CN102898682A - Supported nano zinc oxide composite material - Google Patents

Supported nano zinc oxide composite material Download PDF

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Publication number
CN102898682A
CN102898682A CN2012103659806A CN201210365980A CN102898682A CN 102898682 A CN102898682 A CN 102898682A CN 2012103659806 A CN2012103659806 A CN 2012103659806A CN 201210365980 A CN201210365980 A CN 201210365980A CN 102898682 A CN102898682 A CN 102898682A
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China
Prior art keywords
zinc oxide
nano zinc
oxide composite
carbon black
composite material
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CN2012103659806A
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CN102898682B (en
Inventor
张玉清
李旭阳
赫玉欣
王晓
姚大虎
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Henan University of Science and Technology
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Henan University of Science and Technology
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Abstract

The invention discloses a supported nano zinc oxide composite material, which is prepared by adopting the following method of: adding carbon black for rubber into a zinc sulfate solution, adding urea, stirring uniformly, heating to the temperature of between 90 and 100 DEG C, and reacting for 4 to 6 hours at the temperature; filtering after the reaction, and washing filter cakes by using deionized water till sulfate radicals do not exist; and drying the filter cakes, calcining for 2 to 4 hours at the temperature of between 200 and 300 DEG C under the protection of an inert gas, and thus obtaining the supported nano zinc oxide composite material. According to the supported nano zinc oxide composite material, nano zinc oxide is supported on the carbon black for the rubber, so that the nano zinc oxide has high activity; and the utilization rate of zinc atoms is high, and the adding quantity of the zinc atoms is 30 to 50 percent of common zinc oxide, so that the nano zinc oxide resource can be greatly saved.

Description

The loaded nano zinc oxide composite
Technical field
The present invention relates to a kind of load nano-zinc oxide composite material, also relate to simultaneously a kind of rubber item that adopts this matrix material.
Background technology
Zinc oxide is the requisite additive of rubber item, is vulcanization leveller and the strengthening agent of rubber, has in the world 50% zinc oxide to flow to rubber industry.Common Zinc oxide particles is larger, and is active low, large usage quantity.Nano zine oxide is little because of its particle diameter, and specific surface area is large, and adsorption activity is strong, thereby has surface effects and high reactivity.Nano zine oxide can be realized combination on the molecular level with rubber molecule, is used for rubber and can gives full play to the sulfuration promoter action, improve the performance of rubber, but its consumption decrease has reduced to the dependence of zinc resource and the environmental pollution that brings thereof.Yet, although the activity of nano zine oxide is higher, but because the add-on of nano zine oxide in rubber item seldom, often because disperse insufficient its zinc oxide atom that in Vulcanization Process of Rubber, really plays a role that causes to remain minority, the atom utilization that is zinc oxide is very low, major part only is present in the rubber item as filler, thereby has affected the performance of rubber item.
Summary of the invention
The purpose of this invention is to provide the high loaded nano zinc oxide composite of a kind of nano zine oxide atom utilization.
In order to realize above purpose, the technical solution adopted in the present invention is: a kind of loaded nano zinc oxide composite, adopt following method to be prepared from:
1) rubber grade carbon black is joined in 10~20% the solution of zinc sulfate, the add-on of carbon black is 10~50% of zinc sulfate quality, then add urea according to 0.4~0.6 times of zinc sulfate quality and stir, be warming up to 90~100 ℃ and under this temperature, reacted 4~6 hours;
2) filter after the reaction, with filter cake with deionized water wash to sulfate radical-free;
3) with behind the filtration cakes torrefaction, under protection of inert gas, in 200~300 ℃ of lower calcinings 2~4 hours, obtain the loaded nano zinc oxide composite.
As further improvement, the described churning time of step 1) is 20~90 minutes.
As further improvement, the described precipitation drying temperature of step 3) is 85 ℃.
The application's loaded nano zinc oxide composite, adopt the very large rubber black of surface-area to do carrier, at first make zinc sulfate be deposited in carbon blacksurface with the form of zinc carbonate, then pyrolytic decomposition generates the long-pending very large nano zine oxide of layer of surface on the surface of carbon black, nano zine oxide with respect to other form has higher activity, and carbon black is larger with respect to the particle diameter of nano zine oxide, and its amount ratio nano zine oxide in rubber item is much bigger, therefore the nano zine oxide that loads on carbon blacksurface is easy to realize Uniform Dispersion, therefore adopt loaded nano zinc oxide composite of the present invention can improve significantly the zinc in zinc oxide atom utilization, thereby reduce the consumption of zinc oxide, its consumption only is 30%~50% of common zinc oxide, can greatly save nano oxidized zinc resource.
Embodiment
Embodiment 1
The loaded nano zinc oxide composite of present embodiment adopts following method to be prepared from:
1) purity is dissolved in deionized water for the zinc sulfate greater than 99.5%, forms 10% solution of zinc sulfate; Press zinc sulfate quality 10% and add N110 type carbon black, 0.4 times that then presses the zinc sulfate quality adds urea, behind the rapid stirring 60min, is warming up to 95 ℃, insulation reaction 4 hours;
2) filter after the insulation reaction, filter cake with deionized water wash to sulfate radical-free (SO 4 2-) exist;
3) filter cake enters stoving oven after 85 ℃ of lower dryings, calcines 4 hours the loaded nano zinc oxide composite in nitrogen atmosphere under 200 ℃.
Product index sees attached list 1.ZnO charge capacity 83.0%.
Embodiment 2
The loaded nano zinc oxide composite of present embodiment adopts following method to be prepared from:
1) purity is dissolved in deionized water for the zinc sulfate greater than 99.5%, forms 20% solution of zinc sulfate; Press zinc sulfate quality 30% and add N110 type carbon black, 0.6 times that then presses the zinc sulfate quality adds urea, behind the rapid stirring 90min, is warming up to 90 ℃, insulation reaction 6 hours;
2) filter after the insulation reaction, filter cake with deionized water wash to sulfate radical-free (SO 4 2-) exist;
3) filter cake enters stoving oven after 80 ℃ of lower dryings, calcines 3 hours the loaded nano zinc oxide composite in nitrogen atmosphere under 250 ℃.
Product index sees attached list 1.ZnO charge capacity 82.7%.
Embodiment 3
The loaded nano zinc oxide composite of present embodiment adopts following method to be prepared from:
1) purity is dissolved in deionized water for the zinc sulfate greater than 99.5%, forms 15% solution of zinc sulfate; Press zinc sulfate quality 50% and add N110 type carbon black, 0.5 times that then presses the zinc sulfate quality adds urea, behind the rapid stirring 20min, is warming up to 100 ℃, insulation reaction 5 hours;
2) filter after the insulation reaction, filter cake with deionized water wash to sulfate radical-free (SO 4 2-) exist;
3) filter cake enters stoving oven after 105 ℃ of lower dryings, calcines 2 hours the loaded nano zinc oxide composite in nitrogen atmosphere under 300 ℃.
Product index sees attached list 1.ZnO charge capacity 82.1%.
Subordinate list 1
Figure 2012103659806100002DEST_PATH_IMAGE002
Annotate: quality after the charge capacity %=(carbon black loadings-carbon black mass quality)/carbon black mass.

