CN105419003B - The method that fast slowdown monitoring latex coprecipitation method prepares the coprecipitated behavior of NR/CB composites - Google Patents
The method that fast slowdown monitoring latex coprecipitation method prepares the coprecipitated behavior of NR/CB composites Download PDFInfo
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- CN105419003B CN105419003B CN201510985359.3A CN201510985359A CN105419003B CN 105419003 B CN105419003 B CN 105419003B CN 201510985359 A CN201510985359 A CN 201510985359A CN 105419003 B CN105419003 B CN 105419003B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a kind of method that fast slowdown monitoring latex coprecipitation method prepares the coprecipitated behavior of NR/CB composites.The present invention will keep initial pattern directly to be detected under the conditions of non-metal spraying using SEM after the coprecipitated sizing material drying of NR/CB, by the state for observing " blob of viscose " and " micella " in SEM testing results, to monitor the sorption-coprecipitation behavior of rubber composite, with by rubber vulcanization or it is special prepare the method for CB dispersivenesses that test specimen etc. determines other performances of rubber composite to judge rubber composite compared with, judge that the dispersiveness of CB in rubber composite is operated with the method for the present invention more simple, conveniently.Latex coprecipitation method can be monitored using the present invention and prepare whether the coprecipitated behavior of NR/CB composites reaches demand, have very important meaning to the product quality that monitoring latex coprecipitation method prepares rubber composite.Thinking of the present invention is novel, and swift to operate, effect is obvious.
Description
Technical field
The present invention relates to materials science field, especially a kind of fast slowdown monitoring latex coprecipitation method prepares NR/CB composites
The method of coprecipitated behavior.
Background technology
Filler and the direct glue of Heveatex are current advanced glue methods（Abbreviation latex coprecipitation method）, this method be made
Rubber composite there is good mechanical performance and environment friendly.Research is found, NR/CB is prepared in latex coprecipitation method
In composite material, the coprecipitated behavior of alternating sorbent has a major impact to carbon black dispersion in composite, and carbon black dispersion
Performance to NR/CB rubber composites has a major impact.To ensure CB in latex coprecipitation method prepares NR/CB composites
Good dispersion, the coprecipitated behavior of latex that need to be to composite in glue production process is fast and effectively monitored.
The content of the invention
The purpose of the present invention is：A kind of fast slowdown monitoring latex coprecipitation method is provided and prepares the coprecipitated behavior of NR/CB composites
Method, its fast coprecipitated behavior of slowdown monitoring alternating sorbent, monitoring result can be used as the foundation for adjusting glue related process, the monitoring side
Method has filled up the blank of existing monitoring means.
What the present invention was realized in：The method that fast slowdown monitoring latex coprecipitation method prepares the coprecipitated behavior of NR/CB composites,
Initial pattern is kept directly to be dried the coprecipitated sizing materials of the NR/CB prepared using latex coprecipitation method, then in non-metal spraying
Under the conditions of be scanned Electronic Speculum detection, observe ESEM testing result in blob of viscose and micella state, so as to realize to glue
Newborn coprecipitation method prepares the fast slowdown monitoring of the coprecipitated behavior of NR/CB composites.
The state of blob of viscose and micella is in the testing result of described observation ESEM, it was observed that NR/CB alternating sorbents
It is coprecipitated to produce the blob of viscose of 10-60 μm of particle diameter, and when producing independently without the micella of sheeting, it is determined that the coprecipitated result is expected mesh
Mark.
By adopting the above-described technical solution, compared with prior art, the present invention will be kept after the coprecipitated sizing material drying of NR/CB
Initial pattern is directly detected under the conditions of non-metal spraying using SEM, by observing " blob of viscose " and " glue in SEM testing results
The state of beam ", to monitor the sorption-coprecipitation behavior of rubber composite, with by rubber vulcanization or specially preparing test specimen
Judge that the method for the CB dispersivenesses of rubber composite is compared Deng other performances of rubber composite are determined, with the present invention's
Method judges that the dispersiveness operation of CB in rubber composite is more simple, conveniently.Latex can be monitored using the present invention coprecipitated
Method prepares whether the coprecipitated behavior of NR/CB composites reaches demand, and the production of rubber composite is prepared to monitoring latex coprecipitation method
Quality has very important meaning.Thinking of the present invention is novel, and swift to operate, effect is obvious.
