CN103243133B - Production technology for extracting oxytetracycline dihyclorate by utilizing hydrochloric acid and oxalic acid - Google Patents
Production technology for extracting oxytetracycline dihyclorate by utilizing hydrochloric acid and oxalic acid Download PDFInfo
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- CN103243133B CN103243133B CN201310178383.7A CN201310178383A CN103243133B CN 103243133 B CN103243133 B CN 103243133B CN 201310178383 A CN201310178383 A CN 201310178383A CN 103243133 B CN103243133 B CN 103243133B
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Abstract
The invention discloses a production technology for extracting oxytetracycline dihyclorate by utilizing hydrochloric acid and oxalic acid. The production technology comprises the following steps of: (1) fermenting; (2) acidizing and filtering; (3) decoloring and crystallizing; (4) drying, mixing and packaging to prepare an oxytetracycline dihyclorate product, wherein the step (2) is as follows: acidizing a fermentation liquor, namely adding oxalate to the fermentation liquor prepared in the step (1) to adjust the PH value of the fermentation liquor to 2.10-2.20; and then adding hydrochloric acid to the fermentation liquor, and adjusting the PH value of the fermentation liquor to 1.80-2.0. The production technology has the advantages that adjustment is carried out by an extraction and acidification process; the production cost of a company is greatly reduced by the hydrochloric acid and the oxalate; the purchasing cost of raw materials is reduced; the production cost can be saved by **-** each month; the production cost is reduced; and the market competitiveness of an enterprise is improved.
Description
Technical field
The present invention relates to a kind of production technique extracting Oxytetracycline Base BP (98), particularly relate to a kind of by hydrochloric acid and oxalic acid and by the production technique extracting Oxytetracycline Base BP (98).
Background technology
Oxytetracycline Base BP (98) belongs to Broad spectrum antibiotics, prepared by soil streptomycete, all there is restraining effect to gram-positive microorganism and negative bacterium, attached corpus hemorrhagicum, chlamydozoan, Mycoplasma, Rickettsiae, spirochete, actinomycetes, vibrios and some protozoon (as: coccidia).Be mainly used in livestock and poultry medicine and fodder additives now.
In the production process of Oxytetracycline Base BP (98), owing to using a large amount of oxalic acid, oxalic acid price is caused constantly to rise, high, cause the production cost of Oxytetracycline Base BP (98) (bulk drug) to go up, enterprise's competitive power in Oxytetracycline Base BP (98) production industry is reduced year by year.
Utility model content
The object of the present invention is to provide a kind of Oxytetracycline Base BP (98) production cost of greatly reducing, by hydrochloric acid with oxalic acid and use extracts the production technique of Oxytetracycline Base BP (98).
Object of the present invention is implemented by following technical scheme, and a kind of by hydrochloric acid and oxalic acid and by the production technique extracting Oxytetracycline Base BP (98), it comprises the steps: (1) ferments; (2) acidifying is filtered; (3) decolouring crystallization; (4) the obtained Oxytetracycline Base BP (98) finished product of dry, mixed powder packaging;
Described step (1) fermentation comprises:
Prepared by a, slant pore: cultivate spore condition: slant pore 36 ~ 37 DEG C of cultivations, humidity 55% ~ 60%, incubation time 96 ~ 120h;
B, first class seed pot are cultivated: culture temperature is 30.5 ~ 31.5 DEG C, and equipment seals, pneumatic blending, after fermentation about 26 ~ 28h, move into secondary seed tank;
C, secondary seed tank are cultivated: culture temperature is 30.5 ~ 31.5 DEG C, mechanical stirring, logical sterile air, and fermentation 20 ~ 28h moves into three grade fermemtation tank;
D, three grade fermemtation tank ferment: inoculum size is mass percentage 15 ~ 30%, and omnidistance temperature of fermenting controls at 30 ~ 31 DEG C, mechanical stirring, fermentation 160 ~ 163h, and fermenting process oxygen ventilation amount is: 0.8 ~ 1.0v/m, finally obtained fermented liquid.
Described step (2) acidifying is filtered and is comprised:
A, fermented liquid acidifying: in the described fermented liquid that described step (1) is obtained, add oxalic acid adjust the pH value of described fermented liquid to 2.10 ~ 2.20, make the terramycin release in described fermented liquid complete, and then hydrochloric acid is added in described fermented liquid, adjust the pH value of described fermented liquid to 1.80 ~ 2.0;
The purifying of b, fermented liquid: add yellow prussiate of soda and zinc sulfate in the described fermented liquid after acidifying, wherein, the interpolation quality of described yellow prussiate of soda is the 0.25%-0.35% of described fermentating liquid volume, and the interpolation quality of described zinc sulfate is the 0.2%-0.3% of described fermentating liquid volume; Add described yellow prussiate of soda and described zinc sulfate plays adsorption, be used for adsorbing pigment, protein and the subparticle in fermented liquid, purifying fermentation liquor.
