CN114075013A - Treatment process and system for wastewater generated in vitamin B2 fermentation process - Google Patents
Treatment process and system for wastewater generated in vitamin B2 fermentation process Download PDFInfo
- Publication number
- CN114075013A CN114075013A CN202010807479.5A CN202010807479A CN114075013A CN 114075013 A CN114075013 A CN 114075013A CN 202010807479 A CN202010807479 A CN 202010807479A CN 114075013 A CN114075013 A CN 114075013A
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- membrane
- vitamin
- wastewater
- treatment
- nanofiltration
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- AUNGANRZJHBGPY-SCRDCRAPSA-N Riboflavin Chemical compound OC[C@@H](O)[C@@H](O)[C@@H](O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-SCRDCRAPSA-N 0.000 title claims abstract description 68
- AUNGANRZJHBGPY-UHFFFAOYSA-N D-Lyxoflavin Natural products OCC(O)C(O)C(O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O AUNGANRZJHBGPY-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229960002477 riboflavin Drugs 0.000 title claims abstract description 67
- 229930003471 Vitamin B2 Natural products 0.000 title claims abstract description 66
- 239000011716 vitamin B2 Substances 0.000 title claims abstract description 66
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- 239000002351 wastewater Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000000855 fermentation Methods 0.000 title claims abstract description 32
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F3/30—Aerobic and anaerobic processes
Abstract
The invention relates to a treatment process and a treatment system for wastewater generated in a vitamin B2 fermentation process, and belongs to the technical field of wastewater treatment. The method comprises the following steps: step (a), removing larger suspended matters and strains from the wastewater obtained in the refining process of vitamin B2 by adopting a coarse filtration method; step (b), adding a flocculating agent into the wastewater obtained in the step (a) for flocculation treatment; step (c), the wastewater in the step (b) is filtered by an ultrafiltration membrane, and flocculating constituents and macromolecular substances are removed; concentrating the wastewater obtained in the step (c) through a nanofiltration membrane; and (e) sending the nanofiltration membrane clear liquid obtained in the step (d) into a biochemical treatment process, and drying the obtained nanofiltration membrane concentrated liquid to obtain vitamin B2. On one hand, the vitamin B2 in the wastewater can be recovered, and on the other hand, the wastewater is discharged after reaching the standard.
Description
Technical Field
The invention relates to a treatment process and a treatment system for wastewater generated in a vitamin B2 fermentation process, and belongs to the technical field of wastewater treatment.
Background
Vitamin B2, also known as riboflavin, is a nutrient necessary for humans and animals to maintain normal structure and function of the body and is widely found in various foods and multi-vitamin dietary supplements. The preparation method of the vitamin B2 comprises a chemical total synthesis method and a fermentation semi-synthesis method, the chemical total synthesis method has a complex process route, high production cost and serious environmental pollution, and is gradually eliminated in industrial production. Most of the medicinal vitamin B2 in the global market in recent years is prepared by fermentation semi-synthesis.
The microbial fermentation production of vitamin B2 adopts a three-stage fermentation method, and the typical fermentation process is as follows: preparing a spore suspension from slant spores of mature vitamin B2 producing bacteria cultured at 25 ℃ by using sterile water, inoculating the spore suspension into a seed culture medium for culturing (30 + DEG C) for 30-40 h, and finally transferring the secondary fermentation liquid to a third-stage fermentation tank for fermentation (30 + DEG C, 160 h) to obtain the vitamin B2 fermentation liquid. The industrially used vitamin B2 producing bacteria mainly include Eremothecium ashbyii: (Eremotecium ashbyii) And cotton BursaAshbyagossypii) 2 kinds of bacteria. After strain improvement, the maximum level of vitamin B2 production can reach 10000U/ml.
After raw materials are fermented, centrifuged, extracted and refined, a large amount of mother liquor can be generated during fermentation, centrifugation and refinement, the mother liquor is yellow and milky, more suspended matters exist, fresh wastewater is basically odorless, and when the mother liquor is placed for a period of time, pungent odor is generated, and the mother liquor must be treated in time. When these mother liquors are mixed with other washing waters and the like, COD is about 8000mg/L and vitamin B2 dissolved in the waste water is still contained, which causes waste when directly disposed of. Accordingly, there is a need to provide a process for efficiently treating vitamin B2 wastewater and recycling dissolved vitamin B2 therefrom
Disclosure of Invention
The purpose of the invention is: provides a method for treating vitamin B2 fermentation wastewater, which can recover vitamin B2 in the wastewater and discharge the wastewater after reaching the standard.
