CN107254107A - A kind of graphene MBI is combined pre-dispersed masterbatch particles and preparation method thereof - Google Patents
A kind of graphene MBI is combined pre-dispersed masterbatch particles and preparation method thereof Download PDFInfo
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- CN107254107A CN107254107A CN201710484526.5A CN201710484526A CN107254107A CN 107254107 A CN107254107 A CN 107254107A CN 201710484526 A CN201710484526 A CN 201710484526A CN 107254107 A CN107254107 A CN 107254107A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/06—Waxes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2309/06—Copolymers with styrene
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- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
- C08J2491/06—Waxes
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
Pre-dispersed masterbatch particles are combined the invention discloses a kind of graphene MBI, its percentage by weight composition is:The mercaptobenzimidazole 15~35% of graphene 55~60%, 2, VTES 1~4%, hexanedioic acid dioctyl ester 1~2%, triphenyl phosphate 1~2%, zinc stearate 1~5%, rubber matrix 7~15%, technical white oil 6~14%, the percentage by weight sum of composition described above is 100%;Rubber matrix is made up of main rubber and processing aid, and main rubber is at least one of ethylene propylene diene rubber, butadiene-styrene rubber, nitrile rubber, ACM and chlorohydrin rubber, and processing aid is paraffin and pentaerythritol stearate;The masterbatch particles contain graphene and MBI both active components, it can effectively solve the problem that the dispersiveness and dust pollution question of graphene and MBI in rubber, when being subsequently used for production vulcanization rubber, the vulcanization of rubber can be promoted, the mechanical property and ageing properties of rubber is improved.
Description
Technical field
The present invention relates to the pre-dispersed granulating technique field of processing aid, specifically a kind of graphene-MBI is combined pre-dispersed mother
Micelle and preparation method thereof.
Background technology
Graphene is a kind of carbon atom tightly packed new carbon for forming bi-dimensional cellular lattice in two dimensional surface.Mesh
Preceding graphene is nano material most thin but most hard in the world, and it is almost fully transparent, only absorbs 2.3% light;It is led
Hot coefficient reaches 5300W/mK, far above diamond and CNT;Under normal temperature, its electron mobility reaches 15000cm2/ Vs,
Far above CNT and silicon crystal;Its resistivity is about 10-6Ω cm, excellent electric conductivity is worked as with some metal phases;It has
High specific surface area, limiting value is up to 2630m2/g.Due to the unique property that graphene is shown, its rubber, nano-device,
There is huge application prospect in the fields such as composite, sensor, lithium battery, hydrogen storage material.
However, graphene is applied to also there is more problem in rubber.Graphene thickness is small, and specific surface area is big, generally with
Multi-layer morphology is present, and not only easily reunites in daily storage process, and it is serious to reunite in rubber mixing process, cause its
It is not can be uniformly dispersed in rubber, rubber quality is adversely affected.Scattered and graphenic surface chemistry, the graphene of graphene
Preparation method with rubber interface relation and composite is in close relations.Graphene is in rubber matrix due between piece and piece
Van der Waals force, with higher agglomeration tendency, therefore dispersed in rubber of graphene is a technical barrier.Separately
Outside, the density of graphene is small, packaging and transport inconvenience, the problem of there is bad dispersibility in use.
2 mercapto benzimidazole (i.e. MBI) is a kind of rubber antioxidant, can effectively prevent copper from doing harm to and overcoming over cure
Caused ill-effect, it has retarding action to accelerator such as TMTD, produces cooperative effect with amine, phenolic antioxidant, often
For electric wire, cable and transparent light color article, it is also possible to make polyethylene, polyacrylic heat stabilizer.It is faint yellow under MBI normal temperature
Or white powder, its density 1.42g/cm3, 290 DEG C of just fusing point.MBI has bitter taste, dissolves in ethanol, is insoluble in dichloromethane, no
It is dissolved in carbon tetrachloride and water.MBI is applied to the presence of bitter taste after dust from flying and pollution problem, suction during rubber production, influences work
People's health, and disperse uneven in rubber.
Therefore, for graphene and MBI dispersiveness the problems such as, it is pre-dispersed that the present invention proposes that a kind of graphene-MBI is combined
Masterbatch particles and preparation method thereof.
