CN101134599A - Method for preparing nano ferrous acid copper - Google Patents
Method for preparing nano ferrous acid copper Download PDFInfo
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- CN101134599A CN101134599A CNA2007100441112A CN200710044111A CN101134599A CN 101134599 A CN101134599 A CN 101134599A CN A2007100441112 A CNA2007100441112 A CN A2007100441112A CN 200710044111 A CN200710044111 A CN 200710044111A CN 101134599 A CN101134599 A CN 101134599A
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- copper
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- nano ferrous
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- nitrate trihydrate
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Abstract
The present invention relates to preparation process of nanometer copper ferrite, and belongs to the field of superfine copper ferrite powder preparing technology. The preparation process includes the following steps: dissolving malic acid in water, adding ferric nitrate nonahydrate and copper nitrate trihydrate, stirring at room temperature, dropping ammonia water to regulate pH value, evaporating solvent, drying and heating for self-spreading combustion to obtain nanometer copper ferrite powder. The process has facile material, low cost, simple operation, high yield and low power consumption.
Description
Technical field
The present invention relates to a kind of preparation method of nano ferrous acid copper, belong to the technical field of ultra-fine coppeferrite powder preparing.
Technical background
Nano ferrous acid copper is a kind of novel multifunctional nano material with spinel structure, has a wide range of applications.Coppeferrite is widely used in mutual inductance device, magnetic core bearing, transfer lever and magnetic pipe recording material because of having magnetic.In recent years, find again in nano ferrous acid copper owing to existing oxygen vacancy to have good reductibility, can be with CO
2Be reduced to C,, can be CO in the atmosphere in control atmosphere pollution so good prospects for application is arranged
2, SO
2, NO
2Conversion and recycling valid approach is provided.Coppeferrite also is a kind of important wave absorbing agent, can be used for the development of stealth material.In addition, nano ferrous acid copper also has good catalytic performance, and for example: it can catalysis AP (ammonia perchlorate), and the high-temperature decomposition temperature of AP is obviously reduced; The decomposition temperature of RDX (Cyclotrimethylene trinitramine) is reduced, and thermal discharge increases, activation energy reduction etc.Because coppeferrite has ferromegnetism and the big characteristic of specific surface concurrently, so can be used as sorbent material, some organic pollutants in the water are removed in absorption effectively, and the while can regenerate and can recycle.
At present, the reported method for preparing nano ferrite has: high energy mechanical polishing, chemical coprecipitation, sol-gel method, solid reaction process, self propagating high temperature synthesis method, microemulsion method etc.But the power consumption of high energy mechanical polishing is big, long reaction time, and easily introduce impurity, dispersiveness is good inadequately; Chemical coprecipitation is more to the influence factor of product, makes condition be difficult to control, and needs high-temperature calcination, and to the equipment requirements height, power consumption is big; Sol-gel method and self propagating high temperature synthesis method cause hard aggregation easily after oven dry and high-temperature calcination, shrink big when dry; Microemulsion method is also very unripe on production technique, still can not be applied to suitability for industrialized production on a large scale, in addition, this method raw materials cost height, often will be with an organic solvent in the preparation process or organic raw material and environment is polluted, and the gained presoma needs pyroprocessing.Because there is the production cost height to some extent in above-mentioned these methods, complex manufacturing, severe reaction conditions, shortcomings such as energy consumption height and environmental pollution are restricted its application in suitability for industrialized production.The self-propagating combustion that this experiment is adopted can overcome the shortcomings and deficiencies of additive method, has reaction evenly, and is low for equipment requirements, easy handling, low power consumption and other advantages.
Summary of the invention
The object of the present invention is to provide a kind of raw material to be easy to get, cheap, preparation cost is low, and operating process is simple, and is low for equipment requirements, does not have the loss of raw material in the preparation process, productive rate height, the preparation method of the nano ferrous acid copper that energy consumption is low.
The present invention is by the following technical solutions: self-propagating combustion is a reaction raw materials with nine water iron nitrates and nitrate trihydrate copper, and oxysuccinic acid is a complexing agent, and it is little to obtain particle diameter, is uniformly dispersed the nano ferrous acid copper powder that specific surface is big.Concrete operations are: oxysuccinic acid is soluble in water, add nine water iron nitrates and nitrate trihydrate copper after the dissolving simultaneously, and stir under the room temperature, dropping ammonia is regulated the pH value, gets the nano ferrous acid copper powder behind evaporating solvent, drying and heating self-propagating combustion.This scheme is characterised in that: with nine water iron nitrates and nitrate trihydrate copper is source of iron and Tong Yuan, with the oxysuccinic acid is complexing agent, press oxysuccinic acid and be (0.5～1.5): a certain amount of oxysuccinic acid of 1 weighing with total metal ion mol ratio, with oxysuccinic acid soluble in water after, with nine water iron nitrates and nitrate trihydrate copper is simultaneously to add in malic acid solution at 2: 1 in molar ratio, stir 1～4h under the room temperature of dissolving back, the pH value that adds the ammoniacal liquor regulator solution in above-mentioned mixed solution is between 4.0～8.0,50 ℃～80 ℃ following evaporating solvents obtain wet gel, and vacuum-drying 3～10h gets loose porous xerogel under 50 ℃～90 ℃ conditions then.Xerogel placed on the hot-plate about direct heating to 200 ℃ make its self-propagating combustion get Powdered target product, i.e. nano ferrous acid copper.