The filtration of c, fermented liquid: the described filtering fermentation liquor after purifying is obtained filtrate.
Described step (3) decolouring crystallization comprises:
A, filtrate decolouring: described filtrate is passed into bleacher, by 122 wherein
#resin decolours, and obtains destainer, removes the pigment in filtrate and organic impurity further, to improve filtrate quality;
B, destainer filtering and heating: described destainer is filtered, and be heated to 28 ~ 30 DEG C, obtain filter rear decoloring liquid;
C, filter rear decoloring liquid Crystallization Separation: be add S-WAT in the ammoniacal liquor of 15% to volume percent, the interpolation quality of S-WAT is 2% of ammoniacal liquor volume, make basifier, then in described filter rear decoloring liquid, described basifier is added, described filter rear decoloring liquid pH value is adjusted to 4.4 ~ 4.8, obtain crystal solution, to the obtained wet crystal of crystal solution separating, washing.
The invention has the advantages that, by extracting acidification technique adjustment, adopt hydrochloric acid and oxalic acid also with greatly reducing company's production cost, reduce purchasing of raw materials expense expenditure, as all used oxalic acid to carry out acidifying under existing industrial scale in 2012, monthly oxalic acid usage quantity is 500 tons, but adopt hydrochloric acid and oxalic acid also with technique adjustment, monthly hydrochloric acid consumption is 150 tons, consumption of oxalic acid drops to 350 tons, monthly for company saves oxalic acid 150 tons, according to market prices current, oxalic acid procurement price per ton is 6600 yuan, hydrochloric acid procurement price per ton is 674 yuan, after adopting the present invention program, monthly can save production cost 88.895 ten thousand yuan, production cost reduces, and improves the market competitiveness of enterprise.
Accompanying drawing explanation
Fig. 1 is a kind of by hydrochloric acid and oxalic acid and with the production technological process extracting Oxytetracycline Base BP (98).
Embodiment:
Embodiment 1: a kind of by hydrochloric acid and oxalic acid and by the production technique extracting Oxytetracycline Base BP (98), it comprises the steps: (1) ferments; (2) acidifying is filtered; (3) decolouring crystallization; (4) the obtained Oxytetracycline Base BP (98) finished product of dry, mixed powder packaging;
Wherein, step (1) fermentation comprises:
Prepared by a, slant pore: cultivate spore condition: slant pore 36 DEG C of cultivations, humidity 55%, incubation time 96h;
B, first class seed pot are cultivated: culture temperature is 30.5 DEG C, and equipment seals, pneumatic blending, after the about 26h that ferments, move into secondary seed tank;
C, secondary seed tank are cultivated: culture temperature is 30.5 DEG C, mechanical stirring, logical sterile air, and fermentation 20h moves into three grade fermemtation tank;
D, three grade fermemtation tank ferment: inoculum size is mass percentage 15%, and omnidistance temperature of fermenting controls at 30 DEG C, mechanical stirring, fermentation 160h, and fermenting process oxygen ventilation amount is: 0.8v/m, finally obtained fermented liquid.
Step (2) acidifying is filtered and is comprised:
A, fermented liquid acidifying: the pH value adding oxalic acid adjustment fermented liquid in the fermented liquid that step (1) is obtained is to 2.10, and make the terramycin release in fermented liquid complete, and then add hydrochloric acid in fermented liquid, the pH value of adjustment fermented liquid is to 1.80;
The purifying of b, fermented liquid: add yellow prussiate of soda and zinc sulfate in the fermented liquid after acidifying, wherein, the interpolation quality of yellow prussiate of soda is 0.25% of fermentating liquid volume, and the interpolation quality of zinc sulfate is 0.2% of fermentating liquid volume; Interpolation yellow prussiate of soda and zinc sulfate play adsorption, are used for adsorbing pigment, protein and the subparticle in fermented liquid, purifying fermentation liquor.
The filtration of c, fermented liquid: the filtering fermentation liquor after purifying is obtained filtrate.
Step (3) decolouring crystallization comprises:
A, filtrate decolouring: filtrate is passed into bleacher, by 122 wherein
#resin decolours, and obtains destainer, removes the pigment in filtrate and organic impurity further, to improve filtrate quality;
B, destainer filtering and heating: destainer is filtered, and be heated to 28 DEG C, obtain filter rear decoloring liquid;
C, filter rear decoloring liquid Crystallization Separation: be add S-WAT in the ammoniacal liquor of 15% to volume percent, the interpolation quality of S-WAT is 2% of ammoniacal liquor volume, make basifier, then in described filter rear decoloring liquid, described basifier is added, described filter rear decoloring liquid pH value is adjusted to 4.4, obtain crystal solution, to the obtained wet crystal of crystal solution separating, washing.
