CN103539121B - Porous carbonate and porous oxide preparation methods - Google Patents
Porous carbonate and porous oxide preparation methods Download PDFInfo
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- CN103539121B CN103539121B CN201310474082.9A CN201310474082A CN103539121B CN 103539121 B CN103539121 B CN 103539121B CN 201310474082 A CN201310474082 A CN 201310474082A CN 103539121 B CN103539121 B CN 103539121B
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Abstract
The invention relates to porous carbonate and porous oxide preparation methods. Crystal water-containing salts of same or different metal ions which can form carbonate precipitates are selected, the crystal water-containing salts are added with a precipitator and a pore-forming agent, the mixed raw materials are mixed uniformly and then are grinded at a room temperature for 5-600min, the grinded raw materials are taken out and then is stood for 0.5-24h, the stood raw materials are taken out and then are subjected to suction filtration, the filtration product is washed by a washing agent so that the pore-forming agent is removed, and the washed product is dried to form a porous carbonate; and the porous carbonate is calcined to form a porous oxide. The porous carbonate and porous oxide preparation methods are green and environmentally friendly, can be carried out at a room temperature under normal pressure, are free of high temperature and high pressure conditions and have an obviously reduced cost.
Description
Technical field:
The present invention relates to a kind of preparation method of porous material, simple, environmental protection.
Background technology:
Inorganic porous material is the material being rich in pore structure that a class has the features such as larger specific surface area, low density, lower thermal conductivity, high porosity.The daily life of inorganic porous material on us creates huge directly and indirectly affecting.Inorganic porous material is widely used as commercial catalysts and support of the catalyst, separating agent, sorbent material, insulation, thermal insulation, sewage and off gas treatment, filter liquide and gas (even bacterium), light building material, the NO in air
xeliminate carbonic acid gas and water in the vehicle maintenance service such as compound and sulfurous gas, spaceship, agriculturally can be used to improve soil, what can also be used as in filler in cement, rubber, plastics and paper industry and chromatogram is fixing equal.Except above-mentioned remote effect, inorganic porous material also directly affects our daily life.Such as, zeolite molecular sieve is used as washing assistant in detergent formulation.
With diatomite and molecular sieve (zeolite) most representativeness in natural inorganic porous material.Artificial porous material a multitude of names, existing single composition, have again multi-component, purposes is also different.The inorganic porous material with regular pore canal structure has more excellent application prospect in industrial shape selective catalysis, Subjective and Objective assembling, photoelectricity magnetics contour new science and technology field, causes people to the great interest of this kind of material correlative study and attention.The distribution direct relation of the size in inorganic porous material duct, shape and volume size this material ability possessed in a particular application.In recent years, due to the remarkable application performance of orderly inorganic porous material, create and there is homogeneous size duct, increasing steadily of the inorganic porous material of homogeneous shape and volume.Simultaneously, along with the development of material technology, the function application of people to inorganic porous material proposes more requirements, and the New function of exploitation inorganic porous material has become the vital task of researcher, and the assembling of inorganic porous material and functionalization are for herein is provided more development opportunities.
Along with industrial development, the purposes of carbonate is more and more extensive.Adopt carbonate as activator, activation rice husk, prepares the high specific surface area porous charcoal with meso-hole structure.Utilize carbonate to make electrolytical fuel cell, working temperature is at about 650 DEG C, and the reaction of negative electrode, anode electrochemical is fast, without the need to noble metal catalyst; Due in comparatively high temps work, inside reforming can be carried out to Sweet natural gas, gasification of coal fuel, directly be used, not need the outer reformer apparatus of complex and expensive; In addition, fuel conversion efficiency is high, and utilization rate of waste heat is also higher.Biomimetic mineralization synthesizes the calcium carbonate material that the calcium carbonate material that is prepared into synthesizes compared to ordinary chemical method, often have a lot of special appearance and premium properties, large quantifier elimination is absorbed in crystallization and the growth mechanism of being explained calcium carbonate by the special performance of analysis of biological material and the interaction between research organic substrate and inorganic metal ion.Barium carbonate is as one of important barium salt simultaneously as a kind of important basic chemical raw materials, and be all widely used in numerous areas, the ratio related to is if any industry and departments such as glass, pottery, electronics, optics, chemical industry, Water warfare and three-protection design; In recent years, along with the development of all trades and professions, the Application Areas also expanding day of barium carbonate, and also different to the requirement of the crystal morphology size of barium carbonate etc. in different use fields; For complying with the growth requirement of society, barium carbonate industry is also just towards the future development of high quality, simple process, less energy-consumption.
