CN103030159B - A kind of porous magnesia, preparation method and its usage - Google Patents
A kind of porous magnesia, preparation method and its usage Download PDFInfo
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Abstract
The present invention relates to a kind of without the synthesizing porous magnesian preparation method of hydrothermal template.Described method take water as solvent, and using solubility magnesium salts as magnesium source, soluble carbonate salt is as precipitation agent, in 110 ~ 220 DEG C of isothermal reaction 5 ~ 24h in teflon-lined autoclave, through being separated, washing, drying, by dried white powder roasting, can obtain porous oxidation magnesium granules.Described porous oxidation magnesium granules, mean pore size is at 10 ~ 15nm, and specific surface area is at 100m
2g
-1, pore volume is 0.25 ~ 0.28cm
3g
-1.Described porous magnesia is suitable as sorbent material, also can be used as catalyzer or carrier, and starting material are easy to get, cost is low, process control is simple.
Description
Technical field
The present invention relates to a kind of method not adopting template to prepare porous magnesia and the porous magnesia prepared by the method.
Background technology
Magnesium oxide is widely used in catalysis, the improvement of Toxic waste, the critical function material in the field such as antibacterial.Magnesium oxide can be used as catalyzer and carrier, meanwhile, due to mgo surface there is a large amount of defect, limit, angle, step isoreactivity position make it can as sorbent material, absorption obnoxious flavour or remove harmful metal ion in water.
Compare the magnesium oxide of atresia, porous magnesia can be used as sorbent material, can adsorb and eliminate more obnoxious flavour.In recent years, people adopt multiple method to prepare porous magnesia, as hard template method, soft template method.Hard template method adopts as mesoporous carbon such as CMK-3, CMK-5 as template, and water-soluble magnesium salts, as magnesium source, copies and obtains orderly porous magnesia.But adopting this kind of method to prepare mesoporous magnesia, template is depended in product form and aperture, and building-up process is quite complicated, consuming time and output is very low.The preparation procedure of template is generally: first prepare as mesopore silicon oxides such as SBA-15, KIT-6, and then utilizes sucrose etc. to copy as carbon source, after sulfuric acid carbonization, at N
2high temperature pyrolysis carbonization under gas shielded, finally removes silicon oxide with hydrofluoric acid, the mesoporous carbon obtained, and recycling magnesium salt solution copies, roasting obtains mesoporous magnesia.Such as, JanRoggenbuck(Jan Roggenbuck, Michael Tiemann, J.Am.Chem.Soc., 2005,127 (4): 1096-1097; Jan Roggenbuck, Gunter Koch, and Michael Tiemann, Chem.Mater., 2006,18:4151-4156) etc. the mesoporous magnesium oxide that adopted CMK-3 as Template preparation.In addition, also can adopt as segmented copolymer P123, polyoxyethylene glycol, cetyl trimethylammonium bromide (CTAB), citric acid etc. as dispersion agent, adopt hydro-thermal or solvent-thermal method to obtain presoma, then roasting obtain porous magnesia.Such as: Guozhi Wang etc. adopt P123 to prepare mesoporous magnesium oxide (Guozhi Wang, etc., Inorg.Chem., 2008,47:4015-4022 as soft template; CN 1974881); Dai Hongxing (CN101734691A) etc. are dispersion agent with polyoxyethylene glycol, CTAB, and amino dodecane is solvent, and solvent-thermal method prepares porous magnesia; Limiao Chen(Limiao Chen, et.al., Applied Catalysis A:General, 2004,265:123-128) etc. adopt citric acid to prepare the magnesium oxide structure of porous as dispersion agent.In sum, adopt mesoporous carbon etc. can synthesize relatively orderly mesoporous magnesia as the hard template method of template, but its building-up process complicated and time consumption, output is very low; And adopting organism as soft template method, the porous magnesia of preparation, the relative hard template method of process is simple, but adds the complicacy of synthetic technology.Therefore, rule, particle size are comparatively even relatively not adopt any template or organism dispersion agent to prepare pattern, and the porous magnesia of even aperture distribution has great importance.But, in document with patent, rarely have report not adopt any template or dispersion agent to prepare the method for the relative rule of pattern, the more uniform porous magnesia of particle size.
