CN111634960A - Preparation method of nickel hydrazine carbonate microspheres - Google Patents

Preparation method of nickel hydrazine carbonate microspheres Download PDF

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CN111634960A
CN111634960A CN202010577032.3A CN202010577032A CN111634960A CN 111634960 A CN111634960 A CN 111634960A CN 202010577032 A CN202010577032 A CN 202010577032A CN 111634960 A CN111634960 A CN 111634960A
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fish gelatin
solution
deionized
hydrazine carbonate
nickel hydrazine
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杨明
刘骏
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Wuhan Polytechnic University
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Wuhan Polytechnic University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/16—Hydrazine; Salts thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Inorganic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a preparation method of nickel hydrazine carbonate microspheres, which comprises the following steps: step S10, dissolving fish gelatin in water to prepare a fish gelatin aqueous solution, adding an ethanol solution into the fish gelatin aqueous solution to separate out solid substances in the fish gelatin aqueous solution, and then collecting and drying the solid substances to obtain deionized fish gelatin; step S20, preparing the deionized fish gelatin into deionized fish gelatin water solution and adding NiCl2Solution and NH2NH2·H2CO3Forming a mixed solution, and then stirring and reacting until a precipitate is generated in the mixed solution; and step S30, separating out the precipitate, washing and drying to obtain the nickel hydrazine carbonate microspheres. The nickel hydrazine carbonate microsphere prepared by the invention is of a spherical structure, the particle size is 0.8-1.5 mu m, no impurity peak is contained by XRD determination, and the product has high purity.

Description

Preparation method of nickel hydrazine carbonate microspheres
Technical Field
The invention relates to the technical field of microsphere preparation, in particular to a preparation method of nickel hydrazine carbonate microspheres.
Background
Compared with particles of other shapes, the spherical particles have the characteristics of large bulk density, high uniformity, good flowing property and the like, are in point contact, are not easy to agglomerate, are convenient to store for a long time, and have attracted extensive attention of engineering and academia due to excellent properties. The microsphere material has the characteristics of special periodic structure, higher specific surface area, high adsorbability, assemblability and the like, has wide application prospect in the fields of chemical catalysis, adsorption column packing, environmental management, biopharmaceuticals, gas adsorption, chromatographic separation, sensors, liquid crystal displays, drug sustained release preparations, composite energetic materials and the like, plays an important role in relevant research, but the prior art lacks a method for preparing the nickel hydrazine carbonate microsphere with high product purity.
Disclosure of Invention
The invention mainly aims to provide a preparation method of nickel hydrazine carbonate microspheres, and aims to provide a preparation method of high-purity nickel hydrazine carbonate microspheres.
In order to realize the purpose, the invention provides a preparation method of nickel hydrazine carbonate microspheres, which comprises the following steps:
step S10, dissolving fish gelatin in water to prepare a fish gelatin aqueous solution, adding an ethanol solution into the fish gelatin aqueous solution to separate out solid substances in the fish gelatin aqueous solution, and then collecting and drying the solid substances to obtain deionized fish gelatin;
step S20, preparing the deionized fish gelatin into deionized fish gelatin water solution and adding NiCl2Solution and NH2NH2·H2CO3Forming a mixed solution, and then stirring and reacting until a precipitate is generated in the mixed solution;
and step S30, separating out the precipitate, washing and drying to obtain the nickel hydrazine carbonate microspheres.
Alternatively, in step S10:
the volume fraction of the ethanol solution is 95%, and the mass volume ratio of the fish gelatin to the water to the ethanol solution is 1 g: (45-55) mL: (10-12) mL.
Alternatively, the step of dissolving the fish gelatin in water to prepare an aqueous fish gelatin solution in step S10 may comprise:
adding the fish gelatin into deionized water, heating in a boiling water bath until the fish gelatin is completely dissolved, and cooling to obtain a fish gelatin aqueous solution.
Alternatively, in step S10:
the drying temperature for drying the solid matter is 105-120 ℃, and the drying time is 60-90 min.
Alternatively, in step S20:
the volume of the deionized fish gelatin aqueous solution is the NiCl2Solution and NH2NH2·H2CO3The total volume of the solution is 8-10 times.
