CN101497457A - Method for preparing nano zinc oxide compound powder using natural polysaccharide - Google Patents
Method for preparing nano zinc oxide compound powder using natural polysaccharide Download PDFInfo
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- CN101497457A CN101497457A CNA2009100679859A CN200910067985A CN101497457A CN 101497457 A CN101497457 A CN 101497457A CN A2009100679859 A CNA2009100679859 A CN A2009100679859A CN 200910067985 A CN200910067985 A CN 200910067985A CN 101497457 A CN101497457 A CN 101497457A
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Abstract
The invention relates to a method for preparing nano-zinc oxide composite powder from natural polysaccharide. Starch or carboxymethyl cellulose sodium is dissolved into hot water, the mass concentration is between 0.1 and 1 percent, and then the solution is cooled to the room temperature; zinc nitrate hexahydrate is added and dissolved into the solution, and the concentration of zinc nitrate is 0.1mol/L; the solution is constantly stirred, 0.2mol/L of sodium hydroxide solution with equal volume is dripped into the solution, and the dripping time is between 1 and 2 hours; the solution continues to react for 2 hours after the dripping is finished; a compound obtained by centrifugal separation is washed by water; the compound is dried at a temperature of between 80 and 130 DEG C, and zinc hydroxide is converted into zinc oxide; and the nano-zinc oxide/starch composite powder or nano-zinc oxide/carboxymethyl cellulose sodium composite powder is obtained. The starch and cellulose come from natural plants and are cheap, and the application of the prepared nano-zinc oxide composite powder can be extended in the field of biological medicine. A glucoside structure of the starch and the carboxymethyl cellulose sodium can control the granularity during the generation of the zinc oxide, and can prevent generated nano-zinc oxide from producing large agglomeration at the same time.
Description
Technical field
The present invention relates to a kind of method for preparing nano zinc oxide composite powder with natural polysaccharide.Belong to inorganic-natural polymer composite granule technology of preparing.
Background technology
Zinc oxide is a kind of n N-type semiconductorN material, and nano zine oxide has physical influences such as quantum confined effect, surface effects, macro quanta tunnel effect; Performance at aspects such as magnetic, light, electricity, mechanics, chemistry makes nano zine oxide be widely used in industries such as electronics, chemical industry, information, weaving, medicine.Adopt more nano-ZnO preparation that solid phase method, liquid phase method and vapor phase process are arranged at present.Wherein solution deposit prepares nano zine oxide and has that technology is simple, good product quality, is easy to advantages such as control, production cost is low, is the preparation method of tool development prospect.Usually the nano zinc oxide particles surface energy is big, and adsorption is strengthened between particle, forms coacervate, and loses the nano-powder characteristic.The most cost height of various nano zine oxide surface modifying methods, easily pollution.Develop a kind of environmental protection, preparation method easy and simple to handle, low-cost nano zinc oxide composite powder has important practical significance.
Summary of the invention
The object of the present invention is to provide a kind of environmental protection, the method for preparing nano zinc oxide composite powder with natural polysaccharide easy and simple to handle, low-cost; Prepare nano zine oxide as stablizer and prevent the nano zine oxide reunion with natural polysaccharide, improve biocompatibility, the expansion nano zine oxide is in the application of biomedicine field.
For achieving the above object, the present invention is realized by following technical proposals.
The preparation method of nano zinc oxide composite powder of the present invention, it is characterized in that respectively with starch or Xylo-Mucine preparing nano zine oxide/starch composite granule or nano zine oxide/Xylo-Mucine composite granule at aqueous phase with solution deposit as the stablizer of nano zine oxide.
The preparation method of a kind of nano zinc oxide composite powder of the present invention is: starch or Xylo-Mucine are dissolved in the hot water, and mass concentration is 0.1%-1%, cool to room temperature then; Add zinc nitrate hexahydrate and be dissolved in the above-mentioned solution, zinc nitrate concentration is 0.1mol/L; Constantly stir, drip isopyknic 0.2mol/L sodium hydroxide solution in solution, the dropping time is 1-2 hour; After dropwising, continue reaction 2 hours; The mixture that centrifugation obtains washes with water; 80 ℃ of-130 ℃ of dryings, zinc hydroxide is changed into zinc oxide; Obtain nano zine oxide/starch composite granule or nano zine oxide/Xylo-Mucine composite granule.
