CN105418701B - A kind of method that neomycin is extracted in the zymotic fluid from neomycin - Google Patents

A kind of method that neomycin is extracted in the zymotic fluid from neomycin Download PDF

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Publication number
CN105418701B
CN105418701B CN201510999448.3A CN201510999448A CN105418701B CN 105418701 B CN105418701 B CN 105418701B CN 201510999448 A CN201510999448 A CN 201510999448A CN 105418701 B CN105418701 B CN 105418701B
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neomycin
zymotic fluid
extracted
filter
clear liquid
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CN105418701A (en
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沈联兵
张国宪
何连明
周宜平
张安莲
覃清华
薛勇
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YICHANG SANXIA PHARMACEUTICAL CO Ltd
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YICHANG SANXIA PHARMACEUTICAL CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/22Cyclohexane rings, substituted by nitrogen atoms
    • C07H15/222Cyclohexane rings substituted by at least two nitrogen atoms
    • C07H15/226Cyclohexane rings substituted by at least two nitrogen atoms with at least two saccharide radicals directly attached to the cyclohexane rings
    • C07H15/228Cyclohexane rings substituted by at least two nitrogen atoms with at least two saccharide radicals directly attached to the cyclohexane rings attached to adjacent ring-carbon atoms of the cyclohexane rings
    • C07H15/232Cyclohexane rings substituted by at least two nitrogen atoms with at least two saccharide radicals directly attached to the cyclohexane rings attached to adjacent ring-carbon atoms of the cyclohexane rings with at least three saccharide radicals in the molecule, e.g. lividomycin, neomycin, paromomycin
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Biotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Molecular Biology (AREA)
  • Compounds Of Unknown Constitution (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

A kind of method that neomycin is extracted in zymotic fluid from neomycin, this method comprise the following steps:1)Heating:Neomycin zymotic fluid is heated up to 65 75 DEG C;2)The ﹪ of neomycin zymotic fluid quality 1-2 super-cell is put into the neomycin zymotic fluid after heating;3)By step 2)Obtained neomycin zymotic fluid is filtered by filter, obtains the clear liquid containing neomycin;4)By step 3)The obtained clear liquid containing neomycin directly carries out upper prop absorption;5)Desorbed and concentrated again, that is, neomycin finished product is made.The method that neomycin is extracted in a kind of zymotic fluid from neomycin provided by the present invention, can solve the environmental issue in neomycin production, make the novel technology for extracting of neomycinsulphate more energy efficient, realize clean manufacturing.

Description

A kind of method that neomycin is extracted in the zymotic fluid from neomycin
Technical field
The present invention relates to neomycin production field, the method for extraction neomycin in especially a kind of zymotic fluid from neomycin.
Background technology
At present, the extracting method of neomycin product continues to use traditional handicraft always, i.e., absorption is put into neomycin zymotic fluid Resin, after resin adsorption neomycin saturation to be adsorbed, by resin and neomycin separation of fermentative broth, then will be new using the method for desorption Mycin desorbs from resin.By current factory's neomycin production scale, 300 tons of neomycin zymotic fluids are at least produced daily, These neomycin zymotic fluids need to carry out the separation of resin and neomycin zymotic fluid after launching polymeric adsorbent and having adsorbed.Extraction is adopted Sieved with the vibratory sieve of 80 mesh, meanwhile, it is rinsed during sieving with substantial amounts of water, water consumption substantially remains in 1: 1 ratio, the water of flushing become waste water after being mixed with the water of neomycin zymotic fluid, meanwhile, because of long (8 hours of adsorption time More than), higher plus temperature, the neomycin zymotic fluid of being rich in nutrition composition can be contaminated, and produce niff, cause surrounding The complaint of resident.
There is the above to understand that Conventional processing methods have following defect:
First, water consume is high;
2nd, resin cracky;
3rd, substantial amounts of waste water is produced;
4th, niff is produced.
