35results about How to "The refining method is simple" patented technology

The invention relates to a method for extracting luteolin and beta-sitosterol from peanut shells. The method comprises the following steps: taking the peanut shells as materials, cleaning the peanut shells to remove impurities, crushing the cleaned peanut shells, performing extraction on the crushed peanut shells by an ethanol solution, carrying out filtration, decolorization and concentration under reduced pressure to obtain a luteolin and beta-sitosterol mixture, then mixing the luteolin and beta-sitosterol mixture with an alkali liquor, after that, carrying out extraction separation to obtain beta-sitosterol, performing extraction after pH adjustment to obtain a luteolin crude product, and performing alcohol dissolution, crystallization and recrystallization on the crude product to obtain a luteolin product with relatively high purity. The method is simple to operate, demands less on equipment, lowers the manufacturing cost of luteolin and reduces the risk of environmental pollution.

The invention provides a preparation method suitable for industrially producing oteracil potassium. The method provided by the invention has the advantages that: reaction steps are fewer, oxidants which generate gases polluting the environment are not used, a refining method is simple, the consumption of organic solvents which are harmful to the human body is decreased, the cost is saved, the total yield can reach more than 65%, and the method is suitable for the industrial production; the purity of a product reaches more than 99.8%, the impurity content of the single product is less than 0.1% and the purity and the impurity of the product both reach quality standards for the raw material medicine; and the obtained product is the oteracil potassium raw material medicine which is suitable for preparation of a medicinal preparation.

The invention provides a preparation and refining method of bromfenac sodium. The method has the advantages that the reaction conditions are mild, the operation is simple, and the obtained product is high in purity, high in yield and low in cost and can be industrially produced easily.

Provided is a method for preparing 9-fluorenone through fluorine. The industrial fluorine is adopted as raw materials, the 9-fluorenone and water are adopted as solvents, alkali is adopted as catalysts, quaternary ammonium salt is adopted as phase transfer agents, oxygen-containing gas is piped in as oxidizing agents, the 9-fluorenone is synthetised at the reaction temperature of 70 DEG C to 83 DEG C, and the raw materials of the fluorine are added at one time or constantly replenished along with the reaction. The products, 9-fluorenone, are adopted as solvents, the process of solvent fluorenone separation, recycling and the like is eliminated, reaction liquid separation and 9-fluorenone purification are operated in a coupling mode, and the 9-fluorenone synthetic process is greatly simplified. The alkali, the quaternary ammonium salt and the by-product, water, are all recycled. Through the fluorine replenishing feeding mode, the utilization efficiency of a reactor is improved.

The invention provides a refining method for a tofartinib citrate compound. The method comprises the following steps: preparing a tofartinib citrate crude product by a tofartinib crude product and citric acid monohydrate; adding a prepared mixed solvent, heating and stirring the mixture to be completely dissolved to obtain a clear solution, adding activated carbon, performing keeping warm and stirring, performing filtering, cooling a filtrate and performing recrystallization, performing filtering, washing a filter cake, and performing vacuum drying to obtain a tofatinib citrate refined product. The refining method has simple operation and high yield, the purity of tofartinib citrate reaches 99.93% or more, the maximum single impurity content is controlled to be 0.06% or less, and the totalimpurity content is controlled to be within 0.08%.

The invention relates to a fatty acid amide propyl dimethylamine refining method. The molecular structure of the fatty acid amide propyl dimethylamine is shown in the following specification, wherein n is 7-23. The fatty acid amide propyl dimethylamine refining method is characterized by comprising the steps of step 1, on the basis of the synthesis process of fatty oil or vegetable oil, or animal oil, or fatty acid methyl ester and dimethylamino-1-propylamine, in the process of adding materials, adding 0.01-0.05% (the weight of the fatty oil or vegetable oil, or animal oil, or fatty acid methyl ester) of a reducing catalyst such as one or several of sodium sulfite, sodium borohydride, sodium hypophosphite, making the mixture react under original process condition, step 2, before discharging products, dropwise adding 0.3-0.5 time of original theoretical amount of dimethylamino-1-propylamine, under the original process condition continuing reaction for 0.5-2 hours, step 3, under the reaction temperature, increasing the flow of inert gas such as nitrogen gas to blow and wash from a reactor bottom until no dimethylamino-1-propylamine can be tested in tail gas, complete the refining to acquire the high quality fatty acid amide propyl dimethylamine.

