161 results about "Zirconium chloride" patented technology

The invention provides a synthetic method and application of a metal-organic framework (MOF) composite nanomaterial. The method comprises the following steps: dispersing ferriferrous oxide magnetic spheres which are synthesized through a traditional hydrothermal technology in a weakly alkaline solution of dopamine hydrochloride to carry out self-polymerization of dopamine on the surfaces of the magnetic spheres; and sequentially dispersing polydopamine coated magnetic spheres in a dimethylformamide solution of zirconium chloride and a dimethylformamide solution of 2-amino-terephthalic acid to obtain the MOF composite nanomaterial with the magnetic sphere surfaces coated with polydopamine and modified with an amino group and with zirconium as a center metal ion. The material has the advantages of large specific surface area, good hydrophilicity and suitable pore structure, can be applied to further researches of the proteomics, and can specifically enrich Which can specifically enrich phosphorylated peptide segments and glycopeptides; the synthetic method is simple and quick; and the synthesized material has good hydrophilicity and biocompatibility, and can be used for selectively enriching endogenous phosphorylation peptide segments and glycopeptide in complex biological samples.

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 a PCN (Porous Coordination Network) 222 metal organic framework material as well as a preparation method and application thereof. The preparation method comprises the following steps: mixing porphyrin, zirconium chloride and benzoic acid with N,N-dimethylformamide under the ultrasonic condition to obtain a mixed solution; carrying out hydrothermal reaction on the mixed solution, and carrying out ethanol washing, centrifuging and drying to obtain the PCN 222 metal organic framework material. The microtopography of the material is of a rod-like structure, and a crystal spindle is a hexahedron; the PCN 222 metal organic framework material has good thermal stability and can be used for enhancing the sensitiveness of a pesticide residue detection enzymatic inhibition method; the method disclosed by the invention has the advantages of simplicity, quickness and low cost and provides a practical tool for determining organophosphorus pesticide in a complex sample matrix.

The invention relates to a sponge composite metallic organic framework material for adsorption separation and belongs to the technical field of materials. According to the invention, a two-step in-situ growth method is adopted for loading MOFs (metallic organic framework material) into a duct in a sponge carrier. The MOFs is synthesized from following organic ligands and metal salts, wherein the organic ligands include pyrazine, trimesic acid, terephthalic acid, 2,5-dihydroxyterephthalic acid, and the metal salts include cupric fluosilicate, magnesium nitrate, zirconium chloride, cupric nitrate, chromic nitrate, ferric nitrate, aluminum nitrate and hydrates thereof. According to a preparation method provided by the invention, a large amount of MOFs loaded in the duct in the sponge carriercan be realized; MOFs load rate is high; load is stable; the defects of fragility and easiness in loss of MOFs powder can be overcome; a breakthrough experiment proves that the material provided by the invention has the characteristics of high CO2-absorbing capacity, high adsorption separation selectivity, stable adsorption separation property, and the like.

Provided is a method for preparing a nano anticancer probe of a zirconium-porphyrin metal organic framework material. Anhydrous zirconium chloride, meso-4-carboxyphenyl porphyrin, cetyl trimethyl ammonium bromide, benzoic acid and polyethylene glycol are added into N,N-dimethylformamide for ultrasonic dissolving, and an obtained mixed solution is subjected to a heating reaction till purple sediment is precipitated out at the bottom; after centrifugal separation, the sediment is washed with N,N-dimethylformamide, ethyl alcohol and water, and freeze drying is carried out to obtain a nano anticancer probe 1; chemotherapeutic medicine is dissolved in a 4-hydroxyethylpiperazine ethane sulfonic acid buffer solution, the nano anticancer probe 1 is added, centrifugal separation is carried out after stirring is carried out at normal temperature, washing is carried with a 4-hydroxyethylpiperazine ethane sulfonic acid buffer solution, freeze drying is carried out, and a nano anticancer probe 2 is obtained. The method has the advantages that the process is simple, and implementation is easy; the nano anticancer probe is used as an imaging induced synergic treatment system in the field of biomedicine, and meanwhile cancer is detected and treated.

