32results about How to "Short process reaction time" patented technology

The invention discloses a method for preparing rifampicin by using a microchannel reaction device. Through a microchannel reactor, rifamycin S is used as a raw material to undergo cyclization, hydrolysis, condensation and crystallization processes without post-treatment process, and directly obtains Rifampicin crude. The invention realizes complete continuous production of rifampicin, has high yield, low cost, high profit, environmental protection, energy saving and high efficiency, and is suitable for industrial application.

The invention discloses an acidic iron-containing wastewater recycling system comprising a pickling wastewater storage pool, wherein the pickling wastewater storage pool is connected with a neutral oxidation reaction tank through a raw water acid proof pump, and a stirrer, a 1# online pH meter and a 1# online ORP (oxidation reduction potential) meter are fixed in the neutral oxidation reaction tank; an alkali liquor storage tank is connected with the neutral oxidation reaction tank through a 1# metering pump; a flocculant storage tank is connected with the neutral oxidation reaction tank through a 2# metering pump; the neutral oxidation reaction tank is connected with a settling tank through a slurry pump, the settling tank is connected with a sludge concentration tank, and a supernatant drain pipe is further connected to the settling tank; the sludge concentration tank is connected with a high pressure plate frame filter press through a high pressure slurry pump; and the neutral oxidation reaction tank is further connected with a blower. The invention further discloses an in situ modification method for treating wastewater by the acidic iron-containing wastewater recycling system. By adopting the acidic iron-containing wastewater recycling system disclosed by the invention, more than 55% of Fe3O4 can be stably prepared and recycled through in-situ reaction in an acidic wastewater neutralization tank under normal temperature and normal pressure conditions.

The invention belongs to the field of organic synthesis and particularly relates to a clean synthesis method for di-tert-butyl disulfide, which comprises the following steps: adding tert-butyl mercaptan, a catalyst and a solvent, i.e. acetone, into a reactor container, or only adding the tert-butyl mercaptan and the catalyst into the reactor container firstly and then adding an oxidizer, i.e. oxyful, or a mixture of acetone and oxyful into the reactor container with stirring; controlling a reaction temperature between minus 20 DEG C and 70 DEG C to perform a reaction sufficiently; after the reaction is completed, post-processing the obtained product to obtain the di-tert-butyl disulfide, wherein the catalyst is cuprous chloride, copper chloride or a mixture of the cuprous chloride and thecopper chloride in random mass proportion. The invention meets the requirement for clean production. The catalyst and the reaction solvent have low price, can be conveniently recycled, have small usage in the reaction and have excellent catalytic performance. Meanwhile, the process has short reaction time, the conversion rate of the tert-butyl mercaptan reaches 98 to 100 percent, the selectivity of the di-tert-butyl disulfide is between 90 and 96 percent, the reaction yield is high and the clean synthesis method is suitable for industrial production.

The invention discloses a method for continuously synthesizing benzyl-substituted gluconolactone by using a microchannel reaction device. The method uses methyl-α-D-mannopyranoside as a starting material, and prepares it into an old machine solvent solution and The organic solvent solution of benzyl chloride reacts in the first microreactor to generate methylglucose whose hydroxyl group is protected by benzyl; React demethylation in middle to generate hydroxybenzyl substituted glucose; finally react the reaction solution with aqueous solution of hydrogen peroxide and sodium hydroxide, and organic solvent solution of tetramethylpiperidine nitrogen oxide in the third microreactor to generate high-purity The intermediate of the hypoglycemic drug Dapagliflozin is benzyl substituted gluconolactone. The method of the invention has higher heat and mass transfer efficiency, is easier to scale up industrially, has simple, cheap and easy-to-obtain starting materials, simple process, high purity of obtained intermediates, and high yield, can effectively reduce production costs, and is suitable for industrialized production.

The invention discloses a method for continuously preparing rosuvastatin intermediates by adopting a microchannel modular reaction device. The isopropanol solution of p-fluorobenzaldehyde and the isopropanol solution of methyl isobutyryl acetate are prepared in acetic acid and piperidine Under catalysis, react in the first microreactor to generate the first product; the first product and the free isopropanol solution of S-methyl isothiourate react in the second microreactor to generate the second product; the second The product is reacted with an acetone solution of potassium permanganate and acetic acid in the third microreactor to obtain the third product; finally the third product is reacted with methylamine ethanol solution in the fourth microreactor to obtain the rosuvastatin intermediate. The invention has low toxicity and pollution, low production cost, good product quality, high profit, environmental protection, energy saving and high efficiency, and has the potential of industrial scale-up.

The invention discloses a novel method for preparing an atorvastatin key intermediate L1 through a solvent-free method and belongs to the technical field of drug chemical synthesis. The novel method comprises the following steps that M4 and A9 are taken as raw materials, under the effects of a phase transfer catalyst and an acid catalyst, constant-temperature stirring melting reaction is directlyconducted for 5-7 hours under the solvent-free condition, the reaction temperature is 80-140 DEG C, water distribution is conducted in the reaction process, after reaction is completed, cooling is conducted, then recrystallization is conducted, and thus the atorvastatin key intermediate L1 is obtained. According to the novel method, the phase transfer catalyst and the acid catalyst are adopted, aparent nucleus M4 and a chiral side chain A9 are subjected to stirring melting reaction under the solvent-free condition, after reaction, recrystallization is conducted directly through ethyl alcohol / water, and thus L1 is obtained; and as for the process, the reaction time can be shortened to be 5 h, the conversion rate can reach up to 90%, operation and aftertreatment are easy, no mixed solvent is recovered, pollution is reduced remarkably, and the method is suitable for amplification production.

The invention discloses an oxapium iodide preparation method. The method comprises the steps of S1, preparing 2-phenyl-2-hexamethylene-4-methanol-1,3-dioxolane, S2, preparing 2-phenyl-2-hexamethylene-4-piperidinemethyl-1, 3-dioxolane, and S3, preparing the oxapium iodide. The step S1 comprises the steps of mixing uniformly cyclohexyl phenyl ketone, glycerol, Amberlyst-15 exchange resin and allochroic silicagel, heating, maintaining the temperature, stirring, filtering, taking the filtered solution, adding saturated sodium hydrogen carbonate aqueous solution for washing, keeping static, taking organic layer, drying, releasing pressure, distilling to acquire material A, purifying material A, drying to acquire 2-phenyl-2-hexamethylene-4-methanol-1, 3-dioxolane. The method has the advantages of being mild in reaction condition, simple in operation, suitable for industrialized production, low in material toxicity, easy and cheap for material access, low in cost and good in comprehensive yield rate.

The invention discloses a preparation method for a styrene-diolefin special copolymer. The preparation method comprises the following steps: taking a styrene-diolefin block random copolymer as PS-PB-PB / PS-PS; wherein PS representing a styrene copolymer block, PB representing a diolefin copolymer block, and PB / PS representing a styrene-diolefin random copolymer block; and adopting an anionic continuous polymerization method. The preparation method avoids the defects of a batch still and is characterized by low production cost, short production cycle, low operating cost, short reaction time andhigh yield.