CN102343267A - Method for preparing carbon-hybridized nickel lithium ferrite nano-catalyst - Google Patents
Method for preparing carbon-hybridized nickel lithium ferrite nano-catalyst Download PDFInfo
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- CN102343267A CN102343267A CN2011102122156A CN201110212215A CN102343267A CN 102343267 A CN102343267 A CN 102343267A CN 2011102122156 A CN2011102122156 A CN 2011102122156A CN 201110212215 A CN201110212215 A CN 201110212215A CN 102343267 A CN102343267 A CN 102343267A
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Abstract
The invention relates to a method for preparing a carbon-hybridized nickel lithium ferrite nano-catalyst. The method is characterized by comprising the following steps of: (1) dissolving lithium nitrate, nickel nitrate, iron nitrate and citric acid into water in the molar ratio of 1:0.5:2:3.5, and stirring to form a settled solution; (2) making the settled solution react at the temperature of 160-200 DEG C for 6-8 hours to obtain a foamed intermediate; (3) calcining the intermediate at the temperature of 550-600 DEG C for 3 hours to obtain nickel lithium ferrite; and (4) putting the nickel lithium ferrite and glucose into a high-pressure reaction kettle in the mass ratio of 1-2:1, reacting at the temperature of 160-200 DEG C for 12 hours, washing and drying to obtain the carbon-hybridized nickel lithium ferrite nano-catalyst. The method has the advantages of easiness for operating, cheap and readily-available raw materials, low cost, high yield, no need of purification treatment, no need of large-size special equipment in the reaction process and easiness for realizing large-scale industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of carbon hydridization nickel ferrite based magnetic loaded lithium catalyst.
Background technology
Solid propellant is the power source material of solid propellant rocket, in the development of guided missile and space technology, plays a part very important.Solid propellant mainly is made up of adhesive, oxidant, high-energy fuel and function additive.In the combustion process of solid propellant, condensed phase is heated and is converted into gas phase, and on the one hand through physical evaporation and distillation, main form is that each component of propellant becomes gaseous products at burning surface through the Rapid Thermal decomposition.It is generally acknowledged that the initial stage of SOLID PROPELLANT COMBUSTION process is the thermal decomposition of propellant component (for example AP, RDX, HMX, NC/NG etc.), its gaseous decomposition product generation combustion reaction then.Therefore, become the act of the certainty of improving propellant burning property through adding decomposes temperature that catalyst reduces the main high energy component of propellant.
Nano transition metal oxides can make combustion speed, energy, pressure index of solid catalyst etc. obviously changed.And the polynary composite catalyst development of nanocatalyst forward, because it is compound on nanoscale to form the various unit component of compound, can produce strong " cooperative effect ", have the characteristic of nano particle simultaneously again.Wherein " cooperative effect " mainly is owing to multiple composition in the nanometer multicomponent composite oxide catalyst mixes mutually; Be prone to cause distortion of lattice; Cause having more defectives in the nanocrystal, significantly increase in the activated centre, so have the catalytic activity higher than single catalyst of transition metal oxide.And the nanostructured ferrite is as a kind of typical polynary composite catalyst; Shown remarkable advantages aspect the pyrolysis temperature of AP etc. reducing; Be expected to realizing satisfactory results aspect adjusting NEPE propellant burning rate and the pressure index the bigger effect of performance in rocket launching and Defence business.Yet its synthesis method and await with research aspect the pressure index that we further go exploration regulating NEPE combustion speed.The preparation method of synthetic polynary composite catalyst mainly comprises room temperature solid reaction process, liquid phase deposition, catalystic pyrolysis, spray pyrolysis, high-energy ball milling method etc., and wherein first three methods is the preparation method with industrial potential.