The invention relates to a preparation method of a polycrystal zirconia fiber and zirconia/alumina composite fiber, which is characterized by comprising the following steps of: with zirconium carbonate and hydrochloric acid as raw materials and water or a mixture comprising water and alcohol as a solvent, preparing uniform and transparent polyhydroxy zirconium chloride sol under a refluxing state; adding a phase stabilizer, a grain growth inhibitor and a water-soluble polymer spinning aid to the sol and distilling at reduced pressure to prepare an inorganic zirconium spinning solution, or adding aluminum sol, the phase stabilizer, the crystal grain growth inhibitor and the water-soluble polymer spinning aid to the sol and distilling at reduced pressure to prepare an aluminum-zirconium composite spinning solution; and preparing gelatin fiber through centrifugal fiber throwing or blowing spinning, and carrying out heat treatment to obtain the polycrystal zirconia fiber and zirconia/alumina composite fiber. The preparation method disclosed by the invention has the advantages of low price of raw materials, simple equipment, low requirement on environment, no need of inertial environment, short flow time of the whole process and suitability for industrial production.

The invention provides a preparation method of an electrochemical sensor for detecting heavy metal ions. The preparation method includes the following steps: 1) performing carboxyl functionalization to multi-wall carbon nano-tubes and performing in-situ synthesis with zirconium chloride and 2-aminoterephthalatic acid to prepare an MWCNTs@UiO-66-NH2 composite material; 2) dispersing the MWCNTs@UiO-66-NH2 composite material in N,N-dimethylformamide to prepare a suspension liquid, drop-coating a surface of a glass carbon electrode with the suspension liquid until the surface of the glass carbon electrode is completely covered thereby, and drying the glass carbon electrode in a drying device at room temperature to prepare the MWCNTs@UiO-66-NH2 composite material electrochemical sensor. The electrochemical sensor can achieve ultrasensitive detection on a sample. By an analysis method in the invention, an accurate analytic result can be acquired.

The invention relates to a catalyst for norbornene, acrylate and pentene copolymerization, and a ternary copolymerization method. The catalyst is characterized in that the preparation method of the catalyst comprises the following steps: dissolving zirconium chloride (ZrCl4), a ligand and halogenated hydrocarbon in a first solvent in a dry single-port glass bottle in the inert gas atmosphere, sealing the bottle port of the glass bottle with a latex tube, carrying out constant temperature treatment in a 40-50DEG C water bath for 10-30min, and cooling to obtain the zirconium complex catalyst. Compared with catalysts in the prior art, the catalyst provided by the invention is a novel zirconium complex catalyst, can generate a catalysis activity in a nitrogen protection system at 40-120DEG C under a certain pressure, allows products to be easily washed and separated after immersion in methanol when the catalyst is used for catalyzing the ternary copolymerization of norbornene, acrylate and pentene monomers, and has the characteristics of high copolymer yield, low reaction temperature, low price, easy obtaining, high catalysis efficiency and the like.

The invention belongs to the field of wet metallurgy and the technical field of zirconium and hafnium separation, and in particular, relates to a process for separating zirconium and hafnium by a solvent extracting method. Industrial products containing hafnium zirconium chloride acetyl are used as raw materials for such procedures as water solution, alkali sinking, washing and nitric acid dissolving to prepare zirconium (hafnium) nitrate acetyl solution; TBP kerosene solution of adding phase modifying agent octanol is used as an extracting agent; most zirconium and less hafnium are extracted into an organic phase through multistage counter-current extraction by using the characteristic of TBP priority extraction of zirconium; the loaded organic phase is washed by nitric acid solution with a certain concentration to further remove most hafnium in the organic phase; the acid-washed loaded organic phase is reversely extracted by water to obtain zirconium nitrate acetyl solution; the solution is precipitated in ammonia, dried and calcined to obtain zirconium dioxide powder, and the mass of the zirconium dioxide powder accords with the atomic energy-level zirconium dioxide standard; less zirconium and most hafnium only remained in residual water phase of zirconium after reverse extraction are extracted; the content of zirconium in hafnium meets the requirements on impurity zirconium by atomic energy-level hafnium; and atomic energy-level hafnium can be directly prepared by enrichment.