The synthetic method of porous material is a lot, has the synthetic methods such as sol-gel method, hydrothermal synthesis method, the precipitator method, chemical corrosion method, and what application was maximum at present is sol-gel method and hydrothermal synthesis method.Sol-gel method primary process adopts dissimilar template, the supramolecular structure formed with it is for template, by sol-gel process, under the interface guiding function between inorganics and organism, be self-assembled into the narrow and porous material that pore passage structure is regular of pore size distribution.Hydrothermal method carries out relevant chemical reaction under referring to High Temperature High Pressure in water (aqueous solution) or the fluid such as solvent, steam. by inner at special closed reaction vessel (autoclave), adopt the aqueous solution or other solvents as reaction medium, container is heated, self create high temperature, a reaction under high pressure environment after making water or solvent evaporation, make usual indissoluble or insoluble substance dissolves and recrystallization.Above two kinds of methods experiment processes are complicated, and requirement for experiment condition is high, and production cost is very high.
Summary of the invention:
The object of the invention is to overcome above-mentioned deficiency and the preparation method that a kind of porous carbon hydrochlorate and porous oxide are provided.
The technical scheme that the present invention takes is:
A preparation method for porous carbon hydrochlorate, select the metal ion that can form carbonate deposition containing crystal water salt, containing crystal water salt be same metal ion or different metal ion, crystal water salt is added precipitation agent and pore-forming material, by raw material blending, grinding at room temperature 5-600 minute, raw material after grinding is taken out, leave standstill 0.5-24 hour, after leaving standstill, take out, suction filtration, washing removing pore-forming material, dry, obtain porous carbon hydrochlorate.
The described metal ion that can form carbonate deposition comprises Ba
2+, Ca
2+, Zn
2+, Ge
2+, Gr
3+, Pb
2+, Cu
2+, Ni
2+, Mn
2+, Co
2+, Fe
2+, Zr
4+, La
3+, Sn
2+, Ag
+, Cd
2+, Au
+, Pd
2+, Ru
4+, Sb
3+, In
3+, Mo
3+, group of the lanthanides and actinide elements.
Described contains the preferred hydrated sulfate of crystal water salt.Described precipitation agent is bicarbonate of ammonia or sodium carbonate.
The described molar ratio containing crystal water salt, precipitation agent is 1:0.5-20, preferred 1:2-10; Be 1:0.5-100 containing crystal water salt and pore-forming material mass ratio.
A preparation method for porous oxide, select the metal ion that can form carbonate deposition containing crystal water salt, containing crystal water salt be same metal ion or different metal ion, crystal water salt is added precipitation agent and pore-forming material, by raw material blending, grinding at room temperature 5-600 minute, raw material after grinding is taken out, leave standstill 0.5-24 hour, after leaving standstill, take out, suction filtration, washing removing pore-forming material, dry, obtain porous carbon hydrochlorate; By porous carbonate roasting, maturing temperature 100-1500 DEG C, time 0.2-24 hour, obtains porous oxide.
The described metal ion that can form carbonate deposition comprises Ba
2+, Ca
2+, Zn
2+, Ge
2+, Gr
3+, Pb
2+, Cu
2+, Ni
2+, Mn
2+, Co
2+, Fe
2+, Zr
4+, La
3+, Sn
2+, Ag
+, Cd
2+, Au
+, Pd
2+, Ru
4+, Sb
3+, In
3+, Mo
3+, group of the lanthanides and actinide elements.Described contains the preferred hydrated sulfate of crystal water salt.Described precipitation agent is bicarbonate of ammonia or sodium carbonate.The described molar ratio containing crystal water salt, precipitation agent is 1:0.5-20, preferred 1:2-10; Be 1:0.5-100 containing crystal water salt and pore-forming material mass ratio.
Beneficial effect of the present invention is:
(1) environmental protection.Experimentation achieves zero release, no pollution.Operating process is harmless to experiment operator health, and experimental products is nontoxic.
(2) simple.Experimental procedure comprises: weigh, mixing, and grinding leaves standstill, suction filtration, dries.These experimental procedures are the most basic experimental skills, simple to operate.
(3) experimental situation requires low.Whole process is all under atmospheric pressure at room, and without the need to High Temperature High Pressure, production cost obviously reduces.
Accompanying drawing illustrates:
Fig. 1 is the transmission electron microscope photo of the zinc carbonate of synthesis, and magnification is 150,000 times, can find out that the zinc carbonate obtained is uniform vesicular structure.
