CN106083951B - A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride - Google Patents
A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride Download PDFInfo
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- CN106083951B CN106083951B CN201610504642.4A CN201610504642A CN106083951B CN 106083951 B CN106083951 B CN 106083951B CN 201610504642 A CN201610504642 A CN 201610504642A CN 106083951 B CN106083951 B CN 106083951B
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- kasugarnycin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/207—Cyclohexane rings not substituted by nitrogen atoms, e.g. kasugamycins
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
Abstract
The present invention relates to a kind of method using kasugarnycin broth extraction kasugamycini hydrochloride, processing step is:Kasugarnycin fermentation liquid is preprocessed, ceramic membrane filter, macroreticular resin decoloration, nanofiltration concentration, crystallizes and dries.It is compared with domestic conventional production process, reduces production cost, improve final product quality, be conducive to the domestic and international market competitiveness for enhancing product.
Description
Technical field
The invention belongs to antibiotic extractive technique fields, utilize kasugarnycin broth extraction hydrochloric acid more particularly to a kind of
The method of kasugarnycin.
Background technique
Kasugarnycin is a kind of alkalescent antibiotic generated by small golden streptomysin, which is that dual-purpose antibiotic is cured in agriculture.
Currently, Related domestic documents report in kasugarnycin fermentation liquid, addition oxalic acid is pre-processed, macroreticular resin technology extracts the spring
The method of thunder mycin.Existing main problem is:
Oxalic acid is added in 1 kasugarnycin fermentation liquor pretreatment technique, improves production cost.
2 pertinent literatures report the method for preparing kasugarnycin, but product effective content is relatively low, are unfavorable for going out for product
Mouthful.
3 pertinent literatures, which are reported, prepares kasugarnycin using the method for spray drying, and product is not easy long term storage, transport
With use.
Summary of the invention
It is an object of the invention to overcome above-mentioned defect in the prior art, a kind of guarantee yield, extraction process letter are provided
Single, product quality meets the method using kasugarnycin broth extraction kasugamycini hydrochloride of relevant regulations.
The technical solution taken to achieve the above object is:
A method of utilizing kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that its processing step is:
1)Fermentation liquor pretreatment
It by kasugarnycin fermentation liquid tune pH 4.5-5, is sufficiently stirred and stands, continue to adjust pH to 2.5-3, again sufficiently
It stirs and stands;Then polysilicate aluminum chloride calcium is added, is sufficiently stirred and stands;
2)Ceramic membrane filter
By pretreated fermentation liquid, viscosity is brought down below 3000Pas, after be warming up to 50-55 DEG C, then using high speed
Cross-current flow carries out ceramic membrane filter, collects filtrate;
In filter process, pressure is controlled in 0.2-0.3MPa, and flow control is in 0.5~0.9m3/m2.h.
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water
For the 60-70% of fermentating liquid volume.Film filtering terminates, and collects filtrate.
3)Macroreticular resin decoloration
Through process 2)Gained filtrate temperature is controlled at 35-40 DEG C, with macroreticular resin decolorization;
4)Nanofiltration concentration
By process 2)Gained macroreticular resin de-inking solution temperature is controlled at 40-45 DEG C, carries out nanofiltration concentration;
5)Crystallization
Nanofiltration solution temperature is down to 0-5 DEG C, organic solvent is added in speed of agitator control in 30-50r/min, solution,
Crystal seed is added when there is crystallization situation in 13-15ml/min in flow control, continues to stir 120-150min, stirring terminates, quiet
150-180min is set, is then filtered, wet solid kasugamycini hydrochloride is obtained;
6)Drying.
The process 1)In, adjustment pH uses mass concentration for the hydrochloric acid solution of 20-30%.
The process 1)In, mixing time 20-30min stands 40-80min.
The process 1)In, polysilicate aluminum chloride calcium dosage is the 0.01-0.03% of fermentating liquid volume.
The process 2)In, during ceramic membrane filter, pressure control in 0.2-0.3MPa, flow control 0.5~
0.9m3/m2.h;
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water
For the 60-70% of fermentating liquid volume.
The process 2)In, ceramic membrane is porous ceramic film, and port number 37, material is silica, pore size filter specification
It is 0.2 μm.
The process 3)In, macroreticular resin is D941 anion decolorizing resin, and material is divinylbenzene, and resin column is through high ratio
It is 1: 6-7, charging rate control is controlled in 2-2.5BV/h, discharging speed in 1.1-1.5BV/h.
