CN104803408A - Method for preparing modified nano-zinc oxide - Google Patents
Method for preparing modified nano-zinc oxide Download PDFInfo
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- CN104803408A CN104803408A CN201510155846.7A CN201510155846A CN104803408A CN 104803408 A CN104803408 A CN 104803408A CN 201510155846 A CN201510155846 A CN 201510155846A CN 104803408 A CN104803408 A CN 104803408A
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Abstract
The invention discloses a method for preparing modified nano-zinc oxide. Lignosulfonate is introduced in the hydrothermal synthesis process of zinc oxide to serve as a dispersant, so that the dispersity of zinc oxide obtained by hydrothermal synthesis is improved, and later-period drying is facilitated; further, a vibromill is adopted to conduct dispersion and surface modification on dried zinc oxide particles, so that the obtained modified nano-zinc oxide is uniform in particle size distribution, excellent in dispersity, favorable in hydrophobicity and easy to disperse in organic materials.
Description
Technical field
The present invention relates to nano-powder technology of preparing, be specifically related to a kind of preparation method of modified nanometer zinc oxide.
Background technology
Nano zine oxide is a kind of polyfunctional new inorganic material, due to the granular of crystal grain, its Electronic Structure and crystalline structure change, and create surface effects, volume effect, quantum size effect and macroscopical tunnel effect and the feature such as high-clarity, polymolecularity that macro object do not have.Discovered in recent years it in catalysis, optics, magnetics, mechanics etc., show many specific functions, make it have important using value in many fields such as pottery, chemical industry, electronics, optics, biology, medicine, there is singularity and purposes that common zinc oxide cannot compare.
But in application process, nano zine oxide mixes mutually with organism mostly, and on the one hand nano zine oxide has the features such as the large and specific surface energy of specific surface area is large, and self easily reunites; On the other hand, surface of nanometer zinc oxide polarity is comparatively strong, and therefore not easily dispersed in organic medium, this just significantly limit the performance of its nano effect.Therefore must disperse and surface modification nanometer Zinc oxide powder, to reduce its surface energy, regulate hydrophobicity, the wettability between modification and organic polymer material and bonding force, thus the performance improving material to greatest extent.
Summary of the invention
The technical problem to be solved in the present invention is: the preparation method providing a kind of modified nanometer zinc oxide, the modified nanometer zinc oxide good dispersity obtained, and organic materials has good bonding properties.
The solution that the present invention solves its technical problem is: a kind of preparation method of modified nanometer zinc oxide, carries out successively according to following steps:
1) at room temperature, configuration concentration is the zinc solution of 0.2 ~ 0.5mol/L, adds the ratio of 0.15 ~ 0.5g sulfonated lignin according to every 10mL zinc solution, add sulfonated lignin, under continual stirring conditions, dropwise instill alkali lye, till solution clarification;
2) above-mentioned solution is added in autoclave, at 100 ~ 150 DEG C of reaction 10 ~ 14h, be cooled to room temperature;
3) the throw out centrifugation will obtained, deionized water wash;
4) solid after separation is dry at 80 DEG C, obtain Zinc oxide particles;
5) dried Zinc oxide particles adds in vibration mill, adds the titanic acid ester accounting for zinc oxide weight 1 ~ 5% and carries out modification, finally obtain described modified nanometer zinc oxide.
Sulfonated lignin are by products that sulfite pulping cooking waste liquor reclaims, abundance, cheap, belong to renewable resources.The form that sulfonated lignin combine with the sulfonic group of nonpolar aromatic ring side chain and polarity exists, and polar portion determines its surfactivity, can be used as anion surfactant.When it is adsorbed on various organic or inorganic particle, due to the mutual electrostatic repulsion between anionic group and high molecular sterically hindered, make the dispersion state that particle keeps stable, the present invention introduces in the Hydrothermal Synthesis zinc oxide stage dispersiveness that sulfonated lignin effectively can improve the zinc oxide of synthesis.
Vibration mill is the high-frequency vibration utilizing cylinder, grinding medium in cylinder relies on mass force to impact material, acceleration during media impingement material can reach 10g-15g, there is compact construction, energy consumption be low, output is high, properties of powder performace concentrate advantage, the particle diameter of dried Zinc oxide particles can be improved fast, and surface modification is carried out to it simultaneously.
