CN102504361A - Thermo-oxidative ageing resistance natural rubber nano-composite material and preparation method thereof - Google Patents
Thermo-oxidative ageing resistance natural rubber nano-composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a thermal-oxidative ageing resistance natural rubber nano-composite material, which comprises the following raw materials in parts by weight: 100 parts of natural rubber, 1 to 10 parts of nano-montmorillonite, 15 to 50 parts of carbon black, 2 to 4 parts of age resister, 0.5 to 3 parts of vulcanizing agent, 4 to 8 parts of vulcanizing active agent, and 1 to 4 parts of vulcanizing accelerator. The invention also discloses a preparation method of the composite material, which comprises the following steps of: mechanically intercalating natural rubber and nano-montmorillonite on a two-roll open mill; adding the vulcanizing active agent, the age resister, the carbon black packing, the vulcanizing accelerator and the vulcanizing agent; uniformly mixing to prepare natural master batch; storing at room temperature for over 16 hours; testing the positive vulcanization time by using a foaming curometer; vulcanizing a rubber material by using a plate vulcanizing agent at a temperature of between 143 and 153 DEG C, pressure of between 14 and 20MPa and positive vulcanizing time to obtain the ageing resistance natural rubber composite material. The organic nano-montmorillonite and the carbon black are adopted as packing, so that the thermal stability of natural rubber is improved under a condition that the mechanical performance is not sacrificed, and the natural rubber material with excellent thermal-oxidative ageing resistance is obtained.
Description
Technical field
This patent relates to the forming process field of superpolymer, relates in particular to a kind of heat oxygen aging resistance natural rubber nano composite material and preparation method thereof.
Background technology
Because tree elastomer has good cohesiveness, excellent process industrial art performance and physical and mechanical properties are like high-modulus; High-tensile, high tear resistance etc., and have and cooperate flexibility and processing characteristics widely; Through also having oil resistant, valuable character such as acidproof, alkaline-resisting, heat-resisting, cold-resistant, withstand voltage, wear-resisting after suitably handling, its Application Areas is very extensive, and automobile is arranged; Railway locomotive; The viton that requires has been satisfied not for processing characteristics especially in a plurality of fields such as aerospace and machinofacture, and often the way of employing and tree elastomer and usefulness is improved processing characteristics.
The most frequently used vulcanization system of tree elastomer is the sulfur cross-linking system, comprising: sulphur, promotor, promoting agent.
Different with the relative proportion of promotor according to sulphur, vulcanization system can be divided into: common sulfur cross-linking system, efficient vulcanization system and semi effcient vulcanization system.
More than 70% polysulfide crosslink bond (S in the cross-linked rubber network that common sulfur cross-linking system obtains
X-), have good initial fatigue property and dynamic and static state performance, but thermo-labile oxygen aging, cross-linked rubber can not be at life-time service under the comparatively high temps.And the cross-linked rubber of efficient vulcanization system has higher thermo oxidative aging performance, but initial dynamic fatigue property is poor.The resulting cross-linked rubber of semi effcient vulcanization system had both had an amount of polysulfidic bond, and an amount of single, polysulfide crosslink bond are arranged again, made both to have had the better dynamic performance, and moderate heatproof air aging performance is arranged again.These two kinds of vulcanization systems all are to be cost with the comprehensive physical and mechanical properties of sacrificing traditional sulfur cross-linking system.(Yang Qingzhi etc., rubber industry, 2005; ).
The TR 301 that constitutes tree elastomer connects with covalent linkage; In the environment, be easy under the pulsating stress effect, to give birth to heat and produce thermo-oxidative ageing, rubber molecule backbone breaking under arms because of inside; Simultaneously; The polysulfidic bond desulfurization generates more monosulfidic bond, polysulfidic bond, makes cross-linked rubber sclerosis and produces be full of cracks, lost strength or increase fatigue failure fast because of creep and be full of cracks.Therefore, improve the thermal-oxidative aging property of elastomeric material, the tree elastomer material of preparing heatproof air aging performance has important realistic meaning to practical engineering application.
Polynite is the very abundant a kind of mineral substance silicate of China's standing stock; In recent years; The development of polymer/laminated silicate intercalation nano compounding technology, it is compound to make inorganic materials with nano-lamellar structure and rubber reach nano level, thereby makes it to produce significant strengthening action (significantly improving the mechanical property and the thermostability of ethylene-propylene rubber(EPR)); And can improve other performances of rubber simultaneously, like resistance to air loss, oil-proofness, flame retardant resistance, stability to aging etc.
