically treated, and are ultrasonically treated
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 agitator and thermometer, to
100~120mL sodium hydroxide solutions, 30~40g polyvinyl alcohol, 100~110mL nano-graphite lamellas are added in three-necked flask
Aqueous suspension body fluid, start agitator, after stirring and emulsifying, add 1~3g potassium peroxydisulfates, heat temperature raising, insulation reaction, obtain nanometer
Strengthen nitrile rubber；
（4）40~45g acrylic acid and maleic anhydride acid copolymer are added in the beaker equipped with 100~120mL acetone solns, heating
Heating, 60~70g bentonites are added to beaker, room temperature is cooled to and obtains bentonite suspension, bentonite suspension is placed in height
In fast centrifuge, centrifugation, upper liquid is removed, lamella bentonite is obtained, lamella bentonite is placed in baking oven, heat temperature raising, done
It is dry, obtain modified alta-mud；
（5）Nanometer enhancing nitrile rubber is placed in double roll mill and plasticated, then nanometer enhancing fourth is added into double roll mill
Modified alta-mud, the 20~25g white carbons of nitrile rubber quality 5~8%, mixing are plasticated, discharging, obtain conductive wear-resisting nitrile rubber
Material.
A kind of 2. preparation method of wear-resisting nitrile rubber of conduction according to claim 1, it is characterised in that：Step
（1）Described sets vacuum drying chamber temperature 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.
A kind of 3. preparation method of wear-resisting nitrile rubber of conduction according to claim 1, it is characterised in that：
Step（2）Described mixing time is 10~15min, sets ultrasonic frequency as 30~32KHz.
A kind of 4. preparation method of wear-resisting nitrile rubber of conduction according to claim 1, it is characterised in that：
Step（3）The mass fraction of described sodium hydroxide solution is 5%, and speed of agitator is 80~90r/min, during 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.
A kind of 5. preparation method of wear-resisting nitrile rubber of conduction according to claim 1, it is characterised in that：
Step（4）The mass fraction of described acetone soln is 30~40%, and temperature is 80~85 DEG C after heat temperature raising, centrifuge
Rotating 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.
A kind of 6. preparation method of wear-resisting nitrile rubber of conduction according to claim 1, it is characterised in that：Step
（5）Described condition of plasticating：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
For 1~3 time, mixing plasticates number as 2~3 times.
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