CN102936027A - Method for detonation synthesis of particle size controllable nano-cerium oxide - Google Patents
Method for detonation synthesis of particle size controllable nano-cerium oxide Download PDFInfo
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Abstract
Belonging to the field of physical or chemical methods, the invention provides a formula and a method for detonation synthesis of particle size controllable nano-cerium oxide. The method provided in the invention is characterized in that: a soluble cerium salt water solution, an organic hydrocarbon compound and an emulsifier solution are mixed and sensitized to prepare a paste able to detonate; the dispersion uniformity of the soluble cerium salt in the paste can be controlled by adjustment of the formula and technological parameters, thus further controlling the particle size of a nano-cerium oxide product after explosion. The nano-cerium oxide prepared by the method has the advantages of controllable particle size and high homogeneity. The nano-cerium oxide obtained in the invention has high yield, and over 20g of nano-cerium oxide can be prepared from every hectogram of agents. The method provided in the invention has a production process of less environmental pollution, a simple process and a low cost, and is easy for industrialized production.
Description
Technical field
The present invention relates to a kind of method of detonation synthesis nano material, more particularly, the present invention relates to prescription and the preparation method of the controlled detonation synthesis of nano cerium oxide of a kind of particle diameter.The nano-cerium oxide that generates can be used for the fields such as polishing, catalysis, gas sensor, fuel cell.
Background technology
Nano material causes physicist, material scholar and chemist's great interest in the tempting feature of the aspects such as structure, photoelectricity and chemical property.After the initial stage eighties, this concept of nano material formed, countries in the world gave very big concern to this material.The physics and chemistry character of the uniqueness that it has brings new opportunity for the research of the subjects such as physics, chemistry, material, biology, medicine.
The method of synthetic nano-cerium oxide mainly contains the methods such as vapor phase process, solid phase method, liquid phase method.
Vapor phase process refers to that the method that chemical reaction generates the nano level new compound occurs for two or more simple substance or compound in gas phase.Comprise inert-gas condensation method (Inert Gas Condensation), chemical Vapor deposition process (Chemical Vapor Deposition), gaseous combustion synthesis method (Gas Phase Combustion) etc.Generally speaking, the purity of vapor phase process gained powder is higher, reunion is less, sintering character is also better, and its shortcoming is that apparatus expensive, output are lower, difficult universal.
Solid phase method refers to form presoma by solid chemical compound or by solid state reaction, obtains the method for nano-powder through pyrolytic decomposition.It is generally acknowledged solid state reaction experience four-stage: reactant diffusion-chemical reaction-product nucleation-crystal growth.When nucleation speed during greater than the speed of growth, be conducive to generate small-particle: when the speed of growth during greater than nucleation rate, be conducive to generate macrobead.The solid phase method equipment used is simple, easy to operate, but introduces easily impurity in the gained powder, causes purity inadequate, and size-grade distribution is also larger, is applicable to require lower occasion.
Liquid phase method mainly is by controlling the condition of liquid-phase chemical reaction, such as the method for the formation presomas such as reactant concn, temperature of reaction and time, stirring velocity, hydrolysis rate, co-precipitation in liquid-phase system.Liquid phase method mainly comprises the precipitator method, sol-gel method, hydrothermal method, microemulsion method, electrochemical process etc.Liquid phase method is compared with vapor phase process, liquid phase method have equipment simple, need not the harsh physical condition such as high vacuum, the easy advantage such as amplification, the powder for preparing than solid phase method again simultaneously is pure, reunion is lacked, and is easy to realize suitability for industrialized production, is to prepare at present the most frequently used method of nanoparticle.But the method need to be used the equipment such as autoclave, and output investment ratio is larger, and need to use a large amount of acid or alkali in production process, unavoidably to environment.
In sum, all there is certain shortcoming in the methods such as vapor phase process, solid phase method, liquid phase method, be unfavorable for nano-cerium oxide industrial production and apply.At present, the key of restriction nano-cerium oxide product development is to there is no ripe low-cost preparation method and technology.Therefore the method for studying a kind of new synthesis of nano cerium oxide becomes very necessary.
The nano material synthetic method that detonation synthesis of nano cerium oxide method is that a kind of operation is simple, synthesising reacting speed is fast, environmental pollution is little, synthesis cycle is short, easily amplify output, particle size were is little, purity is high.But studies show that because the wayward ununiformity that causes the detonation reaction of the mixing uniformity of explosive substance, the size distribution of the nano-cerium oxide powder of producing with Detonation Process is wider.