Brief description of the drawings
Accompanying drawing 1-5 is the ESEM result of embodiments of the invention.
Embodiment
Embodiments of the invention：The method that fast slowdown monitoring latex coprecipitation method prepares the coprecipitated behavior of NR/CB composites, is used
Latex coprecipitation method prepares NR/CB composites, sets 5 different mixing speeds, is followed successively by 1000 r/min, 2000 r/
Min, 3000 r/min, 4000 r/min, 5000 r/min, remaining technological parameter use conventional parameter of the prior art,
And keep constant, the coprecipitated sizing materials of the NR/CB prepared are kept after the directly drying of initial pattern, used under the conditions of non-metal spraying
ESEM is detected, observes its initial pattern, as a result as Figure 1-5.
Result is learnt according to the observation, and when mixing speed is 1000 r/min, NR/CB composite material surfaces only have seldom
Sorption-coprecipitation " blob of viscose ", and blob of viscose particle diameter is all very small, nearly all less than 10 μm, as shown in Figure 1；And when mixing speed increases to
During 2000 r/min, sorption-coprecipitation " blob of viscose " quantity of NR/CB composite material surfaces is increased slightly, and the particle diameter of blob of viscose has also increased
Greatly, it is but most no more than 20 μm, as shown in Figure 2；When mixing speed is 3000 r/min, NR/CB composite material surfaces
The quantity and particle diameter of sorption-coprecipitation " blob of viscose " substantially increase, and start micro " micella " occur, and wherein the particle diameter of blob of viscose is in 10-60
Occur, and largely increase more than the blob of viscose of 30 μm of particle diameters in μ m, it is often more important that, occur in that independent without sheeting
Micella, as shown in Figure 3；When mixing speed increases to 4000 r/min, the sorption-coprecipitation " blob of viscose " of NR/CB composite material surfaces
Particle diameter compare being obviously reduced in Fig. 3, and the quantity of " micella " substantially increases, and the phenomenon of sheeting occurs, as shown in Figure 4；
And when mixing speed continues to increase to 5000 r/min, the quantity of the sorption-coprecipitation " blob of viscose " of NR/CB composite material surfaces and
Particle diameter is substantially reduced, and the quantity of " micella " continues to increase, and a large amount of sheeting, as shown in Figure 5.
Think, when mixing speed is 1000r/min and 2000r/min, because mixing speed is relatively low, shear action
Power is weaker, and natural latex rubber particle surface protection damage layer is less, and the rubber molecular chain flowed out from sol layer is less, so shape
Into the negligible amounts of " blob of viscose ", particle diameter is smaller, and almost without unnecessary rubber molecular chain formation micella.When mixing speed increase
During to 3000r/min, the effect for stirring shearing force is stronger, it is sufficient to destroy natural latex rubber particle surface protective layer, has enough
Rubber molecular chain continually flowed out from sol layer and coprecipitated and produce substantial amounts of " blob of viscose " with carbon black particle alternating sorbent, together
When rubber molecule interchain interaction form less " micella ".And when mixing speed continue to increase to 4000 r/min and
During 5000 r/min, because mixing speed is too high, stirring shearing force is too strong, causes latex rubber particle protective layer to break too early
Bad, a large amount of rubber molecular chains are simultaneously from sol layer outflow, and the interaction of rubber molecule interchain is too strong, and the coprecipitated work of alternating sorbent
With decrease, cause the increase of micella quantity and the reduction of coprecipitated " blob of viscose " quantity of alternating sorbent and particle diameter, carbon black distributed pole is not
Uniformly.There is part micella under ESEM because content of carbon black is extremely low and nonconducting brilliant white is presented.