With the implementation of national new environmental law, the environmental protection pressure of enterprise is increasing, does not solve a large amount of waste water and unpleasant Smell, enterprise will be faced with crisis of survival.Therefore it need to improve what extraction process in the production of neomycin neomycin zymotic fluid controlled Method, so as to reach environmental protection, the production requirement of energy-conservation.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method that neomycin is extracted in zymotic fluid from neomycin, can To solve the environmental issue in neomycin production, make the novel technology for extracting of neomycinsulphate more energy efficient, realize clean manufacturing.
In order to solve the above technical problems, the technical solution adopted in the present invention is:One kind is extracted from neomycin zymotic fluid The method of neomycin, this method comprise the following steps:
1) heat:Neomycin zymotic fluid is heated up to 65-75 DEG C;
2) ﹪ of neomycin zymotic fluid quality 1-2 super-cell is put into the neomycin zymotic fluid after heating, and Stir;
Filter aid is super-cell;
3) neomycin zymotic fluid made from step 2) is filtered by filter, by the solid phase and liquid phase of neomycin zymotic fluid Separation, obtains the clear liquid containing neomycin;
4) clear liquid containing neomycin made from step 3) is directly subjected to upper prop absorption;
5) desorbed, concentrated again, turned salt, refine, dusting, that is, neomycin finished product is made.
" upper prop absorption " in step 4) refers to clear liquid being passed through from post is handed over by pipeline, and the mode being passed through is under To upper, for clear liquid when flowing through from post is handed over, contained neomycin is by resin adsorption in post in its liquid, when the neomycin of absorption reaches saturation When, just turn into saturated resin, you can enter lower one of abstraction process.It is exactly by the metal can inner lining glass fiber reinforced plastic of cylinder from post is handed over Container, built-in empty resin composition.
In step 1), neomycin zymotic fluid is heated up to 70 DEG C.
In step 2), rice chaff powder forming agent is additionally added,
Rice chaff silty amount is 2-3 ﹪ of neomycin zymotic fluid quality.
In step 3), filter is flame filter press.
The invention process of the inventive method is as follows:
Make a general survey of in whole technological process, filtering is a wherein the most key step, if can success, others just meet sword and Solution.Enterprise has successively carried out the research of multiple projects such as ceramic membrane filter, centrifuge filtering, and data are shown, both filtering sides Method is all undesirable to neomycin neomycin zymotic fluid, compares by studying repeatedly, have finally chosen plate-frame filtering.
In the case where not adding any filter aid, the rate of filtration of neomycin zymotic fluid is slower, it is impossible to meets production need Ask, suitable filter aid and economical and practical filter condition obtain ideal effect applied to after neomycin extraction process.
1, the selection of filtration adjuvant
The characteristics of viscosity height, solid content for neomycin zymotic fluid is high, and nutrient composition content is high, we pick Various flocculants, sedimentation agent, filter aid carry out filtering contrast test, and specific method is:1.5 tons of neomycin zymotic fluid is taken, by normal Rule amount adds various flocculants, sedimentation agent, filter aid and carries out contrast test, the observation rate of filtration and the quality for crossing cleaner liquid, really Fixed optimal filter aid.
Experimental result is as follows:
As can be seen from the above results, under identical condition, the filtrate quality obtained meets the requirements, but with the addition of Diatomite is substantially many soon as the experiment batch filtering velocity of filter aid.
Flocculant 1# is sodium carboxymethylcellulose;
Flocculant 2# is polyacrylamide.
2, based on super-cell, grope both economic, the process conditions being applicable again
Research through laboratory shows that after carrying out heat treatment to zymotic fluid, zymotic fluid viscosity is decreased obviously, and has to filtering Larger help.
Above-mentioned serial experiment result proves, in the case of 70 DEG C, the super-cell for adding 1%-2%, filtering is new Mycin zymotic fluid, can obtain faster filtering velocity, and filter cake shaping is quick detachable.Part diatomite is replaced with part rice chaff powder, it is simultaneous Economy has been cared for, has also achieved preferable experiment effect.Average yield stably reaches more than 90%.