A method for treating wastewater generated in a vitamin B2 fermentation process comprises the following steps:
step (a), removing larger suspended matters and strains from the wastewater obtained in the refining process of vitamin B2 by adopting a coarse filtration method;
step (b), adding a flocculating agent into the wastewater obtained in the step (a) for flocculation treatment;
step (c), the wastewater in the step (b) is filtered by an ultrafiltration membrane, and flocculating constituents and macromolecular substances are removed;
concentrating the wastewater obtained in the step (c) through a nanofiltration membrane;
and (e) sending the nanofiltration membrane clear liquid obtained in the step (d) into a biochemical treatment process, and drying the obtained nanofiltration membrane concentrated liquid to obtain vitamin B2.
Further, in the step (a), the coarse filtration is carried out by adopting a solid-liquid separation mode.
Further, the solid-liquid separation mode is selected from one or a combination of more of a centrifugal separation mode, a squeezing separation mode, a filtering mode, an upward floating separation mode or a settling separation mode.
Further, the flocculant used in step (b) may be one or a mixture of inorganic flocculants or bioflocculants.
Further, the inorganic flocculant is one or a mixture of aluminum sulfate, polyaluminium chloride, ferrous sulfate, alum and aluminum chloride; the addition amount of the inorganic flocculant is 20-80 mg/L.
Further, the biological flocculant is selected from one or a mixture of more of cellulose, starch, polyglucose, alginate, a microbial flocculant and gamma-polyglutamic acid; the adding amount of the biological flocculant is 100-300 mg/L.
Further, in the step (c), the ultrafiltration membrane is a multi-channel ceramic ultrafiltration membrane, and the pore diameter of the membrane is 20-50 nm.
Further, in the step (c), the concentrated solution after ultrafiltration is subjected to solid-liquid separation and dried to obtain the protein for feed.
Further, in the step (c), the multi-channel ceramic membrane adopts a cross flow filtration mode, and the flow rate of the membrane surface ranges from 1 m/s to 10 m/s.
Further, the residual heat generated in the drying process in the step (e) needs to be transferred to the inlet water entering the ultrafiltration membrane in the step (c) through a heat pump system.
Furthermore, in the process of filtering the multi-channel ceramic ultrafiltration membrane, firstly wetting the surface of a membrane layer of the multi-channel ceramic ultrafiltration membrane with 5-15wt% of sodium carbonate solution, drying, and then enabling 1-2wt% of calcium chloride solution to permeate the membrane layer under the pressure of 0.1-0.15 bar, so as to generate calcium carbonate in membrane pores; and (c) filtering the wastewater in the step (b), stopping filtering when a flocculating filter cake is formed on the surface of the membrane layer, allowing 2-5wt% hydrochloric acid solution to permeate the membrane layer under the pressure of 0.1-0.15 bar to dissolve and seep calcium carbonate, and continuing filtering the wastewater in the step (b).
Further, in the step (c), the multi-channel ceramic membrane is subjected to membrane cleaning after filtering the wastewater, and the cleaning method comprises water washing, alkali liquor washing and acid liquor washing in sequence.
Further, in the step (d), the molecular weight cut-off of the nanofiltration membrane is 200-500 Da.
Further, in the step (e), the biochemical treatment means an A-O or A2/O treatment unit.
A vitamin B2 fermentation process effluent's processing apparatus includes:
the hydrolysis crystallization kettle is used for refining the vitamin B2 prepared by the fermentation method;
the centrifugal machine is connected with the hydrolysis crystallization kettle and is used for carrying out centrifugal filtration treatment on the refined vitamin B2 obtained in the hydrolysis crystallization kettle;
the flocculation tank is connected to the filtrate side of the centrifuge and is used for flocculating the filtrate of the centrifuge;
the flocculating agent storage tank is connected with the flocculating tank and used for adding a flocculating agent into the flocculating tank;
the flocculation clear liquid tank is connected with the flocculant storage tank and used for storing clear liquid obtained by flocculation treatment;
the ultrafiltration membrane is connected with the flocculation clear liquid tank and is used for carrying out ultrafiltration treatment on clear liquid obtained by flocculation treatment;
the nanofiltration membrane is connected to the permeation side of the ultrafiltration membrane and is used for performing nanofiltration concentration on the permeate obtained by ultrafiltration treatment;
the biochemical treatment system is connected to the permeation side of the nanofiltration membrane and is used for performing biochemical treatment on the permeate liquid after nanofiltration treatment;
and the dryer is connected to the concentration side of the nanofiltration membrane and is used for drying the concentrated solution subjected to nanofiltration treatment.