The invention has the beneficial effects as follows:
(1) starch and Mierocrystalline cellulose derive from natural phant, low price, and Xylo-Mucine also is a kind of derivatived cellulose cheaply, and they all are nontoxic polyose polymers; The nano zinc oxide composite powder of preparation is used can expand to biomedicine field.
(2) granularity of the glucoside structure of starch and Xylo-Mucine in can controlled oxidation zinc generative process, the zinc oxide of preparation nanoscale; Can prevent simultaneously that the nano zine oxide that generates from big reunion taking place.
Description of drawings
Fig. 1 (a): nano zine oxide/starch composite granule infrared spectrum;
Fig. 1 (b): nano zine oxide/Xylo-Mucine composite granule infrared spectrum;
Fig. 2: the X-ray diagram of nano zine oxide/starch composite granule and nano zine oxide/Xylo-Mucine composite granule;
Fig. 3: the thermogravimetric curve of nano zine oxide/starch composite granule and nano zine oxide/Xylo-Mucine composite granule;
Fig. 4 (a): nano zine oxide/starch composite granule transmission electron microscope picture;
Fig. 4 (b): nano zine oxide/Xylo-Mucine composite granule transmission electron microscope picture.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1:
90 ℃ of preparation mass concentrations are 0.6% amidin, cool to room temperature then; Add zinc nitrate hexahydrate and be dissolved in the amidin, zinc nitrate concentration is 0.1mol/L; Constantly stir, drip isopyknic 0.2mol/L sodium hydroxide solution in solution, the dropping time is 1 hour; After dropwising, continue reaction 2 hours; 8000rpm centrifugation 20 minutes, the mixture that obtains washes with water; 80 ℃ of dryings 3 hours, zinc hydroxide is changed into zinc oxide; Obtain nano zine oxide/starch composite granule.
Shown in Fig. 1 (a), the stretching vibration absorption peak (430cm of the zinc oxygen key in the zinc oxide 1
-1) and starch 2 in C-O vibration absorption peak (1000-1200cm on the glucose ring
-1) all appear in the composite granule 3 of preparation, illustrate that product is nano zine oxide/starch composite granule.
As shown in Figure 2, nano zine oxide/starch composite granule 3 is consistent with zinc oxide 1 Standard X-Ray spectrogram.
As shown in Figure 3, the mass loss of nano zine oxide/starch composite granule 3 at starch 2 decomposition temperature places is 21%; The amylolysis mass loss is 70%; So the content of estimation starch in nano zine oxide/starch composite granule is about 30%.
Shown in Fig. 4 (a), the about 100nm of nano granular of zinc oxide in nano zine oxide/starch composite granule has the starch parcel outward.
Embodiment 2:
Heating preparation mass concentration is 0.1% amidin, cool to room temperature then; Add zinc nitrate hexahydrate and be dissolved in the amidin, zinc nitrate concentration is 0.1mol/L; Constantly stir, drip isopyknic 0.2mol/L sodium hydroxide solution in solution, the dropping time is 2 hours; After dropwising, continue reaction 2 hours; The mixture that centrifugation obtains washes with water; 130 ℃ of dryings, zinc hydroxide is changed into zinc oxide; Obtain nano zine oxide/starch composite granule.The about 180nm of nano granular of zinc oxide in nano zine oxide/starch composite granule, starch content is about 9%.
Embodiment 3:
Heating preparation mass concentration is 1.0% amidin, cool to room temperature then; Add zinc nitrate hexahydrate and be dissolved in the amidin, zinc nitrate concentration is 0.1mol/L; Constantly stir, drip isopyknic 0.2mol/L sodium hydroxide solution in solution, the dropping time is 1.5 hours; After dropwising, continue reaction 2 hours; The mixture that centrifugation obtains washes with water; 100 ℃ of dryings, zinc hydroxide is changed into zinc oxide; Obtain nano zine oxide/starch composite granule.The about 30nm of nano granular of zinc oxide in nano zine oxide/starch composite granule, starch content is about 38%.