The method that neomycin is extracted in a kind of zymotic fluid from neomycin provided by the invention, has the beneficial effect that:
1st, it is highly soluble in water using neomycin, the neomycin in neomycin zymotic fluid is all present in liquid phase substantially, as long as The solid phase of fermentation and liquid phase are separated, you can the principle of the clear liquid containing neomycin is obtained, it is simple by filter aid and filter The removal of most of organic matter in neomycin zymotic fluid is realized on ground, to solve the environmental issue in neomycin production, makes sulfuric acid new The novel technology for extracting of mycin is more energy efficient, realizes clean manufacturing, and method and step is simple.
2nd, solve fragile undermine of water consume height, resin in existing extraction process and produce substantial amounts of waste water and niff etc. Problem, reach and promote automation degree of equipment to improve, save great lot of water resources, reduce discharge of wastewater, realize clean manufacturing, together When, the bacteria residue filtered out significantly reduces the COD in waste water, alleviates wastewater treatment difficulty.
3rd, suitable filter aid-diatomite is have found, and suitable dosage ratio is determined;Have found shapes filter residue Forming agent-rice chaff powder, and suitable dosage ratio is determined;And zymotic fluid heating mode is have selected, and is determined properly Temperature value, accelerate the rate of filtration.Flame filter press is applied in the extraction process of neomycin, realize clean manufacturing.
4th, the economic benefit obtained is as follows:
In June, 2015 company formally implement plate-frame filtering technique after, Dynamic Adsorption is smoothly implemented, and 6-August part, subtracts Few positive resin is lost 20 tons, converts into 100,000 yuan of RMB;Product loss 30,000 hundred million is reduced, 250,000 yuan of RMB is converted into, excludes Increased diatomaceous about 100,000 yuan of the input of plate-frame filtering, can quarterly have a net increase of 250,000 yuan of profit, the major part in zymotic fluid has Machine matter is removed, and solves the pressure of environmental protection station 70%, and being left a part of waste water environmental protection station can easily solve, annual to reduce More than 3,000,000 yuan of Environmental Inputs.Equivalent to every year can be enterprise increase about 4,000,000 yuan of profit.
5th, other comprehensive benefits obtained are as follows:
After project implementation application, most of organic matter in zymotic fluid is removed, and solves the pressure of environmental protection station 70% Power, being left a part of waste water environmental protection station can easily solve, and solve environmental issue, and it is empty also to bring unlimited development to enterprise Between.Obstacle has been cleared away for the smooth implementation of new technology.
Brief description of the drawings
The invention will be further described with reference to the accompanying drawings and examples:
Fig. 1 is neomycin zymotic fluid using the comparison diagram before the inventive method filtering and after filtering.
Embodiment
Embodiment one
A kind of method that neomycin is extracted in zymotic fluid from neomycin, this method comprise the following steps:
1) heat:Neomycin zymotic fluid is heated up to 65 DEG C;
2) ﹪ of neomycin zymotic fluid quality 2 super-cell is put into the neomycin zymotic fluid after heating, and is stirred Mix uniformly.
Filter aid is super-cell;
3) neomycin zymotic fluid made from step 2) is filtered by filter, by the solid phase and liquid phase of neomycin zymotic fluid Separation, obtains the clear liquid containing neomycin;
4) clear liquid containing neomycin made from step 3) is directly subjected to upper prop absorption;
5) desorbed, concentrated again, turned salt, refine, dusting, that is, neomycin finished product is made.
In step 3), filter is flame filter press.
