CN103991907A - Preparation method for manganese carbonate nano-fiber ball - Google Patents
Preparation method for manganese carbonate nano-fiber ball Download PDFInfo
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- CN103991907A CN103991907A CN201410191556.3A CN201410191556A CN103991907A CN 103991907 A CN103991907 A CN 103991907A CN 201410191556 A CN201410191556 A CN 201410191556A CN 103991907 A CN103991907 A CN 103991907A
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- tartrate
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Abstract
The invention discloses a preparation method for a manganese carbonate nano-fiber ball. The method includes: mixing manganese chloride with potassium sodium tartrate to undergo reaction so as to form manganese tartrate precipitate, then mixing the manganese tartrate precipitate with a potassium carbonate solution and loading the mixture into a reaction kettle, performing heat preservation for 3-10h at 50-200DEG C, conducting hydrothermal treatment, naturally cooling the reaction kettle to room temperature, performing kettle discharge, then washing the reaction product with distilled water repeatedly, and carrying out filtering and drying, thus obtaining the manganese carbonate nano-fiber ball. The manganese carbonate nano-fiber ball prepared by the invention has the advantages of simple process, controllable appearance, good crystallization, high purity, unique self-assembly structure, low cost, and no use of any polluting surfactant, etc.
Description
Technical field
The present invention relates to a kind of preparation method of manganous carbonate nanofiber ball, relate in particular to the manganous carbonate nanofiber ball preparation method of a kind of manganous tartrate precipitation as reaction precursor.
Background technology
Manganous carbonate (MnCO3) is a kind of very important inorganic materials, it is not only the main raw material of producing soft magnetic ferrite, and all there is application very widely in a lot of fields such as electronics, catalyzer, pigment, medicine, pottery, thereby become one of study hotspot in recent years.As everyone knows, the performance of nano material depends on the factor such as pattern and size of its nanocrystal, thereby the nano material with special appearance all can show some excellent performances, therefore the manganous carbonate crystal of, preparing pattern novelty is all having very important significance aspect theoretical basis research and practical application.
At present to the control of manganous carbonate crystal morphology conventionally by be tensio-active agent, tensio-active agent is generally cetyl trimethylammonium bromide, Sodium dodecylbenzene sulfonate, polyoxyethylene glycol, polyvinylpyrrolidone etc.Due to a large amount of uses of tensio-active agent, can make to produce the foam that pile up like a mountain in river, allow people recognize the tremendous influence of tensio-active agent to environment.The water nutrition problem that a large amount of uses of tensio-active agent cause simultaneously is still perplexing us, it has been recognized that environmental problem is by a major issue that is following nano-functional material preparation development.
Summary of the invention
The object of the invention is the deficiency in order to solve the problems of the technologies described above existence, provide that a kind of technique is simple, pattern is controlled, good crystallinity, purity are high, have unique self-assembled structures, and preparation method with low cost, that do not use any manganous carbonate nanofiber ball that has contaminated surface promoting agent.
The preparation method of manganous carbonate nanofiber ball of the present invention, concrete steps are as follows:
Step 1, Manganous chloride tetrahydrate is dissolved in to deionized water, forms the Manganous chloride tetrahydrate aqueous solution, the concentration of the Manganous chloride tetrahydrate in regulator solution is 0.2 ~ 4.0mol/L;
Step 2, Seignette salt is dissolved in to deionized water, forms soluble tartrate sodium water solution, the concentration of the Seignette salt in regulator solution is 0.2 ~ 4.0mol/L;
Step 3, salt of wormwood is dissolved in to deionized water, forms wet chemical, the concentration of the salt of wormwood in regulator solution is 0.2 ~ 4.0mol/L;
The potassium sodium tartrate solution that step 4, the manganese chloride solution that step 1 is made make with step 2 mixes mutually, and blending ratio is 1:1, obtains manganous tartrate precipitation as reaction precursor;
The manganous tartrate precipitation solution that step 5, the solution of potassium carbonate that step 3 is made make with step 4 mixes mutually, blending ratio is 1:1, then join in reactor inner bag, regulate the reaction mass volume in reactor inner bag to reach 70% ~ 90% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that step 5 is equipped with to reaction mass are placed in reactor, and sealing, 50 ~ 200
ounder C, be incubated 3 ~ 10 hours and carry out hydrothermal treatment consists, then allow reactor naturally cool to room temperature, unload after still, by distilled water repetitive scrubbing reaction product, filter, 50
oafter drying at C temperature, obtain manganous carbonate nanofiber ball.