The content of the invention
The technical problems to be solved by the invention are:It is compound there is provided a kind of graphene-MBI in view of the shortcomings of the prior art
Pre-dispersed masterbatch particles and preparation method thereof, the pre-dispersed masterbatch particles contain graphene and MBI both active components, can be effective
The dispersion problem of graphene and MBI in rubber are solved, the curability and mechanical property of rubber size is improved.
The present invention solve the technical scheme that is used of above-mentioned technical problem for:A kind of graphene-MBI is combined pre-dispersed rubber master batch
Grain, its percentage by weight, which is constituted, is:Graphene 55~60%, 2-mercaptobenzimidazole 15~35%, vinyl triethoxyl silicon
Alkane 1~4%, hexanedioic acid dioctyl ester 1~2%, triphenyl phosphate 1~2%, zinc stearate 1~5%, rubber matrix 7~15%,
Technical white oil 6~14%, the percentage by weight sum of composition described above is 100%;Described rubber matrix is by main rubber and adds
Work auxiliary agent is constituted, and described main rubber is ethylene propylene diene rubber, butadiene-styrene rubber, nitrile rubber, ACM and chloropharin
At least one of rubber, described processing aid is paraffin and pentaerythritol stearate.
Preferably, a kind of graphene-MBI is combined pre-dispersed masterbatch particles, described main rubber, described paraffin and institute
The weight ratio for the pentaerythritol stearate stated is 4:1:1.
Preferably, a kind of graphene-MBI is combined pre-dispersed masterbatch particles, its percentage by weight composition is:Graphene
55%, 2-mercaptobenzimidazole 22%, VTES 3%, hexanedioic acid dioctyl ester 2%, triphenyl phosphate 1%,
Zinc stearate 2%, rubber matrix 8%, technical white oil 7%.
The preparation method that above-mentioned graphene-MBI is combined pre-dispersed masterbatch particles comprises the following steps:
(1) weighed according to proportion speed and prepare each raw material needed for masterbatch particles;
(2) processing aid is divided into three parts;Main rubber is put into banbury afterwards, kneaded 1~3 minute;Then
The processing aid of addition 1/3 into banbury, is kneaded 2~5 minutes;Again into banbury add 1/3 processing aid, mixing extremely
Temperature in banbury rises to 80~90 DEG C, adds remaining 1/3 processing aid, and mixing to the temperature in banbury rises to 80
~90 DEG C, dumping obtains rubber matrix sizing material;By rubber matrix sizing material, normal temperature leads glue bottom sheet thin logical three times on a mill, stops
Put stand-by;
(3) the rubber matrix sizing material obtained in graphene and step (2) is divided into three parts respectively;Banbury is heated to
80~90 DEG C, put into first in banbury 1/3 rubber matrix sizing material and 1/3 graphene, with stirring for 120~160r/min
Mix speed to stir 1~3 minute, then put into 1/3 graphene and 2-mercaptobenzimidazole, with 120~160r/min stirring speed
Degree is stirred 1~3 minute, 1/3 rubber matrix sizing material, 1/3 graphene and zinc stearate is then put into, with 150~180r/
Min mixing speed is stirred 2~3 minutes, finally puts into 1/3 rubber matrix sizing material, VTES, hexanedioic acid
Dioctyl ester, triphenyl phosphate and technical white oil, are stirred 2~6 minutes with 120~150r/min mixing speed, mix each raw material
Close uniform, in 85~90 DEG C of temperature bottom discharges, obtain sizing material;
(4) control main frame given rotating speed is 80~100r/min, by the sizing material feeding obtained in step (3) to extruder,
Pelletizing is extruded after the strainer filtering of 100 mesh, graphene-MBI is finally given and is combined pre-dispersed masterbatch particles.
Compared with prior art, the advantage of the invention is that:
1st, in pre-dispersed masterbatch particles of the invention containing graphene and 2 mercapto benzimidazole (i.e. MBI) both it is active into
Point, with collaboration facilitation, when being subsequently used for production vulcanization rubber, the vulcanization of rubber can be promoted, the mechanical property of rubber is improved
Energy and ageing properties;
2nd, VTES and zinc stearate play rush peptizaiton, reduce graphene and MBI in matrix rubber
Reunion, caking phenomenon in glue, improve the dispersiveness of graphene and MBI in masterbatch particles, graphene and MBI is subsequently being vulcanized
Obtained in rubber dispersed, it is ensured that the quality of vulcanized rubber article;
3rd, hexanedioic acid dioctyl ester and triphenyl phosphate play collaboration plasticization, the plasticity of masterbatch particles glue are improved, so as to change
Kind glue mobility, it is ensured that the extruding pelletization effect of masterbatch particles, makes masterbatch particles color, size consistent;
4th, pre-dispersed masterbatch particles of the invention are easy to preserve, transport and weigh, and can effectively improve graphene and MBI in vulcanization rubber
Utilization rate in glue, reduces cost, and solve dust pollution question;
5th, preparation method of the present invention is workable, is adapted to scale industrial production;Obtained graphene-MBI is compound pre-
Scattered masterbatch particles have relatively low Mooney viscosity, can retain graphene and MBI original activity, make black alkene and MBI in masterbatch particles
In obtain dispersed.
