CN107778564A - A kind of nitrile rubber is ageing-resistant material modified and preparation method thereof - Google Patents
A kind of nitrile rubber is ageing-resistant material modified and preparation method thereof Download PDFInfo
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- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
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Abstract
It is ageing-resistant material modified and preparation method thereof the invention discloses a kind of nitrile rubber, including following parts by weight raw material are prepared：65 75 parts of nitrile rubber, 20 30 parts of polyvinyl acetate, 15 20 parts of nano-calcium carbonate, 5 10 parts of modifying agent, 0.3 0.8 parts of coupling agent, 0.3 0.5 parts of crosslinking agent, 13 parts of ultra-violet absorber, 13 parts of antioxidant；The present invention carries out the nano-calcium carbonate Jing Guo specific aim modification with nitrile rubber compound, and nano-calcium carbonate is set to be dispersed in nitrile rubber system, obtained acrylonitrile butadiene rubber modified material ageing-resistant performance is excellent, is advantageous to application of the nitrile rubber in more areas.
Description
Technical field
The present invention relates to modified nitrile rubber field, and in particular to a kind of nitrile rubber it is ageing-resistant material modified and its
Preparation method.
Background technology
Nitrile rubber is that oil resistivity is fabulous, resistance to as made from butadiene and acrylonitrile using emulsion polymerization at low temperature production
Mill property is higher, and heat resistance is preferable, bonding force is strong, good water resistance, air-tightness and excellent.Its shortcoming is that lower temperature resistance is poor, resistance to
Ozon difference, insulating properties are inferior, and elasticity is slightly lower.Nitrile rubber is widely used in the various oil resistant rubber products of system, a variety of resistance to lubricating pads
Circle, pad, sleeve pipe, flexible package, flexible rubber hose, printer's roll, cable glue material etc., in industries such as automobile, aviation, oil, duplicating
In turn into essential elastomeric material.
With the continuous improvement that people are required material ageing-resistant performance, the nitrile rubber without ageing-resistant modification has been difficult to
Meet demand, thus, ageing-resistant modification is carried out to nitrile rubber and necessitated.Now to ABS ageing-resistant modification processing method
Species is various, and modified effect is also fine, especially with the appearance and application of nano material, the resistance to ag(e)ing increase of nitrile rubber
Significant effect, nitrile rubber is set largely to be used in more areas, but there is also deficiency.Although nano material has ageing-resistant increasing
The advantages of potent fruit is good, and addition is small, but there is also difficulties in dispersion, the defects of cost is high.In ageing-resistant modifying process is carried out,
Nano material, which disperses inequality, can influence its ageing-resistant effect, and obtained material modified resistance to ag(e)ing is relatively low, to material modified life
Production and application adversely affect.
The content of the invention
A kind of the defects of it is an object of the invention to overcome existing nitrile rubber resistance to ag(e)ing deficiency, there is provided butyronitrile rubber
Glue is ageing-resistant material modified and preparation method thereof；The present invention is by the nano-calcium carbonate and nitrile rubber Jing Guo specific aim modification
Carry out compound, and nano-calcium carbonate is dispersed in nitrile rubber system, obtained acrylonitrile butadiene rubber modified material is ageing-resistant
Excellent performance, be advantageous to application of the nitrile rubber in more areas.
It is ageing-resistant material modified the invention provides a kind of nitrile rubber including following in order to realize foregoing invention purpose
Parts by weight raw material are prepared：The nitrile rubber of 65-75 parts, the polyvinyl acetate of 20-30 parts, the nano-calcium carbonate of 15-20 parts
Calcium, the modifying agent of 5-10 parts, the coupling agent of 0.3-0.8 parts, the crosslinking agent of 0.3-0.5 parts, the ultra-violet absorber of 1-3 parts, 1-3
The antioxidant of part.
