CN111995061A - Composite biological flocculant and preparation method thereof - Google Patents
Composite biological flocculant and preparation method thereof Download PDFInfo
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- CN111995061A CN111995061A CN202010644752.7A CN202010644752A CN111995061A CN 111995061 A CN111995061 A CN 111995061A CN 202010644752 A CN202010644752 A CN 202010644752A CN 111995061 A CN111995061 A CN 111995061A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
- C12N1/20—Bacteria; Culture media therefor
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Abstract
The invention provides a composite biological flocculant and a preparation method thereof. The magnetic substance is introduced into the microbial flocculant and then the microbial flocculant and the modified bentonite are compounded to prepare the composite biological flocculant, so that the defect that the microbial flocculant is difficult to separate is overcome, and meanwhile, the microbial flocculant and the inorganic flocculant are matched for use, so that the flocculation efficiency can be improved, the addition amount is reduced, and the secondary pollution is reduced.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a composite biological flocculant and a preparation method thereof.
Background
The flocculation technology is a method for improving water quality treatment efficiency which is commonly used at home and abroad, can effectively remove pollutants and some soluble impurities in high-concentration organic wastewater, and the microbial flocculant is more and more applied to wastewater treatment engineering instead of inorganic and organic synthetic polymeric flocculants due to the advantages of high efficiency, easy degradation and no secondary pollution. The adsorption and ion exchange deamination and denitrification technology draws more and more attention to people due to the advantages of simple process, convenient operation and stable operation. But the single use of the microbial flocculant has the disadvantages of long preparation period and difficult separation of the flocculant.
Disclosure of Invention
Aiming at the defects of long preparation period and difficult separation of the existing microbial flocculant, the invention provides the composite biological flocculant and the preparation method thereof.
The strain used in the invention is a flocculogenic strain-KlebsiellaKlebsiellaJ1, accession no: CGMCC NO. 6243.
The invention is realized by the following technical scheme:
a composite biological flocculant is prepared from the following components: microbial flocculant dry powder, ferric chloride, ferrous sulfate and magnesium oxide modified bentonite.
The preparation method of the composite biological flocculant comprises the following steps:
(1) inoculating one loopful of a flocculent-producing strain from a strain culture medium into 100mL of a liquid fermentation culture medium, and culturing for 24h in a shaking table at 30 ℃ and a rotating speed of 120r/min to obtain a seed solution;
(2) inoculating the cultured seed liquid into the liquid fermentation culture medium again according to 7% of the volume of the liquid fermentation culture medium, and fermenting for 21-24 h in a shaking table at 30 ℃ and a rotating speed of 120r/min to ensure that the thalli secrete the flocculating agent;
(3) centrifuging the liquid culture solution secreting the flocculant at 1000r/min to remove thalli, and freeze-drying the supernatant at-80 ℃ to prepare microbial flocculant dry powder;
(4) dissolving ferric chloride and ferrous sulfate in ultrapure water according to the ratio of ferric chloride to ferrous sulfate to ultrapure water of (3-5) to (2-4) 50 to obtain a mixed solution, quickly adding ammonia water with the mass of 10% of the ultrapure water into the mixed solution, heating to 90 ℃, continuously stirring for 30min, cooling to room temperature, filtering, washing and drying, and collecting black precipitate to obtain magnetic particles;
(5) ultrasonically dispersing magnetic particles in ultrapure water according to a solid-liquid ratio of 1:1000, adding dry powder of a microbial flocculant and sodium persulfate, stirring for 5 hours in an ice bath, finally separating precipitates, washing and drying to obtain the magnetic microbial flocculant;
(6) mixing the magnesium oxide modified bentonite and the magnetic microbial flocculant according to the mass ratio of 2:1 to obtain the composite biological flocculant.
The microbial flocculation prepared by the invention is a protein type microbial flocculant which contains hydroxyl, carboxyl and sulfur-containing groups and has good adsorption effect on various heavy metals, ammonia nitrogen and solid particles; the magnetic substance is introduced into the microbial flocculant and then the microbial flocculant and the modified bentonite are compounded to prepare the composite biological flocculant, so that the defect that the microbial flocculant is difficult to separate is overcome, and meanwhile, the microbial flocculant and the inorganic flocculant are matched for use, so that the flocculation efficiency can be improved, the addition amount is reduced, and the secondary pollution is reduced. The bentonite modified by magnesium oxide has good adsorption performance on ammonia nitrogen, and the surface porosity of the modified bentonite is increased, so that the adsorption performance of the bentonite is improved, and the bentonite and a microbial flocculant can adsorb each other after acting together to flocculate wastewater, thereby improving the separation efficiency of the modified bentonite.
As a further improvement of the invention, the mass ratio of the magnetic particles, the microbial flocculant dry powder and the sodium persulfate used in the step (5) is 1:1: 0.1.
