140 results about "Zirconium(IV) chloride" patented technology

The invention discloses an adsorption-photocatalysis composite material synthesized on basis of in-situ synchronous assembly of UIO-66-NH2 and graphene (GR). The composite material is prepared by following steps: (1), weighing a certain amount of GR, dissolving the same in N, N-dimethyl formamide prepared in advance, and performing ultrasonic treatment to enable GR to be dissolved in a solution to obtain a solution A; (2), weighing a certain amount of 2-amino-terephthalic acid, dissolving the same in the solution A, ultrasonically treating, and stirring to obtain a solution B; (3), weighing a certain amount of a precursor, zirconium tetrachloride used for synthesizing MOF, dissolving the precursor in the solution B, ultrasonically treating, and stirring to obtain a solution C; (4), putting the solution C in microwaves for reaction for a period of time to obtain a product; (5), centrifuging and washing the product to obtain the composite material of UIO-66-NH2 and GR.

The invention discloses a method for synthesizing zirconium silicate powder in low temperature with a non-hydrolytic sol-gel method. Commercially pure non-aqueous zirconium chloride and orthosilicate ethyl ester are used as the raw materials of the precursor, LiF or MgF2 is the mineralizer and dichloromethane or ethanol is added in as the solvent. The precursor raw materials, the mineralizer and the solvent are prepared in proportion to form a precursor sol, which is back washed and dried to produce zirconium silicate dry gel which is further smashed and calcined to form the zirconium silicate powder at the low temperature of 700 to 850 degree. Compared with the current techniques, the invention is characterized in lower temperature for forming the zirconium silicate powder, simpler process, convenient operation and the using the commercially pure zirconium chloride as the raw material is more suitable for industrialization production.

The invention discloses preparation methods and application of a mercapto MOFs (Metal-Organic Frameworks) photocatalyst UiO-66(SH)2 and a series of noble metal mercapto MOFs photocatalysts M/UiO-66(SH)2 (M=Au, Pd and Pt). The UiO-66(SH)2 is prepared based on a pre-functionalization strategy by using zirconium tetrachloride and 2,5-dimercapto-1,4-terephthalic acid as precursors and combining with a solvent thermal synthesis method. By utilizing the metal affine effect of a mercapto functional group on a ligand skeleton, a noble metal ion is anchored on the UiO-66(SH)2, so that an M/UiO-66(SH)2 composite photocatalytic material is successfully prepared. In a loading process, an inert atmosphere, the addition of a strong reducing agent or a heat treatment process is not needed; highly dispersed Au, Pd and Pt ions can be loaded on a UiO-66(SH)2 material through a simple mixing process only. The UiO-66(SH)2 and the M/UiO-66(SH)2 both show favorable activity in an experiment of photocatalytically selectively oxidizing benzyl alcohol.

The invention discloses a preparation method of a high-coating-ratio zirconium silicate coated ceramic pigment. The preparation method includes the steps of: dispersing and wetting a to-be-coated substance in a zirconium tetrachloride ethanol solution to prepare a suspension liquid, and volatilizing the ethanol and drying the liquid, and performing a reaction with ammonia gas to form a zirconium hydroxide coating layer on the surface of the to-be-coated substance; mixing the to-be-coated substance with a silicon source solution, and performing gelatination/precipitation to form a silicic acid coating layer on the surface of the zirconium hydroxide coating layer; and drying the substance, mixing the substance with a mineralizing agent and calcining the substance to form the zirconium silicate coated ceramic pigment. The invention also discloses a product prepared through the method. In the invention, a core-shell structure with the to-be-coated substance as a core and the zirconium silicate as a coating layer is formed, so that the coating ratio and the coloring intensity of the coated substance are significantly increased. Meanwhile, applicability of the zirconium silicate as a coating layer material is developed, so that application and development of the zirconium silicate coating ceramic pigment are effectively promoted.

The invention provides an esterification method for synthesizing ethylene/propylene glycol ether carboxylate. A catalyst used in the method consists of an active substance and a carrier, wherein the active substance is tin salt (such as tin tetrachloride), titanium salt (such as titanium sulfate, titanium tetrachloride or titanium nitrate), zirconium salt (such as zirconium sulfate, zirconium tetrachloride or zirconium nitrate) or cerium salt (such as cerous sulfate, cerium tetrachloride or cerous nitrate); the carrier is silica gel, hydrogen-type ZSM-5, activated clay or diatomite; the content of the active substance in percentage by mass is 10 to 30 percent; and the content of the carrier in percentage by mass is 70 to 90 percent. The method has the advantages of inhibiting the occurrence of side reaction during production, improving the selectivity of target products, shortening production cycle, reducing investment in production equipment and avoiding the problems of production equipment corrosion, environmental pollution, high energy consumption and the like.

