141 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 relates to the field of chemical production, and discloses a method for cooling zirconium tetrachloride produced through a fluidizing chlorination method. The cooling method comprises the following steps: fully mixing zircon sand / zirconium dioxide / a mixture of zircon sand and zirconium dioxide with petroleum coke powder according to a certain ratio, adding the mixture into a fluidizing chlorination furnace, introducing chlorine gas into the furnace to carry out chlorination reactions; introducing the gas generated in the chlorination reactions into a reaction gas cooling channel from the outlet of the fluidizing chlorination furnace, spraying liquid coolant into the reaction gas cooling channel to cool the reaction gas; then introducing the cooled reaction gas into a zirconium tetrachloride collecting tank, at the same time, and spraying liquid coolant into the zirconium tetrachloride collecting tank from top part or lateral side of the zirconium tetrachloride collecting tank so as to cool the reaction gas, wherein zirconium tetrachloride in a gas state is cooled and converted into zirconium tetrachloride powder, and the powder falls on the bottom of the zirconium tetrachloride collecting tank. According to the cooling method, liquid coolant is sprayed to the reaction gas so as to cool the reaction gas, the cooling effect is improved, the yield of zirconium tetrachloride is increased, and the production cost is reduced.

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 relates to a preparation method of a heterogeneous catalyst of organic coordination compounds of mesoporous structure metals, belonging to a preparation method of heterogeneous catalysts. Theterogeneous catalyst prepared by the prior art has the defects that the utilization ratio of surface active composition is limited, the direction of catalytic reaction can not be controlled easily, and the activity and the selectivity can not reach the optimal effect. In the invention, the preparation method of the heterogeneous catalyst of organic coordination compounds of mesoporous structure metals comprises the following steps of: mixing zirconium tetrachloride, 1,4-terephthalic acid and N,N-dimethylformamide solvent under the condition of microwaves, and stirring the mixture at room temperature until the solution is clear; adding the solution into a microwave reactor for microwave heating, removing the supernatant solution, and washing the residual solid matters with the N,N-dimethylformamide solvent; and drying the washed matters in a vacuum mode to obtain the heterogeneous catalyst. The invention has the advantages of simple process and easy operation; the prepared heterogeneous catalyst has efficient catalytic activity; and the catalyst can be recycled, thereby reducing the production cost and decreasing the environment pollution.

The invention relates to a Keggin type phosphotungstic acid composited zirconium-based MOF (metal-organic framework) photocatalyst and a preparation method thereof. The technical scheme is that the preparation method comprises the following steps: zirconium tetrachloride, N,N-dimethylformamide and hydrochloric acid are mixed and ultrasonically dissolved, and a zirconium tetrachloride mixed solution is obtained; 2-aminoterephthalic acid is dissolved in N,N-dimethylformamide, and an organic ligand solution is obtained; the zirconium tetrachloride mixed solution and the organic ligand solution are mixed and stirred, a precursor solution of a zirconium-based MOF compound is obtained, then Keggin type phosphotungstic acid is added and stirred, and a precursor solution of the Keggin type phosphotungstic acid composited zirconium-based MOF photocatalyst is obtained; the precursor solution is transferred into a reactor and subjected to a hydrothermal reaction, then centrifugation, washing anddrying are performed, and the Keggin type phosphotungstic acid composited zirconium-based MOF photocatalyst is obtained. The process is simple, operability is high, and the product can improve separation of photo-generated electron-hole pairs in a photocatalysis process and has excellent visible-light-based water splitting for hydrogen production.

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 an Mg-Gd-Y-Zr magnesium alloy refining flux and a production method thereof. The chemical components of the flux are mixed according to the following mass percentages: potassium chloride of ranging from 30 to 50 percent, barium chloride of ranging from 5 to 20 percent, sodium chloride of ranging from 2 to 10 percent, calcium chloride of ranging from 10 to 20 percent, calcium fluoride of ranging from 2 to 8 percent, cryolite of ranging from 1 to 5 percent, gadolinium compound of ranging from 3 to 8 percent, yttrium compound of ranging from 3 to 8 percent, and zirconium compound of ranging from 2 to 8 percent, wherein, the gadolinium compound is gadolinium chloride, gadolinium carbonate or gadolinium fluoride, the yttrium compound is yttrium chloride, yttrium carbonate or yttrium fluoride, the zirconium compound is zirconium tetrachloride or potassium zirconium fluoride. The flux has good melting point, viscosity, wettability and the slag removing performance which is improved greatly. Because the flux does not contain magnesium chloride or react with the lanthanon such as gadolinium and yttrium, the chemical reaction loss of the lanthanon in the refining process is not caused, thereby being particularly suitable for the refining purifying process of the Mg-Gd-Y-Zr magnesium alloy and improving the refining effect of the magnesium fused mass.

