CN103819760A - Process method for preparing high-performance carbon black masterbatch - Google Patents
Process method for preparing high-performance carbon black masterbatch Download PDFInfo
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- CN103819760A CN103819760A CN201410101669.XA CN201410101669A CN103819760A CN 103819760 A CN103819760 A CN 103819760A CN 201410101669 A CN201410101669 A CN 201410101669A CN 103819760 A CN103819760 A CN 103819760A
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Abstract
The invention provides a process method for preparing high-performance carbon black masterbatch, relating to the technical field of carbon black masterbatch preparation processes. The wet-method carbon black masterbatch preparation process method provided by the invention is simple in process, low in energy consumption and excellent in performance. The method comprises the steps: soaking non-granulated carbon black powder in an aqueous solution of a micromolecular volatile solvent, so as to prepare uniformly-dispersed carbon black slurry; flocculating out masterbatch and carbon black at a certain stirring linear speed without adding other flocculating agents, filtrating and drying. The carbon black in the masterbatch prepared by the method disclosed by the invention reaches nano dispersion, vulcanized rubber has the advantages of excellent mechanical property, good resilience, low heat generation and high wear resistance, the preparation process is simple, the equipment investment is small, the energy consumption is low, the cost is low, the method is environmental-friendly, and the influence on the performance of the rubber and the pollution to the environment, caused by a surfactant, a flocculating agent and the like, are avoided.
Description
Technical field
The present invention relates to the fabricating technology field of carbon black rubber master batch, concrete is to utilize wet method to prepare the processing method of carbon black rubber master batch.
Background technology
So far carbon black remains irreplaceable strengthening agent in rubber industry, and its outstanding other strengthening agent of comprehensive reinforcing property still cannot reach.The normal dry process carbon black rubber master batch that uses in industrial production, some shortcomings of the mixing existence of dry method, for example: the dispersion of carbon black is bad, utilization ratio is low and when mixing, easily make rubber molecule splitting of chain serious, has both caused refining, and this performance on rubber has serious impact.
In view of the shortcoming being dry mixed, people attempt to prepare rubber master batch by wet-mixed and overcome these shortcomings.Wet-mixed generally comprises spray-drying process, emulsion flocculence etc.Spray-drying process is mainly that carbon black, zinc oxide, stearic acid, sulphur, promotor etc. are made into carbon black suspension by a certain percentage, then join natural rubber latex, after stirring, use spray-drier that the mixed solution of preparation is passed through to spraying gun atomization, droplet is removed moisture through moisture eliminator again and is obtained dry carbon black rubber master batch.The advantage of this technique is that he can produce continuously, but energy consumption is large, equipment complexity, and bad control, cost is higher.Also can there is adverse influence to the performance of rubber in tensio-active agent and the emulsifying agent etc. adding in slurries preparation process in addition, also easily cause environmental pollution.It is fairly simple that emulsion flocculence is prepared rubber master batch technique, the P(NR/CB that the Zhang Anqiang of South China Science & Engineering University utilizes flocculence to prepare) excellent performance, its preparation method is: first use dispersion agent by carbon black dispersion in water, prevent carbon black reunion, use resin to be coated the carbon black disperseing, obtain like this carbon black of stable dispersion, then carbon black slurry is mixed with natural rubber latex, finally add flocculation agent to make the uniform natural rubber latex co-coagulation of carbon black dispersion out.This processing method still cannot be avoided the use of dispersion agent, flocculation agent, seriously polluted, and technique is still very loaded down with trivial details, and energy consumption is large, cost is high, industrialization difficulty.CEC rubber master batch prepared by Cabot company puts into production, and this production method is to utilize colloidal mill carbon black to be worn in water to uniform carbon black slurry, and the mechanical shearing effect that slurry stream and emulsion flow correlation produce realizes mixing and flocculation of carbon black and latex.This technological effect is good, but equipment complexity, and the method bought out, on market, cannot buy.
It is carbon black slurry preparation that wet method is prepared carbon black rubber master batch technology key, now most ofly carbon black pellet is utilized to Mechanical Crushing is for example ground, the preparation carbon black slurry such as ultrasonic, consume energy so high, the final fineness of dispersion of carbon black of preparation is larger, cause the dispersion effect of carbon black poor, performance is bad.
Summary of the invention
The invention provides a kind of a kind of method addressing the above problem, is mainly to utilize the carbon black of not granulation to be dissolved in the aqueous solution, is then uniformly mixed autoflocculation with natural rubber latex and goes out.Rubber master batch prepared by the method has been given full play to the strengthening action of carbon black, mechanical property excellence, and facility investment is few, and energy consumption is low, and cost is little, and does not add any tensio-active agent, and acid or salt flocculation agent are a kind of methods of environmental protection.