By the ratio and the reaction conditions of control raw material, can regulate the size and the pattern of nanometer particle size.
The advantage of this technical scheme:
1. raw materials used being easy to get, cheap, preparation cost is low, and operating process is simple, and is low for equipment requirements,
Do not have the loss of raw material in the preparation process, the productive rate height does not particularly need pyroprocessing, by loose
The self-propagating combustion of porous xerogel get final product nano ferrous acid copper, energy consumption is low, economical rationality, easily
Realize suitability for industrialized production.
2. by reaction conditionss such as control proportion of raw materials, pH value, vaporization temperature, drying temperatures, can prepare
The nano ferrous acid copper powder that particle diameter is different with pattern.
3. the present invention does not need pyroprocessing, and owing to take place from the time weak point that spreads, temperature is low, thereby has
Be beneficial to the refinement of particle, can also reduce interparticle reunion degree.
Embodiment
Embodiment 1:
With nine water iron nitrates and nitrate trihydrate copper is source of iron and Tong Yuan, oxysuccinic acid is a complexing agent, getting the 1.0072g oxysuccinic acid is dissolved in the 30ml distilled water, add 4.0405g nine water iron nitrates and 1.2082 nitrate trihydrate copper after the dissolving simultaneously, the mol ratio of iron ion and cupric ion is 2: 1, the mol ratio of oxysuccinic acid and total metal ion is 0.5: 1, treat that it all stirs 1 h under the room temperature of dissolving back, it is 4.0 that dropping ammonia is regulated the pH value, 60 ℃ of following constant temperature are until forming gel, put into again under 70 ℃ of the vacuum drying ovens, dry 3h gets the xerogel of bulk multi-hole, xerogel placed on the hot-plate about direct heating to 200 ℃ make it that self-propagating combustion take place, get final product the nano ferrous acid copper powder.
Embodiment 2
With nine water iron nitrates and nitrate trihydrate copper is source of iron and Tong Yuan, oxysuccinic acid is a complexing agent, getting the 1.6092g oxysuccinic acid is dissolved in the 30ml distilled water, add 4.0407g nine water iron nitrates and 1.2085 nitrate trihydrate copper after the dissolving simultaneously, the mol ratio of iron ion and cupric ion is 2: 1, the mol ratio of oxysuccinic acid and total metal ion is 0.8: 1, treat that it all stirs 3h under the room temperature of dissolving back, it is 6.0 that dropping ammonia is regulated the pH value, 70 ℃ of following constant temperature are put into 80 ℃ of vacuum drying ovens again until forming gel, and dry 5 h get the xerogel of bulk multi-hole, xerogel placed on the hot-plate about direct heating to 200 ℃ make it that self-propagating combustion take place, get final product the nano ferrous acid copper powder.
Embodiment 3:
With nine water iron nitrates and nitrate trihydrate copper is source of iron and Tong Yuan, oxysuccinic acid is a complexing agent, getting the 2.0116g oxysuccinic acid is dissolved in the 30ml distilled water, add 4.0404g nine water iron nitrates and 1.2083 nitrate trihydrate copper after the dissolving simultaneously, the mol ratio of iron ion and cupric ion is 2: 1, the mol ratio of oxysuccinic acid and total metal ion is 1: 1, treat that it all stirs 4h under the room temperature of dissolving back, it is 7.0 that dropping ammonia is regulated the pH value, 50 ℃ of following constant temperature are put into 80 ℃ of vacuum drying ovens again until forming gel, and dry 6h gets the xerogel of bulk multi-hole, xerogel placed on the hot-plate about direct heating to 200 ℃ make it that self-propagating combustion take place, get final product the nano ferrous acid copper powder.
Embodiment 4:
With nine water iron nitrates and nitrate trihydrate copper is source of iron and Tong Yuan, oxysuccinic acid is a complexing agent, getting the 2.5145g oxysuccinic acid is dissolved in the 30ml distilled water, add 4.0402g nine water iron nitrates and 1.2082 nitrate trihydrate copper after the dissolving simultaneously, the mol ratio of iron ion and cupric ion is 2: 1, the mol ratio of oxysuccinic acid and total metal ion is 1.25: 1, treat that it all stirs 2h under the room temperature of dissolving back, it is 8.0 that dropping ammonia is regulated the pH value, 80 ℃ of following constant temperature are put into 90 ℃ of vacuum drying ovens again until forming gel, and dry 8h gets the xerogel of bulk multi-hole, xerogel placed on the hot-plate about direct heating to 200 ℃ make it that self-propagating combustion take place, get final product the nano ferrous acid copper powder.
