CN101914123A - Method for recovering natamycin from waste liquid - Google Patents
Method for recovering natamycin from waste liquid Download PDFInfo
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- CN101914123A CN101914123A CN 201010292080 CN201010292080A CN101914123A CN 101914123 A CN101914123 A CN 101914123A CN 201010292080 CN201010292080 CN 201010292080 CN 201010292080 A CN201010292080 A CN 201010292080A CN 101914123 A CN101914123 A CN 101914123A
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- tennecetin
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Abstract
The invention relates to a method for recovering natamycin from waste liquid produced in the natamycin extraction process, which is characterized in that the natamycin is acquired by carrying out processes of adsorption, desorption, crystallization, separation and drying on the waste liquid. The method for recovering the natamycin from the waste liquid can improve the production yield of the natamycin and the biochemical treatment rate, reduce the extraction cost, the natamycin content in discharged waste liquid, the inhibition of the natamycin to fungi microorganisms in a waste liquid biochemical treatment process, the discharge of COD (Chemical Oxygen Demand) and BOD (Biological Oxygen Demand),ensure the normal operation of the device for biochemical treatment of industrial waste water, and not only reduces the cost, but also is green and environmental-friendly.
Description
Technical field
The present invention relates to the extracting method of microbial product, refer in particular to the method that reclaims tennecetin in a kind of discarded liquid that from the tennecetin leaching process, produces.
Background technology
Tennecetin (Natamycin) is a kind of polyene macrolide antibiotics, it be adopt the Na Taer streptomycete (
Streptomysis natalensis), brown yellow spore streptomycete (
Streptomysis gilvosporeus) or streptomyces chatanoogensis (
Streptomyces chattanoogensis) fermentation secondary metabolite under controlled condition.Because it can suppress fungi growth such as yeast, mould, so tennecetin has more special meaning to foodstuffs industry.Some fungi can produce mycotoxins, mycotoxins to the mankind carcinogenic, teratogenesis is arranged, cause the shake mountain peak, cause hemorrhage, cause effect such as dermatitis.Therefore, tennecetin is used for food mould-proof not only can solve food spoilage, can also reduce the murder by poisoning of mycotoxins to the mankind.Tennecetin not only is used for the mildew-resistant of food and anticorrosion, but also is used to prevent and treat the fungi infestation of skin and eye, and the application in feed and livestock-raising also has report in the recent period.
The solubleness of tennecetin in water is extremely low, in the medium-sized scope of pH=5.5-7.5, solubleness between the temperature 25-45 degree in water is 50-110ppm, the content of tennecetin is generally 5.0 grams per liters-8 grams per liter in the fermented liquid, wherein the overwhelming majority with the forms of crystallite be present in the fermented liquid, in the microorganism cells or be adsorbed in the surface of microorganism.
Since people such as nineteen fifty-five Struyk found tennecetin, people constantly explored the separation method of tennecetin from fermented liquid always.
U.S. Pat 3,892,850 report organic solvent methods extract tennecetin, the pH of fermented liquid is transferred to 10 makes tennecetin separate from mycelium, remove by filter mycelium, in filtrate, add propyl carbinol then, pH is controlled between the 3-10, can the throw out that form can be proposed in case of necessity with phosphoric acid with its acidifying.Last constant boiling point evaporation obtains rough tennecetin.Afterwards, can select different organic solvents, for example Glacial acetic acid, pyridine, dimethyl formamide etc. are further purified.
U.S. Pat P337844 adopts the method for saltouing to separate tennecetin from fermented liquid, and is aided with organic solvent dissolution and precipitation.
World patent WO/9210580, WO95/07998 have announced and have adopted low pH value methanol extraction tennecetin, obtained the method for tennecetin then at readjustment pH.
Chinese patent CN1094979C has announced that employing enzyme, acid, the broken biomass cells of alkali remove deproteinize, improve or reduce the method that the pH value obtains tennecetin then.
Chinese patent CN101062934 discloses a kind of method of extracting tennecetin from fermented liquid: under 0-35 ℃ of condition fermenting culture is regulated the pH value to 10.0-14.0 with alkaline matter, stir; Solid-liquid separation is collected filtrate and is obtained the tennecetin aqueous extract; The tennecetin precipitation was separated out the crystal solution that obtains tennecetin when filtrate pH value was regulated in acidifying to 5.0-9.0 under the normal temperature; Crystal solution obtains the tennecetin product through solid-liquid separation.
Above method does not all relate in the leaching process recovery method of residual tennecetin in the tennecetin parting liquid.The content of residual tennecetin accounts for 2-10% of fermentation yield at 100-800ppm in the tennecetin parting liquid, and other material is the glucose of 0.5%-2.5% and the protein of 0.1%-1.5%.It is difficult that the tennecetin of low levels like this takes ordinary method to separate, purify.This part tennecetin does not reclaim the production cost that can improve tennecetin, the more important thing is after tennecetin enters biochemical sewage treatment device yeast, mould specificity are suppressed, and influence the activity of flora in the waste disposal plant, and reduce sewage biochemical treatment efficient, influence wastewater treatment efficiency.
