CN102249343B - Method for synthesizing nanoscale lanthanum ferrate with large specific surface area by utilizing silane coupling agent - Google Patents

Method for synthesizing nanoscale lanthanum ferrate with large specific surface area by utilizing silane coupling agent Download PDF

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CN102249343B
CN102249343B CN 201110125986 CN201110125986A CN102249343B CN 102249343 B CN102249343 B CN 102249343B CN 201110125986 CN201110125986 CN 201110125986 CN 201110125986 A CN201110125986 A CN 201110125986A CN 102249343 B CN102249343 B CN 102249343B
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coupling agent
silane coupling
specific surface
surface area
citric acid
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CN102249343A (en
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井立强
姚常浩
屈宜春
付宏刚
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Heilongjiang University
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Abstract

The invention relates to a method for synthesizing nanoscale lanthanum ferrate with a large specific surface area by utilizing a silane coupling agent, and relates to a synthesis method of nanoscale lanthanum ferrate. The method aims to solve the problem that nanoscale lanthanum ferrate with the large specific surface area can not be produced in the prior art. The method provided by the invention comprises the specific operation steps: (1) preparing a citric acid sol; (2) carrying out hydrothermal synthesis; and (3) preparing nanoscale lanthanum ferrate. The method provided by the invention has the advantages that: (1) the synthesis of nanoscale lanthanum ferrate with the large specific surface area is achieved; (2) the synthesis process has the advantages of simple technique, mild reaction conditions, convenience in operation and low cost; and (3) by the method, new idea and method are provided for the design and synthesis of other perovskite-type composite oxide nanomaterials. The method provided by the invention is mainly used for synthesizing nanoscale lanthanum ferrate with the large specific surface area.

Description

Utilize the method for the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent
Technical field
The present invention relates to a kind of synthetic method of nanometer ferrous acid lanthanum.
Background technology
Nanometer ferrous acid lanthanum is a kind of type material with unique physical and chemical property, and is multiplex in CO, NH 3, CH 4Deng catalytic oxidation, be the ideal product of Study of Catalyst surface and catalytic performance.And specific surface area is one of principal element that affects ferrous acid lanthanum performance.Different synthetic methods can affect surface properties and granular size and the distribution of material, thereby affects size and the performance thereof of specific surface area.The synthetic method of the perovskite composite oxide that prior art adopts (for example: citric acid complex method), when high-temperature roasting, exist serious sintering phenomenon, reduce the specific surface area of sample, and then affect the performance of material, so the nanometer ferrous acid lanthanum of can not the production performance superior large specific surface of prior art.
Summary of the invention
The present invention seeks to solve the nanometer ferrous acid lanthanum problem that prior art can not be produced large specific surface, and a kind of method of utilizing the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent that provides.
Utilize the method for the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent to finish according to the following steps:
One, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.3~0.6mol/L, then add lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirred 0.5~2 hour, namely obtain even colloidal sol russet; The lanthanum nitrate hexahydrate of described adding is 1 with the ratio of the amount of substance of citric acid: (1~3), and the Fe(NO3)39H2O of adding is 1 with the ratio of the amount of substance of citric acid: (1~3); Two, Hydrothermal Synthesis: silane coupling agent is joined in the citric acid colloidal sol of step 1 preparation, at room temperature stirred 0.5~2 hour, silane coupling agent is dispersed in the sol system, then place thermostatic drying chamber, under 150~180 ℃, incubation water heating 6~10 hours takes out the thermosol system and is cooled to room temperature, namely obtain precursor (grey color dress material), the mole number of described adding silane coupling agent is (2~11) with the ratio of the mole number of Fe(NO3)39H2O: 100; Three, preparation nanometer ferrous acid lanthanum: with precursor 70~90 ℃ lower dry 5~10 hours, be ground into powder, powder is placed the retort furnace roasting, under 500~900 ℃, roasting 1~3 hour, namely obtain bigger serface nanometer ferrous acid lanthanum.