The use level of the magnetic particles influences the separation effect of the flocculant, the larger the use level is, the higher the later separation efficiency is, but the adsorption effect between the modified bentonite and the microbial flocculant is reduced, and the two combined separations are not easy to realize.
As a further improvement of the invention, the formula of the strain culture medium is as follows: 10g/L of peptone, 0.1g/L of NaCl0, 5g/L of yeast extract, 7.0-7.2 of pH and 20min of sterilization at 121 ℃.
As a further improvement of the invention, the formula of the liquid fermentation medium is as follows: glucose 10g/L, yeast extract 0.5g/L, K2HPO45g/L，NaCl 0.1g/L，KH2PO42g/L, urea 0.5g/L, MgSO4•7H2O0.2 g/L, pH 7.2-7.5, L12 ℃ for 30 min.
As a further improvement of the invention, the preparation method of the magnesium oxide modified bentonite comprises the following steps:
rinsing bentonite with distilled water, drying at 105 ℃, then completely mixing the bentonite dried to constant weight with magnesium oxide according to the mass ratio of (3-4) to 1, and roasting in a muffle furnace at 400 ℃ for 4h to obtain the modified bentonite.
The invention has the beneficial effects that:
according to the invention, the magnetic material is introduced into the microbial flocculant, and then the microbial flocculant and the inorganic flocculant are mixed to prepare the composite biological flocculant, so that the use amount of the microbial flocculant is effectively reduced, the cost is reduced, secondary pollution is avoided, and the separation efficiency of the flocculant is improved.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A composite biological flocculant is prepared from the following components: microbial flocculant dry powder, ferric chloride, ferrous sulfate and magnesium oxide modified bentonite.
The preparation method of the composite biological flocculant comprises the following steps:
(1) inoculating one loopful of a flocculent-producing strain from a strain culture medium into 100mL of a liquid fermentation culture medium, and culturing for 24h in a shaking table at 30 ℃ and a rotating speed of 120r/min to obtain a seed solution;
(2) inoculating the cultured seed liquid into the liquid fermentation culture medium again according to 7% of the volume of the liquid fermentation culture medium, and fermenting for 21h in a shaking table with the rotation speed of 120r/min at 30 ℃ to ensure that the thalli secrete the flocculating agent;
(3) centrifuging the liquid culture solution secreting the flocculant at 1000r/min to remove thalli, and freeze-drying the supernatant at-80 ℃ to prepare microbial flocculant dry powder;
(4) dissolving ferric chloride and ferrous sulfate in ultrapure water according to the ratio of ferric chloride to ferrous sulfate to ultrapure water =3:2:50 to obtain a mixed solution, quickly adding ammonia water with the mass of 10% of the ultrapure water into the mixed solution, heating to 90 ℃, continuously stirring for 30min, cooling to room temperature, filtering, washing, drying, and collecting black precipitate to obtain magnetic particles;
(5) ultrasonically dispersing magnetic particles into ultrapure water according to a solid-liquid ratio of 1:1000, adding microbial flocculant dry powder and sodium persulfate according to a mass ratio of 1:1:0.1 of the magnetic particles, the microbial flocculant dry powder and the sodium persulfate, stirring for 5 hours in an ice bath, finally separating and precipitating, washing and drying to obtain a magnetic microbial flocculant;
(6) mixing the magnesium oxide modified bentonite and the magnetic microbial flocculant according to the mass ratio of 2:1 to obtain the composite biological flocculant.
The formula of the strain culture medium is as follows: 10g/L of peptone, 0.1g/L of NaCl0, 5g/L of yeast extract, 7.0 pH, and 20min of sterilization at 121 ℃.
The formula of the liquid fermentation medium is as follows: glucose 10g/L, yeast extract 0.5g/L, K2HPO45g/L，NaCl 0.1g/L，KH2PO42g/L, urea 0.5g/L, MgSO4•7H2O0.2 g/L, pH 7.2, L12 ℃ for 30 min.
The preparation method of the magnesium oxide modified bentonite comprises the following steps:
rinsing bentonite with distilled water, drying at 105 ℃, completely mixing the bentonite dried to constant weight with magnesium oxide according to the mass ratio of 3:1, and roasting in a muffle furnace at 400 ℃ for 4h to obtain the modified bentonite.
Example 2
A composite biological flocculant is prepared from the following components: microbial flocculant dry powder, ferric chloride, ferrous sulfate and magnesium oxide modified bentonite.
