CN110627132B - Preparation method of small-size iron disulfide nano hollow sphere - Google Patents
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Abstract
A preparation method of a small-size iron disulfide hollow nanosphere relates to a preparation method of an iron disulfide hollow nanosphere. The invention aims to solve the problem of the existing FeS2The powder preparation process has the problem that a small-size hollow structure is difficult to obtain. The method comprises the following steps: firstly, preparing an iron stearate solution; secondly, preparing a sulfur powder solution; thirdly, preparing a surfactant solution; and fourthly, respectively heating and stirring the ferric stearate solution, the sulfur powder solution and the surfactant solution for reaction, mixing, finally carrying out hydrothermal reaction, centrifuging the hydrothermal reaction product, and cleaning the solid obtained by the centrifugation to obtain the small-size iron disulfide nano hollow sphere. The invention prepares the hollow FeS2The size of the crystal is 10 nm-200 nm, and the crystal has good crystallinity and dispersibility. The method is suitable for preparing the small-size iron disulfide nano hollow sphere.
Description
Technical Field
The invention relates to a preparation method of a hollow iron disulfide nanosphere.
Background
FeS2Is the main component of pyrite and has diamagnetism. It is an inactive substance at room temperature and becomes active after the temperature is raised. FeS2The material is used as an indirect band gap semiconductor material and is widely applied to industries such as rubber, paper making, textile, food, match, battery and the like and agriculture. In recent years, FeS is responsible2The special electronic structure can be used as an electrode material of a lithium ion battery, and has the advantages of high capacity, stable discharge, good compatibility with a dielectric medium and the like. But natural FeS2The application of the FeS is influenced by the defects of more impurities in the material, high cost of the purification process and the like, so that the FeS with high purity, simple preparation and small size is urgently needed2The material can meet the requirement of practical application.
Preparation of FeS at present2The material method mainly comprises a ball milling method, an electrodeposition method, a microwave heating method, a vapor deposition method, a hydrothermal method, a solvent method and the like. Prepared FeS2The material has the advantages of high conductivity, high thermal stability, stable discharge voltage platform, high discharge efficiency and the like, thereby widening the application field of the material. Magnetic iron oxide and H used in Chinese patent 'a method for preparing iron disulfide' (publication number: CN105712410A)2FeS is prepared by taking S gas as raw material in the presence of oxidant2The method simplifies the preparation of FeS2The material process, but the large amount of oxidant in the preparation process can greatly shorten the service life of the preparation equipment. Chinese patent 'a method for preparing iron disulfide' (publication number: CN108793264A) prepares FeS by reacting iron-based desulfurizer as a raw material with hydrogen sulfide under the condition of liquid slurry2The material solves the problem that the oxidant corrodes equipment, and simplifies FeS2The preparation process also reduces the production cost. But the FeS prepared therefrom2The larger size of the powder particles affects the electrochemical performance of the powder. Chinese patent 'a method for preparing iron disulfide' (publication number: CN110127773A) FeS is crushed by crushing equipment2Crushing the ore into fine particles, screening the particles with the size of 0.2-1 mm by using screening equipment, continuously grinding the particles into uniform particles, putting the particles into a reaction kettle, adding acid for heating, cleaning and drying the reacted product to obtain FeS2A powder material. Although high purity FeS is achieved2Powder material, but the preparation process is relatively complicated.
The above conventional preparation of FeS2The powder is prepared from iron oxide, iron and FeS2Mine and other main raw materials, and improves FeS2Purity of the powder or simplified preparationThe processes, however, are all basically aimed at improving the large-particle FeS2Powder preparation process without improvement on FeS2Method for size control of powders. FeS2The powder can be improved in electrochemical properties when reaching the nanometer level, so that the current application needs a high-purity nanoscale FeS2A method for preparing powder.
Disclosure of Invention
The invention aims to solve the problem of the existing FeS2The problem that the powder preparation process is difficult to obtain a small-size hollow structure is solved, and the preparation method of the small-size iron disulfide nano hollow sphere is provided.