Chinese patent CN201010117582.3 has proposed a kind ofly to prepare the method for ball shaped nano cerium oxide with sol method, but the method will be used the equipment such as autoclave, and cost is higher, and the size distribution of spherical cerium oxide is wider, reaches 30-160nm.Chinese patent CN200410020553.X has proposed a kind of with single chmical compound explosive and oxide precursor or with combustiblematerials and oxide precursor physical mixed, forms the explosibility mixture, prepares the method for various oxide compounds by igniting this mixture.But the method that does not relate to control nano-cerium oxide particle diameter in this patent.
Difference of the present invention is solubility cerium salt is uniformly distributed in the explosibility paste with the drop state, and the size that can regulate solubility cerium salt drop in the paste by regulating prescription or processing parameter, thereby the content of cerium salt in the control drop, and then the particle diameter of the rear nano-cerium oxide product of control blast, finally obtain even, the controlled nano-cerium oxide of particle diameter.
Summary of the invention
The prescription and the preparation method that the purpose of this invention is to provide the controlled detonation synthesis of nano cerium oxide that is easy to large-scale production of a kind of particle diameter are to solve problems of the prior art.Greater than 20%, its size distribution is even with the yield of the nano-cerium oxide of the present invention preparation, and particle diameter is adjustable between 10-100nm.Because its stable chemical nature, specific surface area is large, and outward appearance is spherical in shape, can be widely used in the fields such as polishing, catalysis, gas sensor, fuel cell.
Technical scheme provided by the invention is that the method for the detonation synthesis of nano cerium oxide that a kind of particle diameter is controlled may further comprise the steps:
(a) solubility cerium salt mixed with water form the aqueous solution, and be heated to 110-130 ℃ stand-by;
(b) organic hydrocarbon compound and emulsifying agent are mixed into uniform solution, and be heated to 110-130 ℃ stand-by;
(c) linear velocity that requires stirring rake end in the control emulsion process according to the particle diameter of nano-cerium oxide is at (5-20) m/s, with step (a) and the solution of acquisition (b) under 110-130 ℃, be mixed to get mixture;
Add sensitizing agent when the temperature of the mixture that (d) obtains in (c) is 40-60 ℃, and stir, the paste that formation can detonation;
The mass percent of each composition is chosen by following in the paste prescription:
Solubility cerium salt 70.4%-91.8%;
Organic hydrocarbon compound 3%-8%;
Emulsifying agent 1%-3%;
Sensitizing agent 0.2%-20%;
Water 4%-10%;
(e) paste in the ignition (d) in blasting pot, acquisition contains the explosion product of nano-cerium oxide; The explosion product that obtains is purified, obtain the finished product nano-cerium oxide.
Solubility cerium salt of the present invention comprises: cerous nitrate, cerous sulfate, Cerium II Chloride etc.
Described organic hydrocarbon compound is one or more the mixture in compound wax, ceresine, paraffin or the machine oil.
Described emulsifying agent is one or more the mixture in sorbitan oleate, polyisobutene succinimide, polyoxyethylene stearic acid ester, the sylvic acid polyoxyethylene ester.
Described sensitizing agent is one or more the mixture in nitrite, supercarbonate, organic coupling compound, resin microsphere, the single chmical compound explosive.
Paste of the present invention is that the aqueous solution with solubility cerium salt is as disperse phase, with the paste of organic hydrocarbon compound solution as the water-in-oil-type of external phase.
The present invention can regulate the content of solubility cerium salt in each drop by regulating the drop size of disperse phase in the paste, and then the particle diameter of control nano-cerium oxide product; The dispersed phase drop size is less, and the particle diameter of nano-cerium oxide product is just less;
Wherein, the intermediate value grain corresponding relation of dispersed phase drop mean diameter and nano-cerium oxide product is as follows:
Dispersed phase drop mean diameter cerium oxide particle median particle diameter
0.5-6μm 10-30nm
6-9μm 30-50nm
10-13μm 50-70nm
14-17μm 70-90nm 。
The emulsifying agent that the present invention can be by selecting different emulsifying effectivenesses or the consumption that increases emulsifying agent reduce the drop size of disperse phase, and droplet dia is changed at 0.1-20 μ m.Also can reduce by rotating speed of agitator in the raising emulsion process drop size of disperse phase, droplet dia is changed at 0.1-20 μ m.
