CN110041142A - A method of amino acid Water soluble fertilizer is prepared using antibiotic fermentation waste residue - Google Patents
A method of amino acid Water soluble fertilizer is prepared using antibiotic fermentation waste residue Download PDFInfo
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- CN110041142A CN110041142A CN201910469051.1A CN201910469051A CN110041142A CN 110041142 A CN110041142 A CN 110041142A CN 201910469051 A CN201910469051 A CN 201910469051A CN 110041142 A CN110041142 A CN 110041142A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C11/00—Other nitrogenous fertilisers
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/20—Liquid fertilisers
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Abstract
The present invention relates to a kind of methods for preparing amino acid Water soluble fertilizer using antibiotic fermentation waste residue, by preprocessing process, i.e., degradation agent are added into antibiotic fermentation residue, reacted to obtain innoxious waste residue slurries；And hydrolytic process, i.e., the rush hydrolytic reagent of doses is added into waste residue slurries, reaction is hydrolyzed, after being separated by filtration, the amino acid Water soluble fertilizer of resource utilization can be obtained.Compared with prior art, the present invention has energy conservation and environmental protection, efficient, low cost, realizes that waste residue is turned waste into wealth, and improves the advantages that china natural resources synthesization is using level.
Description
Technical field
The present invention relates to antibiotic fermentation waste residue harmless treatment fields, and in particular to a kind of to use antibiotic fermentation waste residue
The method for preparing amino acid Water soluble fertilizer.
Background technique
China is the world's largest antibiotic production of raw medicine and big export country, produces more than 70 kinds antibiotic, Zhan Quanqiu
The 70% of production.In recent years, with the raising of antibiotic yield, domestic each fermentation pharmacy enterprise year waste residue yield by
Year improves, if a large amount of pharmacy waste residue cannot get appropriate disposition and will will cause serious environmental threat, but they are simultaneously
Be it is a kind of potentially can reuse resource, Chinese Ministry of Environmental Protection in 2012 formulates " pharmaceuticals industry pollution prevention technique policy " and encourages research, opens
Hair promotes " reutilization technology, innoxious process for treating, comprehensive utilization technique of the fermentation residue in production technology, hazardous waste
Comprehensive utilization technique in factory ", thus the disposition of antibiotic waste residue has great importance.
Antibiotic waste residue production quantity is big, belongs to danger wastes.US Gov Env Protection Agency (USEPA) and European Union at present
" European pharmacy industry waste register " mainly solve the processing of penicillin waste residue in a manner of burning, landfill and production organic fertilizer
Problem；It is usually to be used to production organic fertilizer in India, Mexico's penicillin waste residue.At home, waste residue harmless resource utilization
Processing technique mainly includes compost and biofermentation, burning, anaerobic digestion methane production, raw material extracts or the paths such as preparation.At present
Various resource reutilization modes are not perfect, it is difficult to which digestion reaches harmless treatment completely, still relies primarily on traditional burning
Or landfill disposal minimizing.However, burning or burying method are at high cost, and pollute environment, and cause a large amount of wastes of resource, detest
Therefore for antibiotic waste residue, waste residue resource integrated application water is widened there are incomplete, drug resistance problems of degrading in oxygen digestion
It puts down extremely urgent.It is produced as drug and uses big country, China should more pay attention to the processing of antibiotic waste residue, gradually accelerate to useless
The research of the innoxious advanced treating of antibiotic in slag, so that the antibiotic waste residue of flood tide during realizing innoxious, is formed
The synergistic effect of resource utilization.
Antibiotic fermentation waste residue is that antibiotics generated bacterium is inoculated in solid or fluid nutrient medium made of agricultural and sideline product
On through multistage purebred culture, then pass through a series of physical, chemical treating process, will antibiotic element extract after the solid that leaves
Object obtains solid dried object through dehydration.Its main component includes: mycelia, remaining culture medium, antibiotics generated bacterium fermentation
The metabolin of process, the degradation product of culture medium and unknown growth factor.It is high that antibiotic fermentation produces protein content in waste residue
Up to 20-60%, and minerals rich in and microelement, if these protein, minerals and microelement can effective benefits
With, it will form good ecological benefits.