The invention belongs to the field of medicine impurities, and particularly relates to a delafloxacin impurity IV and a product refining method. A proper analysis method is selected through optimization to detect related stubborn impurities of a product. The specific structure of related impurities is separated, detected and confirmed. Finally, synthesis and process routes are optimized, impurities are controlled within a safe range, a basis is provided for product process amplification, stability, quality, pharmacology and toxicology and clinical research, and the method has important significance in reducing the safety risk of drug impurities.

The invention discloses a novel method for refining methyl chloroacetate, and belongs to the technical field of organic synthesis. By means of the method, a crude methyl chloroacetate product generated through an esterification reaction of methanol and chloroacetic acid is subjected to freezing layering to separate chloroacetic acid and a water layer. According to the refining method, the purity of methyl chloroacetate can reach 99.4% or above only by simply freezing the crude methyl chloroacetate product to minus 15 DEG C without simple distillation or rectification, little time is needed, the production time is greatly shortened, the production cost is greatly reduced, and the green chemical industry requirements are met.

The invention relates to the technical field of pharmaceutical chemicals, and provides a refining method of thymol. The refining method comprises the steps that a refining solvent is added to crude thymol, and the mixture is heated and stirred sufficiently to obtain a first mixed solution; the amount of the refining solvent is 0.5-3 times the mass-volume ratio of the crude thymol; an adsorbent isadded to the first mixed solution, and thermal insulation decolorization treatment is performed to obtain second mixed liquid; and the second mixed liquid is filtered, the obtained filtrate is subjected to cooling crystallization, thermal insulation crystallization and cooling crystallization separately, then centrifugal filtering is performed, and the thymol is obtained. The refining method can refine impurities such as citronellal and isopulegol in the crude thymol to a hardly detected degree, the purity of the product is effectively improved, and the medical requirements are met; and meanwhile, compared with a traditional rectification method, the refining method is simple, and the refining cost is greatly reduced.

The invention relates to a method for extracting luteolin and beta-sitosterol from peanut shells. The method comprises the following steps: taking the peanut shells as materials, cleaning the peanut shells to remove impurities, crushing the cleaned peanut shells, performing extraction on the crushed peanut shells by an ethanol solution, carrying out filtration, decolorization and concentration under reduced pressure to obtain a luteolin and beta-sitosterol mixture, then mixing the luteolin and beta-sitosterol mixture with an alkali liquor, after that, carrying out extraction separation to obtain beta-sitosterol, performing extraction after pH adjustment to obtain a luteolin crude product, and performing alcohol dissolution, crystallization and recrystallization on the crude product to obtain a luteolin product with relatively high purity. The method is simple to operate, demands less on equipment, lowers the manufacturing cost of luteolin and reduces the risk of environmental pollution.

The invention relates to a refining method of Shugeng sodium gluconate. A crude Shugeng sodium gluconate is purified by using a microreactor. Compared with the prior art, the refining method has the following beneficial technical effects: 1) the refining method of Shugeng sodium gluconate is simple and easy, and lower in energy consumption; 2) the refining method of Shugeng sodium gluconate is shorter in consumption time compared with the existing methods; and 3) the purity of the Shugeng sodium gluconate prepared by using the refining method is not lower than 98.0%, and the yield is not lower than 85%.

The present invention discloses the paraffin adsorption refining method with waste hydrofining catalyst. The waste hdyrofining catalyst is first treated to form paraffin refining adsorbent. The refining process may be intermittent or continuous one with refining temperature of 90-200 deg.C and space velocity 0.1-5.0 / hr. The adsorbent may be regenerated. The said process may be used alone for refining paraffin, or cooperated with hydrofining process as the pre-treatment for hydrofining material paraffin resulting in prolonged service life of hydrogenation catalyst.

The invention provides a pentane refining method. The pentane refining method comprises the following steps: mixing a pentane raw material and a metal-modified HZSM-5 molecular sieve, and refining toobtain refined pentane, wherein in the metal-modified HZSM-5 molecular sieve, modifying metal is copper or silver. According to the invention, the metal-modified HZSM-5 molecular sieve is used as a pentane refining agent, the refining method is simple, the energy consumption is low, and after refining, the content of unsaturated hydrocarbon is lower than 10 ppm; in addition, the pentane refining agent provided by the invention is recyclable, a pentane product obtained after recycling meets index requirements of the unsaturated hydrocarbon, the recycling condition is mild, and the recycling time is short.

The invention provides a preparation method suitable for industrially producing oteracil potassium. The method provided by the invention has the advantages that: reaction steps are fewer, oxidants which generate gases polluting the environment are not used, a refining method is simple, the consumption of organic solvents which are harmful to the human body is decreased, the cost is saved, the total yield can reach more than 65%, and the method is suitable for the industrial production; the purity of a product reaches more than 99.8%, the impurity content of the single product is less than 0.1% and the purity and the impurity of the product both reach quality standards for the raw material medicine; and the obtained product is the oteracil potassium raw material medicine which is suitable for preparation of a medicinal preparation.