Use in the present invention manganous tartrate precipitation as reaction precursor, if without manganous tartrate precipitation, just can not get this manganous carbonate nanofiber ball.This be because: under normal conditions, can pass through external force, the mode of adding tensio-active agent makes the growth of crystal have orientation, obtain one-dimensional square to grow crystal.When added tensio-active agent in reaction system time, because SURFACTANT ADSORPTION is in manganous carbonate growth unit surface, the growth of manganous carbonate crystal has been played to guide effect, therefore can make manganous carbonate crystal occur oriented growth, can obtain one dimension manganous carbonate crystal, as manganese carbonate nanorod.But tensio-active agent has huge pollution to environment.
And in the present invention, do not use any tensio-active agent.In the present invention, change reaction precursor, do not use conventional mn ion, but use manganous tartrate precipitation as reaction precursor, this be because manganous tartrate in the process of growth of manganous carbonate crystal, not only itself there is extraordinary orientation, and can make manganous carbonate crystal in the process of growth, there is self-assembly, thereby the total energy that makes manganous carbonate crystal reaches minimum, therefore the present invention can not use under the condition of tensio-active agent, obtains the nanofiber ball of one dimension manganous carbonate nanofiber composition.In the present invention, must precipitate as reaction precursor using manganous tartrate, otherwise can not get manganous carbonate nanofiber ball.
The purity of described salt of wormwood, Manganous chloride tetrahydrate, Seignette salt and dehydrated alcohol is all not less than chemical pure.
Wherein the reaction mass volume with in distilled water adjusting reactor inner bag in step 5 reaches 70% ~ 90% of reactor inner bag volume, and this is in order to make hydro-thermal reaction system in boiling state, is beneficial to crystallization and the growth of manganous carbonate crystal.
Wherein in step 6 by distilled water repetitive scrubbing reaction product, filter, 50
oat C temperature, dry, this is in order to obtain dry and the higher manganous carbonate crystal of purity.
Beneficial effect of the present invention is:
The present invention has prepared the manganous carbonate nanofiber ball that good crystallinity, purity are high, have unique texture, especially the manganous carbonate nanofiber ball obtaining is formed by the self-assembly of manganous carbonate fiber, the diameter of manganous carbonate fiber is about 10-15nm, and the length of manganous carbonate fiber is about 400-500 nanometer.So-called self-assembly refers to a kind of technology of the spontaneous formation ordered structure of basic structural unit (molecule, nano material, micron or the more material of big scale).In the process of self-assembly, basic structural unit spontaneous tissue or gathering under the interaction based on non covalent bond is a structure of stablizing, have certain regular geometric outward appearance.Self-assembly is the important means of creating novel substance and producing new function, and the special supramolecular structure of utilizing self-assembly to form, can prepare the synthetic functional materials that cannot realize of conventional chemical, be considered to solve the current mankind such as material, the energy, health and environment and develop the hope place of the main challenge facing.
The synthetic method of manganous carbonate nanofiber ball provided by the invention, have simple to operate, do not use the advantages such as any organic surface active agent, pollution-free, with low cost, pattern is controlled, be easy to suitability for industrialized production.The manganous carbonate nanofiber ball that the present invention prepares first, has unique fibrous texture, thereby at aspects such as electronics, pottery, catalyzer, medicine, coating, enamel, will have more excellent performance, has application prospect more widely.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the synthetic manganous carbonate nanofiber ball of the present invention.
Fig. 2 is transmission electron microscope (TEM) photo of the synthetic manganous carbonate nanofiber ball of the present invention.
Embodiment
Further illustrate the present invention below in conjunction with embodiment.