Characteristics of the present invention are: the aqueous solution, organic hydrocarbon compound and emulsifier solution, the sensitizing agent of solubility cerium salt are mixed formation water-in-oil-type paste, wherein the solubility cerium salt solution is disperse phase, and organic hydrocarbon compound and emulsifier solution are external phase.The dispersed phase drop size is less in the paste, and the particle diameter of cerium oxide product is less.Can reduce the dispersed phase drop size by methods such as rotating speed of agitator in emulsifying agent, increase emulsifier or the raising emulsion process of selecting different emulsifying effectivenesses.Therefore in preparation can detonation paste process, kind that can be by changing emulsifying agent and consumption or the size of regulating dispersed phase drop by the adjusting process parameter, the dispersed phase drop diameter is changed at 0.1-20 μ m, with the content of solubility cerium salt in the control dispersed phase drop, and then the particle diameter of the nano-cerium oxide that produces after the control blast; The nano-cerium oxide product purity of the present invention's preparation is high, particle diameter is even, controlled; The nano-cerium oxide yield of the present invention's preparation is up to 20%, and namely 100 gram pastes can obtain more than nano-cerium oxide 20 grams; Method of the present invention has that operation is simple, environmental pollution is little, suitability for industrialized production with short production cycle, easy.
Description of drawings
Fig. 1 is the present invention's sample wiring layout that explodes.
Embodiment
Further by the following Examples, the present invention will be described.
Embodiment 1
According to the present invention fill a prescription preparation 100g paste sample, wherein ceresine 8g, sorbitan oleate 3g, Sodium Nitrite 0.6g, cerous nitrate 80.4g, water 8g.
Cerous nitrate is mixed with water, heating for dissolving, keeping the temperature of solution is 120 ℃; With ceresine and sorbitan oleate fusing, mix, keeping solution temperature is 120 ℃; Above two kinds of solution are mixed the paste that forms water-in-oil-type; The linear velocity of mulser stirring rake end is 10m/s.The dispersed phase drop mean diameter is 11 μ m.
When the temperature for the treatment of paste is 45 ℃, in the paste of above-mentioned water-in-oil-type, adds Sodium Nitrite, and make it fully to mix with paste; With the preparation paste 2 cans in paper roll 3, charge density is 1.15g/cm
3According to accompanying drawing 1 No. 8 commercial electric detonators 1, paste powder stick and inertia heat-eliminating mediums 4 are assembled, then put into blasting pot 5 and ignite.Explosion product is taken out from blasting pot, namely get ball shaped nano cerium oxide finished product through washing with after purifying.
With D8 ADVANCE type X-ray diffractometer sample is detected.The diffracting spectrum characteristic peak of sample is at 28.55 °, 33.08 °, 47.48 °, 56.33 °, and sample is without assorted peak.The product that proof generates is the isometric system cerium oxide.Use the field emission microscopy observation sample, its appearance is spherical; With BT-9300H laser fineness gage specimen granularity, its size-grade distribution interval is in the 40nm-100nm scope, and median particle diameter is d
50=65nm.With the foreign matter content of plasma emission spectrum (ICP) specimen, foreign matter content is less than 0.1%.
Prove that by above test product is purer ball shaped nano cerium oxide, the purity of product is more than 99.9%.
Embodiment 2
According to the present invention fill a prescription preparation 100g paste sample, wherein ceresine 8g, sorbitan oleate 3g, Sodium Nitrite 0.6g, cerous nitrate 80.4g, water 8g.
Cerous nitrate is mixed with water, heating for dissolving, keeping the temperature of solution is 120 ℃; With ceresine and sorbitan oleate fusing, mix, keeping solution temperature is 120 ℃; Above two kinds of solution are mixed the paste that forms water-in-oil-type; The linear velocity of mulser stirring rake end is 15m/s.The dispersed phase drop mean diameter is 5.5 μ m.
When the temperature for the treatment of paste is 45 ℃, in the paste of above-mentioned water-in-oil-type, adds Sodium Nitrite, and make it fully to mix with paste; With the preparation the paste can in paper roll, charge density is 1.15g/cm
3According to accompanying drawing 1 No. 8 commercial electric detonators, paste powder stick and inertia heat-eliminating mediums are assembled, then put into blasting pot and ignite.Explosion product is taken out from blasting pot, namely get ball shaped nano cerium oxide finished product through washing with after purifying.
With D8 ADVANCE type X-ray diffractometer sample is detected.The diffracting spectrum characteristic peak of sample is at 28.55 °, 33.08 °, 47.48 °, 56.33 °, and sample is without assorted peak.The product that proof generates is the isometric system cerium oxide.Use the field emission microscopy observation sample, its appearance is spherical; With BT-9300H laser fineness gage specimen granularity, its size-grade distribution interval is in the 10nm-60nm scope, and median particle diameter is d
50=29nm.With the foreign matter content of plasma emission spectrum (ICP) specimen, foreign matter content is less than 0.1%.
Prove that by above test product is purer ball shaped nano cerium oxide, the purity of product is more than 99.9%.
