CN102553891B - Method for removing residual pharmaceutical ingredients in oxytetracycline pharmaceutical dregs by ultrasonic wave - Google Patents
Method for removing residual pharmaceutical ingredients in oxytetracycline pharmaceutical dregs by ultrasonic wave Download PDFInfo
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- CN102553891B CN102553891B CN201210017665.4A CN201210017665A CN102553891B CN 102553891 B CN102553891 B CN 102553891B CN 201210017665 A CN201210017665 A CN 201210017665A CN 102553891 B CN102553891 B CN 102553891B
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Abstract
The invention discloses a method for removing residual pharmaceutical ingredients in oxytetracycline pharmaceutical dregs by ultrasonic wave, comprising the following steps of: A, heating up oxytetracycline wet pharmaceutical dregs to solidify protein, so that the protein is not influenced by ultrasonic wave; B, cooling the oxytetracycline wet pharmaceutical dregs into normal temperature, adjusting the pH of the oxytetracycline wet pharmaceutical dregs into 0.5-1.0 by hydrochloric acid, and evenly stirring the wet pharmaceutical dregs; and C, putting the evenly-stirred wet pharmaceutical dregs into a container with normal pressure and ultrasonic environment to carry out ultrasonic wave radiation, and degrading and invalidating the oxytetracycline ingredient in the wet pharmaceutical dregs by the acoustic cavitation effect of the ultrasonic wave. The method is quick, low-cost and environment-friendly to treat the oxytetracycline pharmaceutical dregs, and is good in treatment effect, so that the obtained product is heavy in weight and high in use value.
Description
Technical field
The present invention relates to Resource Recovery of Industrial Solid Waste, minimizing and comprehensive utilization technique field, especially a kind of method of utilizing ultrasonic wave to eliminate left drug composition in the terramycin dregs of a decoction.
Background technology
Terramycin is a kind of broad-spectrum antibiotic, is microbial fermentation product, to part gram-positive bacteria, and negative bacterium, Richettsia has stronger bacteriostasis.Terramycin is amphoteric compound, under acid, alkali condition, reaction of degeneration (RD) all easily occurs.Current domestic terramycin production technology is mainly containing fermentation with extract two parts, and it is raw material that fermentation process will be take nearly 10 kinds of organic matters such as starch, soya bean muffin, dextrin, as the synthetic carbon source of microorganism and can; Extraction process regulates pH value for make acidulant of oxalic acid, utilizes potassium ferrocyanide one zinc sulfate to make the collaborative macromolecule impurities such as protein of removing of cleanser, through flame filter press, filters, and removes solid impurity, i.e. the terramycin dregs of a decoction; Filtrate further purifies terramycin filtrate by 122# resin decolorization, finally adjusts the crystallization of pH to 4.8 left and right to obtain Oxytetracycline Base product.Its main component of the terramycin dregs of a decoction is microbial bacteria body cell, undegradable solid organic matters, inorganic salts and the residual compositions such as terramycin.Contain each more than 32% seed amino acid, 30%-40% thick protein and various trace elements, satholith mycin 8-9mg/kg.Due to the antibiotic composition of residual minim in the dregs of a decoction, the environment event unorderedly flow, unordered utilization and unordered disposal causing, has caused certain influence to the people's productive life, and has caused the extensive concern of various circles of society.2009, general office of Chinese Ministry of Environmental Protection has issued " about carrying out the hazardous wastes such as the antibiotic dregs of a decoction, producing and dispose the notice of special examination " (ring is done [2009] No. 80), clear and definite manufacturing enterprise is the first owner of Hazardous Wastes Management prevention and control, and the prevention and cure of pollution situation of the follow-up storage of the terramycin dregs of a decoction, utilization, disposal overall process is monitored.Owing to lacking at present effective processing method, a large amount of terramycin dregs of a decoction can only take expensive burning mode to process, and a large amount of each seed amino acids, thick protein and various trace elements in the dregs of a decoction, also will waste.Approximately 20,000 tons of the annual terramycin output in the whole nation, 1 ton of terramycin of every production approximately produces 4 tons of dregs of a decoction, can produce every year the terramycin dregs of a decoction of 80,000 tons of left and right.The dregs of a decoction have taken a large amount of soils and have stored up for a long time, under natural slacking, run off everywhere, and soil is polluted; Solvable composition permeates downwards from earth's surface with rainwater, to soil, transforms, and makes soil enrichment harmful substance; Or the water that permeates the ground, flow into rivers,lakes and seas, cause the severe contamination of water body; In stacking process, some organic substance decomposes, and produces pernicious gas, causes air pollution.