Embodiment two
A kind of method that neomycin is extracted in zymotic fluid from neomycin, this method comprise the following steps:
1) heat:Neomycin zymotic fluid is heated up to 70 DEG C;
2) ﹪ of neomycin zymotic fluid quality 1 super-cell is put into the neomycin zymotic fluid after heating, and is stirred Mix uniformly;
Filter aid is super-cell;
3) neomycin zymotic fluid made from step 2) is filtered by filter, by the solid phase and liquid phase of neomycin zymotic fluid Separation, obtains the clear liquid containing neomycin;
4) clear liquid containing neomycin made from step 3) is directly subjected to upper prop absorption;
5) desorbed, concentrated again, turned salt, refine, dusting, that is, neomycin finished product is made.
In step 3), filter is flame filter press.
Embodiment three
A kind of method that neomycin is extracted in zymotic fluid from neomycin, this method comprise the following steps:
1) heat:Neomycin zymotic fluid is heated up to 75 DEG C;
2) ﹪ of neomycin zymotic fluid quality 1 super-cell is put into the neomycin zymotic fluid after heating, and is stirred Mix uniformly;
Filter aid is super-cell;
3) neomycin zymotic fluid made from step 2) is filtered by filter, by the solid phase and liquid phase of neomycin zymotic fluid Separation, obtains the clear liquid containing neomycin;
4) clear liquid containing neomycin made from step 3) is directly subjected to upper prop absorption;
5) desorbed, concentrated again, turned salt, refine, dusting, that is, neomycin finished product is made.
In step 3), filter is flame filter press.
Example IV
A kind of method that neomycin is extracted in zymotic fluid from neomycin, this method comprise the following steps:
1) heat:Neomycin zymotic fluid is heated up to 65 DEG C;
2) ﹪ of neomycin zymotic fluid quality 2 super-cell is put into the neomycin zymotic fluid after heating, and is stirred Mix uniformly.
Filter aid is super-cell;
3) neomycin zymotic fluid made from step 2) is filtered by filter, by the solid phase and liquid phase of neomycin zymotic fluid Separation, obtains the clear liquid containing neomycin;
4) clear liquid containing neomycin made from step 3) is directly subjected to upper prop absorption;
5) desorbed, concentrated, turned salt, refine, dusting, that is, neomycin finished product is made.
In step 2), rice chaff powder forming agent is additionally added,
Rice chaff silty amount is 2 ﹪ of neomycin zymotic fluid quality.
In step 3), filter is flame filter press.
Embodiment five
A kind of method that neomycin is extracted in zymotic fluid from neomycin, this method comprise the following steps:
1) heat:Neomycin zymotic fluid is heated up to 70 DEG C;
2) ﹪ of neomycin zymotic fluid quality 1 super-cell is put into the neomycin zymotic fluid after heating, and is stirred Mix uniformly.
Filter aid is super-cell;
3) neomycin zymotic fluid made from step 2) is filtered by filter, by the solid phase and liquid phase of neomycin zymotic fluid Separation, obtains the clear liquid containing neomycin;
4) clear liquid containing neomycin made from step 3) is directly subjected to upper prop absorption;
5) desorbed, concentrated, turned salt, refine, dusting, that is, neomycin finished product is made.
In step 2), rice chaff powder forming agent is additionally added,
Rice chaff silty amount is 3 ﹪ of neomycin zymotic fluid quality.
In step 3), filter is flame filter press.
Embodiment six
A kind of method that neomycin is extracted in zymotic fluid from neomycin, this method comprise the following steps:
1) heat:Neomycin zymotic fluid is heated up to 75 DEG C;
2) ﹪ of neomycin zymotic fluid quality 2 super-cell is put into the neomycin zymotic fluid after heating, and is stirred Mix uniformly.
Filter aid is super-cell;
3) neomycin zymotic fluid made from step 2) is filtered by filter, by the solid phase and liquid phase of neomycin zymotic fluid Separation, obtains the clear liquid containing neomycin;
4) clear liquid containing neomycin made from step 3) is directly subjected to upper prop absorption;
5) desorbed, concentrated, turned salt, refine, dusting, that is, neomycin finished product is made.
In step 2), rice chaff powder forming agent is additionally added,
Rice chaff silty amount is 2 ﹪ of neomycin zymotic fluid quality.