Embodiment 3
According to the present invention fill a prescription preparation 100g paste sample, wherein ceresine 8g, polyisobutene succinimide 3g, Sodium Nitrite 0.6g, cerous nitrate 80.4g, water 8g.
Cerous nitrate is mixed with water, heating for dissolving, keeping the temperature of solution is 120 ℃; With ceresine and sorbitan oleate fusing, mix, keeping solution temperature is 120 ℃; Above two kinds of solution are mixed the paste that forms water-in-oil-type; The linear velocity of mulser stirring rake end is 10m/s.The dispersed phase drop mean diameter is 16 μ m.
When the temperature for the treatment of paste is 45 ℃, in the paste of above-mentioned water-in-oil-type, adds Sodium Nitrite, and make it fully to mix with paste; With the preparation the paste can in paper roll, charge density is 1.15g/cm
3According to accompanying drawing 1 No. 8 commercial electric detonators, paste powder stick and inertia heat-eliminating mediums are assembled, then put into blasting pot and ignite.Explosion product is taken out from blasting pot, namely get ball shaped nano cerium oxide finished product through washing with after purifying.
With D8 ADVANCE type X-ray diffractometer sample is detected.The diffracting spectrum characteristic peak of sample is at 28.55 °, 33.08 °, 47.48 °, 56.33 °, and sample is without assorted peak.The product that proof generates is the isometric system cerium oxide.Use the field emission microscopy observation sample, its appearance is spherical; With BT-9300H laser fineness gage specimen granularity, its size-grade distribution interval is in the 60nm-150nm scope, and median particle diameter is d
50=90nm.With the foreign matter content of plasma emission spectrum (ICP) specimen, foreign matter content is less than 0.1%.
Prove that by above test product is purer ball shaped nano cerium oxide, the purity of product is more than 99.9%.
Embodiment 4
According to the present invention fill a prescription preparation 100g paste sample, wherein paraffin 5g, polyisobutene succinimide 3g, hexogen 12g, Cerium II Chloride 72g, water 8g.
Cerium II Chloride is mixed with water, heating for dissolving, keeping the temperature of solution is 125 ℃; With paraffin and polyisobutene succinimide fusing, mix, keeping solution temperature is 125 ℃; Above two kinds of solution are mixed the paste that forms water-in-oil-type; The linear velocity of mulser stirring rake end is 15m/s.The dispersed phase drop mean diameter is 10 μ m.
When the temperature for the treatment of paste is down to 50 ℃, in the paste of above-mentioned water-in-oil-type, adds RDX, and make it fully to mix with paste; With the preparation the paste can in paper roll, charge density is controlled to be 1.15g/cm
3According to accompanying drawing 1 No. 8 commercial electric detonators, paste powder stick and inertia heat-eliminating mediums are assembled, then put into blasting pot and ignite.Explosion product is taken out from blasting pot, namely get ball shaped nano cerium oxide finished product through washing with after purifying.
With D8 ADVANCE type X-ray diffractometer sample is detected.The diffracting spectrum characteristic peak of sample is at 28.55 °, 33.08 °, 47.48 °, 56.33 °, and sample is without assorted peak.The product that proof generates is the isometric system cerium oxide.Use the field emission microscopy observation sample, its appearance is spherical; With BT-9300H laser fineness gage specimen granularity, its size-grade distribution interval is in the 40nm-85nm scope, and median particle diameter is d
50=60nm.With the foreign matter content of plasma emission spectrum (ICP) specimen, foreign matter content is less than 0.1%.
Prove that by above test product is purer ball shaped nano cerium oxide, the purity of product is more than 99.9%.
Embodiment 5
According to the present invention fill a prescription preparation 100g paste sample, wherein machine oil 3g, emulsifying agent (polyoxyethylene stearic acid ester+sylvic acid polyoxyethylene ester) 1g, sensitizing agent (supercarbonate+organic coupling compound) 0.2g, cerous sulfate 41.8g, cerous nitrate 50g, water 4g.
Cerous sulfate, cerous nitrate are mixed with water, heating for dissolving, keeping the temperature of solution is 130 ℃; With machine oil, polyoxyethylene stearic acid ester, the fusing of sylvic acid polyoxyethylene ester, mix, keeping solution temperature is 130 ℃; Above two kinds of solution are mixed, and setting the terminal linear velocity of mulser stirring rake is 10m/s, forms the paste of water-in-oil-type.The dispersed phase drop mean diameter is 12 μ m.