Silane coupling agent is a kind of coupling agent that contains silicon, and the Chang Zuowei tackiness agent is applied to industrial production on a large scale, and its effect is to connect organism and inorganics.Because silane coupling agent self contains silicon, can form silicon oxide and stable existence in the process of high-temperature heat treatment, this just provides possibility for its regulation and control size of particles.In the present invention, utilize first silane coupling agent as inhibitor, obtain following beneficial effect:
One, the present invention has realized nanometer ferrous acid lanthanum synthetic of bigger serface; Two, building-up process technique of the present invention is simple, reaction conditions is gentle, easy to operate, cost is low, is easy to realize suitability for industrialized production; Three, the present invention regulates and control size of particles take silane coupling agent as inhibitor, improved the shortcoming that traditional synthetic method is easily reunited, thereby can improve the specific surface area of composite oxides ferrous acid lanthanum, this novel nano-material is conducive to material in the raising of many-sided performance, also will provide new thinking and method for designing synthetic other perovskite composite oxide nano material.
Description of drawings
Fig. 1 is the electron-microscope scanning figure of the ferrous acid lanthanum sample of embodiment 12 preparations; Fig. 2 is the electron-microscope scanning figure of the ferrous acid lanthanum sample of embodiment 13 preparations; Fig. 3 is the electron-microscope scanning figure of the ferrous acid lanthanum sample of embodiment 14 preparations; Fig. 4 is the electron-microscope scanning figure of the ferrous acid lanthanum sample of embodiment 15 preparations; Fig. 5 is the x-ray diffraction pattern of the ferrous acid lanthanum sample of embodiment 12 to 15 preparations; Fig. 6 is the x-ray diffraction pattern of the ferrous acid lanthanum sample of embodiment 16 to 19 preparations.
Embodiment
Embodiment one: the present invention utilizes silane coupling agent to synthesize large-specific surface area nano ferrous acid lanthanum, and concrete operation step is as follows:
One, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.3~0.6mol/L, then add lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirred 0.5~2 hour, namely obtain even colloidal sol russet; The lanthanum nitrate hexahydrate of described adding is 1 with the ratio of the amount of substance of citric acid: (1~3), and the Fe(NO3)39H2O of adding is 1 with the ratio of the amount of substance of citric acid: (1~3); Two, Hydrothermal Synthesis: silane coupling agent is joined in the citric acid colloidal sol of step 1 preparation, at room temperature stirred 0.5~2 hour, silane coupling agent is dispersed in the sol system, then place thermostatic drying chamber, under 150~180 ℃, incubation water heating 6~10 hours takes out the thermosol system and is cooled to room temperature, namely obtain precursor (grey color dress material), the mole number of described adding silane coupling agent is (2~11) with the ratio of the mole number of Fe(NO3)39H2O: 100; Three, preparation nanometer ferrous acid lanthanum: with precursor 70~90 ℃ lower dry 5~10 hours, be ground into powder, powder is placed the retort furnace roasting, under 500~900 ℃, roasting 1~3 hour, namely obtain bigger serface nanometer ferrous acid lanthanum.
Embodiment two: the difference of present embodiment and embodiment one is: preparation citric acid amount of substance concentration is 0.5mol/L in the step 1.Other steps are identical with embodiment one.
Embodiment three: the difference of present embodiment and embodiment two is: churning time is 1 hour in the step 1.Other steps are identical with embodiment two.
Embodiment four: one of present embodiment and embodiment one to three difference is: the lanthanum nitrate hexahydrate that adds described in the step 1 is 1: 2 with the ratio of the amount of substance of citric acid.Other steps are identical with embodiment one to three.
Embodiment five: the difference of present embodiment and embodiment four is: the Fe(NO3)39H2O that adds described in the step 1 is 1: 2 with the ratio of the amount of substance of citric acid.Other steps are identical with embodiment four.
Embodiment six: present embodiment and embodiment five differences are: churning time is 1 hour in the step 2.Other steps are identical with embodiment five.
Embodiment seven: the difference of present embodiment and embodiment six is: in the step 2 under 150~170 ℃, incubation water heating 7~9 hours.Other steps are identical with embodiment six.
Embodiment eight: the difference of present embodiment and embodiment seven is: in the step 2 under 160 ℃, incubation water heating 8 hours.Other steps are identical with embodiment seven.