Embodiment 1
Step 1, Manganous chloride tetrahydrate is dissolved in to deionized water, forms the Manganous chloride tetrahydrate aqueous solution, the concentration of the Manganous chloride tetrahydrate in regulator solution is 0.2mol/L;
Step 2, Seignette salt is dissolved in to deionized water, forms soluble tartrate sodium water solution, the concentration of the Seignette salt in regulator solution is 0.2mol/L;
Step 3, salt of wormwood is dissolved in to deionized water, forms wet chemical, the concentration of the salt of wormwood in regulator solution is 0.2mol/L;
The potassium sodium tartrate solution that step 4, the manganese chloride solution that step 1 is made make with step 2 mixes mutually, and blending ratio is 1:1, obtains manganous tartrate precipitation as reaction precursor;
The manganous tartrate precipitation solution that step 5, the solution of potassium carbonate that step 3 is made make with step 4 mixes mutually, blending ratio is 1:1, then join in reactor inner bag, regulate the reaction mass volume in reactor inner bag to reach 90% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that step 5 is equipped with to reaction mass are placed in reactor, and sealing, 60
ounder C, be incubated 10 hours and carry out hydrothermal treatment consists, then allow reactor naturally cool to room temperature, unload after still, by distilled water repetitive scrubbing reaction product, filter, 50
oafter drying at C temperature, obtain manganous carbonate nanofiber ball.Manganous carbonate nanofiber ball is formed by the self-assembly of manganous carbonate fiber, and the diameter of manganous carbonate fiber is about 10nm, and the length of manganous carbonate fiber is about 400 nanometers, and its XRD figure spectrum is shown in Fig. 1; Transmission electron microscope picture is shown in Fig. 2.
Embodiment 2
Step 1, Manganous chloride tetrahydrate is dissolved in to deionized water, forms the Manganous chloride tetrahydrate aqueous solution, the concentration of the Manganous chloride tetrahydrate in regulator solution is 1.8mol/L;
Step 2, Seignette salt is dissolved in to deionized water, forms soluble tartrate sodium water solution, the concentration of the Seignette salt in regulator solution is 1.8mol/L;
Step 3, salt of wormwood is dissolved in to deionized water, forms wet chemical, the concentration of the salt of wormwood in regulator solution is 1.8mol/L;
The potassium sodium tartrate solution that step 4, the manganese chloride solution that step 1 is made make with step 2 mixes mutually, and blending ratio is 1:1, obtains manganous tartrate precipitation as reaction precursor;
The manganous tartrate precipitation solution that step 5, the solution of potassium carbonate that step 3 is made make with step 4 mixes mutually, blending ratio is 1:1, then join in reactor inner bag, regulate the reaction mass volume in reactor inner bag to reach 80% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that step 5 is equipped with to reaction mass are placed in reactor, and sealing, 120
ounder C, be incubated 6 hours and carry out hydrothermal treatment consists, then allow reactor naturally cool to room temperature, unload after still, by distilled water repetitive scrubbing reaction product, filter, 50
oafter drying at C temperature, obtain manganous carbonate nanofiber ball.
Embodiment 3
Step 1, Manganous chloride tetrahydrate is dissolved in to deionized water, forms the Manganous chloride tetrahydrate aqueous solution, the concentration of the Manganous chloride tetrahydrate in regulator solution is 3.3mol/L;
Step 2, Seignette salt is dissolved in to deionized water, forms soluble tartrate sodium water solution, the concentration of the Seignette salt in regulator solution is 3.3mol/L;
Step 3, salt of wormwood is dissolved in to deionized water, forms wet chemical, the concentration of the salt of wormwood in regulator solution is 3.3mol/L;
The potassium sodium tartrate solution that step 4, the manganese chloride solution that step 1 is made make with step 2 mixes mutually, and blending ratio is 1:1, obtains manganous tartrate precipitation as reaction precursor;
The manganous tartrate precipitation solution that step 5, the solution of potassium carbonate that step 3 is made make with step 4 mixes mutually, blending ratio is 1:1, then join in reactor inner bag, regulate the reaction mass volume in reactor inner bag to reach 70% of reactor inner bag volume with distilled water;
Step 6, the reactor inner bag that step 5 is equipped with to reaction mass are placed in reactor, and sealing, 200
ounder C, be incubated 3 hours and carry out hydrothermal treatment consists, then allow reactor naturally cool to room temperature, unload after still, by distilled water repetitive scrubbing reaction product, filter, 50
oafter drying at C temperature, obtain manganous carbonate nanofiber ball.