When the temperature for the treatment of paste is 50 ℃, in the paste of above-mentioned water-in-oil-type, adds sensitizing agent, and make it fully to mix with paste; With the preparation the paste can in paper roll, charge density is controlled to be 1.12g/cm
3According to accompanying drawing 1 No. 8 commercial electric detonators, paste powder stick and inertia heat-eliminating mediums are assembled, then put into blasting pot and ignite.Explosion product is taken out from blasting pot, namely get ball shaped nano cerium oxide finished product through washing with after purifying.
With D8 ADVANCE type X-ray diffractometer sample is detected.The diffracting spectrum characteristic peak of sample is at 28.55 °, 33.08 °, 47.48 °, 56.33 °, and sample is without assorted peak.The product that proof generates is the isometric system cerium oxide.Use the field emission microscopy observation sample, its appearance is spherical; With BT-9300H laser fineness gage specimen granularity, its size-grade distribution interval is in the 40nm-100nm scope, and median particle diameter is d
50=60nm.With the foreign matter content of plasma emission spectrum (ICP) specimen, foreign matter content is less than 0.1%.
Prove that by above test product is purer ball shaped nano cerium oxide, the purity of product is more than 99.9%.
Claims (9)
1. the method for the controlled detonation synthesis of nano cerium oxide of a particle diameter may further comprise the steps:
(a) solubility cerium salt mixed with water form the aqueous solution, and be heated to 110-130 ℃ stand-by;
(b) organic hydrocarbon compound and emulsifying agent are mixed into uniform solution, and be heated to 110-130 ℃ stand-by;
(c) linear velocity that requires stirring rake end in the control emulsion process according to the particle diameter of nano-cerium oxide is at (5-20) m/s, with step (a) and the solution of acquisition (b) under 110-130 ℃, be mixed to get mixture;
Add sensitizing agent when the temperature of the mixture that (d) obtains in (c) is 40-60 ℃, and stir, the paste that formation can detonation;
The mass percent of each composition is chosen by following in the paste prescription:
Solubility cerium salt 70.4%-91.8%;
Organic hydrocarbon compound 3%-8%;
Emulsifying agent 1%-3%;
Sensitizing agent 0.2%-20%;
Water 4%-10%;
(e) paste in the ignition (d) in blasting pot, acquisition contains the explosion product of nano-cerium oxide; The explosion product that obtains is purified, obtain the finished product nano-cerium oxide.
2. method according to claim 1, it is characterized in that: solubility cerium salt comprises: cerous nitrate, cerous sulfate, Cerium II Chloride etc.
3. method according to claim 1 is characterized in that: the organic hydrocarbon compound is one or more the mixture in compound wax, ceresine, paraffin or the machine oil.
4. method according to claim 1 is characterized in that: emulsifying agent is one or more the mixture in sorbitan oleate, polyisobutene succinimide, polyoxyethylene stearic acid ester, the sylvic acid polyoxyethylene ester.
5. method according to claim 1 is characterized in that: paste is that the aqueous solution with solubility cerium salt is as disperse phase, with the paste of organic hydrocarbon compound solution as the water-in-oil-type of external phase.
6. method according to claim 1 is characterized in that: described sensitizing agent is one or more the mixture in nitrite, supercarbonate, organic coupling compound, resin microsphere, the single chmical compound explosive.
7. according to claim 1 to 6 each described methods, it is characterized in that: can regulate the content of solubility cerium salt in each drop by regulating the drop size of disperse phase in the paste, and then the particle diameter of control nano-cerium oxide product; The dispersed phase drop size is less, and the particle diameter of nano-cerium oxide product is just less;
Wherein, the intermediate value grain corresponding relation of dispersed phase drop mean diameter and nano-cerium oxide product is as follows:
Dispersed phase drop mean diameter cerium oxide particle median particle diameter
0.5-6μm 10-30nm
6-9μm 30-50nm
10-13μm 50-70nm
14-17μm 70-90nm 。
8. method according to claim 7 is characterized in that: emulsifying agent that can be by selecting different emulsifying effectivenesses or the consumption that increases emulsifying agent reduce the drop size of disperse phase, and droplet dia is changed at 0.1-20 μ m.
9. method according to claim 7 is characterized in that: can reduce by rotating speed of agitator in the raising emulsion process drop size of disperse phase, droplet dia is changed at 0.1-20 μ m.
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| CN105710382A (en) * | 2016-03-14 | 2016-06-29 | 西安建筑科技大学 | Preparation method of nanometer iron powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105710382A (en) * | 2016-03-14 | 2016-06-29 | 西安建筑科技大学 | Preparation method of nanometer iron powder |
| CN105710382B (en) * | 2016-03-14 | 2018-04-27 | 西安建筑科技大学 | A kind of preparation method of nanometer iron powder |
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