CN102921294A - Method for treating and degrading dichloromethane waste gas by using silicone masterbatch - Google Patents
Method for treating and degrading dichloromethane waste gas by using silicone masterbatch Download PDFInfo
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Abstract
The invention provides a method for treating and degrading dichloromethane waste gas by using silicone masterbatch; and the method comprises the following steps of: adding a mineral culture medium and 5-30 wt % of silicone masterbatch to a reactor; putting Methylobacterium rhodesianum H13 with preservation number of CCTCC No: M2010121; culturing the methylobacterium rhodesianum until cell concentration is 100-2000 mg/L; leading waste gas containing dichloromethane into a fermentation liquor from the bottom of the reactor; stirring and reacting the fermentation liquor; keeping a reaction temperature at 15-40 DEG C, wherein the stirring rotation speed is 200-600 rpm, the pH value is controlled at 5-9 and the staying time is 30-120 s; and obtaining purified gas at an outlet. Compared with the traditional single-phase reaction system, the method for treating and degrading the dichloromethane waste gas by using the silicone masterbatch, provided by the invention, has the advantages as follows: the tolerated concentration of the Methylobacterium rhodesianum H13 to the dichloromethane is increased from 20 mm to 40 mm. When the load at an inlet is 300 g/(m3.h), the removal rate of the single-phase system to the dichloromethane is about 35%; and the removal rate of a solid-liquid double phase system can reach about 90%.
Description
(1) technical field
The present invention relates to a kind of silicone master batch as the application of non-aqueous system (NAP) in the carrene waste gas purification of solid-liquid double-phase bioreactor.
(2) background technology
Carrene (Dichloromethane is called for short DCM) is the compound that generates after two hydrogen atoms in the methane molecule are replaced by chlorine.DCM mainly makes solvent and uses as a kind of important industrial solvent at aspects such as metal material degreasing, paint removal industry and pharmaceuticals industries, along with the quickening of industrialization, urbanization process, its demand is also increased day by day.Although DCM is water-soluble little, fat-soluble very strong, easily accumulate in vivo the fat, the enrichment by food chain accumulates in senior predator, and organism is caused harmful effect.Show according to the study, DCM has stronger excitant to skin and mucous membrane, and carcinogenic effect is more arranged, and can cause tumour in Mouse and rat lung and liver.
The extensive use of DCM makes its pollution to underground water and atmosphere day by day serious, in environment, have accumulation property and sustainability, be listed among the toxic pollutant lists of 129 kinds of preferential controls by Environmental Protection Agency, therefore be badly in need of seeking a kind of efficient removal method.Bioanalysis is based on the metabolic activity of microorganism degraded noxious pollutant, in processing procedure, have environment friendly, operating cost low, can process the advantages such as exhausted air quantity is large.Yet traditional bioanalysis often is difficult to reach ideal effect when the volatile organic contaminant (VOCs) of this class poorly water-soluble of degraded DCM.This is that the gas-liquid mass transfer restriction that poorly water-soluble causes often becomes the primary factor of restriction waste gas purification because the degraded of VOCs is a complex process that relates to gas, liquid, biomembrane phase mass transfer and biochemical degradation.In addition, the impact of the vital movement vulnerable to pollution substrate concentration of microorganism in the VOCs degradation process, the excessive concentration microbial activity is suppressed, and concentration is crossed the basic metabolism of humble biology and is difficult to keep.Therefore bioanalysis is difficult to effectively purify unstable state waste gas, especially contain the unstable state waste gas of DCM.
For the bottleneck problem in the above-mentioned DCM degradation process, two-phase separating bio reactor is applied to waste gas purification gradually.Two-phase separating bio reactor can effectively overcome the inhibition of the high concentration that runs in the course of reaction, highly toxic substrate, intermediate product by add nonaqueous phase (NAP) in reaction system, and the limiting factors such as mass transfer obstacle between water, VOCs and the microorganism, realize that microorganism is to the efficient removal of VCOs.Yeom etc. are take the two-phase separating bio agitator that adds hexadecane as research object, and the removal of benzene load reaches 291 g/ (m
3﹒ h).The two-phase separate reactor of the discoveries such as Arriaga interpolation 10% silicone oil is compared with common stirring reactor, and n-hexane is removed load from 50 g/ (m
3H) be increased to 120 g/ (m
3H).Although the adding of the organic phase such as silicone oil, hexadecane so that two-phase reactor be significantly improved aspect exhaust-gas treatment effect and the anti impulsion load,, there is obvious defective in the liquid NAP of this kind: surface tension is little and easily produce foam; Easily emulsification, causing cell to enter organic phase affects degrading activity.And replace existing liquid NAP with solid-state polymer, then the problems such as the easy foamed of NAP, difficult recovery, high financial cost will be readily solved.
