CN105419003A - Method of quickly monitoring coprecipitation behavior in preparation of NR/CB composite material through latex coprecipitation method - Google Patents
Method of quickly monitoring coprecipitation behavior in preparation of NR/CB composite material through latex coprecipitation method Download PDFInfo
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- CN105419003A CN105419003A CN201510985359.3A CN201510985359A CN105419003A CN 105419003 A CN105419003 A CN 105419003A CN 201510985359 A CN201510985359 A CN 201510985359A CN 105419003 A CN105419003 A CN 105419003A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
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Abstract
The invention discloses a method of quickly a monitoring coprecipitation behavior in preparation of an NR/CB composite material through a latex coprecipitation method. In the method, an NR/CB coprecipitation rubber compound is dried with initial appearance maintained, and detection then is directly carried out through SEM under a non-metal sprayed condition. Through observation of status of "rubber blocks" and "rubber bundles" in an SEM detection result, adsorption and coprecipitation behavior of the rubber composite material is monitored. Compared with a method, in which CB dispersibility of the rubber composite material is determined through measurement on other performance of the rubber composite material through rubber compound vulcanization or special preparation of a test sample, the method for determining the CB dispersibility of the rubber composite material is more simple and convenient. The method can be used for monitoring whether the coprecipitation behavior in preparation of the NR/CB composite material through the latex coprecipitation method meets the requirement. The method has very important significance on monitoring of preparation of the rubber compound vulcanization through the latex coprecipitation method, is creative, is convenient to carry out and is significant in effects.
Description
Technical field
The present invention relates to material science, especially a kind of fast monitored latex coprecipitation method prepares the method for the coprecipitated behavior of NR/CB matrix material.
Background technology
Filler and the direct glue of natural rubber latex are current advanced glue methods (being called for short latex coprecipitation method), and the rubber composite that the method obtains has good mechanical property and environment friendly.Research finds, prepare in NR/CB composite material at latex coprecipitation method, the coprecipitated behavior of alternating sorbent has material impact to carbon black dispersion in matrix material, and the performance of carbon black dispersion to NR/CB rubber composite has material impact.For ensureing that CB to prepare the good dispersion in NR/CB matrix material at latex coprecipitation method, need monitor fast and effectively the coprecipitated behavior of the latex of matrix material in glue production process.
Summary of the invention
The object of the invention is: provide a kind of fast monitored latex coprecipitation method to prepare the method for the coprecipitated behavior of NR/CB matrix material, the coprecipitated behavior of its fast monitored alternating sorbent, monitoring result can be used as the foundation of adjustment glue related process, and this monitoring method has filled up the blank of existing monitoring means.
The present invention is achieved in that fast monitored latex coprecipitation method prepares the method for the coprecipitated behavior of NR/CB matrix material, initial pattern is kept directly to dry the coprecipitated sizing material of NR/CB adopting latex coprecipitation method to prepare, then under non-metal spraying condition, scanning electron microscope detection is carried out, observe the state of blob of viscose and micella in the detected result of scanning electron microscope, thus realize the fast monitored being prepared by latex coprecipitation method to the coprecipitated behavior of NR/CB matrix material.
In the detected result of described observation scanning electron microscope, the state of blob of viscose and micella is, observes the blob of viscose of NR/CB alternating sorbent coprecipitated generation 10-60 μm of particle diameter, and when producing the micella of independently and not sheeting, then determines that this coprecipitated result is re-set target.
Owing to have employed technique scheme, compared with prior art, the present invention keeps initial pattern directly under non-metal spraying condition, to use SEM to detect after being dried by coprecipitated for NR/CB sizing material, by observing the state of " blob of viscose " and " micella " in SEM detected result, to monitor the sorption-coprecipitation behavior of rubber composite, with pass through rubber vulcanization, or other performances preparing the mensuration rubber composites such as test sample are specially compared to the method for the CB dispersiveness judging rubber composite, judge that the dispersiveness operation of CB in rubber composite is more simple by method of the present invention, convenient.Adopt the present invention can monitor latex coprecipitation method to prepare the coprecipitated behavior of NR/CB matrix material and whether reach demand, the quality product being prepared by monitoring latex coprecipitation method to rubber composite has very important meaning.Thinking of the present invention is novel, swift to operate, successful.