The big good nanometer CuFe that waits human room temperature solid state reaction method to prepare 3 kinds of different Cu, iron molal weight ratio of flood
2O
4Powder, the about 5nm of particle diameter, and tested nanometer CuFe with DSC
2O
4Powder is to the catalytic action of RDX thermal decomposition.Research shows, nanometer CuFe
2O
4Thermal decomposition has tangible catalytic effect to RDX.At 3 kinds of nanometer CuFe
2O
4In, the catalytic effect of n (Cu): n (Fe)=1: 1 o'clock is best, and it makes decomposition peak's temperature of RDX move forward 17.8 ℃, and thermal discharge increases 250J/g, and activation energy reduces 2119kJ/mol.And along with nanometer CuFe
2O
4The increase of consumption, its catalytic effect to the RDX thermal decomposition enlarges markedly.In addition, people such as Tian Liu also synthesizes CuFe through the method for spontaneous combustion
2O
4, the result shows CuFe in AP
2O
4Content reach at 5% o'clock, its catalytic effect is best, can make the heat decomposition temperature of AP reduce by 105 ℃.People such as Gurdip Singh adopt the method for co-precipitation to successfully synthesize CoFe
2O
4, CuFe
2O
4And NiFe
2O
4, and tested its influence to the AP pyrolysis temperature through TG and DTA.The result shows that three kinds of ferrites all can reduce the original high pyrolysis temperature of AP effectively, and the catalytic activity that works out the three is in proper order: CoFe
2O
4>CuFe
2O
4>CuFe
2O
4Also further synthesized more complicated polynary composite catalyst NiZnFe simultaneously
2O
4(NZF), CuCoFe
2O
4(CuCoF), NiCuFe
2O
4(NCuF), CuZnFe
2O
4(CuZF), CoNiFe
2O
4(CoNF) and CoZnFe
2O
4(CoZF) etc., and its catalysis active order of reducing the AP pyrolysis temperature be: CoZF>CoNF>CuZF>CuCoF>NCuF>NZF.
To nanostructured acid ferric complex salt catalyst LiNi
0.5Fe
2O
4, adopting synthesis method to select difficulty bigger.Though high-temperature solid phase reaction method is than the metering ratio that is easier to guarantee different elements in the products obtained therefrom; But high-temperature calcination causes growing up of crystal grain and caving in of micro-structural easily; Finally can only obtain the very little block product of specific area, also will consume lot of energy simultaneously, improper economically.Liquid phase deposition is the multicomponent composite oxide preparation method of easy for industrialized, but uses liquid phase deposition to prepare LiNi
0.5Fe
2O
4The problem that faces is how to allow three kinds of transition metals from solution, be precipitated out than simultaneously according to metering.Relative liquid phase deposition, the polymer pyrolysismethod obtains the LiNi of predetermined dose ratio more easily
0.5Fe
2O
4Nano-structured calalyst.If nano combined ferrite and nonmetal (like carbon) are carried out hydridization and coating; Just might be when improving nano combined ferrite adjusting propellant burning property; Reducing the acid ferric complex salt nano particle contacts with the direct of components such as oxidant and ammonium nitrate; Have excellent compatibility and security with other components of propellant; Participate in having better adaptation regulating power in burning and the catalytic process at it; Realize effectively regulating the combustion speed of four constituent element fourth hydroxyl propellants; And improve combustion stability under the high pressure, reduce the susceptibility of low burning rate to pressure and variations in temperature.Yet, how the nanostructured ferrate catalyst is carried out non-metal carbon hydridization and coating, further improve the nanostructured ferrate catalyst in the effect of regulating combustion speed and pressure index, at home and abroad relevant report almost is blank.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst, this method is simple to operate, and raw materials used cheap and easy to get, cost is low, and productive rate is high.
For realizing the object of the invention, technical scheme of the present invention is: a kind of preparation method of carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst is characterized in that it may further comprise the steps:
1) at room temperature, with lithium nitrate, nickel nitrate, ferric nitrate and citric acid according to 1: 0.5: 2: 3.5 mol ratio is soluble in water, stirs, and forms settled solution; Wherein, the concentration of lithium nitrate is 2~4mol/L in the settled solution;
2) step 1) gained settled solution is placed under 160~200 ℃ the temperature and reacted 6~8 hours, obtain foamed intermediate;
3) with step 2) the gained intermediate is 550~600 ℃ temperature lower calcination 3 hours, obtains the nickel ferrite based magnetic loaded lithium;
4) with the nickel ferrite based magnetic loaded lithium of step 3) gained and glucose by 1~2: 1 mass ratio places autoclave; 160~200 ℃ were reacted 12 hours; Water, ethanol wash respectively 2~5 times after taking out, and 50~80 ℃ of oven dry (drying by the fire 8 hours) obtain carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst.
Room temperature refers to 10~30 ℃ among the present invention.
The invention has the beneficial effects as follows:
1) this method is simple to operate, and raw materials used cheap and easy to get, cost is low, and does not introduce any foreign ion;
2) productive rate of products obtained therefrom of the present invention is high, and products obtained therefrom purity is high, and need not to carry out purification processes; The carbon coated process is simple to operation, and is obvious to the thermal decomposition catalytic effect of AP;
3) course of reaction need not large-scale professional equipment, very easily realizes large-scale industrial production.