The process 4)In, when nanofiltration is concentrated, pressure is controlled in 0.5-1MPa, and solution is concentrated into the 40- of original solution volume
50%, the material of nanofiltration membrane used is polyvinyl alcohol, and nanofiltration membrane component is hollow fiber form.
The process 5)In, organic solvent is acetone or methanol or ethyl alcohol or propyl alcohol or isopropanol, dosage are:V is organic molten
Agent:V filtrate=4-6:1.
The process 5)In, crystal seed is kasugamycini hydrochloride sterling, and dosage is the 0.01-0.02% of liquor capacity.
The process 6)In, it is dry to use double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is-
0.02~-0.08 MPa, 12~15h of drying time.
The technology of the present invention advantage is embodied in:
1 present invention replaces conventional oxalic acid preprocess method using membrane filtering method, effectively improves kasugarnycin fermentation liquid
Pretreated yield, reduces production cost.
2 extract kasugarnycin using method of the invention, and effective content has reached 98% or more.
3 extract kasugarnycin using method of the invention, wherein 70% or more kasugarnycin product cut size reaches
50um, product is convenient for storage and long-distance transport.
Specific embodiment
The present invention will be described below by way of examples, it should be understood that example is for illustrating rather than to this
The limitation of invention.The scope of the present invention is determined with core content according to claims.
Kasugarnycin fermentation liquid source in following embodiments:
The acquisition of kasugarnycin fermentation liquid:Use proprietary streptomyces microaureus for producing strains, with low temperature soybean cake powder, ferment
The raw material such as female powder, glucose are configured to fermentation culture, through three grade fermemtation biosynthesis kasugarnycin.
Ceramic membrane is porous ceramic film, and port number 37, material is silica, and pore size filter specification is 0.2 μm.
Macroreticular resin is D941 anion decolorizing resin, and material is divinylbenzene, and resin column is through height than being 1: 6-7.
The material of nanofiltration membrane is polyvinyl alcohol, and nanofiltration membrane component is hollow fiber form.
Crystal seed is kasugamycini hydrochloride sterling, and dosage is the 0.01-0.02% of liquor capacity.
Embodiment 1
Kasugarnycin fermentation liquid 100m3, chemical titer 15201u/ml.
1)Fermentation liquor pretreatment
Kasugarnycin fermentation liquid pH to 5 is adjusted using 20% hydrochloric acid solution, 20min is stirred, stands 40min;Continue to adjust
Kasugarnycin fermentation liquid pH to 3 stirs 20min, stands 40min.
Polysilicate aluminum chloride calcium 100kg is added in fermentation liquid, continues to stir 20min, stands 60min.
2)Ceramic membrane filter
Drinking water is added in pretreated fermentation liquid, viscosity is down to 2943Pas, and fermentation liquid is warming up to 50 DEG C.
In membrane filtration processes, film filtering is carried out using high speed cross-current flow, in filter process, pressure is controlled in 0.2-
0.3MPa, flow control is in 0.5m3/m2.h。
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water
It is the 60% of fermentating liquid volume.
Film filtering terminates, and collects 150 m of kasugarnycin filtrate3, chemical titer 7150u/ml.
3)Macroreticular resin decoloration
Filtrate temperature is warming up to 35 DEG C, through macroreticular resin decolorization, it is desirable that resin column is 1: 6 through height ratio, charging rate
Control is controlled in 2BV/h, discharging speed in 1.1BV/h.
Filtering terminates, and collects 149 m of kasugarnycin filtrate3。
4)Nanofiltration concentration
It controls through macroreticular resin de-inking solution temperature at 40 DEG C, carries out nanofiltration, pressure is controlled in 0.5MPa.Nanofiltration terminates,
Filtrate volume is 60 m3。
5)Crystallization
It is down to 0 DEG C through nanofiltration solution temperature, organic solvent-acetone is added in speed of agitator control in 30r/min, solution
240m3, flow control is in 13ml/min, and when there is crystallization situation, addition crystal seed kasugamycini hydrochloride sterling 6kg continues to stir
120min.Stirring terminates, and stands 150min, then filters, obtain wet solid kasugamycini hydrochloride.
6)It is dry
Wet solid kasugamycini hydrochloride puts into double conic rotary vacuum dryer, and temperature rises to 60 DEG C, and control vacuum degree is-
0.02~-0.08 MPa, dry 15h.It is dry to terminate to obtain kasugamycini hydrochloride 995kg.Through detecting, effective content 98.7%;
74% kasugarnycin product cut size has reached 50um.
Embodiment 2
Kasugarnycin fermentation liquid 100m3, chemical titer 14936u/ml.
