177 results about "Ammonium tetrathiomolybdate" patented technology

The invention discloses a molybdenum disulfide-carbon hollow ball hybrid material. The molybdenum disulfide-carbon hollow ball hybrid material has a hollow ball structure; and the hybrid material formed by embedding a single layer of molybdenum disulfide nanosheet or a few of layers of molybdenum disulfide nanosheets into a carbon material is a shell layer of the hollow ball. The invention further discloses a preparation method of the molybdenum disulfide-carbon hollow ball hybrid material. The method comprises the following steps: with amino-modified silica particles as a template, coating the template with an organic pyrolytic carbon material and ammonium tetrathiomolybdate through solvothermal reaction; carrying out high-temperature treatment in an inert atmosphere; and finally removing a silicon dioxide template, so as to obtain the molybdenum disulfide-carbon hollow ball hybrid material disclosed by the invention. The initial lithium insertion capacity of the molybdenum disulfide-carbon hollow ball hybrid material disclosed by the invention is close to 1010mAh/g; and the specific capacity can still be kept at 662mAh/g after 40 repeated charge and discharge cycles.

The invention relates to a controllable synthesis and synchronous surface modifying method of an MoS2 nanosheet. The method comprises the steps that ammonium tetrathiomolybdate serves as an Mo source and an S source, or the ammonium molybdate serves as the Mo source, the thiourea serves as the S source, the ammonium tetrathiomolybdate or the ammonium molybdate and the thiourea are dissolved in water or the mixed solvent of water and polyethylene glycol, thermal treatment is carried out for 12-18 hours under the temperature ranging from 200 DEG C to 220 DEG C, separating and washing are carried out to obtain the MoS2 nanosheet, and the type and concentration of the Mo source and the S source and/or the adopted solvent are/or controlled so that the size of the MoS2 nanosheet can be controlled.

The invention discloses a three-dimensional nitrogen-doped transition metal oxide/nickel sulfide composite catalyst. The catalyst includes nickel foam, nitrogen-doped transition metal oxide and nickelsulfide, wherein the nickel foam serves as a substrate, and the nitrogen-doped transition metal oxide grows on the nickel foam in situ. The invention further discloses a preparation method of the three-dimensional nitrogen-doped transition metal oxide/nickel sulfide composite catalyst. The method includes the following steps that the nickel foam substrate is impregnated in an ammonium tetrathiomolybdate solution and dried after impregnation, and an ammonium tetrathiomolybdate contained nickel foam precursor is obtained; the nickel foam precursor is subjected to vacuum high-temperature calcination, and the molybdenum dioxide/nickel sulfide composite catalyst is obtained; the molybdenum dioxide/nickel sulfide composite materials are subjected to thermal ammoniation, and the three-dimensional nitrogen-doped transition metal oxide/nickel sulfide composite catalyst is obtained. The invention further provides the application of the composite catalyst as a cathode catalyst material in an electrolytic water cathode HER reaction, the composite catalyst shows excellent electrocatalytic performance in alkaline electrolyte and has good stability, and the possibility of hydrogen energy development and utilization is further improved.

The invention belongs to the field of catalytic materials and particularly provides a flowerlike carbon-loaded MoS<2> nano-particle composite and a preparation method thereof. The preparation method comprises the steps that firstly, flowerlike ZnO serves as a template and biomass serves as a precursor, and flowerlike carbon is obtained through a simple hydrothermal method and subsequent high-temperature heat treatment and acid etching; then the obtained flowerlike carbon and ammonium tetrathiomolybdate are subjected to solvothermal processing, and the composite in which MoS<2> nano-particles are evenly loaded on the flowerlike carbon is obtained. Hydrogen evolution catalysis tests indicate that the composite is low in hydrogen evolution take-off potential and Tafele slope and good in long-term stability, wherein the hydrogen evolution take-off potential is approximately 110 mV, and the Tafele slope is 65 mV/dec. According to the flowerlike carbon-loaded MoS<2> nano-particle composite and the preparation method thereof, the biomass which is wide in source serves as the precursor of the flowerlike carbon, a two-step method, namely the hydrothermal processing and the solvothermal processing, is adopted, the operation is simple, the production cost is low, little pollution is caused to the environment, the serial production and large-scale production are easy to achieve, and the flowerlike carbon-loaded MoS<2> nano-particle composite has a good industrial production basis and a wide application prospect.

