CN102206241B - Technological process for extracting ergosterol with high purity and feed protein from penicillin waste residue - Google Patents
Technological process for extracting ergosterol with high purity and feed protein from penicillin waste residue Download PDFInfo
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- CN102206241B CN102206241B CN2011100676415A CN201110067641A CN102206241B CN 102206241 B CN102206241 B CN 102206241B CN 2011100676415 A CN2011100676415 A CN 2011100676415A CN 201110067641 A CN201110067641 A CN 201110067641A CN 102206241 B CN102206241 B CN 102206241B
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Abstract
The invention discloses a technological process for extracting ergosterol with high purity and a feed protein from penicillin waste residue. According to the invention, mycelium in penicillin waste residue is taken as a production raw material, the invention comprises the following steps of distilling, concentrating, concreting, saponifying, extracting and drying and the like for extracting ergosterol and the feed protein. The method has the advantages of simple extracting method with high efficiency and low cost, the extracted products have the characteristics of high purity and good stability, which is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of technique of from penicillin waste residue, extracting high-purity ergosterol and feedstuff protein.
Background technology
Ergosterol is a kind of important medicine chemical material, and maximum purposes is to produce vitamin D2, and ergosterol can be converted into vitamin D2 through ultraviolet lighting.Ergosterol can also be made biological pesticide for the production of brassinolide.
At present, the production method of domestic ergosterol has two kinds, is respectively the useless mycelia extraction method of yeast fermentation method and penicillin.What approach with the present invention is the useless mycelia extraction method of penicillin.It is useless mycelia after penicillin, citric acid or the lactic fermentation as raw material, extract ergosterols through techniques such as cytoclasis, extraction, crystallizations respectively.
The penicillin extraction method is to utilize microbial fermentation to produce penicillin process while by product to be this reaction mechanism of ergosterol.Because material composition is complicated, differ in the source, contains the extracted amount of the factor affecting ergosterols such as multiple isomer, the general content of ergosterol be lower and extract the purity of product.The factors such as simultaneously, extracting method is complicated, extraction cost is high, leaching process produces waste water and product quality is unstable are also having a strong impact on the extraction of ergosterol.
Summary of the invention
The purpose of this invention is to provide a kind of technique of extracting high-purity ergosterol and feedstuff protein from penicillin waste residue, it has solved that extracting method is complicated, extraction cost is high and the problem such as unstable products.
For achieving the above object, the present invention is by the following technical solutions:
A kind of technique of extracting high-purity ergosterol and feedstuff protein from penicillin waste residue is characterized in that drawing together successively following steps:
(1) circulation is extracted: the raw material penicillin waste residue is dropped into continous way flat turn in the extractor, to the mixed solvent of the methylene dichloride that wherein adds 8 times of quality and methyl alcohol, circulation is extracted, and obtains product A to be extracted and filter residue B after the separation;
(2) concentrated: that described product A to be extracted at 50 ℃-100 ℃, is concentrated under the rough vacuum condition and obtains medicinal extract;
(3) saponification: add sodium hydroxide solution in the enriched product medicinal extract in the step (2), under 20 ℃ of-80 ℃ of conditions, stirred 1-3 hour; The concentration expressed in percentage by weight that wherein adds sodium hydroxide solution is 5%-35%, and the amount that adds sodium hydroxide solution is the 1/10-1/5 of enriched product.
(4) extraction: add extraction agent in the saponification resultant in the step (3), the volume ratio of saponification resultant and extraction agent is 1: 20-1: 40, leave standstill at normal temperatures and pressures, and extraction time is 1-3 hour;
(5) Crystallization Separation: the product that extraction is obtained carries out condensing crystal at 50 ℃-100 ℃ under the rough vacuum condition, crystallization time is 1-15 hour, filters and collects;
(6) decolouring: filter in the step (5) to collect in the product that obtains and add discoloring agent, the mass ratio of product and discoloring agent is 1: 0.5-1: 3.
