74results about How to "Novel process route" patented technology

The invention discloses a preparation method of 2,3-dichloropyridine. 2,3-dichloropyridine is an intermediate in fine chemical industry, which is widely used in the fields of medicine and pesticide. The method comprises the following steps: carrying out chlorination reaction on 2,6-dichloropyridine, which is used as a raw material, to obtain 2,3,6-trichloropyridine; adding the 2,3,6-trichloropyridine, an acid binding agent, a metal catalyst and an organic solvent into a reactor, and carrying out hydrogenation reaction, wherein the mol ratio of 2,3,6-trichloropyridine to acid binding agent is 1:(0.1-0.5); and cooling the hydrogenation reaction liquid, adding water to dissolve the acid binding agent hydrochloride, filtering, standing, separating out the water layer, extracting the organic solvent layer with water-containing acid at least three times, merging the water-containing acid layers after extraction, diluting by adding water, precipitating a solid, filtering, and drying to obtain the 2,3-dichloropyridine product. The invention has the advantages of novel process route, short reaction steps, high yield, low production cost and environmental friendliness, is simple to operate, and is suitable for industrial production.

The invention presents a process method of producing a high-grade TC4 alloy hot rolled plate with a high material-obtaining rate and low cost, which comprises the following steps: slab ingot preparation through an EB, grinding, heat rolling, atmosphere annealing, sand blasting, pickling, grinding and sizing to obtain an annealed TC4 hot rolled plate, wherein a coloring and inspection technology is applied for the surface detection of a cogging bland and for the surface quality detection of a fire rolling blank. According to the invention, the EB is adopted to smelt and roll blank; the material-obtaining rate from the raw materials to slabs is improved to 92 percent, and the material-obtaining rate from the raw materials to finished products is improved to 69-73.6 percent; cracks are ensured to be removed completely, so as to achieve the purpose of no grinding or less grinding in follow-up rolling, and accordingly the labor and material cost for grinding is greatly reduced; and the prepared plate has the tensile strength of 950-1100 MPa, the yield strength of 880-980 MPa, and the elongation percentage among 14-20 percent, and meets the standard requirements of GB/T3621-2007, GT/B14845-2007 and ASTMB265-2006.

The invention discloses a method for preparing 2,5-dimethyl phenylacetic acid. The 2,5-dimethyl phenylacetic acid is a fine chemical engineering intermediate which is widely applied in fields of medicines and pesticides, and particularly is a key intermediate of spirotetramat serving as a novel insecticide. The method comprises the following steps of: mixing paraxylene serving as a raw material and ionic liquid serving as solvent with paraformaldehyde and concentrated hydrochloric acid, and performing a chloromethylation reaction to obtain 2, 5-dimethyl benzyl chloride; and performing a carbonylation reaction and a hydrolysis reaction of the 2, 5-dimethyl benzyl chloride and an acid-binding agent and the solvent in a reactor under the action of a catalyst to obtain the 2,5-dimethyl phenylacetic acid. The method has a novel process, short synthetic reaction steps, simplicity of operation, low production cost, high reaction yield, and environmental friendliness, and is suitable for industrial production.

The invention discloses a ferric fluoride nano material and a preparation method thereof. The preparation method comprises the following steps of: dissolving inorganic ferric salt in an alcohol solvent to obtain alcohol solution containing iron; dispersing an inorganic fluorine source into the alcohol solution containing iron and adding the solution into a hydrothermal reaction kettle; carrying out the hydrothermal reaction kettle solution for 1 hour to 7 days at a temperature of 40 to 140 DEG C, naturally cooling, carrying out centrifugal separation, washing by ethanol and carrying out vacuum drying to obtain the ferric fluoride nano material. According to the preparation method of ferric fluoride, a volatile hydrofluoric acid fluorine source does not need to be used as a raw material, low-toxicity fluoride is used as the fluorine source, common ferric salt is used as a ferric source, the FeF3.0.33H2O nano material containing trace moisture is obtained by the simple solvent heat treatment, the preparation process is simple, the yield is high and the obtained material has high crystallinity. The method disclosed by the invention is a novel and practical process route for preparing the ferric fluoride nano material and has high actual application value.