Summary of the invention
The object of the invention is to solve the relatively poor problem of natural rubber vulcanized rubber heatproof air aging performance; Adopting organo montmorillonite and carbon black is strengthening agent; Cure conditions is half effective sulfur cross-linking system, prepares the good heat oxygen aging resistance natural rubber vulcanized rubber goods of mechanical energy.
A kind of heat oxygen aging resistance natural rubber nano composite material, its raw material is formed as follows, and wherein said raw material umber is all represented with mass fraction except that specified otherwise:
Described vulcanizing agent is a sulphur.
Described nano imvite is the nano imvite of alkylamine modification, and the interlamellar spacing after the modification is 1.5-2.4nm.
Described anti-aging agent is CPPD N cyclohexyl N, N-phenyl-N '-sec.-propyl Ursol D, 2; 2; 4-trimethylammonium-1; 2-dihyaroquinoline polymer, BLE, N-PA or 2, at least a in 2 '-methylene radical-two (4-methyl-6-tert butyl phenol).
Described vulcanization leveller is zinc oxide and Triple Pressed Stearic Acid;
Described vulcanization accelerator is at least a in benzothiazyl disulfide, N cyclohexyl 2 benzothiazole sulfenamide, 2-benzothiazolyl mercaptan, vulkacit D or the tetramethyl-thiuram disulfide.
Described sooty size of particles is: (1) CTAB value is 20-100m
2/ g, (2) DBP value is 20-100m
3/ g.
Vulcanizing agent and vulcanization leveller all are the technology that well known to a person skilled in the art, can be used, and its precondition is that these reagent are realized the object of the invention and obtaining of excellent results of the present invention do not have a negative impact.
The preparation method of heat oxygen aging resistance natural rubber nano composite material of the present invention may further comprise the steps:
100 parts of tree elastomers and nano imvite 1-10 part are carried out mechanical intercalation in two roller mills; Add vulcanization leveller 4-8 part, anti-aging agent 2-4 part, carbon black filler 15-50 part, vulcanization accelerator 1-4 part and vulcanizing agent 0.5-3 part then; Mixingly process natural rubber masterbatch after evenly, deposit more than 16 hours in room temperature, with foaming vulkameter test sulfurizing time; With natural rubber masterbatch with the compression molding agent at 143-153 ℃; Pressure 14-20MPa, sulfurizing time is sulfuration down, obtains ageing-resistant native rubber composite material.
It is strengthening agent that the present invention adopts organic nano imvite and carbon black; The acquisition tensile strength is that 27.8MPa, elongation at break are 478% tree elastomer; These goods have heatproof air aging performance, and the tensile strength behind 100 ℃ of thermal ageing 60h is that 20.9MPa, elongation at break are 447%.
Embodiment
Embodiment 1
A kind of ageing-resistant tree elastomer goods, its composition consists of by weight: 100 parts of tree elastomers, 2 parts of organo montmorillonites; 40 parts of carbon blacks, 0.8 part of vulkacit D, 0.8 part of 2-benzothiazolyl mercaptan; 0.2 part of tetramethyl-thiuram disulfide, 5 parts in zinc oxide, 1 part of Triple Pressed Stearic Acid; 1 part in sulphur, 3 parts of N-phenyl-N '-sec.-propyl Ursol D.
Its step of preparation process is following:
(1) with two roller mills roller is plasticated, wrapped to the tree elastomer raw material on rubber mixing machine;
(2) with the mechanical intercalation of organo montmorillonite adding carrying out;
(3) add above-mentioned vulcanization leveller, anti-aging agent, carbon black respectively, treat that material feeding finishes after, add vulcanization accelerator, vulcanizing agent gradually, mixingly process natural master batch after evenly;
(4) after room temperature is deposited 16 hours; Test the concrete sulfurizing time that obtains with foaming vulkameter test sulfurizing time; With sizing material with the compression molding agent at 143 ℃, pressure 14MPa, sulfurizing time be sulfuration down; Obtain ageing-resistant tree elastomer (tensile strength is that 25.2MPa, elongation at break are 486%), the tensile strength behind 100 ℃ of thermal ageing 60h is that 18.5MPa, elongation at break are 467%.
