CN101555026A - Method for preparing nano-magnesia with cotton cloth form - Google Patents
Method for preparing nano-magnesia with cotton cloth form Download PDFInfo
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- CN101555026A CN101555026A CNA2009100201917A CN200910020191A CN101555026A CN 101555026 A CN101555026 A CN 101555026A CN A2009100201917 A CNA2009100201917 A CN A2009100201917A CN 200910020191 A CN200910020191 A CN 200910020191A CN 101555026 A CN101555026 A CN 101555026A
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- cotton cloth
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Abstract
The invention relates to a method for preparing nano-magnesia with cotton cloth form, mainly comprising the following steps: (1) preparing Mg(CH3COO)2.4H2O into solution with the concentration of 0.3-0.8 mol/L; (2) fully washing cotton cloth with distilled water, drying, placing the cotton cloth into the solution to dip in a sealed condition for 12-24h; (3) taking the cotton cloth treated in the step (2) out and placing the treated cotton cloth into a drying baker, raising the temperature to 80 DEG C to dry for 2h with constant temperature, and baking the cotton cloth with programmed heating in flowing air to obtain nano-magnesia powder. The invention has simple process, gentle condition, easily obtained raw material and low cost, and is easy for large-scale production. The obtained nana-material has favorable appearance characteristic and wide application, and has great potential application foreground.
Description
Technical field
The present invention relates to a kind of method for preparing inorganic nano material, particularly a kind of preparation has the method for the nano magnesia of cotton cloth form.
Background technology
The bitter earth nano material is a kind of novel high function fine inorganic product geared to the 21st century, it also is a kind of novel high function fine inorganic material, the properties such as light, heat, electricity, mechanics and chemistry that are different from bulk material are arranged, because the granular of particle size, specific surface area sharply increases, and makes the MgO nanoparticle in various fields more importantly using value be arranged.In recent years, caused people's extensive concern about MgO surface tissue and Catalytic Performance.A lot of research work point out that because itself has higher surface reaction activity, particularly strong surface alkalinty by improving the specific surface area of MgO, as the preparation nano-MgO, can make it to show good catalysis and absorption property.For example, can be used as the compaction material of refractory materials, sintering metal, makeup, paint, face powder, fat-splitting agent or pharmaceuticals polish, antiseptic-germicide, the matrix material that forms with superpolymer has good microwave absorption coefficient.Because the MgO nanoparticle is nontoxic, tasteless, addition is few, also be exploitation fire-retardant fibre ideal additive.Particularly superfine nano magnesium oxide is because its particle diameter is little, specific surface area is big; have high purity, high rigidity and high-melting-point; high reactive behavior; strong adsorptivity; good low-temperature sintering; advantageous properties such as high resistivity; can be used for high insulating material; high-quality stupalith; the high-performance refractory fiber; fields such as the sorbent material of environment protection, loading type methyl alcohol and low-carbon alcohol synthetic support of the catalyst are a kind of new inorganic material that widespread use is worth that has, and have caused numerous investigators' attention.
At present, the preparation method of nano magnesia mainly contains technologies such as liquid-phase precipitation method, sol-gel method, alkoxide hydrolysis, vapor phase process, solid phase method.But the product crystallinity that these methods obtain is lower, and technology is comparatively complicated, is further improved.
In recent years, template has caused that in the research that preparation has in the nano structural material of complicated form people pay close attention to widely.The advantage of template is to utilize the space confinement effect of template and regulating and controlling effect to control the size of synthetic materials, pattern, structure, arrangement mode etc., and can be according to the size of synthetic materials and pattern design template in advance.
Summary of the invention
For solving the problem of above-mentioned existence, the present invention aims to provide the method that a kind of preparation has the nano magnesia of cotton cloth form.