A kind of above-mentioned nitrile rubber is ageing-resistant material modified, and it is resistance to old to increase resin material according to nano-calcium carbonate and crosslinking
The general principle for the property changed, not only by targetedly screening modifying agent, coupling agent and the species of crosslinking agent, to improve nano-calcium carbonate
Compatibility between calcium and nitrile rubber, and make nano-calcium carbonate disperse evenly, to make nano-calcium carbonate pair in nitrile rubber
The resistance to ag(e)ing humidification of nitrile rubber is more preferable, also the nitrile rubber by controlling the degree of polymerization of nitrile rubber to make modified
It is material modified to reach optimum balance relation between resistance to ag(e)ing and processability, so as to which the acrylonitrile butadiene rubber modified material for making to obtain exists
Under conditions of excellent resistance to ag(e)ing, it may have excellent processability, it is applied in more areas.
A kind of above-mentioned nitrile rubber is ageing-resistant material modified, wherein, described nano-calcium carbonate particle diameter is 10-80nm；Receive
Rice calcium carbonate particle diameter is smaller, and dispersiveness is poorer, and nano-calcium carbonate particle diameter is bigger, and the ageing-resistant humidification of nitrile rubber is got over
Difference；Preferably, described nano-calcium carbonate particle diameter is 30-50nm；Most preferably, described nano-calcium carbonate particle diameter is 40nm.
A kind of above-mentioned nitrile rubber is ageing-resistant material modified, wherein, described modifying agent is triethanolamine and phosphorous acid three
The mixture of phenyl ester composition；Described modifying agent can improve the compatibility of nano-calcium carbonate and nitrile rubber, and and can is in nanometer
Calcium carbonate surface forms polar group, beneficial to scattered；Preferably, triethanolamine and triphenyl phosphite in described modifying agent
The ratio between amount of material is 1 ︰ 1.
A kind of above-mentioned nitrile rubber is ageing-resistant material modified, wherein, the antioxidant is antioxidant 3314, antioxidant 626
One or both of.Described ultra-violet absorber is UV-3813.
A kind of above-mentioned nitrile rubber is ageing-resistant material modified, wherein, the degree of polymerization of polyvinyl acetate is bigger, then fourth after being crosslinked
The material modified resistance to ag(e)ing of nitrile rubber is poorer, and processability is better, and the polymer of polyvinyl acetate is smaller, then butyronitrile rubber after being crosslinked
The material modified resistance to ag(e)ing of glue is better, and processability is poorer, therefore, selects rational polymerization degree of polyvinyl acetate, is that balance is resistance to
The important means of aging and processability.The degree of polymerization of described polyvinyl acetate is 280-380；Preferably, described poly-vinegar
The degree of polymerization of sour ethene is 300-350；Optimal, the degree of polymerization of described polyvinyl acetate is 320；By preferred, obtain
Acrylonitrile butadiene rubber modified material both has excellent resistance to ag(e)ing, it may have preferable processability, is adapted to nitrile rubber more leading
Popularization and application are carried out in domain.
Wherein, the described nitrile rubber degree of polymerization is 600-1200；Preferably, the degree of polymerization of the nitrile rubber is 800-
1100；Most preferably, the degree of polymerization of described nitrile rubber is 1000；By preferred, obtained acrylonitrile butadiene rubber modified material was both
With excellent resistance to ag(e)ing, it may have preferable processability.
A kind of above-mentioned nitrile rubber is ageing-resistant material modified, wherein, described coupling agent is distearyl acyl-oxygen isopropoxy
Aluminate coupling agent；Distearyl acyl-oxygen aluminum isopropoxide acid esters can increase nano-calcium carbonate and nitrile rubber and it is material modified it
Between compatibility, improve the performance of acrylonitrile butadiene rubber modified material.
Wherein, described crosslinking agent is aziridine, and the crosslinking agent can be by the polymer raw materials of two kinds of different polymerization degrees
Appropriate crosslinking, improve the resistance to ag(e)ing of acrylonitrile butadiene rubber modified material.
A kind of above-mentioned nitrile rubber is ageing-resistant material modified, wherein, its raw material also includes dispersant, plasticizer, anti-quiet
One or more auxiliary agents in electric agent, coloring agent, brightener；Above-mentioned auxiliary agent can improve the processing of acrylonitrile butadiene rubber modified material
Property, increase the effect such as its feature, so as to increase its applicability.