Embodiment 5:
With nine water iron nitrates and nitrate trihydrate copper is source of iron and Tong Yuan, oxysuccinic acid is a complexing agent, getting the 3.0171g oxysuccinic acid is dissolved in the 30ml distilled water, add 4.0403g nine water iron nitrates and 1.2084 nitrate trihydrate copper after the dissolving simultaneously, the mol ratio of iron ion and cupric ion is 2: 1, the mol ratio of oxysuccinic acid and total metal ion is 1.5: 1, treat that it all stirs 4h under the room temperature of dissolving back, it is 8.0 that dropping ammonia is regulated the pH value, 80 ℃ of following constant temperature are until forming gel, put into the xerogel that 50 ℃ of following dry 10h of vacuum drying oven get bulk multi-hole again, xerogel placed on the hot-plate about direct heating to 200 ℃ make it that self-propagating combustion take place, get final product the nano ferrous acid copper powder.
Claims (1)
1. the preparation method of a nano ferrous acid copper, adopt self-propagating combustion, it is characterized in that with nine water iron nitrates and nitrate trihydrate copper be source of iron and Tong Yuan, with the oxysuccinic acid is complexing agent, oxysuccinic acid and total metal ion mol ratio are (0.5～1.5): 1, with mol ratio is that 2: 1 nine water iron nitrates and nitrate trihydrate copper adds in the malic acid solution simultaneously, stir 1～4h under the room temperature of dissolving back, the pH value that adds the ammoniacal liquor regulator solution in above-mentioned mixed solution is between 4.0～8.0,50 ℃～80 ℃ following evaporating solvents obtain wet gel, vacuum-drying 3～10h gets loose porous xerogel under 50 ℃～90 ℃ conditions then, places on the hot-plate direct heating to 200 ℃ to make its self-propagating combustion get Powdered nano ferrous acid copper xerogel.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100441112A CN101134599A (en) | 2007-07-23 | 2007-07-23 | Method for preparing nano ferrous acid copper |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100441112A CN101134599A (en) | 2007-07-23 | 2007-07-23 | Method for preparing nano ferrous acid copper |
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| CN101134599A true CN101134599A (en) | 2008-03-05 |
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| CNA2007100441112A Pending CN101134599A (en) | 2007-07-23 | 2007-07-23 | Method for preparing nano ferrous acid copper |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466715A (en) * | 2013-09-16 | 2013-12-25 | 华北电力大学 | Method for preparing nano-copper ferrite composite oxygen carrier by microwave hydrothermal method |
| CN105600828A (en) * | 2016-01-04 | 2016-05-25 | 南京林业大学 | Preparation method of porous nano CuFe2O4 |
| CN106861695A (en) * | 2017-01-16 | 2017-06-20 | 华侨大学 | A kind of preparation method and applications of magnetic anoxic position Copper ferrite catalyst |
| CN107200358A (en) * | 2017-04-25 | 2017-09-26 | 昆明理工大学 | A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material |
| CN108727373A (en) * | 2018-07-05 | 2018-11-02 | 青岛科技大学 | A kind of process for catalytic synthesis of C-3 aryl seleno Imidazopyridine compound |
| CN109761284A (en) * | 2019-01-16 | 2019-05-17 | 昆明理工大学 | A kind of method and its application preparing coppe ferrite nano material using drying process with atomizing |
-
2007
- 2007-07-23 CN CNA2007100441112A patent/CN101134599A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466715A (en) * | 2013-09-16 | 2013-12-25 | 华北电力大学 | Method for preparing nano-copper ferrite composite oxygen carrier by microwave hydrothermal method |
| CN103466715B (en) * | 2013-09-16 | 2016-01-13 | 华北电力大学 | A kind of microwave-hydrothermal method prepares the method for nano-copper ferrite composite oxygen carrier |
| CN105600828A (en) * | 2016-01-04 | 2016-05-25 | 南京林业大学 | Preparation method of porous nano CuFe2O4 |
| CN106861695A (en) * | 2017-01-16 | 2017-06-20 | 华侨大学 | A kind of preparation method and applications of magnetic anoxic position Copper ferrite catalyst |
| CN106861695B (en) * | 2017-01-16 | 2019-08-30 | 华侨大学 | A kind of preparation method and applications of magnetism anoxic position Copper ferrite catalyst |
| CN107200358A (en) * | 2017-04-25 | 2017-09-26 | 昆明理工大学 | A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material |
| CN108727373A (en) * | 2018-07-05 | 2018-11-02 | 青岛科技大学 | A kind of process for catalytic synthesis of C-3 aryl seleno Imidazopyridine compound |
| CN108727373B (en) * | 2018-07-05 | 2021-08-20 | 青岛科技大学 | Catalytic synthesis method of C-3-aryl seleno-imidazopyridine compound |
| CN109761284A (en) * | 2019-01-16 | 2019-05-17 | 昆明理工大学 | A kind of method and its application preparing coppe ferrite nano material using drying process with atomizing |
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Open date: 20080305 |