Alternatively, in step S20:
NiCl in the mixed solution2And NH2NH2·H2CO3In a molar ratio of 1: (2-2.2).
Alternatively, in step S20:
the mass concentration of the deionized fish gelatin aqueous solution is 2-3%.
Alternatively, in step S20:
the reaction temperature of the stirring reaction is 20-30 ℃, and the reaction time is 120-150 min.
According to the technical scheme provided by the invention, the fish gelatin is prepared into deionized fish gelatin, then the deionized fish gelatin is prepared into deionized fish gelatin water solution, and then NiCl is added2Solution and NH2NH2·H2CO3And adding the solution into an aqueous solution of deionized fish gelatin, stirring for reaction, separating out a precipitate generated by the reaction, washing and drying the precipitate to obtain the nickel hydrazine carbonate microsphere, wherein the prepared nickel hydrazine carbonate microsphere is of a spherical structure, has a particle size of 0.8-1.5 mu m, does not contain impurity peaks through XRD determination, and has high purity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart of an embodiment of a method for preparing nickel hydrazine carbonate microspheres according to the present invention;
FIG. 2 is an XRD pattern of nickel hydrazine carbonate microspheres prepared by the invention;
FIG. 3 is an SEM image of nickel hydrazine carbonate microspheres prepared by the invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of nickel hydrazine carbonate microspheres, and fig. 1 shows an embodiment of the preparation method of nickel hydrazine carbonate microspheres provided by the invention. Referring to fig. 1, in this embodiment, the preparation method of nickel hydrazine carbonate microspheres includes the following steps:
step S10, dissolving fish gelatin in water to prepare a fish gelatin aqueous solution, adding an ethanol solution into the fish gelatin aqueous solution to separate out solid substances in the fish gelatin aqueous solution, and then collecting and drying the solid substances to obtain deionized fish gelatin;
in this embodiment, the step of dissolving fish gelatin in water to prepare an aqueous fish gelatin solution in step S10 includes: adding the fish gelatin into deionized water, heating in a boiling water bath until the fish gelatin is completely dissolved, and cooling to obtain a fish gelatin aqueous solution. The fish gelatin is dissolved by boiling water bath heating, so that the dissolving rate of the fish gelatin can be increased, the solubility of the fish gelatin is increased, and the heating temperature can be conveniently controlled.
Further, the volume fraction of the ethanol solution selected in step S10 is 95%, and the mass-to-volume ratio of the fish gelatin, water and ethanol solution is 1 g: (45-55) mL: (10-12) mL. And after the solid matter is not increased, filtering and separating out the solid matter, and drying to obtain the deionized fish gelatin. Further, the drying temperature for drying the solid matter is 105-120 ℃, and the drying time is 60-90 min.
Step S20, preparing the deionized fish gelatin into deionized fish gelatin water solution and adding NiCl2Solution and NH2NH2·H2CO3Forming a mixed solution, and then stirring and reacting until a precipitate is generated in the mixed solution;
after the deionized fish gelatin is prepared, the deionized fish gelatin is dissolved in deionized water to prepare a deionized fish gelatin aqueous solution, preferably, the mass concentration of the deionized fish gelatin aqueous solution is 2-3%, the solution viscosity is appropriate, and the dissolution rate of the deionized fish gelatin is high. Further, in this example, the volume of the deionized aqueous fish gelatin solution is the NiCl2Solution and NH2NH2·H2CO3The total volume of the solution is 8-10 times.
Mixing NiCl2Solution and NH2NH2·H2CO3The solution is added into the deionized fish gelatin water solution in turn, NiCl2And NH2NH2·H2CO3In a molar ratio of 1: (2 to 2.2) by reacting NH2NH2·H2CO3Relative to NiCl2And the excessive nickel ions can be promoted to completely participate in the reaction, so that the utilization rate of the nickel ions is improved. It is understood that the NiCl2Solution and NH2NH2·H2CO3The concentration of the solution may be unlimited, and only need to satisfy NiCl2And NH2NH2·H2CO3In a molar ratio of 1: (2-2.2), in order to calculate the addition amount of the solution, the NiCl is used in the following embodiments2The molar concentration of the solution is 0.1mol/L, the NH2NH2·H2CO3The molar concentration of the solution is 0.2 mol/L.
