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Method for preparing bryonia alcohol acid

A technology for purgative alkyd and resin, which is applied in the field of preparation of purgative alkyd, can solve the problems of low product purity, high energy consumption, pollution and the like, and achieves the effects of being beneficial to large-scale production operations, with low pollution and low energy consumption

Active Publication Date: 2012-10-10
江苏芝能生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the prior art, the methods used to prepare high-purity bryonia alkyd are traditional heating extraction, repeated treatment with organic solvents such as benzene and petroleum ether, the process is backward, the product has low purity, high energy consumption, and serious pollution, which is far from being possible. Adapt to the requirements of modern circular economy

Method used

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  • Method for preparing bryonia alcohol acid

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Take 10Kg of watermelon stems and roots of Cucurbitaceae melons, add 5 times its mass of water, add cellulase, enzymolyze for 2 hours under the conditions of temperature 40°C, pH value 3, enzyme amount 20U / g crude drug, and heat to boiling And decocted for 0.5 hours, filtered, took the filtrate, adsorbed by HPD700 macroporous adsorption resin, eluted with 10% ethanol, collected 3 times the column volume eluate, passed through 201×4 type strong basic styrene type anion Exchange resin adsorption, elute with 0.5mol / L NaOH solution, collect and elute, filter, pass through 001×4 strong acidic styrene type cation exchange resin, collect the effluent, filter, and pass the filtrate through cellulose acetate propionate The reverse osmosis membrane was concentrated, methanol was added to crystallize, the crystals were separated, washed, and dried to obtain 82.6 g of colorless needle crystals-Brygonia alkyd, which was detected by HPLC with a purity of 93.2%, UV, IR, MS, 2 HNMR, 1...

Embodiment 2

[0032] Take 10Kg of the stem and root of the Cucurbitaceae melon plant loofah, add 5 times its mass of water, add cellulase, and enzymolyze it for 5 hours at a temperature of 50°C, a pH value of 6, and an enzyme amount of 40U / g crude drug, and heat to Boil and decoct for 1.5 hours, filter, take the filtrate, adsorb it through H50 macroporous adsorption resin, elute with 50% ethanol, collect 8 times the column volume eluate, and pass it through D201 strong basic styrene type anion exchange Resin adsorption, eluted with 0.5mol / L NaOH solution, collected and eluted, filtered, passed through D001 type strongly acidic styrene type cation exchange resin, collected effluent, filtered, and the filtrate was concentrated through an aromatic polyamide reverse osmosis membrane, Add methanol to crystallize, separate the crystals, wash, and dry to obtain 65.2 g of colorless needle crystals-bryonia alkyd, which was detected by HPLC with a purity of 94.9%, UV, IR, MS, 2 HNMR, 13 The data cha...

Embodiment 3

[0034] Take 10Kg of the stem and root of wax gourd, a melon plant of Cucurbitaceae, add 5 times its mass of water, add cellulase, and enzymolyze it for 3 hours under the conditions of temperature 45°C, pH value 4, enzyme amount 30U / g crude drug, and heat to Boil and decoct for 1 hour, filter, take the filtrate, absorb through AB8 macroporous adsorption resin, elute with 30% ethanol, collect 5 times the column volume eluate, pass through 201×7 strong basic styrene type Anion exchange resin adsorption, eluted with 0.5mol / L NaOH solution, collected and eluted, filtered, passed through 001×7 type strong acidic styrene type cation exchange resin, collected effluent, filtered, and the filtrate was compounded by triacetate fiber The reverse osmosis membrane was concentrated, methanol was added to crystallize, the crystals were separated, washed, and dried to obtain 102.6 g of colorless needle crystals-Brygonia alkyd, which was detected by HPLC with a purity of 96.8%, UV, IR, MS, 2 HN...

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Abstract

The invention relates to a method for preparing bryonia alcohol acid, which is convenient to operate and has the advantages of little pollution and low energy consumption. The method comprises the following steps of adding cucurbitaceous gourd stems and roots into cellulose for enzymolysis for 2 to 5 hours, heating to be boiled and decocting for 0.5 to 1.5 hours, filtering, taking filtering liquid, absorbing with macroporous absorption resin, eluting with ethanol, collecting eluting liquid of 3 to 8-time column measuring volume, absorbing with strongly basic styrene type anion exchange resin,eluting with 0.5 mol / L NaOH solution, collecting and eluting, filtering, absorbing with strong acid styrene type anion exchange resin, collecting flowing liquid, filtering, concentrating filtering liquid by using reverse osmosis membranes, adding methyl alcohol crystals, separating the crystals, washing and drying. When used for preparing the bryonia alcohol acid, the method can obtain high-purity products and is easy to realize industrial expansion.

Description

technical field [0001] The invention relates to a preparation method of bryonia alkyd, in particular to a preparation method of extracting bryogen alkyd from plants. Background technique [0002] Bryonia alkyd acid, alias: Baiyonic acid. English name: Bryonolic acid. Chemical name: 3-Hydroxy-8-multifloren-29-oicacid. [0003] Molecular formula: C 30 h 48 o 3 . Molecular weight: 456.707. Real molecular weight: 456.360345, percentage of each element: C 78.90%, H10.59%, O10.51%. [0004] CAS: 24480-45-3. [0005] The molecular formula is as follows: [0006] [0007] Modern studies have shown that purge root alkyd has multiple functions such as anti-inflammatory, moisturizing, promoting skin cell growth, whitening, etc., and it is also used as a raw material for the synthesis of other active derivatives. [0008] Studies have shown that bryonia alkyd acid mainly exists in various plants of Cucurbitaceae, and is also distributed in individual plants of Meliaceae and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
Inventor 刘东锋杨成东
Owner 江苏芝能生物科技有限公司