CN1562840A - Microwave coprecipitation method for preparing nano glaze of lead metaborate - Google Patents
Microwave coprecipitation method for preparing nano glaze of lead metaborate Download PDFInfo
- Publication number
- CN1562840A CN1562840A CN 200410012908 CN200410012908A CN1562840A CN 1562840 A CN1562840 A CN 1562840A CN 200410012908 CN200410012908 CN 200410012908 CN 200410012908 A CN200410012908 A CN 200410012908A CN 1562840 A CN1562840 A CN 1562840A
- Authority
- CN
- China
- Prior art keywords
- lead
- aqueous solution
- metaborate
- product
- microwave
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Glass Compositions (AREA)
Abstract
The invention relates to prepn. method of nanometre borate. The processing steps are: (1) taking Boratex and lead nitrate with mole ratio 1:1 to prepare 20 percent of aqueous solution; (2) taking 2-ethyl sulfo group sodium succinate to added into said lead nitrate aqueous solution to change density to 2 perent; (3) slowly pouring said sodium succinate into mixed solution to be fully stirred to create precipitation, constant temp. 35-45 deg.C, reaction time 1.5-2 hours, then to be batch processed by 500 W microwave illuminating 4-6 minutes, temp of solution is 80-100 deg.C; (4) said product is centrifugated to generate precipitant which is washed by distilled water two times and by absolute ethyl alcohol three times to produce nanometre lead metaborate; (5) drying said nanometre lead metaborate 10 hours in 60 deg.C vacuum to produce nanometre lead metaborate frit.
Description
Technical field
The present invention relates to a kind of preparation method of nano boric acid salt.
Background technology
Nano material can be comparable with de broglie wavelength because its size is little, has a lot of properties; As quantum size effect, surface effects and small-size effect
[1] [2]Thereby present many peculiar physical and chemical performances, and be with a wide range of applications in a lot of fields, be considered to the most promising material of 21 century.Lead borate is of many uses, except at glass, and ceramic glaze, outside the application in the inorganic materials such as porcelain enamel industry, nanometer lead metaborate powder is wear-resisting, and does that excellent performance is arranged on the luminous host.Behind the lead borate nanometer, its application performance is optimized more, and will be expanded its range of application.It is reported that usefulness Sol-Gel methods such as Wu Lijun have prepared Li
2B
4O
7Film
[3], preparations such as the Renzhi Ma nano boric acid magnesium of going out
[4], Hu Zeshan etc. have prepared nano boric acid copper particle
[5], the position people have prepared β-BaB
2O
4Nano-powder
[6]At present, the study on the synthesis to nanometer lead metaborate powder does not appear in the newspapers both at home and abroad.
Reference:
(1) Zhang Lide, Mu Jimei, nano material and nanostructure, Science Press, 2001.
(2) Du Shiguo, Shi Dongmei, Han Qiwen, LIQUID-PHASE SYNTHESIS TECHNIQUES OF NANOMETER PARTICLES, powder metallurgy technology, 2000,18 (1): 46.
(3) Wu Lijun, Zhou Yadong, the Sol-gel legal system is equipped with Li
2B
4O
7Film, piezoelectricity and acousto-optic, 1997,191 (4): 273.
〔4〕Renzhi?Ma，Yoshio?Bando，Dmitri?Golberg?and?Tadao?Sato。Nanotubs?ofMagnesium?Borate，Angew.Chem.Int.Ed?2003，42，1836
(5) Hu Zeshan, Wang Liguang etc., the preparation of nano boric acid copper and as the tribological property of lubricating oil additive, tribology journal, 2000,20 (4), 202-295.
(6) the position people, β-BaSO
4The preparation of nano-powder, artificial lens journal, 2000,29 (1): 83.
Summary of the invention
The object of the present invention is to provide a kind of microwave co-precipitation preparation method of nanometer lead metaborate glaze.