In the NiCl2Solution and NH2NH2·H2CO3And after the solution is added to obtain a mixed solution, continuously stirring the mixed solution at the temperature of 20-30 ℃ for reaction for 120-150 min, wherein a precipitate is generated in the mixed solution in the reaction process, and after stirring and reacting for 120-150 min, the generation amount of the precipitate is not increased any more, and the reaction is finished.
And step S30, separating out the precipitate, washing and drying to obtain the nickel hydrazine carbonate microspheres.
And after the reaction is finished, centrifugally separating out the generated precipitate, sequentially washing the precipitate by using distilled water and ethanol, then placing the precipitate in a vacuum drying oven to dry at room temperature to obtain light purple powder, namely the nickel hydrazine carbonate microsphere.
According to the technical scheme provided by the invention, the fish gelatin is prepared into deionized fish gelatin, then the deionized fish gelatin is prepared into deionized fish gelatin water solution, and then NiCl is added2Solution and NH2NH2·H2CO3And adding the solution into an aqueous solution of deionized fish gelatin, stirring for reaction, separating out a precipitate generated by the reaction, washing and drying the precipitate to obtain the nickel hydrazine carbonate microsphere, wherein the prepared nickel hydrazine carbonate microsphere is of a spherical structure, has a particle size of 0.8-1.5 mu m, does not contain impurity peaks through XRD (X-ray diffraction) determination, and has high purity.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
(1) Adding 10g of fish gelatin into 500mL of deionized water, heating in a boiling water bath to dissolve the fish gelatin, cooling, adding 110mL of 95% ethanol solution, fully mixing, filtering to collect precipitated solid substances, and drying at 105 ℃ for 90min to obtain deionized fish gelatin;
(2) preparing deionized fish gelatin into deionized fish gelatin water solution with mass concentration of 3%, adding 200mL deionized fish gelatin water solution into 500mL round bottom flask, stirring with magnetic stirrer while maintaining solution temperature at 30 deg.C, and sequentially adding 10mL 0.1mol/L NiCl2Solution and 10mL0.2mol/L NH2NH2·H2CO3Continuously stirring the solution for reaction for 120min, and generating a large amount of light purple precipitates after the reaction is finished;
(3) and (3) centrifugally separating out precipitates generated in the reaction, washing the precipitates by using distilled water and ethanol in sequence, then placing the washed precipitates in a vacuum drying oven, and drying the precipitates at room temperature to obtain light purple powder to prepare the nickel hydrazine carbonate microspheres.
Example 2
(1) Adding 10g of fish gelatin into 500mL of deionized water, heating in a boiling water bath to dissolve the fish gelatin, cooling, adding 120mL of 95% ethanol solution, fully mixing, filtering to collect precipitated solid substances, and drying at 120 ℃ for 60min to obtain deionized fish gelatin;
(2) preparing deionized fish gelatin into deionized fish gelatin water solution with mass concentration of 2.5%, adding 160mL deionized fish gelatin water solution into 500mL round bottom flask, stirring with magnetic stirrer while maintaining solution temperature at 30 deg.C, and sequentially adding 10mL 0.1mol/L NiCl2Solution and 10.5mL of 0.2mol/L NH2NH2·H2CO3Continuously stirring the solution for reaction for 140min, and generating a large amount of light purple precipitates after the reaction is finished;
(3) and (3) centrifugally separating out precipitates generated in the reaction, washing the precipitates by using distilled water and ethanol in sequence, then placing the washed precipitates in a vacuum drying oven, and drying the precipitates at room temperature to obtain light purple powder to prepare the nickel hydrazine carbonate microspheres.