Claims (4)
1. a preparation method for manganous carbonate nanofiber ball, is characterized in that: step 1, Manganous chloride tetrahydrate is dissolved in to deionized water, forms the Manganous chloride tetrahydrate aqueous solution, the concentration of the Manganous chloride tetrahydrate in regulator solution is 0.2 ~ 4.0mol/L; Step 2, Seignette salt is dissolved in to deionized water, forms soluble tartrate sodium water solution, the concentration of the Seignette salt in regulator solution is 0.2 ~ 4.0mol/L; Step 3, salt of wormwood is dissolved in to deionized water, forms wet chemical, the concentration of the salt of wormwood in regulator solution is 0.2 ~ 4.0mol/L; The potassium sodium tartrate solution that step 4, the manganese chloride solution that step 1 is made make with step 2 mixes mutually, obtains manganous tartrate precipitation as reaction precursor; The manganous tartrate precipitation solution that step 5, the solution of potassium carbonate that step 3 is made make with step 4 mixes mutually, then joins in reactor inner bag; Step 6, the reactor inner bag that step 5 is equipped with to reaction mass are placed in reactor, and sealing, 50 ~ 200
ounder C, be incubated 3 ~ 10 hours and carry out hydrothermal treatment consists, then allow reactor naturally cool to room temperature, unload after still, by distilled water repetitive scrubbing reaction product, filter, 50
oafter drying at C temperature, obtain manganous carbonate nanofiber ball.
2. the preparation method of a kind of manganous carbonate nanofiber ball according to claim 1, is characterized in that: manganese chloride solution and potassium sodium tartrate solution blending ratio are 1:1.
3. the preparation method of a kind of manganous carbonate nanofiber ball according to claim 1, is characterized in that: solution of potassium carbonate and manganous tartrate precipitation solution blending ratio are 1:1.
4. the preparation method of a kind of manganous carbonate nanofiber ball according to claim 1, it is characterized in that: the manganous tartrate precipitation solution that the solution of potassium carbonate that step 3 is made makes with step 4 mixes mutually, then join in reactor inner bag, regulate the reaction mass volume in reactor inner bag to reach 70% ~ 90% of reactor inner bag volume with distilled water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108530024A (en) * | 2018-05-28 | 2018-09-14 | 钦州学院 | It is a kind of can shock resistance Nixing pottery manufacture craft |
| CN111704169A (en) * | 2020-07-01 | 2020-09-25 | 洛阳理工学院 | Preparation method of manganese molybdate nanosheet crystal |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101269840A (en) * | 2008-03-05 | 2008-09-24 | 广州融捷材料科技有限公司 | Spherical manganese carbonate and preparing method thereof |
| CN101805024A (en) * | 2010-04-27 | 2010-08-18 | 江苏大学 | Preparation method of manganese carbonate nanorod |
| CN102120618A (en) * | 2011-01-26 | 2011-07-13 | 江苏方舟新能源股份有限公司 | Preparation method of high-tap density manganese carbonate |
| CN102531065A (en) * | 2010-12-30 | 2012-07-04 | 河南科隆集团有限公司 | Spherical manganese carbonate synthetic method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101269840A (en) * | 2008-03-05 | 2008-09-24 | 广州融捷材料科技有限公司 | Spherical manganese carbonate and preparing method thereof |
| CN101805024A (en) * | 2010-04-27 | 2010-08-18 | 江苏大学 | Preparation method of manganese carbonate nanorod |
| CN102531065A (en) * | 2010-12-30 | 2012-07-04 | 河南科隆集团有限公司 | Spherical manganese carbonate synthetic method |
| CN102120618A (en) * | 2011-01-26 | 2011-07-13 | 江苏方舟新能源股份有限公司 | Preparation method of high-tap density manganese carbonate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108530024A (en) * | 2018-05-28 | 2018-09-14 | 钦州学院 | It is a kind of can shock resistance Nixing pottery manufacture craft |
| CN111704169A (en) * | 2020-07-01 | 2020-09-25 | 洛阳理工学院 | Preparation method of manganese molybdate nanosheet crystal |
| CN111704169B (en) * | 2020-07-01 | 2022-09-30 | 洛阳理工学院 | Preparation method of manganese molybdate nanosheet crystal |
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Inventor after: Yang Linlin Inventor after: Wang Yonggang Inventor after: Wang Xiaofeng Inventor after: Wang Yujiang Inventor after: Xu Guohui Inventor after: Lin Haiyan Inventor after: Luo Wei Inventor before: Wang Yonggang Inventor before: Yang Linlin Inventor before: Wang Xiaofeng Inventor before: Wang Yujiang Inventor before: Xu Guohui Inventor before: Lin Haiyan Inventor before: Luo Wei |
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Free format text: CORRECT: INVENTOR; FROM: WANG YONGGANG YANG LINLIN WANG XIAOFENG WANG YUJIANG XU GUOHUI LIN HAIYAN LUO WEI TO: YANG LINLIN WANG YONGGANG WANG XIAOFENG WANG YUJIANG XU GUOHUI LIN HAIYAN LUO WEI |
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