The invention discloses a preparation method of a rhodium catalyst with 1,5-cyclooctadiene/L-alanine as a ligand. The method includes following steps: placing RhCl3.3H2O (50mg, 0.239mmol) into an oblique two-mouth flask and filling the flask with a mixed solvent containing ethanol (3.0ml) and water (1.0ml) with stirring until the RhCl3.3H2O is dissolved completely; adding 1,5-cyclooctadiene (0.2ml, 19.6 mmol), performing stirring for 30 min, increasing the temperature to 60 DEG C for reflux so that a precipitation is generated after the reaction finished, and washing the precipitation through ethanol for three times to obtain a [Rh(cod)Cl]2 catalyst; filling a reagent bottle with L-alanine (13.20mg, 0.13 mmol) and sodium hydroxide (5.50mg, 0,13 mmol), adding deionized water (0.6ml), performing stirring until the L-alanine and the sodium hydroxide are dissolved to obtain a reagent A; placing the [Rh(cod)Cl]2 (30mg, 0.06 mmol) into an oblique two-mouth flask with nitrogen being added for protection; filling the oblique two-mouth flask with 3ml of methanol for dissolving the L-alanine and the sodium hydroxide; and filling the oblique two-mouth flask with the reagent A with stirring for 90 min; performing rotary evaporation after the reaction finished for removing a minor part of the solvent, placing a product in a refrigerator for cooling for two days to enable a precipitation to precipitate out, performing a vacuumizing drying process and then detecting the product. The rhodium complex catalyst, when being used for catalyzing polymerization of substituted acetylene, can further increase polymerization conversion ratio and stereoselectivity.

Preparation of rhodium catalyst with 1, 5-cyclooctadiene/ L - phenylalanine as ligand

The invention provides a preparation method of (1,5-cyclooctadiene) rhodium chloride (I) dimmers. The method comprises the following concrete steps of (a) dissolving rhodium chloride hydrate by deionized water so that the rhodium concentration in the rhodium chloride water solution is 3 to 8 percent; putting the materials into a reaction kettle; connecting the upper end of the reaction kettle with a condensing pipe; adding absolute ethyl alcohol into the reaction kettle; performing heating, stirring and temperature rise; when the temperature rises to 35 DEG C, dripping a mixed solution of 1,5-cyclooctadiene COD and absolute ethyl alcohol; after the solution dripping is completed, adding a phase transfer catalyst PEG-400; performing reaction for 4 to 7 hours at 35 to 80 DEG C to obtain orange precipitates and suspension; performing filtering; (b) cooling the suspension in the step (a) to the room temperature; performing vacuum suction filtration to obtain a solid-state product; (c) washing and drying the solid-state product in the step (b). The product yield is 80 to 85 percent. By using the method, during the synthesis, the phase transfer catalyst PEG-400 is added, so that the raw materials and the ligand can be changed from two phases into one phase under the temperature reduction condition; the reaction temperature is reduced; the reaction temperature is reduced from 60 to 85 DEG C to 30 to 40 DEG C, but the reaction time cannot be prolonged.

Preparation method of (1,5-cyclooctadiene) rhodium chloride (I) dimers

The invention relates to the field of catalysis engineering, and particularly relates to a preparing method of a novel flavone derivative. 2-phenyl-1,4-benzopyrone is synthesized by utilizing a novel chiral rhodium catalyst to catalyze a reaction of 2-formyl phenol and phenylacetylene. Problems which are long synthetic routes, more byproducts in reaction processes and low total yields for flavone compounds at present are overcome. The method is a one-step synthetic method, is short in reaction process, avoids synthesis of intermediates and is high in yield.