Summary of the invention
An object of the present invention is that overcoming hard template method prepares slow, the inefficient problem of speed, dispersion agent legal system must use the problem of multiple dispersion agent for porous magnesia, a kind of method not adopting template or dispersion agent to prepare porous magnesia is provided, described method raw material is easy to get, simple, process easily controls.
In order to achieve the above object, present invention employs following technical scheme:
A preparation method for porous magnesia, described method comprises the steps:
(1) aqueous solution of solubility magnesium salts and the aqueous solution of soluble carbonate salt is prepared;
(2) by the aqueous solution of solubility magnesium salts and the aqueous solution of soluble carbonate salt, the mixing solutions obtained is moved in the reactor of sealing, react at 110 ~ 220 DEG C of temperature;
(3) after reaction terminates, be separated and obtain white depositions, washing, dry;
(4) by dried white powder roasting, porous magnesia is obtained.
The invention provides a kind of without the synthesizing porous magnesian preparation method of hydrothermal template.Described method take water as solvent, and using solubility magnesium salts as magnesium source, soluble carbonate salt is as precipitation agent, in the reaction kettle for reaction of sealing, question response terminates rear separation, washing, drying, then by dried white powder roasting, can obtain porous oxidation magnesium granules.
Described solubility magnesium salts is selected from the mixture of any one or at least two kinds in magnesium nitrate, magnesium chloride, magnesium sulfate or magnesium acetate.The mixture of described mixture such as magnesium nitrate and magnesium chloride, the mixture of magnesium nitrate and magnesium sulfate, the mixture of magnesium nitrate and magnesium acetate, the mixture of magnesium chloride and magnesium sulfate, the mixture of magnesium chloride and magnesium acetate, the mixture of magnesium sulfate, magnesium nitrate and magnesium chloride, the mixture of magnesium chloride, magnesium sulfate and magnesium acetate.Described magnesium chloride, the crystal water containing six molecules, i.e. MgCl
26H
2o, the molecular formula of magnesium nitrate is Mg (NO
3)
26H
2o, the molecular formula of magnesium sulfate is MgSO
47H
2o, the molecular formula of magnesium acetate is C
4h
6o
4mg4H
2o.
Described soluble carbonate salt is selected from the mixture of any one or at least two kinds in sodium carbonate, salt of wormwood or bicarbonate of ammonia.The mixing of described mixture such as sodium carbonate and salt of wormwood, the mixture of sodium carbonate and bicarbonate of ammonia, the mixture of salt of wormwood and bicarbonate of ammonia, the mixture of sodium carbonate, salt of wormwood and bicarbonate of ammonia.
The mol ratio of described solubility magnesium salts and soluble carbonate salt is (0.8 ~ 1.5): 1, such as 0.9:1,1.0:1,1.1:1,1.2:1,1.3:1,1.4:1, preferred 1:1.
Described reactor is the teflon-lined autoclave of sealing.
The temperature of step (2) described reaction is 110 ~ 220 DEG C, such as 120 DEG C, 130 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, 170 DEG C, 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C, preferably 125 ~ 205 DEG C, preferably 140 ~ 180 DEG C further.
Reaction times described in step (2) is 5 ~ 24 hours, such as 6 hours, 8 hours, 10 hours, 12 hours, 14 hours, 16 hours, 18 hours, 20 hours, 22 hours, preferably 7 ~ 22 hours, preferably 8 ~ 20 hours further.
Can stir in described reaction process, accelerate reaction process.