Claims (3)

1. loaded nano zinc oxide composite is characterized in that: adopt following method to be prepared from:
1) rubber grade carbon black being joined mass percent concentration is in 10~20% the solution of zinc sulfate, the add-on of carbon black is 10~50% of zinc sulfate quality, then add urea according to 0.4~0.6 times of zinc sulfate quality and stir, be warming up to 90~100 ℃ and under this temperature, reacted 4~6 hours;
2) filter after the reaction, with filter cake with deionized water wash to sulfate radical-free;
3) with behind the filtration cakes torrefaction, under protection of inert gas, in 200~300 ℃ of lower calcinings 2~4 hours, obtain the loaded nano zinc oxide composite.
2. loaded nano zinc oxide composite according to claim 1, it is characterized in that: the described churning time of step 1) is 20~90 minutes.
3. loaded nano zinc oxide composite according to claim 1, it is characterized in that: the described precipitation drying temperature of step 3) is 80-105 ℃.
CN201210365980.6A 2012-09-27 2012-09-27 Supported nano zinc oxide composite material Expired - Fee Related CN102898682B (en)

Priority Applications (1)

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CN102898682B CN102898682B (en) 2014-04-23

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107216501A (en) * 2017-07-18 2017-09-29 利辛县正大化工原料有限公司 The formula and preparation method of a kind of water base latices for transmission belt infantees soaking paste
CN112159585A (en) * 2020-08-25 2021-01-01 苏州市雄林新材料科技有限公司 High-weather-resistance shading film and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1724138A (en) * 2005-06-22 2006-01-25 中山大学 Porous carbon adsorbing agent containing nano zinc oxide micropartical and its preparation process and application
CN101590420A (en) * 2009-06-30 2009-12-02 哈尔滨工业大学 A kind of preparation method of zeolite supported zinc oxyhydroxide
CN101941731A (en) * 2010-08-20 2011-01-12 桂林电子科技大学 Preparation method of void type nano-sheet zinc oxide and activated carbon load complex

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1724138A (en) * 2005-06-22 2006-01-25 中山大学 Porous carbon adsorbing agent containing nano zinc oxide micropartical and its preparation process and application
CN101590420A (en) * 2009-06-30 2009-12-02 哈尔滨工业大学 A kind of preparation method of zeolite supported zinc oxyhydroxide
CN101941731A (en) * 2010-08-20 2011-01-12 桂林电子科技大学 Preparation method of void type nano-sheet zinc oxide and activated carbon load complex

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107216501A (en) * 2017-07-18 2017-09-29 利辛县正大化工原料有限公司 The formula and preparation method of a kind of water base latices for transmission belt infantees soaking paste
CN112159585A (en) * 2020-08-25 2021-01-01 苏州市雄林新材料科技有限公司 High-weather-resistance shading film and preparation method thereof
CN112159585B (en) * 2020-08-25 2022-06-03 苏州市雄林新材料科技有限公司 High-weather-resistance shading film and preparation method thereof

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