In order to realize foregoing invention purpose, further, present invention also offers a kind of ageing-resistant modified material of nitrile rubber
The preparation method of material, comprises the following steps：
（1）Nano-calcium carbonate is handled with coupling agent；
（2）Nano-calcium carbonate Jing Guo coupling agent treatment is subjected to cladding processing with modifying agent；
（3）Combined Processing is carried out after nano-calcium carbonate after cladding is well mixed with nitrile rubber in the electric field, is mixed
Material；
（4）Compound place is being carried out after compound is well mixed with polyvinyl acetate, crosslinking agent, antioxidant, ultra-violet absorber
Reason, obtains acrylonitrile butadiene rubber modified material.
A kind of ageing-resistant material modified preparation method of nitrile rubber, is first carried out at coupling with coupling agent to nano-calcium carbonate
Reason, increase nano-calcium carbonate and modifying agent, the compatibility of nitrile rubber；Place is modified to nano-calcium carbonate with modifying agent again
Reason, and form polar group on its surface；Finally make the polarity in nano-calcium carbonate surface and nitrile rubber chain using external electric field
Group polarizes, powered,, also can be with while making nano-calcium carbonate dispersed by repelling each other between electric charge or attracting principle
Polar group on nitrile rubber chain is bonded, so that the ageing-resistant enhancing effect of nano-calcium carbonate obtains maximum body
It is existing, so as to get modified butadiene acrylonitrile rubber resistance to ag(e)ing significantly improve；The preparation method is simple and reliable, is suitable for nitrile rubber and changes
Extensive, the industrialized production of property material.
A kind of above-mentioned ageing-resistant material modified preparation method of nitrile rubber, wherein, it is preferred that step 1 is carried out at coupling
Ultrasonic assistant can be used during reason；Shaken by the high speed of ultrasonic wave, make nano-calcium carbonate dispersiveness more preferable, and to coupling
Processing has facilitation.
A kind of above-mentioned ageing-resistant material modified preparation method of nitrile rubber, wherein, the electric field energy described in step 3 is to base
Group produces polarization, makes group powered, so as to promote the scattered and bonded effect of nano-calcium carbonate, improves modified butyronitrile rubber
The resistance to ag(e)ing of glue.
Preferably, described electric-field intensity is 1.5-2.8kv/m；Electric-field intensity is too small, and polarization effect is weak, to nano-calcium carbonate
The dispersion effect of calcium is poor；Electric-field intensity is excessive, and polarization effect is too strong, and intermolecular force is too big, and strand produces displacement,
Arrangement and the bonded performance for having an impact, acrylonitrile butadiene rubber modified material may being reduced to strand；Most preferably, described electricity
Field intensity is 2.0-2.5kv/m.
Wherein, it is preferred that described electric field is the constant parallel electric field of direction of an electric field；The constant parallel electric field of direction of an electric field
Best to the polarization effect of polar group, group intermolecular forces are stable, to the scattered and bonded facilitation of nano-calcium carbonate
Best results.
Compared with prior art, beneficial effects of the present invention：
1st, the acrylonitrile butadiene rubber modified material of the present invention targetedly screens the species of modifying agent, coupling agent and crosslinking agent, makes nano-sized carbon
Compatibility between sour calcium and nitrile rubber is more preferable, and the dispersiveness in nitrile rubber is more preferable, and nano-calcium carbonate is to nitrile rubber
Resistance to ag(e)ing humidification it is more preferable.
2nd, the acrylonitrile butadiene rubber modified material of the present invention makes modification by controlling the degree of polymerization of nitrile rubber and polyvinyl acetate
Acrylonitrile butadiene rubber modified material afterwards reaches optimum balance relation between resistance to ag(e)ing and processability, so as to get nitrile rubber change
Property material is under conditions of with excellent resistance to ag(e)ing, it may have excellent processability.
3rd, the preparation method of the acrylonitrile butadiene rubber modified material of the present invention, using the polarization of external electric field, can promote nano-sized carbon
Sour calcium is scattered and bonded in nitrile rubber system, and the ageing-resistant enhancing effect of nano-calcium carbonate is more preferable, obtained butyronitrile rubber
The material modified resistance to ag(e)ing of glue is higher.