After step (2) reaction terminates, naturally cool to room temperature, be separated and obtain white depositions.The method that solid-liquid separation that what those skilled in the art can be known realize arbitrarily obtains solid all can realize the present invention, as optimal technical scheme, described separation be selected from filtration, centrifugation, precipitation, gravity settling or centrifugal settling any one, preferred filtration or centrifugation, further preferably centrifugation.
After separation obtains solid, water and dehydrated alcohol is adopted to wash respectively.The number of times of described washing is 1 ~ 5 time, preferably 2 ~ 4 times, preferably 2 times further.The number of times that described dehydrated alcohol is washed is 1 ~ 4 time, preferably 1 ~ 3 time, preferably 1 time further.
The temperature of described drying is 80 ~ 100 DEG C, such as 82 DEG C, 84 DEG C, 86 DEG C, 88 DEG C, 90 DEG C, 92 DEG C, 94 DEG C, 96 DEG C, 98 DEG C, preferably 85 ~ 95 DEG C.
Preferably, by the roasting in air atmosphere of dried white powder, porous magnesia is obtained.The equipment such as retort furnace of described roasting.Described maturing temperature is 500 ~ 900 DEG C, such as 520 DEG C, 560 DEG C, 600 DEG C, 640 DEG C, 680 DEG C, 710 DEG C, 730 DEG C, 770 DEG C, 810 DEG C, 840 DEG C, 870 DEG C, preferably 650 ~ 850 DEG C, preferably 700 ~ 800 DEG C further.
Described roasting time is 0.5 ~ 5 hour, such as 0.8 hour, 1.2 hours, 1.5 hours, 1.8 hours, 2.5 hours, 3.2 hours, 4.1 hours, 4.8 hours, preferably 1 ~ 4 hour, preferably 1 ~ 3 hour further.
Temperature rise rate in described roasting process is 4 ~ 12 DEG C/min, such as 4.5 DEG C/min, 5.2 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min, 9 DEG C/min, 10 DEG C/min, 11 DEG C/min, 12 DEG C/min, 13 DEG C/min, 14 DEG C/min, preferably 5 ~ 10 DEG C/min.
After the white powder roasting of drying, naturally cool to room temperature, porous oxidation magnesium granules can be obtained.
A preparation method for porous magnesia, described method comprises the steps:
(1 ') is water-soluble as magnesium source using solubility magnesium salts, the aqueous solution of preparation solubility magnesium salts, and soluble carbonate salt is water-soluble, and the aqueous solution of preparation soluble carbonate salt, as precipitation agent;
The aqueous solution of solubility magnesium salts that step (1 ') obtains by (2 ') and the aqueous solution of soluble carbonate salt, wherein, the mol ratio of solubility magnesium salts and soluble carbonate salt is 1:1;
The mixing solutions that step (2 ') obtains is transferred in teflon-lined autoclave by (3 '), sealing, at 110 ~ 220 DEG C of isothermal reaction 5 ~ 24h, after reaction terminates, naturally cools to room temperature;
(4 ') centrifugation obtains white depositions thing, washing twice, and dehydrated alcohol is washed once, dry at 80 ~ 100 DEG C of temperature;
(5) by dried white powder in air atmosphere, with the ramp of 5 ~ 10 DEG C/min, at 500 ~ 900 DEG C, roasting 1 ~ 3 hour, naturally cools to room temperature, namely obtains porous magnesia.
Two of object of the present invention is to provide a kind of porous magnesia prepared by method described above.The mean pore size of described porous magnesia is 10 ~ 15nm, and specific surface area is 100m
2g
-1, pore volume is 0.25 ~ 0.28cm
3g
-1.Porous magnesia obtained by the present invention is suitable for as sorbent material, also can be used as catalyzer or carrier, and starting material are easy to get, cost is low, process control is simple.
Three of object of the present invention is the purposes providing a kind of porous magnesia as above, and described porous magnesia is as sorbent material, carrier or catalyzer.