Fig. 2 is the XRD comparison diagram of zinc carbonate and the pure zinc subcarbonate of synthesis, can find out that what obtained by the method synthesis is pure zinc carbonate.
The transmission electron microscope photo of the zinc oxide that Fig. 3 obtains after being the zinc carbonate roasting by synthesis, magnification is 80,000 times, can find out that the zinc oxide obtained also is uniform vesicular structure.
Fig. 4 is the transmission electron microscope photo of the manganous carbonate of synthesis, and magnification 200, can find out that the manganous carbonate obtained is uniform vesicular structure by 000 times.
Fig. 5 is the XRD figure of manganous carbonate of synthesis, can find out that what obtained by the method synthesis is pure manganese carbonate.
The transmission electron microscope photo of the manganese oxide that Fig. 6 obtains after being the manganous carbonate roasting by synthesis, magnification is 100,000 times, can find out that the manganese oxide obtained also is uniform vesicular structure.
Fig. 7 is the XRD figure of carbonic acid zinc-manganese mixture of synthesis, can find out the mixture for manganous carbonate and zinc carbonate obtained by the method synthesis.
Fig. 8 is the transmission electron microscope photo of the carbonic acid zinc-manganese of synthesis, magnification 120,000 times, can find out that the carbonic acid zinc-manganese obtained also is uniform vesicular structure.
Embodiment
Further illustrate below in conjunction with preferred embodiment.
Embodiment 1
Zinc vitriol and precipitation agent bicarbonate of ammonia is taken according to mol ratio 1:2, the pore-forming material PEG adding Zinc vitriol quality 2 times mixes with it, abundant grinding left standstill time enough (4 hours) after 40 minutes, take out, suction filtration, washing removing pore-forming material, dry, obtain porous zinc carbonate.By the roasting of a certain amount of porous zinc carbonate, temperature 600 DEG C, time 2 h, can obtain porous zinc bloom.
Embodiment 2
Seven anhydrous manganeses and precipitation agent bicarbonate of ammonia is taken according to mol ratio 1:2, the pore-forming material PEG adding seven anhydrous manganese quality 5 times mixes with it, abundant grinding left standstill time enough (4 hours) after 40 minutes, take out, suction filtration, washing removing pore-forming material, dry, obtain porous zinc carbonate.By the roasting of a certain amount of porous manganous carbonate, temperature 600 DEG C, time 2 h, can obtain how empty manganese oxide.
Embodiment 3
First the mixture of Zinc vitriol and manganous sulfate is taken according to mol ratio 1:2, and then take the precipitation agent bicarbonate of ammonia of vitriol quality 4 times, add appropriate pore-forming material PEG to mix with it, time enough (4 hours) is left standstill after abundant grinding (40 minutes), take out, suction filtration, washing removing pore-forming material, drying, obtains the mixture of porous zinc carbonate and manganous carbonate.
Embodiment 4
Seven anhydrous manganeses and precipitation agent bicarbonate of ammonia is taken according to mol ratio 1:4, the pore-forming material PEG adding seven anhydrous manganese quality 10 times mixes with it, abundant grinding left standstill time enough (6 hours) after 20 minutes, take out, suction filtration, washing removing pore-forming material, dry, obtain porous zinc carbonate.
Embodiment 5
Zinc vitriol and precipitation agent bicarbonate of ammonia is taken according to mol ratio 1:10, the pore-forming material PEG adding Zinc vitriol quality 7 times mixes with it, abundant grinding left standstill time enough (7 hours) after 60 minutes, take out, suction filtration, washing removing pore-forming material, dry, obtain porous zinc carbonate.By the roasting of a certain amount of porous zinc carbonate, temperature 700 DEG C, time 2 h, can obtain porous zinc bloom.
Claims (8)
1. a preparation method for porous carbon hydrochlorate, is characterized in that, that selects the metal ion that can form carbonate deposition contains crystal water salt, containing crystal water salt be same metal ion or different metal ion, crystal water salt added precipitation agent and pore-forming material, by raw material blending, grinding at room temperature 5-600 minute, takes out the raw material after grinding, leaves standstill 0.5-24 hour, after leaving standstill, take out, suction filtration, washing removing pore-forming material, drying, obtains porous carbon hydrochlorate; Described precipitation agent is bicarbonate of ammonia or sodium carbonate.
