CN102898681B - Loaded type nano-zinc oxide composite material - Google Patents
Loaded type nano-zinc oxide composite material Download PDFInfo
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- CN102898681B CN102898681B CN201210365960.9A CN201210365960A CN102898681B CN 102898681 B CN102898681 B CN 102898681B CN 201210365960 A CN201210365960 A CN 201210365960A CN 102898681 B CN102898681 B CN 102898681B
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- zinc oxide
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Abstract
The invention discloses a loaded type nano-zinc oxide composite material. The composite material are prepared through the method of adding rubber into a zinc sulfate solution through carbon black to be stirred and dispersed, dropwise adding an ammonium hydrogen carbonate aqueous solution until thorough sedimentation, performing filtering to obtain sedimentation, and washing the sedimentation with deionized water until no sulfate radical exists; and drying the sedimentation, and calcining the sedimentation at a temperature in a range from 200 DEG C to 300 DEG C for 2 to 4 hours under the protection of inert gases to obtain the loaded type nano-zinc oxide composite material. According to the loaded type nano-zinc oxide composite material, the nano-zinc oxide is loaded on the rubber by using carbon black, the nano-zinc oxide has a high activity, the utilization rate of zinc atoms is high, an additive amount is 30% to 50% of that of ordinary zinc oxide, and the nano-zinc oxide resource can be greatly saved.
Description
Technical field
The present invention relates to a kind of load nano-zinc oxide composite material, also relate to a kind of rubber item that adopts this matrix material simultaneously.
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, active low, large usage quantity.Nano zine oxide because of its particle diameter little, specific surface area is large, adsorption activity is strong, thereby has surface effects and high reactivity.Nano zine oxide can be realized the combination on molecular level with rubber molecule, for rubber, can give full play to sulfuration promoter action, improves the performance of rubber, and its consumption can significantly reduce, and has reduced 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 really playing a role in Vulcanization Process of Rubber that causes to remain minority, the atom utilization that is zinc oxide is very low, major part is only present in rubber item as filler, thereby has affected the performance of rubber item.
Summary of the invention
The object of this invention is to provide the loaded nano zinc oxide composite that a kind of nano zine oxide atom utilization is high.
In order to realize above object, the technical solution adopted in the present invention is: a kind of loaded nano zinc oxide composite, adopts following method to be prepared from:
1) rubber grade carbon black is joined to dispersed with stirring in 10～20% solution of zinc sulfate, the add-on of carbon black is 10～50% of zinc sulfate quality, then drip the molten aqueous solution of bicarbonate of ammonia until precipitation is complete, the quality of bicarbonate of ammonia is 0.5～1.5 times of zinc sulfate quality;
2) filter and to be precipitated, with deionized water wash to sulfate radical-free;
3) will precipitate dry after, under protection of inert gas, at 200～300 ℃, calcine 2 by 4 hours, obtain loaded nano zinc oxide composite.
As further optimization, the concentration of the ammonium bicarbonate aqueous solution in step 1) is 10～20%.
As further optimization, described supercarbonate is bicarbonate of ammonia, sodium bicarbonate or saleratus.
As further optimization, churning time is 30～90 minutes described in step 1).
As further optimization, precipitating drying temperature described in step 3) is 85 ℃.
As further optimization, the loaded nano zinc oxide composite of stating, is characterized in that: step 1) continues reaction 1 hour after dripping ammonium bicarbonate aqueous solution.
The application's loaded nano zinc oxide composite, adopt the very large rubber black of surface-area to do carrier, 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 dispersed, therefore adopt loaded nano zinc oxide composite of the present invention can improve significantly zinc in zinc oxide atom utilization, thereby reduce the consumption of zinc oxide, its consumption is only 30%～50% of common zinc oxide, can greatly save nano oxidized zinc resource.
Embodiment
embodiment 1
The loaded nano zinc oxide composite of the present embodiment is adopted with the following method and is prepared from:
1) by purity, be to be greater than 99.5% zinc sulfate to be dissolved in deionized water, form 10% solution of zinc sulfate; By zinc sulfate quality 50%, add N110 type carbon black, after rapid stirring 30min, form suspension, the bicarbonate of ammonia of 0.5 times of zinc sulfate quality is made into 10% the aqueous solution, slowly add in above-mentioned suspension, add rear reaction and proceed to finish after 1 hour;
2) by suspension filtered, filter cake with deionized water wash to sulfate radical-free (SO
4 2-) exist;
3) after filter cake is dry at 85 ℃, enter stoving oven and at 250 ℃, calcine 2 hours in nitrogen atmosphere, obtain loaded nano zinc oxide composite.