The preparation method of the composite biological flocculant comprises the following steps:
(1) inoculating one loopful of a flocculent-producing strain from a strain culture medium into 100mL of a liquid fermentation culture medium, and culturing for 24h in a shaking table at 30 ℃ and a rotating speed of 120r/min to obtain a seed solution;
(2) inoculating the cultured seed liquid into the liquid fermentation culture medium again according to 7% of the volume of the liquid fermentation culture medium, and fermenting for 24h in a shaking table with the rotation speed of 120r/min at 30 ℃ so that the thalli secrete the flocculating agent;
(3) centrifuging the liquid culture solution secreting the flocculant at 1000r/min to remove thalli, and freeze-drying the supernatant at-80 ℃ to prepare microbial flocculant dry powder;
(4) dissolving ferric chloride and ferrous sulfate in ultrapure water according to the ratio of ferric chloride to ferrous sulfate to ultrapure water =5:4:50 to obtain a mixed solution, quickly adding ammonia water with the mass of 10% of the ultrapure water into the mixed solution, heating to 90 ℃, continuously stirring for 30min, cooling to room temperature, filtering, washing, drying, and collecting black precipitate to obtain magnetic particles;
(5) ultrasonically dispersing magnetic particles into ultrapure water according to a solid-liquid ratio of 1:1000, adding microbial flocculant dry powder and sodium persulfate according to a mass ratio of 1:1:0.1 of the magnetic particles, the microbial flocculant dry powder and the sodium persulfate, stirring for 5 hours in an ice bath, finally separating and precipitating, washing and drying to obtain a magnetic microbial flocculant;
(6) mixing the magnesium oxide modified bentonite and the magnetic microbial flocculant according to the mass ratio of 2:1 to obtain the composite biological flocculant.
The formula of the strain culture medium is as follows: 10g/L of peptone, 0.1g/L of NaCl0, 5g/L of yeast extract, 7.2 of pH and 20min of sterilization at 121 ℃.
The formula of the liquid fermentation medium is as follows: glucose 10g/L, yeast extract 0.5g/L, K2HPO45g/L，NaCl 0.1g/L，KH2PO42g/L, urea 0.5g/L, MgSO4•7H2O0.2 g/L, pH 7.5, L12 ℃ for 30 min.
The preparation method of the magnesium oxide modified bentonite comprises the following steps:
rinsing bentonite with distilled water, drying at 105 ℃, completely mixing the bentonite dried to constant weight with magnesium oxide according to the mass ratio of 4:1, and roasting in a muffle furnace at 400 ℃ for 4h to obtain the modified bentonite.
Example 3
A composite biological flocculant is prepared from the following components: microbial flocculant dry powder, ferric chloride, ferrous sulfate and magnesium oxide modified bentonite.
The preparation method of the composite biological flocculant comprises the following steps:
(1) inoculating one loopful of a flocculent-producing strain from a strain culture medium into 100mL of a liquid fermentation culture medium, and culturing for 24h in a shaking table at 30 ℃ and a rotating speed of 120r/min to obtain a seed solution;
(2) inoculating the cultured seed liquid into the liquid fermentation culture medium again according to 7% of the volume of the liquid fermentation culture medium, and fermenting for 21-24 h in a shaking table at 30 ℃ and a rotating speed of 120r/min to ensure that the thalli secrete the flocculating agent;
(3) centrifuging the liquid culture solution secreting the flocculant at 1000r/min to remove thalli, and freeze-drying the supernatant at-80 ℃ to prepare microbial flocculant dry powder;
(4) dissolving ferric chloride and ferrous sulfate in ultrapure water according to the ratio of ferric chloride to ferrous sulfate to ultrapure water =4:3:50 to obtain a mixed solution, quickly adding ammonia water with the mass of 10% of the ultrapure water into the mixed solution, heating to 90 ℃, continuously stirring for 30min, cooling to room temperature, filtering, washing, drying, and collecting black precipitate to obtain magnetic particles;
(5) ultrasonically dispersing magnetic particles into ultrapure water according to a solid-liquid ratio of 1:1000, adding microbial flocculant dry powder and sodium persulfate according to a mass ratio of 1:1:0.1 of the magnetic particles, the microbial flocculant dry powder and the sodium persulfate, stirring for 5 hours in an ice bath, finally separating and precipitating, washing and drying to obtain a magnetic microbial flocculant;
(6) mixing the magnesium oxide modified bentonite and the magnetic microbial flocculant according to the mass ratio of 2:1 to obtain the composite biological flocculant.
The formula of the strain culture medium is as follows: 10g/L of peptone, 0.1g/L of NaCl0, 5g/L of yeast extract, 7.1 pH, and 20min of sterilization at 121 ℃.
The formula of the liquid fermentation medium is as follows: glucose 10g/L, yeast extract 0.5g/L, K2HPO45g/L，NaCl 0.1g/L，KH2PO42g/L, urea 0.5g/L, MgSO4•7H2O0.2 g/L, pH 7.1, L12 ℃ for 30 min.
