CN102897805A - Preparation method of one-dimensional basic magnesium carbonate nano wire and porous magnesium oxide nano wire - Google Patents
Preparation method of one-dimensional basic magnesium carbonate nano wire and porous magnesium oxide nano wire Download PDFInfo
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- CN102897805A CN102897805A CN2012103435561A CN201210343556A CN102897805A CN 102897805 A CN102897805 A CN 102897805A CN 2012103435561 A CN2012103435561 A CN 2012103435561A CN 201210343556 A CN201210343556 A CN 201210343556A CN 102897805 A CN102897805 A CN 102897805A
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Abstract
The invention relates to a preparation method of one-dimensional basic magnesium carbonate nano wire and porous magnesium oxide nano wire, belonging to the technical field of preparation of nano materials. The method comprises steps of sealing a mixed aqueous solution of metal magnesium salts and urea, heating to 90 to 130 DEG C, and reacting for 6 to 24 hours to obtain the one-dimensional basic magnesium carbonate nano wire with a diameter of 50 to 250 nanometers and a length of 10 to 500 micrometers; and then drying the basic magnesium carbonate nano wire, and calcining under an air atmosphere or an inert atmosphere to obtain the one-dimensional porous magnesium oxide nano wire. The method is simple to process and low in production cost, and is very suitable for industrial production.
Description
Technical field
The invention belongs to the preparations of nanomaterials technical field, be specifically related to a kind of method for preparing one dimension magnesium basic carbonate nano wire and porous magnesia nano wire.
Background technology
Magnesium basic carbonate is a kind of important inorganic chemical product.Can be as weighting agent and the strengthening agent of rubber item, can be used as adiabatic, resistant to elevated temperatures fire-retardant heat-insulation material, also can make siccative, colour protecting agent, carrier, anti-caking agent, pharmaceutically be used as antacid, also can be used for making high glass goods, magnesium salts, pigment, paint and household chemicals etc., also is simultaneously the important presoma of preparation porous magnesia.The character such as the electricity that nano material has, optics, calorifics, magnetics are compared obviously different and more superior from block materials, show bright application prospect, are described as the most promising material of 21st century.Therefore, how to prepare other magnesium basic carbonate product of high-purity nano level, receive much concern always.
The nanometer magnesium basic carbonate of report comprises nanometer sheet, short nanometer rod and nanotube and the aggregates of nanoparticles with three-dimensional structure at present.King's treasured of Dalian University of Technology and grade adopt magnesium chloride and urea in patent CN 101058430A be raw material, and polyoxyethylene glycol or Triton X-100 dispersion agent are prepared the magnesium basic carbonate with three-dimensional manometer structure.The Song Xingfu of East China University of Science etc. at first adopts magnesium chloride and yellow soda ash in patent CN101830489A be that raw material prepares the rodlike magnesium carbonate trihydrate presoma, prepares porous rose-shaped basic magnesium carbonate through after the hot-water cure again.But also there is not synthetic report for one dimension magnesium basic carbonate nano wire.
Summary of the invention
The purpose of this invention is to provide that a kind of technique is simple, low production cost, be highly suitable for the preparation method of high-quality one dimension magnesium basic carbonate nano wire and the one dimension porous magnesia nano wire of suitability for industrialized production.
The present invention is the technical scheme that its purpose of realization is taked:The preparation method of one dimension magnesium basic carbonate nano wire and porous magnesia nano wire may further comprise the steps:
(1) metal magnesium salts and urea are mixed with the aqueous solution of 0.1-3mol/L according to mol ratio 1:1 ~ 1:4, in sealed reaction vessel, are heated to 90 ~ 130 oC, reacted 6-24 hour, be precipitated thing;
(2) with the throw out suction filtration, repeatedly wash with water to the inclusion-free ion, obtain filter cake;
(3) filter cake is placed baking oven, under 80 oC dry 4 hours, obtain diameter 50 ~ 250 nanometers, length is about 10 ~ 500 microns one dimension magnesium basic carbonate nano wire;
(4) one dimension magnesium basic carbonate nano wire is placed retort furnace, under air atmosphere or inert atmosphere, be heated to 350 ~ 500oC calcining 1 ~ 3 hour, obtain one dimension porous magnesia nano wire.
Described metal magnesium salts is magnesium chloride, magnesium nitrate and sal epsom.
Described sealed reaction vessel comprises tool plug glass reaction container and autoclave.
Described inert atmosphere is nitrogen atmosphere or argon gas atmosphere.
The present invention reaches and obtains beneficial effect and be:Preparation technology is simple, and low production cost does not use any dispersion agent and tensio-active agent, and aftertreatment is simple, and preparation process is easily controlled, and is highly susceptible to suitability for industrialized production.The one dimension magnesium basic carbonate nano wire of present method preparation has better crystallinity degree, purity high; The one dimension porous magnesia nano wire of preparation has the characteristics such as high purity and high-specific surface area.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is the scanning electron microscope (SEM) photograph of the one dimension magnesium basic carbonate nano wire prepared of the present invention.