Further, the dryer is a spray dryer.
Furthermore, an evaporator is arranged in a tail gas outlet of the spray dryer, a condenser is arranged in the flocculation clear solution tank, and the evaporator, the compressor, the condenser and the expansion valve are sequentially connected to form a heat pump system circulation of a closed pipeline.
Further, the ultrafiltration membrane is a multichannel ceramic membrane.
Further, the pore size of the ultrafiltration membrane is in the range of 20-50 nm.
Further, the molecular weight cut-off of the nanofiltration membrane is 200-500 Da.
Further, the biochemical treatment system is an A-O system or an A2/O system.
Advantageous effects
The invention treats the wastewater obtained in the processes of fermenting and refining the vitamin B2, and has the advantages that:
(1) vitamin B2 can be obtained from the refined wastewater, and resource utilization is realized;
(2) on the other hand, the protein in the wastewater is recovered by a flocculation mode and combined with the concentration and filtration of an ultrafiltration membrane, and can be used as feed;
(3) the ultrafiltration membrane is not easy to generate membrane hole blocking pollution and is easy to clean in the process of recovering flocculate;
(4) the waste heat of tail gas in the spray drying process is transferred to the raw material entering the ultrafiltration membrane by constructing a heat pump system, so that the energy in the spray drying process is effectively utilized, the temperature of the treated material liquid of the ultrafiltration membrane is improved, the viscosity is reduced, and the filtration flux is improved;
(5) vitamin B2 can be separated from inorganic matters in the wastewater through a nanofiltration membrane, and nanofiltration penetrating fluid can reach the standard and be discharged after biochemical treatment.
Drawings
FIG. 1 is a diagram of the apparatus of the present invention;
the device comprises a hydrolysis crystallization kettle 1, a centrifuge 2, a flocculation tank 3, a flocculant storage tank 4, a flocculation clear solution tank 5, an ultrafiltration membrane 6, a nanofiltration membrane 7, a biochemical treatment system 8, a dryer 9, an evaporator 10, a compressor 11, a condenser 12 and an expansion valve 13.
Detailed Description
The wastewater to be treated by the invention is the wastewater obtained in the vitamin B2 refining process, and the fermentation and refining processes can be generally operated as follows:
1) filtering, and removing coarse impurities from the vitamin B2 fermentation liquor by a rotary vibration sieve; 2) acidifying, heating the obtained filtrate, and adjusting the pH value with hydrochloric acid to obtain acidified hydrolysate; 3) separating, acidifying the hydrolysate, and performing centrifugal separation to obtain concentrated slurry; 4) hydrolyzing for crystallization, diluting the obtained thick slurry with water, adjusting the pH value with acid, heating the treated liquid to boiling, introducing compressed air for boosting pressure, maintaining the pressure, relieving the pressure, and cooling to obtain vitamin B2 crystal slurry; 5) centrifuging, washing with water, and drying the obtained vitamin B2 crystal to obtain vitamin B2.
Wherein, when the purified vitamin B2 is centrifugally separated in the step (5), a large amount of waste water is generated, and the invention recycles and treats the waste water.
In the case of rough filtration of the material obtained in the purification process, a solid-liquid separation method may be employed to remove large suspended matters and strains, and the solid-liquid separation method is not particularly limited. Specific examples of the solid-liquid separation treatment include a centrifugal separation system, a squeezing separation system, a filtration system, a floating separation system, and a settling separation system. Examples of the centrifugal separation method include a horizontal continuous centrifuge (screw decanter treatment), a separation plate centrifuge, a centrifugal filter, and a mansion plez type ultracentrifuge, examples of the filtration method include a belt filter, a belt press, a screw press, a precoat filter, and a filter press, examples of the floating separation method include a continuous floating separation device, and examples of the sedimentation separation method include a coagulation sedimentation separator, a rapid sedimentation separator, and the like, but not particularly limited to any of the above.