The present invention is achieved by the following technical solutions:
Described preparation has the method for the nano magnesia of cotton cloth form, may further comprise the steps:
(1) with Mg (CH
3COO)
24H
2O is made into the solution that concentration is 0.3～0.8mol/L;
(2) with after cotton distilled water thorough washing, the oven dry, put into above-mentioned solution, 12～24h is soaked in sealing;
(3) will put into drying baker through the cotton taking-up that handled step (2), be heated to 80 ℃, constant temperature drying 2h; In flowing air, carry out temperature-programmed calcination then, obtain the nano magnesia powder.
Described temperature-programmed calcination condition is: with the temperature rise rate of 5 ℃/min, be heated to 300 ℃, 500 ℃ or 800 ℃ respectively, and keep constant temperature 1h in the temperature of setting.
The present invention innovates and has proposed the novel method that a kind of preparation has the nano magnesia of cotton cloth form, utilize self space confinement effect of biological template, the cotton that adopts wide material sources by technologies such as immersion, oven dry, calcinings, obtains having the nano magnesia of cotton cloth form as template.Because the space confinement effect of cotton weave construction makes final synthetic magnesium oxide have the pattern of original cotton masterplate, show that biological template has accurate control action kou to material synthetic.
The invention has the beneficial effects as follows: technology is simple, mild condition, environment-friendly high-efficiency, and raw material sources extensively are easy to get, with low cost, be easy to realize scale operation, the material that obtains has good shape characteristic, has higher specific surface area, it is a kind of high-quality new function fine inorganic material, be widely used in fields such as advanced ceramic materials, electrical apparatus insulation material, makeup, face powder, paint, rubber filler, sour gas sorbent material, support of the catalyst, wide application prospect and huge economic potential are arranged, have important practical significance.
Description of drawings
Fig. 1 (a) and (b), (c) are respectively the XRD diffraction spectra of MgO pottery when 300 ℃, 500 ℃, 800 ℃ sintering temperature.
Fig. 2 (a) and (b) be respectively dipping Mg (CH
3COO)
24H
2The DTA curve of O cotton template and original cotton.
Fig. 3 (a) and (b) be respectively dipping Mg (CH
3COO)
24H
2The TG curve of O cotton template and original cotton.
Fig. 4 is the SEM and the EDS figure of cotton fibre.
The SEM figure of the MgO that Fig. 5 records when being 800 ℃ for sintering temperature.
Fig. 6 is that (a) and (b), (c) are respectively the infrared absorpting light spectra of MgO in the time of 300 ℃, 500 ℃, 800 ℃.
Fig. 7 is the MgO TEM microscopic appearance and the selected area electron diffraction spot thereof of 800 ℃ of preparations.
Embodiment
The invention will be further described below in conjunction with specific embodiments and the drawings.
Embodiment 1
Preparation of the present invention has the method for the nano magnesia of cotton cloth form, may further comprise the steps:
(1) with the Mg (CH of purity 〉=99.0%
3COO)
24H
2O is made into the solution that concentration is 0.8mol/L;
(2) with after cotton usefulness distilled water thorough washing and the oven dry, put into the above-mentioned solution for preparing, 24h is soaked in sealing, and the cotton that soaked is taken out, put into drying baker, be heated to 80 ℃, constant temperature drying 2h carries out temperature-programmed calcination: then with the temperature rise rate of 5 ℃/min in flowing air, be heated to 800 ℃, constant temperature 1h obtains biomophic nano magnesia, and particle diameter is 15～40nm, purity 98.5～99.9%.
Fig. 1 (a) curve shows 300 ℃ of sintering, and decomposition reaction does not also take place sample, only has the diffraction peak of Mierocrystalline cellulose in the cotton fibre (110), (200) and (004) crystal face correspondence, the characteristic peak of MgO do not occur.When Fig. 1 (b) curve showed 500 ℃, MgO generated, but the peak type is not sharp-pointed, illustrated that MgO purity is not high at this moment.Fig. 1 (c) and JCPDS standard card 4-0829MgO ten minutes are approaching, and the pairing crystal face of diffraction peak as shown in the figure.With the diffracting spectrum indexing of sample, find that the crystalline structure of MgO belongs to the NaCl type, three the strongest diffraction peaks are respectively 42.91 °, 62.30 °, 36.94 °, and its unit cell parameters is a=0.4213nm.The width of diffracted intensity and diffraction peak reacts the product purity height of gained as can be seen from Fig. 1 (c), and crystallization degree is good.3 significant diffraction peaks, this is the characteristic peak of NaCl structure MgO, illustrates at 800 ℃ of following roasting 1h to have obtained the MgO assembly.In addition, do not have the diffraction peak of other thing phase to exist, illustrate that product is pure phase MgO, wherein the crystal face of highest peak correspondence is (200).