Fig. 2 is the X-ray diffractogram of the one dimension magnesium basic carbonate nano wire prepared of the present invention.
Fig. 3 is the transmission electron microscope picture of the one dimension magnesia nanometer line prepared of the present invention.
Fig. 4 is the X-ray diffractogram of the one dimension magnesia nanometer line prepared of the present invention.
Embodiment
Embodiment 1
(1) 20.3g magnesium chloride hexahydrate, 24g urea and 250ml water are joined in the 500ml tool plug Erlenmeyer flask, be positioned over and be heated to 100 oC in the baking oven, reacted 12 hours, be precipitated thing;
(2) with the throw out suction filtration, repeatedly wash with water to the inclusion-free ion, obtain filter cake;
(3) filter cake is placed baking oven, under 80 oC dry 4 hours, obtain diameter 50 ~ 250 nanometers, length is about 10 ~ 500 microns one dimension magnesium basic carbonate nano wire;
(4) one dimension magnesium basic carbonate nano wire is placed retort furnace, under air atmosphere, be heated to 400oC calcining 1 hour, obtain one dimension porous magnesia nano wire.
Embodiment 2
(1) 4.06g magnesium chloride hexahydrate, 2.4g urea and 100 ml water are joined in the 125 ml tetrafluoroethylene reactors, be positioned over and be heated to 100 oC in the baking oven, reacted 9 hours, be precipitated thing;
(2) with the throw out suction filtration, repeatedly wash with water to the inclusion-free ion, obtain filter cake;
(3) filter cake is placed baking oven, under 80 oC dry 4 hours, obtain diameter 50 ~ 250 nanometers, length is about 10 ~ 500 microns one dimension magnesium basic carbonate nano wire;
(4) one dimension magnesium basic carbonate nano wire is placed retort furnace, under argon gas atmosphere, be heated to 400oC calcining 1 hour, obtain one dimension porous magnesia nano wire.
Embodiment 3
(1) 12.04 g sal epsom, 24g urea and 250ml water are joined in the 500ml tool plug Erlenmeyer flask, be positioned over and be heated to 100 oC in the baking oven, reacted 12 hours, be precipitated thing;
(2) with the throw out suction filtration, repeatedly wash with water to the inclusion-free ion, obtain filter cake;
(3) filter cake is placed baking oven, under 80 oC dry 4 hours, obtain diameter 50 ~ 250 nanometers, length is about 10 ~ 200 microns one dimension magnesium basic carbonate nano wire;
(4) one dimension magnesium basic carbonate nano wire is placed retort furnace, under air atmosphere, be heated to 500oC calcining 1 hour, obtain one dimension porous magnesia nano wire.
Embodiment 4
(1) 25.64 g magnesium nitrate hexahydrates, 24g urea and 250ml water are joined in the 500ml tool plug Erlenmeyer flask, be positioned over and be heated to 100 oC in the baking oven, reacted 12 hours, be precipitated thing;
(2) with the throw out suction filtration, repeatedly wash with water to the inclusion-free ion, obtain filter cake;
(3) filter cake is placed baking oven, under 80 oC dry 4 hours, obtain diameter 50 ~ 250 nanometers, length is about 10 ~ 200 microns one dimension magnesium basic carbonate nano wire;
(4) one dimension magnesium basic carbonate nano wire is placed retort furnace, under air atmosphere, be heated to 350oC calcining 3 hours, obtain one dimension porous magnesia nano wire.
Above-mentioned only is embodiments of the invention, and to one skilled in the art, the present invention has multiple change and variation.Allly within invention thought of the present invention and principle, make any modification, be equal to replacement, improve etc., all should be included within protection scope of the present invention.
Claims (4)
1. the preparation method of one dimension magnesium basic carbonate nano wire and porous magnesia nano wire may further comprise the steps:
(1) metal magnesium salts and urea are mixed with the aqueous solution of 0.1-3mol/L according to mol ratio 1:1 ~ 1:4, in sealed reaction vessel, are heated to 90 ~ 130 oC, reacted 6-24 hour, be precipitated thing;
(2) with the throw out suction filtration, repeatedly wash with water to the inclusion-free ion, obtain filter cake;
(3) filter cake is placed baking oven, under 80 oC dry 4 hours, obtain diameter 50 ~ 250 nanometers, length is about 10 ~ 500 microns one dimension magnesium basic carbonate nano wire;
(4) one dimension magnesium basic carbonate nano wire is placed retort furnace, under air atmosphere or inert atmosphere, be heated to 350 ~ 500oC calcining 1 ~ 3 hour, obtain one dimension porous magnesia nano wire.
2. the preparation method of one dimension magnesium basic carbonate nano wire according to claim 1 and porous magnesia nano wire, it is characterized in that: used metal magnesium salts is magnesium chloride, magnesium nitrate and sal epsom.
