CN102897805B - Preparation method of one-dimensional porous magnesium oxide nano wire - Google Patents
Preparation method of one-dimensional porous magnesium oxide nano wire Download PDFInfo
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- CN102897805B CN102897805B CN201210343556.1A CN201210343556A CN102897805B CN 102897805 B CN102897805 B CN 102897805B CN 201210343556 A CN201210343556 A CN 201210343556A CN 102897805 B CN102897805 B CN 102897805B
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Abstract
The invention relates to a preparation method of 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 preparing technical field of nano material, be specifically related to a kind of method of 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 manufacturing high glass goods, magnesium salts, pigment, paint and household chemicals etc., be also the important presoma of preparing porous magnesia simultaneously.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.It is raw material that king's treasured of Dalian University of Technology and grade adopt magnesium chloride and urea in patent CN 101058430A, and polyoxyethylene glycol or Triton X-100 dispersion agent, prepare the magnesium basic carbonate with three-dimensional manometer structure.First the Song Xingfu of East China University of Science etc. adopts magnesium chloride and sodium carbonate in patent CN101830489A is that raw material is prepared rodlike magnesium carbonate trihydrate presoma, then prepares porous rose-shaped basic magnesium carbonate after hot-water cure.But also there is no synthetic report for one dimension magnesium basic carbonate nano wire.
Summary of the invention
The object 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 realizes the technical scheme that its object is taked:the preparation method of one dimension porous magnesia nano wire, comprises the following steps:
(1) metal magnesium salts and urea are mixed with to the aqueous solution of 0.1-3mol/L according to mol ratio 1:1 ~ 1:4, are heated to 90 ~ 130 oC in sealed reaction vessel, reaction 6-24 hour, is precipitated thing;
(2) by throw out suction filtration, repeatedly wash with water to inclusion-free ion, obtain filter cake;
(3) filter cake is placed in to baking oven, under 80 oC dry 4 hours, obtains diameter 50 ~ 250 nanometers, length is about the one dimension magnesium basic carbonate nano wire of 10 ~ 500 microns;
(4) one dimension magnesium basic carbonate nano wire is placed in to retort furnace, under air atmosphere or inert atmosphere, is 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 magnesium sulfate.
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 is not used 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.One dimension magnesium basic carbonate nano wire prepared by present method has better crystallinity degree, purity high; The one dimension porous magnesia nano wire of preparation has the features such as high purity and high-specific surface area.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described.
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
(1) 20.3g magnesium chloride hexahydrate, 24g urea and 250ml water are joined in 500ml tool plug Erlenmeyer flask, be positioned in baking oven and be heated to 100 oC, react 12 hours, be precipitated thing;
(2) by throw out suction filtration, repeatedly wash with water to inclusion-free ion, obtain filter cake;
(3) filter cake is placed in to baking oven, under 80 oC dry 4 hours, obtains diameter 50 ~ 250 nanometers, length is about the one dimension magnesium basic carbonate nano wire of 10 ~ 500 microns;
(4) one dimension magnesium basic carbonate nano wire is placed in to retort furnace, under air atmosphere, is 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 125 ml tetrafluoroethylene reactors, be positioned in baking oven and be heated to 100 oC, react 9 hours, be precipitated thing;
(2) by throw out suction filtration, repeatedly wash with water to inclusion-free ion, obtain filter cake;
(3) filter cake is placed in to baking oven, under 80 oC dry 4 hours, obtains diameter 50 ~ 250 nanometers, length is about the one dimension magnesium basic carbonate nano wire of 10 ~ 500 microns;
(4) one dimension magnesium basic carbonate nano wire is placed in to retort furnace, under argon gas atmosphere, is heated to 400oC calcining 1 hour, obtain one dimension porous magnesia nano wire.
embodiment 3
(1) 12.04 g magnesium sulfate, 24g urea and 250ml water are joined in 500ml tool plug Erlenmeyer flask, be positioned in baking oven and be heated to 100 oC, react 12 hours, be precipitated thing;
(2) by throw out suction filtration, repeatedly wash with water to inclusion-free ion, obtain filter cake;
(3) filter cake is placed in to baking oven, under 80 oC dry 4 hours, obtains diameter 50 ~ 250 nanometers, length is about the one dimension magnesium basic carbonate nano wire of 10 ~ 200 microns;
(4) one dimension magnesium basic carbonate nano wire is placed in to retort furnace, under air atmosphere, is heated to 500oC calcining 1 hour, obtain one dimension porous magnesia nano wire.
(1) 25.64 g magnesium nitrate hexahydrates, 24g urea and 250ml water are joined in 500ml tool plug Erlenmeyer flask, be positioned in baking oven and be heated to 100 oC, react 12 hours, be precipitated thing;
(2) by throw out suction filtration, repeatedly wash with water to inclusion-free ion, obtain filter cake;
(3) filter cake is placed in to baking oven, under 80 oC dry 4 hours, obtains diameter 50 ~ 250 nanometers, length is about the one dimension magnesium basic carbonate nano wire of 10 ~ 200 microns;
(4) one dimension magnesium basic carbonate nano wire is placed in to retort furnace, under air atmosphere, is heated to 350oC calcining 3 hours, obtain one dimension porous magnesia nano wire.
Above are only embodiments of the invention, 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., within all should being included in protection scope of the present invention.
Claims (4)
1. the preparation method of one dimension porous magnesia nano wire, comprises the following steps:
(1) metal magnesium salts and urea are mixed with to the aqueous solution of 0.1-3mol/L according to mol ratio 1:1 ~ 1:4, are heated to 90 ~ 130 oC in sealed reaction vessel, reaction 6-24 hour, is precipitated thing;
(2) by throw out suction filtration, repeatedly wash with water to inclusion-free ion, obtain filter cake;
(3) filter cake is placed in to baking oven, under 80 oC dry 4 hours, obtains diameter 50 ~ 250 nanometers, length and be the one dimension magnesium basic carbonate nano wire of 10 ~ 500 microns;
(4) one dimension magnesium basic carbonate nano wire is placed in to retort furnace, under air atmosphere or inert atmosphere, is heated to 350 ~ 500oC calcining 1 ~ 3 hour, obtain one dimension porous magnesia nano wire.
2. the preparation method of one dimension porous magnesia nano wire according to claim 1, is characterized in that: metal magnesium salts used is magnesium chloride, magnesium nitrate and magnesium sulfate.
3. the preparation method of one dimension porous magnesia nano wire according to claim 1, is characterized in that: sealed reaction vessel comprises tool plug glass reaction container and autoclave.
4. the preparation method of one dimension porous magnesia nano wire according to claim 1, is characterized in that: described inert atmosphere is nitrogen atmosphere or argon gas atmosphere.
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| CN104607142B (en) * | 2015-01-20 | 2017-09-15 | 中国科学院合肥物质科学研究院 | Micro-nano hierarchy MgO/MgCO3Compound and its application as defluorinating agent |
| 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 |
| CN109371385B (en) * | 2018-09-13 | 2020-07-03 | 福建龙新三维阵列科技有限公司 | Preparation method of flaky magnesium oxide or doped magnesium oxide 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 |
| 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 |
| 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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