Example 3
(1) Adding 10g of fish gelatin into 500mL of deionized water, heating in a boiling water bath to dissolve the fish gelatin, cooling, adding 100mL of 95% ethanol solution, fully mixing, filtering to collect precipitated solid substances, and drying at 110 ℃ for 80min to obtain deionized fish gelatin;
(2) preparing deionized fish gelatin into deionized fish gelatin water solution with mass concentration of 2%, adding 180mL deionized fish gelatin water solution into 500mL round bottom flask, stirring with magnetic stirrer while maintaining solution temperature at 25 deg.C, and sequentially adding 10mL 0.1mol/L NiCl2Solution and 10mL0.2mol/L NH2NH2·H2CO3Continuously stirring the solution for reaction for 130min, and generating a large amount of light purple precipitates after the reaction is finished;
(3) and (3) centrifugally separating out precipitates generated in the reaction, washing the precipitates by using distilled water and ethanol in sequence, then placing the washed precipitates in a vacuum drying oven, and drying the precipitates at room temperature to obtain light purple powder to prepare the nickel hydrazine carbonate microspheres.
Example 4
(1) Adding 6g of fish gelatin into 300mL of deionized water, heating in a boiling water bath to dissolve the fish gelatin, cooling, adding 60mL of 95% ethanol solution, fully mixing, filtering, collecting precipitated solid substances, and drying at 110 ℃ for 70min to obtain deionized fish gelatin;
(2) preparing deionized fish gelatin into deionized fish gelatin water solution with mass concentration of 2.5%, adding 220mL deionized fish gelatin water solution into 500mL round bottom flask, stirring with magnetic stirrer while maintaining solution temperature at 25 deg.C, and sequentially adding 12mL 0.1mol/L NiCl2Solution and 12mL of 0.2mol/L NH2NH2·H2CO3Continuously stirring the solution for reaction for 120min, and generating a large amount of light purple precipitates after the reaction is finished;
(3) and (3) centrifugally separating out precipitates generated in the reaction, washing the precipitates by using distilled water and ethanol in sequence, then placing the washed precipitates in a vacuum drying oven, and drying the precipitates at room temperature to obtain light purple powder to prepare the nickel hydrazine carbonate microspheres.
Example 5
(1) Adding 5g of fish gelatin into 250mL of deionized water, heating in a boiling water bath to dissolve the fish gelatin, cooling, adding 55mL of 95% ethanol solution, fully mixing, filtering, collecting separated solid matters, and drying at 120 ℃ for 60min to obtain deionized fish gelatin;
(2) preparing deionized fish gelatin into deionized fish gelatin water solution with mass concentration of 2%, adding 180mL deionized fish gelatin water solution into 500mL round bottom flask, stirring with magnetic stirrer while maintaining solution temperature at 20 deg.C, and sequentially adding 10mL 0.1mol/L NiCl2Solution and 11mL0.2mol/L NH2NH2·H2CO3Continuously stirring the solution for reaction for 130min, and generating a large amount of light purple precipitates after the reaction is finished;
(3) and (3) centrifugally separating out precipitates generated in the reaction, washing the precipitates by using distilled water and ethanol in sequence, then placing the washed precipitates in a vacuum drying oven, and drying the precipitates at room temperature to obtain light purple powder to prepare the nickel hydrazine carbonate microspheres.
Example 6
(1) Adding 4g of fish gelatin into 200mL of deionized water, heating in a boiling water bath to dissolve the fish gelatin, cooling, adding 45mL of 95% ethanol solution, fully mixing, filtering to collect precipitated solid substances, and drying at 105 ℃ for 90min to obtain deionized fish gelatin;
(2) preparing deionized fish gelatin into deionized fish gelatin water solution with mass concentration of 2.2%, adding 150mL deionized fish gelatin water solution into 250mL round bottom flask, stirring with magnetic stirrer while maintaining solution temperature at 25 deg.C, and sequentially adding 8mL 0.1mol/L NiCl2Solution and 8.5mL of 0.2mol/L NH2NH2·H2CO3Continuously stirring the solution for reaction for 120min, and generating a large amount of light purple precipitates after the reaction is finished;
(3) and (3) centrifugally separating out precipitates generated in the reaction, washing the precipitates by using distilled water and ethanol in sequence, then placing the washed precipitates in a vacuum drying oven, and drying the precipitates at room temperature to obtain light purple powder to prepare the nickel hydrazine carbonate microspheres.