3. the preparation method of one dimension magnesium basic carbonate nano wire according to claim 1 and porous magnesia nano wire, it is characterized in that: sealed reaction vessel comprises tool plug glass reaction container and autoclave.
4. the preparation method of one dimension magnesium basic carbonate nano wire according to claim 1 and porous magnesia nano wire, it is characterized in that: described inert atmosphere is nitrogen atmosphere or argon gas atmosphere.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607142A (en) * | 2015-01-20 | 2015-05-13 | 中国科学院合肥物质科学研究院 | MgO/MgCO3 compound adopting micro-nano hierarchical structure and application of MgO/MgCO3 compound serving as fluorine remover |
| CN105883866A (en) * | 2016-05-20 | 2016-08-24 | 江苏师范大学 | Synthesis method of controllable-length/width basic magnesium carbonate nanorods |
| CN109371385A (en) * | 2018-09-13 | 2019-02-22 | 福建龙新三维阵列科技有限公司 | A kind of sheet magnesia or the preparation method for adulterating magnesia array |
| CN109775734A (en) * | 2019-03-01 | 2019-05-21 | 安徽壹石通材料科技股份有限公司 | A kind of preparation method of low specific surface area basic magnesium carbonate |
| WO2020191691A1 (en) * | 2019-03-22 | 2020-10-01 | 北京化工大学 | Method for efficiently separating magnesium and lithium from salt lake brine and simultaneously preparing high-purity magnesium oxide and battery-grade lithium carbonate |
| CN114171847A (en) * | 2021-12-09 | 2022-03-11 | 江苏厚生新能源科技有限公司 | High-flame-retardance and high-wettability lithium ion battery diaphragm and preparation method thereof |
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| CN101444737A (en) * | 2008-12-22 | 2009-06-03 | 长沙星纳气凝胶有限公司 | Nickel-based catalyst for hydrogen production by ethanol steam reforming and preparation method thereof |
| US20100158788A1 (en) * | 2008-12-22 | 2010-06-24 | Cheil Industries Inc. | Supported Catalyst with Solid Sphere Structure, Method for Preparing the Same and Carbon Nanotubes Prepared Using the Same |
| CN102262994A (en) * | 2011-06-21 | 2011-11-30 | 福州大学 | Oxide-nano-structure-based surface-conduction electron emission source and manufacturing method thereof |
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- 2012-09-17 CN CN201210343556.1A patent/CN102897805B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101444737A (en) * | 2008-12-22 | 2009-06-03 | 长沙星纳气凝胶有限公司 | Nickel-based catalyst for hydrogen production by ethanol steam reforming and preparation method thereof |
| US20100158788A1 (en) * | 2008-12-22 | 2010-06-24 | Cheil Industries Inc. | Supported Catalyst with Solid Sphere Structure, Method for Preparing the Same and Carbon Nanotubes Prepared Using the Same |
| CN102262994A (en) * | 2011-06-21 | 2011-11-30 | 福州大学 | Oxide-nano-structure-based surface-conduction electron emission source and manufacturing method thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607142A (en) * | 2015-01-20 | 2015-05-13 | 中国科学院合肥物质科学研究院 | MgO/MgCO3 compound adopting micro-nano hierarchical structure and application of MgO/MgCO3 compound serving as fluorine remover |
| CN105883866A (en) * | 2016-05-20 | 2016-08-24 | 江苏师范大学 | Synthesis method of controllable-length/width basic magnesium carbonate nanorods |
| CN105883866B (en) * | 2016-05-20 | 2017-11-07 | 江苏师范大学 | A kind of synthetic method of the controllable basic magnesium carbonate nanometer rods of length and width |
| CN109371385A (en) * | 2018-09-13 | 2019-02-22 | 福建龙新三维阵列科技有限公司 | A kind of sheet magnesia or the preparation method for adulterating magnesia array |
| CN109775734A (en) * | 2019-03-01 | 2019-05-21 | 安徽壹石通材料科技股份有限公司 | A kind of preparation method of low specific surface area basic magnesium carbonate |
| WO2020191691A1 (en) * | 2019-03-22 | 2020-10-01 | 北京化工大学 | Method for efficiently separating magnesium and lithium from salt lake brine and simultaneously preparing high-purity magnesium oxide and battery-grade lithium carbonate |
| US11524901B2 (en) | 2019-03-22 | 2022-12-13 | Beijing University Of Chemical Technology | Method for efficiently separating magnesium and lithium from salt lake brine and simultaneously preparing high-purity magnesium oxide and battery-grade lithium carbonate |
| CN114171847A (en) * | 2021-12-09 | 2022-03-11 | 江苏厚生新能源科技有限公司 | High-flame-retardance and high-wettability lithium ion battery diaphragm and preparation method thereof |
| CN114171847B (en) * | 2021-12-09 | 2023-09-01 | 江苏厚生新能源科技有限公司 | High-flame-retardance high-wettability lithium ion battery diaphragm and preparation method thereof |
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