At 300～380 ℃ an exothermic peak is arranged as seen from Figure 2, illustrate under this temperature oxidizing reaction has taken place, be speculated as the organic formwork oxidation, volatilization.380～460 ℃ of endotherm(ic)peaks of locating are corresponding to Mg (CH
3COO)
2Pyrolysis.460～520 ℃ of exothermic peaks of locating are that product magnesium oxide changes the crystalline state material into gradually by non-crystalline state.Fig. 2 (b) is the DTA curve of cotton template, is apparent that an exothermic peak between 300～400 ℃ on the curve the most, this peak correspondence the oxidation of cotton template, remove, the volatilization.
By Fig. 3 (a) as can be known, Mg (CH
3COO)
2Decomposition course in three mass loss steps are arranged, be in 50～110 ℃ respectively, 280～370 ℃ and 430～520 ℃, the former is Mg (CH
3COO)
24H
2O removes planar water and crystal water, mass loss 10%; Secondly remove mass loss 50% for organic formwork (cotton); Last step is Mg (CH
3COO)
2 Decompose mass loss 30%.In the time of 520 ℃, the mass loss curve is tending towards straight line, illustrates that C in the cotton template and O remove substantially in this temperature to finish.Behind 800 ℃ of sintering, generate the MgO quality and account for 10% of the preceding quality of sintering.For guaranteeing that presoma is converted into the MgO nano-powder and reacts completely, select for use 800 ℃ to be maturing temperature during the sample roasting.Fig. 3 (b) is the TG curve of cotton template, only forms a mass loss step in 0～800 ℃ test specification, and between 280～520 ℃, mass loss is near 97%, show the cotton sintering after, the organism in the cotton fibre substantially all is converted into CO
2And water vapour, evaporateing in the air, the material of residue 3% is some nondecomposable material in the cotton.
Fig. 4 is a cotton template microtexture.The cotton fibre pattern is intact as can be seen, and smooth surface is smooth, and fibre array is neat, and the fiber caliber is between 10～25 μ m.Find out from energy spectrum analysis figure and only to contain two kinds of elements of C, O, satisfy the preparation requirement that fully removes behind the sintering.
Fig. 5 is the SEM photo of sample after 800 ℃ of calcinings, and as seen from the figure, sample keeps primeval life template fiber pattern, because nodulizing, it is 4 μ m that caliber is reduced to, and thickness of pipe only is 2～2.5 μ m, is that coreless rolls is curved in the pipe.
Among Fig. 6,710cm
-1The peak at place absorbs 620cm corresponding to the flexural vibration of the Mg-O key in cube MgO crystal
-1The peak at place absorbs 1410cm corresponding to the stretching vibration of Mg-O key in the upright MgO crystal in side
-1Tangible broadening phenomenon has appearred in the absorption peak at place with respect to the base peak of cube MgO, this is owing to the small-size effect and the interfacial effect of nanoparticle; 1100cm
-1The C-O stretching vibration peak more and more littler, show that the C template removes substantially, may be the CO in the atmosphere herein
2Show the poor absorption peak.1620cm
-1The absorption peak correspondence at place the planar water flexural vibration.Above group all has chemically reactive, can show characteristics such as catalysis, absorption under certain condition.
Fig. 7 is the transmission electron microscope photo of the nano-MgO that makes 800 ℃ of roastings.800 ℃ the insulation 1h after gained MgO particle in pelletized form, particle diameter is inhomogeneous, 15～40nm does not wait, product is the MgO of nanoscale.
