CN102584529A - Alcohol recovering and concentrating process method of adsorption resin desorption solutions of plant extracts in membrane method - Google Patents

Alcohol recovering and concentrating process method of adsorption resin desorption solutions of plant extracts in membrane method Download PDF

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Publication number
CN102584529A
CN102584529A CN2011104455271A CN201110445527A CN102584529A CN 102584529 A CN102584529 A CN 102584529A CN 2011104455271 A CN2011104455271 A CN 2011104455271A CN 201110445527 A CN201110445527 A CN 201110445527A CN 102584529 A CN102584529 A CN 102584529A
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alcohol
plant milk
process method
milk extract
membrane
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CN2011104455271A
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王利祥
叶云飞
许萌
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Zhejiang Saite Membrane Technology Co Ltd
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Zhejiang Saite Membrane Technology Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Abstract

An alcohol recovering and concentrating process method of adsorption resin desorption solutions of plant extracts in a membrane method includes: after water solutions of the plant extracts pass through flocculent precipitating and plate frame filter pressing, filter liquor is desalted through ion exchange resin to become desalted filter liquor, effective contents in the plant extracts in the desalted filter liquor are absorbed through the resin, alcohol is used for desorbing the effective contents absorbed on the resin, after pretreatment, nanofiltration membranes with 150-250 molecular weight cutoff are adopted to concentrate and separate product eluent passing through adsorption columns, and subsequent reverse osmosis concentration is conducted for dilute plant extract solutions. Ethanol is recovered from the desorption solutions by aid of the membrane separation technique, and the alcohol recovering and concentrating process method has effects of energy conservation, high efficiency and environment-friendly production at normal temperature, improves concentration of effective components and simultaneously reduces content of impurities.

