CN108455599A - A kind of method that antibiotic bacterium dregs dry powder prepares the high performance active carbon rich in micropore - Google Patents
A kind of method that antibiotic bacterium dregs dry powder prepares the high performance active carbon rich in micropore Download PDFInfo
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- CN108455599A CN108455599A CN201810140012.2A CN201810140012A CN108455599A CN 108455599 A CN108455599 A CN 108455599A CN 201810140012 A CN201810140012 A CN 201810140012A CN 108455599 A CN108455599 A CN 108455599A
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- dry powder
- bacterium dregs
- antibiotic bacterium
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Abstract
The present invention provides a kind of method that antibiotic bacterium dregs dry powder prepares the high performance active carbon rich in micropore, belongs to antibiotic bacterium dregs resource technology field.This method is levigate by pending antibiotic bacterium dregs butt first, then in N2It is pyrolyzed under atmosphere, then is filtered after adding lye to adjust pH, and be dried in vacuo drying, and then obtained bacteria residue dry powder is levigate, it is finally heated to 500 650 DEG C, in CO2It is pyrolyzed in atmosphere, obtains the activated carbon rich in micropore.This method is easy to operate, it is easy to accomplish, the high performance active carbon rich in a large amount of micropores can be made, be the new way that antibiotic bacterium dregs are utilized.
Description
Technical field
The present invention relates to antibiotic bacterium dregs resource technology field, particularly relates to a kind of antibiotic bacterium dregs dry powder preparation and be rich in
The method of the high performance active carbon of micropore.
Background technology
China is maximum antibiotic primary producing country and exported country in the world, domestic product antibiotic yield 12 in 2013
Ten thousand tons, 30,000 tons of middle outlet accounts for the 70% of world market.The large-scale production of antibiotic also produces a large amount of antibiosis simultaneously
Plain bacteria residue.Because they contain, there are many noxious materials (such as antibiotic residues, heavy metal and Metabolic Intermediate), are arranged within 2002
Enter《Forbid the types of drugs catalogue used in feed and animal drinking water》, it is put within 2008《National Hazard waste name
Record》.Many researchs find that the antibiotic residue being exposed in natural environment can lead to the generation of antibiotic resistant bacteria.It defends in the world
Raw tissue (WHO) reports that antibiotic resistant bacteria has occurred and propagated in human and animal.Fresh antibiotic bacteria residue property is not
Stabilization, easily corruption simultaneously distribute stench, and finally threaten human health.Therefore, how antibiotic bacterium dregs safely and effectively to be handled
As the previous urgent problem of mesh.
The existing frequently-used bacteria residue treatment technology of pharmacy corporation is security landfill and burning, and security landfill is to put hazardous waste
A kind of disposal options in the soil are set or stored, the purpose is to bury or change the characteristic of hazardous waste, are suitable for disposition not
The hazardous waste of useful constituent or energy can be recycled.Since antibiotic bacterium dregs moisture content is high, security landfill is directly carried out, is deposited
The problems such as taking up a large area, cost of disposal is high and percolate, and it can result in waste of resources.Burning be it is a kind of most thoroughly, answer
With widest processing disposal technology, harmful components can be used with pyrolytic by most of pharmaceutical factory.But due to bacteria residue
Middle N element content is high, is several times to more than ten times of coal, unavoidably will produce a large amount of NOx, deal with improperly and easily cause environment
Problem.It is low additionally, due to its moisture content height, calorific value so that processing cost reaches 2000 yuan/t or so, seriously constrains pharmacy enterprise
The sound development of industry.Therefore, how economically and safely to handle and recycling antibiotic bacterium dregs are that pharmacy corporation is urgently to be resolved hurrily at present
Major issue.
Contain more rich organic matter in antibiotic bacterium dregs, such as crude fat, crude protein, carbohydrate, by pyrolytic technique,
Under conditions of anaerobic or anoxic, the larger molecular organics in bacteria residue can be made to be cracked into flammable micro-molecular gas (H2、CH4And CO
Deng), the methanol of liquid, acetone, acetic acid, acetaldehyde, tar, solvent naphtha and fixed carbon (coke, carbon black) etc., above-mentioned product can return
It receives and utilizes.Therefore, bacteria residue pyrolysis, which prepares activated carbon, has very big potentiality.
Application No. is 201310051119.7 patents to carry out activation system using ionic liquid and metal to antibiotic bacterium dregs
Standby activated carbon.Application No. is 201110388856.7 patents to prepare activated carbon using penicillin or terramycin, can be to bacteria residue
Carry out recycling treatment.But experiment finds that there are a large amount of protein in bacteria residue, the part is easy to cave in pyrolytic process
Deformation is unfavorable for the formation of micropore so that pore structure reduction.Bacteria residue is etched using containing aqueous slkali, removes part
After protein component, the high performance active carbon rich in micropore can be generated by carrying out activation.
Invention content
The high-performance work rich in micropore is prepared the technical problem to be solved in the present invention is to provide a kind of antibiotic bacterium dregs dry powder
The method of property charcoal.