Brief description of the drawings
Fig. 1 is the TEM photos (10000 ×) of graphene used in embodiment one;
Fig. 2 is combined the TEM photos of the ultrathin section sample, of pre-dispersed masterbatch particles for the graphene-MBI of embodiment one
(20000×)。
Embodiment
The present invention is described in further detail with reference to embodiments.
Graphene-the MBI of embodiment one is combined pre-dispersed masterbatch particles, and its percentage by weight composition is:Graphene 55%, 2-
Mercaptobenzimidazole 22%, VTES 3%, hexanedioic acid dioctyl ester 2%, triphenyl phosphate 1%, zinc stearate
2%, rubber matrix 8%, technical white oil 7%, the percentage by weight sum of composition described above is 100%;Rubber matrix is by main body rubber
Glue and processing aid composition, main rubber are ethylene propylene diene rubber, and processing aid is paraffin and pentaerythritol stearate, main body
The weight ratio of rubber, paraffin and pentaerythritol stearate is 4:1:1.
Graphene-the MBI of embodiment two is combined pre-dispersed masterbatch particles, and its percentage by weight composition is:Graphene 57%, 2-
Mercaptobenzimidazole 24%, VTES 1%, hexanedioic acid dioctyl ester 1%, triphenyl phosphate 1%, zinc stearate
1%, rubber matrix 7%, technical white oil 8%;Rubber matrix is made up of main rubber and processing aid, and main rubber is ternary second
Third rubber and ACM, processing aid are paraffin and pentaerythritol stearate.
Graphene-the MBI of embodiment three is combined pre-dispersed masterbatch particles, and its percentage by weight composition is:Graphene 60%, 2-
Mercaptobenzimidazole 15%, VTES 1%, hexanedioic acid dioctyl ester 1%, triphenyl phosphate 1%, zinc stearate
3%, rubber matrix 10%, technical white oil 9%;Rubber matrix is made up of main rubber and processing aid, and main rubber is propylene
Acid esters rubber and chlorohydrin rubber, processing aid are paraffin and pentaerythritol stearate.
The preparation method that graphene-MBI listed by above-described embodiment is combined pre-dispersed masterbatch particles comprises the following steps:
(1) weighed according to proportion speed and prepare each raw material needed for masterbatch particles;
(2) processing aid is divided into three parts;Main rubber is put into banbury afterwards, kneaded 2 minutes;Then to close
The processing aid of addition 1/3 in mill, is kneaded 2 minutes;Added again into banbury 1/3 processing aid, mixing is to banbury
Interior temperature rises to 85 DEG C, adds remaining 1/3 processing aid, and mixing rises to 85 DEG C to the temperature in banbury, and dumping is obtained
To rubber matrix sizing material;By rubber matrix sizing material, normal temperature leads glue bottom sheet thin logical three times on a mill, parks stand-by;
(3) the rubber matrix sizing material obtained in graphene and step (2) is divided into three parts respectively;Banbury is heated to
80 DEG C, put into first in banbury 1/3 rubber matrix sizing material and 1/3 graphene, stirred with 130r/min mixing speed
Mix 2 minutes, then put into 1/3 graphene and 2-mercaptobenzimidazole, stir 2 minutes with 130r/min mixing speed, then
Rubber matrix sizing material, 1/3 graphene and zinc stearate of input 1/3, are stirred 2~3 minutes with 160r/min mixing speed,
Finally the rubber matrix sizing material of input 1/3, VTES, hexanedioic acid dioctyl ester, triphenyl phosphate and industry are white
Oil, is stirred 4 minutes with 120r/min mixing speed, is well mixed each raw material, in 90 DEG C of temperature bottom discharges, is obtained sizing material;
(4) control main frame given rotating speed is 80r/min, by the sizing material feeding obtained in step (3) to extruder, through 100
Pelletizing is extruded after purpose strainer filtering, graphene-MBI is finally given and is combined pre-dispersed masterbatch particles.