Embodiment nine: one of present embodiment and embodiment one to eight difference is: in the step 3 that precursor is lower dry 8 hours at 80 ℃.Other steps are identical with embodiment one or eight.
Embodiment ten: the difference of present embodiment and embodiment nine is: maturing temperature is 600 ℃ in the step 3, and roasting time is 2 hours.Other steps are identical with embodiment nine.
Embodiment 11: the difference of present embodiment and embodiment nine is: roasting is that maturing temperature is 800 ℃ in the step 3, and roasting time is 2 hours.Other steps are identical with embodiment nine.
Embodiment 12: do not add the simultaneous test with silane coupling agent, concrete operation step is as follows:
One, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.5mol/L, then adds lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirs 1 hour, namely obtains even colloidal sol russet; The lanthanum nitrate hexahydrate of described adding is 1: 2 with the ratio of the amount of substance of citric acid, and the Fe(NO3)39H2O of adding is 1: 2 with the ratio of the amount of substance of citric acid; Two, Hydrothermal Synthesis: do not add silane coupling agent, citric acid colloidal sol is placed thermostatic drying chamber, under 160 ℃, incubation water heating 8 hours takes out the thermosol system and is cooled to room temperature, namely obtains precursor; Three, preparation nanometer ferrous acid lanthanum: precursor was descended dry 8 hours at 80 ℃, be ground into powder, powder is placed the retort furnace roasting, under 600 ℃, roasting 2 hours namely obtains nanometer ferrous acid lanthanum.
The product that obtains is adopted the specific surface area of specific surface area measuring instrument assay products, and obtaining the specific surface area value is 9.2746m 2/ g; By the microscopic appearance of tem study product, can be clearly seen that nanometer ferrous acid lanthanum is block, as shown in Figure 1.
Embodiment 13: concrete operation step is as follows:
One, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.5mol/L, then adds lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirs 1 hour, namely obtains even colloidal sol russet; The lanthanum nitrate hexahydrate of described adding is 1: 2 with the ratio of the amount of substance of citric acid, and the Fe(NO3)39H2O of adding is 1: 2 with the ratio of the amount of substance of citric acid; Two, Hydrothermal Synthesis: silane coupling agent (KH550) is joined in the citric acid colloidal sol of step 1 preparation, at room temperature stirred 1 hour, silane coupling agent is dispersed in the sol system, then place thermostatic drying chamber, under 160 ℃, incubation water heating 8 hours takes out the thermosol system and is cooled to room temperature, namely obtain precursor (grey color dress material), the mole number of described adding silane coupling agent is 2.5: 100 with the ratio of the mole number of Fe(NO3)39H2O; Three, preparation nanometer ferrous acid lanthanum: with precursor 80 ℃ lower dry 8 hours, be ground into powder, powder is placed the retort furnace roasting, under 600 ℃, roasting 2 hours namely obtains the nanometer ferrous acid lanthanum of bigger serface.
The product that obtains is adopted the specific surface area of specific surface area measuring instrument assay products, and obtaining the specific surface area value is 27.5434m 2/ g; By the microscopic appearance of tem study product, can be clearly seen that nanometer ferrous acid lanthanum presents by many macrobeads to be gathered together, as shown in Figure 2.
Embodiment 14: concrete operation step is as follows:
One, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.5mol/L, then adds lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirs 1 hour, namely obtains even colloidal sol russet; The lanthanum nitrate hexahydrate of described adding is 1: 2 with the ratio of the amount of substance of citric acid, and the Fe(NO3)39H2O of adding is 1: 2 with the ratio of the amount of substance of citric acid; Two, Hydrothermal Synthesis: silane coupling agent (KH550) is joined in the citric acid colloidal sol of step 1 preparation, at room temperature stirred 1 hour, silane coupling agent is dispersed in the sol system, then place thermostatic drying chamber, under 160 ℃, incubation water heating 8 hours takes out the thermosol system and is cooled to room temperature, namely obtain precursor (grey color dress material), the mole number of described adding silane coupling agent is 5: 100 with the ratio of the mole number of Fe(NO3)39H2O; Three, preparation nanometer ferrous acid lanthanum: with precursor 80 ℃ lower dry 8 hours, be ground into powder, powder is placed the retort furnace roasting, under 600 ℃, roasting 2 hours namely obtains the nanometer ferrous acid lanthanum of bigger serface.