1)Fermentation liquor pretreatment
Kasugarnycin fermentation liquid pH to 4.8 is adjusted using 22% hydrochloric acid solution, 22min is stirred, stands 45min;Continue to adjust
Kasugarnycin fermentation liquid pH to 2.8 is saved, 22min is stirred, stands 45min.
Polysilicate aluminum chloride calcium 150kg is added in fermentation liquid, continues to stir 22min, stands 65min.
2)Ceramic membrane filter
Drinking water is added in pretreated fermentation liquid, viscosity is down to 2893Pas, and fermentation liquid is warming up to 52 DEG C.
In membrane filtration processes, film filtering is carried out using high speed cross-current flow, in filter process, pressure is controlled in 0.2-
0.3MPa, flow control is in 0.6m3/m2.h。
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water
It is the 62% of fermentating liquid volume.
Film filtering terminates, and collects kasugarnycin filtrate 155m3, chemical titer 6893u/ml.
3)Macroreticular resin decoloration
Filtrate temperature is warming up to 36 DEG C, through macroreticular resin decolorization, it is desirable that for resin column through height than being 1: 6.2, charging is fast
Degree control is controlled in 2.2BV/h, discharging speed in 1.2BV/h.
Filtering terminates, and collects kasugarnycin filtrate 154m3。
4)Nanofiltration concentration
It controls through macroreticular resin de-inking solution temperature at 42 DEG C, carries out nanofiltration, pressure is controlled in 0.6MPa.Nanofiltration terminates,
Filtrate volume is 64.7m3。
5)Crystallization
2 DEG C are down to through nanofiltration solution temperature, organic solvent methanol is added in speed of agitator control in 35r/min, solution
292m3, flow control is in 13.5ml/min, and when there is crystallization situation, crystal seed kasugamycini hydrochloride sterling 8.4kg, continuation is added
Stir 130min.Stirring terminates, and stands 160min, then filters, obtain wet solid kasugamycini hydrochloride.
6)It is dry
Wet solid kasugamycini hydrochloride puts into double conic rotary vacuum dryer, and temperature rises to 65 DEG C, and control vacuum degree is-
0.02~-0.08 MPa, dry 14h.It is dry to terminate to obtain kasugamycini hydrochloride 994kg.Through detecting, effective content 98.9%;
76% kasugarnycin product cut size has reached 50um.
Embodiment 3
Kasugarnycin fermentation liquid 100m3, chemical titer 15106u/ml.
1)Fermentation liquor pretreatment
Kasugarnycin fermentation liquid pH to 4.7 is adjusted using 25% hydrochloric acid solution, 25min is stirred, stands 50min;Continue to adjust
Kasugarnycin fermentation liquid pH to 2.7 is saved, 25min is stirred, stands 50min.
Polysilicate aluminum chloride calcium 200kg is added in fermentation liquid, continues to stir 25min, stands 70min.
2)Ceramic membrane filter
Drinking water is added in pretreated fermentation liquid, viscosity is down to 2851Pas, and fermentation liquid is warming up to 53 DEG C.
In membrane filtration processes, film filtering is carried out using high speed cross-current flow, in filter process, pressure is controlled in 0.2-
0.3MPa, flow control is in 0.7m3/m2.h。
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water
It is the 65% of fermentating liquid volume.
Film filtering terminates, and collects kasugarnycin filtrate 161m3, chemical titer 6746u/ml.
3)Macroreticular resin decoloration
Filtrate temperature is warming up to 37 DEG C, through macroreticular resin decolorization, it is desirable that for resin column through height than being 1: 6.5, charging is fast
Degree control is controlled in 2.3BV/h, discharging speed in 1.3BV/h.
Filtering terminates, and collects kasugarnycin filtrate 160m3。
4)Nanofiltration concentration
It controls through macroreticular resin de-inking solution temperature at 43 DEG C, carries out nanofiltration, pressure is controlled in 0.5MPa.Nanofiltration terminates,
Filtrate volume is 72m3。
5)Crystallization
3 DEG C are down to through nanofiltration solution temperature, organic solvent ethyl alcohol is added in speed of agitator control in 40r/min, solution
360m3, flow control is in 14ml/min, and when there is crystallization situation, addition crystal seed kasugamycini hydrochloride sterling 10.8kg continues to stir
Mix 135min.Stirring terminates, and stands 165min, then filters, obtain wet solid kasugamycini hydrochloride.
