CN107376653A - A kind of method for reducing fouling membrane in Chinese medicine extract or waste water membrane separating process - Google Patents

A kind of method for reducing fouling membrane in Chinese medicine extract or waste water membrane separating process Download PDF

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Publication number
CN107376653A
CN107376653A CN201710866560.9A CN201710866560A CN107376653A CN 107376653 A CN107376653 A CN 107376653A CN 201710866560 A CN201710866560 A CN 201710866560A CN 107376653 A CN107376653 A CN 107376653A
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membrane
waste water
chinese medicine
medicine extract
separating process
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李博
郭立玮
朱华旭
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Nanjing University of Chinese Medicine
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Nanjing University of Chinese Medicine
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The present invention provides a kind of method for reducing fouling membrane in Chinese medicine extract or waste water membrane separating process, is related to Chinese medicine extract field of refinement.The method for reducing fouling membrane in Chinese medicine extract or waste water membrane separating process, including pre-processed using activated carbon to Chinese medicine extract or waste water, the step of activated carbon is then subjected to UF membrane together with Chinese medicine extract or waste water.The inventive method is simply easily operated, and cost is low, on the premise of ensureing that target component has compared with high transmittance, significantly improves membrane flux, shortens Refining times.

Description

A kind of method for reducing fouling membrane in Chinese medicine extract or waste water membrane separating process
Technical field
The present invention relates to Chinese medicine extract field of refinement, and in particular to one kind reduces Chinese medicine extract or waste water UF membrane mistake The method of fouling membrane in journey.
Background technology
Membrane science technology be material science with the subjects such as process engineering science intersect with reference to, interpenetrate and caused Frontier.Micro-filtration (MF), ultrafiltration (UF) and nanofiltration (NF) wherein are referred mainly to using the membrane technology of barometric gradient field, sieves effect One kind, i.e., using each constituent of mixture to be separated quality, volume size and geometric shape difference, it is different by aperture Film reach the purpose of separation.
Inoranic membrane (metal film, ceramic membrane etc.) possesses the advantage such as high mechanical strength, corrosion-resistant, acid and alkali-resistance, easy cleaning, thus It is used widely in Chinese herbal medicine industry.
In membrane separation technique practical application, most important problem is the fouling membrane occurred during use, and it shows as：Film Flux is constantly decayed with the time, if pollutant is more complicated, finally often leads to steady seepage flux only has pure water flux ten / mono-, it is even lower.
In recent years, research of the membrane separation technique in the field of Chinese medicines is increasing, but up to the present, the overwhelming majority is also Laboratory research level is rested on, process of industrialization seriously lags.It is to find out its cause, chemical mainly in Chinese traditional medicine water extract or waste liquid Composition is extremely complex, usually contains substantial amounts of polymer substance (such as starch, pectin, protein).In membrane filtration processes, this The presence of a little polymer substances inevitably causes the generation of fouling membrane phenomenon, so as to cause filtration resistance to increase, membrane flux Decline to a great extent.Due to the complexity of Chinese medicine extract, the degree of its fouling membrane seems compared with unclassified stores system to be particularly acute, And the mechanism of the separation and fouling membrane due to a lack of the theoretical research of system, particularly effective component of chinese medicine is failed to understand so far, serious system About industrialization of the technology in Chinese herbal medicine industry.The solution degree of membrane pollution problem, decides that film industrializes in the field of Chinese medicines The degree of application.How to mitigate the serious membrane pollution problem in Chinese medicine extract or waste liquid membrane process, become part in recent years The research emphasis of Chinese medicine researchers.
The content of the invention
, should it is an object of the invention to provide a kind of method for reducing fouling membrane in Chinese medicine extract or waste water membrane separating process Method is simply easily operated, and cost is low, on the premise of ensureing that target component has compared with high transmittance, significantly improves film and leads to Amount, shorten Refining times.
The purpose of the present invention adopts the following technical scheme that realization：
