CN105000589A - Citric acid-modified nanometer zinc oxide - Google Patents
Citric acid-modified nanometer zinc oxide Download PDFInfo
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- CN105000589A CN105000589A CN201510425763.5A CN201510425763A CN105000589A CN 105000589 A CN105000589 A CN 105000589A CN 201510425763 A CN201510425763 A CN 201510425763A CN 105000589 A CN105000589 A CN 105000589A
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- nano zine
- zine oxide
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Abstract
The invention relates to the technical field of nano-materials, and particularly discloses a citric acid-modified nanometer zinc oxide. The nanometer zinc oxide is prepared through the steps of 1) dissolving the citric acid in deionized water to form a solution, adjusting the pH value of the solution to be 4, adding the nanometer zinc oxide and stirring at a high speed; 2) conducting the constant reflux reaction, controlling the reaction temperature and the reaction time of the constant reflux reaction to be 80-95 DEG C and 0.5-2 hours respectively, conducting the suction filtration after the completion of the constant reflux reaction, washing to enable the pH value of the solution to be 7, and drying in a baking oven to obtain the modified nanometer zinc oxide. The citric acid is adopted for being subjected to the bonding reaction with hydroxyl groups on the surface of the nanometer zinc oxide, so that nanometer zinc oxide particles are less prone to agglomeration. The dispersibility of nanometer zinc oxide particles is improved. Furthermore, the silicon deposition and modification is conducted on the surface of the nanometer zinc oxide, so that the dissolution of zinc is inhibited. Therefore, the dispersibility of the nanometer zinc oxide is improved.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of nano zine oxide of citric acid-modified.
Background technology
Nano zine oxide is a kind of inorganic UV shield agent 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, its size is little, surface energy is high, be difficult to compatible with organic composition, very easily produces serious agglomeration.Therefore the modifying surface to nano zine oxide is necessary.
Patent ZL200910064705.9 discloses a kind of nano zinc oxide surface modifying method, and it comprises step: 1) disperseed in the mixing solutions of deionized water and solubility promoter by nanometer Zinc oxide powder; 2) mixed with solubility promoter by the modifier of tetraethyl orthosilicate and/or positive quanmethyl silicate and organosilane composition, stirring adds in above-mentioned slurry, and adjust ph is 8 ~ 12 to react.This invention adopts common liquid phase chemical reaction method, is completed at nano granular of zinc oxide finishing last layer organism/SiO by single step reaction
2hybrid material, thus reduce the photocatalytic activity of nano zine oxide, but its reaction times and the follow-up product separation time longer, and be unfavorable for suitability for industrialized production.
Summary of the invention
The object of the invention is to the problem of easily reuniting for nano zine oxide in prior art and a kind of nano zine oxide of citric acid-modified is provided.
The technical scheme realizing the object of the invention employing is: a kind of nano zine oxide of citric acid-modified, and it is obtained by following steps:
1) be dissolved in deionized water by citric acid and form solution, regulator solution pH=4, adds nano zine oxide, high-speed stirring;
2) carry out constant temperature back flow reaction, temperature of reaction is 80 ~ 90 DEG C, and reaction times 1 ~ 2h carries out suction filtration after completion of the reaction, washs to pH=7, is then put in baking oven and carries out drying, i.e. the nano zine oxide of obtained modification.
Preferably, the mass volume ratio of the citric acid described in step 1) and deionized water is 1g:10mL, and described nano zine oxide and the mass ratio of citric acid are 1:(1 ~ 3).
Further, modified nano zine oxide be impregnated in the normal hexane solvent of tetraethoxy, stir, obtained mixed solution; Then obtained mixed solution is carried out evaporate to dryness, and be put in baking oven and carry out drying, the nano zine oxide of obtained deposition tetraethoxy; Finally the nano zine oxide of obtained deposition tetraethoxy is placed in retort furnace, carries out high-temperature roasting, obtained surface deposition has the nano zine oxide of silicon-dioxide.
Wherein, the volume ratio of described tetraethoxy and normal hexane solvent is 1:2, and described nano zine oxide and the mass volume ratio of tetraethoxy are 1g:5mL.
Preferably, described high-temperature roasting, its roasting process is: under excess oxygen, with ramp to 450 ~ 550 DEG C of 5 DEG C/min, keeps 2 ~ 4h, makes tetraethoxy change into silicon-dioxide.