Embodiment 4:
Heating preparation mass concentration is 0.6% sodium carboxymethyl cellulose solution, cool to room temperature then; Add zinc nitrate hexahydrate and be dissolved in the sodium carboxymethyl cellulose solution, zinc nitrate concentration is 0.1mol/L; Constantly stir, drip isopyknic 0.2mol/L sodium hydroxide solution in solution, the dropping time is 1 hour; After dropwising, continue reaction 2 hours; Centrifugation, the mixture that obtains washes with water; 80 ℃ of dryings, zinc hydroxide is changed into zinc oxide; Obtain nano zine oxide/Xylo-Mucine composite granule.
Shown in Fig. 1 (b), the stretching vibration absorption peak (430cm of the zinc oxygen key in the zinc oxide 1
-1) and Xylo-Mucine 4 in C-O vibration absorption peak (1000-1200cm on the glucose ring
-1) all appear in the composite granule 5 of preparation, illustrate that product is nano zine oxide/Xylo-Mucine composite granule.
As shown in Figure 2, nano zine oxide/Xylo-Mucine composite granule 5 is consistent with zinc oxide 1 Standard X-Ray spectrogram.
As shown in Figure 3, the mass loss of nano zine oxide/Xylo-Mucine composite granule 5 at Xylo-Mucine 4 decomposition temperature places is 16%; It is 40% that Xylo-Mucine decomposes mass loss; So the content of estimation Xylo-Mucine in composite granule is about 40%.
Shown in Fig. 4 (b), the about 100nm of nano granular of zinc oxide in nano zine oxide/Xylo-Mucine composite granule, particle have the Xylo-Mucine parcel outward.
Embodiment 5:
Heating preparation mass concentration is 0.1% sodium carboxymethyl cellulose solution, cool to room temperature then; Add zinc nitrate hexahydrate and be dissolved in the sodium carboxymethyl cellulose solution, zinc nitrate concentration is 0.1mol/L; Constantly stir, drip isopyknic 0.2mol/L sodium hydroxide solution in solution, the dropping time is 2 hours; After dropwising, continue reaction 2 hours; The mixture that centrifugation obtains washes with water; 130 ℃ of dryings, zinc hydroxide is changed into zinc oxide; Obtain nano zine oxide/Xylo-Mucine composite granule.The about 160nm of nano granular of zinc oxide in nano zine oxide/Xylo-Mucine composite granule, carboxymethylcellulosodium sodium content is about 13%.
Embodiment 6:
Heating preparation mass concentration is 1.0% sodium carboxymethyl cellulose solution, cool to room temperature then; Add zinc nitrate hexahydrate and be dissolved in the sodium carboxymethyl cellulose solution, zinc nitrate concentration is 0.1mol/L; Constantly stir, drip isopyknic 0.2mol/L sodium hydroxide solution in solution, the dropping time is 1.5 hours; After dropwising, continue reaction 2 hours; The mixture that centrifugation obtains washes with water; 100 ℃ of dryings, zinc hydroxide is changed into zinc oxide; Obtain nano zine oxide/Xylo-Mucine composite granule.The about 20nm of nano granular of zinc oxide in nano zine oxide/Xylo-Mucine composite granule, carboxymethylcellulosodium sodium content is about 48%.
The present invention open and propose prepare the method for nano zinc oxide composite powder with natural polysaccharide, those skilled in the art can be by using for reference this paper content, links such as appropriate change raw material, processing parameter, structure design realize.Method of the present invention and technology are described by preferred embodiment, person skilled obviously can be in not breaking away from content of the present invention, spirit and scope to method as herein described with technology is changed or suitably change and combination, realize the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (2)
1. the preparation method of a nano zinc oxide composite powder, it is characterized in that respectively with starch or Xylo-Mucine preparing nano zine oxide/starch composite granule or nano zine oxide/Xylo-Mucine composite granule at aqueous phase with solution deposit as the stablizer of nano zine oxide.