The present invention as the biological cleaning of NAP with promotion DCM waste gas, there is not yet report with silicone master batch so far.
(3) summary of the invention
The objective of the invention is provides a kind of solid-state polymer as NAP and application thereof in the two-phase separating bio reactor degraded DCM process for deficiencies such as above-mentioned bioanalysis degraded DCM poor removal effect, capacity of resisting impact load are low.
The technical solution used in the present invention is:
A kind of method of using silicone master batch processing degraded carrene waste gas, described method is: add minimal medium and silicone master batch in reactor, the consumption of silicone master batch is the 5-30wt%(of minimal medium quality preferred 10 ~ 20wt%), inoculation Rhodesia methyl bacillus (Methylobacterium rhodesianum) H13 in the minimal medium, deposit number: CCTCC No:M 2010121, being cultured to cell concentration is 100-2000 mg/L(preferred 500 ~ 550mg/L), pass into the waste gas that contains carrene from reactor bottom to zymotic fluid, stirring reaction, keeping reaction temperature is 15-40 ℃ (preferred 33 ~ 34 ℃), speed of agitator 200-600rpm, the preferred pH value 7.5 of pH value 5-9(of control reactant liquor), the time of staying 30-120s(of waste gas in zymotic fluid is preferred 60 ~ 80s), and outlet namely obtains the purified gas after the carrene degraded.
Described minimal medium is prepared by following composition: 4.5g Na
2HPO
412H
2O, 1.0g KH
2PO
4, 0.5g (NH
4)
2SO
4, 0.1g MgSO
47H
2O, 0.023g CaCl
2, 1mL trace element mother liquor, water complements to 1000mL; Described micro-mother liquid concentration consists of: FeSO
47H
2O 1.0 g/L, CuSO
45H
2O 0.02 g/L, H
3BO
30.014 g/L, MnSO
44H
2O 0.10 g/L, ZnSO
47H
2O 0.10 g/L, Na
2MoO
42H
2O 0.02 g/L, CoCl
26H
2O 0.02 g/L, solvent are water.
The time of staying of waste gas of the present invention in zymotic fluid is that fermentating liquid volume obtains divided by gas flow rate.Induction air flow ratio by control waste gas can be controlled the time of staying.
Control pH value 5-9 of the present invention, the NaOH adjust pH of available 1mol/L.
24 hours replaceable 10% ~ 15% fresh minimal medium of the every operation of reactor of the present invention.Described reactor can be continuously long-running.
Further, preferred the inventive method is carried out according to the following steps: add minimal medium and silicone master batch in reactor, the consumption of silicone master batch is the 10-20 % of minimal medium quality, drop into Rhodesia methyl bacillus (Methylobacterium rhodesianum) H13 in the minimal medium, deposit number: CCTCC No:M 2010121, being cultured to cell concentration is 500 ~ 550 mg/L, pass into the waste gas that contains carrene from reactor bottom to zymotic fluid, stirring reaction, keeping reaction temperature is 33 ~ 34 ℃, speed of agitator 200-600rpm, the pH value 7.5 of control reactant liquor, the time of staying 60 ~ the 80s of waste gas in reactant liquor, outlet namely obtains the purified gas after the carrene degraded.
Silicone master batch of the present invention can be used as two-phase separate reactor NAP, can buy to obtain on market, and the silicone master batch MB50-008 that uses in the embodiment of the invention derives from DOW Corning, and diameter is about 3 mm, and density is about 0.918 g/m
3Irregular particle, white is siloxanes to be distributed to form silicone in the silica, adds polyolefin and other assistants again and makes.Silicone master batch is a kind of novel high polymer quantity high performance multifunctional granular master batch, has good processing characteristics, is mainly used in the plastic processing industry.Silicone master batch has overcome traditional silicone oil as the weakness of plastic additive: have silicone content high, molecular weight is large, does not separate out, and extrudes the characteristics such as non-slip in screw rod.The present invention is based on the silicone master batch chemical composition similar with silicone oil, in view of the extensive use of silicone oil in the two-phase separate reactor, creatively silicone master batch is applied to two-phase separate reactor degraded DCM.