It is 50.3% that product index sees attached list 1, ZnO charge capacity.
embodiment 2
The loaded nano zinc oxide composite of the present embodiment is adopted with the following method and is prepared from:
1) by purity, be to be greater than 99.5% zinc sulfate to be dissolved in deionized water, form 15% solution of zinc sulfate; By zinc sulfate quality 30%, add N110 type carbon black, after rapid stirring 60min, form suspension, the sodium bicarbonate of 1 times of zinc sulfate quality is made into 15% the aqueous solution, slowly add in above-mentioned suspension, add rear reaction and proceed to finish after 2 hours;
2) by suspension filtered, filter cake with deionized water wash to sulfate radical-free (SO
4 2-) exist;
3) after filter cake is dry at 105 ℃, enter stoving oven and at 200 ℃, calcine 3 hours in nitrogen atmosphere, obtain loaded nano zinc oxide composite.
It is 62.5% that product index sees attached list 1, ZnO charge capacity.
embodiment 3
The loaded nano zinc oxide composite of the present embodiment is adopted with the following method and is prepared from:
1) by purity, be to be greater than 99.5% zinc sulfate to be dissolved in deionized water, form 20% solution of zinc sulfate; By zinc sulfate quality 10%, add N110 type carbon black, after rapid stirring 90min, form suspension, the saleratus of 1.5 times of zinc sulfate quality is made into 15% the aqueous solution, slowly add in above-mentioned suspension, add rear reaction and proceed 3 and as a child finished;
2) by suspension filtered, filter cake with deionized water wash to sulfate radical-free (SO
4 2-) exist;
3) after filter cake is dry at 80 ℃, enter stoving oven and at 300 ℃, calcine 4 hours in nitrogen atmosphere, obtain loaded nano zinc oxide composite.
It is 73.3% that product index sees attached list 1, ZnO charge capacity.
Subordinate list 1
。
Note: quality-carbon black mass quality after charge capacity %=(carbon black loadings)/carbon black mass.
Claims (6)
1. a loaded nano zinc oxide composite, is characterized in that: adopt following method to be prepared from:
1) rubber grade carbon black being joined to mass percent concentration is dispersed with stirring in 10～20% solution of zinc sulfate, the add-on of carbon black is 10～50% of zinc sulfate quality, then drip bicarbonate aqueous solution until precipitation is complete, the quality of bicarbonate of ammonia is 0.5～1.5 times of zinc sulfate quality;
2) filter and to be precipitated, with deionized water wash to sulfate radical-free;
3) will precipitate dry after, under protection of inert gas, at 200～300 ℃, calcine 2～4 hours, obtain loaded nano zinc oxide composite.
2. loaded nano zinc oxide composite according to claim 1, is characterized in that: the concentration of described bicarbonate aqueous solution is 10～20% mass percentage concentration.
3. loaded nano zinc oxide composite according to claim 1, is characterized in that: described supercarbonate is bicarbonate of ammonia, sodium bicarbonate or saleratus.
4. loaded nano zinc oxide composite according to claim 1, is characterized in that: described in step 1), churning time is 30～90 minutes.
5. loaded nano zinc oxide composite according to claim 1, is characterized in that: described in step 3), precipitating drying temperature is 80-105 ℃.
6. loaded nano zinc oxide composite according to claim 1, is characterized in that: step 1) continues reaction 1-3 hour after dripping ammonium bicarbonate aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201210365960.9A CN102898681B (en) | 2012-09-27 | 2012-09-27 | Loaded type nano-zinc oxide composite material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210365960.9A CN102898681B (en) | 2012-09-27 | 2012-09-27 | Loaded type nano-zinc oxide composite material |
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| CN102898681A CN102898681A (en) | 2013-01-30 |
| CN102898681B true CN102898681B (en) | 2014-04-23 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104356424B (en) * | 2014-11-26 | 2018-02-06 | 山东阳谷华泰化工股份有限公司 | A kind of preparation method of low zinc vulcanizing activator |
| CN104857945A (en) * | 2015-04-30 | 2015-08-26 | 信阳师范学院 | Preparation method of zinc oxide/carbon micro-sphere composite material |
| 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 |
| CN109098040B (en) * | 2018-08-22 | 2021-06-08 | 广西大学 | Preparation method of functional filter paper loaded with nano zinc oxide |
| CN112142095A (en) * | 2020-11-19 | 2020-12-29 | 安徽泰龙锌业有限责任公司 | Preparation method of high-performance nano zinc oxide |
| CN113004576B (en) * | 2021-02-20 | 2021-09-07 | 安徽瑞邦橡塑助剂集团有限公司 | Preparation method of supported nano zinc oxide |
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| CN100336587C (en) * | 2005-06-22 | 2007-09-12 | 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 |
| CN101941731B (en) * | 2010-08-20 | 2012-07-18 | 桂林电子科技大学 | Preparation method of void type nano-sheet zinc oxide and activated carbon load complex |
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