146results about "Preparation of aldehyde/ketone chelates" patented technology

The invention provides a method for preparing acetylacetone metallic compound, comprising soluble metal salt solution and aqueous alkali are quickly mixed together through a full back-mixing liquid membrane reactor to prepare precipitation grout of hydroxide with nanometer level, the precipitation of hydroxide is not needed to be separated and directly added with acetylacetone to react at the normal temperature to obtain the acetylacetone metallic compound. The method adopts the full back-mixing liquid membrane reactor to synthesize hydroxide with nanometer level, thus shortening the reaction time between the hydroxide and the acetylacetone and improving the preparation efficiency; meanwhile, by controlling the adding quantity of alkali and the acetylacetone in the crystal-transformation process, the reaction yield is greatly improved. The preparation method is simple in technique, convenient in operation and short in reaction time, and the obtained product has the yield being more than 95%.

This invention provides a method for preparing Pd acetylacetone, which solves dissoluble K-salt or Na-salt and Pd salt in deionized water under warm temperature then converts the Pd salt into Pd(OH)2 under the action of alkali then to add acetylacetone in a reaction mixture with Pd(OH)2, in which, since neutralization reaction occurs to the alpha active H atoms in the molecules and Pd(OH)2, Pd acetylacetone products are got.

The invention discloses a method for preparing 2,2,6,6-tetramethyl-3,5-heptanedione, which comprises the process of using alkyl pivalate as a solvent without using other solvents Alkyl pivalate and pinacolone are reacted in the presence of an alkali metal alkoxide catalyst, or they are reacted in an amide type solvent or a urea type solvent in the presence of an alkali metal alkoxide catalyst. Also disclosed is a method for preparing 2,2,6,6-tetramethyl-3,5-heptanedione metal using 2,2,6,6-tetramethyl-3,5-heptanedione complex method. The method for preparing 2,2,6,6-tetramethyl-3,5-heptanedione is an industrialized method, wherein alkali metal alkoxides are easy to handle and can be used as Catalyst for the preparation of 2,2,6,6-tetramethyl-3,5-heptanedione from esters and pinacolones.

The invention discloses a nitride high-entropy ceramic fiber and a preparation method and application thereof. The high-entropy ceramic fiber contains Ti, Hf, Ta, Nb and Mo elements, the nitride high-entropy ceramic fiber is in a single crystalline phase, and all the elements are uniformly distributed in a molecular level. The preparation method of the high-entropy ceramic fiber comprises the following steps: uniformly mixing a carbide high-entropy ceramic precursor containing a target metal element, a spinning aid and a solvent to prepare a precursor spinning solution, and then carrying out spinning, degumming and nitriding processes to prepare the nitride high-entropy ceramic fiber. The nitride high-entropy ceramic fiber can be applied to a process for preparing methane by photocatalysisof carbon dioxide.

The invention relates to a continuous synthesis method and a synthesis device for an acetylacetone metallic compound. The method comprises the following steps of: adding a metallic compound and acetylacetone into a reactor; adding the acetylacetone into a product collector; uninterruptedly distilling the acetylacetone in the product collector into the reactor in the heating process, and reacting the distilled acetylacetone with the metallic compound; when a liquid level in the reactor is higher than a siphon, siphoning liquid comprising the acetylacetone metallic compound generated during reaction in the reactor into the product collector to separate a product from a reactant; distilling the acetylacetone which is not reacted in a product separator into the reactor, and continuously reacting the acetylacetone with the metallic compound; and reacting and refluxing for a certain period of time, stopping heating, cooling a solution in the product collector, precipitating, filtering, drying, and thus obtaining the product. The method has a simple process and universality, is high in product yield and is environment-friendly.

The present invention relates to a method for producing aluminium acetylacetonate. Said method includes the following steps: firstly, adding isopropanol and acetone into a reactor, heating to 50-60deg.C, then slowly drop-adding pure aluminium powder, controlling temperature below 80deg.C until the reaction is completed, making back flow for 30 plus on minus 10 min; then drop-adding acetylacetone in the reactor, controlling temperature below 80deg.C until the drop-adding procedure is completed, further heating to 100 plus or minus 10deg.C,5 refluxing for 30-50 min, cooling to 40 plus or minus 5deg.C, discharging material, centrifugalizing, filtering and drying so as to obtain the invented product.

[PROBLEMS] To provide a metal complex compound capable of being suitably used for manufacturing a metal-containing thin film by the CVD method and a method for preparing a metal-containing thin film.

[MEANS FOR SOLVING PROBLEMS] A metal complex compound comprising a β-diketonato ligand having an alkoxyalkyl-methyl group, and a method for preparing a metal-containing thin film using the metal complex compound by the CVD method.