The invention discloses preparation and application methods of a solid acid catalyst based on Zr-MOF. The preparation method of the catalyst comprises the following steps: with zirconium tetrachlorideor zirconium oxychloride selected as a zirconium source, 1,4-terephthalic acid or biphenyl-4,4'-dicarboxylic acid as an organic ligand and DMF (N,N-dimethylformamide) as a solvent, a MOF (metal organic framework) material with network topology is synthesized with a solvothermal method, the solid acid catalyst based on zirconia is obtained by calcination in air atmosphere and acidification by strong acid. The catalyst has higher alkylation conversion rate, PXE (1-phenyl-1-xylylethane) yield and reusability at high temperature and under normal pressure.

The invention provides a preparation method of a lanthanum-doped metal organic framework material. The preparation method comprises the following steps: firstly, fully reacting zirconium tetrachloridewith terephthalic acid to generate a base framework material; preferably reacting lanthanum chloride heptahydrate with the terephthalic acid while avoiding the reaction of the lanthanum chloride heptahydrate and the base framework material. The invention provides the lanthanum-doped metal organic framework material and application thereof in adsorption of phosphate radical. The lanthanum-doped metal organic framework material has two adsorption sites of zirconium ions and lanthanum ions which can be used for well adsorbing the phosphate radical. The results of the embodiment show that the maximal adsorption capacity of the lanthanum-doped metal organic framework material to the phosphate radical is 348.43mg/g; in the presence of more heteroions, the recognition of the phosphate radical can be maintained; after repeated use for five times, the adsorption capacity of La-UIO-66 to the phosphate radical is also kept at 100 percent; the lanthanum-doped metal organic framework material hasexcellent stability and recycling performance.

The invention discloses a method for separating trace sulfamethoxazole enriched pollutants based on a molecularly imprinted polymer loaded with an ionic liquid metal organic framework, which comprisesthe following steps: ultrasonically dissolving 2-aminoterephthalic acid and zirconium tetrachloride in N, N-dimethylformamide for later use; adding ionic liquid brominated 1-allyl-3-vinyl imidazole and a template molecule sulfamethoxazole into an organic reagent to carry out a pre-polymerization reaction; and mixing the obtained solvents, adding a cross-linking agent ethylene glycol dimethacrylate and an initiator azodiisobutyronitrile, carrying out ultrasonic treatment, carrying out a hot solvent reaction under the protection of nitrogen, centrifuging the product, eluting, and drying to obtain the molecularly imprinted polymer. The molecularly imprinted polymer prepared in the invention has an ultra-large specific surface area and good physical stability and chemical stability, has strong selective recognition ability on sulfamethoxazole in the environment as a solid phase extraction adsorbent, has a fast mass transfer rate and a large adsorption capacity, and can be repeatedly used.

The invention discloses ferrocene-based ultrathin metal organic framework nano-sheets and a preparation method thereof, wherein the ferrocene-based ultrathin metal organic framework nano-sheets are prepared from an organic ligand 1,1'-ferrocene dicarboxylic acid, a metal salt zirconium tetrachloride and a modulating agent acid. According to the present invention, the preparation method is simple,the obtained ferrocene-based ultrathin metal organic framework nano-sheets have characteristics of porous structure and stable chemical property, and the thickness and the horizontal size of the obtained ferrocene-based ultrathin metal organic framework nano-sheets can be adjusted through the reaction conditions.

The invention provides a method for producing zirconium tetrachloride by carbochlorination and a method for producing zirconium sponge. The method for producing zirconium tetrachloride comprises the following steps: mixing 100 parts by weight of zircon sand with 26-45 parts by weight of carbonaceous reducing agent, and adding into a chlorination furnace; preheating a mixture to 1200-1500 DEG C; introducing chlorine at the temperature of 500-1100 DEG C, performing carbon-adding boiling chlorination reaction with the mixture, heating, and controlling the chlorination reaction temperature at 1050-1200 DEG C to obtain a reaction product. The method for producing zirconium sponge comprises the following steps: preparing the reaction product taking zirconium tetrachloride as a main component by using the method for producing zirconium tetrachloride; performing reduction treatment on the reaction product to obtain zirconium sponge. The methods provided by the invention have the beneficial effects of short process flow, low power consumption, low cost and continuous and stable reaction.

The invention discloses a preparation method and application of an organic phosphine grafted hollow metal organic framework material. The preparation method comprises the following steps: firstly, letting 2-aminoterephthalic acid react with zirconium tetrachloride to obtain a zirconium organic framework material with amino, then obtaining a hollow zirconium organic framework material through a metal-acid assisted etching method, and finally grafting organic phosphine DOPO through a Kabachnik-Fiels reaction. The synergistic effect among metal, hollow and organic phosphine in the organic phosphine grafted hollow zirconium metal organic framework material greatly enhances the flame retardancy and smoke suppression performance of the high polymer material; due to the existence of the organic ligand, the compatibility of a flame retardant and a polymer matrix is improved, and compared with other metal-based flame retardants, the flame-retardant polymer composite material has excellent flameretardancy and good mechanical properties.