After testing, the graphene-MBI of embodiment one, embodiment two and embodiment three is combined pre-dispersed 50 DEG C of masterbatch particles
Mooney viscosity ML (1+4) is respectively 52.6,52.1 and 53.3.
By taking embodiment one as an example, the TEM photos of its graphene used are shown in Fig. 1, and as seen from Figure 1, graphene is with sandwich construction
State is present, lamella size is larger and lamella between have overlap joint phenomenon.Graphene-the MBI of embodiment one is combined pre-dispersed rubber master batch
The TEM photos of ultrathin section sample, of grain are shown in Fig. 2, from Figure 2 it can be seen that graphene uniform be scattered in graphene-MBI be combined it is pre-dispersed
In masterbatch particles, lamella is relatively thin.
Using the masterbatch particles of embodiment one and graphene used as raw material, it is added in butadiene-styrene rubber, is formulated as sulphur
Change butadiene-styrene rubber, formula is shown in Table one, wherein the content of the graphene added in masterbatch particles form is the content after conversion.Wherein 1#
Vulcanize the graphene in butadiene-styrene rubber to add in the former powder form of graphene, the graphene in 2# vulcanization butadiene-styrene rubber is with embodiment one
Masterbatch particles form add.Vulcanization butadiene-styrene rubber preparation technology be:To add after SBR inputs mill 1min small powder (ZnO,
SA, TBBS), mix and graphene or the masterbatch particles of embodiment one are added after 1min, mix thin after 3min after vulcanization sulphurs, mixing 1min
Logical bottom sheet, whole mixing cycle about 9min;Elastomeric compound after parking is true according to vulcameter on 160 DEG C of vulcanizing press
Fixed sulfurizing time is vulcanized.
The 1# of table one vulcanizes butadiene-styrene rubber and 2# vulcanizes the formula (unit of butadiene-styrene rubber:phr)
1# vulcanizes butadiene-styrene rubber and the mechanical property of 2# vulcanization butadiene-styrene rubber is shown in Table two.
The 1# of table two vulcanizes butadiene-styrene rubber and 2# vulcanizes the mechanical property of butadiene-styrene rubber
Project | 1# | 2# |
Shao Er A type hardness testers/A | 42 | 45 |
100% stress at definite elongation/MPa | 0.69 | 0.92 |
300% stress at definite elongation/MPa | 1.09 | 1.57 |
Reinforcement coefficient | 1.58 | 1.70 |
Tensile strength/MPa | 1.6 | 2.36 |
Elongation rate of tensile failure/% | 519 | 530 |
Tearing strength/kNm-1 | 9.79 | 13.59 |
From table two, add graphene-MBI of the present invention and be combined after pre-dispersed masterbatch particles, vulcanize the mechanics of butadiene-styrene rubber
Performance is significantly improved and enhanced, and graphene-MBI of the present invention is combined the power that pre-dispersed masterbatch particles are conducive to improving butadiene-styrene rubber
Learn performance.
Claims (4)
1. a kind of graphene-MBI is combined pre-dispersed masterbatch particles, it is characterised in that its percentage by weight, which is constituted, is:Graphene 55~
60%, 2-mercaptobenzimidazole 15~35%, VTES 1~4%, hexanedioic acid dioctyl ester 1~2%, phosphoric acid triphen
Ester 1~2%, zinc stearate 1~5%, rubber matrix 7~15%, technical white oil 6~14%, the percentage by weight sum of composition described above
For 100%;Described rubber matrix is made up of main rubber and processing aid, and described main rubber is ethylene propylene diene rubber, fourth
At least one of benzene rubber, nitrile rubber, ACM and chlorohydrin rubber, described processing aid are paraffin and season penta
Tetrol stearate.
2. a kind of graphene-MBI according to claim 1 is combined pre-dispersed masterbatch particles, it is characterised in that described main body
The weight ratio of rubber, described paraffin and described pentaerythritol stearate is 4:1:1.
3. a kind of graphene-MBI according to claim 1 is combined pre-dispersed masterbatch particles, it is characterised in that its weight percent
It is than composition:Graphene 55%, 2-mercaptobenzimidazole 22%, VTES 3%, hexanedioic acid dioctyl ester 2%, phosphoric acid
Triphenylmethyl methacrylate 1%, zinc stearate 2%, rubber matrix 8%, technical white oil 7%.