In order to solve the technical problem of above-mentioned existence, the present invention has adopted following proposal:
1. select the solution immersion carbon black powder of small molecules easy volatile solvent to prepare finely dispersed carbon black slurry, the mass percent 2.5%～10% of carbon black slurry; Add carbon black slurry to stir 20-60min at 100～300m/min after rotating speed 10～40m/min stirs 10～30min latex, latex and carbon black are wadded a quilt with cotton out, filter, dry; Described small molecules easy volatile solvent is methyl alcohol, ethanol, propyl alcohol, tetrahydrofuran (THF), acetone, butanone, or their mixture; Take dry glue quality in latex as 100 parts, the add-on of carbon black is at 30 parts～80 parts; Treating compound adds 10 parts～300 parts.
2. as preferred: preferably ethanol of the volatile carbon black treating compound of small molecules;
3 as preferred: latex is fresh natural emulsion or concentrated natural latex, styrene-butadiene latex, nitrile rubber, neoprene latex, fourth pyrrole and butylbenzene pyrrole latex, and above mixed latex;
4 as preferred: when the mass percent concentration of latex is 5%～40%, the mobility of latex is better easily disperseed;
While utilizing granulation carbon black to prepare carbon black slurry, carbon black is difficult for fragmentation, be difficult to prepare homodisperse carbon black slurry, and energy consumption is high.This technology utilization carbon black powder is prepared carbon black slurry, select the aqueous solution of small molecules easy volatile solvent to do treating compound, the surface that treating compound has reduced between the particle of carbon black can, the surface tension of carbon black is reduced, therefore speed soluble in water is accelerated, the reunion degree of carbon black is weakened, dispersiveness in water improves the carbon black dissolving in pure water as seen from Figure 1 and assembles closely, do not see the form of spheroidal particle completely, the arrangement of dissolving in ethanol is more loose, ball-type particle is obvious and particle is less, the carbon black particle dissolving in tetrahydrofuran (THF) is arranged also more loose, but particle is larger, visible treating compound has significantly reduced the self aggregation degree of carbon black, improve to a certain extent the dispersiveness of carbon black, when adding after latex, because having dehydration, treating compound goes steady demulsification on the one hand, carbon black has pair latex to have strong adsorption that rubber latex is gone surely on the other hand, originally arrange loose carbon black particle, under the power that pulls and mechanical shear stress effect carbon black being produced due to adsorption at rubber molecular chain, absorption one deck rubber molecular chain of surface uniform, form little rubber coated carbon black fine particle, further strengthen mechanical shear stress, collision mutually between rubber coated carbon black fine particle, be bonded together, finally form the carbon black rubber master batch that carbon black becomes nano-dispersed, after leaching, the treating compound remaining in when oven dry in rubber master batch can be removed due to volatile, have like this and got rid of the impact for the treatment of compound on rubber performance.Fig. 2 is the scatter diagram of carbon black in black rubber rubber master batch of wadding a quilt with cotton out, and the carbon black pellet size in rubber master batch is at 80～100nm as seen from the figure, and this is the high structural original size of carbon black N234, and is evenly distributed.Sulfuration after carbon black significantly do not reassociate phenomenon (as Fig. 4,5) therefore mechanical property improve greatly.
Beneficial effect of the present invention:
1, the present invention uses volatile small molecule solvent to do treating compound, has discharged the impact on rubber performance that adds of other materials, and has improved solvability and the dispersiveness of carbon black in water.
2, the present invention utilizes treating compound to destroy the stability of latex, less mechanical shear stress has been realized the mixing of dispersion, carbon black slurry and the natural rubber latex slurries of carbon black in water, and thereby larger shearing force has realized carbon black and the flocculation of latex sharp impacts, greatly simplify technological process, discharged the impact of flocculation agent on rubber performance and environment.
3, technique involved in the present invention is simple, energy consumption is few, security is good, reduced tooling cost, is applicable to industrial production.
Accompanying drawing explanation:
Fig. 1, different solvents soaked the accumulation shape comparison diagram of carbon black pellet, wherein carbon black respectively in (1) water, the microscopic pattern figure of molten mistake in (2) ethanol, (3) tetrahydrofuran (THF).
Carbon black dispersion SEM figure in Fig. 2, wadding plastic emitting, wherein (1) is the surface topography of rubber particles of wadding a quilt with cotton out, (2) are the partial enlarged drawings of (1); (3) be the sectional elevation of particle of wadding a quilt with cotton out, (4) are the partial enlarged drawings of (3).
