CN1872865A

CN1872865A - Method for picking up saponin of tea

Info

Publication number: CN1872865A
Application number: CNA2006100504066A
Authority: CN
Inventors: 方夏敏
Original assignee: Individual
Current assignee: Individual
Priority date: 2006-04-15
Filing date: 2006-04-15
Publication date: 2006-12-06
Anticipated expiration: 2026-04-15
Also published as: CN100393737C

Abstract

This invention discloses a method for extracting tea saponin by using tea dreg as the raw material and anhydrous methanol as the solvent. The method comprises: (1) pulverizing tea dreg; (2) placing in an immersing tank; (3) introducing 3 times of anhydrous methanol into the immersing tank from the bottom, and continuously extracting by reverse-cycling for 3 h; (4) removing the immersed solution from the bottom, filtering and introducing into an enamel reactor with a jacket; (5) adding 1/3 of ethyl ether to the reactor to obtain white precipitate of tea saponin; (6) sucking the supernatant from the reactor with an intubator in vacuum, and drying the precipitate in the reactor at 0-50 deg.C to obtain the final product. The method can extract tea saponin at a low temperature, thus preserving the active components of tea saponin. The obtain tea saponin has unchanged molecular structure and active components. Besides, the color is whit, and the color transfer problem can be avoided.

Description

A kind of extracting method of tea saponin

Technical field

The invention belongs to a kind of extracting method of chemical mixture, especially relate to a kind of extracting method of tea saponin.

Background technology

Tea saponin is a kind of crystal that is fine column in the leached tea oil slag that is present in, and its fusing point is 223-224 ℃, and bitter and pungent is soluble in aqueous methanol, aqueous ethanol isopolarity solvent, is insoluble to non-polar solvent.

The medical science aspect is mainly as impervious, antiphlogistic, but expelling phlegm for arresting cough, diuresis anti-inflammatory and anti-floating are swollen; Industrial aspect can be made WO emulsion, whipping agent, washing composition, shampoo etc. as a kind of good natural surface active agent; On pesticide industry, can make sterilant, farm chemical emulgent.

The extensive use of tea saponin make people to the research of tea saponin with utilize constantly pay attention to deeply.At present, the operational path that extracts tea saponin from leached tea oil slag is: with aqueous methanol or ethanol be immersed in the lixiviate tea dregs of rice under the 40-50 ℃ of condition → vat liquor filter → at pre-concentration under the 0-80 ℃ of condition → under 80-100 ℃ of condition, be condensed into red-brown glop → spraying drying → light brown powdery tea saponin.

There is defective in this extracting method: because tea saponin is formed by aglucon, sugared body and organic acid, has baroque mixture, because the existence of sugared body concentrating under the action of high temperature, very easily is oxidized to red-brown, so, the daily product that the tea saponin of producing with this method is produced is although for example wash the reason shampoo, the detergent scourability is good, washes the staining problem that there is tea saponin in the back fabric, do not approved by market that the application of farm chemical emulgent is also influenced because of the problem of color.

The color and luster problem of tea saponin has had a strong impact on its application in every respect, therefore, people are seeking the method that solves by every means for a long time, as: the someone attempts to adopt the method for decolouring to solve the color and luster problem, but, the decolouring detected result shows, the effective active content of tea saponin is almost nil, trace it to its cause: from its molecular structure, the part that the tea saponin activity is the strongest is the part that very easily forms color, that is to say, color has been removed, activity has not just had yet, and has influenced the performance of product.

CN200410046824.9 discloses " a kind of use water as solvent extracts tea saponin from cake of camellia oleifera seeds production method " this method with water as solvent, and comprises and adopt steps such as discoloring agent decolours.Its defective is: can occur impurity such as carbohydrate, protein, starch with water as solvent, therefore, the technological process of settlement separate, the separation of removing impurity, pre-filtering, press filtration must be arranged also in the step; Adopt discoloring agent technology can cause the effective active damage of tea saponin, thereby influence product performance.

Summary of the invention

For overcoming the above-mentioned deficiency of prior art, the present invention aims to provide a kind of extracting method of tea saponin, the tea saponin that extracts with this method has that molecular structure does not change, color and luster is the characteristics of white, thereby reached the purpose that keeps the tea saponin primary characteristic, also the staining problem can not occur with the daily necessities of its preparation.

