CN102746939A - Method for extracting tea saponin and tea seed oil with mixed solvent - Google Patents
Method for extracting tea saponin and tea seed oil with mixed solvent Download PDFInfo
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- CN102746939A CN102746939A CN2012102453647A CN201210245364A CN102746939A CN 102746939 A CN102746939 A CN 102746939A CN 2012102453647 A CN2012102453647 A CN 2012102453647A CN 201210245364 A CN201210245364 A CN 201210245364A CN 102746939 A CN102746939 A CN 102746939A
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Abstract
The invention provides a method for simultaneously extracting tea saponin and tea seed oil in tea seed cakes with a mixed solvent. The method is characterized by the steps of: after grinding squeezed tea seed cakes in a grinder, putting a certain quantity of ground tea seed cakes into a flask to be mixed with a certain volume of ethanol water and a normal hexane mixed solvent; carrying out continuous extraction in a rotary evaporator at 55-60 DEG C, wherein the ethanol concentration is 60-80%(V/V); the feed-liquid ratio is (2:1)-(5:1), the volume ratio of ethanol water to normal hexane is (7:3)-(4:6), the extraction time is 90-180 minutes for each time; and carrying out standing and layering on extracted mixed oil at 10-40 DEG C to obtain a normal hexane-tea seed oil phase on an upper layer and an ethanol water-tea saponin phase on a lower layer, evaporating the two phases respectively to obtain tea saponin and tea seed oil, and recycling the solvent. For extracted meal, the content of residual saponins is less than 1% and the content of residual oil is less than 1.5%. The yield of crude saponins is 20.9-36.9%. The crude saponins are light yellow powder and have purity being more than 60%.
Description
Technical field
The present invention relates to tea saponin and the selection of oily mixed solvent extracting condition, the recovery of mixed solvent and the method that adopts this mixed solvent while lixiviate tea saponin and tea-seed oil in the tea seed cake.
Background technology
Nearly 1,000,000 tons of annual tea seed cake (tea-seed pancake and the tealeaves seedcake) output of China; Tea seed cake contains a certain amount of tea saponin and tea-seed oil etc.; Wherein tea saponin is a kind of good natural surface active agent; Have kinds of surface activity such as emulsification, dispersion, wetting, decontamination, foaming, steady bubble, and do not receive the influence of water hardness.Ethanol-normal hexane mixed solvent single stage method is extracted tea saponin does not still have publication at present, and bibliographical information is only arranged.Zhong Haiyan etc. adopt the tea saponin in 95% ethanol-normal hexane mixed solvent lixiviate oleifera dry cake, and the extract technology condition is: oil cake contains saponin 8.6%, oil-containing 4.7%; The oil cake granularity is 1～3 mm, 58 ℃ of extraction temperatures, and solvent volume and oil cake mass ratio are 2:1; The ethanol volume(tric)fraction is 95%; The volume ratio 5:5 of 95% ethanol and hexane, extraction time 5h, the yield of Residual oil and oil tea saponin is respectively 3.6% and 7.0% (extraction yield 81.4%).This process limitations must adopt high concentration ethanol (95%) just can reach above extracting effect.One of problem that this technology is maximum is that extraction time is long, optimised process extraction time 5h; And present grease extraction time is generally at 60～90min; Therefore this technology is bigger to the grease lixiviating process influence, is mainly reflected in the oil extraction equipment of same scale, and the treatment capacity that adopts this explained hereafter is 1/5 of normal grease leaching; The cost that greases such as water power vapour consumption simultaneously leach significantly increases, be unfavorable for existing extract technology and equipment bonded basis on carry out industrial applications.Two of problem is, because mixed solvent adopts 95% ethanol, follow-up ethanol recovery needs to increase rectifying device, and facility investment increases, and complicated operation increases solvent recuperation loss and cost.
Summary of the invention
The purpose of this invention is to provide a kind of safe, efficiently, adopt the method for tea saponin and tea-seed oil in low volume fraction ethanol-normal hexane mixed solvent lixiviate simultaneously tea seed cake.
Technical scheme of the present invention is: the method for tea saponin and tea-seed oil in the mixed solvent lixiviate simultaneously tea seed cake, it is characterized in that squeezing tea seed cake after kibbler is pulverized, and get a certain amount of flask that places; Mix with the aqueous ethanolic solution and the normal hexane mixed solvent of certain volume, under 55～60 ℃ condition, continuous extraction in rotatory evaporator; During lixiviate, ethanol volume(tric)fraction 60～80%, solid-liquid ratio 2:1～5:1; The volume ratio 7:3 of aqueous ethanolic solution and normal hexane～4:6, extraction time 90～120 min, lixiviate number of times 1 time; Leach mixing oil at 10～40 ℃ of standing demix, the upper strata is normal hexane-tea-seed oil phase, and lower floor is aqueous ethanolic solution-tea saponin phase; Evaporate respectively tea saponin and tea-seed oil, reclaim the solvent cycle utilization.