Technical scheme of the present invention is: the microwave co-precipitation preparation method of nanometer lead metaborate glaze is characterized in that it is realized by following steps:
(1) taking by weighing mol ratio is that 1: 1 Sodium Tetraborate and lead nitrate are mixed with 20% the Sodium Tetraborate aqueous solution and 20% the lead nitrate aqueous solution respectively;
(2) take by weighing 2-ethylhexyl sodium sulfosuccinate and add that to make the concentration of 2-ethylhexyl sodium sulfosuccinate in the above-mentioned lead nitrate aqueous solution for preparing be 2%, fully stir;
(3) the above-mentioned Sodium Tetraborate aqueous solution is slowly injected solution after the aqueous solution of 2-ethylhexyl sodium sulfosuccinate and lead nitrate, and fully stir, produce precipitation, constant temperature 35-45 degree, reaction 1.5-2h; 500w microwave irradiation intermittent type was handled 4-6 minute again, and making solution temperature is the 80-100 degree;
(4) above-mentioned product centrifugation goes out throw out, uses distilled water wash throw out 2 times earlier, washes throw out 3 times (immeasurable requirement) with dehydrated alcohol again, gets nanometer lead metaborate product;
(5) nanometer lead metaborate product gets nanometer lead metaborate glaze product 60 ℃ of vacuum-dryings 10 hours.
Can in above-mentioned (2), add a small amount of band look ion, as: the ion of elements such as Fe, Cu, Co, Ni, Cr, realize dopen Nano borate glaze product, realize the colouring of glaze.
With X ray powder diffraction analysis product phase structure, with TEM electron microscopy study powder microscopic pattern.This research application microwave co-precipitation synthesis method has been prepared the nanometer lead metaborate, and size distribution is 30-70nm, and median size is 50nm.
Adopt microwave co-precipitation synthesis method successfully to synthesize the lead metaborate glaze of median size 50nm, its preparation method is simple, can shorten the reaction times, improves reaction yield, and the granular size shape is uniformly dispersed.Fig. 1 is the X-ray diffractogram of nanometer lead metaborate powder, determines that by consulting the JCPDS card product is a lead metaborate: Pb (BO
2)
2.H
2O, find with the standard diagram contrast: the stronger characteristic peak and the XRD figure of product can well be coincide.Fig. 2, Fig. 3 are the transmission electron microscope picture of nanometer lead metaborate, as can be seen from the figure, the particle shape rule of the nanometer lead metaborate of this method preparation, particle shape is ball-type, is evenly distributed, and particle diameter is at 30～70nm, and median size is 50nm.Fig. 4 is the polycrystalline electron-diffraction diagram of nanometer lead metaborate, and particle becomes brilliant general as we can see from the figure.
Description of drawings
Fig. 1 is a wilfully lead borate XRD figure of nanometer of the present invention
Fig. 2 is nanometer lead metaborate TEM of the present invention (* 45000) figure
Fig. 3 is nanometer lead metaborate TEM of the present invention (* 100000) figure
Fig. 4 is a nanometer lead metaborate polycrystalline electron-diffraction diagram of the present invention
Embodiment
The microwave co-precipitation preparation method of nanometer metaborate glaze, it is realized by following steps:
(1) taking by weighing mol ratio is that 1: 1 Sodium Tetraborate and lead nitrate are mixed with 20% the Sodium Tetraborate aqueous solution and 20% the lead nitrate aqueous solution respectively;
(2) take by weighing 2-ethylhexyl sodium sulfosuccinate (AOT) and add that to make the concentration of 2-ethylhexyl sodium sulfosuccinate in the above-mentioned lead nitrate aqueous solution for preparing be 2%, fully stir;
(3) the above-mentioned Sodium Tetraborate aqueous solution is slowly injected solution after 2-ethylhexyl sodium sulfosuccinate and the lead nitrate aqueous solution, and fully stir, produce precipitation, constant temperature 35-45 degree, reaction 1.5-2h; 500w microwave irradiation intermittent type was handled 4-6 minute again, and making solution temperature is the 80-100 degree;
(4) above-mentioned product centrifugation goes out throw out, uses distilled water wash throw out 2 times earlier, washes 3 times with dehydrated alcohol again, gets nanometer lead metaborate product;
(5) nanometer lead metaborate product gets nanometer lead metaborate glaze product 60 ℃ of vacuum-dryings 10 hours.