The method of at present the terramycin dregs of a decoction being processed has two kinds: a kind of is to utilize biotechnology to carry out harmless treatment (200510012998.8) to the antibiotic dregs of a decoction, and it comprises culture medium preparation, inoculation, fermentation.Main component with the antibiotic dregs of a decoction as culture medium, inserts bacterial classification and culture medium in fermentation tank and carries out normal pressure anaerobic fermentation, and fermentation condition is: 24 ℃-28 ℃ of temperature, and pH value is 6.2-6.8, fermentation period is 36-264 hour.It is high that process conditions require, process complexity and the cycle long, and the waste residue proposing after albumen also needs processing.Another kind is to process the terramycin dregs of a decoction are processed to (ZL200710185390.4) by chemical method, and the required time is long, and hydrochloric acid consumption concentration is high, and consumption is large, and processing procedure methyl alcohol, unavoidably has the residual of methyl alcohol.So the resource of the terramycin dregs of a decoction, innoxious industrial applications are still problem anxious to be resolved at present.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of utilizing ultrasonic wave to eliminate the left drug composition in the terramycin dregs of a decoction, can solve the deficiencies in the prior art,, environmental protection quick, cheap to the processing procedure of the terramycin dregs of a decoction, and treatment effect is good, and the heavy value of products therefrom is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows.
Utilize ultrasonic wave to eliminate a method for left drug composition in the terramycin dregs of a decoction, its step comprises:
A, the wet dregs of a decoction of terramycin are heated to 60 ℃-80 ℃, to solidify protein, make it not to be subject to hyperacoustic impact;
B, the wet dregs of a decoction of terramycin utilize hydrochloric acid to regulate its pH for 0.5-1.0 after being cooled to normal temperature, and the dregs of a decoction that will wet stir;
C, the wet dregs of a decoction that stir are put into the container of normal pressure, ultrasound environments, under stable cavitation condition, controlling the sound intensity is (0.5-10) W/cm
2, supersonic frequency is 20kHz-200kHz; Carry out Ultrasonic Radiation, utilize hyperacoustic sound cavitation effect to make the degraded of terramycin composition, the inefficacy in the wet dregs of a decoction, then filter, add basifier the pH value of gained filter residue is adjusted to 4-5, oven dry or natural drying.
As a preferred technical solution of the present invention, in steps A, the wet dregs of a decoction of terramycin are heated to 70 ℃-75 ℃ and be incubated 5min-15min, to solidify protein, make it not to be subject to hyperacoustic impact.
As a preferred technical solution of the present invention, in step B, the wet dregs of a decoction of terramycin are cooled to after normal temperature, the ratio that adds the hydrochloric acid 10mL-25mL of 0.4mol/L-0.6mol/L in the wet dregs of a decoction of every 50 grams of terramycin, regulating its pH is 0.5-1.0, the dregs of a decoction obtain dilution simultaneously, and the dregs of a decoction that finally will wet stir.
As a preferred technical solution of the present invention, in step C, the duration of Ultrasonic Radiation is 10min-30min.
As a preferred technical solution of the present invention, in step C, filter gained filtrate and return to step B, Substitute For Partial hydrochloric acid recycles as pH adjusting agent, realizes refuse zero-emission.
As a preferred technical solution of the present invention, in step C, utilize calcium hydroxide or calcium oxide that the pH value of the gained dregs of a decoction is adjusted to 4-5.