The invention discloses a preparation method for lithium secondary battery micro water ferric fluoride anode materials, wherein, firstly, teracidic malysite and alkali are uniformly mixed in an aqueous solution under normal temperature in proportion from 1 to 1 - 1 to 10; water is removed after sucking filtration; iron-alkali mixture is obtained after drying for 1 to 48 hours; secondly, the iron-alkali mixture and 5 to 40 percent hydrofluoric acids are uniformly reacted in a plastic sealed container in proportion from 1 to 1 - 1 to 10, and heat preservation is performed for 1 to 48 hours under the temperature of 40 to 100 DEG C; thirdly, mixture is filtered, cleaned by utilization of ethanol and dried for 1 to 36 hours in the air; fourthly, the mixture is dried for 1 to 72 hours under vacuum state of 50 to 250 DEG C; fifthly, the mixture is crushed in a ball mill and passes through a 100 to 400 mesh sieve, and then a ferric fluoride product is obtained. The invention has the advantages that: firstly, systematic temperature is automatically controlled, and technological parameters are determined through precise calculation on the basis; secondly, yield of the method is high and product purity is larger than 95 percent. Obtained FeF3 (H2O) 0.33 has an integrated orthorhombic system structure, regular surface topography, small grain diameter and uniform distribution, and good discharge performance. The method is a novel and practical technological line for preparation of the FeF3 (H2O) 0.33.

The invention relates to a preparation method of prednisolone. The preparation method comprises the steps of sequentially carrying out 3, 20-keto protective reaction, 11-keto reduction reaction, 21-hydroxyl esterification reaction, 3, 20-keto deprotection reaction and 21-acetic ester hydrolysis reaction by taking prednisone acetate as a raw material to obtain prednisolone. The invention provides a novel synthesis route sequentially comprising the steps of esterifying and deprotecting; nitrosification quenching reaction and resin hydrolysis reaction are omitted in the deprotection process; and ester hydrolysis reaction is finished under the protection of a mixed solvent and inert gases, so that the condition that byproducts are produced by hydrolysis reaction is avoided. The preparation method is novel in process route, simple and rapid in operation process, low in production cost and suitable for large-scale industrial production.

The invention discloses a method for producing polysilicon with silicon tetrafluoride reduced by plasmas, specifically comprising the following steps: pumping the mixture of the silicon tetrafluoride gas and hydrogen as the raw materials into a plasma reactor filled with hydrogen, heating the silicon tetrafluoride gas and hydrogen to 1200-3500 DEG C instantaneously under the action of the plasmas and the silicon tetrafluoride gas and hydrogen carrying out chemical reaction to produce the polysilicon solid and the hydrogen fluoride gas; the produced polysilicon solid and hydrogen fluoride gas and the unreacted silicon tetrafluoride gas and hydrogen jointly entering into a gas-solid separation device, separating the polysilicon solid from the gases, the purity being more than 99.9999% and producing the finished product; and the hydrogen fluoride gas and the unreacted silicon tetrafluoride gas and hydrogen jointly entering into a condenser, condensing the hydrogen fluoride gas to liquid and the silicon tetrafluoride gas and hydrogen returning to the plasma reactor. The method has the advantages of novel and reasonable process routes, low equipment requirements, easy industrialization realization and low energy consumption.

The invention discloses a method for preparing lenalidomide (3-(7-amino-3-oxo-1H-isoindazole-2-yl) piperidine-2,6-diketone). The method comprises the steps of: intramolecular cyclization, deprotection, phase-transfer catalytic reaction, catalytic hydrogenation, alkalization and the like. The technology is novel in path, short in step, high in reaction yield, and low in production cost, and has large implementation value and social and economic benefits.

The invention belongs to the field of non-ferrous metal processing, and specifically relates to a TA23 alloy plate with high impact toughness and high plasticity and preparation and an application. According to the TA23 alloy plate, a whole process design concept is adopted, and key processes of cast ingot components, forging processes, rolling and heat treatment and the like are controlled in alldirections, so that the TA23 alloy plate with high impact toughness and high plasticity is prepared. The tensile strength Rm of the TA23 alloy plate is greater than or equal to 740 Mpa, the yield strength Rp0.2 is greater than or equal to 630 Mpa, the elongation A is greater than or equal to 19%, the room temperature impact KV2 is greater than or equal to 80 J, the low temperature impact at -40 DEG C is greater than or equal to 30 J, the overall performance is good, wherein the room temperature impact toughness is increased by more than 100%, the low temperature impact toughness is increasedby more than 190%, the elongation is increased by more than 3%, all indexes meet the customer standard, enough performance allowance is left, the safety factor of the product is greatly increased, andthe TA23 alloy plate is used for manufacturing ship structural parts and has the advantages of high impact resistant capability and high safety.

