CN105000589B - Citric acid-modified nanometer zinc oxide - Google Patents
Citric acid-modified nanometer zinc oxide Download PDFInfo
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- CN105000589B CN105000589B CN201510425763.5A CN201510425763A CN105000589B CN 105000589 B CN105000589 B CN 105000589B CN 201510425763 A CN201510425763 A CN 201510425763A CN 105000589 B CN105000589 B CN 105000589B
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- nano zine
- zine oxide
- citric acid
- zinc oxide
- nanometer zinc
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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, and in particular 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 sun care preparationss, nanometer
The fields such as function textile, functional plastics and coating.However, nano zine oxide is a kind of inorganic oxide, its size is little, table
Face can high and organic principle be difficult compatible, easily produce serious agglomeration.It is therefore desirable to the surface to nano zine oxide
It is modified.
Patent ZL200910064705.9 discloses a kind of nano zinc oxide surface modifying method, and it includes step：1）Will
Nanometer Zinc oxide powder is disperseed in the mixed solution of deionized water and cosolvent；2）By tetraethyl orthosilicate and/or just
The dressing agent of quanmethyl silicate and organosilan composition is mixed homogeneously with cosolvent, and stirring is added in above-mentioned slurry, adjusts pH value
Reacted for 8~12.The invention adopts common liquid phase chemical reaction method, is completed in nano zine oxide by single step reaction
Grain surface modification last layer Organic substance/SiO2Hybrid material, so as to reduce the photocatalytic activity of nano zine oxide, but during its reaction
Between and follow-up product disengaging time it is longer, and be unfavorable for industrialized production.
The content of the invention
Present invention aims to the problem that nano zine oxide is easily reunited in prior art and a kind of citric acid is provided
Modified nano zine oxide.
Realize technical scheme that the object of the invention adopts for：A kind of nano zine oxide of citric acid-modified, it is by walking as follows
It is rapid to be obtained：
1）Citric acid is dissolved in deionized water and forms solution, adjust pH value of solution=4, add nano zine oxide, high-speed stirring
Mix；
2）Constant temperature back flow reaction is carried out, reaction temperature is 80~90 DEG C, and 1~2h of response time is taken out after completion of the reaction
Filter, washs to pH=7, is then put in baking oven and is dried, that is, modified nano zine oxide is obtained.
Preferably, step 1）Described in the mass volume ratio of citric acid and deionized water be 1g：10mL, described nanometer
Zinc Oxide is 1 with the mass ratio of citric acid：（1~3）.
Further, during modified nano zine oxide impregnated in the normal hexane solvent of tetraethyl orthosilicate, stir,
Prepared mixed liquor；Then obtained mixed liquor is evaporated, and is put in baking oven and is dried, deposition tetraethyl orthosilicate is obtained
Nano zine oxide；Finally the nano zine oxide of obtained deposition tetraethyl orthosilicate is placed in Muffle furnace, high-temperature roasting is carried out,
Prepared surface deposition has the nano zine oxide of silicon dioxide.
Wherein, described tetraethyl orthosilicate and the volume ratio of normal hexane solvent are 1：2, described nano zine oxide and positive silicon
The mass volume ratio of acetoacetic ester is 1g：5mL.
Preferably, described high-temperature roasting, its roasting process is：Under excess oxygen, with the ramp of 5 DEG C/min extremely
450~550 DEG C, 2~4h is kept, make tetraethyl orthosilicate change into silicon dioxide.
It is highly preferred that secondary or secondary above siliceous deposits can be carried out.
It is an advantage of the current invention that：1st, there is bonding reaction to the hydroxyl of surface of nanometer zinc oxide from citric acid, make to receive
It is difficult to reunite between rice Zinc oxide particles, improves the dispersibility of nano zine oxide；2nd, further, in the table of nano zine oxide
Face carries out siliceous deposits and is modified, it is suppressed that the dissolution of nano zine oxide, improves the dispersibility of nano zine oxide.
Specific embodiment
The present invention is further described with reference to embodiment.
Embodiment 1
1）5g citric acids are dissolved in 50mL deionized waters and form solution, adjust pH value of solution=4, add 5g nano zine oxides,
High-speed stirred；
2）Constant temperature back flow reaction is carried out, reaction temperature is 80 DEG C, and response time 2h carries out after completion of the reaction sucking filtration, washing
To pH=7, then it is put in baking oven and is dried, that is, modified nano zine oxide is obtained.