Description

A kind of embrane method of polymeric adsorbent desorbed solution of plant milk extract reclaims alcohol and concentrates process method
[technical field]
The present invention relates to a kind of membrane-concentrated technology, the recovery alcohol that is specifically related to a kind of polymeric adsorbent desorbed solution of a kind of plant milk extract that adopts embrane method concentrates process method.
[background technology]
Plant milk extract is to be raw material with the plant, according to needs to the ground that extracts, through physical chemistry extraction separation process, orientation obtain and the plant of concentrating in a certain or plurality of active ingredients, and do not change its effective constituent structure and the product that forms.Different according to the composition that extracts plant, form glucoside, acid, polyphenol, polysaccharide, terpene, flavones, vegeto-alkali etc.; Different according to proterties, can be divided into vegetables oil, medicinal extract, powder, lens etc.The conventional procedure of plant milk extract is that dried plant water purifying soaks, and leaching liquid behind double salt precipitation, removes protein, colloid, tannin and pigment etc. in anhydrating again, and the liquid of post precipitation reaches solid-liquid separation through Plate Filtration, sees through liquid and goes to make with extra care again.Subsequent process is a macroporous absorption, and alcohol is resolved, and desalination bleaching concentrates, and Sterile Filtration is dusted etc.The content that contains effective composition in the former plant milk extract production process in the desorbed solution is 0.1~2%; Methyl alcohol (ethanol) content is 25%~80%; Reclaim, adopt traditional distillation, evaporation technology for the methyl alcohol in the desorbed solution (ethanol), energy consumption is higher, and product quality Yin Gaowen is influenced.
[summary of the invention]
In order to overcome the deficiency that traditional plant extract desorbed solution alcohol reclaims, concentration technology exists; The invention provides a kind of membrane separation technique of utilizing and carry out plant milk extract desorbed solution alcohol recovery concentration technology method; This technology can realize at normal temperatures, cuts down the consumption of energy simultaneously, has improved effective constituent concentration; Improve production efficiency, had very strong practicality.
Technical problem to be solved by this invention is: the polymeric adsorbent desorbed solution of traditional plant milk extract reclaims, concentration technology adopts distillation, evaporation technology, and energy consumption is high, influences product quality simultaneously.
The technical scheme that the present invention adopted is: a kind of embrane method of polymeric adsorbent desorbed solution of plant milk extract reclaims alcohol and concentrates process method; Its process method be with the plant milk extract aqueous solution behind flocculation sediment and filter press; The desalination filtrating of filtrating after the ion exchange resin desalination is adopted the effective constituent of plant milk extract in the resin absorption desalination filtrating; With alcohol the effective constituent that is adsorbed on the resin is resolved then, content of effective is 0.1~2%, and pure content is 25%~80%; Adopt millipore filter to filter impurity in the desorbed solution; Adopting molecular weight cut-off after the pre-treatment is that the nf membrane of 150-250 is carried out concentrating and separating to the product elutriant through adsorption column, and the plant milk extract solution for rare goes follow-up reverse osmosis concentration; See through determining alcohol and be not less than 90% of charging determining alcohol, hold back greater than 99.5% through working substance in the liquid.
As preferably; The embrane method of the polymeric adsorbent desorbed solution of described a kind of plant milk extract reclaims alcohol and concentrates process method; It is characterized in that described plant milk extract comprises Folium Ginkgo extract, Pericarpium Citri tangerinae extract, Flos Carthami extract, Folium Chrysanthemi extract water soluble extract.
As preferably; The embrane method of the polymeric adsorbent desorbed solution of described a kind of plant milk extract reclaims alcohol and concentrates process method; It is characterized in that said stripping liquid is the aqueous solution that contains 0.2%~2.0% effective constituent, 5.0%~80.0% alcohol, small amount of impurities, alcohol comprises methyl alcohol and ethanol.
As preferably; The embrane method of the polymeric adsorbent desorbed solution of described a kind of plant milk extract reclaims alcohol and concentrates process method; It is characterized in that said millipore filter is high precision micron order metallic filter, ceramic capillary strainer, triumphant film filter, bohr membrane filtration.
As preferably; The embrane method of the polymeric adsorbent desorbed solution of described a kind of plant milk extract reclaims alcohol and concentrates process method; It is characterized in that described nf membrane is that molecular weight cut-off is NF270 film, the DK of Osmosis company, DL, the SG film of the Dow FilmTech company of 150-250.
As preferably, the embrane method of the polymeric adsorbent desorbed solution of described a kind of plant milk extract reclaims alcohol and concentrates process method, it is characterized in that described anti-seepage membrane is polyamide composite film, the Dow FilmTech company polyamide composite film of GE company.