Adding a flocculating agent into the centrifuged wastewater to further reduce the chroma and remove COD pollutants in the wastewater, wherein the flocculating agent adopted can be an inorganic flocculating agent or a biological flocculating agent, and the inorganic flocculating agent is selected from one or a mixture of aluminum sulfate, polyaluminium chloride, ferrous sulfate, alum and aluminum chloride; the addition amount of the inorganic flocculant is 20-80 mg/L; the biological flocculant is one or a mixture of more of cellulose, starch, polyglucose, alginate, microbial flocculant and gamma-polyglutamic acid; the adding amount of the biological flocculant is 100-300 mg/L.
After the flocculation reaction, an ultrafiltration membrane is adopted for filtering, so that a flocculating constituent can be filtered out, and colloidal pollutants can be removed, thereby reducing the load of subsequent filtration of the nanofiltration membrane. The materials of the ultrafiltration membrane and ultrafiltration membrane used herein are roughly classified into inorganic membranes and organic membranes, and further classified into hydrophobic and hydrophilic. The hydrophobic organic film is not limited thereto, and examples thereof include polysulfone, polyethersulfone, polyether, polyvinylidene fluoride, polyethylene, polypropylene, and the like. The hydrophilic organic film is not limited to this, and examples thereof include polyacrylonitrile, polyamide, polyimide, cellulose acetate, and the like. The material of the porous membrane constituting the ceramic separation membrane can be appropriately selected from conventionally known ceramic materials. For example, oxide-based materials such as alumina, zirconia, magnesia, silica, titania, ceria, yttria, and barium titanate; composite oxide materials such as cordierite, mullite, forsterite, steatite, sialon, zircon, ferrite and the like; nitride materials such as silicon nitride and aluminum nitride; carbide-based materials such as silicon carbide; hydroxide materials such as hydroxyapatite; elemental materials such as carbon and silicon; or an inorganic composite material containing two or more of them. Natural minerals (clay, clay minerals, earthenware slag, silica sand, pottery stone, feldspar, white sand) or blast furnace slag, fly ash, etc. may also be used. Among these, 1 or 2 or more kinds selected from alumina, zirconia, titania, magnesia and silica are preferable, and ceramic powder mainly composed of alumina, zirconia or titania is more preferable. The term "mainly" as used herein means that 50 mass% or more (preferably 75 mass% or more, and more preferably 80 to 100 mass%) of the entire ceramic powder is alumina or silica. For example, among porous materials, alumina is inexpensive and excellent in handling properties. Further, since a porous structure having pore diameters suitable for liquid separation can be easily formed, a ceramic separation membrane having excellent liquid permeability can be easily produced. Among the above aluminas, alpha-alumina is particularly preferably used. Alpha-alumina has the characteristics of being chemically stable and having high melting point and mechanical strength. Therefore, by using α -alumina, a ceramic separation membrane that can be utilized in a wide range of applications (e.g., industrial fields) can be manufactured. The filter element shape comprises flat membrane, tubular membrane, spiral membrane, hollow fiber (hollow silk) membrane and all module forms. The filtration method includes a total filtration method and a cross-flow method. The total filtration system is a system in which all of the water supplied to the membrane is filtered. In contrast, the cross-flow method is a method of filtering while suppressing the accumulation of suspended substances or colloids contained in water supplied to a membrane on a membrane surface by causing a water flow to flow parallel to the membrane surface.
In the process of filtering the ultrafiltration membrane, macromolecular colloids, other proteins and other components in the fermentation wastewater can block membrane pores, and the membrane pores are not easy to eliminate membrane pore blocking pollution in a surface washing and cleaning manner after being blocked; therefore, in the invention, firstly, the ceramic ultrafiltration membrane is soaked in the sodium carbonate solution, and the solution can be absorbed into the inner pore canal because the surface micropores of the membrane can generate the slurry absorption function, at the moment, the sodium carbonate solution is wetted in the inner pore canal, after drying, sodium carbonate is remained in the pore canal, at the moment, the calcium chloride solution is slowly pressed into the pore of the membrane under the condition of micro-positive pressure, can generate calcium carbonate in situ, partially block the membrane pore, and when the flocculating solution is filtered, the protein, the colloid and the flocculating constituent are not easy to drill into the membrane pore and only form a filter cake layer, at the moment, by pressing acid solution under the condition of micro positive pressure, can dissolve calcium carbonate generated in situ and remove calcium carbonate from the penetrating fluid, remove the blockage in the membrane pores, recover the filtration flux, while maintaining the coverage of the cake layer on the membrane surface to prevent further contamination from penetrating into the membrane pores during filtration. Because the filter cake layer is easier to remove in the cleaning process relative to the pollutants in the membrane pores, the recovery rate of the cleaning flux on the membrane surface is higher when the filtration is carried out by the method. The membrane cleaning method adopted in the invention can be water washing, alkali liquor washing and acid liquor washing.