The invention discloses a molybdenum disulfide nano-catalyst preparation method and catalyst which can be applied to a catalytic hydrogenation process of heavy oil. According to the preparation method disclosed by the invention, ammonium tetrathiomolybdate is utilized as a raw material and a surface active agent, the ammonium tetrathiomolybdate is dissolved into absolute methanol, then a reducing agent is added after the ammonium tetrathiomolybdate is mixed evenly, and the ammonium tetrathiomolybdate is put into a constant-temperature oven of 100 to 250 DEG C to be stored for 3 to 48 hours; the molybdenum disulfide nano-catalyst can be obtained after separation. The molybdenum disulfide nano-catalyst prepared through the invention has smaller size and uniform particle size. The molybdenum disulfide nano-catalyst prepared through the invention has a larger contact angle so as to have better dispersion in organic solvent, and catalytic performance of the molybdenum disulfide nano-catalyst in a catalytic process can be improved. According to the research, the MoS2 nano-catalyst is applied to the catalytic hydrogenation process of heavy oil for the first time. Furthermore, the preparation method disclosed by the invention is simple to operate, has moderate condition, low cost and a simple synthesizing device and can be hopefully applied to industrial production.

The invention provides a preparation method of molybdenum disulfide nano-fibers. The preparation method uses ammonium thiomolybdate as a raw material, and comprises the steps of electro-spinning liquid preparation, electrostatic spinning and sintering, wherein, an electro-spinning liquid is acquired by dissolving the ammonium thiomolybdate in a polyvinyl alcohol solution with a concentration of 7wt% to 15wt%; electrostatic spinning is conducted in a manner that the electro-spinning liquid achieves electro-spinning in an electrostatic field formed by a voltage of 10kV to 30kV between a syringeneedle and a collection screen and falls on the collection screen to form fiber felt; and sintering is conducted in a manner that the collection screen loaded with the fiber felt is sintered for 1 to3 hours at a temperature of 500 DEG C to 850 DEG C under a hydrogen atmosphere. The preparation method has the advantages that MoS2 fibers with the diameters evenly ranging from 50nm to 300nm can be prepared, equipment is simple, the operation is convenient, and XRD (X-ray diffraction) analysis shows that molybdenum disulfide is well crystallized.

The invention discloses a molybdenum-tungsten separating process for a molybdenum-tungsten mixed ammonium salt solution in tungsten hydrometallurgy and relates to the molybdenum-tungsten separating process for cooling and crystallizing an ammonium tungstate solution from high-concentration molybdenum to separate out tetrathio ammonium molybdate. The ammonium tungstate solution is subjected to sulfo-treatment, so that the molybdenum in the solution preferably generates the tetrathio ammonium molybdate. Under the condition of no addition of any chemical agent, the temperature of the solution isproperly reduced; and by standing or mechanical stirring, majority of molybdenum is separated out in a (NH4)2MoS4 crystal form without separating out the tungsten, thereby achieving the effects of effectively separating and recycling the molybdenum from the ammonium tungstate solution.

The invention discloses a method for synthesizing mesoporous molybdenum disulphide by taking a mesoporous silica molecular sieve as a hard template. The method comprises the following steps of: firstly, preparing a hydrochloric acid solution of alcohol amine; secondly, adding ammonium tetrathiomolybdate, standing at room temperature after stirred reaction, filtering, cleaning and drying in vacuumto obtain a precursor; thirdly, dissolving the precursor into water and absolute methanol, adding the mesoporous silica molecular sieve, and carrying out ultrasonography after stirred reaction to obtain a solid and liquid mixture; fourthly, placing the solid and liquid mixture into a muffle furnace after filtering, cleaning and drying, raising the temperature to 400-450 DEG C under the protectionof hydrogen, then, preserving the temperature for 1-2h, and cooling to the room temperature to obtain mesoporous molybdenum disulphide powder containing the mesoporous silica molecular sieve; and fifthly, cleaning 1-5 times by using an HF (Hydrogen Fluoride) aqueous solution and drying to obtain the mesoporous molybdenum disulphide. The mesoporous molybdenum disulphide synthesized by using the method provided by the invention is high in catalytic activity, the yield of tar obtained in coal pyrolysis reaction is high, and the using amount of catalysts is small, and no assistant is needed.