Embodiment 2
A kind of ageing-resistant tree elastomer goods, its composition consists of by weight: 100 parts of tree elastomers, 2 parts of organo montmorillonites, 40 parts of carbon blacks; 1.5 parts of N cyclohexyl 2 benzothiazole sulfenamides; Tetramethyl-thiuram disulfide 0.2,5 parts in zinc oxide, 1 part of Triple Pressed Stearic Acid; 1 part in sulphur, 2 parts of N-phenyl-N '-sec.-propyl Ursol D.
Its step of preparation process is following:
(1) with two roller mills roller is plasticated, wrapped to the tree elastomer raw material on rubber mixing machine;
(2) with the mechanical intercalation of organo montmorillonite adding carrying out;
(3) add vulcanization leveller, anti-aging agent, carbon black respectively, treat that material feeding finishes after, add vulcanization accelerator, vulcanizing agent gradually, mixingly process natural master batch after evenly;
(4) after room temperature is deposited 16 hours; With foaming vulkameter test sulfurizing time; With sizing material with the compression molding agent at 143 ℃, pressure 14MPa, sulfurizing time be sulfuration down; Obtain ageing-resistant tree elastomer (tensile strength is that 27.8MPa, elongation at break are 478%), the tensile strength behind 100 ℃ of thermal ageing 60h is that 20.9MPa, elongation at break are 447%.And the tensile strength of tree elastomer behind 100 ℃ of thermal ageing 60h of not adding organo montmorillonite is 12.8MPa, elongation at break is 165%
Embodiment 3
A kind of ageing-resistant tree elastomer goods, its composition consists of by weight: tree elastomer 100g, 2 parts of organo montmorillonites, 40 parts of carbon blacks; 0.8 part of vulkacit D, 0.8 part of 2-benzothiazolyl mercaptan, tetramethyl-thiuram disulfide 0.2,5 parts in zinc oxide; 1 part of Triple Pressed Stearic Acid, 1 part in sulphur, 2,2; 4-trimethylammonium-1,2 parts of 2-dihyaroquinoline polymers, 1 part of N cyclohexyl-N '-diphenyl-para-phenylene diamine
Its step of preparation process is following:
(1) with two roller mills roller is plasticated, wrapped to the tree elastomer raw material on rubber mixing machine;
(2) with the mechanical intercalation of organo montmorillonite adding carrying out;
(3) add vulcanization accelerator, anti-aging agent, carbon black respectively, treat that material feeding finishes after, add vulcanization accelerator, vulcanizing agent gradually, mixingly process natural master batch after evenly;
(4) after room temperature is deposited 16 hours; With foaming vulkameter test sulfurizing time; With sizing material with the compression molding agent at 143 ℃, pressure 14MPa, sulfurizing time be sulfuration down; Obtain ageing-resistant tree elastomer (tensile strength is that 25.4MPa, elongation at break are 469%), the tensile strength behind 100 ℃ of thermal ageing 60h is that 20.2MPa, elongation at break are 425%.
Embodiment 4
A kind of ageing-resistant tree elastomer goods, its composition consists of by weight: 100 parts of tree elastomers, 2 parts of organo montmorillonites, 40 parts of carbon blacks; 2 parts of benzothiazyl disulfides, 5 parts in zinc oxide, 1 part of Triple Pressed Stearic Acid, 1 part in sulphur;, 2,2; 4-trimethylammonium-1,2 parts of 2-dihyaroquinoline polymers, 1 part of N cyclohexyl-N '-diphenyl-para-phenylene diamine.
Its step of preparation process is following:
(1) with opening rubber mixing machine roller is plasticated, wrapped to the tree elastomer raw material on rubber mixing machine;
(2) with the mechanical intercalation of organo montmorillonite adding carrying out;
(3) add vulcanization accelerator, anti-aging agent, carbon black respectively, treat that material feeding finishes after, add vulcanization accelerator, vulcanizing agent gradually, mixingly process natural master batch after evenly;
(4) after room temperature is deposited 16 hours; With foaming vulkameter test sulfurizing time; With sizing material with the compression molding agent at 143 ℃, pressure 14MPa, sulfurizing time be sulfuration down; Obtain ageing-resistant tree elastomer (tensile strength is that 23.8MPa, elongation at break are 496%), the tensile strength behind 100 ℃ of thermal ageing 60h is that 18.9MPa, elongation at break are 464%.