It is as follows that the method comprising the steps of：
(1) by pending antibiotic bacterium dregs butt, the levigate particle for 0.2-2mm；
(2) by the obtained antibiotic bacterium dregs butt particle in step (1) with 10-20 DEG C/min heating rates in 250-
350℃、N2It is pyrolyzed 0.5-2h under atmosphere, obtains coke；
(3) add lye to adjust pH to 9.0-11.0 in the coke that pyrolysis obtains in step (2), stir 1-5h, stand 3-8h
After filter；
(4) coke being obtained by filtration in step (3) is dried under the conditions of 40-80 DEG C by being dried in vacuo；
(5) the levigate particle for 0.3-1mm of coke dry powder after drying step (4)；
(6) dry powder particle of the step (5) after levigate is heated to 500- with 10-20 DEG C/min heating rates in tube furnace
650 DEG C, in CO2It is pyrolyzed 2-7h in atmosphere, obtains the activated carbon rich in micropore.
Wherein, antibiotic bacterium dregs butt pending in step (1) is in ospeneff, gentamicin, streptomysin bacteria residue
The solids that are obtained after drying and other treatment of one or more.
Lye is one or both of sodium hydroxide, potassium hydroxide in step (3).
Alternatively, lye is Ca (OH) in step (3)2The mixed liquor prepared with one or both of NaCl or KCl, wherein
Ca(OH)2Molar ratio with NaCl or KCl is 0.3-0.7:1.
Above two concentration of lye is with OH-Concentration is calculated as 0.3-1.5mol/L.
The above-mentioned technical proposal of the present invention has the beneficial effect that：
This method is easy to operate, it is easy to accomplish, the high performance active carbon rich in a large amount of micropores can be made, be for antibiosis
The new way that plain bacteria residue utilizes.
Description of the drawings
Fig. 1 is that the antibiotic bacterium dregs dry powder of the present invention prepares the method and process flow of the high performance active carbon rich in micropore
Figure.
Specific implementation mode
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
The present invention provides a kind of method that antibiotic bacterium dregs dry powder prepares the high performance active carbon rich in micropore.
As shown in Figure 1, this method step is：
(1) by pending antibiotic bacterium dregs butt, the levigate particle for 0.2-2mm；
(2) by the obtained antibiotic bacterium dregs butt particle in step (1) with 10-20 DEG C/min heating rates in 250-
350℃、N2It is pyrolyzed 0.5-2h under atmosphere, obtains coke；
(3) add lye to adjust pH to 9.0-11.0 in the coke that pyrolysis obtains in step (2), stir 1-5h, stand 3-8h
After filter；
(4) coke being obtained by filtration in step (3) is dried under the conditions of 40-80 DEG C by being dried in vacuo；
(5) the levigate particle for 0.3-1mm of coke dry powder after drying step (4)；
(6) dry powder particle of the step (5) after levigate is heated to 500- with 10-20 DEG C/min heating rates in tube furnace
650 DEG C, in CO2It is pyrolyzed 2-7h in atmosphere, obtains the activated carbon rich in micropore.
It is explained with reference to specific embodiment.
Embodiment 1
The ospeneff bacteria residue butt that certain pharmaceutical factory is obtained by desiccation, the levigate particle for 0.2mm sizes, with 10 DEG C/
Min heating rates are at 350 DEG C, N2It is pyrolyzed 0.5h under atmosphere.The hydroxide of concentration 0.3mol/L is added in the coke that pyrolysis is obtained
Sodium (NaOH) solution is adjusted to pH value 9, stirs 1h, is filtered after standing 8h.The solid being obtained by filtration is passed through under the conditions of 40 DEG C
Dry powder is heated to 500 DEG C by vacuum drying, the levigate particle for 1mm sizes with 20 DEG C/min heating rates in tube furnace,
CO22h is pyrolyzed in atmosphere, it is 677m to obtain specific surface area2The activated carbon of/g, yield 27.7%.
Embodiment 2
The streptomysin bacteria residue butt that certain pharmaceutical factory is obtained by desiccation, the levigate particle for 2mm sizes, with 20 DEG C/min liters
Warm rate is at 250 DEG C, N2It is pyrolyzed 0.5h under atmosphere.The potassium hydroxide of concentration 1.5mol/L is added in the coke that pyrolysis is obtained
(KOH) solution is adjusted to pH value 11, and mechanical agitation 1h is filtered after standing 3h.The solid being obtained by filtration is led under the conditions of 80 DEG C
Vacuum drying drying is crossed, dry powder is heated to 10 DEG C/min heating rates in tube furnace by the levigate particle for 0.3mm sizes
650 DEG C, in CO27h is pyrolyzed in atmosphere, it is 821m to obtain specific surface area2The activated carbon of/g, yield 23.0%.