4th, the preparation method of the acrylonitrile butadiene rubber modified material of the present invention is simple, reliable, is adapted to the big of acrylonitrile butadiene rubber modified material
Scale, industrialized production.
Embodiment
With reference to test example and embodiment, the present invention is described in further detail.But this should not be understood
Following embodiment is only limitted to for the scope of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that present invention is realized
The scope of invention.
Embodiment 1
（1）28 parts of nano-calcium carbonate is handled with 0.5 part of distearyl acyl-oxygen aluminum isopropoxide acid esters；
（2）Nano-calcium carbonate Jing Guo coupling agent treatment is carried out with 3.5 parts of triethanolamine and 3.5 parts of triphenyl phosphite
Cladding processing；
（3）In electric-field intensity after nano-calcium carbonate after cladding is well mixed with the nitrile rubber that 70 parts of the degree of polymerization is 900
To be extruded in the constant parallel electric field of 2.0kv/m direction of an electric field, compound is obtained；
（4）Polyvinyl acetate that the compound that step 3 is obtained and 25 parts of the degree of polymerization are 320,0.4 part of aziridine, 2 parts
Extruded after ultra-violet absorber, 2 parts of antioxidant are well mixed, obtain acrylonitrile butadiene rubber modified material.
Embodiment 2
（1）15 parts of nano-calcium carbonate is handled with 0.3 part of distearyl acyl-oxygen aluminum isopropoxide acid esters；
（2）Nano-calcium carbonate Jing Guo coupling agent treatment is carried out with 2.5 parts of triethanolamine and 2.5 parts of triphenyl phosphite
Cladding processing；
（3）In electric-field strength after nano-calcium carbonate after cladding is well mixed with the nitrile rubber that 65 parts of the degree of polymerization is 1200
Spend in the electric field for 2.8kv/m and extruded, obtain compound；
（4）Polyvinyl acetate that the compound that step 3 is obtained and 20 parts of the degree of polymerization are 280,0.3 part of aziridine, 1 part
Extruded after ultra-violet absorber, 3 parts of antioxidant are well mixed, obtain acrylonitrile butadiene rubber modified material.
Embodiment 3
（1）20 parts of nano-calcium carbonate is handled with 0.8 part of distearyl acyl-oxygen aluminum isopropoxide acid esters；
（2）Nano-calcium carbonate Jing Guo coupling agent treatment is coated with 5 parts of triethanolamine and 5 parts of triphenyl phosphite
Processing；
（3）In electric-field strength after nano-calcium carbonate after cladding is well mixed with the nitrile rubber that 75 parts of the degree of polymerization is 600
Spend to be extruded in the constant parallel electric field of 1.5kv/m direction of an electric field, obtain compound；
（4）Polyvinyl acetate that the compound that step 3 is obtained and 30 parts of the degree of polymerization are 380,0.5 part of aziridine, 3 parts
Extruded after ultra-violet absorber, 1 part of antioxidant are well mixed, obtain acrylonitrile butadiene rubber modified material.
Comparative example 1
（1）18 parts of nano-calcium carbonate is handled with 0.5 part of distearyl acyl-oxygen aluminum isopropoxide acid esters；
（2）By the nano-calcium carbonate Jing Guo coupling agent treatment and 8 parts of dispersant, the nitrile rubber that 70 parts of the degree of polymerization is 900
Extruded after well mixed in the constant parallel electric field of the direction of an electric field that electric-field intensity is 2.0kv/m, obtain compound；
（3）0.4 part of aziridine of polyvinyl acetate that the compound that step 2 is obtained and 25 parts of the degree of polymerization are 320,2 parts
Extruded after ultra-violet absorber, 2 parts of antioxidant are well mixed, obtain acrylonitrile butadiene rubber modified material.
