45results about How to "The production process is economical and environmentally friendly" patented technology

The invention discloses natural perfume refining fluid suitable for cigarette fluid of electronic cigarettes and cigarette fluid and a preparation method thereof, and belongs to the technical field of cigarette fluid of electronic cigarettes. Separation and impurity removal are performed on natural perfume such as extract, tincture and absolute oil through a macroporous adsorption resin column chromatography technology, high-boiling-point components such as monosaccharide and disaccharide and macromolecular components such as protein, polysaccharide and pectin in the natural perfume are simultaneously and effectively removed according to the differences of polarities and molecular sizes of all the components in the mixture, the components unfavorable for the smoking mouthfeel of the electronic cigarettes are removed, and the problem that charring flavor is generated due to the fact that the substances are deposited on heating wires is solved; meanwhile, the solubleness of the natural perfume in propylene glycol and glycerinum is improved, therefore, the cigarette fluid of the electronic cigarettes becomes clear and bright, the emission performance of perfume is significantly improved, the sweet greasy feeling is reduced, and the sensory effect is significantly improved.

The invention discloses a preparation method of β-menadione, comprising the following steps: step 1, dissolving ceric sulfate in a sulfuric acid solution to obtain a ceric sulfate solution, dissolving β-methylnaphthalene in an organic solvent, Obtain the β-methylnaphthalene organic solution; Step 2, add the ceric sulfate solution and the β-methylnaphthalene organic solution into the reaction kettle at the same time, keep the temperature and stir for the reaction, after the reaction, cool down and crystallize, and obtain the finished product β-methylnaphthalene through filtration Menadione; step 3, separating the cerium sulfate solution and the organic solvent in the liquid phase obtained by filtration, recycling the organic solution after distillation and recycling, and recycling the cerium sulfate solution after electrolytic oxidation of the diaphragm. The preparation method of β-menadione of the present invention completely replaces the oxidation of chromium, so that the product does not contain hexavalent chromium, and β-methylnaphthalene is dissolved in the organic phase for reaction. The material contact area is larger, and the reaction rate is faster. β ‑ Menadione will not peroxidize and the product is of high purity.

The invention discloses a method for preparing 16a-hydroxy prednisolone. The method includes the steps of adopting 17a-dehydroxyl prednisolone as a raw material and making the 16th locus and 17th locus of initial raw material 17a-dehydroxyl prednisolone subjected to an epoxidation reaction with organic peracid in a first organic solvent to obtain an epoxy object; making the epoxy object reacted with glacial acetic acid for ring opening under catalysis of acid catalysts in a second organic solvent to obtain 16a,21-diacetoxy prednisolone; then dissolving 16a,21-diacetoxy prednisolone in a thirdorganic solvent, hydrolyzing acetate at two positions under the catalytic action of a solid-phase base catalyst, and preparing 16a-hydroxy prednisolone, wherein the solid-phase base catalyst adopts aluminum oxide and silica gel or calcium carbonate as carriers, and the catalysts of sodium carbonate or sodium hydroxide are adsorbed on the carriers. 16a-hydroxy prednisolone is prepared by means of the efficient, environment-friendly and economical method.

The invention provides a method for preparing a 16a-hydroxyprednisolone product. The method comprises the steps that 17a-dehydroprednisolone is used as a raw material, and firstly the starting material 17a-dehydroprednisolone performs an epoxidation reaction with organic peroxide acid at 16 and 17 sites in a first organic solvent to prepare an epoxy material; then the epoxy material reacts with glacial acetic acid under catalysis of an acid catalyst in a second solvent for loop opening, and thus 16a,21-diacetoxyprednisolone is prepared; 16a,21-diacetoxyprednisolone is dissolved in a third organic solvent, under the catalytic action of a solid-phase base catalyst, acetic ester on the two sites are hydrolyzed, and thus 16a-hydroxyprednisolone is prepared; and finally the 16a-hydroxyprednisolone crude product obtained by solid-phase base-catalyzed hydrolysis is heated and refluxed, decolorized, and recrystallized through low-carbon alcohol below C4, and thus the 16a-hydroxyprednisolone product is obtained. According to the method, 16a-hydroxyprednisolone is prepared in an efficient, environment-friendly and low-cost mode.