More preferably, secondary or the above siliceous deposits of secondary can be carried out.
The invention has the advantages that: 1, select citric acid to the hydroxyl generation bonding reaction of surface of nanometer zinc oxide, make not easily to reunite between nano granular of zinc oxide, improve the dispersiveness of nano zine oxide; 2, further, carry out siliceous deposits modification on the surface of nano zine oxide, inhibit the stripping of nano zine oxide, improve the dispersiveness of nano zine oxide.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
embodiment 1
1) 5g citric acid is dissolved in 50mL deionized water forms solution, regulator solution pH=4, add 5g nano zine oxide, high-speed stirring;
2) carry out constant temperature back flow reaction, temperature of reaction is 80 DEG C, and reaction times 2h carries out suction filtration after completion of the reaction, washs to pH=7, is then put in baking oven and carries out drying, i.e. the nano zine oxide of obtained modification.
embodiment 2
1) 10g citric acid is dissolved in 50mL deionized water forms solution, regulator solution pH=4, add 5g nano zine oxide, high-speed stirring;
2) carry out constant temperature back flow reaction, temperature of reaction is 85 DEG C, and reaction times 1h carries out suction filtration after completion of the reaction, washs to pH=7, is then put in baking oven and carries out drying, i.e. the nano zine oxide of obtained modification.
embodiment 3
1) 15g citric acid is dissolved in 50mL deionized water forms solution, regulator solution pH=4, add 5g nano zine oxide, high-speed stirring;
2) carry out constant temperature back flow reaction, temperature of reaction is 90 DEG C, and reaction times 1h carries out suction filtration after completion of the reaction, washs to pH=7, is then put in baking oven and carries out drying, i.e. the nano zine oxide of obtained modification.
embodiment 4
In order to improve the dispersiveness of nano zine oxide further, embodiment 4 carries out modification further to the nano zine oxide of the modification obtained by embodiment 1.
1) 25mL tetraethoxy is dissolved in the alcohol solvent of 50mL, then adds 5 grams of nano zine oxides, stir, obtained mixed solution;
2) mixed solution obtained for step 1) is carried out evaporate to dryness at bath temperature 80 DEG C, and be put in baking oven and carry out drying, the nano zine oxide of obtained deposition tetraethoxy;
3) by step 2) nano zine oxide of obtained deposition tetraethoxy is placed in retort furnace, under excess oxygen, with the ramp to 500 DEG C of 5 DEG C/min, insulation 3h, tetraethoxy is made to change into silicon-dioxide, the nano zine oxide that namely obtained surface silicon is deposition modified.
In order to improve coverage effect further, secondary or the above siliceous deposits of secondary can be carried out.
Claims (6)
1. a nano zine oxide for citric acid-modified, is characterized in that: obtained by following steps:
1) be dissolved in deionized water by citric acid and form solution, regulator solution pH=4, adds nano zine oxide, high-speed stirring;
2) carry out constant temperature back flow reaction, temperature of reaction is 80 ~ 90 DEG C, and reaction times 1 ~ 2h carries out suction filtration after completion of the reaction, washs to pH=7, is then put in baking oven and carries out drying, i.e. the nano zine oxide of obtained modification.
2. the nano zine oxide of a kind of citric acid-modified according to claim 1, it is characterized in that: the mass volume ratio of the citric acid described in step 1) and deionized water is 1g:10mL, and described nano zine oxide and the mass ratio of citric acid are 1:(1 ~ 3).
3. the nano zine oxide of a kind of citric acid-modified according to claim 1, is characterized in that: be impregnated in the normal hexane solvent of tetraethoxy by modified nano zine oxide, stir, obtained mixed solution; Then obtained mixed solution is carried out evaporate to dryness, and be put in baking oven and carry out drying, the nano zine oxide of obtained deposition tetraethoxy; Finally the nano zine oxide of obtained deposition tetraethoxy is placed in retort furnace, carries out high-temperature roasting, obtained surface deposition has the nano zine oxide of silicon-dioxide.
4. the nano zine oxide of a kind of citric acid-modified according to claim 3, is characterized in that: the volume ratio of described tetraethoxy and normal hexane solvent is 1:2, and described nano zine oxide and the mass volume ratio of tetraethoxy are 1g:5mL.
