CN103588239A - Method for preparing nano-zinc oxide by hydrothermal method - Google Patents
Method for preparing nano-zinc oxide by hydrothermal method Download PDFInfo
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- CN103588239A CN103588239A CN201310296843.6A CN201310296843A CN103588239A CN 103588239 A CN103588239 A CN 103588239A CN 201310296843 A CN201310296843 A CN 201310296843A CN 103588239 A CN103588239 A CN 103588239A
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Abstract
The invention discloses a method for preparing nano-zinc oxide by a hydrothermal method. The method comprises the following step: by taking lignosulphonate as a surfactant, carrying out reaction on zinc nitrate and sodium hydroxide to prepare nano-zinc oxide by the hydrothermal method. Lignosulphonate is a byproduct of pulping by a sulfurous method, and has abundant functional groups and good diffusivity. By adopting lignosulphonate as the surfactant, nano-zinc oxide is prepared by the hydrothermal method. The method is easy to control in operating condition, simple in equipment and low in preparation cost. The prepared product is uniform in particle distribution, high in particle performance, good in grain size dispersibility, smaller in split reuniting degree, better in shape and easy for industrialization.
Description
Technical field
The present invention relates to a kind of method of preparing nano zinc oxide by hydro thermal method, the sulfonated lignin of particularly take are prepared the method for nano zine oxide as tensio-active agent.
Background technology
In recent years, semiconductor material is because it is applied widely and has obtained deep research.The zinc oxide with wide forbidden band (337eV) and large exciton binding energy (60eV) is a kind of material that has semi-conductor and piezoelectric property simultaneously and cause thus various peculiar properties.Nano zine oxide, as a kind of new function type nano material, is compared with conventional oxidation Zinc material, and it has, and specific surface area is large, chemically reactive is higher, the product granularity advantage such as be nano level.Due to the peculiar surface effects of nano material, quantum size effect and macro quanta tunnel effect etc., make nano zine oxide at aspects such as magnetic, optical, electrical, chemical, physics, susceptibility than the incomparable property of general zinc oxide product and new purposes, can be used to manufacture gas sensor, fluor, UV-preventing material, varistor, image recording material, pressure sensitive, piezoelectric, effective catalyst etc., in rubber, coating, ink, color stuffing, catalyzer, the cosmetics of super quality and medicine and other fields, show wide application prospect.
Hydrothermal method is called again hydrothermal method, refer in special closed reactor (autoclave), adopt the aqueous solution as reaction system, by reaction system is heated, produce the environment of a High Temperature High Pressure, speeding-up ion reaction and facilitation of hydrolysis reaction are prepared oxide compound in the aqueous solution or steam flow, through separated and thermal treatment, obtain oxide nano-particles again, can make some very slow thermodynamical reaction realization responses under hydrothermal condition of speed of reaction at normal temperatures and pressures rapid.The present invention be take sulfonated lignin as tensio-active agent, adopt preparing nano zinc oxide by hydro thermal method, operational condition is easy to control, and equipment is simple, and preparation cost is low, made product even particle distribution, particle performance is high, and Particle dispersity is good, and split reunion degree is less, pattern is better, is easy to realize industrialization.
summary of the invention
The object of the invention is to adopt sulfonated lignin is tensio-active agent, and by hydrothermal method synthesis of nano-zinc oxide, technique is simple, and raw material is easy to obtain, with low cost, of reduced contamination, is suitable for suitability for industrialized production.
Technical scheme of the present invention is as follows:
Under A, room temperature, getting concentration is 0.1 mol ﹒ L
-1zinc solution, by every 50mL zinc solution, add 0.05-0.2g sulfonated lignin, stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1naOH solution, until solution clarification just;
B, above-mentioned solution is moved in autoclave, at 100-200 ℃ of temperature, react 10-22h, be cooled to room temperature;
C, by the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then with dehydrated alcohol, cleans 3 times centrifugation;
D, the solid after separation is put into the dry 12h of thermostatic drying chamber, the temperature of described thermostatic drying chamber is 60 ℃;
In a more excellent open example of the present invention, described sulfonated lignin are sodium lignosulfonates.
In a more excellent open example of the present invention, zinc salt used is Zn (NO
3)
2.
In a more excellent open example of the present invention, in steps A, by every 50mL zinc solution, add 0.1-0.15g sulfonated lignin.
In a more excellent open example of the present invention, in step B, in autoclave, at 150 ℃ of temperature, react 14-18h.
This is tested reagent used and is all analytical pure, is commercially available.
beneficial effect
The present invention be take sulfonated lignin as tensio-active agent, adopt preparing nano zinc oxide by hydro thermal method, operational condition is easy to control, and equipment is simple, and preparation cost is low, made product even particle distribution, particle performance is high, and Particle dispersity is good, and split reunion degree is less, pattern is better, is easy to realize industrialization.
Accompanying drawing explanation
The X ray diffracting spectrum of Fig. 1 sample (XRD) is the XRD figure spectrum of embodiment 2 samples.