As preferably; The embrane method of the polymeric adsorbent desorbed solution of described a kind of plant milk extract reclaims alcohol and concentrates process method, it is characterized in that, described nanofiltration membrane separation device be combined as one section of one section of one-level or secondary; The working pressure scope is 0.5MPa-6.0MPa, and TR is 5 ℃~55 ℃.
Beneficial effect of the present invention: adopt membrane separation technique that desorbed solution is reclaimed ethanol, this process is carried out at normal temperatures, need not steam; Reach effect energy-conservation, efficient, that environmental protection is produced; Seeing through liquid can recycle or to go rectifying tower to carry dense as elutriant without any processing, and liquid concentrator then continues to get into subsequent production workshop section, and this technology realizes separating of effective constituent and alcohol at normal temperatures; Make most of alcohol behind wash-out, can obtain reclaiming; And make the concentration of effective constituent improve 5~10 times, when improving effective constituent concentration, reduce the content of impurity.
Further understand characteristic of the present invention and technology contents for making, see accompanying drawing and embodiment for details, yet appended embodiment is only for reference and explanation usefulness, is not to be that the present invention is limited.
[description of drawings]
Fig. 1 is a process method flow chart of the present invention;
Fig. 2 is a filtration operation mode synoptic diagram of the present invention;
Fig. 3 is the process flow sheet of the nanofiltration liquid concentrator of reverse osmosis concentration plant milk extract of the present invention;
[embodiment]
With specific embodiment the present invention is elaborated below:
Embodiment 1, shown in Fig. 1-3, is 0.3% with 120L blueberry content; Ethanol content is that 60% desorbed solution carries out pre-treatment through the metallic filter that topping-up pump pumps into 0.45 μ m; Pump into NF270 nf membrane device through HPP at 1.0MPa through pretreated desorbed solution and circulate concentratedly, the stevioside content in the liquid concentrator is about 2.0%, and liquid concentrator then continues to get into reverse osmosis membrane and carries out further concentrating; The sugared concentration of liquid concentrator is about 40-50%, gets into follow-up treatment process; Reverse osmosis membrane sees through the liquid water white transparency, and blueberry content returns the extracting technology of front below 0.01%.Nf membrane sees through the liquid light-coloured transparent, and stevioside content is below 0.07%, sees through liquid and can recycle or mix with 95% without any processing and be made into certain concentration as elutriant.The average permeation flux of nf membrane is 24.5L/m 2H, the alcoholic acid recovery is more than 85%.Move after 1 month, film is cleaned once, can recover the processing power about 95%.
Embodiment 2; Shown in Fig. 1-3; With 200L stevioside content is 5.0%, and ethanol content is that 50% desorbed solution carries out pre-treatment through the metallic filter that topping-up pump pumps into 0.45 μ m, pumps into NF270 nf membrane device through HPP at 1.5MPa through pretreated desorbed solution and circulates concentrated; When be concentrated into the liquid stock volume 85% the time (the liquid concentrator volume is 30L), see through that concentration of ethanol is 43% in the liquid (1); Concentration of ethanol is 54% in the liquid concentrator, and the concentration of stevioside is about 30%.Adopting this moment the operating method of the diafiltration that adds pure water to carry out alcoholic acid reclaims; The add-on of pure water is the pure water of 20~25% (40-50L) of initial total feed liquid; While adding the water diafiltration; Continue then to be concentrated into that stevioside concentration is about 40% in the liquid concentrator, the liquid glucose that reclaims behind the ethanol goes the subsequent film concentration technology to handle.It is about 20% that nanofiltration this moment sees through the middle concentration of ethanol of liquid (2).It is dense that this part alcohol goes rectifying tower to carry, and sweet liquid returns and soaks operation or remove macropore at the bottom of the tower.Maybe will mix with 95% ethanol and be made into finite concentration as elutriant through liquid (1) with through liquid (2) mixing.The average permeation flux of nf membrane is 19.8L/m 2H, the recovery of methyl alcohol is more than 80%.After moving for 1 week, film is cleaned once, can recover the processing power about 90%.
Embodiment 3: according to above-mentioned same mode, several different plant milk extracts are handled under different operating conditions, can obtain following result:
Figure DEST_PATH_GSB00000780188600031
Adopt membrane separation technique that desorbed solution is reclaimed ethanol, this process is carried out at normal temperatures, need not steam; Reach effect energy-conservation, efficient, that environmental protection is produced; Seeing through liquid can recycle or to go rectifying tower to carry dense as elutriant without any processing, and liquid concentrator then continues to get into subsequent production workshop section, and this technology realizes separating of effective constituent and alcohol at normal temperatures; Make most of alcohol behind wash-out, can obtain reclaiming; And make the concentration of effective constituent improve 5~10 times, when improving effective constituent concentration, reduce the content of impurity.
Yet the preferable feasible embodiment of above-mentioned only the present invention, non-so limitation protection domain of the present invention is done various distortion or is applied mechanically all within this technical scheme protection domain according to the foregoing description.