Compared with prior art, the present invention has following beneficial effect:
(1) the method for the invention is without any need for template, can prepare porous magnesia;
(2) adopt the magnesium oxide grain-size for preparing of the method for the invention relatively more even, generally several to tens microns, avoid the hazardness of nano particle to human body;
(3) the method for the invention, presoma magnesium basic carbonate crystal grain heats in common heating equipment can realize decomposition, and this process does not need atmosphere protection, simplifies technical process, reduces cost, makes heavy industrialization become possibility.
Accompanying drawing explanation
Technical scheme of the present invention is further illustrated by embodiment below in conjunction with accompanying drawing.
Fig. 1: the XRD spectra of porous magnesia crystal grain prepared by the present invention, the XRD spectra of the porous magnesia sample that wherein curve (a) and (b), (c) are respectively embodiment 1, embodiment 2, embodiment 3 prepare;
Fig. 2: the scanning electron microscope of porous magnesia crystal grain prepared by the present invention and transmission electron microscope photo, wherein Fig. 2-1, Fig. 2-2, Fig. 2-4 are respectively the stereoscan photograph of embodiment 1 sample, embodiment 2 sample and embodiment 3 sample, and Fig. 2-3 is the transmission electron microscope photo of embodiment 2 sample;
Fig. 3: be the N of porous magnesia crystal grain prepared by the present invention
2aspiration is attached-desorption curve and pore distribution curve, and wherein Fig. 3-1 is the N of embodiment 1 sample, embodiment 2 sample
2aspiration is attached-desorption curve, and Fig. 3-2 is the pore distribution of embodiment 1 sample, embodiment 2 sample, and 1 represents that embodiment 1,2 represents embodiment 2;
Fig. 4: magnesian stereoscan photograph in comparative example 1 in the present invention.
Embodiment
For better the present invention being described, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
Take 4.005gMg (NO
3)
26H
2o is placed in 100ml beaker, adds 50ml water, and magnetic agitation makes it dissolve; Take 1.66g anhydrous sodium carbonate and be placed in 100ml beaker, then add 30ml water, magnetic agitation makes it dissolve; Then sodium carbonate solution is poured in magnesium nitrate solution, form white mixture immediately, then white mixture being moved into volume is in the teflon-lined autoclave of 100ml, in 110 DEG C of constant temperature process 5h, be cooled to room temperature after taking-up, the mixture centrifugation of gained, wash 2 times, dehydrated alcohol washes 1 time, then that it is dry in 80 DEG C of baking ovens.Dried powder puts into retort furnace, rises to 500 DEG C, and be incubated 2h at such a temperature with 5 DEG C/min speed from room temperature, namely obtains the porous magnesia micron particle of cubic crystal structure.
Embodiment 2
Take 4.066gMgCl
26H
2o is placed in 100ml beaker, adds 50ml water, and magnetic agitation makes it dissolve; Take 2.764g Anhydrous potassium carbonate and be placed in 100ml beaker, then add 30ml water, magnetic agitation makes it dissolve; Then solution of potassium carbonate is poured in magnesium chloride solution, form white mixture immediately, then white mixture being moved into volume is in the teflon-lined autoclave of 100ml, in 180 DEG C of constant temperature process 24h, be cooled to room temperature after taking-up, the mixture centrifugation of gained, wash 2 times, dehydrated alcohol washes 1 time, then that it is dry in 100 DEG C of baking ovens.Dried powder puts into retort furnace, rises to 650 DEG C, and be incubated 3h at such a temperature with 8 DEG C/min speed from room temperature, namely obtains the porous magnesia micron particle of cubic crystal structure.