Amino acid Water soluble fertilizer is prepared through processing using innoxious biological medicine industry fermentation residue the present invention relates to a kind of
The method of product.Specifically, after by carrying out environmental protection treatment to antibiotic waste residue, resource product --- amino sour water is formed
The exploitation of molten fertilizer realizes that resource turns waste into wealth, with more inexpensive, more effective processing antibiotic dangerous waste waste residue, to improve money
Source level of comprehensive utilization, this will not only become the following new business growth point of dangerous waste treatment industry, gets a profit considerable, present good
Economic effect；Meanwhile full-range technique is opened for realizing that the industry great development of ecology, minimizing, recycling will play
Good Social Ecology effect can form benign industry development chain, can both reduce the waste residue pair of pharmaceutical industry production process
The pollution of ecological environment, and ensure the safety of human being's production environment, promote pharmaceutical industry to develop in a healthy way, the ecosystem is put down
Weighing apparatus, Environmental security, human health and social sustainable development all have important meaning.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of energy efficient degradation is useless
Antibiotic residue in slag simultaneously, a large amount of protein in waste residue is hydrolyzed, are obtained containing various amino acid and middle microelement
Nutriment, for the active principle for preparing raw material, making full use of in waste residue of the water-soluble fertilizer product of amino acid, realize become give up into
The precious method that amino acid Water soluble fertilizer is prepared using biological medicine fermentation residue.
The present invention is that the technology of amino acid Water soluble fertilizer is obtained by the protein in degradation waste residue.
Operation process of the invention mainly includes: preprocessing process, hydrolytic process are separated by filtration or dry.This
A little main process are easy to operate, highly-safe, nontoxic.The production technology of the water-soluble fertilizer product of the amino acid, meets green association
Sustainable development theory is adjusted, the energy-saving and environment-friendly requirement that country advocates is met.
The purpose of the present invention can be achieved through the following technical solutions:
A method of amino acid Water soluble fertilizer is prepared using antibiotic fermentation waste residue, comprising the following steps:
(1) preprocessing process: degradation agent being added into antibiotic fermentation residue, reacted to obtain innoxious waste residue
Slurries；
(2) hydrolytic process: being added the rush hydrolytic reagent of doses, reaction be hydrolyzed in waste residue slurries after to processing, after
After being separated by filtration, the amino acid Water soluble fertilizer of resource utilization can be obtained.
Further, degradation agent described in step (1) is in chemical oxidation reagent, biodegradation agent or biochemicals
One or more, the chemical oxidation reagent are sulfate, perchloric acid, hypochlorous acid, ferrous oxide, hydrogen peroxide, phosphoric acid, nitre
Acid, sulfuric acid or potassium, sodium, calcium or barium oxide or one or more of hydroxide or peroxide, the biology
Degradation agent is the strain or flora that specific degradation is known as to antibiosis, and the biochemicals is enzyme material or other albumen
Matter.
Further, the mass ratio of degradation agent described in step (1) and waste residue is 1:(1-1000)；Preferably 1:(1-
100), degradation reaction temperature is 25-150 DEG C, reaction pressure 0-0.5Mpa, reaction time 0.5h-72h.When degradation agent is
When chemical oxidation reagent, reaction time preferably 1~3h, more preferable 2h；When degradation agent is biodegradation agent, the reaction time is preferred
30~40h, more preferable 34-37h；When degradation agent is biochemicals, reaction time preferably 10~30h, more preferable 22-26h.