A process for preparing the MoS2 particles with inorganic fullerene structure includes such steps as dissolving the ammonium tetrathiomolybdate in water, spray drying to obtain superfine MoS3 particles, and heating the MoS3 in the mixture gas of H2 and Ar gas to reduce MoS3 into MoS2 with inorganic fullerene structure.

The invention discloses a preparation method and application of an MoS2/transition metal/graphene composite hydrogen dissociation electrode in a microbial electrolytic tank. The preparation method comprises the following steps: (1) dissolving graphene oxide with deionized water, performing ultrasonic peeling to obtain a graphene oxide solution, then, adding ammonium tetrathiomolybdate, a salt compound of transition metal and a reducing agent in sequence, and dispersing uniformly to obtain a mixed solution; (2) transferring the mixed solution into a reaction kettle, preserving heat for 10 to 12hours at 170 to 200 DEG C, and centrifuging, washing and drying a product to obtain the MoS2/transition metal/graphene composite hydrogen dissociation catalyst; (3) uniformly loading an electrode material with the MoS2/transition metal/graphene composite hydrogen dissociation catalyst to obtain the hydrogen dissociation electrode. According to the preparation method and the application of the MoS2/transition metal/graphene composite hydrogen dissociation electrode in the microbial electrolytic tank, a reaction system is uniform; the production cost is low; the MoS2/transition metal/graphene composite hydrogen dissociation electrode has good electrochemical performance, has a good catalytic hydrogen production effect, and can achieve double effects of treating pollution and producing energy.

The invention discloses a highly dispersed nano molybdenum disulfide catalyst synthetic method, homemade ammonium tetrathiomolybdate is used as a raw material, hydrazine hydrate is used as a reducing agent for solvent thermal direct preparation of a highly dispersed nano molybdenum disulfide catalyst by use of solvents of different viscosity in the solvent with special proportion, and the highly dispersed nano molybdenum disulfide catalyst has good dispersion in both organic and inorganic solvents. The molybdenum disulfide agglomeration can be inhibited by use of solvent viscosity in the solvent thermal synthetic process, so that molybdenum disulfide nanoparticles with good dispersion and uniform size can be produced. The highly dispersed nano molybdenum disulfide catalyst synthetic method has the advantages of being simple, low in cost, short in synthesis time and high in application value.

The invention discloses a method for preparing oil-soluble nano-molybdenum disulfide. The method comprises the following steps: uniformly mixing ammonium tetrathiomolybdate and oleylamine, continuously stirring in protection of inert gas, heating to 345-455 DEG C, and keeping for 1-2 hours; cooling to room temperature to obtain a black liquid, centrifugally collecting precipitates, and repeatedly washing with an organic solvent to obtain oil-soluble ultra-thin nano-molybdenum disulfide having a grain size of about 200nm. The nano-molybdenum disulfide prepared by the method is only formed by one layer or multiple layers of molecules, has an ultra-thin structure, and can be stably dispersed in a lubricant.

The invention relates to a high-density boundary double-layer molybdenum disulfide nano sheet and a preparation method thereof. The preparation method comprises the following steps: S1, placing a glass slide as a substrate into a hydrofluoric acid for soaking for 5-10 minutes, then cleaning and removing the silicate reaction product on the surface, and carrying out drying for later use; and S2, using a chemical vapor deposition method, using sublimated sulfur as a sulfur source, and molybdenum trioxide, molybdenum chloride and ammonium tathiomolybdate as molybdenym sources, and using a three-temperature-zone tube furnace to make molybdenum disulfide to grow on the substrate. The double-layer molybdenum disulfide nano sheet provided by the invention has uniform size, higher density boundary, and good conductivity and catalytic performance, and the preparation method is simple in operation, less in process flow and low in cost.

The invention relates to a preparation method of monodisperse spherical MoS2 ultrafine powder, comprising the following steps: 1) adding a tetrathio ammonium molybdate solution with the concentration of 0.01-0.05 mol/L in a reactor, adding an acid solution dropwisely with the molar ratio of tetrathio ammonium molybdate and acid being 1:0.8-1.5, stirring, reacting, curing, and then carrying out solid-liquid separation, cleaning the solids to obtain monodisperse MoS3 particles; and 2) heating the MoS3 particles obtained in the step 1) under the protection of inert gases, then letting in reducing gases for reacting, cooling to obtain the MoS2 ultrafine powder. According to the invention, (NH4)2MoS4 and the acid solution are used as the raw materials, liquid-phase deposit-hydrogen reduction method is adopted, thus the preparation of the monodisperse spherical MoS2 ultrafine powder is realized, the production conditions are mild, the device requirement is simple, the process flow is short, the utilization rate of raw materials is high, the energy consumption is low, no other impurity is introduced in the production process, the product quality is good, and the purity is high.