Fig. 3, process flow sheet
The atomic force microscope modulus figure of Fig. 4, example 1
The atomic force microscope modulus figure of Fig. 5, example 2
The atomic force microscope modulus figure of Fig. 6, example 3
The atomic force microscope modulus figure of Fig. 7, comparison example 1
Embodiment
Embodiment 1:
Take dry glue quality in natural emulsion as 100 parts, 50phr carbon black powder (N234) is joined in the aqueous solution containing 10phr ethanol, quality percentage composition is 2.5% carbon black slurry, stir 20min, natural emulsion is diluted to 40%(quality percentage composition, below without special instruction percentage composition be quality percentage composition) after join in carbon black slurry, rotating speed 40m/min stir 10min by rotating speed be adjusted to 300m/min stir 40min, the rubber master batch of wadding a quilt with cotton out is taken out, dry.Above-mentioned rubber master batch is containing glue 100phr, ZnO5phr, stearic acid 2phr, anti-aging agent 1010NA1phr, accelerant CZ 1.2phr, sulphur 2phr, and refining glue is surveyed vulcanization curve and Rubber processing performance after parking 8h, and sulfuration at 143 ℃, surveys mechanical property.
Embodiment 2:
Take dry glue quality in natural emulsion as 100 parts, 50phr carbon black powder (N234) is added in the aqueous solution containing 50phr ethanol, the carbon black slurry that quality percentage composition processed is 5%, stir 20min, after being diluted to 30%, natural emulsion (wherein dry glue is 100 parts) joins in carbon black slurry, stir 20min at rotating speed 20m/min rotating-speed modulation 200m/min is stirred to 50min, the rubber of wadding a quilt with cotton out is taken out, all the other steps are as embodiment 1.
Embodiment 3:
Take dry glue quality in natural emulsion as 100 parts, 50phr carbon black powder (N234) is joined in the aqueous solution containing 150phr ethanol, the carbon black slurry that quality percentage composition processed is 7%, stir 20min, after being diluted to 25%, natural emulsion (wherein dry glue is 100 parts) joins in carbon black slurry, stir 30min at rotating speed 10m/min rotating-speed modulation 300m/min is stirred to 30min, the rubber of wadding a quilt with cotton out is taken out, all the other steps are as embodiment 1.
Embodiment 4:
Take dry glue quality in natural gum glue gel resin as 100 parts, 50phr carbon black powder (N234) is joined in the aqueous solution containing 50phr ethanol, the carbon black slurry that quality percentage composition processed is 10%, stir 20min, by natural gum glue gel resin (molecular weight, quality percentage composition are 5%) wherein dry glue be 100 parts, join in carbon black slurry, rotating speed 20m/min stir 20min by rotating-speed modulation 100m/min stir 60min, the rubber of wadding a quilt with cotton out is taken out, and all the other steps are as embodiment 1.
Embodiment 5:
Take dry glue quality in natural emulsion as 100 parts, 50phr carbon black powder (N234) is joined in the aqueous solution containing 25phr tetrahydrofuran (THF), the carbon black slurry that quality percentage composition processed is 5%, stir 20min, fresh natural rubber latex (wherein dry glue is 100 parts) is joined in carbon black slurry, stir 10min at rotating speed 30m/min rotating-speed modulation 200m/min is stirred to 40min, the rubber of wadding a quilt with cotton out is taken out, all the other steps are as embodiment 1.
Comparative example 1:
On two rollers are begun to pratise machine by formula: natural gum (No. 1, cloud mark) 100phr, carbon black (N234) 50phr, all the other Synergist S-421 95s are as embodiment 1, and all the other steps are as embodiment 1.
Embodiment 6
Take dry glue quality in natural emulsion as 100 parts, (30phr) carbon black powder (N234) is joined in the aqueous solution containing 50phr acetone, the carbon black slurry that quality percentage composition processed is 5%, stir 20min, after being diluted to 40%, natural rubber latex (wherein dry glue is 100 parts) joins in carbon black slurry, stir 10min at rotating speed 30m/min rotating-speed modulation 100m/min is stirred to 30min, the rubber of wadding a quilt with cotton out is taken out, all the other steps are as embodiment 1.
Comparative example 2:
On two rollers are begun to pratise machine by formula: natural gum (No. 1, cloud mark) 100phr, carbon black (N234) 30phr, all the other Synergist S-421 95s are as embodiment 1, and all the other steps are as embodiment 1.