Summary of the invention
Reclaim the method for tennecetin in a kind of discarded liquid that from the tennecetin leaching process, produces that purpose of the present invention provides at existing problem in the above-mentioned prior art just, can improve the extract yield of tennecetin, the content that tennecetin in the liquid is discarded in minimizing, guarantee the normal operation of the device of plant effuent biochemical treatment.
The objective of the invention is to be achieved through the following technical solutions: the method that reclaims tennecetin in a kind of discarded liquid that from the tennecetin leaching process, produces, it is characterized in that: will discard liquid and obtain tennecetin by absorption, desorption, crystallization, separation drying process, its concrete steps are as follows:
(1) absorption: by the adsorption column that sorbent material is housed discarded liquid is adsorbed under 10 ℃-50 ℃, pH=4.0-7.5, the adsorption column volume is the 0.1-4.0% of fermentating liquid volume;
(2) desorption: with the water washing adsorption column of 1-5 times of adsorption column volume, with the stripping liquid desorption agent post of 1-3 adsorption column volume doubly, stripping liquid is organic solvent or the water-containing organic solvent of pH=1.8-2.5 or pH=9.5-11.5 then;
(3) crystallization: with the stripping liquid after the desorption, use acid or adjusting PH with base between the 5.0-7.5, temperature is reduced to-10 ℃ to 10 ℃, stirs 5-24 hour;
(4) separate drying: crystallization finishes to adopt the method for filtration, gravity settling or centrifugal settling to obtain the tennecetin crystallization, and vacuum-drying obtains the tennecetin product after water or the organic solvent washing.
In the present invention, the organic solvent as stripping liquid described in the step 2 is any one in methyl alcohol, ethanol, propyl alcohol, Virahol, glycerine, methane amide, dimethyl formamide, N-methylpyrroline or the Glacial acetic acid.
The organic solvent of step (4) washing usefulness is acetone, ethanol, methylene dichloride or tetrachloromethane, pH scope=5.5-7.5.Sorbent material described in the step (1) is at least a or two above compositions in diatomite, expanded pearlite salt, gac, macroporous resin, ion exchange resin or the adsorbing fiber element.
Present method adopts absorption, desorb, crystallization, exsiccant method to obtain tennecetin, can improve the content of producing yield, reducing cost, reduce tennecetin in the discharging waste liquid, reduce the inhibition of tennecetin to fungi microbe in the waste liquid biochemical treatment, improve the biochemical treatment rate, reduce the discharging of COD, BOD.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
The present invention is described further below in conjunction with accompanying drawing (embodiment):
Embodiment 1
Method of the present invention provides with the technology that reclaims tennecetin in the discarded liquid of adsorption method from the tennecetin leaching process.Just adopt absorption, desorb, crystallization, separation, exsiccant step to obtain tennecetin.
Concrete steps are as follows:
One, filtering fermentation liquor:
At first the fermented liquid 10000L of tennecetin content 6.5 grams per liters that will be produced by streptomycete fermentation separates with Plate Filtration, obtains tennecetin filtrate 9000L, and measuring tennecetin content is 350ppm, contains tennecetin 3150 grams altogether.
Two, absorption:
Subsequently, under 25 ℃, pH=5.8 condition,, the 300L particle diameter adsorbs less than the adsorption column of the grain active carbon of 2mm by being housed.Tennecetin content is less than 10ppm in the mensuration eliminating waste liquid.
Three, desorption:
Absorption finishes back 500L, the solution washing adsorption column, emptying moisture is used 500L then, the methanol solution washing adsorption column of pH=3.0 pushes up with 300L water and washes adsorption column, obtains 550 liters of methanol solutions that contain tennecetin, mensuration tennecetin content 5000ppm.
Four, crystallization:
Transfer pH=6.5 with 4% sodium hydroxide solution, add 100 premium on currency, heat up 40 ℃, vacuum concentration is removed 300 liters of methyl alcohol.Temperature is reduced to-10 ℃, stirs 12 hours.
Five, separate
Crystallization finishes to adopt whizzer to separate tennecetin, obtains the tennecetin crystallization, and after water, the washing with acetone, vacuum-drying obtains the tennecetin product, is weighed as 2200 grams.
Embodiment 2
Concrete steps are as follows:
One, filtering fermentation liquor:
At first the fermented liquid 10000L of tennecetin content 7.2 grams per liters that will be produced by streptomycete fermentation separates with Plate Filtration, obtains tennecetin filtrate 9000L, and measuring tennecetin content is 420ppm, contains tennecetin 3780 grams altogether.