Can in above-mentioned (2) solution, add a small amount of band look ion, as: the ion of elements such as Fe, Cu, Co, Ni, Cr, realize dopen Nano borate glaze product, realize the colouring of glaze.
This method also is fit to nanometer metaborate glaze products such as nano boric acid strontium glaze.
The common weakness of gel method, phase transfer method and microemulsion method is that reaction soln concentration is low, long reaction time, and control condition is strict.Therefore microwave is introduced and can be induced or quicken some chemical reaction, simultaneously, and the preparation that heat effect that shows during with microwave and material matter interaction and non-thermal effect are used for ultrafine powder.Can shorten the reaction times, improve reaction yield, the granular size shape is uniformly dispersed.
Claims (1)
1. the microwave co-precipitation preparation method of nanometer lead metaborate glaze is characterized in that it is realized by following steps:
(1) taking by weighing mol ratio is that 1: 1 Sodium Tetraborate and lead nitrate are mixed with 20% the Sodium Tetraborate aqueous solution and 20% the lead nitrate aqueous solution respectively;
(2) take by weighing 2-ethylhexyl sodium sulfosuccinate and add that to make the concentration of 2-ethylhexyl sodium sulfosuccinate in the above-mentioned lead nitrate aqueous solution for preparing be 2%, fully stir;
(3) the above-mentioned Sodium Tetraborate aqueous solution is slowly injected solution after the aqueous solution of 2-ethylhexyl sodium sulfosuccinate and lead nitrate, and fully stir, produce precipitation, constant temperature 35-45 degree, reaction 1.5-2h; 500w microwave irradiation intermittent type was handled 4-6 minute again, and making solution temperature is the 80-100 degree;
(4) above-mentioned product centrifugation goes out throw out, uses distilled water wash throw out 2 times earlier, washes throw out 3 times with dehydrated alcohol again, gets nanometer lead metaborate product;
(5) nanometer lead metaborate product gets nanometer lead metaborate glaze product 60 ℃ of vacuum-dryings 10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012908 CN1562840A (en) | 2004-03-29 | 2004-03-29 | Microwave coprecipitation method for preparing nano glaze of lead metaborate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012908 CN1562840A (en) | 2004-03-29 | 2004-03-29 | Microwave coprecipitation method for preparing nano glaze of lead metaborate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1562840A true CN1562840A (en) | 2005-01-12 |
Family
ID=34478053
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410012908 Pending CN1562840A (en) | 2004-03-29 | 2004-03-29 | Microwave coprecipitation method for preparing nano glaze of lead metaborate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1562840A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515855A (en) * | 2011-12-12 | 2012-06-27 | 重庆鸽牌电瓷有限公司 | Raw material formula of wire-post type sand-coating glaze |
| CN108585503A (en) * | 2018-06-28 | 2018-09-28 | 中山市武汉理工大学先进工程技术研究院 | A kind of novel electrostatic prevention ceramic glaze and its preparation method and application |
| WO2020086014A1 (en) | 2018-10-25 | 2020-04-30 | Yeditepe Universitesi | Use of mutant p53 gene targeted lead borate nanoparticles in cancer treatment and production method of these nanoparticles |
| RU2781098C1 (en) * | 2018-10-25 | 2022-10-05 | Едитепе Университеси | Application of lead borate nanoparticles targeted to mutant gene 53 in the treatment and method for obtaining these nanoparticles |
-
2004
- 2004-03-29 CN CN 200410012908 patent/CN1562840A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515855A (en) * | 2011-12-12 | 2012-06-27 | 重庆鸽牌电瓷有限公司 | Raw material formula of wire-post type sand-coating glaze |
| CN102515855B (en) * | 2011-12-12 | 2013-04-10 | 重庆鸽牌电瓷有限公司 | Raw material formula of wire-post type sand-coating glaze |
| CN108585503A (en) * | 2018-06-28 | 2018-09-28 | 中山市武汉理工大学先进工程技术研究院 | A kind of novel electrostatic prevention ceramic glaze and its preparation method and application |