According to Fig. 1-5 SEM image it is known that can slowdown monitoring latex coprecipitation method soon using technical scheme
The coprecipitated behavior of NR/CB composites is prepared, and adjusts according to monitoring result related adhesive-preparing technology in time, it is ensured that product quality.
The principle of embodiment is：Heveatex is can for a long time to disperse and keep a kind of stable suspension.It is contained therein
1.06 microns of rubber particles particle diameter average out to, and with protective layer, gel layer and sol layer three-decker.And in latex coprecipitation method
, it is necessary to by stirring its protective layer and gel damage layer, so that in carbon black and micelle sol layer during preparation NR/CB composites
Rubber molecule segment directly adsorb, wind, to reach reinforcement purpose.When weaker, natural latex rubber particle table is sheared in stirring
Face protection damage layer it is less, from sol layer flow out rubber molecular chain it is less when, its formed " blob of viscose " negligible amounts, particle diameter compared with
It is small, and almost without unnecessary rubber molecular chain formation micella, now coprecipitated effect is poor；And it is appropriate when stirring shear action,
When natural latex rubber particle surface protective layer is sufficiently damaged, there are enough rubber molecular chains continually to be flowed out from sol layer
And it is coprecipitated and produce substantial amounts of " blob of viscose " with carbon black particle alternating sorbent, while the interaction of rubber molecule interchain is initially formed
Less " micella ", now sorption-coprecipitation best results；And when stirring shearing force is too strong, cause latex rubber particle to be protected
Sheath premature failure, a large amount of rubber molecular chains are simultaneously from sol layer outflow, and the interaction of rubber molecule interchain is too strong, and replaces
Sorption-coprecipitation declines, cause micella quantity substantially increase and the reduction of coprecipitated " blob of viscose " quantity of alternating sorbent and particle diameter,
Now coprecipitated effect is poor, and carbon black distributed pole is uneven, and have part micella under ESEM because content of carbon black is extremely low and
Nonconducting brilliant white is presented.Therefore, the initial pattern of the coprecipitated sizing materials of NR/CB prepared by observation latex coprecipitation method, can be monitored
Its sorption-coprecipitation behavior.
Claims (2)
1. a kind of method that fast slowdown monitoring latex coprecipitation method prepares the coprecipitated behavior of NR/CB composites, it is characterised in that：It will use
The coprecipitated sizing materials of NR/CB that latex coprecipitation method is prepared keep initial pattern directly to be dried, then under the conditions of non-metal spraying
Electronic Speculum detection is scanned, the state of blob of viscose and micella in the testing result of ESEM is observed, so as to realize coprecipitated to latex
Method prepares the fast slowdown monitoring of the coprecipitated behavior of NR/CB composites.
2. the method that fast slowdown monitoring latex coprecipitation method according to claim 1 prepares the coprecipitated behavior of NR/CB composites, its
It is characterised by：The state of blob of viscose and micella is in the testing result of described observation ESEM, it was observed that NR/CB alternating sorbents
It is coprecipitated to produce the blob of viscose of 10-60 μm of particle diameter, and when producing independently without the micella of sheeting, it is determined that the coprecipitated result is expected mesh
Mark.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510985359.3A CN105419003B (en) | 2015-12-25 | 2015-12-25 | The method that fast slowdown monitoring latex coprecipitation method prepares the coprecipitated behavior of NR/CB composites |
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| CN201510985359.3A CN105419003B (en) | 2015-12-25 | 2015-12-25 | The method that fast slowdown monitoring latex coprecipitation method prepares the coprecipitated behavior of NR/CB composites |
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| CN105419003B true CN105419003B (en) | 2017-08-11 |
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| JP5825797B2 (en) * | 2011-02-08 | 2015-12-02 | 株式会社ブリヂストン | Evaluation method for polymer materials |
| US20130051656A1 (en) * | 2011-08-23 | 2013-02-28 | Wakana Ito | Method for analyzing rubber compound with filler particles |
| CN105043945A (en) * | 2015-06-30 | 2015-11-11 | 人本集团有限公司 | Particle size testing method of carbon black in rubber materials |
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