Description of drawings
Fig. 1 is the XRD diffracting spectrum of corresponding embodiment 1 gained nickel ferrite based magnetic loaded lithium;
Fig. 2 is the sem photograph of embodiment 1 gained nickel ferrite based magnetic loaded lithium;
Fig. 3 is the sem photograph of embodiment 1 gained carbon hydridization nickel ferrite based magnetic loaded lithium;
Fig. 4 is embodiment 1 gained nickel ferrite based magnetic loaded lithium and the carbon hydridization nickel ferrite based magnetic loaded lithium thermal decomposition catalytic effect figure to AP.Wherein, AP (ammonium perchlorate) is 98: 2 with the mass ratio of product (carbon hydridization nickel ferrite based magnetic loaded lithium).
The specific embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with instance, but the present invention not only is confined to the following examples.
Embodiment 1:
A kind of preparation method of carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst, it may further comprise the steps:
1) at room temperature (10~30 ℃); In the beaker of 100mL; Take by weighing lithium nitrate, nickel nitrate, ferric nitrate and citric acid and be dissolved in the 50mL water, stir, the concentration that is made into lithium nitrate, nickel nitrate, ferric nitrate and citric acid is respectively the settled solution of 2mol/L, 1mol/L, 4mol/L, 7mol/L;
2) beaker (in settled solution is arranged) is placed 200 ℃ of air dry ovens 8 hours, obtain foamed intermediate;
3) intermediate was calcined 3 hours in 550 ℃ Muffle furnace, promptly obtained nickel ferrite based magnetic loaded lithium (graininess);
The XRD diffracting spectrum of resulting nickel ferrite based magnetic loaded lithium is seen Fig. 1, illustrates that the gained sample is pure nickel ferrite based magnetic loaded lithium.Gained nickel ferrite based magnetic loaded lithium sem photograph is seen Fig. 2.
4) gained nickel ferrite based magnetic loaded lithium sample and glucose are mixed by 1: 1 mass ratio after; Add in the polytetrafluoroethylene (PTFE) agitated reactor; 160 ℃ of hydro-thermal reactions 12 hours; Water, ethanol wash respectively 2 times after taking out; 50 ℃ of oven dry (drying by the fire 8 hours); Obtain carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst (product, i.e. carbon hydridization nickel ferrite based magnetic loaded lithium).Yield of product is calculated as 98%.
Carbon hydridization nickel ferrite based magnetic loaded lithium sem photograph is seen Fig. 3, illustrates that carbon hydridization process changes sample topography to some extent.Its XRD is consistent with Fig. 1, proves that carbon hydridization products therefrom crystalline phase does not change.
Gained nickel ferrite based magnetic loaded lithium and carbon hydridization nickel ferrite based magnetic loaded are seen Fig. 4 to the thermal decomposition catalytic effect figure of AP, illustrate that carbon hydridization process can be reduced to 98.7 from 109.5 degree with the difference at pyrolytic peak and low-temperature decomposition peak, shows better combustion velocity modulation joint performance.
Embodiment 2
A kind of preparation method of carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst, it may further comprise the steps:
1) under room temperature (10~30 ℃); In the beaker of 100mL; Take by weighing lithium nitrate, nickel nitrate, ferric nitrate and citric acid and be dissolved in the 50mL water, stir, the concentration that is mixed with lithium nitrate, nickel nitrate, ferric nitrate and citric acid is respectively the settled solution of 2mol/L, 1mol/L, 4mol/L, 7mol/L;
2) beaker (in settled solution is arranged) is placed 160 ℃ of air dry ovens 8 hours, obtain foamed intermediate;
3) intermediate was calcined 3 hours in 550 ℃ Muffle furnace, promptly got the nickel ferrite based magnetic loaded lithium.
4) gained nickel ferrite based magnetic loaded lithium sample and glucose are mixed by 2: 1 mass ratio after; Add in the polytetrafluoroethylene (PTFE) agitated reactor (being autoclave); 160 ℃ of hydro-thermal reactions 12 hours; Water, ethanol wash respectively 3 times after taking out; 50 ℃ of oven dry (drying by the fire 8 hours) obtain carbon hydridization nickel ferrite based magnetic loaded lithium (carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst).Yield of product is calculated as 97%.