An alkaline earth metal salt of beta-diketo compound is produced using 1 mol of a powdery alkaline earth metal compound and 2.04 mol or more of an aliphatic beta-diketo compound. The reaction may be carried out while supplying both components to a reactor continuously or intermittently, or may be carried out by adding one component to the other continuously or intermittently. The highest temperature during the reaction may be at 50° C. or higher. The reaction mixture may be aged, and then dried at a temperature of at 100 to 180° C. in an atmosphere of an inert gas. The alkaline earth metal compound may be calcium hydroxide, magnesium hydroxide, or barium hydroxide. The aliphatic beta-diketo compound may be represented by the following formula, particularly an acetoacetic acid ester or acetylacetone.According to the production method as mentioned above, highly stable alkaline earth metal salts of beta-diketo compounds of high quality can be produced.

The invention relates to chelate type ionic liquid prepared by using coordinating capacity of beta-diketone anions. The chelate type ionic liquid is prepared by combining different cations and different anions. The cations may be quaternary amine, quaternary phosphorus, alkyl pyridine, alkyl iminazole or the like, the anions may be different alkyls, fluorinated alkyl, phenyl or furyl substituted beta-diketone complex ions and the metal may be Cu, Ni, Co, Mn, Cr, Zn or Fe. The preparation process of the chelate type ionic liquid is simple, quick, and low in energy consumption, does not require any strict conditions and makes product purification easy; and the chelate type ionic liquid has high chemical stability and high thermodynamic stability, and the melting point is easy to regulate. The ionic liquid enriches the ionic liquid range greatly and has high potential use value.

The invention belongs to the field of fine chemistry industry, and in particular relates to a method for preparing cupric acetylacetonate using cupric oxide powder to synthesize with acetylacetone, characterized in that water is used as solvent, and protonic acid is used as a catalyst and protonic base is used for regulating the acidity; the protonic acid is one of hydrochloric acid, sulphuric acid and phosphorous acid, and the protonic base is one of sodium hydroxide, potassium hydroxide and ammonia water. Compared with the prior art, the method has the by-products of trace soluble inorganic salts and simple production process, the product of cupric acetylacetonate with high purity can be obtained without special purification, and the yield is greater than 95 percent; using water as the solvent eliminates pollution from organic solvent; the mol ratio of reactant of cupric oxide to acetylacetone is 1.0:2.0 to 1.0:2.4, with low usage of acetylacetone, low production cost and high benefit.

The invention provides a preparation process of zinc acetylacetonate. The process includes: adding acetylacetone and zinc oxide into a reactor mixedly, conducting stirring heating to 110DEG C-140DEG C, and adding a certain amount of catalyst for reaction for 30min, thus obtaining the target product zinc acetylacetonate. The whole technological process is simple and efficient, and is easy to operate, not only saves the production cost, but also greatly improves the production efficiency, and is in line with the requirements of green chemistry. Proven by IR and DSC tests, the product obtained bythe technological conditions provided by the invention has the characteristics of few by-product and high purity. The static thermal stability of the product is superior to that of similar products.

The invention discloses a preparation method for high-brightness calcium acetylacetonate for PVC (Polyvinyl Chloride) heat stabilizer. A report about the preparation of high-brightness calcium acetylacetonate is not provided at present. The preparation method comprises the following steps of: oxidizing divalent iron ion and divalent manganese iron in a calcium chloride aqueous solution into trivalent iron ion and tetravalent manganese by oxidant, respectively; adjusting the pH value of the solution, so that iron and manganese are separated from the liquid phase in the forms of ferric hydroxide precipitates and hydrated manganese dioxide precipitates; filtering the solution to obtain calcium chloride solution free of iron and manganese impurities after the solution is treated by an adsorbent; preparing calcium chloride into calcium hydroxide by a conventional method; and enabling calcium chloride and acetylacetone to react to generate high-brightness calcium acetylacetonate. The preparation method disclosed by the invention is low in cost, good in quality and high in cost performance; and the obtained high-brightness calcium acetylacetonate is compounded with other additives to form the PVC heat stabilizer, so that the PVC product has good initial brightness during the processing process.

The invention relates to a preparation method of a beta-diketone tine (IV) compound, in particular to a method for preparing the beta-diketone tine (IV) compound by using a tin (II) compound. The method is used for preparing the beta-diketone tine (IV) compound by adopting the reaction of the tin (II) compound and beta-diketone. The beta-diketone tine (IV) compound prepared in the method has the advantages of easy obtainment of raw materials, low cost, simple operation of the preparation method, reclamation of mother liquid, no environmental pollution, high yield and purity of the production and suitability for industrial production.

The present invention provides a method to effectively inhibit the oxidization of VO(acac)₂ in solution for months. It is believed that VO(acac)₂ forms a π-complex with as many as three allylic alcohols which precludes reaction with any oxygen in the system. Although saturated and homo-allylic alcohols were also tested, this effect appears only in the allylic-alcohol based solutions. This ability to inhibit oxidation of VO(acac)₂ allows these solutions to be used for making thermochromic VO₂ film much more easily and economically as it avoids the requirement of operating under low oxygen level conditions. Thus the present invention provides a method of stabilizing vanadium oxyacetylacetonate (VO(acac)₂) in solution against oxidation for extended periods of time, comprising the steps of mixing the oxyacetylacetonate precursor in an allylic alcohol prior to spin-coating for VO₂ film formation. The allylic alcohol may be (β-methallyl alcohol. Alternatively, the allylic alcohol may be any one of 4-buten-2-ol, 2-buten-1-ol, 1-penten-3-ol, 2-hexen-1-ol and 1-hexen-3-ol.