That the present invention utilizes is that this laboratory screening identifies, take DCM as sole carbon source with Rhodesia methyl bacillus (Methylobacterium rhodesianum) H13 of the energy, deposit number: CCTCC No:M 2010121, patent of invention publication number CN 101993839.In the embodiment of the invention, the two-phase system that the H13 bacterium is seeded to respectively the single_phase system that only contains minimal medium and adds 10% silicone master batch, two kinds of systems are degraded to DCM respectively, and experimental result shows the adding of silicone master batch so that the H13 bacterium is brought up to 40mM to the tolerance concentration of DCM by 20mM.Same at the import load is 300 g/ (m
3H) time, the homogeneous reaction device is about 35% to the clearance of carrene, and the clearance of solid-liquid double-phase reactor can reach about 90%.
Also change the import load in the embodiment of the invention, investigate two kinds of systems to the removal effect of DCM.And instantaneous change impact load, investigate the ability that two kinds of reactors are resisted impact loads.The result shows, the adding of silicone master batch is conducive to improve the removal effect of DCM, be conducive to improve the ability of system anti-shock loading, under the high concentration impact load, the two-phase reactor that adds silicone master batch still can keep the clearance more than 80%, and the place an order clearance of phase reactor of similarity condition is reduced to 30%.
Beneficial effect of the present invention is mainly manifested in: filtered out this common plastic processing raw material of silicone master batch, with its creationary two-phase separate reactor that is applied to.The two-phase separate reactor that makes up can effectively degrade DCM, opposing high concentration impact load are used for the engineering of biological cleaning DCM waste gas and to be laid a good foundation.
(4) description of drawings
Fig. 1 is the comparison of H13 bacterium after not adding silicone master batch and adding 10% silicone master batch to DCM tolerance concentration, and left figure is the single-phase minimal medium that does not add silicone master batch, and right figure is the two-phase minimal medium that adds 10% silicone master batch.
Fig. 2 is in the single-phase and two-phase reactor degraded DCM process, clearance and the comparison of removing load, and left figure is the homogeneous reaction device, right figure be the two-phase reactor of adding 10% silicone master batch.
Fig. 3 imports and exports concentration, clearance, dissolved oxygen over time under the low impact load, and left figure is the homogeneous reaction device, and right figure is the two-phase reactor that adds 10% silicone master batch.
Fig. 4 is that the HI high impact load is lower, imports and exports concentration, clearance, dissolved oxygen over time, and left figure is the homogeneous reaction device, and right figure is the two-phase reactor that adds 10% silicone master batch.
(5) specific embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
The MB50-008 that the silicone master batch of using among the embodiment uses DOW Corning to produce.
Embodiment 1: the distribution coefficient of silicone master batch
In the 250ml air-tight bottle, the air Mixture that adds respectively 5g silicone master batch and adding 1,5,10,15,20,25mM DCM, vibration 30min, DCM concentration in the gas chromatographic detection gas phase, calculate DCM concentration in the silicone master batch according to mass balance again, thereby calculate the distribution coefficient in silicone master batch/gas phase.Concentration dichloromethane in distribution coefficient=silicone master batch in silicone master batch/gas phase/airborne concentration dichloromethane
In like manner, after adding silicone master batch in the 250ml air-tight bottle, fill with respectively the DCM of water and adding 1,5,10,15,20,25mM, measure the DCM concentration of aqueous phase behind the magnetic stirrer 30min, according to the DCM concentration in the mass balance calculating silicone master batch, calculate the distribution coefficient of silicone master batch/aqueous phase again.Concentration dichloromethane in concentration dichloromethane/water in the distribution coefficient=silicone master batch of silicone master batch/water.
After tested, the distribution coefficient of silicone master batch in silicone master batch/gas phase is 186.5, is 341 at the distribution coefficient of silicone master batch/aqueous phase.
Embodiment 2: the substrate tolerance
Minimal medium is prepared by following composition: 4.5g Na
2HPO
412H
2O, 1.0g KH
2PO
4, 0.5g (NH
4)
2SO
4, 0.1g MgSO
47H
2O, 0.023g CaCl
2, 1mL trace element mother liquor, water complements to 1000mL.
The trace element mother liquid concentration forms: FeSO
47H
2O 1.0 g/L, CuSO
45H
2O 0.02 g/L, H
3BO
30.014 g/L, MnSO
44H
2O 0.10 g/L, ZnSO
47H
2O 0.10 g/L, Na
2MoO
42H
2O 0.02 g/L, CoCl
26H
2O 0.02 g/L, solvent are water.