Take dry glue quality in natural emulsion as 100 parts, (80phr) carbon black powder (N330) is joined in the aqueous solution containing 50phr methyl alcohol, the carbon black slurry that quality percentage composition processed is 5%, stir 20min, after being diluted to 40%, natural rubber latex (wherein dry glue is 100 parts) joins in carbon black slurry, stir 10min at rotating speed 30m/min rotating-speed modulation 100m/min is stirred to 30min, the rubber of wadding a quilt with cotton out is taken out, all the other steps are as embodiment 1.
Comparative example 3:
On two rollers are begun to pratise machine by formula: natural gum (No. 1, cloud mark) 100phr, carbon black (N330) 80phr, all the other Synergist S-421 95s are as embodiment 1, and all the other steps are as embodiment 1.
Embodiment 8
Take dry glue in latex (being following butadiene-styrene latex (1502)) as 100 parts, (50phr) carbon black powder (N330) is joined in the aqueous solution of 50phr ethanol, the carbon black slurry slurries that quality percentage composition processed is 5%, stir 20min, by butadiene-styrene latex (1502) mass percentage content be 18%(wherein dry glue be 100 parts) join in carbon black slurry, stir 10min at rotating speed 30m/min rotating-speed modulation 100m/min is stirred to 30min, the rubber of wadding a quilt with cotton out is taken out, and all the other steps are as embodiment 1.
Comparative example 4:
On two rollers are begun to pratise machine by formula: breast poly-butadiene-styrene rubber (1502) 100phr, carbon black (N330) 50phr, all the other Synergist S-421 95s are as embodiment 1, all the other steps are as embodiment 1.
Embodiment 9
Take dry glue in latex (being following butyronitrile latex) as 100 parts, (50phr) carbon black powder (N220) is joined in the aqueous solution containing 50phr ethanol, the carbon black slurry that quality percentage composition processed is 5%, stir 20min, by butyronitrile latex mass percentage content be 25%(wherein dry glue be 100 parts) join in carbon black slurry, stir 10min at rotating speed 30m/min rotating-speed modulation 100m/min is stirred to 30min, the rubber of wadding a quilt with cotton out is taken out, all the other steps are as embodiment 1.
Comparative example 5:
On two rollers are begun to pratise machine by formula: butadiene-acrylonitrile rubber 100phr, carbon black (N220) 50phr, all the other Synergist S-421 95s are as embodiment 1, all the other steps are as embodiment 1.
Embodiment 10
Take dry glue in latex (being the following natural emulsion mixing and butadiene-styrene latex) as 100 parts, (50phr) carbon black powder (N234) is added in the aqueous solution containing 50phr ethanol, the carbon black slurry slurries that quality percentage composition processed is 5%, stir 20min, amount to dry glue each 50phr the natural emulsion mixing and butadiene-styrene latex, the mass percentage content of mixed latex is 28% to join in carbon black slurry, rotating speed 30m/min stirs 10min rotating-speed modulation 100m/min is stirred to 30min, the rubber of wadding a quilt with cotton out is taken out, and all the other steps are as embodiment 1.
Comparative example 6
On two rollers are begun to pratise machine by formula: the each 50phr of natural gum butadiene-styrene rubber, carbon black (N234) 50phr, all the other Synergist S-421 95s are as embodiment 1, and all the other steps are as embodiment 1.
Table one embodiment and the contrast of comparative example mechanical property
Claims (4)
1. a processing method of preparing high-performance carbon black rubber master batch, is characterized in that:
Select the solution immersion carbon black powder of small molecules easy volatile solvent to prepare finely dispersed carbon black slurry, the mass percent 2.5%～10% of carbon black slurry; Add carbon black slurry to stir 20-60min at 100～300m/min after rotating speed 10～40m/min stirs 10～30min latex, latex and carbon black are wadded a quilt with cotton out, filter, dry; Described small molecules easy volatile solvent is methyl alcohol, ethanol, propyl alcohol, tetrahydrofuran (THF), acetone, butanone, or their mixture; Take dry glue quality in latex as 100 parts, the add-on of carbon black is at 30 parts～80 parts; Treating compound adds 10 parts～300 parts.
2. a kind of processing method of preparing high-performance carbon black rubber master batch according to claim 1, is characterized in that: the volatile carbon black treating compound of small molecules is ethanol.
3. a kind of processing method of preparing high-performance carbon black rubber master batch according to claim 1, is characterized in that: latex is fresh natural emulsion or concentrated natural latex, butadiene-styrene latex, butyronitrile latex, neoprene latex, fourth pyrrole and butylbenzene pyrrole latex, and the mixed latex of above latex.