A preparation method of small-size iron disulfide nano hollow spheres is completed according to the following steps:
firstly, dissolving ferric stearate into liquid paraffin to obtain a ferric stearate solution;
the mass fraction of ferric stearate in the ferric stearate solution in the step one is 1-20%;
secondly, dissolving sulfur powder into oleic acid to obtain a sulfur powder solution;
the mass fraction of the sulfur powder in the sulfur powder solution in the step two is 1-25%;
dispersing a surfactant into the liquid to obtain a surfactant solution;
the mass fraction of the surfactant in the surfactant solution in the step three is 0.1-3%;
fourthly, heating the ferric stearate solution to 50-80 ℃, and then stirring and reacting for 10-30 min under the conditions that the temperature is 50-80 ℃ and the stirring speed is 50-200 r/min to obtain reaction liquid I;
secondly, heating the sulfur powder solution to 40-60 ℃, and then stirring and reacting for 10-30 min under the conditions that the temperature is 40-60 ℃ and the stirring speed is 50-200 r/min to obtain reaction liquid II;
thirdly, heating the surfactant solution to 40-60 ℃, and then stirring and reacting for 10-30 min under the conditions that the temperature is 40-60 ℃ and the stirring speed is 50-200 r/min to obtain reaction liquid III;
mixing the reaction solution I, the reaction solution II and the reaction solution III, stirring for 10-30 min at the temperature of 40-60 ℃ and the stirring speed of 50-200 r/min, transferring to a hydrothermal reaction kettle, and reacting for 120-480 min at the temperature of 150-200 ℃ to obtain a reaction solution IV;
the volume ratio of the reaction liquid I, the reaction liquid II and the reaction liquid III in the step IV is (0.5-1.5): 0.05-0.2;
fifthly, cooling the reaction liquid IV to room temperature, centrifuging for 10-40 min under the condition that the centrifugation speed is 5000-10000 r/min, then removing the supernatant, and collecting the lower-layer solid matter; and (3) washing the collected solid matters at the lower layer for 5-10 times by using heptane with the temperature of 50-60 ℃ to obtain the small-size iron disulfide nano hollow spheres.
The principle and the advantages of the invention are as follows:
the invention uses sulfur powder and ferric stearate as raw materials, uses liquid paraffin as reaction solution, prepares ferric sulfide nano-particles with different sizes by a solvothermal method, and utilizes a surfactant to make the nano-particles become a hollow structure, and the structure is beneficial to the application in the fields of electrochemistry and electromagnetic wave absorption;
secondly, the ferric stearate reacts with sulfur powder to generate FeS2The nano-crystal gradually grows into the hollow nanosphere under the constraint of the surfactant, and because the oil-soluble raw material and the reaction liquid are adopted, the size and the crystallinity of the generated particles are easy to control;
the method is simple, the raw materials are easy to obtain, the operation is simple, the cost is low, and the method is suitable for large-scale production;
fourthly, the FeS prepared by the invention2The particle size is uniform, and can be controlled according to the use requirement;
fifthly, the hollow FeS prepared by the invention2Has large specific surface area and is suitable for the fields of electrochemistry and electromagnetic wave absorption.
Fifthly, the invention prepares the hollow FeS2The size of the crystal is 10 nm-200 nm, and the crystal has good crystallinity and dispersibility.
The method is suitable for preparing the small-size iron disulfide nano hollow sphere.
Drawings
FIG. 1 is a transmission electron microscope image of small-sized iron disulfide hollow nanospheres prepared in example one;
FIG. 2 is an XRD pattern of small-sized iron disulfide hollow nanospheres prepared in example one;
FIG. 3 is a transmission electron microscope image of small-sized iron disulfide hollow nanospheres prepared in example two.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a small-size iron disulfide nano hollow sphere, which is completed according to the following steps:
firstly, dissolving ferric stearate into liquid paraffin to obtain a ferric stearate solution;
the mass fraction of ferric stearate in the ferric stearate solution in the step one is (1-20%);
secondly, dissolving sulfur powder into oleic acid to obtain a sulfur powder solution;
the mass fraction of the sulfur powder in the sulfur powder solution in the step two is (1-25%);
dispersing a surfactant into the liquid to obtain a surfactant solution;
the mass fraction of the surfactant in the surfactant solution in the step three is 0.1-3%;
fourthly, heating the ferric stearate solution to 50-80 ℃, and then stirring and reacting for 10-30 min under the conditions that the temperature is 50-80 ℃ and the stirring speed is 50-200 r/min to obtain reaction liquid I;
secondly, heating the sulfur powder solution to 40-60 ℃, and then stirring and reacting for 10-30 min under the conditions that the temperature is 40-60 ℃ and the stirring speed is 50-200 r/min to obtain reaction liquid II;
thirdly, heating the surfactant solution to 40-60 ℃, and then stirring and reacting for 10-30 min under the conditions that the temperature is 40-60 ℃ and the stirring speed is 50-200 r/min to obtain reaction liquid III;
mixing the reaction solution I, the reaction solution II and the reaction solution III, stirring for 10-30 min at the temperature of 40-60 ℃ and the stirring speed of 50-200 r/min, transferring to a hydrothermal reaction kettle, and reacting for 120-480 min at the temperature of 150-200 ℃ to obtain a reaction solution IV;
the volume ratio of the reaction liquid I, the reaction liquid II and the reaction liquid III in the step IV is (0.5-1.5): 0.05-0.2;
fifthly, cooling the reaction liquid IV to room temperature, centrifuging for 10-40 min under the condition that the centrifugation speed is 5000-10000 r/min, then removing the supernatant, and collecting the lower-layer solid matter; and (3) washing the collected solid matters at the lower layer for 5-10 times by using heptane with the temperature of 50-60 ℃ to obtain the small-size iron disulfide nano hollow spheres.