Two, absorption:
Subsequently, under 25 ℃, pH=5.8 condition,, the plain adsorption column of 200L adsorbing fiber adsorbs by being housed.Tennecetin content is less than 5ppm in the mensuration eliminating waste liquid.
Three, desorption:
Absorption finishes back 500L, the solution washing adsorption column, emptying moisture, use 300L then, the 80%(V/V of pH=10.5) ethanolic soln washing adsorption column, push up with 200L water again and wash adsorption column, obtain 350 liters of ethanolic solns that contain tennecetin, measure tennecetin content 10500ppm.
Four, crystallization:
Transfer pH=6.5 with hydrochloric acid soln, temperature is reduced to-10 ℃, stirs 12 hours.
Five, separate
Crystallization finishes to adopt whizzer to separate tennecetin, obtains the tennecetin crystallization, and after water, the washing with acetone, vacuum-drying obtains the tennecetin product, is weighed as 2620 grams.
Certainly, can also select other above-mentioned sorbent material (as expanded pearlite salt or gac etc.) and desorption agent (as propyl alcohol or methane amide etc.) to implement technical scheme of the present invention, because processing method is basic identical, so do not repeat.
Claims (4)
1. reclaim the method for tennecetin in the discarded liquid, it is characterized in that: the discarded liquid that will produce from the tennecetin leaching process is by absorption, desorption, crystallization, separation drying process acquisition tennecetin, and its concrete steps are as follows:
(1) absorption: adsorb in discarded liquid by the adsorption column that sorbent material is housed under 10 ℃-50 ℃, pH=4.0-7.5, the adsorption column volume is the 0.1-4.0% of fermentating liquid volume;
(2) desorption: with the water washing adsorption column of 1-5 times of adsorption column volume, with the stripping liquid desorption agent post of 1-3 adsorption column volume doubly, stripping liquid is organic solvent or the water-containing organic solvent of pH=1.8-2.5 or pH=9.5-11.5 then;
(3) crystallization: with the stripping liquid after the desorption, use acid or adjusting PH with base between the 5.0-7.5, temperature is reduced to-10 ℃ to 10 ℃, stirs 5-24 hour;
(4) separate drying: crystallization finishes to adopt the method for filtration, gravity settling or centrifugal settling to obtain the tennecetin crystallization, and vacuum-drying obtains the tennecetin product after water or the organic solvent washing.
2. reclaim the method for tennecetin in the discarded liquid according to claim 1, it is characterized in that: the organic solvent as stripping liquid described in the step 2 is any one in methyl alcohol, ethanol, propyl alcohol, Virahol, glycerine, methane amide, dimethyl formamide, N-methylpyrroline or the Glacial acetic acid.
3. reclaim the method for tennecetin in the discarded liquid according to claim 1, it is characterized in that: the organic solvent of step (4) washing usefulness is acetone, ethanol, methylene dichloride or tetrachloromethane, pH scope=5.5-7.5.
4. reclaim the method for tennecetin in the discarded liquid according to claim 1, it is characterized in that: sorbent material described in the step (1) is at least a or two above compositions in diatomite, expanded pearlite salt, gac, macroporous resin, ion exchange resin or the adsorbing fiber element.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010292080 CN101914123A (en) | 2010-09-27 | 2010-09-27 | Method for recovering natamycin from waste liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010292080 CN101914123A (en) | 2010-09-27 | 2010-09-27 | Method for recovering natamycin from waste liquid |
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| CN 201010292080 Pending CN101914123A (en) | 2010-09-27 | 2010-09-27 | Method for recovering natamycin from waste liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851721A (en) * | 2021-01-21 | 2021-05-28 | 浙江新银象生物工程有限公司 | Method for recovering natamycin crystallization mother liquor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB846933A (en) * | 1956-07-23 | 1960-09-07 | American Cyanamid Co | New antifungal substance, pimaricin, and method of producing same |
| CN101693732A (en) * | 2009-08-19 | 2010-04-14 | 北京东方瑞德生物技术有限公司 | Method for extracting and purifying natamycin |
-
2010
- 2010-09-27 CN CN 201010292080 patent/CN101914123A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB846933A (en) * | 1956-07-23 | 1960-09-07 | American Cyanamid Co | New antifungal substance, pimaricin, and method of producing same |
| CN101693732A (en) * | 2009-08-19 | 2010-04-14 | 北京东方瑞德生物技术有限公司 | Method for extracting and purifying natamycin |
Non-Patent Citations (1)
| Title |
|---|
| 《中国抗生素杂志》 20100331 王海燕等 大孔树脂法分离纯化那他霉素的工艺研究 194-201 1-4 第35卷, 第3期 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851721A (en) * | 2021-01-21 | 2021-05-28 | 浙江新银象生物工程有限公司 | Method for recovering natamycin crystallization mother liquor |
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Application publication date: 20101215 |