6)It is dry
Wet solid kasugamycini hydrochloride puts into double conic rotary vacuum dryer, and temperature rises to 70 DEG C, and control vacuum degree is-
0.02~-0.08 MPa, dry 13.5h.It is dry to terminate to obtain kasugamycini hydrochloride 994kg.Through detecting, effective content is
99.2%;79% kasugarnycin product cut size has reached 50um.
Embodiment 4
Kasugarnycin fermentation liquid 100m3, chemical titer 15002u/ml.
1)Fermentation liquor pretreatment
Kasugarnycin fermentation liquid pH to 4.6 is adjusted using 27% hydrochloric acid solution, 27min is stirred, stands 55min;Continue to adjust
Kasugarnycin fermentation liquid pH to 2.6 is saved, 27min is stirred, stands 55min.
Polysilicate aluminum chloride calcium 250kg is added in fermentation liquid, continues to stir 28min, stands 75min.
2)Ceramic membrane filter
Drinking water is added in pretreated fermentation liquid, viscosity is down to 2830Pas, and fermentation liquid is warming up to 54 DEG C.
In membrane filtration processes, film filtering is carried out using high speed cross-current flow, in filter process, pressure is controlled in 0.2-
0.3MPa, flow control is in 0.8m3/m2.h。
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water
It is the 67% of fermentating liquid volume.
Film filtering terminates, and collects kasugarnycin filtrate 164m3, chemical titer 6494u/ml.
3)Macroreticular resin decoloration
Filtrate temperature is warming up to 38 DEG C, through macroreticular resin decolorization, it is desirable that for resin column through height than being 1: 6.8, charging is fast
Degree control is controlled in 2.4BV/h, discharging speed in 1.4BV/h.
Filtering terminates, and collects kasugarnycin filtrate 163m3。
4)Nanofiltration concentration
It controls through macroreticular resin de-inking solution temperature at 44 DEG C, carries out nanofiltration, pressure is controlled in 0.5MPa.Nanofiltration terminates,
Filtrate volume is 78m3。
5)Crystallization
4 DEG C are down to through nanofiltration solution temperature, organic solvent propyl alcohol is added in speed of agitator control in 45r/min, solution
430m3, flow control is in 14.5ml/min, and when there is crystallization situation, addition crystal seed kasugamycini hydrochloride sterling 14kg continues to stir
Mix 145min.Stirring terminates, and stands 175min, then filters, obtain wet solid kasugamycini hydrochloride.
6)It is dry
Wet solid kasugamycini hydrochloride puts into double conic rotary vacuum dryer, and temperature rises to 75 DEG C, and control vacuum degree is-
0.02~-0.08 MPa, dry 13h.It is dry to terminate to obtain kasugamycini hydrochloride 987kg.Through detecting, effective content 99.0%;
78% kasugarnycin product cut size has reached 50um.
Embodiment 5
Kasugarnycin fermentation liquid 100m3, chemical titer 14926u/ml.
1)Fermentation liquor pretreatment
Kasugarnycin fermentation liquid pH to 4.5 is adjusted using 30% hydrochloric acid solution, 30min is stirred, stands 60min;Continue to adjust
Kasugarnycin fermentation liquid pH to 2.5 is saved, 30min is stirred, stands 60min.
Polysilicate aluminum chloride calcium 300kg is added in fermentation liquid, continues to stir 30min, stands 80min.
2)Ceramic membrane filter
Drinking water is added in pretreated fermentation liquid, viscosity is down to 2816Pas, and fermentation liquid is warming up to 55 DEG C.
In membrane filtration processes, film filtering is carried out using high speed cross-current flow, in filter process, pressure is controlled in 0.2-
0.3MPa, flow control is in 0.9m3/m2.h。
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and total amount is added in drinking water
It is the 70% of fermentating liquid volume.
Film filtering terminates, and collects kasugarnycin filtrate 167m3, chemical titer 6338u/ml.
4)Macroreticular resin decoloration
Filtrate temperature is warming up to 40 DEG C, through macroreticular resin decolorization, it is desirable that resin column is 1: 7 through height ratio, charging rate
Control is controlled in 2.5BV/h, discharging speed in 1.5BV/h.
Filtering terminates, and collects kasugarnycin filtrate 166m3。
4)Nanofiltration concentration
It controls through macroreticular resin de-inking solution temperature at 45 DEG C, carries out nanofiltration, pressure is controlled in 0.5MPa.Nanofiltration terminates,
Filtrate volume is 83m3。
5)Crystallization
5 DEG C are down to through nanofiltration solution temperature, organic solvent isopropanol is added in speed of agitator control in 50r/min, solution
498m3, flow control is in 15ml/min, and when there is crystallization situation, addition crystal seed kasugamycini hydrochloride sterling 16.6kg continues to stir
Mix 150min.Stirring terminates, and stands 180min, then filters, obtain wet solid kasugamycini hydrochloride.