The present invention discloses a preparation method for palladium acetylacetonate. The preparation method comprises: adding high purity metal palladium or sponge palladium to a container; adding concentrated nitric acid and hydrogen peroxide; heating and dissolving; cooling to a room temperature; adding a strong alkali solution to adjust the pH value to 8-11; and adding excess acetylacetone to obtain the product palladium acetylacetonate. Compared with the preparation method in the prior art, the preparation method of the present invention has the following characteristics that: a palladium salt compound is not required to be adopted as a starting material so as to substantially reduce cost; when the high purity metal palladium or the sponge palladium is adopted as a starting material, concentrated nitric acid and hydrogen peroxide are added during the dissolution process to generate pernitric acid so as to enhance dissolution on palladium, accelerate reaction speed, reduce a use amount of hydrogen peroxide, and improve product yield and purity. In addition, the method of the present invention has characteristics of mild process conditions, simple steps and the like.

The present invention relates to beta-diketone cerium (IV) compound represented by a formula (I), wherein R1, R2 and R3 are defined in the specification, and the compound is wide in absorption band, is suitable for curing in a near ultraviolet-visible light region as a photoinitiator, and has the advantages of high sensitivity, low toxicity, low cost, easiness in obtaining and the like. The invention also relates to preparation and use of the compound represented by the formula (I). The compound represented by the formula (I) is particularly suitable as photoinitiator in a UV-LED photocuring system, specifically in a photocuring system having a radiation wavelength of 300 to 600 nm.

The invention discloses a technology for producing calcium acetylacetonate with a solid phase method. technology is characterized in that acetylacetone, a calcium compound and water are added to a high-shear reaction device in the ratio being 42%-44%: 12%-17%: 41%-44% to be subjected to a shear stirring reaction for 1.5-2 h, vacuum drying is performed under the negative pressure of 0-0.1 MPa and at the temperature of 50-80 DEG C, and calcium acetylacetonate is obtained. With the adoption of the technology, the operation steps are simplified, the yield is increased, the energy consumption and the cost are reduced, the wastewater treatment expense is reduced, and the environmental pollution problem caused by wastewater is solved. No waste is emitted in the whole technological process, production technology integration is realized, and automatic production can be realized after combination. The technology conforms to the policy orientation of the national green and environment-friendly advanced industry.

The invention discloses a technology for producing zinc acetylacetonate with a solid phase method. The technology is characterized in that acetylacetone, a zinc compound and water are added to a self-made high-shear reaction device in the ratio being 38%-42%: 16%-24%: 38%-42% to be subjected to a shear stirring reaction for 1.5-2 h, vacuum drying is performed under the negative pressure of 0-0.1 MPa and at the temperature of 30-60 DEG C, and zinc acetylacetonate is obtained.

The invention discloses a preparation method of a PVC heat stabilizer tin-doped lanthanum acetylacetonate. The preparation method comprises the following steps: (1) preparing a reaction solution, (2)preparing a sodium hydroxide solution, (3) feeding acetylacetone, (4) carrying out a first-stage reaction process, (5) carrying out a second-stage reaction process, (6) carrying out reaction liquid pretreatment, and (7) carrying out ultrasonic-assisted cleaning and after the cleaning is finished, collecting precipitates, namely the PVC heat stabilizer tin-doped lanthanum acetylacetonate. Accordingto the prepared PVC heat stabilizer tin-doped lanthanum acetylacetonate, the adding amount of the tin-doped lanthanum acetylacetonate in PVC is 0.10%-0.15%, and the adding amount of the tin-doped lanthanum acetylacetonate is reduced by 25%-50% compared with that of a common heat stabilizer, by adding and using the heat stabilizer, rapid reduction of the heat stability of PVC can be remarkably inhibited, and meanwhile, the color change time of PVC is prolonged.

The invention relates to a method for producing a compound, in particular to a method for producing acetylacetone beryllium. The method comprises the steps of: dispersing beryllium oxide powder into solvent in a reaction kettle; adding acetylacetone into the reaction kettle, and carrying out reaction under the temperature condition of 50-80 DEG C; filtering while being hot, cooling filtrate and filtering again; and drying to obtain acetylacetone beryllium. The product obtained by the method is high in purity and fine in particles; and the yield is 90-95%, and the product purity reaches 99%. The method is fewer in steps, simple in technology, less in dosage of acetylacetone and low in production cost; and isopropanol or ethanol is used as solvent and can be recycled, so that the environment is not influenced.