Preferably, in described step 1), zinc solution is zinc nitrate solution or liquor zinci chloridi.
Preferably, in described step 1), alkali lye is sodium carbonate solution, sodium hydroxide solution, sodium acetate soln or ammonia soln.
Preferably, in described step 1), sulfonated lignin are sodium lignosulfonate.
Preferably, in described step 5), vibration mill is Horizontal vibration mill.
Further preferably, when adopting vibration mill grinding, the mass ratio of mill ball and material is 30-50:1, and described mill ball is zirconia ball.
Further, the diameter of described mill ball is 3 ~ 5mm.
The invention has the beneficial effects as follows: the present invention, by introducing sulfonated lignin as dispersion agent in Zinc oxide water thermal synthesis process, the dispersiveness of the nano zine oxide obtained when improving Hydrothermal Synthesis, is convenient to later stage drying; Further, adopt vibration mill to disperse and surface modification dried Zinc oxide particles, make the modified nano zinc oxide even particle size distribution obtained, good dispersity, and there is good hydrophobic performance, be easy to disperse in organic materials.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the modified nanometer zinc oxide that embodiments of the invention 2 obtain.
Embodiment
Below with reference to specific embodiment, preparation method of the present invention is described.
Embodiment 1:
1) at room temperature, configuration concentration is the zinc nitrate solution of 0.2mol/L, adds the ratio of 0.15g sodium lignosulfonate according to every 10mL zinc nitrate solution, add sodium lignosulfonate, under continual stirring conditions, dropwise instill the sodium hydroxide solution of 0.2mol/L, till solution clarification;
2) above-mentioned solution is added in autoclave, at 100 DEG C of reaction 14h, be cooled to room temperature;
3) the throw out centrifugation will obtained, deionized water wash three times;
4) solid after separation is dry at 80 DEG C, obtain Zinc oxide particles;
5) dried Zinc oxide particles adds in Horizontal vibration mill, add the titanic acid ester accounting for zinc oxide weight 1% and carry out modification, the zirconia ball of grinding medium to be diameter be 3 ~ 5mm, the weight ratio of mill ball and material is 30:1, grind about 20min, obtain described modified nanometer zinc oxide sample, test result is in table 1.
Embodiment 2:
1) at room temperature, configuration concentration is the liquor zinci chloridi of 0.5mol/L, adds the ratio of 0.5g sodium lignosulfonate according to every 10mL zinc solution, add sodium lignosulfonate, under continual stirring conditions, dropwise instill the ammonia soln of 3mol/L, till solution clarification;
2) above-mentioned solution is added in autoclave, at 130 DEG C of reaction 12h, be cooled to room temperature;
3) the throw out centrifugation will obtained, deionized water wash 3 times;
4) solid after separation is dry at 80 DEG C, obtain Zinc oxide particles;
5) dried Zinc oxide particles adds in Horizontal vibration mill, add the titanic acid ester accounting for zinc oxide weight 3% and carry out modification, the zirconia ball of grinding medium to be diameter be 3 ~ 5mm, the weight ratio of mill ball and material is 40:1, grind about 20min, obtain described modified nanometer zinc oxide, test result is in table 1, and wherein transmissioning electric mirror test the results are shown in Figure 1.
Embodiment 3:
1) at room temperature, configuration concentration is the zinc acetate solution of 0.35mol/L, adds the ratio of 0.4g sodium lignosulfonate according to every 10mL zinc solution, add sodium lignosulfonate, under continual stirring conditions, dropwise instill 0.2mol/L sodium acetate soln, till solution clarification;
2) above-mentioned solution is added in autoclave, at 150 DEG C of reaction 10h, be cooled to room temperature;
3) the throw out centrifugation will obtained, deionized water wash 3 times;
4) solid after separation is dry at 80 DEG C, obtain Zinc oxide particles;
5) dried Zinc oxide particles adds in Horizontal vibration mill, add the titanic acid ester accounting for zinc oxide weight 5% and carry out modification, the zirconia ball of grinding medium to be diameter be 3 ~ 5mm, the weight ratio of mill ball and material is 50:1, grind about 15min, obtain described modified nanometer zinc oxide sample, test result is in table 1.