Embodiment 3
Take 6.432gC
4h
6o
4mg4H
2o is placed in 100ml beaker, adds 80ml water, and magnetic agitation makes it dissolve; Take 2.372g bicarbonate of ammonia and be placed in 100ml beaker, then add 80ml water, magnetic agitation makes it dissolve; Then ammonium bicarbonate soln is poured in magnesium acetate solution, form white mixture immediately, then white mixture being moved into volume is in the teflon-lined autoclave of 200ml, in 220 DEG C of constant temperature process 15h, be cooled to room temperature after taking-up, the mixture centrifugation of gained, wash 2 times, dehydrated alcohol washes 1 time, then that it is dry in 100 DEG C of baking ovens.Dried powder puts into retort furnace, rises to 900 DEG C, and be incubated 1h at such a temperature with 10 DEG C/min speed from room temperature, namely obtains the porous magnesia micron particle of cubic crystal structure.
Comparative example 1
Take 4.005gMg (NO
3)
26H
2o is placed in 100ml beaker, adds 50ml water, and magnetic agitation makes it dissolve; Take 1.66g anhydrous sodium carbonate and be placed in 100ml beaker, then add 30ml water, magnetic agitation makes it dissolve; Then sodium carbonate solution is poured in magnesium nitrate solution, form white mixture immediately, then white mixture being moved into volume is in the teflon-lined autoclave of 100ml, in 100 DEG C of constant temperature process 24h, be cooled to room temperature after taking-up, the mixture centrifugation of gained, wash 2 times, dehydrated alcohol washes 1 time, then that it is dry in 80 DEG C of baking ovens.Dried powder puts into retort furnace, rises to 600 DEG C, and is incubated 2h at such a temperature, obtain magnesium oxide rod-shpaed particle with 5 DEG C/min speed from room temperature.
Fig. 1 is the XRD spectra of porous magnesia crystal grain prepared by the present invention, wherein curve (a) and (b), (c) are respectively the XRD spectra of porous magnesia sample of embodiment 1, embodiment 2, embodiment 3 gained, by comparing with JCPDS 45-0946 spectrogram diffraction peak parameter, be defined as cubic structure magnesium oxide.
Fig. 2 is scanning electron microscope and the transmission electron microscope photo of porous magnesia crystal grain prepared by the present invention, wherein Fig. 2-1, Fig. 2-2, Fig. 2-4 are respectively the stereoscan photograph of embodiment 1 sample, embodiment 2 sample and embodiment 3 sample, Fig. 2-3 is the transmission electron microscope photo of embodiment 2 sample, shows that sample has meso-hole structure.
Fig. 3 is the N of porous magnesia crystal grain prepared by the present invention
2aspiration is attached-desorption curve and pore distribution curve, and wherein Fig. 3-1 is the N of embodiment 1 sample, embodiment 2 sample
2aspiration is attached-desorption curve, and Fig. 3-2 is the pore distribution of embodiment 1 sample, embodiment 2 sample, shows that sample has mesoporous pore structure.
Fig. 4 is magnesian stereoscan photograph in comparative example 1 in the present invention.
Embodiment 4
Take 3.253gMgCl
26H
2o is placed in 100ml beaker, adds 50ml water, and magnetic agitation makes it dissolve; Take 2.764g Anhydrous potassium carbonate and be placed in 100ml beaker, then add 30ml water, magnetic agitation makes it dissolve; Then solution of potassium carbonate is poured in magnesium chloride solution, form white mixture immediately, then white mixture being moved into volume is in the teflon-lined autoclave of 100ml, in 110 DEG C of constant temperature process 24h, be cooled to room temperature after taking-up, the mixture centrifugation of gained, wash 1 time, dehydrated alcohol washes 1 time, then that it is dry in 80 DEG C of baking ovens.Dried powder puts into retort furnace, rises to 500 DEG C, and be incubated 5h at such a temperature with 4 DEG C/min speed from room temperature, namely obtains the porous magnesia micron particle of cubic crystal structure.