After the ultrafiltration treatment, most of the protein and cell debris in the wastewater can be removed, and the ultrafiltration concentrated solution mainly contains flocculating constituents and macromolecular protein which can be used as animal feed after further concentration.
The filtrate of ultrafiltration mainly contains vitamin B2 and inorganic salt, and vitamin B2 can be concentrated by the separation treatment of a nanofiltration membrane and separated from the inorganic salt, so that the purity of the recovered product is improved. Nanofiltration membranes in the present invention are membranes defined as "pressure driven membranes that block particles smaller than 2nm and dissolved macromolecules". Effective nanofiltration membranes suitable for use in the present invention are preferably such membranes: there is an electric charge on the membrane surface, and thus improved separation efficiency is exhibited by a combination of fine pore separation (particle size separation) and electrostatic separation benefiting from the electric charge on the membrane surface. Therefore, it is necessary to use a nanofiltration membrane capable of removing a high molecular substance by particle size separation while separating an alkali metal ion to be recovered from another ion having a different charge characteristic by means of charge. As a material of the nanofiltration membrane used in the present invention, a polymer material such as cellulose acetate polymer, polyamide, sulfonated polysulfone, polyacrylonitrile, polyester, polyimide, vinyl polymer, or the like can be used. The film is not limited to one composed of only one material, and may be a film containing a plurality of the materials. With respect to the membrane structure, the membrane may be an asymmetric membrane having a dense layer on at least one side of the membrane and having micropores with pore diameters gradually increasing from the dense layer toward the inside of the membrane or the other side; or a composite membrane having a very thin functional layer of another material on the dense layer of the asymmetric membrane.
The nanofiltration concentrated solution can be obtained by drying, wherein the drying can be realized by adopting a reduced pressure drying mode, a spray drying mode and the like, and the nanofiltration penetrating fluid can be further sent into a biochemical system for treatment and can be discharged after reaching the standard.
The tail gas has residual heat in the spray drying process, and in the filtering process of the ultrafiltration membrane, when the temperature of the raw material liquid is increased, the viscosity of the raw material liquid is reduced, so that the filtering flux can be increased. Therefore, an evaporator is arranged in a tail gas outlet of the spray dryer, a condenser is arranged in the flocculation clear liquid tank, and the evaporator, the compressor, the condenser and the expansion valve are sequentially connected to form a heat pump system circulation of a closed pipeline. The evaporator can absorb heat from the tail gas of the spray dryer, and the heat can be transferred to a flocculation clear solution tank used for storing ultrafiltration membrane raw material liquid through a heat pump circulating system formed by a closed pipeline, so that the temperature of the raw material liquid entering the ultrafiltration membrane is increased, the tail gas in the spray drying process is transferred to the raw material of the ultrafiltration membrane, the temperature of the ultrafiltration membrane material liquid is increased, and the filtration flux is increased.
Example 1
Centrifuging mother liquor in the refining process of vitamin B2, wherein the COD content is 23870mg/L, SS 35230mg/L, NaCl 5.3g/L and vitamin B28105 mg/L; adding a ferric oxide flocculating agent of 30mg/L and a gamma-polyglutamic acid flocculating agent of 220mg/L for flocculation treatment, and settling flocculated wastewater to obtain bottom flocculation residues and clear liquid; sending the clear liquid into a multi-channel ceramic ultrafiltration membrane for cross-flow filtration treatment, wherein the membrane aperture of the ultrafiltration membrane is 50nm, the cross-flow rate is 4m/s, and the concentrated solution of the ultrafiltration membrane is mixed with flocculation residues and then dehydrated to be used as animal feed; after the ultrafiltration membrane is filtered, sequentially adopting deionized water to wash the surface for 20min, 1wt% of NaOH for 30min and 1wt% of HCl for 10min to wash; the clear liquid of the ultrafiltration membrane is sent into a nanofiltration membrane with the molecular weight cutoff of 200Da for filtration, vitamin B2 and micromolecular impurities are separated, the concentrated solution of the nanofiltration membrane is subjected to spray drying to obtain vitamin B2, and the permeate of the nanofiltration membrane is sent into an A2/O processing unit for advanced treatment; an evaporator is arranged in a tail gas pipe of the spray dryer, and waste heat is transferred to feed liquid of the ultrafiltration membrane through a heat pump system.