The principle and advantages of the embodiment are as follows:
the method comprises the following steps of firstly, preparing iron sulfide nano-particles with different sizes by using sulfur powder and ferric stearate as raw materials and liquid paraffin as a reaction solution through a solvothermal method, and enabling the iron sulfide nano-particles to be of a hollow structure by utilizing a surfactant, wherein the structure is beneficial to application in the fields of electrochemistry and electromagnetic wave absorption;
secondly, in the embodiment, ferric stearate reacts with sulfur powder to generate FeS2The nano-crystal gradually grows into the hollow nanosphere under the constraint of the surfactant, and because the oil-soluble raw material and the reaction liquid are adopted, the size and the crystallinity of the generated particles are easy to control;
the method is simple, raw materials are easy to obtain, the operation is simple, the cost is low, and the method is suitable for large-scale production;
fourthly, the FeS prepared by the embodiment2The particle size is uniform, and can be controlled according to the use requirement;
fifthly, the hollow FeS prepared by the embodiment2Has large specific surface area and is suitable for the fields of electrochemistry and electromagnetic wave absorption.
Fifthly, the hollow FeS is prepared by the embodiment2The size of the crystal is 10 nm-200 nm, and the crystal has good crystallinity and dispersibility.
The method is suitable for preparing the small-size iron disulfide nano hollow sphere.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the mass fraction of the ferric stearate in the ferric stearate solution in the step one is (8-10%). Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and the mass fraction of the sulfur powder in the sulfur powder solution in the step two is (8-10%). The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: the surfactant in the third step is oleic acid diethanolamide, oleylamine, castor oil polyoxyethylene ether, sorbitan fatty acid ester or polyvinyl alcohol. The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the mass fraction of the surfactant in the surfactant solution in the third step is 1-1.5%. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: heating the ferric stearate solution to 50-60 ℃, and stirring and reacting for 10-30 min under the conditions that the temperature is 50-60 ℃ and the stirring speed is 50-100 r/min to obtain reaction liquid I. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: fourthly, heating the sulfur powder solution to 40-50 ℃, and then stirring and reacting for 10-15 min under the conditions that the temperature is 40-50 ℃ and the stirring speed is 50-100 r/min to obtain reaction liquid II. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: and fourthly, mixing the reaction solution I, the reaction solution II and the reaction solution III, stirring for 10-15 min at the temperature of 40-50 ℃ and the stirring speed of 50-100 r/min, transferring to a hydrothermal reaction kettle, and reacting for 120-300 min at the temperature of 150-200 ℃ to obtain a reaction solution IV. The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: and in the step IV, the volume ratio of the reaction liquid I to the reaction liquid II to the reaction liquid III is 1:1: 0.1. The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: and the size of the small-size iron disulfide nano hollow sphere in the step five is 10-200 nm. The other steps are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows: a preparation method of small-size iron disulfide nano hollow spheres is completed according to the following steps:
firstly, dissolving ferric stearate into liquid paraffin to obtain a ferric stearate solution;
the mass fraction of ferric stearate in the ferric stearate solution in the step one is 10 percent;
secondly, dissolving sulfur powder into oleic acid to obtain a sulfur powder solution;
the mass fraction of the sulfur powder in the sulfur powder solution in the second step is 10 percent;
dispersing a surfactant into the liquid to obtain a surfactant solution;
the surfactant in the third step is oleic acid diethanolamide;
the mass fraction of the surfactant in the surfactant solution in the step three is 1%;
fourthly, heating the ferric stearate solution to 50 ℃, and stirring and reacting for 10min under the conditions that the temperature is 50 ℃ and the stirring speed is 50r/min to obtain reaction liquid I;
secondly, heating the sulfur powder solution to 40 ℃, and then stirring and reacting for 10min under the conditions that the temperature is 40 ℃ and the stirring speed is 50r/min to obtain reaction liquid II;
thirdly, heating the surfactant solution to 40 ℃, and then stirring and reacting for 10min under the conditions that the temperature is 40 ℃ and the stirring speed is 50r/min to obtain reaction liquid III;
mixing the reaction solution I, the reaction solution II and the reaction solution III, stirring for 30min at the temperature of 40 ℃ and the stirring speed of 100r/min, transferring to a hydrothermal reaction kettle, and reacting for 240min at the temperature of 180 ℃ to obtain a reaction solution IV;
the volume ratio of the reaction liquid I, the reaction liquid II and the reaction liquid III in the step IV is 1:1: 0.1;
fifthly, cooling the reaction liquid IV to room temperature, centrifuging for 10min at the centrifugal speed of 5000r/min, removing the supernatant, and collecting the solid matter at the lower layer; washing the collected solid matter at the lower layer for 5 times by using heptane with the temperature of 50 ℃ to obtain small-size iron disulfide nano hollow spheres;
and fifthly, the size of the small-size iron disulfide nano hollow sphere is 100-200 nm.