Accompanying drawing explanation
Accompanying drawing 1-5 is the scanning electron microscope result of embodiments of the invention.
Embodiment
Embodiments of the invention: fast monitored latex coprecipitation method prepares the method for the coprecipitated behavior of NR/CB matrix material, latex coprecipitation method is adopted to prepare NR/CB matrix material, 5 different stirring velocitys are set, be followed successively by 1000r/min, 2000r/min, 3000r/min, 4000r/min, 5000r/min, all the other processing parameters all adopt conventional parameter of the prior art, and remain unchanged, after keeping initial pattern directly to dry coprecipitated for the NR/CB prepared sizing material, under non-metal spraying condition, use scanning electron microscope to detect, observe its initial pattern, result as Figure 1-5.
Result is learnt according to the observation, and when stirring velocity is 1000r/min, NR/CB composite material surface only has little sorption-coprecipitation " blob of viscose ", and blob of viscose particle diameter is all very little, nearly all less than 10 μm, as shown in Figure 1; And when stirring velocity is increased to 2000r/min, sorption-coprecipitation " blob of viscose " quantity of NR/CB composite material surface slightly increases, the particle diameter of blob of viscose also increases to some extent, but majority is no more than 20 μm, as shown in Figure 2; When stirring velocity is 3000r/min, quantity and the particle diameter of the sorption-coprecipitation " blob of viscose " of NR/CB composite material surface obviously increase, and start to occur trace " micella ", wherein the particle diameter of blob of viscose occurs within the scope of 10-60 μm, and increase in a large number more than the blob of viscose of 30 μm of particle diameters, the more important thing is, occurred independent and micella that is not sheeting, as shown in Figure 3; When stirring velocity is increased to 4000r/min, the particle diameter of the sorption-coprecipitation " blob of viscose " of NR/CB composite material surface compares the obvious reduction in Fig. 3, and the quantity of " micella " obviously increases, and occurs the phenomenon of sheeting, as shown in Figure 4; And when stirring velocity continues to be increased to 5000r/min, quantity and the particle diameter of the sorption-coprecipitation " blob of viscose " of NR/CB composite material surface all obviously reduce, the quantity of " micella " continues to increase, and a large amount of sheeting, as shown in Figure 5.
Think; when stirring velocity is 1000r/min and 2000r/min; because stirring velocity is lower; shear force is more weak; natural latex rubber particle surface protective layer destroys less, and the rubber molecular chain flowed out from sol layer is less, so form the comparatively small amt of " blob of viscose "; particle diameter is less, and does not almost have unnecessary rubber molecule chain formation micella.When stirring velocity is increased to 3000r/min; the effect of stirring shearing force is stronger; be enough to destroy natural latex rubber particle surface protective layer; have enough rubber molecular chains to flow out continually and coprecipitated and produce a large amount of " blob of viscose " with carbon black particle alternating sorbent from sol layer, the interaction of rubber molecule interchain simultaneously defines less " micella ".And when stirring velocity continues to be increased to 4000r/min and 5000r/min; because stirring velocity is too high; stir shear action excessively strong; cause latex rubbers particle protective layer premature failure; a large amount of rubber molecular chain flows out from sol layer simultaneously, and the interaction of rubber molecule interchain is excessively strong, and the coprecipitated declines of alternating sorbent; cause the reduction of the increase of micella quantity and coprecipitated " blob of viscose " quantity of alternating sorbent and particle diameter, carbon black distributed pole is uneven.Part micella is had to present nonconducting brilliant white because content of carbon black is extremely low under scanning electron microscope.