The 43ml minimal medium adds 5g silicone master batch bead, H13 bacterium (deposit number: make initial cell concentration (take OD) be 0.07 CCTCC No:M 2010121) after the access 2ml activation, the initial concentration that adds DCM is respectively 5,10,20,30,40,50,60,70,80mM, in 34 ℃, the shaking table of 160r/min, carry out degradation experiment, measure at regular intervals DCM concentration, pH value 7.5 keeps stable in the incubation, with similarity condition but the single-phase minimal medium that does not add silicone master batch is done contrast.The DCM concentration changes with time the results are shown in Figure among 1, Fig. 1, and left figure is the single-phase minimal medium that does not add silicone master batch, and right figure is the two-phase minimal medium that adds 10% silicone master batch.
In single_phase system, when the concentration of DCM was higher than 20mM, the H13 bacterium almost can not utilize, and thalline aggregate and precipitate phenomenon occurred in the saline bottle behind the cultivation 24h, showed that the DCM of high concentration produces very strong inhibitory action to thalline.And after adding 10% silicone master batch, DCM brings up to 40mM to the inhibition concentration of H13 bacterium by 20mM.As seen the effective DCM in the absorption system of silicone master batch is alleviated substrate to the inhibitory action of cell.
The degraded of embodiment 3:DCM in single-phase and two-phase reactor
Adopt the Bioflo415/14L stirred-tank fermenter as reaction vessel, this reactor can be controlled the condition elements such as pH, dissolved oxygen, temperature.Add the minimal medium that 8L presses embodiment 2 preparations in the homogeneous reaction device, add minimal medium and the 800g silicone master batch that 8L presses embodiment 2 preparations in the two-phase reactor.In reactor, add first H13 bacterium (deposit number: CCTCC No:M 2010121), make cell concentration reach 500 mg/L.。Then in reactor bottom, pass into the air that contains DCM, stirring reaction, keeping temperature in the running is 34 ℃, speed of agitator 400rpm, pH value 7.5(regulates with the NaOH of 1mol/L), the fermentating liquid volume 8L of time of staying 60s(homogeneous reaction device, at 8L/min, calculating the time of staying is 60s by spinner flowmeter control charge flow rate; The cumulative volume of two-phase reactor zymotic fluid and silicone master batch is 8.8L, and at 8.8L/min, calculating the time of staying is 60s by spinner flowmeter control charge flow rate).Change the 1L fresh culture every day, reactor operation 7 days.Import load in the course of reaction, outlet load, the comparative result of clearance and removal load is seen Fig. 2, and among Fig. 2, left figure is the homogeneous reaction device, and right figure is the two-phase reactor that adds 10% silicone master batch.Inlet concentration/the time of staying of import load=DCM among the figure, exit concentration/time of staying of corresponding outlet load=DCM, remove load=import load-outlet load, clearance=removal load/import load.Inlet concentration and exit concentration are to stay an air hatch at the air inlet of fermentation tank and gas outlet, and sampling is surveyed gas-chromatography and obtained.
Can find out among Fig. 2, originally the import of DCM load is 350 g/ (m in the homogeneous reaction device
3H) during the left and right sides, its clearance is removed load near 300 g/ (m about about 80%
3H); And when moving to the 6th day, its clearance is reduced to about 40% under the same terms, removes load reduction to 100 g/ (m
3H) about, the ability of DCM is removed in basic forfeiture.And the removal duty ratio common response device of two-phase separate reactor is high, and its clearance remains at about 90% in the whole service process.Although the two-phase separate reactor has only moved 7 days in the experiment, in fact can also continue operation, still can keep good removal capacity.
Change the inlet concentration of reactor, make it from 1000 mg/m
3Be increased to 5000 mg/m
3, keep 60min, more single-phase and two-phase reactor is resisted the ability that temporary impact is loaded.Import and export concentration, clearance, dissolved oxygen in the process and see over time Fig. 3.Among Fig. 3, left figure is the homogeneous reaction device, and right figure is the two-phase reactor that adds 10% silicone master batch.Fig. 3 can find out, when inlet concentration is increased to 5000 mg/m
3The time, exit concentration moment of common response device is from 160 mg/m
3Be increased to 2800 mg/m
3About, clearance drops to 40% by 90%.And two-phase reactor is under similar impact load, and exit concentration and clearance do not have significant change, and exit concentration is all the time at 500 mg/m
3Below, clearance is more than 85%.