FIG. 1 is a transmission electron microscope image of small-sized iron disulfide hollow nanospheres prepared in example one;
as can be seen from fig. 1, the small-sized iron disulfide hollow nanospheres prepared in the first embodiment are spherical, the hollow structure is formed by combining a plurality of small-sized particles under the action of the surfactant, and the size of the hollow structure is about 100 to 200 nanometers, so that the hollow structure is favorably dispersed in the carrier liquid.
Fig. 2 is an XRD pattern of the small-sized iron disulfide nano hollow sphere prepared in example one.
As can be seen from the XRD chart of fig. 2, peaks (111), (200), (210), (211), (220), (311) and (321) correspond to 28.51 °, 33.03 °, 37.07 °, 40.75 °, 47.04 °, 56.48 ° and 64.26 °, respectively, which is related to FeS2(PDF #65-3321) Standard card agreement, demonstrating that the material prepared is FeS2. The prepared material is about 10 nanometers from the half-peak width, and the hollow FeS can be found by combining a transmission electron microscope2Is composed of multiple 10nmFeS2The particles are assembled into a structure.
The small-size iron disulfide nano hollow sphere prepared in the first embodiment can be used as an electromagnetic wave absorbent, and test results show that the small-size iron disulfide nano hollow sphere has good absorption performance at high frequency, because when electromagnetic waves are injected into the hollow FeS2The loss is generated by multiple refractions when the nanospheres are used, so that the electromagnetic wave absorption performance is improved.
Example two: a preparation method of small-size iron disulfide nanospheres is completed according to the following steps:
firstly, dissolving ferric stearate into liquid paraffin to obtain a ferric stearate solution;
the mass fraction of ferric stearate in the ferric stearate solution in the step one is 5%;
secondly, dissolving sulfur powder into oleic acid to obtain a sulfur powder solution;
the mass fraction of the sulfur powder in the sulfur powder solution in the second step is 5 percent;
dispersing a surfactant into the liquid to obtain a surfactant solution;
the surfactant in the third step is oleylamine;
the mass fraction of the surfactant in the surfactant solution in the step three is 0.5%;
fourthly, heating the ferric stearate solution to 50 ℃, and stirring and reacting for 10min under the conditions that the temperature is 50 ℃ and the stirring speed is 50r/min to obtain reaction liquid I;
secondly, heating the sulfur powder solution to 40 ℃, and then stirring and reacting for 10min under the conditions that the temperature is 40 ℃ and the stirring speed is 50r/min to obtain reaction liquid II;
thirdly, heating the surfactant solution to 40 ℃, and then stirring and reacting for 10min under the conditions that the temperature is 40 ℃ and the stirring speed is 50r/min to obtain reaction liquid III;
mixing the reaction solution I, the reaction solution II and the reaction solution III, stirring for 30min at the temperature of 40 ℃ and the stirring speed of 100r/min, transferring the mixture into a hydrothermal reaction kettle, and reacting for 120min at the temperature of 150 ℃ to obtain a reaction solution IV;
the volume ratio of the reaction liquid I, the reaction liquid II and the reaction liquid III in the step IV is 1:1: 0.2;
fifthly, cooling the reaction liquid IV to room temperature, centrifuging for 10min at the centrifugation speed of 10000r/min, removing the supernatant, and collecting the lower-layer solid matter; washing the collected solid matter at the lower layer for 5 times by using heptane with the temperature of 50 ℃ to obtain small-size iron disulfide nano hollow spheres;
and the size of the small-size iron disulfide nanospheres in the step five is 10-20 nm.