The scanning electron microscope (SEM) photograph of Fig. 2 sample (SEM) is the SEM figure of embodiment 1 sample.
embodiment
Below in conjunction with concrete embodiment, the present invention will be further described, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
embodiment 1
Under room temperature, getting concentration is 0.1 mol ﹒ L
-1zn (NO
3)
2solution, by every 50mL Zn (NO
3)
2solution adds 0.2g sodium lignosulfonate, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1naOH solution, until solution clarification just; Above-mentioned solution is moved in autoclave, at 100 ℃ of temperature, react 18h, be cooled to room temperature; By the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then with dehydrated alcohol, cleans 3 times centrifugation; Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.The SEM figure of sample is as Fig. 2.
embodiment 2
Under room temperature, getting concentration is 0.1 mol ﹒ L
-1zn (NO
3)
2solution, by every 50mL Zn (NO
3)
2solution adds 0.1g sodium lignosulfonate, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1naOH solution, until solution clarification just; Above-mentioned solution is moved in autoclave, at 100 ℃ of temperature, react 22h, be cooled to room temperature; By the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then with dehydrated alcohol, cleans 3 times centrifugation; Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.The XRD figure of sample is as Fig. 1.
embodiment 3
Under room temperature, getting concentration is 0.1 mol ﹒ L
-1zn (NO
3)
2solution, by every 50mL Zn (NO
3)
2solution adds 0.1g sodium lignosulfonate, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1naOH solution, until solution clarification just; Above-mentioned solution is moved in autoclave, at 100 ℃ of temperature, react 10h, be cooled to room temperature; By the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then with dehydrated alcohol, cleans 3 times centrifugation; Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.
embodiment 4
Under room temperature, getting concentration is 0.1 mol ﹒ L
-1zn (NO
3)
2solution, by every 50mL Zn (NO
3)
2solution adds 0.05g sodium lignosulfonate, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1naOH solution, until solution clarification just; Above-mentioned solution is moved in autoclave, at 150 ℃ of temperature, react 14h, be cooled to room temperature; By the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then with dehydrated alcohol, cleans 3 times centrifugation; Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.
embodiment 5
Under room temperature, getting concentration is 0.1 mol ﹒ L
-1zn (NO
3)
2solution, by every 50mLZn (NO
3)
2solution adds 0.2g sodium lignosulfonate, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1naOH solution, until solution clarification just; Above-mentioned solution is moved in autoclave, at 200 ℃ of temperature, react 18h, be cooled to room temperature; By the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then with dehydrated alcohol, cleans 3 times centrifugation; Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.
embodiment 6
Under room temperature, getting concentration is 0.1 mol ﹒ L
-1zn (NO
3)
2solution, by every 50mL Zn (NO
3)
2solution adds 0.15g sodium lignosulfonate, and stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1naOH solution, until solution clarification just; Above-mentioned solution is moved in autoclave, at 100 ℃ of temperature, react 14h, be cooled to room temperature; By the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then with dehydrated alcohol, cleans 3 times centrifugation; Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.
Claims (5)
1. a method for preparing nano zinc oxide by hydro thermal method, carry out in the steps below:
Under A, room temperature, getting concentration is 0.1 mol ﹒ L
-1zinc solution, by every 50mL zinc solution, add 0.05-0.2g sulfonated lignin, stirring and dissolving, under continuously stirring, dropwise splashes into 2 mol ﹒ L
-1naOH solution, until solution clarification just;
B, above-mentioned solution is moved in autoclave, at 100-200 ℃ of temperature, react 10-22h, be cooled to room temperature;
C, by the centrifugation of gained precipitation mixture, precipitate with deionized water is cleaned 3 times, then with dehydrated alcohol, cleans 3 times centrifugation;
D, the solid after separation is put into the dry 12h of thermostatic drying chamber, the temperature of described thermostatic drying chamber is 60 ℃.
2. according to a kind of method that adopts preparing nano zinc oxide by hydro thermal method described in claim 1, it is characterized in that described sulfonated lignin are sodium lignosulfonates.
3. according to a kind of method that adopts preparing nano zinc oxide by hydro thermal method described in claim 1, it is characterized in that the zinc salt described in steps A is Zn (NO
3)
2.
4. according to a kind of method that adopts preparing nano zinc oxide by hydro thermal method described in claim 1, it is characterized in that by every 50mL zinc solution, adding 0.1-0.15g sulfonated lignin in steps A.
5. according to a kind of method that adopts preparing nano zinc oxide by hydro thermal method described in claim 1, it is characterized in that in autoclave, at 150 ℃ of temperature, reacting 14-18h in step B.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553801A (en) * | 2018-11-19 | 2019-04-02 | 青岛中科和源新材料有限公司 | A kind of preparation of zinc electroplating bath |
| CN115652616A (en) * | 2022-10-31 | 2023-01-31 | 现代纺织技术创新中心(鉴湖实验室) | Light aging resistant protective radiation refrigeration filler particle and coating, and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591037A (en) * | 2009-07-03 | 2009-12-02 | 北京化工大学 | A kind of one-dimensional zinc oxide nanometer material and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591037A (en) * | 2009-07-03 | 2009-12-02 | 北京化工大学 | A kind of one-dimensional zinc oxide nanometer material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 郭元茹等: "以木质素磺酸钠为结构导向剂直接沉淀法制备纳米氧化锌的研究", 《黑龙江大学自然科学学报》, vol. 29, no. 3, 30 June 2012 (2012-06-30), pages 359 - 362 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553801A (en) * | 2018-11-19 | 2019-04-02 | 青岛中科和源新材料有限公司 | A kind of preparation of zinc electroplating bath |
| CN115652616A (en) * | 2022-10-31 | 2023-01-31 | 现代纺织技术创新中心(鉴湖实验室) | Light aging resistant protective radiation refrigeration filler particle and coating, and preparation method and application thereof |
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