CN102898681A - Loaded type nano-zinc oxide composite material - Google Patents
Loaded type nano-zinc oxide composite material Download PDFInfo
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- CN102898681A CN102898681A CN2012103659609A CN201210365960A CN102898681A CN 102898681 A CN102898681 A CN 102898681A CN 2012103659609 A CN2012103659609 A CN 2012103659609A CN 201210365960 A CN201210365960 A CN 201210365960A CN 102898681 A CN102898681 A CN 102898681A
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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 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 dispersed with stirring in 10～20% the 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 drying after, under protection of inert gas in 200～300 ℃ of lower calcinings 2 by 4 hours, obtain the loaded nano zinc oxide composite.
As further optimization, the concentration of the ammonium bicarbonate aqueous solution in the step 1) is 10～20%.
As further optimization, described supercarbonate is bicarbonate of ammonia, sodium bicarbonate or saleratus.
As further optimization, the described churning time of step 1) is 30～90 minutes.
As further optimization, the described precipitation drying temperature of 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, 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 50% and add N110 type carbon black, form suspension behind the rapid stirring 30min, the bicarbonate of ammonia of 0.5 times of zinc sulfate quality is made into 10% the aqueous solution, slowly add in the above-mentioned suspension, add afterreaction and proceed to finish after 1 hour;
2) with suspension filtered, filter cake with deionized water wash to sulfate radical-free (SO
4 2-) exist;
3) with filter cake after 85 ℃ of lower dryings, enter stoving oven in nitrogen atmosphere in 250 ℃ of lower calcinings 2 hours, obtain the loaded nano zinc oxide composite.
Product index 1, the ZnO charge capacity of seeing attached list is 50.3%.
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 15% solution of zinc sulfate; Press zinc sulfate quality 30% and add N110 type carbon black, form suspension behind the rapid stirring 60min, the sodium bicarbonate of 1 times of zinc sulfate quality is made into 15% the aqueous solution, slowly add in the above-mentioned suspension, add afterreaction and proceed to finish after 2 hours;
2) with suspension filtered, filter cake with deionized water wash to sulfate radical-free (SO
4 2-) exist;
3) with filter cake after 105 ℃ of lower dryings, enter stoving oven in nitrogen atmosphere in 200 ℃ of lower calcinings 3 hours, obtain the loaded nano zinc oxide composite.
Product index 1, the ZnO charge capacity of seeing attached list is 62.5%.
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 20% solution of zinc sulfate; Press zinc sulfate quality 10% and add N110 type carbon black, form suspension behind the rapid stirring 90min, the saleratus of 1.5 times of zinc sulfate quality is made into 15% the aqueous solution, slowly add in the above-mentioned suspension, add afterreaction and proceed 3 and as a child finished;
2) with suspension filtered, filter cake with deionized water wash to sulfate radical-free (SO
4 2-) exist;
3) with filter cake after 80 ℃ of lower dryings, enter stoving oven in nitrogen atmosphere in 300 ℃ of lower calcinings 4 hours, obtain the loaded nano zinc oxide composite.
Product index 1, the ZnO charge capacity of seeing attached list is 73.3%.
Subordinate list 1
Annotate: quality after the charge capacity %=(carbon black loadings-carbon black mass quality)/carbon black mass.
Claims (6)
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 dispersed with stirring in 10～20% the 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 drying after, 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 concentration of described bicarbonate aqueous solution is 10～20% mass percentage concentration.
3. loaded nano zinc oxide composite according to claim 1, it is characterized in that: described supercarbonate is bicarbonate of ammonia, sodium bicarbonate or saleratus.
4. loaded nano zinc oxide composite according to claim 1, it is characterized in that: the described churning time of step 1) is 30～90 minutes.
5. 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 ℃.
6. loaded nano zinc oxide composite according to claim 1 is characterized in that: continue reaction 1-3 hour behind the step 1) dropping 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 true CN102898681A (en) | 2013-01-30 |
| CN102898681B CN102898681B (en) | 2014-04-23 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356424A (en) * | 2014-11-26 | 2015-02-18 | 山东阳谷华泰化工股份有限公司 | 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 |
| CN109098040A (en) * | 2018-08-22 | 2018-12-28 | 广西大学 | A kind of preparation method of supported nano zinc oxide function filter paper |
| 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 |
| CN113004576A (en) * | 2021-02-20 | 2021-06-22 | 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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| 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 |
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2012
- 2012-09-27 CN CN201210365960.9A patent/CN102898681B/en not_active Expired - Fee Related
Patent Citations (3)
| 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 (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356424A (en) * | 2014-11-26 | 2015-02-18 | 山东阳谷华泰化工股份有限公司 | Preparation method of low-zinc vulcanizing activator |
| 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 |
| CN109098040A (en) * | 2018-08-22 | 2018-12-28 | 广西大学 | A kind of preparation method of supported nano zinc oxide function filter paper |
| 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 |
| CN113004576A (en) * | 2021-02-20 | 2021-06-22 | 安徽瑞邦橡塑助剂集团有限公司 | Preparation method of supported 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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| CN102898681B (en) | 2014-04-23 |
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