The invention discloses a dopamine based UiO-66 membrane modifying method. The method includes: immersing a fixing frame for a porous substrate in a precursor solution configured by dissolving zirconium chloride and p-phthalic acid in N,N-dimethylamino-amine, and performing thermal treatment for 48-96 hours at the constant temperature; performing ultrasonic treatment for 3-30 seconds to obtain a substrate with seed crystal; performing thermal treatment for at least twice on the substrate deposited with the seed crystal till a continuous UiO-66 membrane is obtained; immersing the obtained membrane for twice to obtain a polydopamine grafted UiO-66 membrane, wherein the concentration of dopamine solutions for twice immersion is the same, the optical selection is in the range of 6.54-26.1mmol/L, and the immersing time is optimized in the range of 6-12 hours. The modifying method is simple, efficiency and easy to operate, and the modified UiO-66 membrane is greatly improved in selectivity and flux; the method has the advantages of environmental friendliness, energy conservation and the like in the production of MOF (metal-organic framework) membranes and application of gas separation membranes, and high prospect of industrial application in the trapping application of CO2 is achieved.

The invention discloses a preparing method for a mud stopping agent used for compound polycarboxylate superplasticizer. The preparing method includes the following steps that reaction monomer unsaturated alcohol or a derivative thereof, dimethyl diallyl ammonium chloride and water are selected and added into reaction equipment to prepare a reaction solution, or reaction monomer acrylamide or a derivative thereof, unsaturated alcohol or a derivative thereof, dimethyl diallyl ammonium chloride and water are selected and added into reaction equipment to prepare a reaction solution, the temperature of the reaction solution is adjusted to be 50 DEG C-60 DEG C, a copolymerization reaction is conducted for 3-4 h in a stirred mode under the action of an initiating agent, after the reaction is completed, the pH value of the reaction solution is adjusted by an alkaline solution to be 6-8, and then polymeric aluminum chloride or polymeric zirconium chloride is added for complexing to obtain the mud stopping agent used for the compound polycarboxylate superplasticizer. The problem that high-mud-content concrete is poor in usability is solved, and the prepared mud stopping agent is good in affinity with the polycarboxylate superplasticizer and can reduce the influence on the polycarboxylate superplasticizer by mud.

The invention discloses a preparation method and application of Fe3O4@SiO2@Zr-MOF. A synthesizing method of the magnetic hybrid MOF includes: under a hydrothermal condition, sealing Fe3O4@SiO2 particles and mixed solution, dissolved into DMF, of zirconium chloride and terephthalic acid into a 25ml reaction kettle, heating to certain temperature, keeping the temperature for 24 hours, cooling to room temperature, performing certain post-treatment, and circulating for three times to obtain the Fe3O4@SiO2@Zr-MOF. The Fe3O4@SiO2@Zr-MOF prepared by the method is good in magnetic response, good in stability, thick and adjustable in MOF layer, and the like, good absorption material can be obtained, and the Fe3O4@SiO2@Zr-MOF has application potential in organic dye absorption.

The invention discloses a process for preparing highly active aluminum zirconium tetrochlorohydrate glycine powder by forming aluminum chloride glycine and zirconium chloride glycine solution individually, and then blending such aluminum chloride glycine and zirconium chloride glycine together to form aluminum zirconium tetrochlorohydrate glycine.

The invention discloses a chromate-free metal composite tanning agent, comprising the following ingredients: 27.5-37.5 wt% of tetravalent zircon salt, 2.0-5.0 wt% of trivalent aluminium salt, 2.5-10.0 wt% of 15-45 wt% tetravalent titanium salt, 2.5-7.5 wt% of La-Ce mixed chlorinated rare earth, 0-2.5 wt% of antifreezing agent, and 55-60 wt% of water, wherein, the tetravalent zircon salt is selected from zirconium sulfate, zirconium nitrate or zirconium chloride, the trivalent aluminium salt is selected from aluminium sulfate, aluminium chloride, aluminum potassium sulfate or aluminium ammonium sulfate, the tetravalent titanium salt is selected from titanyl sulfate, titanium sulfate or ammonium titanyl sulfate complex salt, the antifreezing agent is glycol, and the water is deionized water. The invention also discloses a preparation method of the chrome-free metal composite tanning agent. The chrome-free metal composite tanning agent has the advantages of good comprehensive properties, simple production technology, and environmentally friendly; and the preparation method is simple without special devices.