Leach in the dregs of rice residual saponin content less than 1%, Residual oil is less than 1.5%, saponin yield 90%～98.9%, and thick saponin is a pale yellow powder, purity is greater than 60%.
Compared with present technology the present invention has the following advantages:
(1) the present invention is guaranteeing to leach under the prerequisite of the low Residual oil of the dregs of rice, and tea saponin extraction yield (90%～98.9%) is higher than the yield (81.4%) of existing extractive technique.
(2) this process using lower concentration (60～80%) ethanol-normal hexane mixed solvent; Broken through and required the necessary restriction more than 85% of alcoholic acid volume(tric)fraction during the conventional hybrid solvent once leaches; And short 2h of extraction time; And existing technology be 5h, and compared with present technology the cost of leaching significantly reduces, thus be more conducive to existing extract technology and equipment bonded basis on carry out the industrialization promotion application.
(3) the present invention adopts low volume fraction ethanol-normal hexane mixed solvent; Not only can leach the tea saponin in the cake to greatest extent; And ethanol recovery Processes and apparatus is simple, easy to operate; Problems such as the facility investment of having avoided the employing distillation operation to bring is big, complicated operation, thereby reduced production cost, be easier to further suitability for industrialized production.
(4) the present invention leaches mixing oil and is approaching standing demix under the condition of normal temperature, and layering is thorough, and energy is more saved in relative 95% ethanol-normal hexane mixing oil layering.
(5) the processing condition scope of application of the present invention is more wide in range, does not extract when not being only applicable to grease and the saponin of tea-seed pancake, and is applicable to tealeaves seedcake.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing and instance the present invention is described further.
The good characteristics of effect when the present invention utilizes in the mixed solvent each component to leach in the oil plant respective components and its leaching effect respectively to leach than single solvent; Selecting aqueous ethanolic solution and normal hexane is mixed solvent, selects best extract technology condition and mixed solvent recovery technology through testing sieve.
1 technology and equipment
1.1 supplementary material
The squeezing tea seed cake: oil-containing 9.0% contains tea saponin 19.1%, moisture 4.1%.
95% ethanol, analytical pure; Normal hexane, analytical pure; First water.
1.2 main testing installation
Rotatory evaporator, microphyte sample kibbler, Soxhlet extractor, loft drier, thermostat water bath, recirculated water are used vacuum pump, electronic balance more.
2 experimentations and conclusion
2.1 raw material is handled
The squeezing tea seed cake is pulverized through microphyte sample kibbler, and grinding particle size is less than 5 mm, and is subsequent use.
2.2 the selection of optimum process condition
The squeezing tea seed cake is after kibbler is pulverized; Get a certain amount of flask that places; Mix with the aqueous ethanolic solution and the normal hexane mixed solvent of certain volume; Under 55～60 ℃ of conditions, continuous extraction in rotatory evaporator is investigated the influence to leaching effect of volume ratio, extraction time and the solid-liquid ratio of ethanol volume(tric)fraction, aqueous ethanolic solution and normal hexane.The processing condition of confirming are: ethanol volume(tric)fraction 60～80%, and the volume ratio 7:3 of aqueous ethanolic solution and normal hexane～4:6 (V/V), extraction time 60～120min, solid-liquid ratio 1:1～5:1, extraction temperature are 55～60 ℃.
2.3 mixed solvent reclaims
The lixiviate mixing oil leaves standstill certain hour at a certain temperature, and mixing oil is divided into two-layer, and the upper strata is tea-seed oil-normal hexane phase, and lower floor is tea saponin-aqueous ethanolic solution phase, respectively to evaporating mutually up and down, gets tea-seed oil and tea saponin respectively.The processing condition of confirming are: separation time 5～10min, stratification temperature are 10～40 ℃, and last phase vaporization temperature is 70～105 ℃, and following phase vaporization temperature is 80～105 ℃.