Claims (7)

1. the embrane method of the polymeric adsorbent desorbed solution of a plant milk extract reclaims alcohol and concentrates process method; Its process method be with the plant milk extract aqueous solution behind flocculation sediment and filter press, the desalination filtrating of filtrating after the ion exchange resin desalination is adopted the effective constituent of plant milk extract in the resin absorption desalination filtrating, with alcohol the effective constituent that is adsorbed on the resin is resolved then; Content of effective is 0.1~2%; Alcohol content is 25%~80%, adopts millipore filter to filter impurity in the desorbed solution, and adopting molecular weight cut-off after the pre-treatment is that the nf membrane of 150-250 is carried out concentrating and separating to the product elutriant through adsorption column; For rare plant milk extract solution; Go follow-up reverse osmosis concentration, see through determining alcohol and be not less than 90% of charging determining alcohol, hold back greater than 99.5% through working substance in the liquid.
2. the embrane method of the polymeric adsorbent desorbed solution of a kind of plant milk extract according to claim 1 reclaims alcohol and concentrates process method; It is characterized in that described plant milk extract comprises Folium Ginkgo extract, Pericarpium Citri tangerinae extract, Flos Carthami extract, Folium Chrysanthemi extract water soluble extract.
3. the embrane method of the polymeric adsorbent desorbed solution of a kind of plant milk extract according to claim 1 reclaims alcohol and concentrates process method; It is characterized in that; Said stripping liquid is the aqueous solution that contains 0.2%~2.0% effective constituent, 5.0%~80.0% alcohol, small amount of impurities, and alcohol comprises methyl alcohol and ethanol.
4. the embrane method of the polymeric adsorbent desorbed solution of a kind of plant milk extract according to claim 1 reclaims alcohol and concentrates process method; It is characterized in that said millipore filter is high precision micron order metallic filter, ceramic capillary strainer, triumphant film filter, bohr membrane filtration.
5. the embrane method of the polymeric adsorbent desorbed solution of a kind of plant milk extract according to claim 1 reclaims alcohol and concentrates process method; It is characterized in that described nf membrane is that molecular weight cut-off is NF270 film, the DK of Osmosis company, DL, the SG film of the Dow FilmTech company of 150-250.
6. the embrane method of the polymeric adsorbent desorbed solution of a kind of plant milk extract according to claim 1 reclaims alcohol and concentrates process method, it is characterized in that described anti-seepage membrane is polyamide composite film, the Dow FilmTech company polyamide composite film of GE company.
7. the embrane method of the polymeric adsorbent desorbed solution of a kind of plant milk extract according to claim 1 reclaims alcohol and concentrates process method; It is characterized in that; Described nanofiltration membrane separation device be combined as one section of one section of one-level or secondary; The working pressure scope is 0.5MPa-6.0MPa, and TR is 5 ℃~55 ℃.
CN2011104455271A 2011-12-28 2011-12-28 Alcohol recovering and concentrating process method of adsorption resin desorption solutions of plant extracts in membrane method Pending CN102584529A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106630350A (en) * 2016-12-26 2017-05-10 赛鼎工程有限公司 Zero-drainage technology of biochemical effluent water deep treatment and resource recycling of coal chemical industry wastewater
CN113975968A (en) * 2021-11-29 2022-01-28 四川和诚过滤科技集团有限公司 Membrane concentration ethanol recovery equipment for industrial hemp alcohol extract

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1112565A (en) * 1995-03-06 1995-11-29 北京市环境保护科学研究院 Technology for extracting stevioside by membrane method combined technique
CN101117345A (en) * 2007-08-29 2008-02-06 南京九思高科技有限公司 Method for extracting stevioside
CN101774989A (en) * 2009-02-04 2010-07-14 王来忠 Preferable method for extracting refined yellow pigment from red flowers

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1112565A (en) * 1995-03-06 1995-11-29 北京市环境保护科学研究院 Technology for extracting stevioside by membrane method combined technique
CN101117345A (en) * 2007-08-29 2008-02-06 南京九思高科技有限公司 Method for extracting stevioside
CN101774989A (en) * 2009-02-04 2010-07-14 王来忠 Preferable method for extracting refined yellow pigment from red flowers

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106630350A (en) * 2016-12-26 2017-05-10 赛鼎工程有限公司 Zero-drainage technology of biochemical effluent water deep treatment and resource recycling of coal chemical industry wastewater
CN113975968A (en) * 2021-11-29 2022-01-28 四川和诚过滤科技集团有限公司 Membrane concentration ethanol recovery equipment for industrial hemp alcohol extract
CN113975968B (en) * 2021-11-29 2024-02-06 四川和诚过滤科技集团有限公司 Membrane concentration ethanol recovery equipment for industrial cannabis ethanol extract

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Application publication date: 20120718