Example 2
Centrifuging mother liquor in the refining process of vitamin B2, wherein the COD content is 21130mg/L, the SS 33730mg/L, the NaCl content is 5.7g/L, and the vitamin B content is 28330 mg/L; adding 35mg/L ferric oxide flocculant and 200mg/L gamma-polyglutamic acid flocculant for flocculation treatment, and settling flocculated wastewater to obtain bottom flocculation residues and clear liquid; sending the clear liquid into a multi-channel ceramic ultrafiltration membrane for cross-flow filtration treatment, wherein the membrane aperture of the ultrafiltration membrane is 50nm, the cross-flow rate is 4m/s, and the concentrated solution of the ultrafiltration membrane is mixed with flocculation residues and then dehydrated to be used as animal feed; after the ultrafiltration membrane is filtered, washing the surface of the ultrafiltration membrane for 15min by using deionized water, washing the ultrafiltration membrane for 35min by using 1wt% of NaOH and washing the ultrafiltration membrane for 15min by using 1wt% of HCl in sequence; the clear liquid of the ultrafiltration membrane is sent into a nanofiltration membrane with the molecular weight cutoff of 300Da for filtration, vitamin B2 and micromolecular impurities are separated, the concentrated solution of the nanofiltration membrane is subjected to spray drying to obtain vitamin B2, and the permeate of the nanofiltration membrane is sent into an A2/O processing unit for advanced treatment; an evaporator is arranged in a tail gas pipe of the spray dryer, and waste heat is transferred to feed liquid of the ultrafiltration membrane through a heat pump system.
Example 3
The difference from example 3 is that when the flocculated supernatant is filtered by the ceramic membrane, the in-situ generation of calcium carbonate prevents the fouling of the membrane pores by clogging. Centrifuging mother liquor in the refining process of vitamin B2, wherein the COD content is 23870mg/L, SS 35230mg/L, NaCl 5.3g/L and vitamin B28105 mg/L; adding a ferric oxide flocculating agent of 30mg/L and a gamma-polyglutamic acid flocculating agent of 220mg/L for flocculation treatment, and settling flocculated wastewater to obtain bottom flocculation residues and clear liquid; wetting the surface of a membrane layer of the multi-channel ceramic ultrafiltration membrane with 10wt% of sodium carbonate solution, drying, and enabling 1wt% of calcium chloride solution to permeate the membrane layer under the pressure of 0.1bar to generate calcium carbonate in membrane pores; then, filtering the clear liquid, stopping filtering when a flocculating constituent filter cake is formed on the surface of the membrane layer, enabling a 3wt% hydrochloric acid solution to permeate the membrane layer under the pressure of 0.1bar so as to dissolve and seep calcium carbonate, and then continuously filtering the clear liquid, wherein the membrane aperture of the ultrafiltration membrane is 50nm, the cross flow velocity is 4m/s, and the concentrated solution and the flocculation residues of the ultrafiltration membrane are mixed and then dehydrated to be used as animal feed; after the ultrafiltration membrane is filtered, sequentially adopting deionized water to wash the surface for 20min, 1wt% of NaOH for 30min and 1wt% of HCl for 10min to wash; the clear liquid of the ultrafiltration membrane is sent into a nanofiltration membrane with the molecular weight cutoff of 200Da for filtration, vitamin B2 and micromolecular impurities are separated, the concentrated solution of the nanofiltration membrane is subjected to spray drying to obtain vitamin B2, and the permeate of the nanofiltration membrane is sent into an A2/O processing unit for advanced treatment; an evaporator is arranged in a tail gas pipe of the spray dryer, and waste heat is transferred to feed liquid of the ultrafiltration membrane through a heat pump system.