The chemical formula of a modified organic metal framework used for efficiently adsorbing elemental mercury in flue gas is Zr6O4(OH)4[C6H2M2(CO2)2]6 or Zr6O4(OH)4[C6H3M(CO2)2]6, wherein M is Br or Cl or I. A preparation method includes the steps that zirconium tetrachloride serves as an MOF metal center, terephthalic acid series ligands provided with a mercury affine substituent group serve as active organic ligands, and a mercury affine active MOF series is synthesized; the modified organic metal framework can be used for efficiently removing elemental mercury in the flue gas. The modified organic metal framework has the advantages that 2-chlorine terephthalic acid with mercury affine functional group and the other three organic ligands are adopted for synthesizing an active MOP series, a mercury static adsorption experiment represents that the demercuration efficiency of active MOF elemental mercury is larger than 90%. By means of the modified organic metal framework, the efficient and high-amount elementary mercury adsorption characteristic is given, and the modified organic metal framework is a flue gas demercuration adsorption material with good application prospects.

The invention relates to a synthetic method of tetra(dimethylamino)zirconium, which comprises the following steps: 1)under argon atmosphere, adding dimethylamine and hexane in a three-necked bottle according to a proportion that 100-300 milliliters n-hexane is added in 100g dimethylamine, uniformly stirring, and placing the reaction bottle between the temperature of -20--60 DEG C, adding a n-butyllithium solution drop by drop in the reaction bottle, stirring after dropping, and reacting for 10 hours; 2)adding zirconium tetrachloride in the above reaction system, keeping the temperature of the reaction system between -20-0 DEG C, after adding zirconium tetrachloride, stirring the reaction system under the protection of inert gas to react for 24-30 hours; and 3)after the reaction is finished, removing a solvent of the reaction under one atmospheric pressure, after solvent n-hexane is completely removed, performing underpressure distillation, and collecting the fraction at 110-112 DEG C / 4mmHg which is the tetra(dimethylamino)zirconium compound. According to the invention, the reaction employs the raw material dimethylamino lithium and hafnium tetrachloride which are simple and easy to obtain, the operation is simple, and the cost is reduced.

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 relates to a Pd / UiO-66 catalyst having a morphology-controllable Pd metal nanocrystal core and a preparation method and application thereof. The preparation method of the Pd / UiO-66 catalyst comprises S1: dissolving terephthalic acid in dimethyl formamide to obtain a solution A, dissolving a palladium salt in dimethyl formamide to obtain a solution B and dissolving zirconium tetrachloride in dimethyl formamide to obtain a solution C for next use, S2: mixing the solutions A and B, carrying out stirring, mixing the mixture and the solution C and adding a small molecule acid into themixed solution, S3: sealing the mixed solution obtained by the step S2, carrying out heating along with stirring for 20-26h, after the reaction, carrying out centrifugation on the mixed solution andwashing and drying the centrifugal product to obtain the Pd / UiO-66 catalyst having a morphology-controllable Pd metal nanocrystal core. The Pd / UiO-66 catalyst obtained by the one step method has controllable Pd nanocrystal morphology and the morphology-controllable Pd nanoparticle is spherical or tetrahedral. The Pd / UiO-66 catalyst has a good UiO-66 crystalline state and a high specific surface area.

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 relates to a preparation method of a particle size adjustable mesoporous metal organic framework nanomaterial, which comprises the steps of dissolving zirconium tetrachloride and monoacid in a solvent, adding a dicarboxylic acid ligand and organic base for reaction to form a mesoporous metal organic framework precursor, taking a zirconia cluster provided by zirconium tetrachloride asa node, allowing monoacid and the dicarboxylic acid ligand to perform competition coordination with zirconium tetrachloride to form the zirconia cluster, allowing the dicarboxylic acid ligand to be coordinated with zirconium tetrachloride to serve as a connector of a metal organic framework, inserting monoacid into hole channels of the metal organic framework via a coordination bond, dispersing the mesoporous metal organic framework precursor in a mixed solution of the solvent and inorganic acid to remove monoacid to form the particle size adjustable mesoporous metal organic framework nanomaterial, wherein inorganic acid damages the coordination bond between monoacid and zirconium tetrachloride. The preparation method is simple in technology and good in reproducibility; the prepared mesoporous metal organic framework nanomaterial is adjustable in particle size, uniform in dimension and good in dispersity.

The invention relates to a preparation method and application of a metal organic framework material, and belongs to the technical field of crystalline materials. Under the condition that the temperature is not higher than 40 DEG C, zirconium tetrachloride, hafnium tetrachloride and 2-amino terephthalic acid are dissolved in a mixed organic phase to obtain a mixed solution A, wherein the mixed organic phase is an organic mixture of N,N-dimethylformamide and acetic acid; at the temperature of 100-120 DEG C, the mixed solution A reacts for 12-24 h under the stirring condition, the product is filtered, washed with N,N-dimethyl formamide and subjected to vacuum drying, and then the metal organic framework material is obtained. The metal organic framework material prepared through the method can be used for adsorbing carbon dioxide (CO2) and has the advantages of being high in adsorption rate and capable of being 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 discloses a method for preparing a catalyst Cu-UiO-66 for preparing methanol from a synthesis gas, wherein Cu(NO3)2.3H2O, trimesic acid, sodium carboxymethyl cellulose, ammonium chloride, 2-amino terephthalic acid, zirconium tetrachloride and terephthalaldehyde are taken as the main raw materials, Schiff base organic modified UiO-66 is taken as a seed crystal, a hydrolysate of the sodium carboxymethyl cellulose and the trimesic acid are induced under the condition of ultrasonic treatment to have a coordination reaction with Cu<2+>, the crystallization time is greatly shortened, and the metal organic catalyst is rapidly prepared. The prepared organic modified metal catalyst Cu-UiO-66 has the advantages of high selectivity and fast kinetic equilibrium, and no secondary pollution in the technical process, and the catalyst is higher in stability and catalytic activity in the reaction for preparing methanol from synthesis gas.