Further, rush hydrolytic reagent described in step (2) is acidic hydrolysis agent, basic hydrolysis agent or salt compounds
It is one or more, specifically include phosphoric acid, nitric acid, sulfuric acid, potassium, sodium, calcium or barium oxide or hydroxide, copper sulphate, sulphur
One kind of sour zinc, copper nitrate, zinc nitrate, sulfuric acid boron, magnesium nitrate, magnesium sulfate, molybdenum trisulfate, calcium nitrate, ferrous sulfate or ferric sulfate
Or it is several；Or ethylenediamine tetra-acetic acid magnesium sodium (EDTA-Mg), cupric ethylene diamine tetraacetate sodium (EDTA-Cu), ethylenediamine tetra-acetic acid zinc
The one or more of the water-soluble metallo-chelates such as sodium (EDTA-Zn).
Further, hydrolysis described in step (2), solution final pH is between 3-9 after reaction.
Further, the condition of hydrolysis described in step (2) are as follows: reaction temperature is 25-150 DEG C, reacts absolute pressure
Power is 0-0.5Mpa, reaction time 0.1-10h.
Further, the mass ratio of rush hydrolytic reagent and waste residue described in step (2) is 1:(1-250), preferably 1:(1-
100)。
Compared with prior art, the invention has the following advantages that
(1) present invention provide a kind of energy conservation and environmental protection, efficiently, the antibiotic waste residue resource of low cost using path, not only
Residual antibiotic in waste residue can will be rapidly removed, while the progress of the waste residue after harmless treatment resource utilization can be obtained attached
The value added water-soluble fertilizer product of high amino acid.
(2) the invention belongs to the product development technique of the resource utilization of waste residue after harmless treatment, waste residue may be implemented
Turn waste into wealth, there is certain economic benefit；Reduce harm of the waste residue to the mankind and ecological environment simultaneously, reduce secondary pollution and
The environmental risks such as drug resistance have good ecological benefits；
(3) present invention can also improve china natural resources synthesization using level, promote national green environmental protection sustainable development,
Human ecology safety is protected, there is preferable social benefit.
Specific embodiment
It elaborates below to the embodiment of the present invention, the present embodiment carries out under the premise of the technical scheme of the present invention
Implement, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
Penicillin Content is the waste residue of 3800ppm.50g water is added into 100g waste residue, forms slurries, then to containing mould
Be added calcium oxide 4g in the fermentation residue of plain class antibiotic, 120 DEG C, react 4 hours under 0.15Mpa after, then to innoxious place
CuSO is added in the waste residue slurries of reason4The ammonia of resource utilization can be obtained after hydrolysis a period of time after being separated by filtration in 5g
The molten fertile liquid form product of base sour water.Penicillin noresidue in water-soluble fertilizer product is detected, and free aminoacid content is greater than 100g/L,
Microelement Cu content is greater than 20g/L, product pH=7.8.
Embodiment 2
Griseofulvin content is the waste residue of 4812ppm.100g water is added into 100g waste residue, forms slurries, then to containing
It is added sodium oxide molybdena 4g in fermentation residue, 100 DEG C, innoxious waste residue is reacted after 2h to obtain under normal pressure, then to the useless of harmless treatment
ZnSO is added in dreg slurry410g, MoSO4After 10g, hydrolysis stirring 4h, after being separated by filtration, the ammonia of resource utilization can be obtained
The molten fertile liquid form product of base sour water.Griseofulvin noresidue in water-soluble fertilizer product is detected, and free aminoacid content is greater than 100g/
L, trace elements zn and Mo total amount are greater than 20g/L, product pH=9.
Embodiment 3
Cephalosporin content is the waste residue of 5000ppm.10g water is added into 100g waste residue, forms slurries, then Xiang Hanfa
Sulfuric acid 10g is added in ferment waste residue, degrade agent hydrogen peroxide 5g, 10g catalyst Fe SO4·7H2O, after reacting 4h under 80 DEG C, normal pressure
Innoxious waste residue is obtained, phosphatase 11 0g is then added into the waste residue slurries of harmless treatment and is separated by filtration after 2h is stirred in hydrolysis
Afterwards, the amino acid Water soluble fertilizer liquid and solid product of resource utilization are respectively obtained.Through detecting cephalosporin in water-soluble fertilizer product
Noresidue, and free aminoacid content is greater than 100g/L, microelement Fe total amount is greater than 20g/L, product pH=3.