Embodiment 5
A kind of ageing-resistant tree elastomer goods, its composition consists of by weight: 100 parts of tree elastomers, 5 parts of organo montmorillonites; 30 parts of carbon blacks,, 1.5 parts of N cyclohexyl 2 benzothiazole sulfenamides; Tetramethyl-thiuram disulfide 0.2,5 parts in zinc oxide, 1 part of Triple Pressed Stearic Acid; 1 part in sulphur, 3 parts of N-phenyl-N '-sec.-propyl Ursol D.
Its step of preparation process is following:
(1) with opening rubber mixing machine roller is plasticated, wrapped to the tree elastomer raw material on rubber mixing machine;
(2) with the mechanical intercalation of organo montmorillonite adding carrying out;
(3) add vulcanization accelerator, anti-aging agent, carbon black respectively, treat that material feeding finishes after, add vulcanization accelerator, vulcanizing agent gradually, mixingly process natural master batch after evenly;
(4) after room temperature is deposited 16 hours; With foaming vulkameter test sulfurizing time; With sizing material with the compression molding agent at 143 ℃, pressure 14MPa, sulfurizing time be sulfuration down; Obtain ageing-resistant tree elastomer (tensile strength is that 25.8MPa, elongation at break are 474%), the tensile strength behind 100 ℃ of thermal ageing 60h is that 20.1MPa, elongation at break are 452%.
Claims (8)
1. heat oxygen aging resistance natural rubber nano composite material, it is characterized in that: in mass fraction, raw material consists of:
2. heat oxygen aging resistance natural rubber nano composite material as claimed in claim 1 is characterized in that: described vulcanizing agent is a sulphur.
3. heat oxygen aging resistance natural rubber nano composite material as claimed in claim 1 is characterized in that: described nano imvite is the nano imvite of alkylamine modification, and the interlamellar spacing after the modification is 1.5-2.4nm.
4. heat oxygen aging resistance natural rubber nano composite material as claimed in claim 1; It is characterized in that: described anti-aging agent is CPPD N cyclohexyl N, N-phenyl-N '-sec.-propyl Ursol D, 2; 2; 4-trimethylammonium-1,2-dihyaroquinoline polymer, BLE, N-PA or 2, at least a in 2 '-methylene radical-two (4-methyl-6-tert butyl phenol).
5. heat oxygen aging resistance natural rubber nano composite material as claimed in claim 1 is characterized in that: described vulcanization leveller is zinc oxide and Triple Pressed Stearic Acid.
6. heat oxygen aging resistance natural rubber nano composite material as claimed in claim 1 is characterized in that: described vulcanization accelerator is at least a in benzothiazyl disulfide, N cyclohexyl 2 benzothiazole sulfenamide, 2-benzothiazolyl mercaptan, vulkacit D or the tetramethyl-thiuram disulfide.
7. heat oxygen aging resistance natural rubber nano composite material as claimed in claim 1 is characterized in that: described sooty size of particles is: the CTAB value is 20-100m
2/ g, the DBP value is 20-100m
3/ g.
8. the preparation method like the arbitrary described heat oxygen aging resistance natural rubber nano composite material of claim 1～7 is characterized in that, may further comprise the steps:
100 parts of tree elastomers and nano imvite 1-10 part are carried out mechanical intercalation in two roller mills; Add vulcanization leveller 4-8 part, anti-aging agent 2-4 part, carbon black filler 15-50 part, vulcanization accelerator 1-4 part and vulcanizing agent 0.5-3 part then; Mixingly process natural rubber masterbatch after evenly; Deposit more than 16 hours in room temperature; With foaming vulkameter test sulfurizing time, natural rubber masterbatch is vulcanized under 143-153 ℃, pressure 14-20MPa, sulfurizing time with the compression molding agent, obtain ageing-resistant native rubber composite material.
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| CN101735493A (en) * | 2010-01-27 | 2010-06-16 | 四川大学 | Fatigue-resisting natural rubber nano composite material and preparation method thereof |
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| CN101735493A (en) * | 2010-01-27 | 2010-06-16 | 四川大学 | Fatigue-resisting natural rubber nano composite material and preparation method thereof |
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| CN110511454A (en) * | 2019-09-12 | 2019-11-29 | 中国热带农业科学院农产品加工研究所 | A kind of ageing-resistant natural rubber and preparation method thereof, ageing-resistant natural rubber vulcanized rubber and preparation method thereof |
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Application publication date: 20120620 |