The present invention relates to improved preparation process of high purity chemical. High purity ammonium tetrathiomolybdate is prepared through the reaction between ammonium para-molybdate or molybdenum trioxide and ammonium sulfate solution. Preparing high purity ammonium tetrathiomolybdate in the said process of the present invention has ammonium sulfate amount near the required stoichiometric amount, mild reaction condition, short reaction period, less waste exhaust, high product yield, high product purity, and no need of treating virulent and effluvial hydrogen sulfide gas.

The invention relates to a hollow carbon sphere/molybdenum disulfide bipolar composite material and a preparation method and application thereof, and belongs to the technical field of materials. According to the hollow carbon sphere/molybdenum disulfide bipolar composite material, ammonium tetrathiomolybdate and hollow carbon spheres are used as raw materials, MoS2 nano-sheets are prepared througha hydrothermal method to be uniformly coated on the surface of the hollow carbon spheres, and the hollow structure is favorable for storage of the active substance sulfur and alleviating the volumetric expansion of sulfur during the electrochemical cycle process and also providing a place for reaction. Besides, polysulfides produced in the electrochemical process can also be adsorbed to reduce the loss of active substances. The hollow carbon sphere/molybdenum disulfide bipolar material is uniformly coated on the glass fiber to form a composite membrane; and the composite material is obtainedby injecting the active substance sulfur into the hollow structure of the hollow carbon sphere/molybdenum disulfide bipolar material and can be used as the positive electrode material of a room temperature sodium-sulfur battery to be applied to the room temperature sodium-sulfur battery so as to obtain good rate performance and stable cycle performance.

The invention discloses a graphene-like carbon nitride-based composite photocatalyst. The catalyst is a loaded catalyst, wherein the carrier of the catalyst is graphene-like carbon nitride; an activeload is ternary transition metal sulfide. The catalyst is prepared by performing a hydrothermal reaction on the graphene carbon nitride, ammonium tetrathiomolybdate and a copper-containing precursor.The catalyst has the advantages of higher visible light catalyzing performance, superior recycling performance, and a good application prospect in the fields of preparation of hydrogen by photocatalytic water splitting, synthesis of organic matters with photocatalysis, waste water treatment with photocatalysis and the like.

The invention relates to a preparation method for a hollow molybdenum disulfide/molybdenum trioxide flower-like spherical heterostructure nano material. The preparation method comprises the following steps: 1) dispersing ammonium tetrathiomolybdate, urea and hydrazine hydrate into N,N-dimethyl formamide so as to form a homogeneous solution; 2) transferring the solution obtained in the step 1) into a reaction kettle, and performing reaction for 8-10 hours at 160-240 DEG C; 3) after the reaction is completed, naturally cooling to the room temperature, performing solid-liquid separation, and washing and drying precipitate, thereby obtaining the hollow MoS2/MoO3 flower-like spherical heterostructure nano material. By adopting the hollow MoS2/MoO3 flower-like spherical heterostructure nano material provided by the invention, the hydrogen evolution(HER) performance of a catalyst is remarkably improved.

The invention relates to a molybdenum disulfide-coated lithium nickel cobalt manganate composite material, and a preparation method and an application thereof, wherein the composite material is composed of a core material and a coating layer; the core material is lithium nickel cobalt manganate, and the chemical formula of the core material is LiNixCoyMn1-x-yO2, wherein x is greater than or equalto 0, and y is less than or equal to 1; and the coating layer is MoS2. The preparation method comprises the following steps of adding ammonium tetrathiomolybdate into a solvent, and performing stirring at 40-80 DEG C, so as to obtain a dispersion liquid; and adding lithium nickel cobalt manganate into the dispersion liquid to obtain a mixed solution, performing continuous stirring until the solvent is dried, and drying the product in a vacuum drying oven, and carrying out sintering on the mixture in a protective atmosphere to obtain the molybdenum disulfide-coated lithium nickel cobalt manganate composite material. The method is simple in preparation process, simple and convenient to operate and high in element utilization rate. When the composite material is applied to a lithium ion battery, characteristics of high primary coulombic efficiency, stable cycle performance and excellent rate performance are shown.