4. graphene-the MBI any one of claim 1-3 is combined the preparation method of pre-dispersed masterbatch particles, its feature exists
In comprising the following steps:
(1)Weighed according to proportion speed and prepare each raw material needed for masterbatch particles;
(2)Processing aid is divided into three parts;Main rubber is put into banbury afterwards, kneaded 1~3 minute;Then to close
The processing aid of addition 1/3 in mill, is kneaded 2~5 minutes;Added again into banbury 1/3 processing aid, mixing is to banburying
Temperature in machine rises to 80~90 DEG C, adds remaining 1/3 processing aid, and mixing to the temperature in banbury rises to 80~
90 DEG C, dumping obtains rubber matrix sizing material;By rubber matrix sizing material, normal temperature leads glue bottom sheet thin logical three times on a mill, parks
It is stand-by;
(3)By graphene and step(2)In obtained rubber matrix sizing material be divided into three parts respectively;Banbury is heated to 80~
90 DEG C, put into first in banbury 1/3 rubber matrix sizing material and 1/3 graphene, with 120~160 r/min stirring
Speed is stirred 1~3 minute, then puts into 1/3 graphene and 2-mercaptobenzimidazole, with 120~160 r/min mixing speed
Stir 1~3 minute, 1/3 rubber matrix sizing material, 1/3 graphene and zinc stearate is then put into, with 150~180 r/min
Mixing speed stir 2~3 minutes, finally put into 1/3 rubber matrix sizing material, VTES, hexanedioic acid two
Monooctyl ester, triphenyl phosphate and technical white oil, are stirred 2~6 minutes with 120~150 r/min mixing speed, mix each raw material
Uniformly, in 85~90 DEG C of temperature bottom discharges, sizing material is obtained;
(4)Control main frame given rotating speed is 80~100 r/min, by step(3)In obtained sizing material feeding to extruder, warp
Pelletizing is extruded after the strainer filtering of 100 mesh, graphene-MBI is finally given and is combined pre-dispersed masterbatch particles.
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CN109096562A (en) * | 2018-08-20 | 2018-12-28 | 江苏飞亚化学工业有限责任公司 | A kind of anti-oxidant predispersed masterbatch of liquid |
CN109180968A (en) * | 2018-08-20 | 2019-01-11 | 江苏飞亚化学工业有限责任公司 | A kind of preparation method of the anti-oxidant predispersed masterbatch of liquid |
CN110509448A (en) * | 2018-05-22 | 2019-11-29 | 邹先云 | The production equipment and its production procedure of a kind of graininess basis glue |
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CN104910526A (en) * | 2015-06-08 | 2015-09-16 | 宁波硫华聚合物有限公司 | MBT (2-mercaptobenzthiazole) predispersion master batch and preparation method thereof |
CN106117935A (en) * | 2016-07-01 | 2016-11-16 | 宁波硫华聚合物有限公司 | Pre-dispersed masterbatch particles of Graphene and its preparation method and application |
CN106496884A (en) * | 2016-10-19 | 2017-03-15 | 钟光 | A kind of carbon functional nano-composites and preparation method thereof |
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CN104910526A (en) * | 2015-06-08 | 2015-09-16 | 宁波硫华聚合物有限公司 | MBT (2-mercaptobenzthiazole) predispersion master batch and preparation method thereof |
CN106117935A (en) * | 2016-07-01 | 2016-11-16 | 宁波硫华聚合物有限公司 | Pre-dispersed masterbatch particles of Graphene and its preparation method and application |
CN106496884A (en) * | 2016-10-19 | 2017-03-15 | 钟光 | A kind of carbon functional nano-composites and preparation method thereof |
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CN110509448A (en) * | 2018-05-22 | 2019-11-29 | 邹先云 | The production equipment and its production procedure of a kind of graininess basis glue |
CN109096562A (en) * | 2018-08-20 | 2018-12-28 | 江苏飞亚化学工业有限责任公司 | A kind of anti-oxidant predispersed masterbatch of liquid |
CN109180968A (en) * | 2018-08-20 | 2019-01-11 | 江苏飞亚化学工业有限责任公司 | A kind of preparation method of the anti-oxidant predispersed masterbatch of liquid |
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