(7) Crystallization Separation is dry: the product after will decolouring carries out condensing crystal at 50 ℃-100 ℃ under the rough vacuum condition, crystallization time is 5-25 hour; Centrifugation under 1000-3000 rev/min condition, then vacuum-drying under 40 ℃ of-80 ℃ of conditions namely gets the ergosterol product.
(8) crushing packing: the ergosterol product is pulverized Vacuum Package under the normal temperature.
(9) filter residue B is volatilized under 50 ℃ of-120 ℃ of conditions and reclaim solvent, then remaining solid is carried out high-temperature sterilization under 100 ℃-140 ℃, the product of will sterilizing is again made 60 orders-100 purpose particle, is packaged to be byproduct feed crude protein after 40 ℃ of-80 ℃ of lower dryings.
In the mixed solvent of described methylene dichloride and methyl alcohol, methylene dichloride and methyl alcohol are the analytical pure solvent, and the volume ratio of methylene dichloride and methyl alcohol is 5: 5.
Described extraction agent is the normal hexane of massfraction 74% and the mixture of massfraction 16% hexanaphthene.
Described discoloring agent is gac.
Step (9) but described in reclaim solvent recirculation and extract.
The present invention compares with the like product preparation method, has outstanding having a few and beneficial effect:
(1) the present invention extracts the technique of high-purity ergosterol and feedstuff protein from penicillin waste residue, and its experimental technique is simple, and flow process is shorter, and production cost is low.
(2) the present invention extracts the technique of high-purity ergosterol and feedstuff protein from penicillin waste residue, and the waste residue after extracting is processed into the feed crude protein, has greatly improved the recovery utilization rate of penicillin waste residue.
(3) the present invention extracts the technique of high-purity ergosterol and feedstuff protein from penicillin waste residue, has realized ergosterol extraction at a lower temperature, and it is comparatively stable to obtain product.
Embodiment
Embodiment 1
1 kilogram of raw material penicillin waste residue is dropped into continous way extract in the device of flatting turn, to the mixed solvent of the methylene dichloride that wherein adds 8 times of quality and methyl alcohol, the volume ratio of methylene dichloride and methyl alcohol is 5: 5, and circulation is extracted, and obtains product A to be extracted and filter residue B after the separation.Product A to be extracted at 80 ℃, is concentrated under the rough vacuum condition and obtains medicinal extract; Add concentration expressed in percentage by weight in the enriched product and be 15% sodium hydroxide solution, under 60 ℃ of conditions, stir and carried out saponification in 2 hours; The amount that adds sodium hydroxide solution is 1/10 of enriched product.Add No. 6 gasoline again in saponification resultant, the volume ratio of saponification resultant and No. 6 gasoline is 1: 30, leaves standstill at normal temperatures and pressures 2 hours; The product that extraction is obtained carried out condensing crystal 3 hours at 60 ℃ under the rough vacuum condition, filter and collect.Add gac to filtering to collect in the product that obtains, the mass ratio of control product and discoloring agent is 1: 2.Product after the decolouring at 60 ℃, was carried out condensing crystal 5 hours under the rough vacuum condition; Centrifugation under 1000 rev/mins condition, then vacuum-drying under 60 ℃ of conditions namely gets the ergosterol product.The ergosterol product is crushed to 60 orders, Vacuum Package under the normal temperature.
Filter residue B is volatilized under 80 ℃ of conditions and reclaim solvent, then remaining solid is carried out high-temperature sterilization under 120 ℃, the product of will sterilizing is again made 80 purpose particles, is packaged to be byproduct feed crude protein after 60 ℃ of lower dryings.
The above has carried out exemplary description to the present invention; obvious realization of the present invention is not subjected to the restriction of aforesaid way; as long as the various improvement of having adopted method design of the present invention and technical scheme to carry out; or without improving design of the present invention and technical scheme are directly applied to other occasion, all in protection scope of the present invention.