| CN108585503B (en) * | 2018-06-28 | 2021-01-26 | 中山市武汉理工大学先进工程技术研究院 | Novel anti-static ceramic glaze and preparation method and application thereof |
| WO2020086014A1 (en) | 2018-10-25 | 2020-04-30 | Yeditepe Universitesi | Use of mutant p53 gene targeted lead borate nanoparticles in cancer treatment and production method of these nanoparticles |
| CN113164516A (en) * | 2018-10-25 | 2021-07-23 | 耶迪特普大学 | Application of lead borate nanoparticles targeting mutant p53 gene in cancer treatment and preparation method of nanoparticles |
| JP2022509736A (en) * | 2018-10-25 | 2022-01-24 | イェディテペ・ウニヴェルシテシ | Use of lead borate nanoparticles targeting the mutant p53 gene in cancer treatment and methods for producing these nanoparticles |
| RU2781098C1 (en) * | 2018-10-25 | 2022-10-05 | Едитепе Университеси | Application of lead borate nanoparticles targeted to mutant gene 53 in the treatment and method for obtaining these nanoparticles |
| JP7333969B2 (en) | 2018-10-25 | 2023-08-28 | イェディテペ・ウニヴェルシテシ | Use of Lead Borate Nanoparticles Targeting Mutant p53 Gene in Cancer Therapy and Methods of Making These Nanoparticles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Sagadevan et al. | Hydrothermal synthesis of zirconium oxide nanoparticles and its characterization | |
| Zhang et al. | Control of ZnO morphology via a simple solution route | |
| Moghri Moazzen et al. | Change in the morphology of ZnO nanoparticles upon changing the reactant concentration | |
| Verma et al. | Morphology, mechanism and optical properties of nanometer-sized MgO synthesized via facile wet chemical method | |
| Sobhani et al. | Morphological control of MnSe2/Se nanocomposites by amount of hydrazine through a hydrothermal process | |
| Selvi et al. | Synthesis, structural and optical characterization of ZrO 2 core–ZnO@ SiO 2 shell nanoparticles prepared using co-precipitation method for opto-electronic applications | |
| CN110745790B (en) | Hydrothermal preparation method of bismuth selenide nano powder | |
| Ding et al. | Efficient exfoliation of layered materials by waste liquor | |
| Singh et al. | Synthesis of zinc oxide by sol-gel method and to study it’s structural properties | |
| Wu et al. | A unique synthesis of rare-earth-Co-based single crystal particles by “self-aligned” Co nano-arrays | |
| Prakash et al. | Evaluation of structural, morphological and optical properties of CdO nanostructures | |
| Yang et al. | Template-free synthesis of CuS nanorods with a simple aqueous reaction at ambient conditions | |
| Jiang et al. | Bi2Te3 nanostructures prepared by microwave heating | |
| CN1562840A (en) | Microwave coprecipitation method for preparing nano glaze of lead metaborate | |
| Yang et al. | Synthesis of CdSe microspheres via solvothermal process in a mixed solution | |
| Borah et al. | Structural Characterization and Surface Environment of ZnOnanoflowers | |
| Li et al. | Rapid synthesis of Ag2Se nanocrystals by sonochemical reaction | |
| Tang et al. | Preparation and surface modification of uniform ZnO nanorods via a one-step process | |
| Chu et al. | Synthesis of Bi–Bi2O3/C hybrid nanocomposite as a high performance photocatalyst | |
| Wang et al. | General solution-based route to V–VI semiconductors nanorods from hydrolysate | |
| Jia et al. | Morphology transformation of nanoscale magnesium hydroxide: from nanosheets to nanodisks | |
| Selvi et al. | Interfacial effect: magnetism in pure ZrO 2, ZnO and SiO 2 coated core/shell/shell hybrid nanoparticles | |
| Khosravi-Nouri et al. | Fabrication and characterization of silver-tin dioxide core-shell structured nanocomposite particles | |
| Wang et al. | Controllable Preparation of PbMoO4 Nanorods and Nanowires by a Simple Sonochemical Method | |
| CN114195181B (en) | Preparation method of micron-sized copper sulfide nanosheets and copper sulfide nanosheets |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| AD01 | Patent right deemed abandoned | ||
| C20 | Patent right or utility model deemed to be abandoned or is abandoned |