The beneficial effect that adopts technique scheme to produce is:
The present invention adopts supercritical ultrasonics technology to remove the residual drug in the terramycin dregs of a decoction, hyperacoustic cavitation that process conditions of the present invention are created, it can produce localized hyperthermia's hyperbaric environment of about 5000K and 100MPa in instant of detonation, and the about 110m/s of the speed that produces has the microjet of intense impact power, these conditions are enough to make the chemical bond rupture of residual active constituent in the dregs of a decoction and water burning occur, pyrolytic or radical reaction, thereby residual active ingredient in the elimination dregs of a decoction, and retain the thick protein in the dregs of a decoction, make the dregs of a decoction as feed addictive, whole processing procedure is quick, cheap, environmental protection, the degradation condition of satholith mycin is gentle, degradation rate is fast, there is no secondary pollution,
Processing method of the present invention, in step B, adds the ratio of the hydrochloric acid 10mL-25mL of 0.5mol/L in the wet dregs of a decoction of every 50 grams of terramycin, regulating its pH is 0.5-1.0, like this, when regulating dregs of a decoction pH, it has been carried out to effective dilution, for follow-up ultrasonic processing is got ready;
The wet dregs of a decoction after ultrasonic processing filter gained filter residue as finished product, left drug composition has wherein obtained effective elimination, several amino acids, trace element and thick protein have been retained, can be used as safe forage protein application, there is high industrial or agricultural industrial value, and filter gained filtrate because of hydrochloric, add wherein the hydrochloric acid that purity is higher to be adjusted to after suitable concn, can return to step B as regulating the reagent of pH to recycle, realize refuse zero-emission;
The concrete test data that the embodiment that vide infra partly provides, utilizes processing method of the present invention, and in the dregs of a decoction, the clearance of satholith mycin is 90%-100%, there is no discharge of wastewater; With mouse, to processing the rear terramycin dregs of a decoction, carry out subchronic toxicity test, confirm that the terramycin dregs of a decoction do not produce noxious material in processing procedure.
The specific embodiment
Following examples describe the present invention in detail.Various raw material used in the present invention and items of equipment are conventional commercially available prod, all can be bought directly and be obtained by market.
Embodiment 1
Get the wet dregs of a decoction of 50 grams of terramycin and put in beaker, place heating water bath to 70 ℃-75 ℃ of insulation 10min, be cooled to the hydrochloric acid solution 25mL that adds 0.5mol/L after room temperature, be uniformly mixed, measuring pH is 0.5; The dregs of a decoction that mix are placed in ultrasonic instrument, are 1W/cm at supersonic frequency 20kHz, the sound intensity
2time, process centrifugal filtration after 30min, reclaim filtrate and recycle as pH adjusting agent, calcium oxide regulates pH value 4.5 for filter residue, puts and in drying box, at 90 ℃, is dried 30min; Cooling Hou An《 People's Republic of China (PRC) veterinary drug allusion quotation " standard surveys the terramycin dregs of a decoction after processed, and the mould cellulose content of satholith is reduced to 0.07% by 0.57%, and clearance is 87.7%, and crude protein content, by 40.3%, drops to 36.9%, reduces 8.4%.
Embodiment 2
Get the wet dregs of a decoction of 50 grams of terramycin and put in beaker, place heating water bath to 70 ℃-75 ℃ of insulation 20min, be cooled to the hydrochloric acid solution 20mL that adds 0.5mol/L after room temperature, be uniformly mixed, measuring pH is 0.6; The dregs of a decoction that mix are placed in ultrasonic instrument, are 2W/cm at supersonic frequency 40kHz, the sound intensity
2time, process centrifugal filtration after 10min, reclaim filtrate and recycle as pH adjusting agent, calcium oxide regulates pH value 4.5 for filter residue, puts and in drying box, at 90 ℃, is dried 30min; Cooling Hou An《 People's Republic of China (PRC) veterinary drug allusion quotation " standard surveys the terramycin dregs of a decoction after processed, and the mould cellulose content of satholith is reduced to 0.055% by 0.57%, and clearance is 90.3%, and crude protein content, by 40.3%, drops to 36.9%, reduces 8.4%.