The invention discloses a preparation method for 3-(trifluoromethyl)benzenepropanol. According to the method, in an inert solvent, 3-(trifluoromethyl)hydrocinnamic acid is reduced to generate 3-(trifluoromethyl)benzenepropanol under the presence of boron hydride as a reducing agent and Lewis acid as a cocatalyst. The inert solvent is composed of one or two components selected from methyl tert-butyl ether, isopropyl ether, methyl tetrahydrofuran and tetrahydrofuran. The molar ratio of boron hydride to 3-(trifluoromethyl)hydrocinnamic acid is 1:1 to 3:1. The boron hydride is in the form of sodium borohydride, potassium borohydride, lithium borohydride or zinc borohydride. The molar ratio of Lewis acid to 3-(trifluoromethyl)hydrocinnamic acid is 1:1 to 2:1. The Lewis acid is in the form of methanesulfonic acid, concentrated sulfuric acid, trifluoroacetic acid, zinc chloride, aluminium trichloride or zirconium chloride. The method is mild in reaction condition, simple in operation and post-treatment, and especially high in safety, thus being suitable for industrial mass production.

The invention belongs to the technical field of copper electrolyte treatment and discloses a method for removing lead ions in electrolytic copper foil electrolyte. In the production process of the electrolytic copper foil, the lead ion content in the electrolyte can be effectively reduced. The method takes zirconium chloride as a metal salt, terephthalic acid as an organic ligand, N, N-dimethyl formamide as an organic solvent, adopts a solvent method to prepare UiO-66, and loads UiO-66 on expanded graphite as a filling material of an adsorption column, wherein the adsorption column has good capability of removing lead ions in copper electrolyte, and the lead ion concentration in the electrolyte is reduced to less than 0.1Mug/ml after the electrolyte flows through the adsorption column. Dueto the reduction of the lead ion concentration in the electrolyte, the service time of titanium-based iridium-tantalum oxide coated anode is effectively prolonged.

The invention discloses an ultra-microporous zirconium-based metal organic framework material as well as a preparation method and application thereof. The method comprises the following steps: (1) respectively dissolving precursor zirconium chloride and alkaline N-pyrazine molecules in an organic solvent DMF (Dimethyl Formamide) according to a mass ratio of 100: (1.5-7.0), and carrying out ultrasonic dissolution to obtain a mixed solution; (2) transferring the mixed solution into a microwave reaction tank, and carrying out microwave reaction; (3) adding DMF (Dimethyl Formamide), acetic acid and precursor terephthalic acid with the same molar weight as zirconium chloride, and continuing to stir at room temperature to obtain a mixed solution; (4) transferring the mixed solution into a reaction kettle, putting the reaction kettle into a temperature programming box, and reacting at 120 DEG C; and (5) washing a product obtained after the reaction in the step (4) by using DMF and ethanol respectively, and centrifuging and drying the product. The zirconium-based MOFs material constructed by adopting a microwave-assisted strategy has relatively high specific surface area and relatively small pore size distribution, and meanwhile, the acidic sites of MOF metal sites are weakened, so that the CO2 adsorption capacity is remarkably improved due to the synergistic effect.

A process of preparing ZrW2O8 unit crystal, a kind of negative heating expanding material. Materials are ZrOCl2.8H2O(AR), N5H35W6O24.H2O(BR), HCl(AR). Prepare basic zirconium chloride and ammonia tungstate solution to equal molZr and molW. Then mix them. Volume ratio of basic zirconium chloride and ammonia tungstate solution is 1to 2. add HCl(6-12mol/L) to the mixture at 70-90deg.C. Volume of HCl is 1/3 of that of the mixture. Then put the mixture solution into reactor with polytetrafluoroethylene inside. Heat hermetically at 180deg.C , filter and dry at 60deg.C after reaction, ZrW2O8 is obtained after heating at 500-700deg.C in muffle wall.