Comparative example 2
（1）18 parts of nano-calcium carbonate is handled with 0.5 part of distearyl acyl-oxygen aluminum isopropoxide acid esters；
（2）Nano-calcium carbonate Jing Guo coupling agent treatment is carried out with 3.5 parts of triethanolamine and 3.5 parts of triphenyl phosphite
Cladding processing；
（3）It is 320 by nitrile rubber that the nano-calcium carbonate after cladding and 70 parts of the degree of polymerization are 900,25 parts of the degree of polymerization
Extruded, obtained after polyvinyl acetate, 0.4 part of aziridine, 2 parts of ultra-violet absorber, 2 parts of antioxidant are well mixed
Acrylonitrile butadiene rubber modified material.
Comparative example 3
（1）18 parts of nano-calcium carbonate is handled with 0.5 part of distearyl acyl-oxygen aluminum isopropoxide acid esters；
（2）Nano-calcium carbonate Jing Guo coupling agent treatment is carried out with 3.5 parts of polystyrene and 3.5 parts of triphenyl phosphite
Cladding processing；
（3）In electric-field intensity after nano-calcium carbonate after cladding is well mixed with the nitrile rubber that 70 parts of the degree of polymerization is 900
To be extruded in the constant parallel electric field of 2.0kv/m direction of an electric field, compound is obtained；
（4）Polyvinyl acetate that the compound that step 3 is obtained and 25 parts of the degree of polymerization are 320,0.4 part of aziridine, 2 parts
Extruded after ultra-violet absorber, 2 parts of antioxidant are well mixed, obtain acrylonitrile butadiene rubber modified material.
Comparative example 4
（1）18 parts of nano-calcium carbonate is handled with 0.5 part of distearyl acyl-oxygen aluminum isopropoxide acid esters；
（2）Nano-calcium carbonate Jing Guo coupling agent treatment is carried out with 3.5 parts of triethanolamine and 3.5 parts of triphenyl phosphite
Cladding processing；
（3）By polyvinyl acetate that the nano-calcium carbonate after cladding and 25 parts of the degree of polymerization are 320,0.4 part of aziridine, 2 parts
Ultra-violet absorber, 2 parts of antioxidant, 70 parts of the degree of polymerization be 900 nitrile rubber it is well mixed after in electric-field intensity be
Extruded in the constant parallel electric field of 2.0kv/m direction of an electric field, obtain acrylonitrile butadiene rubber modified material.
Comparative example 5
（1）18 parts of nano-calcium carbonate is handled with 0.5 part of distearyl acyl-oxygen aluminum isopropoxide acid esters；
（2）Nano-calcium carbonate Jing Guo coupling agent treatment is carried out with 3.5 parts of triethanolamine and 3.5 parts of triphenyl phosphite
Cladding processing；
（3）In electric-field intensity after nano-calcium carbonate after cladding is well mixed with the nitrile rubber that 70 parts of the degree of polymerization is 500
To be extruded in the constant parallel electric field of 2.0kv/m direction of an electric field, compound is obtained；
（4）The compound that step 3 is obtained and 25 parts of the degree of polymerization are 250 polyvinyl acetate, 2 parts of ultra-violet absorber, 2
Extruded after the antioxidant of part, 0.4 part of aziridine are well mixed, obtain acrylonitrile butadiene rubber modified material.
By the acrylonitrile butadiene rubber modified material in above-described embodiment 1-3 and comparative example 1-5, performance detection, record data are carried out
It is as follows：
| Performance | Ageing resistance | Processability |
| Embodiment 1 | ++++++ | ++++ |
| Embodiment 2 | ++++++ | ++++ |
| Embodiment 3 | ++++++ | ++++ |
| Comparative example 1 | ++++ | ++++ |
| Comparative example 2 | ++++ | ++++ |
| Comparative example 3 | ++++ | ++++ |
| Comparative example 4 | ++++ | ++++ |
| Comparative example 5 | ++++++ | ++ |
Note："+" is more, illustrates that performance is better.