2.4 experiment conclusion
Tea saponin and tea-seed oil in the mixed solvent of employing low volume fraction aqueous ethanolic solution and the normal hexane lixiviate simultaneously tea seed cake; Under certain extracting condition, residual saponin is less than 1% in the leaching leached tea oil slag, and Residual oil is less than 1.5%; The extraction yield of saponin is 90%～98.9%, and thick saponin purity is greater than 60%.The mixing of this explanation aqueous ethanolic solution and normal hexane is used and can be extracted tea saponin and the tea-seed oil in the tea seed cake efficiently, improves actual production efficient, and can obtain high-quality tea saponin and tea-seed oil.
Embodiment 1
The squeezing tea seed cake 50g that pulverizes mixes in flask with 60% ethanol and the normal hexane mixed solvent (60% ethanol is 1:1 with the volume ratio of normal hexane) of 100mL; Under 55～60 ℃ condition in rotatory evaporator a lixiviate 120min; Residual saponin is 0.7% in the leaching dregs of rice; Residual oil is 2.1%, and the saponin extraction yield is 97.3%, and thick saponin purity is 60.2%.
Get and leach mixing oil 100mL in Erlenmeyer flask, standing demix 10min in the time of 30 ℃ changes over to and separates levels in the separating funnel; Respectively to evaporating mutually up and down; Last phase vaporization temperature is 105 ℃, and following phase vaporization temperature is 105 ℃, gets tea-seed oil and thick tea saponin respectively.Oleaginousness is 0.12% in the tea saponin.
Embodiment 2
The squeezing tea seed cake 50g that pulverizes mixes in flask with 70% ethanol and the normal hexane mixed solvent (70% ethanol is 1:1 with the volume ratio of normal hexane) of 150mL; Under 55～60 ℃ condition in rotatory evaporator a lixiviate 120min; Residual saponin is 0.5% in the leaching dregs of rice; Residual oil is 0.8%, and the saponin extraction yield is 98.1%, thick saponin purity 61.1%.
Get and leach mixing oil 100mL in Erlenmeyer flask, standing demix 10min in the time of 30 ℃ changes over to and separates levels in the separating funnel; Respectively to evaporating mutually up and down; Last phase vaporization temperature is 105 ℃, and following phase vaporization temperature is 105 ℃, gets tea-seed oil and thick tea saponin respectively.Oleaginousness is 0.12% in the tea saponin.
Embodiment 3
The squeezing tea seed cake 50g that pulverizes mixes in flask with 70% ethanol and the normal hexane mixed solvent (70% ethanol is 1:1 with the volume ratio of normal hexane) of 250mL; Under 55～60 ℃ condition in rotatory evaporator a lixiviate 120min; Residual saponin is 0.3% in the leaching dregs of rice; Residual oil is 0.4%, and the saponin extraction yield is 98.9%, thick saponin purity 60.3%.
Get and leach mixing oil 100mL in Erlenmeyer flask, standing demix 10min in the time of 10 ℃ changes over to and separates levels in the separating funnel; Respectively to evaporating mutually up and down; Last phase vaporization temperature is 105 ℃, and following phase vaporization temperature is 105 ℃, gets tea-seed oil and thick tea saponin respectively.Oleaginousness is 0.04% in the tea saponin.
More than content of the present invention has been carried out detailed introduction, and used concrete example among this paper principle of the present invention and embodiment set forth, the explanation of above embodiment just is used for helping understanding method of the present invention and core concept.Should be pointed out that for those skilled in the art, do not breaking away under the prerequisite of the present invention, can also carry out some improvement and modification, equally also fall in the protection domain of claim of the present invention invention.
Claims (2)
1. a mixed solvent extracts the method for tea saponin and tea-seed oil, it is characterized in that squeezing tea seed cake after the kibbler pulverizing, gets a certain amount of flask that places; Mix with the aqueous ethanolic solution and the normal hexane mixed solvent of certain volume, under 55～60 ℃ condition, continuous extraction in rotatory evaporator; During lixiviate, ethanol volume(tric)fraction 60～80%, solid-liquid ratio 2:1～5:1; The volume ratio of aqueous ethanolic solution and normal hexane is 7:3～4:6, extraction time 90～120 min, lixiviate number of times 1 time; Leach mixing oil at 10～40 ℃ of standing demix, the upper strata is normal hexane-tea-seed oil phase, and lower floor is aqueous ethanolic solution-tea saponin phase; Evaporate respectively tea saponin and tea-seed oil, reclaim the solvent cycle utilization.