A kind of method for reducing fouling membrane in Chinese medicine extract or waste water membrane separating process, including using activated carbon to Chinese medicine Extract solution or waste water are pre-processed, the step of activated carbon then is carried out into UF membrane together with Chinese medicine extract or waste water.
In the present invention, in the membrane separating process, using inoranic membrane.
In preferable technical scheme, the inoranic membrane is ceramic membrane or metal film.
In the present invention, the Chinese medicine extract is huanglian jiedu decoction Aqueous extracts, and the waste water is that Mailuoning produces waste water.
In preferable technical scheme, the addition of active carbon powder is 5~80g in every liter of Chinese medicine extract or waste water, living The particle diameter of property carbon powder is 5 μm~1mm, and active carbon powder pretreatment time is 10~30min.
In preferable technical scheme, inoranic membrane is the CrO that aperture is 5~200nm2Ceramic membrane, effective membrane area are 0.005 ~1m2。
In preferred technical scheme, the inoranic membrane is the CrO that aperture is 5~80nm2Ceramic membrane, the active powdered carbon The particle diameter at end is 30 μm~80 μm.
In the present invention, in the membrane separating process, transmembrane pressure is 0.05~0.5mpa, and crossflow velocity is 0.5~4m/ S, -20 DEG C of operation temperature~120 DEG C.
By carrying out many experiments of UF membrane to Chinese medicine extract or waste water, inoranic membrane (ceramic membrane, metal film are found Deng) there is higher intensity, Chinese medicine extract or Pollutants in Wastewater can usually be formed on inoranic membrane surface to be deposited, so as to be formed Gel layer, the gel layer on film surface can reduce mass transfer rate, so as to influence membrane flux.The present invention uses active carbon powder first Chinese medicine aqueous extract or useless impurities in water are adsorbed, active carbon powder is then subjected to film together with Chinese medicine aqueous extract or waste water Lock out operation, i.e., active carbon powder is coupled into membrane separating process, on the premise of ensureing target component compared with high transmittance, significantly dropped Fouling membrane in low membrane separating process, improve membrane flux, to shorten sample processing time, cost low, simple to operate.
Brief description of the drawings
Fig. 1 cross-flow Porous Ceramics Membrane separator structural representations, wherein 1- storage tanks, 2- feed pumps, 3- tubular membrane groups Part, 4- flowmeters, 51- are the first valves, the valves of 52- second, the valves of 53- the 3rd, the valves of 54- the 4th, the valves of 55- the 5th, 56- 6th valve, 6- liquid medicine collecting grooves.
Tri- kinds of method membrane fluxs of Fig. 2 compare figure, and the wherein time refers to the time of UF membrane.
Embodiment
With reference to embodiment, the present invention will be further described, and theme protection domain involved in the present invention not only limits In these embodiments.
The method that embodiment 1 reduces fouling membrane in huanglian jiedu decoction Chinese traditional medicine water extract membrane separating process
1. prepare huanglian jiedu decoction Chinese traditional medicine water extract
It is prepared by the following method huanglian jiedu decoction Chinese traditional medicine water extract：According to mass parts, 9 parts of the coptis, golden cypress 6 are weighed respectively 9 parts of part, 6 parts of radix scutellariae and cape jasmine, add water to cook 2 times.1st amount of water is 10 times of medicinal material gross mass, decocts 1h；2nd time plus Water is 8 times of medicinal material gross mass, decocts 1h, filters while hot, merging filtrate, obtain huanglian jiedu decoction Chinese traditional medicine water extract.
In the prior art, huanglian jiedu decoction is refined usually using separation methods such as centrifugation, water extract-alcohol precipitations, due to coptis solution Malicious soup solution system is relative complex, existing a large amount of colloids, substantial amounts of solia particle again be present, and particle diameter distribution is wide in range, causes its film During flux decline it is fast, while active ingredient transmitance is undesirable.
2. UF membrane is carried out to huanglian jiedu decoction Chinese traditional medicine water extract using the inventive method
By huanglian jiedu decoction Chinese traditional medicine water extract (turbidity 1041NTU, viscosity 2.57mPas-1) use mistake as shown in Figure 1 Flow Porous Ceramics Membrane separator and carry out UF membrane.The separator core component is tubular membrane component 3, tubular membrane component 3 In seperation film select 19 duct CrO2Ceramic membrane (Jiangsu Jiuwu High-Tech Co., Ltd.), in the present embodiment, using hole Footpath is 50nm, effective membrane area 0.05m2Membrane sample.Cross-flow occurs at membrane module for Chinese traditional medicine water extract.
Specific method is as follows：