In step 3), filter is flame filter press.
Contrast photo before neomycin filtering fermentation liquor and after filtering is as shown in figure 1, it can be seen that new mould before filtering Plain zymotic fluid is substantially clarified into cloudy state after filtering.
In the various embodiments described above, in step 4), " upper prop absorption " refers to clear liquid being passed through from post is handed over by pipeline, leads to The mode entered is that from down to up, for clear liquid when flowing through from post is handed over, contained neomycin is by resin adsorption in post in its liquid, when absorption When neomycin reaches saturation, just turn into saturated resin, you can enter lower one of abstraction process, be exactly by the gold of cylinder from post is handed over Belong to the container of tank inner lining glass fiber reinforced plastic, built-in empty resin composition.
In step 5), concentrate, turn salt, refine, dusting for existing process,
Desorption points to saturated resin and is passed through certain density desorption ammonia solution, by under the neomycin desorption on saturated resin Come;
Concentration refers to moisture unnecessary contained by the stripping liquid that will be desorbed and ammonia is evaporated by thin film evaporator, is allowed to The concentration of neomycin reaches technological requirement;
Turn salt to be directed to add a certain amount of sulfuric acid in the neomycin concentrate of pH meta-alkalis, be allowed to be formed pH in neutral sulphur Sour neomycin;
Activated carbon is added in the refined neomycinsulphate concentrate being directed to turn after salt, it is miscellaneous to remove pigment in concentrate etc. Matter, the refined liquid that light transmittance reaches quality requirement is allowed to by plate-frame filtering;
Dust and refer to go moisture removal to form the new mould of powdery by spraying tower high-temperature injection, moment refined liquid made from decolouring The former powder of element.

Claims (3)

1. the method for neomycin is extracted in a kind of zymotic fluid from neomycin, it is characterised in that this method comprises the following steps:
1)Heating:Neomycin zymotic fluid is heated up to 65-75 DEG C;
2)The ﹪ of neomycin zymotic fluid quality 1-2 super-cell and rice chaff powder is put into the neomycin zymotic fluid after heating Forming agent, and stir;
Rice chaff silty amount is 2-3 ﹪ of neomycin zymotic fluid quality;
3)By step 2)Obtained neomycin zymotic fluid is filtered by filter, by the solid phase of neomycin zymotic fluid and liquid phase point From obtaining the clear liquid containing neomycin;
4)By step 3)The obtained clear liquid containing neomycin directly carries out upper prop absorption;
5)Desorbed, concentrated again, turned salt, refine, dusting, that is, neomycin finished product is made.
2. the method for neomycin is extracted in a kind of zymotic fluid from neomycin according to claim 1, it is characterised in that:Step 1)In, neomycin zymotic fluid is heated up to 70 DEG C.
3. the method for neomycin is extracted in a kind of zymotic fluid from neomycin according to claim 1, it is characterised in that:Step 3)In, filter is flame filter press.
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Publication number Priority date Publication date Assignee Title
CN106317138A (en) * 2016-08-25 2017-01-11 宁夏泰益欣生物科技有限公司 Extraction method of neomycin sulfate
CN107915763A (en) * 2016-10-09 2018-04-17 津药新瑞制药股份有限公司 A kind of method of neomycin fermented waste fluid slag-liquid separation and recycling residual neomycin
CN108203453A (en) * 2016-12-19 2018-06-26 宜昌三峡制药有限公司 The method of automatic flame filter press large-scale production neomycin
CN109399835B (en) * 2018-12-24 2020-10-27 宜昌三峡制药有限公司 Solid-liquid separation method for neomycin sulfate fermentation waste liquid
CN110872333A (en) * 2019-11-25 2020-03-10 宜昌三峡制药有限公司 Process control method for neomycin preparation process
CN114011157A (en) * 2021-11-08 2022-02-08 江苏力凡胶囊有限公司 Additive-free filtering method for high-viscosity fermentation liquor

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