The invention relates to the technical field of chemical processes and in particular discloses a method for producing zirconium tetrachloride. The method comprises the following steps: respectively crushing zircon sand, petroleum coke powder and a chemical auxiliary agent; fully mixing the zircon sand and petroleum coke powder according to a ratio, adding the mixture into a boiling chloridizing furnace, and introducing chlorine for carrying out a chlorination reaction; regulating the amount of the added chemical auxiliary agent by virtue of an automatic control system, so that the temperature of the boiling chloridizing furnace is always preserved to 1100 DEG C. The chemical auxiliary agent accounts for 15-30 percent of the total weight of the zircon sand and petroleum coke powder; the weight ratio of the zircon sand to petroleum coke powder is 10:(1-2.5); and the chemical auxiliary agent refers to metal silicon, silicon carbide or a mixture of metal silicon and silicon carbide. According to the method disclosed by the invention, the reaction temperature can be constantly controlled, the complicated operation of frequently stopping and replacing is avoided, the production efficiency is improved, and the production cost is reduced.

The invention relates to a UiO-66-NH2/TiO2/Ti3C2 composite photocatalyst with efficient hydrogen production and a preparation method thereof. The preparation method comprises the following steps: Ti3AlC2 is placed in a polytetrafluoroethylene inner liner, a hydrofluoric acid solution is added, and obtained Ti3C2Tx is annealed to obtain a TiO2/Ti3C2 compound; zirconium tetrachloride, N,N-dimethylformamide and hydrochloric acid are mixed to obtain a zirconium tetrachloride solution; the TiO2/Ti3C2 compound is added to the zirconium tetrachloride solution and stirred to obtain a Zr<4+>/TiO2/Ti3C2mixed solution; 2-aminoterephthalic acid and the N,N-dimethylformamide are mixed to obtain an organic ligand solution; and the organic ligand solution is added to the Zr<4+>/TiO2/Ti3C2 mixed solutionfor hydrothermal reaction to obtain the UiO-66-NH2/TiO2/Ti3C2 composite photocatalyst with efficient hydrogen production. The UiO-66-NH2/TiO2/Ti3C2 composite photocatalyst with efficient hydrogen production and the preparation method thereof have simple process and strong operability, and the prepared product can significantly improve the separation of photogenerated electrons-hole pairs in the photocatalytic process, and has excellent visible light decomposition water hydrogen production performance.

The invention relates to the field of zirconium oxychloride production devices, in particular to a device and a method for producing zirconium oxychloride with a boiling chlorination process. The device comprises a chlorination furnace, a multi-stage cooling device and a tail gas treatment device, wherein the chlorination furnace, the multi-stage cooling device and the tail gas treatment device are connected through a pipe from left to right sequentially; the chlorination furnace is used for boiling chlorination reaction; the multi-stage cooling device is used for separating high-purity zirconium tetrachloride, silicon tetrachloride and titanium tetrachloride; the tail gas treatment device is used for treating tail gas. The invention aims to provide the device and the method for producing zirconium oxychloride with the boiling chlorination process. to solve the problems that an existing device and method for producing zirconium oxychloride with the boiling chlorination process are low in production efficiency and poor in product quality and pollute the environment easily.

The invention provides a method for preparing ultrapure zirconium oxychloride and a byproduct silicon tetrachloride through zircon sand boiling chlorination, belonging to preparation methods of halides of zirconium. A device comprises a zircon sand boiling chlorination system, a zirconium tetrachloride condensing and collecting system, a silicon tetrachloride rectifying system and a system for preparing high-purity zirconium oxychloride through silicon tetrachloride hydrolysis. The device is characterized by also comprising a tail gas recovery system, wherein the tail gas recovery system comprises a tail gas storage device, a chlorine separation and recovery device and a CO recovery and storage device. The method is characterized by firstly separating and collecting chlorine in the tail gas, using chlorine as the raw material of zircon sand boiling chlorination reaction and recycling chlorine; and utilizing the tail gas after chlorine is separated as the raw material of an industrial production device involved synthetic reaction in which CO participates. The method for preparing ultrapure zirconium oxychloride and the byproduct silicon tetrachloride through zircon sand boiling chlorination can achieve the effects of effectively utilizing Cl2 and CO resources, reducing emission of the greenhouse gas CO2, reducing the product production cost of a zircon sand boiling chlorination device and improving the production capacity of the device.

The invention relates to a method used for preparing higher aliphatic phthalates via ester exchange. According to the method, lower aliphatic phthalates such as dimethyl phthalate, diethyl ester, and dibutyl ester, and high alcohols such as isononyl alcohol, isodecanol, and 2-propyI-1-heptanol are taken as raw materials, one or a mixture of more than one ingredient selected from titanium potassium oxalate, aluminium titanate, potassium titanate, magnesium titanate, calcium titanate, zirconium titanite, barium titanate, aluminium trichloride, antimony trichloride, titanium tetrachloride, zirconium tetrachloride, titanium methoxide, tetra(2-propyl heptanol)titanium, tetra isononanol titamium, and tetra isodecanol titamium is taken as a catalyst; reaction is carried out for 2 to 6h at 160 to 200 DEG C; and the highest lower aliphatic phthalate conversion rate and the highest higher aliphatic phthalate selectivity are higher than 99%. The production process is clean; energy is saved; raw material storage and transportation stability is high; feeding is convenient; catalyst corrosivity is less; reaction conditions are mild; less side effect is caused; and raw material consumption is low.