FIG. 3 is a transmission electron microscope image of small-sized iron disulfide hollow nanospheres prepared in example two.
As can be seen from fig. 3, the small-sized iron disulfide hollow nanospheres prepared in example two were substantially 10nm to 20nm in size, and the main reason why the small-sized iron disulfide hollow nanospheres prepared in example two were reduced in size was that the concentration of the reaction raw material in the reaction solution was reduced, the HLB value of the surfactant was reduced, and the reaction temperature was lowered to reduce the size of the nanoparticles.
Claims (6)
1. A preparation method of a small-size iron disulfide hollow nanosphere is characterized in that the preparation method of the small-size iron disulfide hollow nanosphere is completed according to the following steps:
firstly, dissolving ferric stearate into liquid paraffin to obtain a ferric stearate solution;
the mass fraction of ferric stearate in the ferric stearate solution in the step one is 10-20%;
secondly, dissolving sulfur powder into oleic acid to obtain a sulfur powder solution;
the mass fraction of the sulfur powder in the sulfur powder solution in the step two is 10-25%;
dispersing a surfactant into the liquid to obtain a surfactant solution;
the surfactant in the third step is oleic acid diethanolamide, oleylamine, castor oil polyoxyethylene ether, sorbitan fatty acid ester or polyvinyl alcohol;
the mass fraction of the surfactant in the surfactant solution in the third step is 1% -3%;
fourthly, heating the ferric stearate solution to 50-80 ℃, and stirring and reacting for 10-30 min under the conditions that the temperature is 50-80 ℃ and the stirring speed is 50-200 r/min to obtain a reaction solution I;
secondly, heating the sulfur powder solution to 40-60 ℃, and then stirring and reacting for 10-30 min under the conditions that the temperature is 40-60 ℃ and the stirring speed is 50-200 r/min to obtain a reaction solution II;
thirdly, heating the surfactant solution to 40-60 ℃, and then stirring and reacting for 10-30 min under the conditions that the temperature is 40-60 ℃ and the stirring speed is 50-200 r/min to obtain reaction liquid III;
mixing the reaction liquid I, the reaction liquid II and the reaction liquid III, stirring for 10-30 min at the temperature of 40-60 ℃ and the stirring speed of 50-200 r/min, transferring to a hydrothermal reaction kettle, and reacting for 120-480 min at the temperature of 150-200 ℃ to obtain a reaction liquid IV;
the volume ratio of the reaction liquid I, the reaction liquid II and the reaction liquid III in the step IV is (0.5-1.5): 0.05-0.2;
fifthly, cooling the reaction liquid IV to room temperature, centrifuging for 10-40 min under the condition that the centrifugation speed is 5000-10000 r/min, then removing the supernatant, and collecting the solid matter at the lower layer; washing the collected solid matters on the lower layer 5-10 times by using heptane with the temperature of 50-60 ℃ to obtain small-size iron disulfide nano hollow spheres;
and fifthly, the size of the small-size iron disulfide nano hollow sphere is 10-200 nm.
2. The method for preparing the small-size iron disulfide hollow nanospheres according to claim 1, wherein the mass fraction of the surfactant in the surfactant solution in the step three is 1% -1.5%.
3. The preparation method of the small-size iron disulfide hollow nanospheres according to claim 1, wherein in the fourth step, an iron stearate solution is heated to 50-60 ℃, and then stirred and reacted for 10-30 min under the conditions that the temperature is 50-60 ℃ and the stirring speed is 50-100 r/min, so as to obtain a reaction solution I.
4. The preparation method of the small-size iron disulfide hollow nanospheres according to claim 1, wherein in the fourth step, the sulfur powder solution is heated to 40-50 ℃, and then stirred and reacted for 10-15 min under the conditions that the temperature is 40-50 ℃ and the stirring speed is 50-100 r/min, so as to obtain a reaction solution II.
5. The preparation method of the small-size iron disulfide hollow nanospheres according to claim 1, wherein in the fourth step, the reaction liquid I, the reaction liquid II and the reaction liquid III are mixed, stirred for 10min to 15min at the temperature of 40 ℃ to 50 ℃ and at the stirring speed of 50r/min to 100r/min, transferred to a hydrothermal reaction kettle, and reacted at the temperature of 150 ℃ to 200 ℃ for 120min to 300min to obtain the reaction liquid IV.
6. The method for preparing the small-size iron disulfide hollow nanospheres according to claim 1, wherein the volume ratio of the reaction liquid I, the reaction liquid II and the reaction liquid III in the fourth step is 1:1: 0.1.
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