Embodiment 5
Take 6.099gMgCl
26H
2o is placed in 100ml beaker, adds 50ml water, and magnetic agitation makes it dissolve; Take 2.764g Anhydrous potassium carbonate and be placed in 100ml beaker, then add 30ml water, magnetic agitation makes it dissolve; Then solution of potassium carbonate is poured in magnesium chloride solution, form white mixture immediately, then white mixture being moved into volume is in the teflon-lined autoclave of 100ml, in 220 DEG C of constant temperature process 5h, be cooled to room temperature after taking-up, the mixture centrifugation of gained, wash 5 times, dehydrated alcohol washes 4 times, then that it is dry in 100 DEG C of baking ovens.Dried powder puts into retort furnace, rises to 900 DEG C, and be incubated 1h at such a temperature with 12 DEG C/min speed from room temperature, namely obtains the porous magnesia micron particle of cubic crystal structure.
Applicant states, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (32)
1. a preparation method for porous magnesia, is characterized in that, described porous magnesia mean pore size is 10 ~ 15nm, and specific surface area is 100m
2g
-1, pore volume is 0.25 ~ 0.28cm
3g
-1, described method comprises the steps:
(1) aqueous solution of solubility magnesium salts and the aqueous solution of soluble carbonate salt is prepared;
(2) by the aqueous solution of solubility magnesium salts and the aqueous solution of soluble carbonate salt, the mixing solutions obtained is moved in the reactor of sealing, react at 140 ~ 200 DEG C of temperature, described soluble carbonate salt is selected from sodium carbonate or/and salt of wormwood, and the mol ratio of described solubility magnesium salts and soluble carbonate salt is (0.8 ~ 1.5): 1;
(3) after reaction terminates, be separated and obtain white depositions, washing, dry;
(4) by dried white powder roasting, porous magnesia is obtained.
2. the method for claim 1, is characterized in that, described solubility magnesium salts is selected from the mixture of any one or at least two kinds in magnesium nitrate, magnesium chloride, magnesium sulfate or magnesium acetate.
3. method as claimed in claim 1 or 2, it is characterized in that, the mol ratio of described solubility magnesium salts and soluble carbonate salt is 1:1.
4. the method as described in one of claim 1-2, is characterized in that, described reactor is the teflon-lined autoclave of sealing.
5. the method as described in one of claim 1-2, is characterized in that, the temperature of step (2) described reaction is 140 ~ 180 DEG C.
6. the method as described in one of claim 1-2, is characterized in that, the reaction times described in step (2) is 5 ~ 24 hours.
7. method as claimed in claim 6, it is characterized in that, the reaction times described in step (2) is 7 ~ 22 hours.
8. method as claimed in claim 7, it is characterized in that, the reaction times described in step (2) is 8 ~ 20 hours.
9. the method as described in one of claim 1-2, is characterized in that, described separation be selected from filtration, centrifugation, precipitation, gravity settling or centrifugal settling any one.
10. method as claimed in claim 9, is characterized in that, described separation is selected from filtration or centrifugation.
11. methods as claimed in claim 10, it is characterized in that, described separation is selected from centrifugation.
12. methods as described in one of claim 1-2, is characterized in that, are separated after obtaining white depositions, adopt water and dehydrated alcohol to wash respectively.
13. methods as claimed in claim 12, is characterized in that, the number of times of described washing is 1 ~ 5 time.
14. methods as claimed in claim 13, is characterized in that, the number of times of described washing is 2 ~ 4 times.
15. methods as claimed in claim 14, is characterized in that, the number of times of described washing is 2 times.
16. methods as claimed in claim 12, it is characterized in that, the number of times that described dehydrated alcohol is washed is 1 ~ 4 time.
17. methods as claimed in claim 16, it is characterized in that, the number of times that described dehydrated alcohol is washed is 1 ~ 3 time.
18. methods as claimed in claim 17, it is characterized in that, the number of times that described dehydrated alcohol is washed is 1 time.