A method of preparing 2-phenyl-1,4-benzopyrone

The invention discloses a zinc complex and a preparation method thereof as well as the application of the zinc complex as a near ultraviolet photoluminescence material, and belongs to the technical field of synthesis of chemical novel materials The chemical formula of the complex is [Zn(C6H5N2O2)2]n; the zinc complex belongs to a tetragonal system, the space group is P4(3)2(1)2(No96), and unit cell parameters are that both a and b are equal to 78691 (1), (the formula is shown in the description) alpha, beta and gamma are all 90 degrees and z is equal to 4 The zinc complex is prepared by adopting a solvothermal method The synthesis process of the zinc complex disclosed by the invention has the advantages of simplicity, feasibility, good reproducibility, easiness in implementation, abundant raw material sources and wide range in application; the zinc complex which can be used as the near ultraviolet luminescent material is applied to various fields of scientific experiments, drug production and research, and the like

Zinc complex and preparation method thereof as well as application of zinc complex as near ultraviolet photoluminescence material

The invention discloses a method for catalyzing an ethyl diazoacetate polymer by a rhodium catalyst with L-phenylalanine as a ligand. According to the method, the ethyl diazoacetate polymer is prepared, then a representation test is performed on a structure of the polymer to find that the obtained polymer has a very high decomposition temperature, and the polymer cannot be decomposed under 330 DEGC and can serve as a high temperature resistance polymer.

Ethyl diazoacetate polymer preparation method

The invention discloses a preparation method of a rhodium catalyst by using 2,5-norbornadiene (nbd) and 2-aminonicotinic acid as ligands. The preparation method comprises the following steps: taking 26 mg of 2-aminonicotinic acid and 40 mg of potassium hydroxide into a reagent bottle, adding 1.0-2.0 mL of deionized water, and stirring for dissolving; taking 45 mg-55mg of Rh Cl3.3H2O in an inclined two-port flask, injecting 3.0 mL of alcohol and 1.0 mL of a mixed solvent in the presence of a nitrogen gas, and stirring until dissolving completely; adding 0.10 mL-0.20 mL of 2,5-norbornadiene (nbd), stirring for 30 minutes, then heating to 60 DEG C, refluxing, and stirring until liquor is yellow; when 3 hours later, placing under the room temperature and stirring. The novel rhodium complex catalyst obtained by the preparation method disclosed by the invention can be used for further improving the polymerization conversion rate and stereoselectivity while catalyzing substituted acetylene to polymerize.

Preparation method of rhodium catalyst by using 2,5-norbornadiene (nbd) and 2-aminonicotinic acid as ligands

The invention belongs to the field of high polymer material engineering, and particularly relates to N-propene-N-diethoxy methyl silicone propyl pyromellitic imide and a preparation method thereof. The method comprises steps: taking N-propene-N-diethoxy methyl silicone propyl pyromellitic imide as an initial raw material, under nitrogen gas protection, adopting methylbenzene and dimethylformamideas solvents, and stirring N-propene-N-diethoxy methyl silicone propyl pyromellitic imide and 3-amino propyl diethoxy methyl silane for 24 hours at 130 DEG C; cooling, concentrating under reduced pressure, washing with water in ethyl acetate, drying with anhydrous MgSO4, and concentrating; and finally, purifying a crude product by adopting silica gel column chromatography to obtain a target productwith the yield of 82.30%. The method solves the problems of instability and low yield in the silicon-oxygen-containing substance synthesis process.

N-propylene-N-diethoxy methyl silicone propyl pyromellitic imide and preparation method thereof

The invention belongs to the field of high polymer materials and engineering, and specifically relates to a preparation method for an imide-bridged polysiloxane gas separation membrane. The preparation method is used for preparing a gas separation membrane by copolymerizing diallyl imide and a hydrogen-containing siloxane oligomer. By adoption of a solution polymerization method, a polymer is precipitated through methyl alcohol; film laying is carried out on glass after tetrahydrofuran is used to dissolve the polymer; and the imide-bridged polysiloxane gas separation membrane prepared by usingthe preparation method provided by the invention has enough stability, good permeability to oxygen and high selectivity to oxygen/nitrogen, and solves the problem that the gas permeability and selectivity of a conventional macromolecular gas separation membrane are mutually restricted.

Jia Hongge

Papers

Preparation of rhodium catalyst with 1, 5-cyclooctadiene/ L - phenylalanine as ligand

Preparation method of rhodium catalyst by using 2,5-norbornadiene (nbd) and 2-aminonicotinic acid as ligands

A method of preparing 2-phenyl-1,4-benzopyrone

N-propylene-N-diethoxy methyl silicone propyl pyromellitic imide and preparation method thereof

Imide-bridged polysiloxane gas separation membrane and preparation method thereof