The product that obtains is adopted the specific surface area of specific surface area measuring instrument assay products, and obtaining the specific surface area value is 30.7847m 2/ g; By the microscopic appearance of tem study product, can be clearly seen that nanometer ferrous acid lanthanum presents by many small-particles to be gathered together, as shown in Figure 3.
Embodiment 15: concrete operation step is as follows:
One, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.5mol/L, then adds lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirs 1 hour, namely obtains even colloidal sol russet; The lanthanum nitrate hexahydrate of described adding is 1: 2 with the ratio of the amount of substance of citric acid, and the Fe(NO3)39H2O of adding is 1: 2 with the ratio of the amount of substance of citric acid; Two, Hydrothermal Synthesis: silane coupling agent (KH550) is joined in the citric acid colloidal sol of step 1 preparation, at room temperature stirred 1 hour, silane coupling agent is dispersed in the sol system, then place thermostatic drying chamber, under 160 ℃, incubation water heating 8 hours takes out the thermosol system and is cooled to room temperature, namely obtain precursor (grey color dress material), the mole number of described adding silane coupling agent is 10: 100 with the ratio of the mole number of Fe(NO3)39H2O; Three, preparation nanometer ferrous acid lanthanum: with precursor 80 ℃ lower dry 8 hours, be ground into powder, powder is placed the retort furnace roasting, under 600 ℃, roasting 2 hours namely obtains the nanometer ferrous acid lanthanum of bigger serface.
The product that obtains is adopted the specific surface area of specific surface area measuring instrument assay products, and obtaining the specific surface area value is 34.8712m 2/ g; By the microscopic appearance of tem study product, can be clearly seen that nanometer ferrous acid lanthanum presents by many small-particles and form and present dispersion state, as shown in Figure 4.
The product that embodiment 12 to 15 is obtained carries out the X-ray diffraction analysis, as shown in Figure 5, analyze the crystalline phase the Nomenclature Composition and Structure of Complexes, add as shown in Figure 5 after the silane coupling agent, the degree of crystallinity of ferrous acid lanthanum obviously descends, and proves that grain-size obtains fine regulation and control, and along with silane coupled agent concentration increases, size constantly diminishes, and namely specific surface area increases gradually;
Embodiment 16: do not add the simultaneous test with silane coupling agent, concrete operation step is as follows:
One, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.5mol/L, then adds lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirs 1 hour, namely obtains even colloidal sol russet; The lanthanum nitrate hexahydrate of described adding is 1: 2 with the ratio of the amount of substance of citric acid, and the Fe(NO3)39H2O of adding is 1: 2 with the ratio of the amount of substance of citric acid; Two, Hydrothermal Synthesis: do not add silane coupling agent, citric acid colloidal sol is placed thermostatic drying chamber, under 160 ℃, incubation water heating 8 hours takes out the thermosol system and is cooled to room temperature, namely obtains precursor; Three, preparation nanometer ferrous acid lanthanum: precursor was descended dry 8 hours at 80 ℃, be ground into powder, powder is placed the retort furnace roasting, under 800 ℃, roasting 2 hours namely obtains nanometer ferrous acid lanthanum.
The product that obtains is adopted the specific surface area of specific surface area measuring instrument assay products, and obtaining the specific surface area value is 4.2663m 2/ g.
Embodiment 17: concrete operation step is as follows:
One, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.5mol/L, then adds lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirs 1 hour, namely obtains even colloidal sol russet; The lanthanum nitrate hexahydrate of described adding is 1: 2 with the ratio of the amount of substance of citric acid, and the Fe(NO3)39H2O of adding is 1: 2 with the ratio of the amount of substance of citric acid; Two, Hydrothermal Synthesis: silane coupling agent (KH550) is joined in the citric acid colloidal sol of step 1 preparation, at room temperature stirred 1 hour, silane coupling agent is dispersed in the sol system, then place thermostatic drying chamber, under 160 ℃, incubation water heating 8 hours takes out the thermosol system and is cooled to room temperature, namely obtain precursor (grey color dress material), the mole number of described adding silane coupling agent is 2.5: 100 with the ratio of the mole number of Fe(NO3)39H2O; Three, preparation nanometer ferrous acid lanthanum: with precursor 80 ℃ lower dry 8 hours, be ground into powder, powder is placed the retort furnace roasting, under 800 ℃, roasting 2 hours namely obtains the nanometer ferrous acid lanthanum of bigger serface.