Example 4
The difference from example 3 is that when the flocculated supernatant is filtered by the ceramic membrane, the in-situ generation of calcium carbonate prevents the fouling of the membrane pores by clogging. Centrifuging mother liquor in the refining process of vitamin B2, wherein the COD content is 21130mg/L, the SS 33730mg/L, the NaCl content is 5.7g/L, and the vitamin B content is 28330 mg/L; adding 35mg/L ferric oxide flocculant and 200mg/L gamma-polyglutamic acid flocculant for flocculation treatment, and settling flocculated wastewater to obtain bottom flocculation residues and clear liquid; wetting the surface of a membrane layer of the multi-channel ceramic ultrafiltration membrane with 10wt% of sodium carbonate solution, drying, and enabling 1wt% of calcium chloride solution to permeate the membrane layer under the pressure of 0.1bar to generate calcium carbonate in membrane pores; then, filtering the clear liquid, stopping filtering when a flocculating constituent filter cake is formed on the surface of the membrane layer, enabling a 3wt% hydrochloric acid solution to permeate the membrane layer under the pressure of 0.1bar so as to dissolve and seep calcium carbonate, and then continuously filtering the clear liquid, wherein the membrane aperture of the ultrafiltration membrane is 50nm, the cross flow velocity is 4m/s, and the concentrated solution and the flocculation residues of the ultrafiltration membrane are mixed and then dehydrated to be used as animal feed; after the ultrafiltration membrane is filtered, washing the surface of the ultrafiltration membrane for 15min by using deionized water, washing the ultrafiltration membrane for 35min by using 1wt% of NaOH and washing the ultrafiltration membrane for 15min by using 1wt% of HCl in sequence; the clear liquid of the ultrafiltration membrane is sent into a nanofiltration membrane with the molecular weight cutoff of 300Da for filtration, vitamin B2 and micromolecular impurities are separated, the concentrated solution of the nanofiltration membrane is subjected to spray drying to obtain vitamin B2, and the permeate of the nanofiltration membrane is sent into an A2/O processing unit for advanced treatment; an evaporator is arranged in a tail gas pipe of the spray dryer, and waste heat is transferred to feed liquid of the ultrafiltration membrane through a heat pump system.
The results of the above examples after treating vitamin B2 refined wastewater were as follows:
as can be seen from the table above, the method can realize the recycling of the components in the wastewater generated in the vitamin B2 refining process after the wastewater is treated, can obtain the vitamin B2 with the purity of more than 30 percent, and simultaneously realizes the standard discharge treatment of the wastewater. It can be seen from the comparison between the embodiment 1 and the embodiment 3 that after the ceramic membrane is subjected to surface treatment by adopting the in-situ calcium carbonate generation mode, the blockage and pollution in the membrane pores caused by the drilling of colloids, proteins and the like into the membrane pores can be effectively avoided when the flocculated clear liquid is filtered, so that the ultrafiltration membrane has higher flux recovery rate after the cleaning process, the flux recovery rate can reach more than 90%, and if the membrane pores are blocked, the flux recovery rate is about 70%.
Claims (10)
1. A method for treating wastewater generated in a vitamin B2 fermentation process is characterized by comprising the following steps:
step (a), removing larger suspended matters and strains from the wastewater obtained in the refining process of vitamin B2 by adopting a coarse filtration method;
step (b), adding a flocculating agent into the wastewater obtained in the step (a) for flocculation treatment;
step (c), the wastewater in the step (b) is filtered by an ultrafiltration membrane, and flocculating constituents and macromolecular substances are removed;
concentrating the wastewater obtained in the step (c) through a nanofiltration membrane;
and (e) sending the nanofiltration membrane clear liquid obtained in the step (d) into a biochemical treatment process, and drying the obtained nanofiltration membrane concentrated liquid to obtain vitamin B2.
2. The method for treating vitamin B2 fermentation process wastewater, according to claim 1, wherein the step (a) is further performed by a solid-liquid separation method to perform coarse filtration;
further, the solid-liquid separation mode is selected from one or a combination of more of a centrifugal separation mode, a squeezing separation mode, a filtering mode, an upward floating separation mode or a settling separation mode.
3. The method for treating wastewater from vitamin B2 fermentation according to claim 1, wherein the flocculating agent used in step (B) is one or a mixture of inorganic flocculating agent and biological flocculating agent;
further, the inorganic flocculant is one or a mixture of aluminum sulfate, polyaluminium chloride, ferrous sulfate, alum and aluminum chloride; the addition amount of the inorganic flocculant is 20-80 mg/L;
further, the biological flocculant is selected from one or a mixture of more of cellulose, starch, polyglucose, alginate, a microbial flocculant and gamma-polyglutamic acid; the adding amount of the biological flocculant is 100-300 mg/L.