For achieving the above object, the present invention has adopted following technical scheme, and a kind of extracting method of tea saponin is a solvent with the anhydrous methanol, may further comprise the steps:

1, tea waste is ground into particulate state, stand-by;

2, the tea waste particle is packed in the batch extractor

3, under 0-30 ℃ of condition, will place the anhydrous methanol of 3 times of amounts of a circulation tank to squeeze into the continuous extracting of reverse circulation 3 hours in advance from the jar end of batch extractor;

4, at the bottom of the batch extractor jar, extract leaching liquid out, squeeze into after the filtration in the enamel still of strap clamp cover;

5, in enamel still, add the ether of leaching liquid 1/3 amount, the tea saponin flocks that is white in color is separated out;

6, under vacuum condition, with the supernatant liquor sucking-off in the enamel still, the throw out evaporate to dryness under 0-50 ℃ of condition in the enamel still stirs to scrape through agitator and gets product with intubate.

During concrete enforcement, the particle diameter of pulverizing the back tea waste is less than or equal to 3cm.

During concrete enforcement, batch extractor adopts stainless material to make, and its volume is 1.5m*h2.0m.

Beneficial effect: the present invention compared with prior art, the present invention is solvent with the anhydrous methanol, thereby increase ether sedimentation technology and omitted enrichment step, the leaching process of tea saponin is finished under lower temperature all the time, to guarantee the active ingredient of tea saponin, product is separated out with white flocks, has avoided the color and luster problem, has solved the problem that never solves for a long time.

Embodiment

The present invention is when implementing, and concrete extracting method is as follows:

1, choose the tea waste that fresh nothing is gone mouldy, and with hammer mill it is crushed to diameter and is less than or equal to the 3cm particle, stand-by;

2, the particle that will pulverize the volume of packing into is in the stainless steel batch extractor of 1.5m*h2.0m;

3, under 0-30 ℃ of condition, the anhydrous methanol that leaves 3 times of amounts in the circulation tank in advance in is squeezed into the continuous extracting of reverse circulation 3 hours from the jar end of batch extractor with solvent pump;

[embodiment]:

1, adopt hammer mill that tea waste is ground into particle about the about 2cm of diameter, transport to conveying belt in the carbon steel storage tank of 10000L, then material is packed in the batch extractor of Stainless Steel Band chuck of φ 1.5m*h2.0m, the material amount should be suitable, is advisable with 85-90%.Adopting the hoirzontally rotating leaching will expect directly to transport to the leaching lattice gets final product.

2, will place the interior anhydrous methanol of a circulation tank in advance, squeeze at the bottom of the batch extractor jar with solvent pump, the amount of squeezing into is about 3 times of tea waste, anhydrous methanol overflows from the batch extractor upper end, forms circulation, and squeeze into pipeline and adopts aluminium matter at a jar end, and this pipeline soaked be embedded in the refrigerating fulid, make it to keep low temperature, under 15 ℃ of conditions, the continuous extracting of reverse circulation 3 hours.

3, leaching liquid is extracted out from the batch extractor bottom and is squeezed into after filtration the 2000L strap clamp cover enamel still.The remaining tea dregs of rice are heated through the batch extractor chuck, reclaim methyl alcohol by the condenser cooling, after the oven dry, and the discharging at the bottom of the movable batch extractor of the tea dregs of rice.

4, the ether that adds leaching liquid 1/3 amount in enamel still makes the tea saponin cotton-shaped precipitation fully that is white in color.

5, after precipitation leaves standstill, with intubate the supernatant liquor vacuum is drawn in another evaporating pot, ether (34.5 ℃ of boiling points) and methyl alcohol (64.65 ℃ of boiling points) are reclaimed in evaporation.

6, throw out is at vacuum 1Mpa, and quick evaporate to dryness reclaims residue methyl alcohol and ether under 40 ℃ of conditions.

7, after the cooling, the agitator made from high-temperature resistant rubber is scraped along the still wall and to be stirred dry thing, and white powdery tea saponin is emitted at the bottom of still.

Claims

1, a kind of extracting method of tea saponin is a solvent with the anhydrous methanol, may further comprise the steps:

(1), tea waste is ground into particulate state, stand-by;

(2), the tea waste particle is packed in the batch extractor;

(3), under 0-30 ℃ of condition, the anhydrous methanol of 3 times of amounts in the circulation tank is squeezed into the continuous extracting of reverse circulation 3 hours from the jar end of batch extractor;

(4), extract leaching liquid at the bottom of the batch extractor jar out, squeeze into after the filtration in the enamel still of strap clamp cover;

(5), in enamel still, add the ether of leaching liquid 1/3 amount, the tea saponin flocks that is white in color is separated out;

(6), under vacuum condition, with the supernatant liquor sucking-off in the enamel still, the throw out evaporate to dryness under 0-50 ℃ of condition in the enamel still stirs to scrape through agitator and gets product with intubate.

2, the extracting method of a kind of tea saponin as claimed in claim 1 is characterized in that: after the pulverizing, tea waste particulate diameter is less than or equal to 3cm.

3, the extracting method of a kind of tea saponin as claimed in claim 2 is characterized in that: batch extractor adopts stainless material to make, and its volume is 1.5m*h2.0m.