2166results about "Carboxylic acid esters separation/purification" patented technology

An improvement in the production of methylidene malonates is attained by use of specific reaction phase and/or separation phase polymerization inhibitors and combinations thereof.

The present invention relates to process of extracting chlorogenic acid from honeysuckle and belongs to the field of medicinal chemical technology. The process includes the steps of: reflux extraction of honeysuckle with water or ethanol, filtering to collect filtrate, recovering solvent, ethanol deposition to eliminating impurity, letting stand overnight, filtering, decompression recovering solvent, adding water and letting stand overnight, filtering, eluting the filtrate in macroporous resin column, concentrating eluent, collecting chlorogenic acid component, eluting on polyamide column with eluent, collecting chlorogenic acid component, concentration, rectification to obtain chlorogenic acid product with content over 95 %. The present invention is suitable for industrial application.

A process for preparing danshinolic acid A from red sage root includes such steps as extracting in water or alcohol, concentrating, high-temp and -pressure reaction, purifying by chromatographic column, regulating pH value, extracting in organic solvent, concentrating and drying.

The present invention relates to a process for preparing an alkylester of fatty acid with high purity via one-step continuous process by reacting an animal fat and/or vegetable oil with a lower alcohol in the presence of alkali catalyst by passing through a continuous tubular reactor while maintaining a single-phase, removing residual lower alcohol from the reaction mixture and removing residual glycerin, catalyst, etc. by phase separation. In accordance with the present invention, an alkylester of fatty acid can be produced with a high yield of 97% or more via one-step continuous process in a continuous tubular reactor without any limitation in flow types by reacting an animal fat and/or vegetable oil with a lower alcohol in the presence of alkali catalyst and carrying out a simple separating process.

Novel improved processes for the production and isolation of methylidene malonates via direct and indirect adduct processes.

The invention is concerned with a kind of extract of total ketone of salviae miltiorrhizae and total phenolic acid and its produce method form radix Salviae Miltiorrhizae. The extract of total ketone of salviae miltiorrhizae has cryptotanshinone, tanshinone I, tanshinone IIA, methyl Tanshinon, dihydrotanshinon I and ramification. The extract of total phenolic acid has salvianolic acid A, salvianolic acid B, protocatechuic aldehyde and ramification. The extract can be got form one or arbitrary compound of extraction with solvent method, macroporous resin method, column chromatography and liquid-liquid counter-current chromatography. The summation of the content to each total ketone of salviae miltiorrhizae is 20 to 100 percnte (w/w) of the extract of total ketone of salviae miltiorrhizae, the contene of cryptotanshinone, tanshinone I and tanshinone IIA is 5 to 100 percent (w/w) of whole content of total ketone of salviae miltiorrhizae. The summation of the content to each total phenolic acid is 5 to 100 percent (w/w) of the extract of the radix salviae miltiorrhizae total phenolic acid. The content of salvianolic acid B is the 5 to 100 percent (w/w) of the whole salvianolic acid.

The invention provides an industrialized production method for synchronously producing stevioside, flavone and chlorogenic acid. The method includes the following steps that step1, stevia rebaudiana leaves are weighed, extracted by adding water and filtered to obtain an extracting solution, flocculating agents are added under the condition of heat preservation, the pH is adjusted to 7-12, standing is performed for 0-120 minutes at the temperature of 30 DEG C-75 DEG C, then filtering is performed to obtain filter mud and filter liquid, and resin purification is performed on the filter liquid so as to obtain the stevioside product; step2, the filter mud is extracted through acid solvent, and extracting solutions are merged and concentrated; step3, solvent is added into a concentrated solution for dilution, and macroporous adsorption resin is added for adsorption; step4, gradient resolution is performed on the macroporous adsorption resin in the step3, a low-concentration resolution liquid is concentrated and dried to obtain the chlorogenic acid product, and high-concentration resolution liquid is concentrated to be standby; step5, after water is added into the high-concentration resolution liquid for dilution, organic solvent the same as the high-concentration resolution liquid in volume is used for extraction, and organic phases are merged, concentrated and dried to obtain the flavone product. By the adoption of the method, the stevioside, flavone and chlorogenic acid are extracted at the same time, the production cost is lowered, and the comprehensive utilization value of the stevioside is increased.

The present invention relates to a novel process for preparing alkyl polycarboxylates from an aqueous solution of an ammonium salt of the polycarboxylic acid by reactive distillation, and to a process for hydrogenating the alkyl carboxylates prepared in this way.

Provided are methods for the preparation and purification of alkyl tetrahalophthalate esters by the reaction of a tetrahalophthalic compound with an alkanol in the presence of a titanate catalyst. More particularly, improved methods are provided for making and recovering an ester with little contamination by catalytic metal components and color bodies, and with little acidity, in a high yield from the esterification reaction by pretreating the starting materials to reduce the acidity thereof, reacting the starting materials in the presence of a titanate catalyst, stripping excess alcohol, hydrolyzing the catalyst, and filtering out solids to yield a high purity tetrahalophthalate ester product.