The preparation method of the magnesium oxide modified bentonite comprises the following steps:
rinsing bentonite with distilled water, drying at 105 ℃, completely mixing the bentonite dried to constant weight with magnesium oxide according to the mass ratio of 3.2:1, and roasting in a muffle furnace at 400 ℃ for 4h to obtain the modified bentonite.
Application example
Taking a wastewater sample of a certain pig farm, measuring to obtain that the initial ammonia nitrogen concentration and COD of the wastewater sample are respectively 800mg/L and 1100mg/L, dividing the wastewater sample into three groups, wherein each group is 100mL of water sample, 10g of the flocculating agent prepared in the embodiments 1-3 is added into each group, stirring for 30min, standing for 30min, and measuring the ammonia nitrogen concentration and COD, wherein the results are shown in Table 1.
TABLE 1 data table of the concentrations of the respective substances after the treatment of each group (unit: mg/L)
As can be seen from Table 1, the flocculants prepared in the examples of the present invention have excellent flocculation effects.
The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the scope of the present invention is defined by the claims. Various modifications and equivalents may be made thereto by those skilled in the art within the spirit and scope of the present invention, and such modifications and equivalents should be considered as falling within the scope of the present invention.
Claims (6)
1. The composite biological flocculant is characterized by being prepared from the following components: microbial flocculant dry powder, ferric chloride, ferrous sulfate and magnesium oxide modified bentonite.
2. The preparation method of the composite bioflocculant according to claim 1, characterized by comprising the following steps:
(1) inoculating one loopful of a flocculent-producing strain from a strain culture medium into 100mL of a liquid fermentation culture medium, and culturing for 24h in a shaking table at 30 ℃ and a rotating speed of 120r/min to obtain a seed solution;
(2) inoculating the cultured seed liquid into the liquid fermentation culture medium again according to 7% of the volume of the liquid fermentation culture medium, and fermenting for 21-24 h in a shaking table at 30 ℃ and a rotating speed of 120r/min to ensure that the thalli secrete the flocculating agent;
(3) centrifuging the liquid culture solution secreting the flocculant at 1000r/min to remove thalli, and freeze-drying the supernatant at-80 ℃ to prepare microbial flocculant dry powder;
(4) dissolving ferric chloride and ferrous sulfate in ultrapure water according to the ratio of ferric chloride to ferrous sulfate to ultrapure water of (3-5) to (2-4) 50 to obtain a mixed solution, quickly adding ammonia water with the mass of 10% of the ultrapure water into the mixed solution, heating to 90 ℃, continuously stirring for 30min, cooling to room temperature, filtering, washing and drying, and collecting black precipitate to obtain magnetic particles;
(5) ultrasonically dispersing magnetic particles in ultrapure water according to a solid-liquid ratio of 1:1000, adding dry powder of a microbial flocculant and sodium persulfate, stirring for 5 hours in an ice bath, finally separating precipitates, washing and drying to obtain the magnetic microbial flocculant;
(6) mixing the magnesium oxide modified bentonite and the magnetic microbial flocculant according to the mass ratio of 2:1 to obtain the composite biological flocculant.
3. The method for preparing the composite bioflocculant according to claim 2, wherein: the mass ratio of the magnetic particles, the microbial flocculant dry powder and the sodium persulfate used in the step (5) is 1:1: 0.1.
4. The method for preparing the composite bioflocculant according to claim 2, wherein: the formula of the strain culture medium is as follows: 10g/L of peptone, 0.1g/L of NaCl0, 5g/L of yeast extract, 7.0-7.2 of pH and 20min of sterilization at 121 ℃.
5. The method for preparing the composite bioflocculant according to claim 2, wherein: the formula of the liquid fermentation medium is as follows: glucose 10g/L, yeast extract 0.5g/L, K2HPO45g/L，NaCl 0.1g/L，KH2PO42g/L, urea 0.5g/L, MgSO4•7H2O0.2 g/L, pH 7.2-7.5, L12 ℃ for 30 min.
6. The method for preparing the composite bioflocculant according to claim 2, wherein: the preparation method of the magnesium oxide modified bentonite comprises the following steps:
rinsing bentonite with distilled water, drying at 105 ℃, then completely mixing the bentonite dried to constant weight with magnesium oxide according to the mass ratio of (3-4) to 1, and roasting in a muffle furnace at 400 ℃ for 4h to obtain the modified bentonite.
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| CN115716671A (en) * | 2022-12-08 | 2023-02-28 | 山东珺宜环保科技有限公司 | Composite microbial flocculant and preparation method and application thereof |
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| CN115716671A (en) * | 2022-12-08 | 2023-02-28 | 山东珺宜环保科技有限公司 | Composite microbial flocculant and preparation method and application thereof |
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