2. the preparation method of a kind of porous carbon hydrochlorate according to claim 1, is characterized in that, the described metal ion that can form carbonate deposition comprises Ba
2+, Ca
2+, Zn
2+, Ge
2+, Gr
3+, Pb
2+, Cu
2+, Ni
2+, Mn
2+, Co
2+, Fe
2+, Zr
4+, La
3+, Sn
2+, Ag
+, Cd
2+, Au
+, Pd
2+, Ru
4+, Sb
3+, In
3+, Mo
3+.
3. the preparation method of a kind of porous carbon hydrochlorate according to claim 1, is characterized in that, described selects hydrated sulfate containing crystal water salt.
4. the preparation method of a kind of porous carbon hydrochlorate according to claim 1, is characterized in that, the described molar ratio containing crystal water salt, precipitation agent is 1:0.5-20, is 1:0.5-100 containing crystal water salt and pore-forming material mass ratio.
5. a preparation method for porous oxide, is characterized in that, that selects the metal ion that can form carbonate deposition contains crystal water salt, containing crystal water salt be same metal ion or different metal ion, crystal water salt added precipitation agent and pore-forming material, by raw material blending, grinding at room temperature 5-600 minute, takes out the raw material after grinding, leaves standstill 0.5-24 hour, after leaving standstill, take out, suction filtration, washing removing pore-forming material, drying, obtains porous carbon hydrochlorate; By porous carbonate roasting, maturing temperature 100-1500 DEG C, time 0.2-24 hour, obtains porous oxide; Described precipitation agent is bicarbonate of ammonia or sodium carbonate.
6. the preparation method of a kind of porous oxide according to claim 5, is characterized in that, the described metal ion that can form carbonate deposition comprises Ba
2+, Ca
2+, Zn
2+, Ge
2+, Gr
3+, Pb
2+, Cu
2+, Ni
2+, Mn
2+, Co
2+, Fe
2+, Zr
4+, La
3+, Sn
2+, Ag
+, Cd
2+, Au
+, Pd
2+, Ru
4+, Sb
3+, In
3+, Mo
3+.
7. the preparation method of a kind of porous oxide according to claim 5, is characterized in that, described selects hydrated sulfate containing crystal water salt.
8. the preparation method of a kind of porous oxide according to claim 5, is characterized in that, the described molar ratio containing crystal water salt, precipitation agent is 1:0.5-20, is 1:0.5-100 containing crystal water salt and pore-forming material mass ratio.
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| TWI618577B (en) * | 2016-02-01 | 2018-03-21 | 新綠科學股份有限公司 | Method for producing metal carbonate and catalyst for producing the same |
| CN107293733B (en) * | 2017-05-24 | 2020-07-14 | 厦门大学 | Dual-ion battery |
| CN112430103B (en) * | 2020-11-19 | 2022-01-25 | 中国科学院金属研究所 | Photocuring 3D printing hierarchical pore ceramic material and preparation method thereof |
| CN115777703A (en) * | 2022-11-09 | 2023-03-14 | 普沃思环保科技无锡有限公司 | Metal oxide sterilization material and preparation method and application thereof |
Citations (4)
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|---|---|---|---|---|
| CN1431169A (en) * | 2003-02-18 | 2003-07-23 | 山东大学 | Method for preparing porous nano solid by using hot pressing technique through controllable vaporized solvent |
| CN1935655A (en) * | 2005-09-20 | 2007-03-28 | 中国科学院大连化学物理研究所 | Method for preparing bird-nest type monodisperse magnesium oxide |
| CN101376517A (en) * | 2008-10-10 | 2009-03-04 | 北京工业大学 | Method for preparing ordered mesoporous aluminum oxide in batch |
| CN101830489A (en) * | 2010-02-02 | 2010-09-15 | 华东理工大学 | Preparation method of porous rose-shaped basic magnesium carbonate |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1431169A (en) * | 2003-02-18 | 2003-07-23 | 山东大学 | Method for preparing porous nano solid by using hot pressing technique through controllable vaporized solvent |
| CN1935655A (en) * | 2005-09-20 | 2007-03-28 | 中国科学院大连化学物理研究所 | Method for preparing bird-nest type monodisperse magnesium oxide |
| CN101376517A (en) * | 2008-10-10 | 2009-03-04 | 北京工业大学 | Method for preparing ordered mesoporous aluminum oxide in batch |
| CN101830489A (en) * | 2010-02-02 | 2010-09-15 | 华东理工大学 | Preparation method of porous rose-shaped basic magnesium carbonate |
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