1. 8L huanglian jiedu decoction Chinese traditional medicine water extracts are fitted into storage tank 1, the active powdered carbon that particle diameter is 30 μm~80 μm is added Last 400g, the valve 52 of feed pump 2 and second is opened, other valves are closed, and circulate Chinese traditional medicine water extract in storage tank 1, so that The inner liquid medicine of storage tank 1 is uniform, and the circulation time of feed pump 2 is 15 minutes.The circulation of 15 minutes instead of stirring after activated carbon adds Mix so that activated carbon and decoction fully contact, and fully adsorb the impurity in decoction.
2. closing the second valve 52, the 3rd~the 6th valve 53,54,55,56 is opened, Chinese traditional medicine water extract in storage tank 1 is connected It is transported in tubular type membrane separation assemblies 3 by feed pump 2 with active carbon powder, is controlled by adjusting the five, the six valves 55,56 Transmembrane pressure and crossflow velocity, carry out membrane separating process using transmembrane pressure.Specifically, transmembrane pressure during UF membrane is 0.15mpa, crossflow velocity 3m/s, 30 DEG C of operation temperature, decoction cross-flow are returned in storage tank 1, followed by membrane module 3, trapped fluid Ring uses；It is collected into through the penetrating fluid of tubular membrane component 3 in collecting tank 6.The membrane flux in separation process is recorded, when film point It is 45min from the time, is collected into penetrating fluid 5.5L, terminates membrane separating process.Comparative indices composition transmitance, general character macromolecule Composition rejection.As a result Fig. 2, table 1 and 2 are seen.
3. carry out UF membrane using a pair of huanglian jiedu decoction Chinese traditional medicine water extracts of contrast method
Huanglian jiedu decoction Chinese traditional medicine water extract (in the present embodiment title 1 prepared by method) is more using cross-flow as shown in Figure 1 Duct ceramic membrane separation device carries out UF membrane.Seperation film in tubular membrane component 3 is the same as in the present embodiment title 2.
Specific method is as follows：8L huanglian jiedu decoction Chinese traditional medicine water extracts are fitted into storage tank 1, open the 3rd~the 6th valve 53rd, 54,55,56, other valves are closed, and the herb liquid of storage tank 1 is transported in membrane separation assemblies 3 by feed pump 2 and carries out film point From controlling transmembrane pressure and crossflow velocity by adjusting the five, the six valves 55,56, utilize transmembrane pressure to carry out UF membrane mistake Journey.Specifically, transmembrane pressure during UF membrane is 0.15mpa, crossflow velocity 3m/s, 30 DEG C of operation temperature, decoction cross-flow By membrane module 3, trapped fluid is returned in storage tank 1, is recycled；It is collected into through the penetrating fluid of membrane module 3 in collecting tank 6. The membrane flux in separation process is recorded, is 100min when the UF membrane time, is collected into penetrating fluid 5.5L, terminates membrane process.Compare Index composition transmitance, general character macromolecule component rejection.As a result Fig. 2, table 1 and 2 are seen.
4. UF membrane is carried out to huanglian jiedu decoction Chinese traditional medicine water extract using contrast method two
Huanglian jiedu decoction Chinese traditional medicine water extract (in the present embodiment title 1 prepared by method) is more using cross-flow as shown in Figure 1 Duct ceramic membrane separation device carries out UF membrane.Seperation film in tubular membrane component 3 is the same as in the present embodiment title 2.
Specific method is as follows：
1. 8L huanglian jiedu decoction Chinese traditional medicine water extracts are fitted into storage tank 1, the active powdered carbon that particle diameter is 30 μm~80 μm is added Last 400g, the valve 52 of feed pump 2 and second is opened, other valves are closed, and circulate Chinese traditional medicine water extract in storage tank 1, so that Storage tank inner liquid medicine is uniform, the 15 minutes circulation time of feed pump 2, active carbon powder is fully adsorbed the impurity in decoction.
2. closing the valve 52 of feed pump 2 and second, the first valve 51 is opened, Chinese traditional medicine water extract is released and active carbon powder mixes Compound, centrifugation, takes supernatant (i.e. the method for conventional activated carbon adsorption treatment Chinese traditional medicine water extract).
3. 2. supernatant that step is obtained is fitted into storage tank 1, open the valve 53 of feed pump 2 and the 3rd~the 6th, 54, 55th, 56, the herb liquid of storage tank 1 is transported in membrane separation assemblies 3 progress UF membrane operation by feed pump 2, by regulation the 5th, Six valves 55,56 control transmembrane pressure and crossflow velocity.Specifically, transmembrane pressure during UF membrane is 0.15mpa, film surface Flow velocity is 3m/s, 30 DEG C of operation temperature, and decoction cross-flow is returned in storage tank 1 by membrane module 3, trapped fluid, is recycled；Through film The penetrating fluid of component 3 is collected into collecting tank 6.The membrane flux in separation process is recorded, is 135min when the UF membrane time, is received Collect penetrating fluid 5.5L, terminate membrane process.Comparative indices composition transmitance, general character macromolecule component rejection.As a result figure is seen 2nd, table 1 and 2.