19. methods as described in one of claim 1-2, it is characterized in that, the temperature of described drying is 80 ~ 100 DEG C.
20. methods as claimed in claim 19, is characterized in that, the temperature of described drying is 85 ~ 95 DEG C.
21. methods as described in one of claim 1-2, is characterized in that, by the roasting in air atmosphere of dried white powder.
22. methods as described in one of claim 1-2, it is characterized in that, described maturing temperature is 500 ~ 900 DEG C.
23. methods as claimed in claim 22, it is characterized in that, described maturing temperature is 650 ~ 850 DEG C.
24. methods as claimed in claim 23, it is characterized in that, described maturing temperature is 700 ~ 800 DEG C.
25. methods as described in one of claim 1-2, it is characterized in that, described roasting time is 0.5 ~ 5 hour.
26. methods as claimed in claim 25, it is characterized in that, described roasting time is 1 ~ 4 hour.
27. methods as claimed in claim 26, it is characterized in that, described roasting time is 1 ~ 3 hour.
28. methods as described in one of claim 1-2, it is characterized in that, the temperature rise rate in described roasting process is 4 ~ 12 DEG C/min.
29. methods as claimed in claim 28, it is characterized in that, the temperature rise rate in described roasting process is 5 ~ 10 DEG C/min.
30. methods as claimed in claim 22, it is characterized in that, described method comprises the steps:
(1 ') is water-soluble as magnesium source using solubility magnesium salts, the aqueous solution of preparation solubility magnesium salts, and soluble carbonate salt is water-soluble, and the aqueous solution of preparation soluble carbonate salt, as precipitation agent;
The aqueous solution of solubility magnesium salts that step (1 ') obtains by (2 ') and the aqueous solution of soluble carbonate salt, wherein, the mol ratio of solubility magnesium salts and soluble carbonate salt is 1:1;
The mixing solutions that step (2 ') obtains is transferred in teflon-lined autoclave by (3 '), sealing, at 140 ~ 200 DEG C of isothermal reaction 5 ~ 24h, after reaction terminates, naturally cools to room temperature;
(4 ') centrifugation obtains white depositions thing, washing twice, and dehydrated alcohol is washed once, dry at 80 ~ 100 DEG C of temperature;
(5) by dried white powder in air atmosphere, with the ramp of 5 ~ 10 DEG C/min, at 500 ~ 900 DEG C, roasting 1 ~ 3 hour, naturally cools to room temperature, namely obtains porous magnesia.
31. 1 kinds of porous magnesias prepared by the described method of one of claim 1-30, it is characterized in that, described porous magnesia mean pore size is 10 ~ 15nm, specific surface area is 100m
2g
-1, pore volume is 0.25 ~ 0.28cm
3g
-1.
The purposes of 32. 1 kinds of porous magnesias as claimed in claim 31, is characterized in that, described porous magnesia is as sorbent material, carrier or catalyzer.
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| CN108584999A (en) * | 2018-06-12 | 2018-09-28 | 程桂平 | A kind of preparation method of magnesia presoma |
| CN109524647A (en) * | 2018-11-07 | 2019-03-26 | 新奥石墨烯技术有限公司 | A kind of mesoporous grapheme material of micron order |
| CN109292757A (en) * | 2018-11-20 | 2019-02-01 | 张家港博威新能源材料研究所有限公司 | A kind of graphene and preparation method thereof |
| CN109734081A (en) * | 2019-03-18 | 2019-05-10 | 新奥石墨烯技术有限公司 | Mesoporous template and preparation method thereof, three-dimensional meso-hole graphene and preparation method thereof, energy storage material and battery |
| WO2020205839A1 (en) * | 2019-04-01 | 2020-10-08 | Technology Applications Group, Inc. | Anodized coating for magnesium |
| CN111943238A (en) * | 2020-08-21 | 2020-11-17 | 西南科技大学 | Preparation method of porous pompon-like magnesium oxide |
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