4. a kind of processing method of preparing high-performance carbon black rubber master batch according to claim 1, is characterized in that: preparation latex mass percent concentration is 5%～40%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072831A (en) * | 2014-06-27 | 2014-10-01 | 青岛大学 | Oil-extended carbon-nanotubes-extended binary emulsion coprecipitation rubber and preparation method thereof |
| CN104211837A (en) * | 2014-07-15 | 2014-12-17 | 华南理工大学 | Preparation method of carbon-black-containing butadiene styrene rubber master batch |
| WO2017088503A1 (en) * | 2015-11-29 | 2017-06-01 | 北京化工大学 | Method for preparing high-filling composite masterbatch by means of semi-open type superheated steam spray drying method |
| CN107505480A (en) * | 2017-08-16 | 2017-12-22 | 四川理工学院 | A kind of method for detecting filler dispersiveness in rubber composite material |
| CN108794821A (en) * | 2018-06-07 | 2018-11-13 | 浙江环能传动科技有限公司 | A kind of method of plasticating of natural gum |
| CN109517195A (en) * | 2017-09-18 | 2019-03-26 | 北京化工大学 | A kind of method that wet process is kneaded preparation carbon black rubber master batch |
| CN109715708A (en) * | 2016-12-14 | 2019-05-03 | 通伊欧轮胎株式会社 | The manufacturing method of the preparation method of masterbatch, the preparation method of rubber composition and tire |
| CN109923155A (en) * | 2016-12-27 | 2019-06-21 | 通伊欧轮胎株式会社 | The manufacturing method of masterbatch and the manufacturing method of tire |
| CN112852189A (en) * | 2021-01-21 | 2021-05-28 | 山东联科科技股份有限公司 | Preparation method of carbon black |
| CN115970569A (en) * | 2023-03-17 | 2023-04-18 | 青岛黑猫新材料研究院有限公司 | Carbon black intermediate product treatment system and method |
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| CN104072831A (en) * | 2014-06-27 | 2014-10-01 | 青岛大学 | Oil-extended carbon-nanotubes-extended binary emulsion coprecipitation rubber and preparation method thereof |
| CN104072831B (en) * | 2014-06-27 | 2016-03-09 | 青岛大学 | One is oil-filled fills carbon nanotube dual emulsion coprecipitation rubber and preparation method thereof |
| CN104211837A (en) * | 2014-07-15 | 2014-12-17 | 华南理工大学 | Preparation method of carbon-black-containing butadiene styrene rubber master batch |
| CN104211837B (en) * | 2014-07-15 | 2016-05-04 | 华南理工大学 | A kind of preparation method of carbon black extended SBR rubber master batch |
| WO2017088503A1 (en) * | 2015-11-29 | 2017-06-01 | 北京化工大学 | Method for preparing high-filling composite masterbatch by means of semi-open type superheated steam spray drying method |
| CN109715708A (en) * | 2016-12-14 | 2019-05-03 | 通伊欧轮胎株式会社 | The manufacturing method of the preparation method of masterbatch, the preparation method of rubber composition and tire |
| CN109715708B (en) * | 2016-12-14 | 2022-02-15 | 通伊欧轮胎株式会社 | Method for producing masterbatch, method for producing rubber composition, and method for producing tire |
| CN109923155A (en) * | 2016-12-27 | 2019-06-21 | 通伊欧轮胎株式会社 | The manufacturing method of masterbatch and the manufacturing method of tire |
| US10544291B2 (en) | 2016-12-27 | 2020-01-28 | Toyo Tire Corporation | Masterbatch manufacturing method and tire manufacturing method |
| CN109923155B (en) * | 2016-12-27 | 2021-08-17 | 通伊欧轮胎株式会社 | Method for producing masterbatch and method for producing tire |
| CN107505480A (en) * | 2017-08-16 | 2017-12-22 | 四川理工学院 | A kind of method for detecting filler dispersiveness in rubber composite material |
| CN107505480B (en) * | 2017-08-16 | 2020-05-08 | 四川理工学院 | Method for detecting filler dispersibility in rubber composite material |
| CN109517195A (en) * | 2017-09-18 | 2019-03-26 | 北京化工大学 | A kind of method that wet process is kneaded preparation carbon black rubber master batch |
| CN108794821A (en) * | 2018-06-07 | 2018-11-13 | 浙江环能传动科技有限公司 | A kind of method of plasticating of natural gum |
| CN112852189A (en) * | 2021-01-21 | 2021-05-28 | 山东联科科技股份有限公司 | Preparation method of carbon black |
| CN112852189B (en) * | 2021-01-21 | 2022-04-05 | 山东联科科技股份有限公司 | Preparation method of carbon black |
| CN115970569A (en) * | 2023-03-17 | 2023-04-18 | 青岛黑猫新材料研究院有限公司 | Carbon black intermediate product treatment system and method |
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