The invention relates to a method for preparing hydrocortisone. The method includes: subjecting a cortisone acetate raw material to sites No. 3,20-keto protective reaction, site No.11-keto reduction reaction, site No.21-hydroxy esterification reaction, sites No. 3,20-ketone deprotection reaction, and site No. 21-acetate hydrolysis to obtain hydrocortisone. The method provides a new synthetic route containing esterification and deprotection in order, greatly improves the reaction selectivity, easily separates deprotection reaction products and avoids the posttreatment of tedious several times of extraction of a large amount of solvents in the traditional deprotection reaction process, and also avoids the side reaction caused by quenching reaction in the posttreatment of the traditional process; and the ester hydrolysis reaction is carried out under protection of inert gases in a mixed solvent, so as to avoid by-products produced in the hydrolysis reaction. The process route of the invention is novel, simple for operation, low in production cost, and applicable to industrial scale production.

A preparation method of lenalidomide comprises the following steps: 1, reacting a raw material methyl 2-methyl-3-nitro-benzoate with a halogenating reagent to obtain methyl 2-halomethyl-3-nitro-benzoate represented by formula (I); 2, reacting the methyl 2-halomethyl-3-nitro-benzoate with dimethyl D,L-glutamate hydrochloride in the presence of an alkaline compound to obtain dimethyl 3-(7-nitro-1-oxo-1,3-dihydroisoindole-2-yl)glutarate represented by formula (II); 3, hydrolyzing the above compound of formula (II) to obtain 3-(7-nitro-1-oxo-1,3-dihydroisoindole-2-yl)glutaric acid represented by formula (III); 4, reducing the above compound of formula (III) to obtain 3-(7-amino-1-oxo-1,3-dihydroisoindole-2-yl)glutaric acid represented by formula (IV); and 5, carrying out ring closure on the above compound of formula (IV) to obtain lenalidomide represented by formula (V). The method has the advantages of simple process, high safety, cheap and easily available raw materials, good quality of the above product, and suitableness for industrial production.

The invention discloses a preparation method of 3-chloropyridine. 3-chloropyridine is a fine chemical engineering intermediate extensively used in the fields of medicine and pesticides. The preparation method comprises the following steps of: taking 2,6-dichloropyridine as a raw material and performing chlorination reaction to obtain 2,3,6-trichloropyridine; putting the 2,3,6-trichloropyridine, an acid-binding agent, a metal catalyst and an organic solvent into a reactor for performing hydrogenation reaction, wherein the mol ratio of the 2,3,6-trichloropyridine to the acid-binding agent is 1:(0.5-1.0); cooling the hydrogenation reaction liquid, adding water to dissolve the hydrochlorate of the acid-binding agent, filtering and standing to separate the water layer; extracting the organic solvent layer by aqueous acid at least more than three times; combining the extracted aqueous acid layers, thinning up with water, alkalizing for adjusting the pH value of the filtrate to be 7; and layering the filtrate to obtain the liquid product of 3-chloropyridine. The preparation method of 3-chloropyridine has a novel process route, short reaction steps, simplicity of operation, high yield, low production cost and environmental friendliness, and is suitable for industrialized production.

The invention relates to the technical field of chemical industry and in particular relates to a method for preparing ethyl silicate and magnesium fluoride by utilizing reactions of silicon tetrafluoride, ethanol and magnesium. The method comprises the following steps of: a. adding ethanol and magnesium powder to a reaction kettle; b. raising the temperature of the reaction system to a preset temperature to react; c. after reaction is completed, cooling the reaction system, adding prepared ethanol solution of silicon tetrafluoride to the reaction kettle until the reaction system is neutral; d. separating solid from liquid through filtration; e. washing the solid obtained in step d with ethanol and drying the washed solid to obtain the target product magnesium fluoride; and f. distilling the filtrate obtained in step d to remove ethanol, thus obtaining ethyl silicate with high boiling point. The method can be used for producing by-product silicon tetrafluoride by efficiently utilizing phosphate fertilizers.

The invention discloses a method for preparing talipexole (6-allyl-2-amino-5,6,7,8-tetrahydro-4H-thiazole [4,5-d]-aza-dihydrochloride). The method comprises the following steps: using ethyl acrylate as starting raw materials; firstly, carrying out addition reaction on the ethyl acrylate and allyl to generate 3-allylamine base ethyl propionate, then reacting with 4-bromobutyrate to generate 4-(allyl(3-ethoxyl-3-oxopropyl)amino) ethyl butyrate; performing the ring closing reaction under the condition of strong base, decarboxylasing under strong acid to generate 1-allyl azacycloheptane-4-ketone;then performing the nuclear bromination to generate 1-allyl-5-bromine azacycloheptane-4-ketone, and finally, reacting with thiourea to generate a target product (formula I). The invention has novel process, short procedures, high reaction yield, low production cost, and larger implementation value and social and economic benefits.