Embodiment 3
Get the wet dregs of a decoction of 50 grams of terramycin and put in beaker, place heating water bath to 70 ℃-75 ℃ of insulation 10min, be cooled to the hydrochloric acid solution 1mL that adds 0.5mol/L after room temperature, be uniformly mixed, measuring pH is 0.8; The dregs of a decoction that mix are placed in ultrasonic instrument, are 3.5W/cm at supersonic frequency 80kHz, the sound intensity
2time, process centrifugal filtration after 20min, reclaim filtrate and recycle as pH adjusting agent, calcium oxide regulates pH value 4.5 for filter residue, puts and in drying box, at 90 ℃, is dried 30min; Cooling Hou An《 People's Republic of China (PRC) veterinary drug allusion quotation " standard surveys the terramycin dregs of a decoction after processed, and the mould cellulose content of satholith 0.57% is reduced to 0.06%, and clearance is 89.5%, and crude protein content, by 40.3%, drops to 36.9%, reduces 8.4%.
Embodiment 4
Get the wet dregs of a decoction of 50 grams of terramycin and put in beaker, place heating water bath to 70 ℃-75 ℃ of insulation 10min, be cooled to the hydrochloric acid solution 10mL that adds 0.5mol/L after room temperature, be uniformly mixed, measuring pH is 1; The dregs of a decoction that mix are placed in ultrasonic instrument, are 4W/cm at supersonic frequency 120kHz, the sound intensity
2time, process centrifugal filtration after 10min, reclaim filtrate and recycle as pH adjusting agent, calcium oxide regulates pH value 4.5 for filter residue, puts and in drying box, at 90 ℃, is dried 30min; Cooling Hou An《 People's Republic of China (PRC) veterinary drug allusion quotation " standard surveys the terramycin dregs of a decoction after processed, and the mould cellulose content of satholith 0.57% is reduced to 0.03%, and clearance is 94.7%, and crude protein content, by 40.3%, drops to 36.9%, reduces 8.4%.
Embodiment 5
Get the wet dregs of a decoction of 50 grams of terramycin and put in beaker, place heating water bath to 70 ℃-75 ℃ of insulation 10min, be cooled to the hydrochloric acid solution 10mL that adds 0.5mol/L after room temperature, be uniformly mixed, measuring pH is 1; The dregs of a decoction that mix are placed in ultrasonic instrument, are 5W/cm at supersonic frequency 200kHz, the sound intensity
2time, process centrifugal filtration after 10min, reclaim filtrate and recycle as pH adjusting agent, calcium oxide regulates pH value 4.5 for filter residue, puts and in drying box, at 90 ℃, is dried 30min; Cooling Hou An《 People's Republic of China (PRC) veterinary drug allusion quotation " standard surveys the terramycin dregs of a decoction after processed, and the mould cellulose content of satholith 0.57% is reduced to 0.02%, and clearance is 96.5%, and crude protein content, by 40.3%, drops to 36.9%, reduces 8.4%.
Embodiment 6
Get the wet dregs of a decoction of 50 grams of terramycin and put in beaker, place heating water bath to 70 ℃-75 ℃ of insulation 10min, be cooled to the hydrochloric acid solution 10mL that adds 0.5mol/L after room temperature, be uniformly mixed, measuring pH is 1; The dregs of a decoction that mix are placed in ultrasonic instrument, are 5W/cm at supersonic frequency 200kHz, the sound intensity
2time, centrifugal filtration after ultrasonic processing 10min, reclaims filtrate and recycles as pH adjusting agent, and calcium hydroxide regulates pH value 4.5 for filter residue, puts and in drying box, at 90 ℃, is dried 30min; Cooling Hou An《 People's Republic of China (PRC) veterinary drug allusion quotation " standard surveys the terramycin dregs of a decoction after processed, and the mould cellulose content of satholith 0.57% is reduced to 0.025%, and clearance is 95.6%, and crude protein content, by 40.3%, drops to 36.9%, reduces 8.4%.
Foregoing description only proposes as the enforceable technical scheme of the present invention, not as the Single restriction condition to its technical scheme itself.