2. the preparation method of a kind of nano zinc oxide composite powder as claimed in claim 1, it is characterized in that: starch or Xylo-Mucine are dissolved in the hot water, and mass concentration is 0.1%-1%, cool to room temperature then; Add zinc nitrate hexahydrate and be dissolved in the above-mentioned solution, zinc nitrate concentration is 0.1mol/L; Constantly stir, drip isopyknic 0.2mol/L sodium hydroxide solution in solution, the dropping time is 1-2 hour; After dropwising, continue reaction 2 hours; The mixture that centrifugation obtains washes with water; 80 ℃ of-130 ℃ of dryings, zinc hydroxide is changed into zinc oxide; Obtain nano zine oxide/starch composite granule or nano zine oxide/Xylo-Mucine composite granule.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723437B (en) * | 2009-12-22 | 2012-05-30 | 聊城大学 | Method for preparing porous laminated zinc oxide sphere |
| CN104355331A (en) * | 2014-10-28 | 2015-02-18 | 常州市创捷防雷电子有限公司 | Biological environment-friendly method for preparing mono-dispersed nano-zinc oxide |
| CN104495910A (en) * | 2014-11-28 | 2015-04-08 | 江苏省中国科学院植物研究所 | Method for preparing nano zinc oxide employing catharanthus roseus leaf extract |
| CN106006709A (en) * | 2016-05-18 | 2016-10-12 | 南京林业大学 | Method for preparing ZnO nanopowder from cellulose zinc chloride solution |
| CN106084253A (en) * | 2016-07-12 | 2016-11-09 | 武汉大学 | A kind of solvent dissolving cellulose and application thereof |
| CN113149061A (en) * | 2021-04-26 | 2021-07-23 | 江苏贝丽得新材料有限公司 | Preparation method of superfine zinc oxide powder |
| CN113460995A (en) * | 2021-07-12 | 2021-10-01 | 上海海洋大学 | Method for simultaneously preparing carbon dots and nano zinc oxide |
| CN113735158A (en) * | 2021-09-09 | 2021-12-03 | 陕西科技大学 | Method for preparing high-dispersity spherical nano zinc oxide by microwave hydrothermal method |
| CN115043423A (en) * | 2022-07-01 | 2022-09-13 | 仲恺农业工程学院 | Method for preparing olive-shaped nano zinc oxide based on microreactor |
-
2009
- 2009-02-27 CN CNA2009100679859A patent/CN101497457A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723437B (en) * | 2009-12-22 | 2012-05-30 | 聊城大学 | Method for preparing porous laminated zinc oxide sphere |
| CN104355331A (en) * | 2014-10-28 | 2015-02-18 | 常州市创捷防雷电子有限公司 | Biological environment-friendly method for preparing mono-dispersed nano-zinc oxide |
| CN104495910A (en) * | 2014-11-28 | 2015-04-08 | 江苏省中国科学院植物研究所 | Method for preparing nano zinc oxide employing catharanthus roseus leaf extract |
| CN106006709A (en) * | 2016-05-18 | 2016-10-12 | 南京林业大学 | Method for preparing ZnO nanopowder from cellulose zinc chloride solution |
| CN106084253A (en) * | 2016-07-12 | 2016-11-09 | 武汉大学 | A kind of solvent dissolving cellulose and application thereof |
| CN113149061A (en) * | 2021-04-26 | 2021-07-23 | 江苏贝丽得新材料有限公司 | Preparation method of superfine zinc oxide powder |
| CN113149061B (en) * | 2021-04-26 | 2024-01-19 | 江苏贝丽得新材料有限公司 | Preparation method of superfine zinc oxide powder |
| CN113460995A (en) * | 2021-07-12 | 2021-10-01 | 上海海洋大学 | Method for simultaneously preparing carbon dots and nano zinc oxide |
| CN113735158A (en) * | 2021-09-09 | 2021-12-03 | 陕西科技大学 | Method for preparing high-dispersity spherical nano zinc oxide by microwave hydrothermal method |
| CN115043423A (en) * | 2022-07-01 | 2022-09-13 | 仲恺农业工程学院 | Method for preparing olive-shaped nano zinc oxide based on microreactor |
| CN115043423B (en) * | 2022-07-01 | 2023-08-04 | 仲恺农业工程学院 | Method for preparing olive-shaped nano zinc oxide based on microreactor |
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Open date: 20090805 |