Embodiment 4
Terramycin content is the waste residue of 4500ppm.Biological enzyme agent 20g is added into 1000g waste residue, under 30 DEG C, normal pressure
React 18h；Then calcium oxide 40g and 400g water is added, reaction is hydrolyzed, after separation is dry, obtaining liquid hold-up is
78% amino acid Water soluble fertilizer product 1039.4g, the residual quantity for being detected product terramycin are less than 1ppm, free aminoacid content
Greater than 100g/L, moderate-element Ca total amount is greater than 100g/L, product pH=8.
Embodiment 5
Erythromycin content is the waste residue of 3700ppm.1000g water is added into 2500g waste residue, forms slurries；Backward slurry
Sodium oxide molybdena 50g is added in liquid, reacts 6h under being 0.5Mpa in 150 DEG C, pressure；5g FeSO is then added4With 5g MoSO4, 40
It after being hydrolyzed under the conditions of DEG C, is separated and is dried, obtain the product 3204.8g that liquid hold-up is 73%, through detection erythromycin
Residual quantity is less than 1ppm, and free aminoacid content is greater than 100g/L, and microelement Fe and Mo total amount is greater than 20g/L, product pH
=7.2.
Embodiment 6
Penicillin Content is the waste residue of 4780ppm.400g water is added into 2000g waste residue, forms slurries；Backward slurries
Middle addition chemical oxidizing agent sodium peroxydisulfate 2g reacts 0.1h under being 0.5Mpa in 150 DEG C, pressure；Then hydrolytic reagent Ca is added
(OH)220g reacts 10h at 80 DEG C, after separation, obtains the amino acid Water soluble fertilizer product that liquid hold-up is 82%
2097.5g, the residual quantity for being detected penicillin is less than 1ppm, and free aminoacid content is greater than 100g/L, and moderate-element Ca is total
Amount is greater than 100g/L, product pH=6.
Embodiment 7
Cephalosporin content is the waste residue of 3800ppm.50g water is added into 100g waste residue and forms slurries；Backward slurries
Middle addition 0.2g catalyst CoCl2, oxidant hydrogen peroxide 1g reacts 0.1h under 80 DEG C, normal pressure；Add FeSO4Carry out water
Solution reacts 6h at 80 DEG C, and the product 115g that liquid hold-up is 76% is obtained after separation, and the residual quantity through detecting cephalosporin is small
In 1ppm, and free aminoacid content is greater than 100g/L, and microelement Fe total amount is greater than 20g/L, product pH=6.
Embodiment 8
Penicillin Content is the waste residue of 6000ppm.1000g water is added into 750g waste residue, forms slurries；Backward slurries
Middle addition oxidant caustic soda 10g reacts 4h in 120 DEG C, reaction pressure 0.5Mpa；Then H is added2SO45g, at 30 DEG C
Under, 10h to be reacted, after separation, obtains the product 1402g that liquid hold-up is 75%, the residual quantity for being detected penicillin is less than 1ppm,
And free aminoacid content is greater than 100g/L, moderate-element Ca total amount is greater than 20g/L, product pH=3.
Embodiment 9
Penicillin Content is the waste residue of 4780ppm.20g water is added into 200g waste residue, forms slurries；Backward slurries in
5g potassium hydroxide is added, reacts 0.5h at 105 DEG C, 0.05MPa；Add Ca (NO3)22h is reacted at 50 DEG C, through separating,
The product 182.6g that liquid hold-up is 92% is obtained, the residual quantity for being detected penicillin is less than 1ppm, and free aminoacid content is big
In 100g/L, moderate-element Ca content is greater than 20g/L, product pH=7.8.