The invention discloses a capsanthin residue refining method and belongs to the field of plant extraction. The capsanthin residue refining method comprises freezing and weak alkaline solution treatment. The capsanthin residue refining method can reduce the content of phospholipid, wax, pectin and polysaccharides in capsanthin residues; refined capsanthin residues have the advantages of being goodin mobility and free from solidification at low temperature; the capsanthin residue refining method is simple and applicable large-scale industrialized production.

The invention provides a method for purifying S-3-cyclohexenecarboxylic acid, the specific steps comprising: mixing crude S-3-cyclohexenecarboxylic acid, R-a-phenethylamine and ethyl acetate, stirring under reflux, filtering Obtain S-3-cyclohexenecarboxylic acid-R-a-phenethylamine salt, wherein, described S-3-cyclohexenecarboxylic acid crude product refers to the S-3-cyclohexenecarboxylic acid with ee value less than 97%; The S-3-cyclohexenecarboxylic acid-R-a-phenethylamine salt and ethanol are mixed, crystallized and filtered to obtain a recrystallized material; methylene chloride, water and the recrystallized material are mixed and stirred, and the The organic layer is collected after the liquid, and the organic layer is subjected to distillation treatment to obtain S-3-cyclohexenecarboxylic acid. The method for purifying S-3-cyclohexenecarboxylic acid provided by the invention can make the ee value of the prepared S-3-cyclohexenecarboxylic acid reach more than 99%, and simultaneously the resolving agent R-phenethylamine is recycled ,save costs.

The invention relates to a refining method of Shugeng sodium gluconate. A crude Shugeng sodium gluconate is purified by using a microreactor. Compared with the prior art, the refining method has the following beneficial technical effects: 1) the refining method of Shugeng sodium gluconate is simple and easy, and lower in energy consumption; 2) the refining method of Shugeng sodium gluconate is shorter in consumption time compared with the existing methods; and 3) the purity of the Shugeng sodium gluconate prepared by using the refining method is not lower than 98.0%, and the yield is not lower than 85%.

The invention relates to a chrysene refining method and aims to provide a chrysene refining method aiming at the problem that the chrysene purity is low and the chrysene application is limited in the traditional method. The method comprises the following steps of: 1, mixing raw material chrysene and acid for pickling, cooling to room temperature, filtering to obtain solid, washing the solid through distilled water, filtering and drying; and 2, mixing the dried solid and benzene solvents, repeatedly crystallizing twice, and finishing chrysene refining. According to the method, the product with the purity more than 98 percent can be obtained, and the method is applied to the field of luminous materials.

The invention provides a method for preparing and refining bromfenac sodium which is mild in reaction conditions, simple in operation, high in purity, high in yield, low in cost and easy for industrial production.

The invention discloses a refining method for tetracycline. The method comprises the following steps: (1) adding crude tetracycline into an acid solvent, and adding an acid precipitant and borax for dissolving to obtain a mixture A; (2) adjusting the pH of the mixture A to 1.2-2.8, standing the mixture A, and filtering the mixture A to obtain filtrate A; (3) adding zinc sulfate, potassium ferrocyanide and active carbon into the filtrate A to obtain a mixture B, standing the mixture B, and filtering the mixture B to obtain filtrate B; (4) performing ultrafiltration on the filtrate B to obtain filtrate C, adjusting the pH of the filtrate C to 4.5-5.0, standing the filtrate C, and filtering the filtrate C to obtain a filter cake A; (5) taking the filter cake A out, dissolving the filter cake A by using the acid solvent, adjusting the pH of the dissolved filter cake A to 4.5-5.0, standing the dissolved filter cake A, and filtering the dissolved filter cake A to obtain a filter cake B; and (6) drying the filter cake B in vacuum to obtain refined tetracycline. The refining method disclosed by the invention has the advantages of high product yield, high product purity, easiness and feasibility in operation, need of simple equipment, adoption of cheap and readily-available raw materials and low cost, and is suitable for large-scale industrial production.