The invention discloses a lithium-ion battery anode material molybdenum disulfide/carbon and a preparation method thereof. A dry tremella-like MoS2/C composite material is prepared by a thermal reduction method; a half-battery is prepared; the electrochemical property of the half-battery is tested; and the result shows that the half-battery is high in specific capacity and stable in cycle performance. The method is simple, reliable, good in process repeatability and high in operability, and can be widely popularized. The preparation method comprises the following steps: (1), taking a proper amount of ammonium tetrathiomolybdate, hexadecyl trimethyl ammonium bromide and silica nanospheres as raw materials; (2), preparing a sample by the thermal reduction method; and (3), removing silicon dioxide with hydrofluoric acid to obtain the required product.

The invention discloses a preparation method of three-dimensional foamed MoS2/graphene. With a mixed solution of ammonium tetrathiomolybdate and dimethyl formamide as a three-dimensional MoS2 reaction material solution, graphene is dipped and dyed and then is subjected to heat preservation in hydrogen and argon atmosphere of a tube furnace, so as to obtain the three-dimensional foamed MoS2/graphene. Compared with the traditional lithium ion battery anode composite material, the preparation method has obvious advantages that (a) the material loss in the preparation process is reduced, and the preparation method is easy to operate and industrially produce; and (b) the prepared three-dimensional foamed MoS2/graphene has the advantages of high specific capacity and high cycling stability.

The invention discloses an electrochemical preparation method of an MoS<2>/graphene composite counter electrode. A three-electrode electrochemical deposition system is adopted firstly, a graphene oxide/lithium perchlorate mixed aqueous solution is taken as an electrolyte, and a graphene oxide thin film is directly formed on FTO conductive glass in an electro-deposition manner and forms a graphene thin film through electrochemical reduction at the same time; and the graphene thin film is taken as a substrate then, MoS<2> is continue to formed in an ammonium tetrathiomolybdate/potassium chloride aqueous solution in an electro-deposition manner and an MoS<2>/graphene composite thin film is obtained. The MoS<2>/graphene composite thin film prepared through the method can be directly used as a counter electrode of a dye-sensitized solar cell, and any postprocessing procedure does not needed.

The invention discloses a method for preparing a composite material by embedding MoS2 nanosheets in a carbon substrate and an application of the composite material and belongs to the technical field of new materials. The method comprises the steps of by adopting an ammonium tetrathiomolybdate solution dissolved in dimethylformamide as a reaction precursor, putting in a self-made reaction device, sealing, putting in a heating furnace capable of introducing protective gas, heating to an appropriate temperature, decomposing the precursor into gas and generating high pressure to prepare the MoS2/Cnanocomposite material under high pressure. The MoS2/C nanocomposite material is composed of a microstructure formed by uniformly embedding the MoS2 nanosheets in the nitrogen-oxygen co-doped carbonsubstrate; and the MoS2/C nanocomposite material serves as a negative electrode material for lithium ion and sodium ion batteries. The method has the beneficial effects that the method is simple in process, abundant in raw materials and low in cost; when the MoS2/C nanocomposite material prepared by adopting the method serves as the negative electrode material for the lithium ion and sodium ion batteries, the cycle performance and the rate performance of the batteries can be improved; and therefore, the method is suitable for large-scale popularization and has a good application prospect.

The invention discloses a molybdenum disulfide/graphene composite material and a preparation method and application thereof, belonging to the field of electrochemistry and new energy material. The preparation method of the invention comprises the following steps: (1) preparing ammonium tetrathiomolybdate; (2) preparation of graphene slurry by electrochemical method; (3) surface modification of graphene; (4) Preparation of molybdenum disulfide/graphene composites. The process of the invention is simple and easy to operate, the condition is mild, the repeatability is high, the yield is high, andthe invention is suitable for batch production. The conductivity of MoS 2 was improved and the aggregation of MoS 2 and graphene was inhibited by the composites. When the composites were used as cathode materials for lithium ion batteries, they showed high specific capacity and excellent cycle stability. The first discharge specific capacity reaches 700-1200 mAh/g at 0.01- 3.0 V and 200 mA/g current density, and the discharge specific capacity maintains at 550 -850 mAh/g after 200 cycles. The results show that the first discharge specific capacity reaches 700-1200 mAh/g at 200 mA/g current density.