The invention relates to the field of the medicine, in particular to a method for extracting and separating a chlorogenic acid monomer from honeysuckle. The prior art is lack of a method for the mass preparation of the chlorogenic acid monomer from the honeysuckle. In the invention, the technology is realized by the following preparation steps of: (1) soaking by alcohol: putting the honeysuckle into an alcohol solution for soaking, heating, refluxing, filtering and concentrating; (2) degreasing: degreasing the obtained filtrate thrice by adopting a weak-polarity solvent, and taking a water layer; (3) enriching by macroporous resin: enabling a water layer solution obtained in the step (2) to pass through the macroporous resin, washing by water, collecting effluent liquid and water washing liquid, concentrating and regulating the pH value; (4) extracting: extracting a solution obtained in the step (3) by adopting a moderate-polarity solvent, taking an organic layer, concentrating and recovering the solvent to obtain a faint yellow puffy solid substance; and (5) recrystallizing. The invention adopts an alcohol extraction method to enhance the extraction rate and the transfer rate of the chlorogenic acid, the final transfer rate of the chlorogenic acid is as high as 84 percent, and the purity of the obtained product can reach more than 98 percent.

The invention relates to a method for extracting chlorogenic acid, which belongs to the technical field of pharmaceutical chemicals. The method combines macroporous resin enrichment, ethyl acetate extraction and a mixed solvent split-phase method to achieve multi-step gradient purification of the chlorogenic acid so as to obtain a chlorogenic acid product with high purity. The method comprises the processes of water extraction, column passing, extraction, phase splitting and recrystallization. The macroporous resin adopted by the column passing process is 306 type or XAD series resin; and the split-phase agent adopted by the split-phase method is petroleum ether, chloroform or the mixture of the petroleum ether and the chloroform. The method is applicable to the process of extracting and preparing the chlorogenic acid from honeysuckles, cortex eucommiae leaves and cortex eucommiae barks.

An ester-forming monomer obtained by depolymerization of polytrimethylene terephthalate and having an acrolein content of no greater than 0.5 wt %. Polymers obtained using the monomer and fibers, films and molded articles comprising the polymers. The ester-forming monomer is obtained by reacting polytrimethylene terephthalate with at least one compound selected from among monoalcohols, 1,3-propanediol and water in the presence of a basic substance. When the recovered ester-forming monomer is used as the starting material for production of a polymer, it is possible to produce a molding polymer for fibers, films and the like with quality equivalent to or higher than that obtained using virgin monomer.

A method of making a hindered phenolic antioxidant is disclosed wherein the method comprises:

reacting an ester of the formula:

wherein

• • R¹, R², and R³ are independently selected alkyl groups and n is 0, 1, or 2, with an aliphatic polyhydroxyl alcohol of the general formula R(OH)_n wherein R is an aliphatic group of from 2 to about 12 carbon atoms and n is an integer of from 2 to 7, provided that one hydroxyl is primary and the others are secondary or tertiary, in the presence of a strong acid catalyst; then, neutralizing the strong acid catalyst with an overbased detergent; and isolating the hindered phenolic antioxidant after the neutralization step.

The process of preparing high purity chlorogenic acid and flavonid with eucommia leaf includes the following steps: crushing eucommia leaf and extracting with pH 3-6 alcohol solution of 45 %-55 % concentration; saturation adsorbing the extracted solution with medium polarity JD-1 macroporous resin, and eluting successively with water, 20 %-45 % concentration alcohol solution and 60 %-75 % concentration alcohol solution to obtain crude chlorogenic acid product and flavonid-containing powder separately; eluting the crude chlorogenic acid product in silica gel column with ethyl acetate, acetone, methanol or ethanol, collecting the eluted solution, decompression concentrating, and re-crystallizing the concentrate in acetone or water to obtain refined chlorogenic acid product. The present invention has simple technological process, convenient operation, reuse of the macroporous resin, low comprehensive cost and excellent industrial application foreground.

The invention discloses a separating method of butyl para-acetate from the reacted compound of acetic acid and C4, which comprises the following steps: flashing to remove non-reacted C4 and light component; flowing production from the bottom of flashing tower into coboiling rectifying tower; adding coboiler A to separate butyl para-acetate and acetic acid; transmitting mass from coboiler into acid condensing tower; adding coboiler B to coboil and rectify again; condensing acetic acid; obtaining the product with purity over 99% and acetic acid content less than 0.01% and water less than 0.05%; recycling acetic acid.