The invention provides a preparation method of a 17a-dehydroxy prednisolone acetate product. The method includes the following steps: step A, dissolving prednisolone acetate in a first organic solvent, and subjecting the solvent and trimethylchlorosilane to 11th-position silicon etherification reaction under the catalysis of organic base to obtain a protector; step B, in a second organic solvent,subjecting the protector and SO3 to 17th-position dehydration reaction under the catalysis of the organic base, directly adding acid for treatment after the reaction to deprotect the 11th position, and obtaining a crude 17a-dehydroxy prednisolone acetate product; subjecting the crude product to decolorization and recrystallization in the presence of C4-below low carbon alcohol and activated carbonto obtain the 17a-dehydroxy prednisolone acetate product. The preparation method has the advantages that the problems such as many side reactions and impurities and difficulty in impurity refining inthe dehydration reaction in a traditional production process of 17a-dehydroxy prednisolone acetate are solved, the total synthesis yield is remarkably increased, and the production cost is reduced.

The invention provides a method for preparing 16a,21-diacetyloxy prednisolone. The method comprises the following steps: adopting 17a-deshydroxy prednisolone as a raw material, firstly, enabling the starting raw material 17a-deshydroxy prednisolone to generate epoxidation reaction with organic peroxy acid on 16 and 17 sites in a first organic solvent to prepare an epoxy product; enabling the epoxyproduct to react with glacial acetic acid under the catalysis of an acid catalyst in a second organic solvent to be subjected to ring opening, to prepare a target product, i.e., 16a,21-diacetyloxy prednisolone. According to the efficient, environment-friendly and fair-price method, the intermediate 16a,21-diacetyloxy prednisolone of 16 alpha-hydroxyprednisolone is prepared.

The invention discloses a preparation method of 16a-hydroxy prednisolone. The preparation method comprises the following steps: dissolving 16a-hydroxy prednisolone acetate into an organic solvent, adding an inert solid carrier adsorbed with strong base as a hydrolysis reaction solid-phase base catalyst, and hydrolyzing 21-acetate to obtain a 16a-hydroxy prednisolone crude product; and carrying out lower alcohol recrystallization on the crude product under the condition of below C4 to obtain a 16a-hydroxy prednisolone competitive product, wherein the refined weight yield is 85% to 90%, and the preparation weight total yield is 75% to 80%. The solid carrier is selected from aluminum oxide, silica gel or calcium carbonate; the base catalyst is selected from sodium carbonate; and the organic solvent is selected from methylbenzene or chloroform. Compared with a traditional method, the method disclosed by the invention is simple and convenient in production operation, impurities generated in traditional production can be greatly reduced, and the total yield for synthesis is greatly improved; compared with the traditional method, the production cost is reduced by 10% to 15%; and a synthetic reaction solvent can be recycled, and industrial production is facilitated.

The invention provides a preparation method of finished 16alpha,21-diacetoxy prednisolone product, comprising: subjecting 17alpha-deshydroxy prednisolone acetate as an initial material to 16,17-epoxidation with an organic peroxy acid in a first organic solvent to obtain an epoxide; subjecting the epoxide, in a second organic solvent, to ring-opening reaction with glacial acetic acid under the catalysis of an acid catalyst to obtain the target product, 16alpha,21-diacetoxy prednisolone; subjecting the crude 16alpha,21-diacetoxy prednisolone to heating reflux discoloration and crystallization with a lower carbon alcohol of C4 and below so as to obtain the finished 16alpha,21-diacetoxy prednisolone. The intermediate, 16alpha,21-diacetoxy prednisolone, to 16alpha-hydroxy prednisolone is prepared herein via the method that is efficient, environmentally friendly and fair in cost.

The invention discloses a high-combination leather fatliquoring agent and a preparation method thereof, comprising the following steps: (1) adding a certain amount of long-chain fatty alcohol and maleic anhydride into a reactor, raising the temperature to 80-90°C for esterification , to obtain product A; (2) cooling product A to 70-75° C., adding a certain amount of initiator azobisisobutyronitrile, and then dropwise adding a certain amount of monomer vinyl acetate to carry out polymerization reaction to obtain product B; (3 ) raising the temperature of product B to 100-110°C, adding a certain amount of long-chain fatty alcohol for esterification reaction to obtain product C; (4) cooling product C to 65-70°C, using 30% sodium hydroxide The aqueous solution neutralizes the pH of the reactant to 7.0, then adds a certain amount of sulfite aqueous solution, and carries out sulfitation reaction at 80-90°C, and after cooling down, a high-binding leather fatliquoring agent is obtained. The invention has the advantages of simple process, clean and environment-friendly, and the prepared product has excellent properties such as acid resistance stability, fatliquoring effect, filling performance and solvent extraction resistance, and can reduce the COD content of waste liquid.