Example 7
(1) Adding 8g of fish gelatin into 400mL of deionized water, heating in a boiling water bath to dissolve the fish gelatin, cooling, adding 90mL of 95% ethanol solution, fully mixing, filtering to collect precipitated solid substances, and drying at 115 ℃ for 70min to obtain deionized fish gelatin;
(2) preparing deionized fish gelatin into deionized fish gelatin water solution with mass concentration of 2.5%, adding 290mL deionized fish gelatin water solution into 500mL round bottom flask, stirring with magnetic stirrer while maintaining solution temperature at 30 deg.C, and sequentially adding 15mL 0.1mol/L NiCl2Solution and 16mL of 0.2mol/L NH2NH2·H2CO3Continuously stirring the solution for reaction for 130min, and generating a large amount of light purple precipitates after the reaction is finished;
(3) and (3) centrifugally separating out precipitates generated in the reaction, washing the precipitates by using distilled water and ethanol in sequence, then placing the washed precipitates in a vacuum drying oven, and drying the precipitates at room temperature to obtain light purple powder to prepare the nickel hydrazine carbonate microspheres.
Example 8
(1) Adding 10g of fish gelatin into 500mL of deionized water, heating in a boiling water bath to dissolve the fish gelatin, cooling, adding 110mL of 95% ethanol solution, fully mixing, filtering to collect precipitated solid substances, and drying at 120 ℃ for 85min to obtain deionized fish gelatin;
(2) preparing deionized fish gelatin into deionized fish gelatin water solution with mass concentration of 2.6%, adding 320mL deionized fish gelatin water solution into 500mL round bottom flask, stirring with magnetic stirrer, maintaining solution temperature at 20 deg.C, and sequentially adding 20mL 0.1mol/L NiCl2Solution and 20mL of 0.2mol/L NH2NH2·H2CO3Continuously stirring the solution for reaction for 150min, and generating a large amount of light purple precipitates after the reaction is finished;
(3) and (3) centrifugally separating out precipitates generated in the reaction, washing the precipitates by using distilled water and ethanol in sequence, then placing the washed precipitates in a vacuum drying oven, and drying the precipitates at room temperature to obtain light purple powder to prepare the nickel hydrazine carbonate microspheres.
Example 9
(1) Adding 10g of fish gelatin into 450mL of deionized water, heating in a boiling water bath to dissolve the fish gelatin, cooling, adding 100mL of 95% ethanol solution, fully mixing, filtering to collect precipitated solid substances, and drying at 115 ℃ for 75min to obtain deionized fish gelatin;
(2) preparing deionized fish gelatin into deionized fish gelatin water solution with mass concentration of 2.8%, adding 200mL deionized fish gelatin water solution into 500mL round bottom flask, stirring with magnetic stirrer while maintaining the solution temperature at 23 deg.C, and sequentially adding 10mL 0.1mol/L NiCl2Solution and 10mL of 0.2mol/L NH2NH2·H2CO3Continuously stirring the solution for reacting for 135min, and generating a large amount of light purple precipitates after the reaction is finished;
(3) and (3) centrifugally separating out precipitates generated in the reaction, washing the precipitates by using distilled water and ethanol in sequence, then placing the washed precipitates in a vacuum drying oven, and drying the precipitates at room temperature to obtain light purple powder to prepare the nickel hydrazine carbonate microspheres.
Example 10
(1) Adding 10g of fish gelatin into 550mL of deionized water, heating in a boiling water bath to dissolve the fish gelatin, cooling, adding 120mL of 95% ethanol solution, fully mixing, filtering to collect precipitated solid substances, and drying at 120 ℃ for 65min to obtain deionized fish gelatin;
(2) preparing deionized fish gelatin into deionized fish gelatin water solution with mass concentration of 2.4%, adding 200mL deionized fish gelatin water solution into 500mL round bottom flask, stirring with magnetic stirrer while maintaining solution temperature at 28 deg.C, and sequentially adding 10mL 0.1mol/L NiCl2Solution and 10mL of 0.2mol/L NH2NH2·H2CO3The solution is continuously stirred and reacted for 125min, and after the reaction is finished, a large amount of light purple precipitate is generatedForming;
(3) and (3) centrifugally separating out precipitates generated in the reaction, washing the precipitates by using distilled water and ethanol in sequence, then placing the washed precipitates in a vacuum drying oven, and drying the precipitates at room temperature to obtain light purple powder to prepare the nickel hydrazine carbonate microspheres.
