C07C45/79

Acetone recovery and purification

Methods and systems for preparing acetone from cumene hydroperoxide (CHP) are disclosed. The disclosed methods involve cleaving CHP to form a cleavage product stream. In some embodiments, the cleavage product stream is separated into an overhead stream and a bottoms stream. The bottoms stream is neutralized, washed and then treated in a crude acetone column to provide a crude acetone stream. The overhead stream of the cleavage product is flashed forward in the process, bypassing the neutralization, washing, and crude acetone column and is then combined with the crude acetone stream. The combined acetone streams are provided to an acetone product column. According to some embodiments, the acetone product column comprises a side draw for obtaining a recycle acetone stream, which is recycled to the cleavage reactor(s). The recycle acetone side draw may be located lower on the acetone product column than the point from which product acetone is obtained. The disclosed methods increase the efficiency of the process.

Acetone recovery and purification

Methods and systems for preparing acetone from cumene hydroperoxide (CHP) are disclosed. The disclosed methods involve cleaving CHP to form a cleavage product stream. In some embodiments, the cleavage product stream is separated into an overhead stream and a bottoms stream. The bottoms stream is neutralized, washed and then treated in a crude acetone column to provide a crude acetone stream. The overhead stream of the cleavage product is flashed forward in the process, bypassing the neutralization, washing, and crude acetone column and is then combined with the crude acetone stream. The combined acetone streams are provided to an acetone product column. According to some embodiments, the acetone product column comprises a side draw for obtaining a recycle acetone stream, which is recycled to the cleavage reactor(s). The recycle acetone side draw may be located lower on the acetone product column than the point from which product acetone is obtained. The disclosed methods increase the efficiency of the process.

Chalcone compound and preparation method thereof

A method for preparing 2,2′,4,4′-Tetrahydroxy-3-(2″-hydroxy-3″-methylbutyl-3″-alkenyl)chalcone includes the following steps: subjecting a Morus alba leaf to extraction with an aqueous solution of methanol or ethanol having a volume fraction of 40%-100%, concentrating an extract to remove methanol or ethanol and dissolving in water, subjecting to extraction with petroleum ether and ethyl acetate successively, and concentrating an ethyl acetate extract to obtain a paste; chromatographing the paste over a silica gel column using chloroform-methanol, collecting an eluate where the volume ratio of chloroform-methanol is 95/5; chromatographing the eluate over a reversed-phase column using methanol-water, collecting an eluate where the volume ratio of methanol-water is 60/40, and thereby the compound is obtained.

Chalcone compound and preparation method thereof

A method for preparing 2,2′,4,4′-Tetrahydroxy-3-(2″-hydroxy-3″-methylbutyl-3″-alkenyl)chalcone includes the following steps: subjecting a Morus alba leaf to extraction with an aqueous solution of methanol or ethanol having a volume fraction of 40%-100%, concentrating an extract to remove methanol or ethanol and dissolving in water, subjecting to extraction with petroleum ether and ethyl acetate successively, and concentrating an ethyl acetate extract to obtain a paste; chromatographing the paste over a silica gel column using chloroform-methanol, collecting an eluate where the volume ratio of chloroform-methanol is 95/5; chromatographing the eluate over a reversed-phase column using methanol-water, collecting an eluate where the volume ratio of methanol-water is 60/40, and thereby the compound is obtained.

SUPERCRITICAL FLUID CHROMATOGRAPHY SYSTEM

Provided is a chiller and system that may be utilized in a supercritical fluid chromatography method, wherein a non-polar solvent may replace a portion or all of a polar solvent for the purpose of separating or extracting desired sample molecules from a combined sample/solvent stream. The system may reduce the amount of polar solvent necessary for chromatographic separation and/or extraction of desired samples. The system may incorporate a supercritical fluid chiller, a supercritical fluid pressure-equalizing vessel and a supercritical fluid cyclonic separator. The supercritical fluid chiller allows for efficient and consistent pumping of liquid-phase gases employing off-the-shelf HPLC pumps. The pressure equalizing vessel allows the use of off-the-shelf HPLC column cartridges. The system may further incorporate the use of one or more disposable cartridges containing silica gel or other suitable medium. The system may also utilize an open loop cooling circuit using fluids with a positive Joule-Thompson coefficient.