Comparative example 1:
1) at room temperature, configuration concentration is the zinc nitrate solution of 0.2mol/L, adds the ratio of 0.15g sodium lignosulfonate according to every 10mL zinc nitrate solution, add sodium lignosulfonate, under continual stirring conditions, dropwise instill the sodium hydroxide solution of 0.2mol/L, till solution clarification;
2) above-mentioned solution is added in autoclave, at 100 DEG C of reaction 14h, be cooled to room temperature;
3) the throw out centrifugation will obtained, deionized water wash three times;
4) solid after separation is dry at 80 DEG C, obtain Zinc oxide particles;
5) dried Zinc oxide particles adds in Horizontal vibration mill, and the zirconia ball of grinding medium to be diameter be 3 ~ 5mm, the weight ratio of mill ball and material is 30:1, grinds about 20min, and obtain nano zine oxide sample, test result is in table 1.
To the zinc oxide sample obtained in embodiment 1-3 and comparative example 1, by laser particle analyzer testing graininess powder granularity, simultaneously by nano zine oxide compressing tablet, the contact angle of throughput supreme people's court test distilled water on compressing tablet, to characterize its hydrophobic performance.Table 1 is test result.
Embodiment 1 is identical with comparative example 1 experiment condition, but do not add titanic acid ester in comparative example 1 and carry out modification, as can be seen from test result, the granularity of titanic acid ester coating modification to powder does not have a significant effect, but its hydrophobicity is had clear improvement, can greatly improve its hydrophobicity, be beneficial to the combination of nano zine oxide and organic materials.
As can be seen from the above-described embodiment, the modified nanometer zinc oxide that preparation method of the present invention obtains, even particle distribution and dispersed better, and hydrophobicity is better, is easy to disperse in organic materials.
Above better embodiment of the present invention is illustrated, but the invention is not limited to described embodiment, those of ordinary skill in the art also can make all equivalent modifications or replacement under the prerequisite without prejudice to spirit of the present invention, and these equivalent modification or replacement are all included in the application's claim limited range.
Claims (7)
1. a preparation method for modified nanometer zinc oxide, is characterized in that, carries out successively according to following steps:
1) at room temperature, configuration concentration is the zinc solution of 0.2 ~ 0.5mol/L, adds the ratio of 0.15 ~ 0.5g sulfonated lignin according to every 10mL zinc solution, add sulfonated lignin, under continual stirring conditions, dropwise instill alkali lye, till solution clarification;
2) above-mentioned solution is added in autoclave, at 100 ~ 150 DEG C of reaction 10 ~ 14h, be cooled to room temperature;
3) the throw out centrifugation will obtained, deionized water wash;
4) solid after separation is dry at 80 DEG C, obtain Zinc oxide particles;
5) dried Zinc oxide particles adds in vibration mill, adds the titanic acid ester accounting for zinc oxide weight 1 ~ 5% and carries out modification; Finally obtain described modified nanometer zinc oxide.
2. the preparation method of modified nanometer zinc oxide according to claim 1, is characterized in that: in described step 1), and zinc solution is zinc nitrate solution or liquor zinci chloridi.
3. the preparation method of modified nanometer zinc oxide according to claim 1, is characterized in that: in described step 1), and alkali lye is any one in sodium carbonate solution, sodium hydroxide solution, sodium acetate soln and ammonia soln.
4. the preparation method of modified nanometer zinc oxide according to claim 1, is characterized in that: in described step 1), and sulfonated lignin are sodium lignosulfonate.
5. the preparation method of modified nanometer zinc oxide according to claim 1, is characterized in that: in described step 5), and vibration mill is Horizontal vibration mill.
6. the preparation method of modified nanometer zinc oxide according to claim 5, is characterized in that: in described step 5), and when adopting vibration mill grinding, the mass ratio of mill ball and material is 30-50:1, and described mill ball is zirconia ball.