Claims (4)
1. technique of extracting high-purity ergosterol and feedstuff protein from penicillin waste residue may further comprise the steps successively:
(1) circulation is extracted: the raw material penicillin waste residue is dropped into continous way flat turn in the extractor, to the mixed solvent of the methylene dichloride that wherein adds 8 times of quality and methyl alcohol, circulation is extracted, and obtains product A to be extracted and filter residue B after the separation;
(2) concentrated: that described product A to be extracted at 50 ℃-100 ℃, is concentrated under the rough vacuum condition and obtains medicinal extract;
(3) saponification: add sodium hydroxide solution in the enriched product medicinal extract in the step (2), under 20 ℃ of-80 ℃ of conditions, stirred 1-3 hour; The concentration expressed in percentage by weight that wherein adds sodium hydroxide solution is 5%-35%, and the amount that adds sodium hydroxide solution is the 1/10-1/5 of enriched product;
(4) extraction: add extraction agent in the saponification resultant in the step (3), described extraction agent is No. 6 gasoline, and the volume ratio of saponification resultant and extraction agent is 1: 20-1: 40, leave standstill at normal temperatures and pressures, and extraction time is 1-3 hour;
(5) Crystallization Separation: the product that extraction is obtained carries out condensing crystal at 50 ℃-100 ℃ under the rough vacuum condition, crystallization time is 1-15 hour, filters and collects;
(6) decolouring: filter in the step (5) to collect in the product that obtains and add discoloring agent, the mass ratio of product and discoloring agent is 1: 0.5-1: 3;
(7) Crystallization Separation is dry: the product after will decolouring carries out condensing crystal at 50 ℃-100 ℃ under the rough vacuum condition, crystallization time is 5-25 hour; Centrifugation under 1000-3000 rev/min condition, then vacuum-drying under 40 ℃ of-80 ℃ of conditions namely gets the ergosterol product;
(8) crushing packing: the ergosterol product is pulverized Vacuum Package under the normal temperature;
(9) filter residue B is volatilized under 50 ℃ of-120 ℃ of conditions and reclaim solvent, then remaining solid is carried out high-temperature sterilization under 100 ℃-140 ℃, the product of will sterilizing is again made 60 orders-100 purpose particle, is packaged to be byproduct feed crude protein after 40 ℃ of-80 ℃ of lower dryings.
2. described technique according to claim 1, it is characterized in that: in the mixed solvent of described methylene dichloride and methyl alcohol, methylene dichloride and methyl alcohol are the analytical pure solvent, and the volume ratio of methylene dichloride and methyl alcohol is 5: 5.
3. described technique according to claim 2, it is characterized in that: described discoloring agent is gac.
4. each described technique according to claim 1-3 is characterized in that: step (9) but described in reclaim solvent recirculation and extract.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100676415A CN102206241B (en) | 2011-03-21 | 2011-03-21 | Technological process for extracting ergosterol with high purity and feed protein from penicillin waste residue |
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| CN2011100676415A CN102206241B (en) | 2011-03-21 | 2011-03-21 | Technological process for extracting ergosterol with high purity and feed protein from penicillin waste residue |
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| CN102206241B true CN102206241B (en) | 2013-04-03 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104171412A (en) * | 2014-08-03 | 2014-12-03 | 哈尔滨伟平科技开发有限公司 | Method for preparing laying hen feed additive for calcium supplement by using penicillin residues |
| CN108558977A (en) * | 2018-05-08 | 2018-09-21 | 刘健 | A method of extracting ergosterol from amylofermentation object |
| CN113045618B (en) * | 2021-03-19 | 2022-08-16 | 河北华旭化工有限公司 | Process for extracting ergosterol from penicillin fermentation mycelium and preparing microecology |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322728A (en) * | 2000-05-09 | 2001-11-21 | 北京化工大学 | Method of extracting ergosterol from waste mycelium |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322728A (en) * | 2000-05-09 | 2001-11-21 | 北京化工大学 | Method of extracting ergosterol from waste mycelium |
Non-Patent Citations (2)
| Title |
|---|
| 李振亚，等.用青霉素菌丝提取浓缩蛋白质.《饲料工业》.2002,第23卷(第8期),第38-39页. * |
| 程俊山,等.青霉素菌渣中提取麦角固醇工艺的研究.《河北化工》.2009,第32卷(第9期),第22-24页. * |
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