SUPERCRITICAL FLUID CHROMATOGRAPHY SYSTEM

Provided is a chiller and system that may be utilized in a supercritical fluid chromatography method, wherein a non-polar solvent may replace a portion or all of a polar solvent for the purpose of separating or extracting desired sample molecules from a combined sample/solvent stream. The system may reduce the amount of polar solvent necessary for chromatographic separation and/or extraction of desired samples. The system may incorporate a supercritical fluid chiller, a supercritical fluid pressure-equalizing vessel and a supercritical fluid cyclonic separator. The supercritical fluid chiller allows for efficient and consistent pumping of liquid-phase gases employing off-the-shelf HPLC pumps. The pressure equalizing vessel allows the use of off-the-shelf HPLC column cartridges. The system may further incorporate the use of one or more disposable cartridges containing silica gel or other suitable medium. The system may also utilize an open loop cooling circuit using fluids with a positive Joule-Thompson coefficient.

ISOLATION OF CHROMOPLASTID CAROTENOIDS FROM FRUITS
20220259128 · 2022-08-18 ·

The present invention relates to a method for the production of chromoplastid carotenoids that can be isolated from fruits. The procedure of the invention allows to selectively isolate, on the basis of the size (Size Exclusion Chromatography) and in pure form, the carotenoid in the form of regularly shaped and sized aggregates. The process includes the following steps: i) production, in suspension, of homogeneous fragments of the chromoplastidial membranes from the fruits; ii) solution isolation of the membrane components by solubilization with detergents; iii) selective and high-purity isolation of the carotenoid in the form of regular paracrystalline aggregates by a screening technique such as size exclusion chromatography (SEC—Size Exclusion Chromatography).

ISOLATION OF CHROMOPLASTID CAROTENOIDS FROM FRUITS
20220259128 · 2022-08-18 ·

The present invention relates to a method for the production of chromoplastid carotenoids that can be isolated from fruits. The procedure of the invention allows to selectively isolate, on the basis of the size (Size Exclusion Chromatography) and in pure form, the carotenoid in the form of regularly shaped and sized aggregates. The process includes the following steps: i) production, in suspension, of homogeneous fragments of the chromoplastidial membranes from the fruits; ii) solution isolation of the membrane components by solubilization with detergents; iii) selective and high-purity isolation of the carotenoid in the form of regular paracrystalline aggregates by a screening technique such as size exclusion chromatography (SEC—Size Exclusion Chromatography).

Method for separating eighteen components in traditional Chinese medicine composition

The disclosure provides a method for separating eighteen components in a traditional Chinese medicine composition, including: (1) preparing the traditional Chinese medicine composition into a total extract of the traditional Chinese medicine composition, separating by resin through sequentially eluting with water, 10% ethanol and 30% ethanol, and collecting the 30% ethanol eluate to obtain a 30% ethanol extract; (2) adding the 30% ethanol extract to a reverse phase silica gel ODS-AQ-HG, and separating in a medium pressure separation column to obtain differently numbered elution dry pastes; (3) dissolving the differently numbered elution dry paste with 30% methanol as a solvent, and passing the solution through a 0.45 μm microporous membrane, carrying out a primary separation by high performance liquid chromatography and collecting chromatographic peaks with different retention times, and further purifying by high performance liquid chromatography; finally obtaining the components of eighteen components.

Method for separating eighteen components in traditional Chinese medicine composition

The disclosure provides a method for separating eighteen components in a traditional Chinese medicine composition, including: (1) preparing the traditional Chinese medicine composition into a total extract of the traditional Chinese medicine composition, separating by resin through sequentially eluting with water, 10% ethanol and 30% ethanol, and collecting the 30% ethanol eluate to obtain a 30% ethanol extract; (2) adding the 30% ethanol extract to a reverse phase silica gel ODS-AQ-HG, and separating in a medium pressure separation column to obtain differently numbered elution dry pastes; (3) dissolving the differently numbered elution dry paste with 30% methanol as a solvent, and passing the solution through a 0.45 μm microporous membrane, carrying out a primary separation by high performance liquid chromatography and collecting chromatographic peaks with different retention times, and further purifying by high performance liquid chromatography; finally obtaining the components of eighteen components.