5. compare contrast method one, contrast method two and membrane flux in the inventive method disengaging time, separation process, refer to Mark property composition transmitance, general character macromolecule component rejection.
(1) comparison of membrane flux
As it is clear from fig. 2 that the inventive method (adsorbs active carbon powder coupling membrane separating process using active carbon powder Afterwards, active carbon powder is subjected to UF membrane together with decoction), film stabilized flux is significantly larger than contrast method one and contrast method Two.The film stabilized flux of contrast method one is 44.5L/m2H, the film stabilized flux of contrast method two is 63.5L/m2H, this The film stabilized flux of inventive method is 124.1L/m2H, contrast discovery, the inventive method film stabilized flux and contrast method one Compare, bring up to 279%, compared with contrast method two, bring up to 195%.The stabilized flux and pure water flux of the inventive method Compare, up to the 39.78% of pure water flux.
(2) comparison of UF membrane time
When obtaining 5.5L trapped fluids, the inventive method UF membrane time is used as 45min, using the UF membrane of contrast method one Time is 100min, uses the UF membrane time of contrast method two as 135min, therefore the inventive method significantly shorten UF membrane Time.
(3) comparison of index composition transmitance
After huanglian jiedu decoction Chinese traditional medicine water extract UF membrane, index composition transmitance is shown in Table 1.As can be seen from Table 1, relatively For contrast method one, using contrast method two, the rate of transform of 4 kinds of index compositions has a little reduction, it may be possible to due to portion Point index composition is tightly held by activated carbon；And the inventive method, 4 kinds of index composition transmitances have a certain degree of rise, Reason is probably：Active carbon powder washes away film surface as " rigid particles ", has cleaned the pollutant on film surface so that UF membrane During gel layer it is thinner, thus index composition readily penetrates through；In addition, the purpose of refined Chinese traditional medicine water extract be make index into Divide and general character macromolecule component is separated, in the membrane separating process of the inventive method, activated carbon can be to part general character high score Subconstiuent is adsorbed so that this balance tilts towards the direction for being advantageous to its separation.
The index composition transmitance table of table 1
(4) comparison of general character polymer substance clearance
From table 2, the inventive method may be such that general character polymer substance clearance improves compared with contrast method one 2.29%~17.16%.
The general character polymer substance clearance of table 2
In summary, membrane flux greatly improved by charcoal absorption and the coupling of membrane separating process in the inventive method, Processing time is saved, improves the transmitance of index composition and the clearance of general character macromolecule component, achieves and expects not The effect arrived.
The membrane separation of Nanjing medicine company Mailuoning production waste water of embodiment 2
In the waste line of Nanjing medicine company production MAILUONING ZHUSHEYE, collection in worksite MAILUONING ZHUSHEYE production waste water. MAILUONING ZHUSHEYE production waste water (turbidity 198.8NTU, viscosity 1.41mPas-1), from MAILUONING ZHUSHEYE production process In medicinal material cleaning, utensil cleaning, the multi unit operation such as alcohol precipitation.In order that MAILUONING ZHUSHEYE production waste water can be for follow-up money Sourceization recycles, and membrane separation is carried out using the inventive method in embodiment 1, to remove β-ecdysterone and chlorogenic acid.Together Contrast method one, contrast method two carry out membrane separation to MAILUONING ZHUSHEYE production waste water in Shi Caiyong embodiments 1.It is different Part is that seperation film selects 19 duct CrO in the present embodiment2Ceramic membrane (Jiangsu Jiuwu High-Tech Co., Ltd.), hole Footpath is 20nm, and effective membrane area is 0.05m2.The addition of active carbon powder is 1g/100ml waste water, and activated carbon is inhaled before UF membrane The attached time (i.e. the time of pump circulation) is 30 minutes.
As a result：Compared with contrast method one, the inventive method may be such that film stabilized flux is improved to 213%, β-husking steroid Ketone transmitance improves 15.2%, and chlorogenic acid transmitance improves 9.3%.Compared with contrast method two, the inventive method may be such that film Flux improves to 174%, β-ecdysterone transmitance and improves 17.5%, and chlorogenic acid transmitance improves 10.1%.5.5L is collected to ooze During transparent liquid, the UF membrane time in contrast method one is 300 minutes, and the UF membrane time in contrast method two is 270 minutes, this The UF membrane time in inventive method is 140 minutes.