The invention discloses a separation method of zirconium tetrachloride synthesis gas. The zirconium tetrachloride synthesis gas is prepared from zirconium tetrachloride by a chlorination method. The method comprises the following steps of (1) lowering the temperature of the zirconium tetrachloride synthesis gas to 150 to 180 DEG C; separating out first coarse zirconium tetrachloride to obtain first synthesis gas; (2) lowering the temperature of the first synthesis gas to 80 to 120 DEG C; separating out second coarse zirconium tetrachloride to obtain second synthesis gas. The separation methodand device of zirconium tetrachloride synthesis gas provided by the method have the advantages that according to the method, the first coarse zirconium tetrachloride and the second coarse zirconium tetrachloride are respectively cooled and separated through stepped temperature reduction; the first coarse zirconium tetrachloride and the second coarse zirconium tetrachloride can be respectively usedas a coarse product to be used; the temperature used for separating out the first coarse zirconium tetrachloride through temperature reduction is lower; most zirconium tetrachloride in the zirconiumtetrachloride synthesis gasis separated out; the cold quantity is greatly saved; the separation cost of the zirconium tetrachloride synthesis gas is reduced.

A stable aluminum-zirconium aqueous solution of enhanced efficacy having a high concentration free of amino acid and polyhydric alcohol is disclosed. Such aluminum-zirconium salts are selected from aluminum / zirconium tetrachlorohydrate; aluminum / zirconium pentachlorohydrate, and aluminum / zirconium octachlorohydrate in which the aluminum to zirconium (Al / Zr) atomic ratio of said salt falls within the limits of the shaded areas A, B, and C, respectively, of the drawing graph wherein the aluminum / zirconium tetrachlorohydrate has an Al / Zr atomic ratio from about 2 to about 6 and metal / chloride molecular ratio about 0.9 to about 1.25; aluminum / zirconium pentachlorohydrate having Al / Zr atomic ratio from about 6 to about 10 and metal / chloride atomic ratio from about 1.5 to about 1.65; and aluminum / zirconium octachlorohydrate having Al / Zr molecular ratio from about 6 to about 10 and metal / chloride molecular ratio from about 0.9 to about 1.5.

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.

The present invention relates to a magnesium alloy zirconium compound silicon-removnig flux and its production method. Its composition includes (wt%) 30-45% of aqueous magnesium chloride; 15-25% of potassium chloride, 5-12% of barium chloride, 10-17% of calcium fluoride, 10-25% of magnesium fluoride, 3-8% of sodium fluoride and 2-8% of zirconium tetrachloride and / or potassium fluorozirconide. It includes the following steps: firstly, heating crucible, adding potassium chloride and barium chloride, heating and melting part of them, adding calcium fluoride, magnesium fluoride and sodium fluoride, heating to 750-790 deg.C, uniformly stirring them, pouring to obtain block, breaking it and placing it into ball-grinding machine, more adding magnesium chloride, zirconium tetrachloride and / or potassium fluorozirconide, grinding them.

The invention relates to a preparation method of tris(dimethylamino) cyclopentadienyl zirconium. The preparation method comprises the following steps: 1) lithium dimethylamide preparation: adding an n-hexane solution of n-butyllithium in a reactor, and under stirring starting and inert atmosphere protection, introducing dimethylamine gas to prepare lithium dimethylamide; 2) tetrakis(dimethylamino)zirconium preparation: under stirring starting and inert atmosphere protection, adding zirconium tetrachloride in a lithium dimethylamide solution; 3) cyclopentadienyl monomer preparation with dicyclopentadiene: adding dicyclopentadiene in the reactor, and distilling out a cyclopentadienyl monomer under the condition with the temperature higher than 160 DEG C; 4) dropwise adding the cyclopentadienyl monomer in the tetrakis(dimethylamino)zirconium, and carrying out reaction to produce tris(dimethylamino) cyclopentadienyl zirconium; and 5) distilling the tris(dimethylamino)cyclopentadienyl zirconium. According to the preparation method, the tris(dimethylamino)cyclopentadienyl zirconium is synthesized by a one-pot method, the reaction raw materials are simple and available, and reaction operation is simple; and cyclotentadienyl sodium does not need to be synthesized firstly, and separation of an intermediate is not needed.