Claims (3)
1. utilize ultrasonic wave to eliminate a method for left drug composition in the terramycin dregs of a decoction, its characterization step comprises:
A, the wet dregs of a decoction of terramycin are heated to 70 ℃-75 ℃ and be incubated 5min-15min, to solidify protein, make it not to be subject to hyperacoustic impact;
B, the wet dregs of a decoction of terramycin are cooled to after normal temperature, add the ratio of the hydrochloric acid 10mL-25mL of 0.4mol/L-0.6mol/L in the wet dregs of a decoction of every 50 grams of terramycin, and regulating its pH is 0.5-1.0, and the dregs of a decoction obtain dilution simultaneously, and the dregs of a decoction that finally will wet stir;
C, the wet dregs of a decoction that stir are put into the container of normal pressure, ultrasound environments, under stable cavitation condition, controlling the sound intensity is (0.5-10) W/cm
2, supersonic frequency is 20kHz-200kHz; Carry out Ultrasonic Radiation, the duration of Ultrasonic Radiation is 10min-30min, utilizes hyperacoustic sound cavitation effect to make the degraded of terramycin composition, the inefficacy in the wet dregs of a decoction, then filters, add basifier the pH value of gained filter residue is adjusted to 4-5, oven dry or natural drying.
2. the method for utilizing ultrasonic wave to eliminate left drug composition in the terramycin dregs of a decoction according to claim 1, is characterized in that: in step C, filter gained filtrate and return to step B, Substitute For Partial hydrochloric acid recycles as pH adjusting agent, realizes refuse zero-emission.
3. the method for utilizing ultrasonic wave to eliminate left drug composition in the terramycin dregs of a decoction according to claim 1, is characterized in that: in step C, utilize calcium hydroxide or calcium oxide that the pH value of the gained dregs of a decoction is adjusted to 4-5.
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| CN104351483A (en) * | 2014-11-13 | 2015-02-18 | 河北圣雪大成制药有限责任公司 | Preparation method of completely fermented oxytetracycline calcium granules |
| CN105127178A (en) * | 2015-09-01 | 2015-12-09 | 宁夏大学 | Method for eliminating residual tetracycline in pharmaceutical dregs in physical-chemical oxidation combination manner |
| CN106422152B (en) * | 2016-09-22 | 2020-07-03 | 上海化工研究院有限公司 | Method for removing oxytetracycline in biological medicine waste residues |
Citations (5)
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| CN1613534A (en) * | 2003-11-03 | 2005-05-11 | 浙江工业大学 | Processing method for antibiotics bacterial slag containing zinc |
| CN101176511A (en) * | 2007-12-13 | 2008-05-14 | 河北大学 | Method for removing or reducing residual medicament component in ursocycline medicine slag |
| CN101380509A (en) * | 2008-10-16 | 2009-03-11 | 河南工业大学 | Macrolide antibiotic bacterium dregs innocent treatment method |
| CN102126813A (en) * | 2011-01-25 | 2011-07-20 | 山东美泉环保科技有限公司 | System and process for treating oxytetracycline waste water by anaerobic bio-treatment method |
| CN102285703A (en) * | 2011-06-15 | 2011-12-21 | 南京信息工程大学 | Method for ultrasonic removal of sulfadiazine in water |
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| JP3234640B2 (en) * | 1992-08-03 | 2001-12-04 | キヤノン株式会社 | Soil restoration method |
| JP2006182579A (en) * | 2004-12-27 | 2006-07-13 | Ichimura:Kk | Manufacturing method of compost |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613534A (en) * | 2003-11-03 | 2005-05-11 | 浙江工业大学 | Processing method for antibiotics bacterial slag containing zinc |
| CN101176511A (en) * | 2007-12-13 | 2008-05-14 | 河北大学 | Method for removing or reducing residual medicament component in ursocycline medicine slag |
| CN101380509A (en) * | 2008-10-16 | 2009-03-11 | 河南工业大学 | Macrolide antibiotic bacterium dregs innocent treatment method |
| CN102126813A (en) * | 2011-01-25 | 2011-07-20 | 山东美泉环保科技有限公司 | System and process for treating oxytetracycline waste water by anaerobic bio-treatment method |
| CN102285703A (en) * | 2011-06-15 | 2011-12-21 | 南京信息工程大学 | Method for ultrasonic removal of sulfadiazine in water |
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