The product that obtains is adopted the specific surface area of specific surface area measuring instrument assay products, and obtaining the specific surface area value is 17.2960m 2/ g.
Embodiment 18: concrete operation step is as follows:
One, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.5mol/L, then adds lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirs 1 hour, namely obtains even colloidal sol russet; The lanthanum nitrate hexahydrate of described adding is 1: 2 with the ratio of the amount of substance of citric acid, and the Fe(NO3)39H2O of adding is 1: 2 with the ratio of the amount of substance of citric acid; Two, Hydrothermal Synthesis: silane coupling agent (KH550) is joined in the citric acid colloidal sol of step 1 preparation, at room temperature stirred 1 hour, silane coupling agent is dispersed in the sol system, then place thermostatic drying chamber, under 160 ℃, incubation water heating 8 hours takes out the thermosol system and is cooled to room temperature, namely obtain precursor (grey color dress material), the mole number of described adding silane coupling agent is 5: 100 with the ratio of the mole number of Fe(NO3)39H2O; Three, preparation nanometer ferrous acid lanthanum: with precursor 80 ℃ lower dry 8 hours, be ground into powder, powder is placed the retort furnace roasting, under 800 ℃, roasting 2 hours namely obtains the nanometer ferrous acid lanthanum of bigger serface.
The product that obtains is adopted the specific surface area of specific surface area measuring instrument assay products, and obtaining the specific surface area value is 20.3615m 2/ g.
Embodiment 19: concrete operation step is as follows:
One, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.5mol/L, then adds lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirs 1 hour, namely obtains even colloidal sol russet; The lanthanum nitrate hexahydrate of described adding is 1: 2 with the ratio of the amount of substance of citric acid, and the Fe(NO3)39H2O of adding is 1: 2 with the ratio of the amount of substance of citric acid; Two, Hydrothermal Synthesis: with silane coupling agent (KH550) in the citric acid colloidal sol of step 1 preparation, at room temperature stirred 1 hour, silane coupling agent is dispersed in the sol system, then place thermostatic drying chamber, under 160 ℃, incubation water heating 8 hours takes out the thermosol system and is cooled to room temperature, namely obtain precursor (grey color dress material), the mole number of described adding silane coupling agent is 10: 100 with the ratio of the mole number of Fe(NO3)39H2O; Three, preparation nanometer ferrous acid lanthanum: with precursor 80 ℃ lower dry 8 hours, be ground into powder, powder is placed the retort furnace roasting, under 800 ℃, roasting 2 hours namely obtains the nanometer ferrous acid lanthanum of bigger serface.
The product that obtains is adopted the specific surface area of specific surface area measuring instrument assay products, and obtaining the specific surface area value is 26.4101m 2/ g.
The product that embodiment 16 to 19 is obtained carries out the X-ray diffraction analysis, as shown in Figure 6, analyze the crystalline phase the Nomenclature Composition and Structure of Complexes, add as shown in Figure 6 after the silane coupling agent, the degree of crystallinity of ferrous acid lanthanum obviously descends, and proves that grain-size obtains fine regulation and control, and along with silane coupled agent concentration increases, size constantly diminishes, and namely specific surface area increases gradually.
As can be known when stoving temperature is adjusted to 800 ℃, specific surface area descends to some extent by analysis chart 5 and Fig. 6, but can significantly learn add silane coupling agent after, specific surface area obviously increases.