Embodiment 10
Terramycin content is the waste residue of 3812ppm.1000g water is added into 150g waste residue, forms slurries；Backward slurries
Middle addition 15g catalyst Fe Cl2, oxidant perchloric acid 100g reacts 0.6h under 60 DEG C, normal pressure；Add CuSO410g and
ZnSO410g hydrolyzes 4h at 80 DEG C, after separation, obtains the product 1083.7g that liquid hold-up is 81%, is detected native penicillin
Residual quantity be less than 1ppm, and free aminoacid content be greater than 100g/L, microelement Cu and Zn total amount be greater than 20g/L, product
PH=6.5.
Embodiment 11
Penicillin Content is the waste residue of 5800ppm.20g water is added into 100g waste residue, forms slurries；Backward slurries in
100g nitric acid is added, reacts 10h at 30 DEG C, 0.05MPa；It adds 100g magnesium nitrate and reacts 20d at 30 DEG C, through separating,
The product that liquid hold-up is 92% is obtained, the residual quantity for being detected penicillin is less than 1ppm, and free aminoacid content is greater than 100g/
L, moderate-element Mg content are greater than 20g/L, product pH=3.8.
Embodiment 12
Penicillin Content is the waste residue of 3780ppm.20g water is added into 100g waste residue, forms slurries；Backward slurries in
1g nitric acid is added, reacts 0.1h at 150 DEG C, 0.5MPa；It adds 1g ferric sulfate and reacts 0.1h at 150 DEG C, separated, obtained
The product for being 90% to liquid hold-up, the residual quantity for being detected penicillin is less than 1ppm, and free aminoacid content is greater than 100g/L,
Moderate-element Fe content is greater than 20g/L, product pH=5.9.
Embodiment 13
Penicillin Content is the waste residue of 3780ppm.1g biodegradation agent, specially commercially available gemma are added into 100g waste residue
Bacillus adds cupric ethylene diamine tetraacetate sodium (EDTA-Cu) 5g, ethylenediamine tetra-acetic acid zinc sodium (EDTA- after 25 DEG C, 36 hours
Zn after being separated by filtration, the amino acid Water soluble fertilizer liquid form product of resource utilization is can be obtained in) 5g.Through detecting water-soluble fertilizer product
Middle penicillin noresidue, and free aminoacid content is greater than 100g/L, microelement Cu/Zn content and greater than 20g/L, product pH
=7.8.
Embodiment 14
Cephalosporin content is the waste residue of 2500ppm.1g biochemicals, the specially road Dong Henghua are added into 100g waste residue
The alkaline proteolytic enzyme substance of companies market adds ethylenediamine tetra-acetic acid zinc sodium (EDTA- after reacting 4h at 55 DEG C
Zn after being separated by filtration, the amino acid Water soluble fertilizer liquid form product of resource utilization is can be obtained in) 10g.Through detecting water-soluble fertilizer product
Middle penicillin noresidue, and free aminoacid content is greater than 100g/L, trace elements zn content is greater than 20g/L, product pH=8.
Embodiment 15
Penicillin Content is the waste residue of 3780ppm.0.1g biodegradation agent, specially commercially available bud are added into 100g waste residue
Spore bacillus adds ethylenediamine tetra-acetic acid magnesium sodium (EDTA-Mg) 10g, after being separated by filtration, i.e., after 32 DEG C, processing in 12 hours
The amino acid Water soluble fertilizer liquid form product of resource utilization can be obtained.Penicillin noresidue in water-soluble fertilizer product is detected, and free
Amino acid content is greater than 100g/L, and moderate-element Mg content is greater than 30g/L, product pH=7.2.