2. extract the method for tea saponin and tea-seed oil like claims 1 described mixed solvent, it is characterized in that: said squeezing tea seed cake flour granularity is less than 3mm, and said squeezing tea seed cake comprises pressed oil tea seed cake and tealeaves seedcake.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103060084A (en) * | 2013-01-27 | 2013-04-24 | 管天球 | Method for leaching and processing residual oil of tea cakes |
| CN104479853A (en) * | 2014-11-27 | 2015-04-01 | 晨光生物科技集团股份有限公司 | Industrial production method for simultaneously extracting tea seed oil and tea saponin |
| CN108893203A (en) * | 2018-06-26 | 2018-11-27 | 安徽山美生物科技有限公司 | A kind of granulation of Oil-tea-cake dust, which is leached, goes Residual oil technique |
| CN108997471A (en) * | 2018-09-17 | 2018-12-14 | 中国科学院青岛生物能源与过程研究所 | A kind of environment-friendly preparation method thereof of high-purity tea saponin |
| CN110726688A (en) * | 2019-10-30 | 2020-01-24 | 闽江学院 | Extraction method and application of unsaponifiable vegetable oil |
| CN111018939A (en) * | 2019-12-16 | 2020-04-17 | 中国科学院青岛生物能源与过程研究所 | Rapid refining method of tea saponin |
| CN111394177A (en) * | 2020-03-30 | 2020-07-10 | 山东凯斯达机械制造有限公司 | Process for extracting soybean mixed oil and soybean liquid by using mixed solvent |
| CN111592578A (en) * | 2020-05-29 | 2020-08-28 | 信阳师范学院 | Process for extracting tea saponin from camellia sinensis dregs and application of tea saponin in amino acid facial soap |
| CN112048379A (en) * | 2020-09-16 | 2020-12-08 | 湖南一代伟仁科技有限公司 | One-step method for extracting tea saponin and preparing tea oil |
| CN112679556A (en) * | 2020-12-29 | 2021-04-20 | 青岛职业技术学院 | Production process of high-purity tea saponin |
| CN114685598A (en) * | 2022-04-07 | 2022-07-01 | 合肥工业大学 | Method for synchronously extracting camellia oleifera cake residual oil and tea saponin |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103060084A (en) * | 2013-01-27 | 2013-04-24 | 管天球 | Method for leaching and processing residual oil of tea cakes |
| CN104479853A (en) * | 2014-11-27 | 2015-04-01 | 晨光生物科技集团股份有限公司 | Industrial production method for simultaneously extracting tea seed oil and tea saponin |
| CN104479853B (en) * | 2014-11-27 | 2017-06-27 | 晨光生物科技集团股份有限公司 | It is a kind of while extracting the industrialized preparing process of tea-seed oil and Tea Saponin |
| CN108893203A (en) * | 2018-06-26 | 2018-11-27 | 安徽山美生物科技有限公司 | A kind of granulation of Oil-tea-cake dust, which is leached, goes Residual oil technique |
| CN108997471B (en) * | 2018-09-17 | 2021-02-19 | 中国科学院青岛生物能源与过程研究所 | Green preparation method of high-purity tea saponin |
| CN108997471A (en) * | 2018-09-17 | 2018-12-14 | 中国科学院青岛生物能源与过程研究所 | A kind of environment-friendly preparation method thereof of high-purity tea saponin |
| CN110726688A (en) * | 2019-10-30 | 2020-01-24 | 闽江学院 | Extraction method and application of unsaponifiable vegetable oil |
| CN111018939A (en) * | 2019-12-16 | 2020-04-17 | 中国科学院青岛生物能源与过程研究所 | Rapid refining method of tea saponin |
| CN111394177A (en) * | 2020-03-30 | 2020-07-10 | 山东凯斯达机械制造有限公司 | Process for extracting soybean mixed oil and soybean liquid by using mixed solvent |
| CN111592578A (en) * | 2020-05-29 | 2020-08-28 | 信阳师范学院 | Process for extracting tea saponin from camellia sinensis dregs and application of tea saponin in amino acid facial soap |
| CN111592578B (en) * | 2020-05-29 | 2021-11-19 | 信阳师范学院 | Process for extracting tea saponin from camellia sinensis dregs and application of tea saponin in amino acid facial soap |
| CN112048379A (en) * | 2020-09-16 | 2020-12-08 | 湖南一代伟仁科技有限公司 | One-step method for extracting tea saponin and preparing tea oil |
| CN112679556A (en) * | 2020-12-29 | 2021-04-20 | 青岛职业技术学院 | Production process of high-purity tea saponin |
| CN112679556B (en) * | 2020-12-29 | 2023-10-24 | 青岛职业技术学院 | Production process of high-purity tea saponin |
| CN114685598A (en) * | 2022-04-07 | 2022-07-01 | 合肥工业大学 | Method for synchronously extracting camellia oleifera cake residual oil and tea saponin |
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Application publication date: 20121024 |