5. the nano zine oxide of a kind of citric acid-modified according to claim 3, it is characterized in that: described high-temperature roasting, its roasting process is: under excess oxygen, with ramp to 450 ~ 550 DEG C of 5 DEG C/min, insulation 2 ~ 4h, makes tetraethoxy change into silicon-dioxide.
6. the nano zine oxide of a kind of citric acid-modified according to claim 3, is characterized in that: carry out secondary or the above siliceous deposits of secondary.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517307A (en) * | 2016-10-31 | 2017-03-22 | 苏州宇希新材料科技有限公司 | Preparation method for oil soluble nano zinc oxide |
| CN107082565A (en) * | 2017-06-12 | 2017-08-22 | 景德镇陶瓷大学 | A kind of photocatalysis antibacterial glaze |
| CN107099158A (en) * | 2017-05-27 | 2017-08-29 | 湖北中能木业有限公司 | A kind of preparation method of the plain plate of multifunctional fibre |
| CN107312362A (en) * | 2017-06-06 | 2017-11-03 | 安徽锦华氧化锌有限公司 | It is a kind of to improve the processing method that nano zine oxide uses characteristic |
| CN108502916A (en) * | 2018-06-13 | 2018-09-07 | 宣城晶瑞新材料有限公司 | A kind of novel nano zinc oxide material prepares and application |
| CN110041678A (en) * | 2019-05-09 | 2019-07-23 | 马鞍山卓凡新材料科技有限公司 | A kind of preparation method of toy for children antibacterial wear-resistant plastic |
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| CN103360854A (en) * | 2012-03-28 | 2013-10-23 | 厦门纳诺泰克科技有限公司 | High-transparency low-radiation energy-saving combined material for glass and preparation method thereof |
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| CN103360854A (en) * | 2012-03-28 | 2013-10-23 | 厦门纳诺泰克科技有限公司 | High-transparency low-radiation energy-saving combined material for glass and preparation method thereof |
Non-Patent Citations (1)
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| 马明等: "反胶束体系中Fe3O4/SiO2核壳结构纳米粒子的制备和表征", 《东南大学学报(自然科学版)》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517307A (en) * | 2016-10-31 | 2017-03-22 | 苏州宇希新材料科技有限公司 | Preparation method for oil soluble nano zinc oxide |
| CN106517307B (en) * | 2016-10-31 | 2017-12-01 | 苏州宇希新材料科技有限公司 | A kind of preparation method of oil solubility nanometer zinc oxide |
| CN107099158A (en) * | 2017-05-27 | 2017-08-29 | 湖北中能木业有限公司 | A kind of preparation method of the plain plate of multifunctional fibre |
| CN107312362A (en) * | 2017-06-06 | 2017-11-03 | 安徽锦华氧化锌有限公司 | It is a kind of to improve the processing method that nano zine oxide uses characteristic |
| CN107082565A (en) * | 2017-06-12 | 2017-08-22 | 景德镇陶瓷大学 | A kind of photocatalysis antibacterial glaze |
| CN108502916A (en) * | 2018-06-13 | 2018-09-07 | 宣城晶瑞新材料有限公司 | A kind of novel nano zinc oxide material prepares and application |
| CN110041678A (en) * | 2019-05-09 | 2019-07-23 | 马鞍山卓凡新材料科技有限公司 | A kind of preparation method of toy for children antibacterial wear-resistant plastic |
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| CN105000589B (en) | 2017-05-17 |
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Effective date of registration: 20191106 Address after: Magi Road, Changshu high tech Industrial Development Zone, Suzhou City, Jiangsu Province, No. 1 215500 Patentee after: Suzhou Hui Xin bang Mstar Technology Ltd 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: 20210120 Address after: 215400 No. 20, Jian Xiong Road, science and Education Town, Taicang, Suzhou, Jiangsu Patentee after: SUZHOU YUANLUE INTELLECTUAL PROPERTY OPERATION Co.,Ltd. Address before: 215400 1 1 Beijing West Road, Taicang Economic Development Zone, Suzhou, Jiangsu. Patentee before: SUZHOU YUXI NEW MATERIAL TECHNOLOGY Co.,Ltd. |