Preparation of the present invention has the method for the nano magnesia of cotton cloth form, may further comprise the steps:
(1) with the Mg (CH of purity 〉=99.0%
3COO)
24H
2O is made into the solution that concentration is 0.5mol/L;
(2) with after cotton usefulness distilled water thorough washing and the oven dry, put into the above-mentioned solution for preparing, 24h is soaked in sealing, and the cotton that soaked is taken out, put into drying baker, be heated to 80 ℃, constant temperature drying 2h carries out temperature-programmed calcination: then with the temperature rise rate of 5 ℃/min in flowing air, be heated to 500 ℃, constant temperature 1h obtains biomophic nano magnesia, and particle diameter is 10～25nm, and purity is 96.3～98.1.
Embodiment 3
Preparation of the present invention has the method for the nano magnesia of cotton cloth form, may further comprise the steps:
(1) with the Mg (CH of purity 〉=99.0%
3COO)
24H
2O is made into the solution that concentration is 0.3mol/L;
(2) with after cotton usefulness distilled water thorough washing and the oven dry, put into the above-mentioned solution for preparing, 12h is soaked in sealing, and the cotton that soaked is taken out, put into drying baker, be heated to 80 ℃, constant temperature drying 2h carries out temperature-programmed calcination: then with the temperature rise rate of 5 ℃/min in flowing air, be heated to 300 ℃, constant temperature 1h obtains biomophic nano magnesia, and particle diameter is 5～20nm, and purity is 87.6～88.2%.
Claims (2)
1. method for preparing the nano magnesia with cotton cloth form is characterized in that may further comprise the steps:
(1) with Mg (CH
3COO)
24H
2O is made into the solution that concentration is 0.3～0.8mol/L;
(2) with after cotton distilled water thorough washing, the oven dry, put into above-mentioned solution, 12～24h is soaked in sealing;
(3) will put into drying baker through the cotton taking-up that handled step (2), be heated to 80 ℃, constant temperature drying 2h; In flowing air, carry out temperature-programmed calcination then, obtain having the nano magnesia of cotton cloth form.
2. preparation method according to claim 1 is characterized in that: described temperature-programmed calcination condition is: the temperature rise rate with 5 ℃/min is heated to 300 ℃, 500 ℃ or 800 ℃, and keeps constant temperature 1h in the temperature of setting.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100201917A CN101555026A (en) | 2009-05-07 | 2009-05-07 | Method for preparing nano-magnesia with cotton cloth form |
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| CNA2009100201917A CN101555026A (en) | 2009-05-07 | 2009-05-07 | Method for preparing nano-magnesia with cotton cloth form |
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Cited By (12)
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|---|---|---|---|---|
| CN102115147A (en) * | 2011-03-28 | 2011-07-06 | 许昌学院 | Chemical method for preparing copper oxide crystals with biological micro-nano structures by thermal decomposition |
| CN104264448A (en) * | 2014-10-21 | 2015-01-07 | 山东理工大学 | Method for preparing aluminum ferrous spinel fiber cloth by taking cloth containing cotton as template |
| CN104291848A (en) * | 2014-10-21 | 2015-01-21 | 山东理工大学 | Method of assisted synthesis of ferrous aluminous spinel by using cotton-containing cloth |
| CN104311006A (en) * | 2014-10-21 | 2015-01-28 | 山东理工大学 | Simple method for preparing zirconia fiber bricks |
| CN104311092A (en) * | 2014-10-21 | 2015-01-28 | 山东理工大学 | Simple method for preparing magnesium-aluminum spinel fiber brick |
| CN104326735A (en) * | 2014-10-21 | 2015-02-04 | 山东理工大学 | Simple method for preparing magnesium oxide fiber cloth by taking cotton-containing fabric as template |