6)It is dry
Wet solid kasugamycini hydrochloride puts into double conic rotary vacuum dryer, and temperature rises to 80 DEG C, and control vacuum degree is-
0.02~-0.08 MPa, dry 12h.It is dry to terminate to obtain kasugamycini hydrochloride 980kg.Through detecting, effective content 98.9%;
77% kasugarnycin product cut size has reached 50um.
Claims (10)
1. a kind of method using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that its processing step is:
1)Fermentation liquor pretreatment
With mass concentration it is 20-30% hydrochloric acid solution tune pH 4.5-5 by kasugarnycin fermentation liquid, is sufficiently stirred and stands, continues
It is 20-30% hydrochloric acid solution adjustment pH to 2.5-3 with mass concentration, is sufficiently stirred and stands again;Then polysilicate aluminum chloride is added
Calcium is sufficiently stirred and stands;
2)Ceramic membrane filter
By pretreated fermentation liquid, viscosity is brought down below 3000Pas, after be warming up to 50-55 DEG C, then use high speed cross-flow
Mode carries out ceramic membrane filter, collects filtrate;
In filter process, pressure is controlled in 0.2-0.3MPa, and flow control is in 0.5~0.9m3/m2.h;
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and it is hair that total amount, which is added, in drinking water
The 60-70% of zymotic fluid volume, film filtering terminate, and collect filtrate;
3)Macroreticular resin decoloration
Through process 2)Gained filtrate temperature is controlled at 35-40 DEG C, with macroreticular resin decolorization;
4)Nanofiltration concentration
By process 3)Gained macroreticular resin de-inking solution temperature is controlled at 40-45 DEG C, carries out nanofiltration concentration;
5)Crystallization
Nanofiltration solution temperature is down to 0-5 DEG C, organic solvent, flow velocity is added in speed of agitator control in 30-50r/min, solution
Crystal seed is added when there is crystallization situation in 13-15ml/min in control, continues to stir 120-150min, and stirring terminates, and stands
Then 150-180min is filtered, obtain wet solid kasugamycini hydrochloride;
6)Drying.
2. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that
The process 1)In, mixing time 20-30min stands 40-80min.
3. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that
The process 1)In, polysilicate aluminum chloride calcium dosage is the 0.01-0.03% of fermentating liquid volume.
4. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that
The process 2)In, during ceramic membrane filter, pressure is controlled in 0.2-0.3MPa, and flow control is in 0.5~0.9m3/m2.h;
When fermentating liquid volume is down to 35%, drinking water is added, control fermentating liquid volume is 35-40%, and it is hair that total amount, which is added, in drinking water
The 60-70% of zymotic fluid volume.
5. according to, using the method for kasugarnycin broth extraction kasugamycini hydrochloride, feature exists described in claim 1 or 4
In the process 2)In, ceramic membrane is porous ceramic film, and port number 37, material is silica, and pore size filter specification is 0.2 μ
m。
6. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that
The process 3)In, macroreticular resin is D941 anion decolorizing resin, and material is divinylbenzene, and it is 1: 6-7 that resin column diameter height, which compares,
Charging rate control is controlled in 2-2.5BV/h, discharging speed in 1.1-1.5BV/h.
7. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that
The process 4)In, when nanofiltration is concentrated, pressure is controlled in 0.5-1MPa, and solution is concentrated into the 40-50% of original solution volume, used
The material of nanofiltration membrane is polyvinyl alcohol, and nanofiltration membrane component is hollow fiber form.
8. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that
The process 5)In, organic solvent is acetone or methanol or ethyl alcohol or propyl alcohol or isopropanol, dosage are:V organic solvent:V filtrate=
4-6:1。
9. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that
The process 5)In, crystal seed is kasugamycini hydrochloride sterling, and dosage is the 0.01-0.02% of liquor capacity.
10. the method described in accordance with the claim 1 using kasugarnycin broth extraction kasugamycini hydrochloride, it is characterised in that
The process 6)In, dry to use double conic rotary vacuum dryer, 60~80 DEG C of drying temperature, vacuum degree is -0.02~-0.08
MPa, 12~15h of drying time.
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CN110452275B (en) * | 2019-09-17 | 2023-04-07 | 陕西绿盾环境工程研究院有限公司 | Preparation method of high-purity kasugamycin |
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