Above-mentioned analysis of experimental data is understood, the acrylonitrile butadiene rubber modified material of the invention being prepared in embodiment 1-3, received
Rice calcium carbonate is uniformly dispersed, and good with the compatibility of nitrile rubber, material modified resistance to ag(e)ing is good, and processability is good；And comparative example 1
In, modifying agent is not used processing is modified to nano-calcium carbonate, although adding dispersant, nano-calcium carbonate dispersion effect
Difference, the poor compatibility with nitrile rubber, material modified resistance to ag(e)ing significantly reduce；Do not answered in the electric field in comparative example 2
Conjunction is handled, and nano-calcium carbonate dispersion effect is poor, and material modified resistance to ag(e)ing significantly reduces；Modifying agent is not this in comparative example 3
Apply for defined, nano-calcium carbonate dispersion effect is poor, and material modified resistance to ag(e)ing significantly reduces；It is crosslinked in comparative example 4 anti-
Equally should carry out in the electric field, electric field has a negative impact to cross-linking reaction, so as to get material modified resistance to ag(e)ing reduce；
The nitrile rubber and polymerization degree of polyvinyl acetate used in comparative example 5 is too small, although resistance to ag(e)ing increased after compound, its
Processability significantly reduces, and is unfavorable for the application of acrylonitrile butadiene rubber modified material.
Claims (10)
1. a kind of nitrile rubber is ageing-resistant material modified, it is characterised in that is prepared including following parts by weight raw material：65-
75 parts of nitrile rubber, the nano-calcium carbonate of 15-20 parts, the polyvinyl acetate of 20-30 parts, the modifying agent, 0.3-0.8 of 5-10 parts
The coupling agent, the crosslinking agent of 0.3-0.5 parts, the ultra-violet absorber of 1-3 parts, the antioxidant of 1-3 parts of part；The modifying agent is three
The mixture of monoethanolamine and triphenyl phosphite composition；The coupling agent is distearyl acyl-oxygen aluminum isopropoxide acid esters coupling agent,
The crosslinking agent is aziridine；The degree of polymerization of the polyvinyl acetate is 280-380；The nitrile rubber degree of polymerization is 600-
1200。
It is 2. according to claim 1 material modified, it is characterised in that triethanolamine and phosphorous triphenyl phosphate in the modifying agent
The ratio between amount of material of ester is 1 ︰ 1.
It is 3. according to claim 1 material modified, it is characterised in that the degree of polymerization of the polyvinyl acetate is 300-350.
It is 4. according to claim 3 material modified, it is characterised in that the degree of polymerization of the polyvinyl acetate is 320.
It is 5. according to claim 1 material modified, it is characterised in that the nitrile rubber degree of polymerization is 800-1100.
It is 6. according to claim 5 material modified, it is characterised in that the nitrile rubber degree of polymerization is 1000.
7. a kind of material modified preparation method as described in claim any one of 1-6, it is characterised in that comprise the following steps：
（1）Nano-calcium carbonate is handled with coupling agent；
（2）Nano-calcium carbonate Jing Guo coupling agent treatment is subjected to cladding processing with modifying agent；
（3）Combined Processing is carried out after nano-calcium carbonate after cladding is well mixed with nitrile rubber in the electric field, is mixed
Material；
（4）Compound place is being carried out after compound is well mixed with polyvinyl acetate, crosslinking agent, antioxidant, ultra-violet absorber
Reason, obtains acrylonitrile butadiene rubber modified material.
8. preparation method according to claim 7, it is characterised in that step（3）Middle electric-field intensity is 1.5-2.8kv/m.
9. preparation method according to claim 8, it is characterised in that step（3）Middle electric-field intensity is 2.0-2.5kv/m.
10. preparation method according to claim 7, it is characterised in that step（3）Middle electric field, which is that direction of an electric field is constant, puts down
Row electric field.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711271422.2A CN107778564A (en) | 2017-12-05 | 2017-12-05 | A kind of nitrile rubber is ageing-resistant material modified and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711271422.2A CN107778564A (en) | 2017-12-05 | 2017-12-05 | A kind of nitrile rubber is ageing-resistant material modified and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN107778564A true CN107778564A (en) | 2018-03-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711271422.2A Withdrawn CN107778564A (en) | 2017-12-05 | 2017-12-05 | A kind of nitrile rubber is ageing-resistant material modified and preparation method thereof |
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| Country | Link |
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- 2017-12-05 CN CN201711271422.2A patent/CN107778564A/en not_active Withdrawn
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Application publication date: 20180309 |