Embodiment 2
1）10g citric acids are dissolved in 50mL deionized waters and form solution, adjust pH value of solution=4, add 5g nano oxidized
Zinc, high-speed stirred；
2）Constant temperature back flow reaction is carried out, reaction temperature is 85 DEG C, and response time 1h carries out after completion of the reaction sucking filtration, washing
To pH=7, then it is put in baking oven and is dried, that is, modified nano zine oxide is obtained.
Embodiment 3
1）15g citric acids are dissolved in 50mL deionized waters and form solution, adjust pH value of solution=4, add 5g nano oxidized
Zinc, high-speed stirred；
2）Constant temperature back flow reaction is carried out, reaction temperature is 90 DEG C, and response time 1h carries out after completion of the reaction sucking filtration, washing
To pH=7, then it is put in baking oven and is dried, that is, modified nano zine oxide is obtained.
Embodiment 4
In order to further improve the dispersibility of nano zine oxide, embodiment 4 is to the modified nanometer obtained by embodiment 1
Zinc Oxide is further modified.
1）25mL tetraethyl orthosilicates are dissolved in the alcohol solvent of 50mL, 5 grams of nano zine oxides are subsequently adding, stirring is equal
It is even, mixed liquor is obtained；
2）By step 1）Obtained mixed liquor is evaporated at 80 DEG C of bath temperature, and is put in baking oven and is dried,
The nano zine oxide of deposition tetraethyl orthosilicate is obtained；
3）By step 2）The nano zine oxide of obtained deposition tetraethyl orthosilicate is placed in Muffle furnace, under excess oxygen,
With the ramp of 5 DEG C/min to 500 DEG C, 3h is incubated, makes tetraethyl orthosilicate change into silicon dioxide, that is, surface siliceous deposits is obtained
Modified nano zine oxide.
In order to further improve coverage effect, secondary or secondary above siliceous deposits can be carried out.
Claims (2)
1. a kind of nano zine oxide of citric acid-modified, it is characterised in that：It is obtained by following steps：
1）Citric acid is dissolved in deionized water and forms solution, adjust pH value of solution=4, add nano zine oxide, high-speed stirred；
2）Constant temperature back flow reaction is carried out, reaction temperature is 80~90 DEG C, and 1~2h of response time carries out after completion of the reaction sucking filtration, washes
Wash to pH=7, be then put in baking oven and be dried, that is, modified nano zine oxide is obtained；
3）During modified nano zine oxide impregnated in the normal hexane solvent of tetraethyl orthosilicate, stir, mixed liquor is obtained；
Then obtained mixed liquor is evaporated, and is put in baking oven and is dried, the nano oxidized of deposition tetraethyl orthosilicate is obtained
Zinc；Finally the nano zine oxide of obtained deposition tetraethyl orthosilicate is placed in Muffle furnace, high-temperature roasting is carried out, surface is obtained and is sunk
Product has the nano zine oxide of silicon dioxide；
Wherein, step 1）Described in the mass volume ratio of citric acid and deionized water be 1g：10mL, described nano zine oxide
It is 1 with the mass ratio of citric acid：（1~3）；
Wherein, step 3）Described in the volume ratio of tetraethyl orthosilicate and normal hexane solvent be 1：2, described nano zine oxide with
The mass volume ratio of tetraethyl orthosilicate is 1g：5mL；
Wherein, step 3）Described in high-temperature roasting, its roasting process is：Under excess oxygen, with the ramp of 5 DEG C/min
To 450~550 DEG C, 2~4h is incubated, makes tetraethyl orthosilicate change into silicon dioxide.
2. the nano zine oxide of a kind of citric acid-modified according to claim 1, it is characterised in that：Carry out secondary or secondary
Above siliceous deposits.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN107312362B (en) * | 2017-06-06 | 2018-07-17 | 安徽锦华氧化锌有限公司 | A kind of processing method for improving nano zine oxide and using 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 |
Citations (1)
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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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)
| Title |
|---|
| 反胶束体系中Fe3O4/SiO2核壳结构纳米粒子的制备和表征;马明等;《东南大学学报(自然科学版)》;20090731;第39卷(第4期);799-802 * |
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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. |
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