SEM image according to Fig. 1-5 can be learnt, adopts technical scheme of the present invention can prepare the coprecipitated behavior of NR/CB matrix material by fast monitored latex coprecipitation method, and adjusts relevant adhesive-preparing technology in time according to monitoring result, ensures quality product.
The principle of embodiment is: natural rubber latex can disperse for a long time and keep stable a kind of suspension.Wherein contained rubber particles particle diameter average out to 1.06 microns, and there is protective layer, gel coat and sol layer three-decker.And when latex coprecipitation method prepares NR/CB matrix material, need by stirring, its protective layer and gel coat to be destroyed, to make the rubber molecule segment in carbon black and micelle sol layer directly adsorb, be wound around, to reach reinforcement object.When stirring is sheared more weak, natural latex rubber particle surface protective layer destroys less, time less from the rubber molecular chain of sol layer outflow, it forms the comparatively small amt of " blob of viscose ", particle diameter is less, and does not almost have unnecessary rubber molecule chain formation micella, and now coprecipitated effect is poor; And it is suitable when stirring shearing action, when natural latex rubber particle surface protective layer is sufficiently damaged, enough rubber molecular chains are had to flow out continually and coprecipitated and produce a large amount of " blob of viscose " with carbon black particle alternating sorbent from sol layer, the interaction of rubber molecule interchain simultaneously starts to define less " micella ", now sorption-coprecipitation best results; And it is excessively strong when stirring shear action; cause latex rubbers particle protective layer premature failure; a large amount of rubber molecular chain flows out from sol layer simultaneously; the interaction of rubber molecule interchain is excessively strong; and the coprecipitated declines of alternating sorbent, cause micella quantity obviously to increase and the reduction of coprecipitated " blob of viscose " quantity of alternating sorbent and particle diameter, now coprecipitated effect is poor; carbon black distributed pole is uneven, and has part micella to present nonconducting brilliant white because content of carbon black is extremely low under scanning electron microscope.Therefore, observe the initial pattern of the coprecipitated sizing material of NR/CB prepared by latex coprecipitation method, its sorption-coprecipitation behavior can be monitored.
Claims (2)
1. a fast monitored latex coprecipitation method prepares the method for the coprecipitated behavior of NR/CB matrix material, it is characterized in that: keep initial pattern directly to dry the coprecipitated sizing material of NR/CB adopting latex coprecipitation method to prepare, then under non-metal spraying condition, scanning electron microscope detection is carried out, observe the state of blob of viscose and micella in the detected result of scanning electron microscope, thus realize the fast monitored being prepared by latex coprecipitation method to the coprecipitated behavior of NR/CB matrix material.
2. fast monitored latex coprecipitation method according to claim 1 prepares the method for the coprecipitated behavior of NR/CB matrix material, it is characterized in that: in the detected result of described observation scanning electron microscope, the state of blob of viscose and micella is, observe the blob of viscose of NR/CB alternating sorbent coprecipitated generation 10-60 μm of particle diameter, and when producing the micella of independently and not sheeting, then determine that this coprecipitated result is re-set target.
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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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| 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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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102954975A (en) * | 2011-08-23 | 2013-03-06 | 住友橡胶工业株式会社 | Method for analyzing rubber compound with filler particles |
| CN103348236A (en) * | 2011-02-08 | 2013-10-09 | 株式会社普利司通 | Method for evaluating polymer material |
| 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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- 2015-12-25 CN CN201510985359.3A patent/CN105419003B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103348236A (en) * | 2011-02-08 | 2013-10-09 | 株式会社普利司通 | Method for evaluating polymer material |
| CN102954975A (en) * | 2011-08-23 | 2013-03-06 | 住友橡胶工业株式会社 | 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 |
Non-Patent Citations (1)
| Title |
|---|
| 王炼石等: "高耐磨炭黑填充型粉末SBR研究 I. 粉末化条件与粒径分布", 《合成橡胶工业》 * |
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