Provided is a method for preparing 9-fluorenone through fluorine. The industrial fluorine is adopted as raw materials, the 9-fluorenone and water are adopted as solvents, alkali is adopted as catalysts, quaternary ammonium salt is adopted as phase transfer agents, oxygen-containing gas is piped in as oxidizing agents, the 9-fluorenone is synthetised at the reaction temperature of 70 DEG C to 83 DEG C, and the raw materials of the fluorine are added at one time or constantly replenished along with the reaction. The products, 9-fluorenone, are adopted as solvents, the process of solvent fluorenone separation, recycling and the like is eliminated, reaction liquid separation and 9-fluorenone purification are operated in a coupling mode, and the 9-fluorenone synthetic process is greatly simplified. The alkali, the quaternary ammonium salt and the by-product, water, are all recycled. Through the fluorine replenishing feeding mode, the utilization efficiency of a reactor is improved.

The invention provides a pentane refining method. The pentane refining method comprises the following steps: mixing a pentane raw material and a metal-modified HZSM-5 molecular sieve, and refining toobtain refined pentane, wherein in the metal-modified HZSM-5 molecular sieve, modifying metal is copper or silver. According to the invention, the metal-modified HZSM-5 molecular sieve is used as a pentane refining agent, the refining method is simple, the energy consumption is low, and after refining, the content of unsaturated hydrocarbon is lower than 10 ppm; in addition, the pentane refining agent provided by the invention is recyclable, a pentane product obtained after recycling meets index requirements of the unsaturated hydrocarbon, the recycling condition is mild, and the recycling time is short.

The invention relates to a refining method of high-purity cariprazine. The refining method comprises the following steps: adding dichloromethane and alcohol into a cariprazine crude product, heating and stirring until the crude product is dissolved, adding an ester solvent or a ketone solvent; cooling, crystallizing, filtering, collecting cariprazine crystals, washing cariprazine crystals by ethylacetate, and drying cariprazine crystals in vacuum to obtain high-purity cariprazine. According to the refining method, the yield of cariprazine is 80% or above, the purity (HPLC) reaches 99.5%, andthe impurity content is reduced to about 0.1%.

The invention discloses a method for extracting secoisolariciresinol diglucoside, an obtained extract and use of the extract. The method comprises the following steps: extracting linseed oil dregs with 70% ethanol, and concentrating, filtering and centrifugalizing; ultrafiltering; adding ultrafiltrate into macroporous resin to be washed, and sequentially eluting with 20% and 30% ethanol to colorless; and collecting and combining the eluant, decompressing and concentrating and drying to obtain. The method has the advantages that 1) the process is simple; 2) the extracting solvent is low in price and available; 3) impurities are not removed by acid and alkali treatment, and the refining method is simpler and more reasonably and low in production cost; 5) the obtained intermediate is high in content of secoisolariciresinol diglucoside; 6) the obtained extract has the effect of treating woman climacteric syndrome and can be clinically applied, and the extracted linseed oil dregs still can be used as feed for livestock, thereby greatly improving the comprehensive utilization value of the oil dregs.

The present invention is applicable to the technical field of medicine and chemical industry, and provides a method for refining thymol, comprising: adding a refining solvent to the crude thymemol, heating and stirring sufficiently to obtain a first mixed solution; the amount of the refining solvent is 0.5~3 times of the mass-volume ratio of the thymemol crude product; add an adsorbent to the first mixed solution, carry out heat preservation and decolorization treatment, and obtain the second mixed solution; filter the second mixed solution, and obtain The filtrate is subjected to cooling crystallization, heat preservation crystallization, cooling crystallization, and rejection filtration to obtain the filtrate. The refining method of the present invention can refine the impurities such as citronellal and isopulegol in the crude product of thymol to almost no detection, effectively improve the product purity, and meet the requirements of medicine; at the same time, compared with the traditional rectification method, the present invention The refining method is simple, and the refining cost is greatly reduced.

The invention discloses a capsanthin residue refining method and belongs to the field of plant extraction. The capsanthin residue refining method comprises freezing and weak alkaline solution treatment. The capsanthin residue refining method can reduce the content of phospholipid, wax, pectin and polysaccharides in capsanthin residues; refined capsanthin residues have the advantages of being goodin mobility and free from solidification at low temperature; the capsanthin residue refining method is simple and applicable large-scale industrialized production.

The invention provides a refining method for a tofartinib citrate compound. The method comprises the following steps: preparing a tofartinib citrate crude product by a tofartinib crude product and citric acid monohydrate; adding a prepared mixed solvent, heating and stirring the mixture to be completely dissolved to obtain a clear solution, adding activated carbon, performing keeping warm and stirring, performing filtering, cooling a filtrate and performing recrystallization, performing filtering, washing a filter cake, and performing vacuum drying to obtain a tofatinib citrate refined product. The refining method has simple operation and high yield, the purity of tofartinib citrate reaches 99.93% or more, the maximum single impurity content is controlled to be 0.06% or less, and the totalimpurity content is controlled to be within 0.08%.