Claims (10)

1. utilize the method for the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent, it is characterized in that utilizing the concrete operation step of method of the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent as follows: one, preparation citric acid colloidal sol: at first citric acid is dissolved in the dehydrated alcohol, obtaining citric acid amount of substance concentration is 0.3~0.6mol/L, then add lanthanum nitrate hexahydrate and Fe(NO3)39H2O, stirred 0.5~2 hour, and namely obtained russet, uniform citric acid colloidal sol; The lanthanum nitrate hexahydrate of described adding is 1:(1~3 with the ratio of the amount of substance of citric acid), the Fe(NO3)39H2O of described adding is 1:(1~3 with the ratio of the amount of substance of citric acid); Two, Hydrothermal Synthesis: silane coupling agent is joined in the citric acid colloidal sol of step 1 preparation, at room temperature stirred 0.5~2 hour, silane coupling agent is dispersed in the citric acid sol system, then place thermostatic drying chamber, under 150~180 ℃, incubation water heating 6~10 hours takes out hot citric acid sol system and is cooled to room temperature, namely obtain precursor, the mole number of described adding silane coupling agent is (2~11) with the ratio of the mole number of Fe(NO3)39H2O: 100; Three, preparation nanometer ferrous acid lanthanum: with precursor 70~90 ℃ lower dry 5~10 hours, be ground into powder, powder is placed the retort furnace roasting, under 500~900 ℃, roasting 1~3 hour namely obtains the nanometer ferrous acid lanthanum of bigger serface.
2. the method for utilizing the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent according to claim 1, its feature is prepared citric acid amount of substance concentration in step 1 be 0.5mol/L.
3. the method for utilizing the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent according to claim 1 and 2, its feature is 1:2 in the ratio of the lanthanum nitrate hexahydrate that adds described in the step 1 and the amount of substance of citric acid, and the Fe(NO3)39H2O of described adding is 1:2 with the ratio of the amount of substance of citric acid.
4. the method for utilizing the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent according to claim 1, its feature churning time in step 1 is 1 hour.
5. the method for utilizing the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent according to claim 1, its feature in step 2 under 160 ℃, incubation water heating 8 hours.
6. the method for utilizing the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent according to claim 1, its feature is 2.5:100 in the ratio of the mole number that adds silane coupling agent described in the step 2 and the mole number of Fe(NO3)39H2O.
7. the method for utilizing the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent according to claim 1, its feature is 5:100 in the ratio of the mole number that adds silane coupling agent described in the step 2 and the mole number of Fe(NO3)39H2O.
8. the method for utilizing the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent according to claim 1, its feature is 10:100 in the ratio of the mole number that adds silane coupling agent described in the step 2 and the mole number of Fe(NO3)39H2O.
9. the method for utilizing silane coupling agent to synthesize large-specific surface area nano ferrous acid lanthanum of stating according to claim 8, its feature is lower dry 8 hours at 80 ℃ with precursor in step 3.
10. according to claim 9 the method for utilizing the synthetic large-specific surface area nano ferrous acid lanthanum of silane coupling agent, its feature maturing temperature in step 3 is 600 ℃, roasting time is 2 hours.
CN 201110125986 2011-05-16 2011-05-16 Method for synthesizing nanoscale lanthanum ferrate with large specific surface area by utilizing silane coupling agent Expired - Fee Related CN102249343B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1553538A (en) * 2003-06-06 2004-12-08 中国科学院过程工程研究所 Intermediate temperature solid oxide fuel battery material combing system
US20070022878A1 (en) * 2005-07-26 2007-02-01 Rojana Pornprasertsuk Ion irradiated electrolyte membrane, anode, and/or cathode
CN101318708A (en) * 2008-07-23 2008-12-10 黑龙江大学 Method for synthesizing high-specific surface area nano-lanthanum ferrous acid with mesoporous silicon dioxide as mould plate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1553538A (en) * 2003-06-06 2004-12-08 中国科学院过程工程研究所 Intermediate temperature solid oxide fuel battery material combing system
US20070022878A1 (en) * 2005-07-26 2007-02-01 Rojana Pornprasertsuk Ion irradiated electrolyte membrane, anode, and/or cathode
CN101318708A (en) * 2008-07-23 2008-12-10 黑龙江大学 Method for synthesizing high-specific surface area nano-lanthanum ferrous acid with mesoporous silicon dioxide as mould plate

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