7. the preparation method of modified nanometer zinc oxide according to claim 6, is characterized in that: the diameter of described mill ball is 3 ~ 5mm.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106366701A (en) * | 2016-08-24 | 2017-02-01 | 江苏爱特恩高分子材料有限公司 | Preparation method of high-dispersed zinc oxide |
| CN107118592A (en) * | 2017-05-15 | 2017-09-01 | 广西放心源生物科技有限公司 | A kind of preparation method of modified nano zinc oxide |
| CN107904545A (en) * | 2017-11-18 | 2018-04-13 | 张晓娟 | A kind of metal die surface duplex hardening treatment process |
| CN109134820A (en) * | 2018-06-22 | 2019-01-04 | 同济大学 | A kind of anion aqueous polyurethane nano-zinc oxide composite material and preparation method thereof |
| EP3450010A1 (en) * | 2017-08-30 | 2019-03-06 | National Research-Development Institute for Non-ferrous and Rare Metals (IMNR) | Inorganic phase change materials based on potassium nitrate micro encapsulation process in a nanostructured inorganic zinc oxide shell with application in thermal energy storage |
| CN111040267A (en) * | 2019-12-30 | 2020-04-21 | 广州飞粤新材料有限公司 | Alloy rubber and production process thereof |
| CN111704157A (en) * | 2020-05-30 | 2020-09-25 | 上海应用技术大学 | Preparation method of microchannel of nano zinc oxide |
| CN114656824A (en) * | 2022-04-15 | 2022-06-24 | 肇庆市盛浩新材料科技有限公司 | Modified nano zinc oxide powder and preparation method and application thereof |
| US11583924B2 (en) | 2018-12-31 | 2023-02-21 | Tata Consultancy Services Limited | Synthesis of nano particles |
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| CN103408063A (en) * | 2013-08-07 | 2013-11-27 | 江苏大学 | Hydrothermal method for preparation of nano-zinc oxide by taking lignosulphonate as surfactant |
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| CN103408063A (en) * | 2013-08-07 | 2013-11-27 | 江苏大学 | Hydrothermal method for preparation of nano-zinc oxide by taking lignosulphonate as surfactant |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106366701A (en) * | 2016-08-24 | 2017-02-01 | 江苏爱特恩高分子材料有限公司 | Preparation method of high-dispersed zinc oxide |
| CN106366701B (en) * | 2016-08-24 | 2018-02-27 | 江苏爱特恩高分子材料有限公司 | A kind of preparation method of high dispersive zinc oxide |
| CN107118592A (en) * | 2017-05-15 | 2017-09-01 | 广西放心源生物科技有限公司 | A kind of preparation method of modified nano zinc oxide |
| EP3450010A1 (en) * | 2017-08-30 | 2019-03-06 | National Research-Development Institute for Non-ferrous and Rare Metals (IMNR) | Inorganic phase change materials based on potassium nitrate micro encapsulation process in a nanostructured inorganic zinc oxide shell with application in thermal energy storage |
| CN107904545A (en) * | 2017-11-18 | 2018-04-13 | 张晓娟 | A kind of metal die surface duplex hardening treatment process |
| CN109134820A (en) * | 2018-06-22 | 2019-01-04 | 同济大学 | A kind of anion aqueous polyurethane nano-zinc oxide composite material and preparation method thereof |
| CN109134820B (en) * | 2018-06-22 | 2021-03-26 | 同济大学 | Anionic waterborne polyurethane nano zinc oxide composite material and preparation method thereof |
| US11583924B2 (en) | 2018-12-31 | 2023-02-21 | Tata Consultancy Services Limited | Synthesis of nano particles |
| CN111040267A (en) * | 2019-12-30 | 2020-04-21 | 广州飞粤新材料有限公司 | Alloy rubber and production process thereof |
| CN111704157A (en) * | 2020-05-30 | 2020-09-25 | 上海应用技术大学 | Preparation method of microchannel of nano zinc oxide |
| CN114656824A (en) * | 2022-04-15 | 2022-06-24 | 肇庆市盛浩新材料科技有限公司 | Modified nano zinc oxide powder and preparation method and application thereof |
| CN114656824B (en) * | 2022-04-15 | 2023-08-11 | 肇庆市盛浩新材料科技有限公司 | Modified nano zinc oxide powder and preparation method and application thereof |
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