CN105036178B - A kind of preparation method of modified nano zinc oxide - Google Patents
A kind of preparation method of modified nano zinc oxide Download PDFInfo
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- CN105036178B CN105036178B CN201510425773.9A CN201510425773A CN105036178B CN 105036178 B CN105036178 B CN 105036178B CN 201510425773 A CN201510425773 A CN 201510425773A CN 105036178 B CN105036178 B CN 105036178B
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Abstract
The preparation method that the invention discloses a kind of modified nano zinc oxide, the concrete preparation process of described surface deposited silicon dioxide silicon is: 1) be impregnated in by unmodified nano zine oxide in the normal hexane solvent of methyl-silicone oil, stirs, and prepares mixed liquor；2) prepared mixed liquor is evaporated, and is put in baking oven and is dried, prepare the nano zine oxide that methyl-silicone oil is modified；3) being placed in Muffle furnace by the nano zine oxide that prepared methyl-silicone oil is modified, carry out high-temperature roasting, preparing surface deposition has the nano zine oxide of silicon dioxide.It is an advantage of the current invention that: 1, carry out siliceous deposits on the surface of nano zine oxide and modifiy, it is suppressed that the dissolution of nano zine oxide, improve the dispersibility of nano zine oxide.2, further, by citric acid, the hydroxyl of surface of nanometer zinc oxide is carried out bonding reaction, make not easily to reunite between nano granular of zinc oxide, improve the dispersibility of nano zine oxide.
Description
Technical field
The invention belongs to technical field of nano material, the preparation method being specifically related to a kind of modified nano zinc oxide.
Background technology
Nano zine oxide is the inorganic UV shield agent of a kind of excellent performance, is widely used in the fields such as sun care preparations, nano-function textile, functional plastics and coating.But, nano zine oxide is a kind of inorganic oxide, and its size is little, surface energy is high and organic principle is difficult to compatible, very easily produces serious agglomeration.It is therefore desirable to the modifying surface to nano zine oxide.
Document: Yang Zhanhong etc., the preparation of the zinc oxide of Surface coating silicon dioxide and character thereof, functional material, 2010.It discloses employing chemical deposition, be coated with one layer of silicon compound at zinc oxide surface.The present invention belongs to different technical fields from it, and technical scheme is different, and solves the technical problem that entirely different.
Summary of the invention
Present invention aims to the problem that nano zine oxide in prior art is easily reunited and the preparation method that a kind of modified nano zinc oxide is provided, promote dispersibility and the stability of nano zine oxide.
The technical scheme realizing the object of the invention employing is: the preparation method of a kind of modified nano zinc oxide, it is characterised in that: concrete preparation process is:
1) unmodified nano zine oxide be impregnated in the normal hexane solvent of methyl-silicone oil, stir, prepare mixed liquor；
2) mixed liquor that step 1) prepares is evaporated, and is put in baking oven and is dried, prepare the nano zine oxide that methyl-silicone oil is modified；
3) by step 2) the modified nano zine oxide of the methyl-silicone oil for preparing is placed in Muffle furnace, carry out high-temperature roasting, prepare surface deposition and have the nano zine oxide of silicon dioxide, described high-temperature roasting, its roasting process is: under excess oxygen, with the ramp of 5 DEG C/min to 450～550 DEG C, keep 2～4h, make methyl-silicone oil change into silicon dioxide.
Preferably, the volume ratio of the methyl-silicone oil described in step 1) and normal hexane solvent is 1:2, and the mass volume ratio of described nano zine oxide and methyl-silicone oil is 1g:5mL.
It is highly preferred that the unmodified nano zine oxide described in step 1) is through citric acid pretreatment, processing step is: 1) is dissolved in deionized water by citric acid and forms solution, regulate pH value of solution=4, add nano zine oxide, high-speed stirred；2) carrying out constant temperature back flow reaction, reaction temperature is 80～95 DEG C, response time 0.5～2h, carries out sucking filtration after completion of the reaction, and washing, to pH=7, is then put in baking oven and is dried.
It is further preferred that the mass volume ratio of described citric acid and deionized water is 1g:5mL, the mass ratio of described nano zine oxide and citric acid is 1:4.
It is an advantage of the current invention that: 1, carry out siliceous deposits on the surface of nano zine oxide and modifiy, it is suppressed that the dissolution of nano zine oxide, improve the dispersibility of nano zine oxide.2, further, by citric acid, the hydroxyl of surface of nanometer zinc oxide is carried out bonding reaction, make not easily to reunite between nano granular of zinc oxide, improve the dispersibility of nano zine oxide.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described.
The preparation method of a kind of modified nano zinc oxide of the present invention, its concrete preparation process is:
1) unmodified nano zine oxide be impregnated in the normal hexane solvent of methyl-silicone oil, stir, prepare mixed liquor；
2) mixed liquor that step 1) prepares is evaporated, and is put in baking oven and is dried, prepare the nano zine oxide that methyl-silicone oil is modified；
3) by step 2) the modified nano zine oxide of the methyl-silicone oil for preparing is placed in Muffle furnace, carry out high-temperature roasting, prepare surface deposition and have the nano zine oxide of silicon dioxide, described high-temperature roasting, its roasting process is: under excess oxygen, with the ramp of 5 DEG C/min to 450～550 DEG C, keep 2～4h, make methyl-silicone oil change into silicon dioxide.