Change the inlet concentration of reactor, by 2500 mg/m
3Be increased to 8500 g/ (m
3H), keep 60min, more single-phase and two-phase reactor is resisted the ability of instantaneous HI high impact load.Import and export concentration, clearance, dissolved oxygen in the process and see over time Fig. 4.Among Fig. 4, left figure is the homogeneous reaction device, and right figure is the two-phase reactor that adds 10% silicone master batch.Fig. 4 can find out, when inlet concentration is increased to 8000 mg/m
3The time, the exit concentration of homogeneous reaction device is by 400 mg/m
3Be increased to 6000 mg/m
3, clearance drops to 30% by 90%.The exit concentration of two-phase reactor is by 450 mg/m
3Be increased to 1650 mg/m
3, clearance drops to 80% by 90%.This shows that the two-phase reactor that adds silicone master batch has very large advantage at the opposing impact load, this is significant to overcoming the sudden variation (waste gas composition and the variation of concentration, the variation of gas velocity, the time-out of processing procedure etc.) that runs in the industrial treatment VOCs process.
Claims (5)
1. use the method that silicone master batch is processed degraded carrene waste gas for one kind, it is characterized in that described method is: in reactor, add minimal medium and silicone master batch, the consumption of silicone master batch is the 5-30 wt% of minimal medium quality, drop into Rhodesia methyl bacillus (Methylobacterium rhodesianum) H13 in the minimal medium, deposit number: CCTCC No:M 2010121, being cultured to cell concentration is 100-2000 mg/L, pass into the waste gas that contains carrene from reactor bottom to zymotic fluid, stirring reaction, keeping reaction temperature is 15-40 ℃, speed of agitator 200-600rpm, the pH value 5-9 of control reactant liquor, the time of staying 30-120s of waste gas in reactant liquor, outlet namely obtains the purified gas after the carrene degraded.
2. require 1 described method such as claim, it is characterized in that described minimal medium prepares by following composition: 4.5g Na
2HPO
412H
2O, 1.0g KH
2PO
4, 0.5g (NH
4)
2SO
4, 0.1g MgSO
47H
2O, 0.023g CaCl
2, 1mL trace element mother liquor, water complements to 1000mL; Described micro-mother liquid concentration consists of: FeSO
47H
2O 1.0 g/L, CuSO
45H
2O 0.02 g/L, H
3BO
30.014 g/L, MnSO
44H
2O 0.10 g/L, ZnSO
47H
2O 0.10 g/L, Na
2MoO
42H
2O 0.02 g/L, CoCl
26H
2O 0.02 g/L, solvent are water.
3. require 1 described method such as claim, it is characterized in that the fresh minimal medium of every operation replacing 10% ~ 15% in 24 hours.
4. requiring 1 described method such as claim, it is characterized in that described control pH value 5-9, is the NaOH adjust pH with 1mol/L.
5. the method for claim 1, it is characterized in that described method is: in reactor, add minimal medium and silicone master batch, the consumption of silicone master batch is the 10-20 % of minimal medium quality, drop into Rhodesia methyl bacillus (Methylobacterium rhodesianum) H13 in the minimal medium, deposit number: CCTCC No:M 2010121, being cultured to cell concentration is 500 ~ 550 mg/L, pass into the waste gas that contains carrene from reactor bottom to zymotic fluid, stirring reaction, keeping reaction temperature is 33 ~ 34 ℃, speed of agitator 200-600rpm, the pH value 7.5 of control reactant liquor, the time of staying 60 ~ the 80s of waste gas in reactant liquor, outlet namely obtains the purified gas after the carrene degraded.
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| CN115287246A (en) * | 2021-12-28 | 2022-11-04 | 浙江海洋大学 | Method for efficiently breeding hydrophobic VOC (volatile organic compounds) degrading bacteria |
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| CN101993839A (en) * | 2010-07-23 | 2011-03-30 | 浙江工业大学 | Methylobacterium rhodesianum H13 capable of efficiently degrading dichloromethane and application thereof |
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| CN101993839A (en) * | 2010-07-23 | 2011-03-30 | 浙江工业大学 | Methylobacterium rhodesianum H13 capable of efficiently degrading dichloromethane and application thereof |
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| Title |
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| 魏连爽等: "两相分配生物反应器治理高浓度有机污染研究进展", 《应用与环境生物学报》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115287246A (en) * | 2021-12-28 | 2022-11-04 | 浙江海洋大学 | Method for efficiently breeding hydrophobic VOC (volatile organic compounds) degrading bacteria |
| CN115287246B (en) * | 2021-12-28 | 2024-03-12 | 浙江海洋大学 | Method for efficiently breeding hydrophobic VOC degrading bacteria |
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