4. The method for treating vitamin B2 fermentation process wastewater according to claim 1, wherein in step (c), the ultrafiltration membrane is a multi-channel ceramic ultrafiltration membrane with a pore size ranging from 20 nm to 50 nm;
further, in the step (c), the concentrated solution after ultrafiltration is subjected to solid-liquid separation and dried to obtain protein for feed;
further, in the step (c), the multi-channel ceramic membrane adopts a cross flow filtration mode, and the flow rate of the membrane surface ranges from 1 m/s to 10 m/s;
further, the waste heat generated in the drying process in the step (e) needs to be transferred into the water entering the ultrafiltration membrane in the step (c) through a heat pump system;
furthermore, in the process of filtering the multi-channel ceramic ultrafiltration membrane, firstly wetting the surface of a membrane layer of the multi-channel ceramic ultrafiltration membrane with 5-15wt% of sodium carbonate solution, drying, and then enabling 1-2wt% of calcium chloride solution to permeate the membrane layer under the pressure of 0.1-0.15 bar, so as to generate calcium carbonate in membrane pores; and (c) filtering the wastewater in the step (b), stopping filtering when a flocculating filter cake is formed on the surface of the membrane layer, allowing 2-5wt% hydrochloric acid solution to permeate the membrane layer under the pressure of 0.1-0.15 bar to dissolve and seep calcium carbonate, and continuing filtering the wastewater in the step (b).
5. The method for treating vitamin B2 fermentation process wastewater according to claim 1,
further, in the step (c), after the multi-channel ceramic membrane filters the wastewater, membrane cleaning is carried out, and the cleaning method comprises water washing, alkali liquor washing and acid liquor washing in sequence;
further, in the step (d), the molecular weight cut-off of the nanofiltration membrane is 200-;
further, in the step (e), the biochemical treatment means an A-O or A2/O treatment unit.
6. A vitamin B2 fermentation process effluent's processing apparatus which characterized in that includes:
the hydrolysis crystallization kettle (1) is used for refining the vitamin B2 prepared by a fermentation method;
the centrifugal machine (2) is connected with the hydrolysis crystallization kettle (1) and is used for carrying out centrifugal filtration treatment on the refined vitamin B2 obtained in the hydrolysis crystallization kettle (1);
the flocculation tank (3) is connected to the filtrate side of the centrifuge (2) and is used for flocculating the filtrate of the centrifuge (2);
the flocculant storage tank (4) is connected with the flocculation tank (3) and is used for adding a flocculant into the flocculation tank (3);
the flocculation clear liquid tank (5) is connected with the flocculant storage tank (4) and is used for storing clear liquid obtained by flocculation treatment;
the ultrafiltration membrane (6) is connected with the flocculation clear liquid tank (5) and is used for carrying out ultrafiltration treatment on clear liquid obtained by flocculation treatment;
a nanofiltration membrane (7) connected to the permeation side of the ultrafiltration membrane (6) and used for carrying out nanofiltration concentration on the permeate obtained by ultrafiltration treatment;
the biochemical treatment system (8) is connected to the permeation side of the nanofiltration membrane (7) and is used for performing biochemical treatment on the permeation liquid subjected to nanofiltration treatment;
and a dryer (9) connected to the concentration side of the nanofiltration membrane (7) for drying the nanofiltration-treated concentrated solution.
7. The vitamin B2 fermentation process wastewater treatment device of claim 6, wherein, further, the dryer (9) is a spray dryer;
furthermore, an evaporator (10) is arranged in a tail gas outlet of the spray dryer, a condenser (12) is arranged in the flocculation clear liquid tank (5), and the evaporator (10), the compressor (11), the condenser (12) and the expansion valve (13) are sequentially connected to form a heat pump system circulation of a closed pipeline.
8. The vitamin B2 fermentation process wastewater treatment device of claim 6, wherein, further, the ultrafiltration membrane (6) is a multi-channel ceramic membrane;
further, the pore diameter of the ultrafiltration membrane (6) is in the range of 20-50 nm.
9. The vitamin B2 fermentation process wastewater treatment device as claimed in claim 6, wherein, the cut-off molecular weight of the nanofiltration membrane (7) is 200-500 Da.
10. The apparatus for treating vitamin B2 fermentation process wastewater as claimed in claim 6, wherein the biochemical treatment system is an A-O system or an A2/O system.
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