Embodiment 2: a kind of by hydrochloric acid and oxalic acid and by the production technique extracting Oxytetracycline Base BP (98), it comprises the steps: (1) ferments; (2) acidifying is filtered; (3) decolouring crystallization; (4) the obtained Oxytetracycline Base BP (98) finished product of dry, mixed powder packaging;
Wherein step (1) fermentation comprises:
Prepared by a, slant pore: cultivate spore condition: slant pore 37 DEG C of cultivations, humidity 60%, incubation time 120h;
B, first class seed pot are cultivated: culture temperature is 31.5 DEG C, and equipment seals, pneumatic blending, after the about 28h that ferments, move into secondary seed tank;
C, secondary seed tank are cultivated: culture temperature is 31.5 DEG C, mechanical stirring, logical sterile air, and fermentation 28h moves into three grade fermemtation tank;
D, three grade fermemtation tank ferment: inoculum size is mass percentage 30%, and omnidistance temperature of fermenting controls at 31 DEG C, mechanical stirring, fermentation 163h, and fermenting process oxygen ventilation amount is: 1.0v/m, finally obtained fermented liquid.
Step (2) acidifying is filtered and is comprised:
A, fermented liquid acidifying: the pH value adding oxalic acid adjustment fermented liquid in the fermented liquid that described step (1) is obtained is to 2.20, and make the terramycin release in fermented liquid complete, and then add hydrochloric acid in fermented liquid, the pH value of adjustment fermented liquid is to 2.0;
The purifying of b, fermented liquid: add yellow prussiate of soda and zinc sulfate in the fermented liquid after acidifying, wherein, the interpolation quality of yellow prussiate of soda is 0.35% of fermentating liquid volume, and the interpolation quality of zinc sulfate is 0.3% of fermentating liquid volume; Interpolation yellow prussiate of soda and zinc sulfate play adsorption, are used for adsorbing pigment, protein and the subparticle in fermented liquid, purifying fermentation liquor.
The filtration of c, fermented liquid: the filtering fermentation liquor after purifying is obtained filtrate.
Described step (3) decolouring crystallization comprises:
A, filtrate decolouring: filtrate is passed into bleacher, by 122 wherein
#resin decolours, and obtains destainer, removes the pigment in filtrate and organic impurity further, to improve filtrate quality;
B, destainer filtering and heating: destainer is filtered, and be heated to 30 DEG C, obtain filter rear decoloring liquid;
C, filter rear decoloring liquid Crystallization Separation: be add S-WAT in the ammoniacal liquor of 15% to volume percent, the interpolation quality of S-WAT is 2% of ammoniacal liquor volume, make basifier, then in filter rear decoloring liquid, basifier is added, filter rear decoloring liquid pH value is adjusted to 4.8, obtain crystal solution, to the obtained wet crystal of crystal solution separating, washing.
Embodiment 3: a kind of by hydrochloric acid and oxalic acid and by the production technique extracting Oxytetracycline Base BP (98), it comprises the steps: (1) ferments; (2) acidifying is filtered; (3) decolouring crystallization; (4) the obtained Oxytetracycline Base BP (98) finished product of dry, mixed powder packaging;
Wherein, step (1) fermentation comprises:
Prepared by a, slant pore: cultivate spore condition: slant pore 36.5 DEG C of cultivations, humidity 58%, incubation time 110h;
B, first class seed pot are cultivated: culture temperature is 31 DEG C, and equipment seals, pneumatic blending, after the about 27h that ferments, move into secondary seed tank;
C, secondary seed tank are cultivated: culture temperature is 31 DEG C, mechanical stirring, logical sterile air, and fermentation 24h moves into three grade fermemtation tank;
D, three grade fermemtation tank ferment: inoculum size is mass percentage 20%, and omnidistance temperature of fermenting controls at 30.5 DEG C, mechanical stirring, fermentation 161h, and fermenting process oxygen ventilation amount is: 0.9v/m, finally obtained fermented liquid.
Described step (2) acidifying is filtered and is comprised:
A, fermented liquid acidifying: the pH value adding oxalic acid adjustment fermented liquid in the fermented liquid that described step (1) is obtained is to 2.15, and make the terramycin release in fermented liquid complete, and then add hydrochloric acid in fermented liquid, the pH value of adjustment fermented liquid is to 1.90;
The purifying of b, fermented liquid: add yellow prussiate of soda and zinc sulfate in the fermented liquid after acidifying, wherein, the interpolation quality of yellow prussiate of soda is 0.3% of fermentating liquid volume, and the interpolation quality of zinc sulfate is 0.25% of fermentating liquid volume; Interpolation yellow prussiate of soda and zinc sulfate play adsorption, are used for adsorbing pigment, protein and the subparticle in fermented liquid, purifying fermentation liquor.