| CN104326738A (en) * | 2014-10-21 | 2015-02-04 | 山东理工大学 | Simple method for preparing aluminum oxide fiber cloth by taking cotton-containing cloth as template |
| CN104326736A (en) * | 2014-10-21 | 2015-02-04 | 山东理工大学 | Simple method for preparing magnesium oxide fiber brick |
| CN104326737A (en) * | 2014-10-21 | 2015-02-04 | 山东理工大学 | Simple method for preparing aluminum oxide fiber brick |
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2009
- 2009-05-07 CN CNA2009100201917A patent/CN101555026A/en active Pending
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115147A (en) * | 2011-03-28 | 2011-07-06 | 许昌学院 | Chemical method for preparing copper oxide crystals with biological micro-nano structures by thermal decomposition |
| CN102115147B (en) * | 2011-03-28 | 2012-11-21 | 许昌学院 | Chemical method for preparing copper oxide crystals with biological micro-nano structures by thermal decomposition |
| CN104264448A (en) * | 2014-10-21 | 2015-01-07 | 山东理工大学 | Method for preparing aluminum ferrous spinel fiber cloth by taking cloth containing cotton as template |
| CN104291848A (en) * | 2014-10-21 | 2015-01-21 | 山东理工大学 | Method of assisted synthesis of ferrous aluminous spinel by using cotton-containing cloth |
| CN104311006A (en) * | 2014-10-21 | 2015-01-28 | 山东理工大学 | Simple method for preparing zirconia fiber bricks |
| CN104311092A (en) * | 2014-10-21 | 2015-01-28 | 山东理工大学 | Simple method for preparing magnesium-aluminum spinel fiber brick |
| CN104326735A (en) * | 2014-10-21 | 2015-02-04 | 山东理工大学 | Simple method for preparing magnesium oxide fiber cloth by taking cotton-containing fabric as template |
| CN104326738A (en) * | 2014-10-21 | 2015-02-04 | 山东理工大学 | Simple method for preparing aluminum oxide fiber cloth by taking cotton-containing cloth as template |
| CN104326736A (en) * | 2014-10-21 | 2015-02-04 | 山东理工大学 | Simple method for preparing magnesium oxide fiber brick |
| CN104326737A (en) * | 2014-10-21 | 2015-02-04 | 山东理工大学 | Simple method for preparing aluminum oxide fiber brick |
| CN104326741A (en) * | 2014-10-21 | 2015-02-04 | 山东理工大学 | Simple method for preparing magnesium aluminate spinel fiber cloth with cotton-containing cloth as template |
| CN104341151A (en) * | 2014-10-21 | 2015-02-11 | 山东理工大学 | Simple method for preparing zirconium oxide fiber fabric by using cotton-containing fabric as template |
| CN104387098A (en) * | 2014-10-21 | 2015-03-04 | 山东理工大学 | Simple preparation method of ferrous aluminum spinel fiber brick |
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| CN104326738B (en) * | 2014-10-21 | 2016-03-23 | 山东理工大学 | A kind of simple method to be Template preparation alumina fibre cloth containing cotton cloth |
| CN104291848B (en) * | 2014-10-21 | 2016-04-27 | 山东理工大学 | A kind of use assists the method for synthesizing ferrous aluminum spinel containing cotton cloth |
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| CN104341151B (en) * | 2014-10-21 | 2016-08-17 | 山东理工大学 | A kind of straightforward procedure to prepare zirconium oxide fiber cloth for template containing cotton cloth |
| CN104326735B (en) * | 2014-10-21 | 2016-09-28 | 山东理工大学 | A kind of straightforward procedure to prepare magnesia fibers cloth for template containing cotton cloth |
| CN104326736B (en) * | 2014-10-21 | 2016-09-28 | 山东理工大学 | A kind of straightforward procedure preparing magnesia fibers brick |
| CN104311006B (en) * | 2014-10-21 | 2016-09-28 | 山东理工大学 | A kind of method of the Zirconium oxide fibre brick prepared containing 3mol% yittrium oxide |
| CN104387098B (en) * | 2014-10-21 | 2017-01-11 | 山东理工大学 | Simple preparation method of ferrous aluminum spinel fiber brick |
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Application publication date: 20091014 |