When the nickel hydrazine carbonate microspheres prepared in the embodiment of the invention are subjected to XRD and SEM tests, the nickel hydrazine carbonate microspheres with spherical structures, uniformly distributed particle sizes and high purity can be successfully prepared in the embodiments 1 to 10 of the invention, and the test results are basically the same, so the nickel hydrazine carbonate microspheres prepared in the embodiment 4 are taken as an example to analyze the test results.
Fig. 2 shows an XRD pattern of the nickel hydrazine carbonate microspheres prepared by the present invention, and fig. 3 shows an SEM image of the nickel hydrazine carbonate microspheres prepared by the present invention. As can be seen from FIG. 2, the peak positions 2 θ are 20.06 °, 25.35 °, 32.80 °, 34.48 °, 44.18 °, 48.72 ° and 52.61 °, respectively, and the peak intensities and positions are matched with literature values (see: Joint Committee on powder Diffraction Standards (JCPDS), File No. 21-0586]), and No impurity peak is found, indicating that the product has higher purity, indicating that the product prepared by the invention is pure nickel hydrazine carbonate. As can be seen from FIG. 3, the nickel hydrazine carbonate microspheres prepared by the invention are spherical in structure, and the particle size is uniformly distributed in the range of 0.8-1.5 μm.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.

Claims (8)

1. The preparation method of the nickel hydrazine carbonate microspheres is characterized by comprising the following steps:
step S10, dissolving fish gelatin in water to prepare a fish gelatin aqueous solution, adding an ethanol solution into the fish gelatin aqueous solution to separate out solid substances in the fish gelatin aqueous solution, and then collecting and drying the solid substances to obtain deionized fish gelatin;
step S20, preparing the deionized fish gelatin into deionized fish gelatin water solution and adding NiCl2Solution and NH2NH2·H2CO3Forming a mixed solution, and then stirring and reacting until a precipitate is generated in the mixed solution;
and step S30, separating out the precipitate, washing and drying to obtain the nickel hydrazine carbonate microspheres.
2. The method for preparing nickel hydrazine carbonate microspheres according to claim 1, wherein in step S10:
the volume fraction of the ethanol solution is 95%, and the mass volume ratio of the fish gelatin to the water to the ethanol solution is 1 g: (45-55) mL: (10-12) mL.
3. The method for preparing nickel hydrazine carbonate microspheres according to claim 1, wherein the step of dissolving fish gelatin in water to prepare an aqueous fish gelatin solution in step S10 comprises:
adding the fish gelatin into deionized water, heating in a boiling water bath until the fish gelatin is completely dissolved, and cooling to obtain a fish gelatin aqueous solution.
4. The method for preparing nickel hydrazine carbonate microspheres according to claim 1, wherein in step S10:
the drying temperature for drying the solid matter is 105-120 ℃, and the drying time is 60-90 min.
5. The method for preparing nickel hydrazine carbonate microspheres according to claim 1, wherein in step S20:
the volume of the deionized fish gelatin aqueous solution is the NiCl2Solution and NH2NH2·H2CO3The total volume of the solution is 8-10 times.
6. The method for preparing nickel hydrazine carbonate microspheres according to claim 1, wherein in step S20:
NiCl in the mixed solution2And NH2NH2·H2CO3In a molar ratio of 1: (2-2.2).
7. The method for preparing nickel hydrazine carbonate microspheres according to claim 1, wherein in step S20:
the mass concentration of the deionized fish gelatin aqueous solution is 2-3%.
8. The method for preparing nickel hydrazine carbonate microspheres according to claim 1, wherein in step S20:
the reaction temperature of the stirring reaction is 20-30 ℃, and the reaction time is 120-150 min.
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