Specific implementation process:
1) 25mL methyl-silicone oil is dissolved in 50mL normal hexane solvent, is subsequently adding in 5g nano zine oxide, stirs, prepare mixed liquor；
2) mixed liquor that step 1) prepares is evaporated, and is put in baking oven and is dried, prepare the nano zine oxide that methyl-silicone oil is modified；
3) by step 2) the modified nano zine oxide of the methyl-silicone oil for preparing is placed in Muffle furnace, under excess oxygen, with the ramp of 5 DEG C/min to 450～550 DEG C, keep 2～4h, making methyl-silicone oil change into silicon dioxide, preparing surface deposition has the nano zine oxide of silicon dioxide.
In order to make not easily to reunite between nano granular of zinc oxide, improve the dispersibility of nano zine oxide, by unmodified nano zine oxide through citric acid pretreatment, process step is: 1) is dissolved in by 20g citric acid in 80mL deionized water and forms solution, regulate pH value of solution=4, add nano zine oxide, high-speed stirred；2) carrying out constant temperature back flow reaction, reaction temperature is 80～95 DEG C, response time 0.5～2h, carries out sucking filtration after completion of the reaction, and washing, to pH=7, is then put in baking oven and is dried.
Claims (3)
1. the preparation method of a modified nano zinc oxide, it is characterised in that: concrete preparation process is:
1) unmodified nano zine oxide be impregnated in the normal hexane solvent of methyl-silicone oil, stir, prepare mixed liquor；
2) mixed liquor that step 1) prepares is evaporated, and is put in baking oven and is dried, prepare the nano zine oxide that methyl-silicone oil is modified；
3) by step 2) the modified nano zine oxide of the methyl-silicone oil for preparing is placed in Muffle furnace, carry out high-temperature roasting, prepare surface deposition and have the nano zine oxide of silicon dioxide, described high-temperature roasting, its roasting process is: under excess oxygen, with the ramp of 5 DEG C/min to 450～550 DEG C, keep 2～4h, make methyl-silicone oil change into silicon dioxide;
Unmodified nano zine oxide described in step 1), through citric acid pretreatment, processing step is: 1) is dissolved in deionized water by citric acid and forms solution, regulate pH value of solution=4, add nano zine oxide, high-speed stirred；2) carrying out constant temperature back flow reaction, reaction temperature is 80～95 DEG C, response time 0.5～2h, carries out sucking filtration after completion of the reaction, and washing, to pH=7, is then put in baking oven and is dried.
2. the preparation method of a kind of modified nano zinc oxide according to claim 1, it is characterised in that: the volume ratio of the methyl-silicone oil described in step 1) and normal hexane solvent is 1:2, and the mass volume ratio of described nano zine oxide and methyl-silicone oil is 1g:5mL.
3. the preparation method of a kind of modified nano zinc oxide according to claim 2, it is characterised in that: the mass volume ratio of described citric acid and deionized water is 1g:5mL, and the mass ratio of described nano zine oxide and citric acid is 1:4.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105565367A (en) * | 2016-01-25 | 2016-05-11 | 延安大学 | Preparation method of nanometer zinc oxide powder material |
| CN106006713B (en) * | 2016-07-07 | 2017-12-08 | 安徽省含山县锦华氧化锌厂 | A kind of preparation technology of active nano-ZnO |
| CN107010651A (en) * | 2017-05-15 | 2017-08-04 | 广西放心源生物科技有限公司 | The surface modifying method of nano zine oxide |
| CN107082565A (en) * | 2017-06-12 | 2017-08-22 | 景德镇陶瓷大学 | A kind of photocatalysis antibacterial glaze |
| CN109265020A (en) * | 2018-11-07 | 2019-01-25 | 安徽省绩溪县华宇防火滤料有限公司 | A kind of novel glass fiber size |
| CN114672236A (en) * | 2022-05-09 | 2022-06-28 | 河北宇阳泽丽防水材料有限公司 | High-durability waterborne polyurethane waterproof coating and preparation method thereof |
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| CN103159251A (en) * | 2011-12-15 | 2013-06-19 | 贵州省纳米材料工程中心 | Preparation method for modified transparent nano-zinc oxide sol |
| CN103974906A (en) * | 2011-11-17 | 2014-08-06 | 堺化学工业株式会社 | Surface-treated zinc oxide powder, anti-bacterial agent, and anti-bacterial composition |
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| CN103974906A (en) * | 2011-11-17 | 2014-08-06 | 堺化学工业株式会社 | Surface-treated zinc oxide powder, anti-bacterial agent, and anti-bacterial composition |
| CN103159251A (en) * | 2011-12-15 | 2013-06-19 | 贵州省纳米材料工程中心 | Preparation method for modified transparent nano-zinc oxide sol |
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Inventor after: Wang Peiyu Inventor after: Chen Weilin Inventor before: Zuo Shixiang Inventor before: Zhang Yu |
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Effective date of registration: 20180206 Address after: Room 505, No. 86, rhino North Street, Dongshan District, Guangzhou, Guangdong Province, Guangdong Co-patentee after: Chen Weilin Patentee after: Wang Peiyu Address before: 215400 Suzhou City, Taicang Province Economic Development Zone, Beijing West Road, No. 1, building 6, No. Patentee before: Suzhou Yuxi New Material Technology Co., Ltd. |
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Effective date of registration: 20181207 Address after: Room 2A019, Innovation and Entrepreneurship Service Center, Construction Road, Zhaoqing High-tech Zone, Guangdong 510000 Patentee after: Zhaoqing Shenghao new Mstar Technology Ltd Address before: 510000 Room 505, 86 Rhinoceros North Street, Dongshan District, Guangzhou, Guangdong Province Co-patentee before: Chen Weilin Patentee before: Wang Peiyu |