Embodiment 3
The gentamicin bacteria residue butt that certain pharmaceutical factory is obtained by desiccation, the levigate particle for 0.2mm sizes, with 20 DEG C/
Min heating rates are at 350 DEG C, N2It is pyrolyzed 2h under atmosphere.The Ca (OH) of concentration 2mol/L is added in the coke that pyrolysis is obtained2With
The mixed liquor of NaCl, mixing ratio 0.3:1, it is adjusted to pH value 9, stirs 3h, is filtered after standing 5h.The solid being obtained by filtration is existed
It is dried under the conditions of 40 DEG C by being dried in vacuo, the levigate particle for 0.3mm sizes, by dry powder with 20 DEG C/min heating rates in pipe
500 DEG C are heated in formula stove, in CO27h is pyrolyzed in atmosphere, it is 890m to obtain specific surface area2The activated carbon of/g, yield are
27.1%.
Embodiment 4
The ospeneff bacteria residue butt that certain pharmaceutical factory is obtained by desiccation, the levigate particle for 2mm sizes, with 10 DEG C/
Min heating rates are at 250 DEG C, N2It is pyrolyzed 2h under atmosphere.The Ca (OH) of concentration 0.2mol/L is added in the coke that pyrolysis is obtained2With
The mixed liquor of NaCl, mixing ratio 0.7:1, it is adjusted to pH value 11, mechanical agitation 5h is filtered after standing 8h.By what is be obtained by filtration
Solid is dried under the conditions of 80 DEG C by being dried in vacuo, the levigate particle for 1mm sizes, by dry powder with 10 DEG C/min heating rates
650 DEG C are heated in tube furnace, in CO22h is pyrolyzed in atmosphere, it is 605m to obtain specific surface area2The activated carbon of/g, yield are
25.9%.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of method that antibiotic bacterium dregs dry powder prepares the high performance active carbon rich in micropore, it is characterised in that：Including step
It is as follows：
(1) by pending antibiotic bacterium dregs butt, the levigate particle for 0.2-2mm；
(2) by the obtained antibiotic bacterium dregs butt particle in step (1) with 10-20 DEG C/min heating rates 250-350 DEG C,
N2It is pyrolyzed 0.5-2h under atmosphere, obtains coke；
(3) add lye to adjust pH to 9.0-11.0 in the coke that pyrolysis obtains in step (2), stir 1-5h, stand mistake after 3-8h
Filter；
(4) coke being obtained by filtration in step (3) is dried under the conditions of 40-80 DEG C by being dried in vacuo；
(5) the levigate particle for 0.3-1mm of coke dry powder after drying step (4)；
(6) dry powder particle of the step (5) after levigate is heated to 500-650 with 10-20 DEG C/min heating rates in tube furnace
DEG C, in CO2It is pyrolyzed 2-7h in atmosphere, obtains the activated carbon rich in micropore.
2. the method that antibiotic bacterium dregs dry powder according to claim 1 prepares the high performance active carbon rich in micropore, special
Sign is：Pending antibiotic bacterium dregs butt is in ospeneff, gentamicin, streptomysin bacteria residue in the step (1)
The solid that one or more obtain after drying and other treatment.
3. the method that antibiotic bacterium dregs dry powder according to claim 1 prepares the high performance active carbon rich in micropore, special
Sign is：Lye is one or both of sodium hydroxide, potassium hydroxide in the step (3).
4. the method that antibiotic bacterium dregs dry powder according to claim 1 prepares the high performance active carbon rich in micropore, special
Sign is：Lye is Ca (OH) in the step (3)2The mixed liquor prepared with one or both of NaCl or KCl, wherein Ca
(OH)2Molar ratio with NaCl or KCl is 0.3-0.7:1.
5. the method that antibiotic bacterium dregs dry powder according to claim 3 or 4 prepares the high performance active carbon rich in micropore,
It is characterized in that：The concentration of lye is with OH-Concentration is calculated as 0.3-1.5mol/L.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111003710A (en) * | 2020-01-17 | 2020-04-14 | 宿州学院 | Method for preparing nitrogen-doped graded porous carbon by using waste medicine residues and application of method |
| CN112919463A (en) * | 2021-04-09 | 2021-06-08 | 南京理工大学 | Activated carbon prepared from tiamulin waste salt and preparation method thereof |
| CN114212791A (en) * | 2022-01-06 | 2022-03-22 | 华东理工大学 | Comprehensive treatment method for recycling antibiotic fungi residues |
| CN114229841A (en) * | 2022-01-17 | 2022-03-25 | 华东理工大学 | Method for preparing high-specific-surface-area activated carbon from antibiotic fungi residues |
| CN114832780A (en) * | 2022-06-06 | 2022-08-02 | 华东理工大学 | Antibiotic fungi residue based activated carbon and preparation method and application thereof |
| CN116786082A (en) * | 2023-07-27 | 2023-09-22 | 大同同星抗生素有限责任公司 | Specific adsorbent for oxytetracycline and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114832780A (en) * | 2022-06-06 | 2022-08-02 | 华东理工大学 | Antibiotic fungi residue based activated carbon and preparation method and application thereof |
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| CN116786082B (en) * | 2023-07-27 | 2024-05-28 | 大同同星抗生素有限责任公司 | Specific adsorbent for oxytetracycline and preparation method thereof |
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