Embodiment 16
Cephalosporin content is the waste residue of 2500ppm.0.2g biochemicals is added into 100g waste residue, specially the permanent China in east
The alkaline proteolytic enzyme substance of road companies market after reacting for 24 hours at 50 DEG C, adds ethylenediamine tetra-acetic acid zinc sodium
(EDTA-Zn) after being separated by filtration, the amino acid Water soluble fertilizer liquid form product of resource utilization is can be obtained in 7g.It is water-soluble through detecting
Penicillin noresidue in fertilizer product, and free aminoacid content is greater than 100g/L, trace elements zn content is greater than 20g/L, product
PH=7.5.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (7)
1. a kind of method for preparing amino acid Water soluble fertilizer using antibiotic fermentation waste residue, which comprises the following steps:
(1) preprocessing process: degradation agent being added into antibiotic waste residue to be processed, reacted to obtain innoxious waste residue slurry
Liquid；
(2) it hydrolytic process: is added into waste residue slurries and promotees hydrolytic reagent, reaction is hydrolyzed, after being separated by filtration, can be obtained
The amino acid Water soluble fertilizer of resource utilization.
2. a kind of method for preparing amino acid Water soluble fertilizer using antibiotic fermentation waste residue according to claim 1, feature
It is, degradation agent described in step (1) is one or more of chemical oxidation reagent, biodegradation agent or biochemicals,
The chemical oxidation reagent be sulfate, perchloric acid, hypochlorous acid, ferrous oxide, hydrogen peroxide, phosphoric acid, nitric acid, sulfuric acid, or
Potassium, sodium, calcium or barium oxide or one or more of hydroxide or peroxide, the biodegradation agent is confrontation
The raw strain or flora for being known as specific degradation, the biochemicals are enzyme material or other protein.
3. a kind of method for preparing amino acid Water soluble fertilizer using antibiotic fermentation waste residue according to claim 1, feature
It is, the mass ratio of degradation agent described in step (1) and waste residue to be processed is 1:(1-1000)；Degradation reaction temperature is 25-
150 DEG C, reaction pressure is 0-0.5 Mpa, reaction time 0.5h-72h.
4. a kind of method for preparing amino acid Water soluble fertilizer using antibiotic fermentation waste residue according to claim 1, feature
It is, rush hydrolytic reagent described in step (2) is one kind or more of acidic hydrolysis agent, basic hydrolysis agent or salt compounds
Kind, specifically include phosphoric acid, nitric acid, sulfuric acid, potassium, sodium, calcium or barium oxide or hydroxide, copper sulphate, zinc sulfate, nitric acid
The one or more of copper, zinc nitrate, sulfuric acid boron, magnesium nitrate, magnesium sulfate, molybdenum trisulfate, calcium nitrate, ferrous sulfate or ferric sulfate, or
Person's ethylenediamine tetra-acetic acid magnesium sodium (EDTA-Mg), cupric ethylene diamine tetraacetate sodium (EDTA-Cu), ethylenediamine tetra-acetic acid zinc sodium (EDTA-
The one or more of water-soluble metallo-chelate such as Zn).
5. a kind of method for preparing amino acid Water soluble fertilizer using antibiotic fermentation waste residue according to claim 1, feature
It is, hydrolysis described in step (2), solution final pH is between 3-9 after reaction.
6. a kind of method for preparing amino acid Water soluble fertilizer using antibiotic fermentation waste residue according to claim 1, feature
It is, the condition of hydrolysis described in step (2) are as follows: reaction temperature is 25-150 DEG C, and reaction pressure is 0-0.5 Mpa, instead
It is 0.1-10h between seasonable.
7. a kind of method for preparing amino acid Water soluble fertilizer using antibiotic fermentation waste residue according to claim 1, feature
It is, the mass ratio of rush hydrolytic reagent and waste residue to be processed described in step (2) is 1:(1-250).
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Cited By (3)
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| CN112409033A (en) * | 2020-11-29 | 2021-02-26 | 上海化工研究院有限公司 | Method for preparing fertilizer product by recycling tetracyclic antibiotic fermentation waste residues |
| CN112934932A (en) * | 2021-04-14 | 2021-06-11 | 同济大学 | Harmless treatment method for antibiotic mushroom dregs |
| CN114380647A (en) * | 2021-12-09 | 2022-04-22 | 上海化工研究院有限公司 | Method for preparing organic fertilizer by materializing traditional Chinese medicine residues |
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