CN102206241A - 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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- CN102206241A CN102206241A CN2011100676415A CN201110067641A CN102206241A CN 102206241 A CN102206241 A CN 102206241A CN 2011100676415 A CN2011100676415 A CN 2011100676415A CN 201110067641 A CN201110067641 A CN 201110067641A CN 102206241 A CN102206241 A CN 102206241A
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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 technology 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 used to produce brassinolide and make biological pesticide.
At present, the production method of domestic ergosterol has two kinds, is respectively the useless mycelia extraction method of yeast fermentation method and penicillin.With the present invention approaching be the useless mycelia extraction method of penicillin.It is to be raw material with the useless mycelia after penicillin, citric acid or the lactic fermentation, extracts ergosterols through technologies 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.Owing to differ in material composition complexity, source, contain the extracted amount of factor affecting ergosterols such as multiple isomer, the general content of ergosterol be lower and extract degree of purity of production.Simultaneously, extracting method complexity, extraction cost height, leaching process produce the extraction that factors such as waste water and product quality instability are also having a strong impact on ergosterol.
Summary of the invention
The purpose of this invention is to provide a kind of technology of extracting high-purity ergosterol and feedstuff protein from penicillin waste residue, it has solved problems such as extracting method complexity, extraction cost height and unstable products.
For achieving the above object, the present invention is by the following technical solutions:
A kind of technology 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 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) concentrate: 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 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 step (3), the volume ratio of saponification resultant and extraction agent is 1: 20-1: 40, to leave standstill at normal temperatures and pressures, and the 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: filtration is collected in the product that obtains and is added discoloring agent in step (5), and the mass ratio of product and discoloring agent is 1: 0.5-1: 3.
(7) Crystallization Separation drying: 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, vacuum-drying under 40 ℃ of-80 ℃ of conditions promptly gets the ergosterol product then.
(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 following 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 a 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 technology 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 technology 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 improved the recovery utilization rate of penicillin waste residue greatly.
(3) the present invention extracts the technology 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 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; The adding concentration expressed in percentage by weight is 15% sodium hydroxide solution in enriched product, stirs under 60 ℃ of conditions and carries out saponification in 2 hours; The amount that adds sodium hydroxide solution is 1/10 of an 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, vacuum-drying under 60 ℃ of conditions promptly gets the ergosterol product then.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 following dryings.
Above the present invention has been carried out exemplary description; 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 design of the present invention and technical scheme are directly applied to other occasion without improving, all in protection scope of the present invention.
Claims (5)
1. technology of from penicillin waste residue, extracting high-purity ergosterol and feedstuff protein, draw together following 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 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) concentrate: 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 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 step (3), the volume ratio of saponification resultant and extraction agent is 1: 20-1: 40, to leave standstill at normal temperatures and pressures, and the 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: filtration is collected in the product that obtains and is added discoloring agent in step (5), and the mass ratio of product and discoloring agent is 1: 0.5-1: 3;
(7) Crystallization Separation drying: 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, vacuum-drying under 40 ℃ of-80 ℃ of conditions promptly gets the ergosterol product then;
(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 following dryings.
2. according to the described technology of 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. according to claim 1 or 2 described technologies, it is characterized in that: described extraction agent is the normal hexane of massfraction 74% and the mixture of massfraction 16% hexanaphthene.
4. according to the described technology of claim 3, it is characterized in that: described discoloring agent is a gac.
5. according to each described technology of claim 1-4, it 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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| CN102206241A true CN102206241A (en) | 2011-10-05 |
| CN102206241B CN102206241B (en) | 2013-04-03 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113045618A (en) * | 2021-03-19 | 2021-06-29 | 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 |
-
2011
- 2011-03-21 CN CN2011100676415A patent/CN102206241B/en active Active
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 |
|---|
| 《河北化工》 20090920 程俊山，等 青霉素菌渣中提取麦角固醇工艺的研究 第22-24页 1-5 第32卷, 第9期 * |
| 《饲料工业》 20020917 李振亚，等 用青霉素菌丝提取浓缩蛋白质 第38-39页 1-5 第23卷, 第8期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113045618A (en) * | 2021-03-19 | 2021-06-29 | 河北华旭化工有限公司 | Process for extracting ergosterol from penicillin fermentation mycelium and preparing microecology |
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| CN102206241B (en) | 2013-04-03 |
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