Claims (8)

  1. A kind of 1. method for reducing fouling membrane in Chinese medicine extract or waste water membrane separating process, it is characterised in that including using activity Charcoal is pre-processed to Chinese medicine extract or waste water, and activated carbon then is carried out into UF membrane together with Chinese medicine extract or waste water The step of.
  2. 2. reducing the method for fouling membrane in Chinese medicine extract or waste water membrane separating process according to claim 1, its feature exists In the membrane separating process, using inoranic membrane.
  3. 3. reducing the method for fouling membrane in Chinese medicine extract or waste water membrane separating process according to claim 2, its feature exists In the inoranic membrane be ceramic membrane or metal film.
  4. 4. according to one of the claim 1-3 methods for reducing fouling membrane in Chinese medicine extract or waste water membrane separating process, its It is huanglian jiedu decoction Aqueous extracts to be characterised by the Chinese medicine extract, and the waste water is that Mailuoning produces waste water.
  5. 5. reducing the method for fouling membrane in Chinese medicine extract or waste water membrane separating process according to claim 4, its feature exists The addition of active carbon powder is 5 ~ 80g in every liter of Chinese medicine extract or waste water, and the particle diameter of active carbon powder is 5 μm ~ 1mm, Active carbon powder pretreatment time is 10 ~ 30min.
  6. 6. reducing the method for fouling membrane in Chinese medicine extract or waste water membrane separating process according to claim 5, its feature exists In inoranic membrane be aperture be 5 ~ 200nm CrO2Ceramic membrane, effective membrane area are 0.005 ~ 1 ㎡.
  7. 7. reducing the method for fouling membrane in Chinese medicine extract or waste water membrane separating process according to claim 6, its feature exists In the inoranic membrane be aperture be 5 ~ 80nm CrO2Ceramic membrane, the particle diameter of the active carbon powder is 30 μm ~ 80 μm.
  8. 8. reducing the method for fouling membrane in Chinese medicine extract or waste water membrane separating process according to claim 7, its feature exists In the membrane separating process, transmembrane pressure is 0.05 ~ 0.5mpa, and crossflow velocity is 0.5 ~ 4m/s, -20 DEG C of operation temperature ~ 120 ℃。
CN201710866560.9A 2017-09-22 2017-09-22 A kind of method for reducing fouling membrane in Chinese medicine extract or waste water membrane separating process Withdrawn CN107376653A (en)

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Cited By (1)

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CN117339396A (en) * 2023-11-24 2024-01-05 北京理工大学 Film pollution control method of hydrogel modified granular activated carbon coupling pattern film
CN117339396B (en) * 2023-11-24 2024-03-22 北京理工大学 Film pollution control method of hydrogel modified granular activated carbon coupling pattern film

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Application publication date: 20171124