An environmental friendly chromium-free insulating paint contains the following components: 100 parts by weight of metal dihydrogen phosphate; 10-200 parts by weight of one or more than one of vinyl acetate, acrylic acid, styrene-acrylic acid copolymer or phenolic resin; 1-40 parts by weight of one or more than one of zirconium acetate, zirconium nitrate, zirconium chloride, zirconium oxychloride, zirconium n-propoxide, and zirconium n-butoxid; and 200-500 parts by weight of pure water. The insulating coating obtained by the paint of the present invention exhibits good corrosion resistance, adhesiveness, and heat resistance; the invention successfully realizes the replacement of chromium compounds and therefore realizes the environmental protection of the production process; and the chromium-free insulating paint is applicable to non-oriented silicon steel.

The invention relates to a preparation method for high-purity nanometer-type poly-hydroxy zirconium chloride sol, which is characterized by comprising the following steps: (1) adding water into hydrochloric acid to prepare hydrochloric acid solution of which the concentration is 3-6mol/l, adding water into zirconium carbonate powder while stirring to prepare even suspension, and adding the filtered zirconium carbonate powder into the hydrochloric acid solution to be evenly stirred; (2) back flowing and hydrolyzing the mixture obtained in the step (1) at the temperature of 70-90DEG C until the zirconium carbonate is completely dissolved; (3) adding phase stabilizing agent of which the molar percentage by weight is 3-8% into the solution obtained in the step (2) by taking the mole number of zirconium oxide as a base number, and evenly stirring; and (4) carrying out reduced pressure distillation and dehydration on the mixed liquor obtained in the step (3) at the temperature of 60-80DEG C, and obtaining the poly-hydroxy zirconium chloride sol of which the concentration is 20-40% after filtering. The obtained sol has the advantages of high purity and good stability and is clear and transparent. On a modular level, the sol can be easily doped, and certain organic matters or inorganic matters are added according to the use requirement, so zirconium oxide products of different performances can be conveniently prepared.

The invention relates to an environmental-protection high-strength easy-dispersible nanometer zirconia material. A preparation method of the environmental-protection high-strength easy-dispersible nanometer zirconia material comprises following steps: a, a zirconium-containing solution is pepared; b, pretreated carbon nanotube is prepared; c, a zirconium dioxide matrix is prepared; and d, the zirconium dioxide matrix is subjected to heat treatment under nitrogen protection so as to obtain modified nanometer zirconia. According to the preparation method, zirconium chloride is taken as a raw material of nanometer zirconia, the modified carbon nanotube is added in preparation process, so that the stability of zirconia is improved obviously, and when the environmental-protection high-strengtheasy-dispersible nanometer zirconia material is used in ceramic preparation, relatively high mechanical strength and dimension stability are achieved.

The invention discloses a metal-organic framework material of Zr as well as a preparation method and application thereof, belonging to the technical field of crystalline materials. The chemical formula of the metal-organic framework material of Zr is [Zr6O4(OH)8(HCOO)2(BCPIA)2], and H4BCPIA is an organic ligand, namely 5-(2,6-bis(4-carboxyphenyl) pyridine-4-substituted) isophthalic acid. Under a closed condition, the organic ligand 5-(2,6-bis(4-carboxyphenyl) pyridine-4-substituted) isophthalic acid and zirconium chloride undergo a thermal reaction in N,N-dimethylformamide to obtain a metal-organic framework crystal; the metal-organic framework material has larger pore size and excellent fluorescence property, and can be used as a detection material for poly-o-chlorinated dibenzodioxin.

The invention discloses a bimetallic sulfide-based composite material, preparation of the nano composite catalytic material of which the ZnCdS nano microspheres and the organic framework material forma heterostructure and an application of the composite material in photocatalytic hydrogen production, and belongs to the technical fields of nanomaterial preparation and green energy sources. The composite material of the bimetallic sulfide nano microspheres and the metal organic framework (MOF) using Zr as a metal center is prepared by using a one-step hydrothermal method; and the method comprises the following steps: firstly performing a solvothermal reaction by utilizing zirconium chloride and terephthalic acid as raw materials to synthesize a square block shaped Zr metal organic frameworkmaterial (called UIO-66(Zr) for short), and further synthesizing the ZnCdS nano microsphere modified metal organic framework UIO-66(Zr) nano composite material by utilizing cadmium acetate and zinc acetate. The nano composite material provided by the invention has excellent catalytic activity in the photocatalytic hydrogen production.