The invention discloses a method for extracting high-purity chlorogenic acid from honey suckle flower. The technical scheme of the invention comprises the following steps of: firstly, smashing the honey suckle flower material by the low-temperature supersonic air stream to obtain the cell-level honey suckle flower micro powder; secondly, carrying out the enzyme treatment, ultrasonic treatment, water extraction and filtering on the cell-level honey suckle flower micro powder to obtain the initial solution of the chlorogenic acid; and finally, flocculating, decolouring, purifying, condensing and drying the initial solution to obtain the high-purity chlorogenic acid. The invention solves the problems that the chlorogenic acid extract of the prior art is difficult to filter due to the large quantity of the precipitate in the impurity-removal and purification process; the invention has the advantages of advanced technique, simple and convenient operation, low cost, no harmful solvent, highpurity, high yielding rate, suitability for industrial large-mass production and the like.

The invention discloses a method for comprehensively extracting multiple effective components from tobacco leaves. The method comprises the following steps: performing twice ultrasonic circulation extraction on the tobacco leaves to respectively obtain crude ointment containing solanesol, nicotine and chlorogenic acid and an extract containing protein and sugar, and with the combination of separation and purification methods such as liquid-liquid two-phase extraction, column chromatography, recrystallization, steam distillation and precipitation, separating five effective components, namely, solanesol, nicotine, chlorogenic acid, protein and sugar from the tobacco leaves one by one. The method can continuously extract and separate the multiple effective components form the tobacco leaves, can greatly improve the utilization rate of a tobacco leaf raw material, has the advantages that the extraction efficiency is high, a great number of separation products are obtained and a small amount of wastes are discharged, and is an efficient and environment-friendly comprehensive tobacco leaf multi-component extraction technique.

The invention discloses a method for preparing chlorogenic acid in Eucommia ulmoides leaves, which comprises the following steps of: crushing the Eucommia ulmoides leaves, performing warm water extraction assisted by cellulose, performing conventional filtration, removing impurities by using an ultrafiltration membrane, performing nanofiltration and concentration, separating and purifying by using macroporous resin, and concentrating and drying to obtain chlorogenic acid powder. The chlorogenic acid in the Eucommia ulmoides leaves is subjected to warm water extraction assisted by cellulose, the extraction rate can reach 95 percent, the water extraction temperature is lower, and the extraction time is shortened; the ultrafiltration membrane is adopted to remove the impurities from the extracting solution and separate other byproducts, the membrane operating process is simple, the membrane flux can be stable for a long time, and the membrane is easy to clean, has long service life and is suitable for industrialization; a nanofiltration membrane is adopted to concentrate the extracting solution from which the impurities are removed, the load of the subsequent process is lightened, and the service life of the resin can be prolonged; the filtrate obtained through nanofiltration has the chemical oxygen demand (COD) value of less than or equal to 100 and can be returned to the production process, and wastewater is not generated basically; and the macroporous adsorbent resin can effectively purify the chlorogenic acid, the purity of the chlorogenic acid in the prepared powder is more than 60 percent and the extraction ratio is more than 1.4 percent.

The invention discloses a making method of salviol acid A, which comprises the following steps: extracting salvia miltiorrhizae through water or alcohol; removing solid impurity; purifying salviol acid A through column chromatogram; condensing eluent; adjusting pH value of organic solvent; extracting; condensing; drying; obtaining the product with high-extracting rate; fitting for large-scale of manufacturing.

The invention relates to a method for simultaneously extracting and separating chlorogenic acid, solanesol, alkaloid and rutin in tobacco. The method comprises the following steps: 1, extracting simultaneously, namely, crushing a tobacco raw material, extracting by using 80% ethanol once under the conditions that the temperature is 40-50 DEG C, the ultrasonic frequency is 45KHz and the ratio of material to liquid is 10:1, and performing suction filtration or centrifugation, respectively extracting the residue by using 80% and 95% ethanol once; combining the extract solutions of three times, thereby obtaining crude extract of chlorogenic acid, solanesol, alkaloid and rutin in tobacco, wherein the extraction rates of chlorogenic acid, solanesol, alkaloid and rutin in tobacco are 100%; and 2, separating, namely, separating solanesol, separating chlorogenic acid and rutin, and separating alkaloid. By adopting the method, simultaneous and efficient extraction on chlorogenic acid, solanesol, alkaloid and rutin in tobacco is achieved, the extraction rates are all 100%, the four components are effectively separated through simple steps, the utilization rate of the tobacco resource is improved, at the same time the operation is simple, the organic solvent is saved, and the energy consumption is reduced.

The invention discloses a method for using by-products of maleic anhydride to prepare BDO or succinic acid diester, wherein, the by-products comprise at least one of wastewater, waste residues and maleic anhydride residues, a preparation method thereof includes the major steps of esterification, distillation, reduction, etc., thereby obtaining a BDO or succinic acid diester product. The method can fully recycle maleic anhydride, fumaric acid, maleic acid, succinic acid, etc. in the by-products such as wastewater, waste residues and maleic anhydride residues in the production process of maleic anhydride, thereby obtaining products such as chemical intermediate BDO or succinic acid diester with great market demands, and maximally reducing the discharge of wastes; and the preparation method has advantages of simple and controllable technical process and rather low cost.