The filtration of c, fermented liquid: the filtering fermentation liquor after purifying is obtained filtrate.
Described step (3) decolouring crystallization comprises:
A, filtrate decolouring: filtrate is passed into bleacher, by 122 wherein
#resin decolours, and obtains destainer, removes the pigment in filtrate and organic impurity further, to improve filtrate quality;
B, destainer filtering and heating: destainer is filtered, and be heated to 29 DEG C, obtain filter rear decoloring liquid;
C, filter rear decoloring liquid Crystallization Separation: be add S-WAT in the ammoniacal liquor of 15% to volume percent, the interpolation quality of S-WAT is 2% of ammoniacal liquor volume, make basifier, then in filter rear decoloring liquid, basifier is added, filter rear decoloring liquid pH value is adjusted to 4.6, obtain crystal solution, to the obtained wet crystal of crystal solution separating, washing.
Claims (2)
1. hydrochloric acid and oxalic acid are also used the production technique extracting Oxytetracycline Base BP (98), fermentation that it comprises the steps: (1); (2) acidifying is filtered; (3) decolouring crystallization; (4) the obtained Oxytetracycline Base BP (98) finished product of dry, mixed powder packaging; It is characterized in that, described step (2) acidifying is filtered and is comprised:
A, fermented liquid acidifying: in the fermented liquid that described step (1) is obtained, add the pH value of oxalic acid adjustment fermented liquid to 2.10 ~ 2.20, and then add hydrochloric acid in fermented liquid, the pH value of adjustment fermented liquid is to 1.80 ~ 2.0;
The purifying of b, fermented liquid: add yellow prussiate of soda and zinc sulfate in the described fermented liquid after acidifying, wherein, the interpolation quality of described yellow prussiate of soda is the 0.25%-0.35% of described fermentating liquid volume, and the interpolation quality of described zinc sulfate is the 0.2%-0.3% of described fermentating liquid volume;
The filtration of c, fermented liquid: the described filtering fermentation liquor after purifying is obtained filtrate;
Described step (3) decolouring crystallization comprises:
A, filtrate decolouring: described filtrate is passed into bleacher, is decoloured by 122# resin wherein, obtain destainer;
B, destainer filtering and heating: described destainer is filtered, and be heated to 28 ~ 30 DEG C, obtain filter rear decoloring liquid;
C, filter rear decoloring liquid Crystallization Separation: be add S-WAT in the ammoniacal liquor of 15% to volume percent, the interpolation quality of S-WAT is 2% of ammoniacal liquor volume, make basifier, then in described filter rear decoloring liquid, described basifier is added, described filter rear decoloring liquid pH value is adjusted to 4.4 ~ 4.8, obtain crystal solution, to the obtained wet crystal of crystal solution separating, washing.
2. according to claim 1ly a kind ofly hydrochloric acid and oxalic acid by the production technique extracting Oxytetracycline Base BP (98), to be it is characterized in that, described step (1) ferments and comprises:
Prepared by a, slant pore: cultivate spore condition: slant pore 36 ~ 37 DEG C of cultivations, humidity 55% ~ 60%, incubation time 96 ~ 120h;
B, first class seed pot are cultivated: culture temperature is 30.5 ~ 31.5 DEG C, and equipment seals, pneumatic blending, after fermentation about 26 ~ 28h, move into secondary seed tank;
C, secondary seed tank are cultivated: culture temperature is 30.5 ~ 31.5 DEG C, mechanical stirring, logical sterile air, and fermentation 20 ~ 28h moves into three grade fermemtation tank;
D, three grade fermemtation tank ferment: inoculum size is mass percentage 15 ~ 30%, and omnidistance temperature of fermenting controls at 30 ~ 31 DEG C, mechanical stirring, fermentation 160 ~ 163h, and fermenting process oxygen ventilation amount is: 0.8 ~ 1.0v/m, final obtained described fermented liquid.
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| CN104894203A (en) * | 2015-05-27 | 2015-09-09 | 合肥卓元科技服务有限公司 | Production technique of high-purity oxytetracycline |
| CN106380422B (en) * | 2016-08-29 | 2018-04-03 | 河北健民淀粉糖业有限公司 | A kind of method that low phosphorus content terramycin finished product is extracted from Performance in Oxytetracycline Fermentation Broth |
| CN106119332A (en) * | 2016-08-29 | 2016-11-16 | 河北健民淀粉糖业有限公司 | A kind of oxytetracycline production technology |
| CN107904276A (en) * | 2017-12-25 | 2018-04-13 | 安徽永生堂药业有限责任公司 | A kind of production technology of hydroxytetracycline tablet |
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