Embodiment 3
A kind of preparation method of carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst, it may further comprise the steps:
1) at room temperature; In the beaker of 100mL; Take by weighing lithium nitrate, nickel nitrate, ferric nitrate and citric acid and be dissolved in the 50mL water, stirring and dissolving, the concentration that is mixed with lithium nitrate, nickel nitrate, ferric nitrate and citric acid is respectively the settled solution of 4mol/L, 2mol/L, 8mol/L, 14mol/L;
2) beaker was placed 200 ℃ of air dry ovens 8 hours, obtain foamed intermediate;
3) intermediate was calcined 3 hours in 550 ℃ Muffle furnace, promptly got nickel ferrite based magnetic loaded lithium sample.
4) gained nickel ferrite based magnetic loaded lithium sample and glucose are mixed by 1: 1 mass ratio after; Add in the polytetrafluoroethylene (PTFE) agitated reactor, 200 ℃ of hydro-thermal reactions 12 hours are taken out the back water, ethanol washs respectively 5 times; 50 ℃ of oven dry (drying by the fire 8 hours) get the nickel ferrite based magnetic loaded lithium (product) that carbon coats.Yield of product is calculated as 98%.
Embodiment 4
A kind of preparation method of carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst, it may further comprise the steps:
1) at room temperature; In the beaker of 100mL; Take by weighing lithium nitrate, nickel nitrate, ferric nitrate and citric acid and be dissolved in the 50mL water, stirring and dissolving, the concentration that is mixed with lithium nitrate, nickel nitrate, ferric nitrate and citric acid is respectively the settled solution of 4mol/L, 2mol/L, 8mol/L, 14mol/L;
2) beaker was placed 160 ℃ of air dry ovens 8 hours, obtain foamed intermediate;
3) intermediate was calcined 3 hours in 550 ℃ Muffle furnace, promptly got nickel ferrite based magnetic loaded lithium sample.
4) gained nickel ferrite based magnetic loaded lithium sample and glucose are mixed by 2: 1 mass ratio after; Add in the polytetrafluoroethylene (PTFE) agitated reactor; 200 ℃ of hydro-thermal reactions 12 hours; Water, ethanol wash respectively 4 times after taking out; 50 ℃ of oven dry (drying by the fire 8 hours); Get the nickel ferrite based magnetic loaded lithium (product, i.e. carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst) that carbon coats.Yield of product is calculated as 98%.
Embodiment 5
A kind of preparation method of carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst, it may further comprise the steps:
1) at room temperature; In the beaker of 100mL; Take by weighing lithium nitrate, nickel nitrate, ferric nitrate and citric acid and be dissolved in the 50mL water, stirring and dissolving, the concentration that is mixed with lithium nitrate, nickel nitrate, ferric nitrate and citric acid is respectively the settled solution of 4mol/L, 2mol/L, 8mol/L, 14mol/L;
2) beaker was placed 160 ℃ of air dry ovens 6 hours, obtain foamed intermediate;
3) intermediate was calcined 3 hours in 600 ℃ Muffle furnace, promptly got nickel ferrite based magnetic loaded lithium sample.
4) gained nickel ferrite based magnetic loaded lithium sample and glucose are mixed by 1: 1 mass ratio after; Add in the polytetrafluoroethylene (PTFE) agitated reactor; 200 ℃ of hydro-thermal reactions 12 hours; Water, ethanol wash respectively 3 times after taking out; 80 ℃ of oven dry (drying by the fire 8 hours); Get the nickel ferrite based magnetic loaded lithium (product, i.e. carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst) that carbon coats.Yield of product is calculated as 98%.
Claims (1)
1. the preparation method of a carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst is characterized in that it may further comprise the steps:
1) at room temperature, with lithium nitrate, nickel nitrate, ferric nitrate and citric acid according to 1: 0.5: 2: 3.5 mol ratio is soluble in water, stirs, and forms settled solution; Wherein, the concentration of lithium nitrate is 2~4mol/ in the settled solution;
2) step 1) gained settled solution is placed under 160~200 ℃ the temperature and reacted 6~8 hours, obtain foamed intermediate;
3) with step 2) the gained intermediate is 550~600 ℃ temperature lower calcination 3 hours, obtains the nickel ferrite based magnetic loaded lithium;
4) with the nickel ferrite based magnetic loaded lithium of step 3) gained and glucose by 1~2: 1 mass ratio places autoclave; 160~200 ℃ were reacted 12 hours; Water, ethanol wash respectively 2~5 times after taking out, and 50~80 ℃ of oven dry obtain carbon hydridization nickel ferrite based magnetic loaded lithium nanocatalyst.
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CN101376101A (en) * | 2007-08-30 | 2009-03-04 | 中国科学院福建物质结构研究所 | Bitter earth nano-catalyst material capable of being used for high-energy solid propellant and synthetic method thereof |
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Non-Patent Citations (4)
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