CN103721677B - A kind of preparation method of the biomass carbon composite for waste water dephosphorization - Google Patents
A kind of preparation method of the biomass carbon composite for waste water dephosphorization Download PDFInfo
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- CN103721677B CN103721677B CN201410013467.XA CN201410013467A CN103721677B CN 103721677 B CN103721677 B CN 103721677B CN 201410013467 A CN201410013467 A CN 201410013467A CN 103721677 B CN103721677 B CN 103721677B
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Abstract
The present invention provides the preparation method of a kind of biomass carbon composite for waste water dephosphorization, this preparation method includes joining in metal salt solution by abandoned biomass, and stirring and evenly mixing adds aqueous slkali, continue stirring 30 120min, then carry out hydrothermal carbonization, after question response is complete, products therefrom is cooled to room temperature, sucking filtration, surface unreacting substance is washed away again with water and/or ethanol, then it is dried under 60 120 DEG C of temperature conditionss to constant weight, crosses 40 180 mesh sieves, to obtain final product.The preparation method of the present invention is with abandoned biomass as raw material, with low cost, uses hydrothermal carbonization method reaction condition gentle, and whole preparation process is simple, it is thus achieved that biomass carbon composite good stability, there is efficient phosphor-removing effect.
Description
Technical field
The invention belongs to adsorbing material technical field, relate to the preparation method of a kind of biomass carbon composite, relate to especially
And a kind of method of the biomass carbon composite using hydrothermal carbonization legal system to be ready for use on waste water dephosphorization.
Background technology
Phosphorus is the one of the chief elements causing body eutrophication, controls P elements and more can effectively control than controlling nitrogen element
Body eutrophication processed, the water body polluted by phosphorus, algal bloom, dissolved oxygen falls sharply, and water quality fouls, and has a strong impact on Fish etc.
Hydrobiological existence；Phosphorus is also the restriction factor that water distribution system water quality biological is stable, and its removal in Water purification is also subject to
Pay close attention to increasing.On the other hand, phosphorus is one-way flow in biosphere, and a large amount of consumption of phosphorus will make phosphorus become valuable
Scarce resource.Therefore, recycled while removing the phosphorus in water, will be had important Significance for Environment.Conventional biology removes
Phosphorus method and chemical dephosphorization method exist that operating condition is strict, produce secondary pollution and can not reclaim the shortcomings such as phosphor resource, and adsorb
Method is little due to floor space, and technique is simple, easy to operate, it is easy to the recovery of phosphorus and extremely people pay close attention to.
Adsorbent application in terms of the removal and recovery of phosphorus is relatively broad, but traditional adsorbent sinks often through chemistry
Phosphorus is received in long-pending and desorbing back and forth, which results in relatively low phosphorus organic efficiency, but biomass carbon composite can be straight after phosphorus adsorbs
Connect as phosphate fertilizer for agricultural production, it is also possible to obtained the phosphate ash of high concentration by burning, thus realize returning of phosphorus
Receive.
Hydrothermal carbonization is biomass heat chemistry changes under the pressure condition that relatively mild temperature and steam are formed.Closely
Although hydrothermal carbonization is in carbon sequestration material, catalyst, fuel cell, bio-imaging, drug delivery, sensor and water process etc. over Nian
The preparation aspect of material, and be used widely in terms of the high heating value transformation of abandoned biomass (such as straw, changing food waste etc.),
But the application preparing aspect at dephosphorization material has not yet to see report.The elements such as calcium, ferrum, magnesium, aluminum and lanthanum are at efficient phosphorus adsorbing material
Having obtained substantial amounts of application in preparation, the most efficiently in phosphorus adsorbing material, mixing of these elements mainly passes through biomass high-temperature
Thermal cracking, but high temperature pyrolytic cracking exists, and reaction temperature is high, condition is harsh, high in cost of production defect high to equipment requirements.
Summary of the invention
The problem that it is an object of the invention to exist for prior art, it is provided that a kind of reaction condition is gentle, preparation technology letter
Single, with low cost, good stability, there is the preparation method of the biomass carbon composite of controllability.This preparation method include by
Abandoned biomass joins in metal salt solution, stirring and evenly mixing, adds aqueous slkali, continues stirring 30-120min so that it is fully
Reaction, then carries out hydrothermal carbonization, products therefrom is cooled to after question response is complete room temperature, sucking filtration, then washes with water and/or ethanol
Remove surface unreacting substance, be then dried under 60-120 DEG C of temperature conditions to constant weight, cross 40-180 mesh sieve, to obtain final product.
The present invention soaks by being joined by abandoned biomass in metal salt solution, adds aqueous slkali after fully soaking,
Thus realizing the hydroxide load at biological surface, the surface of the biomass carbon that hydrothermal carbonization has loaded hydroxide possesses
Abundant oxy radical, and some metallic elements have higher affinity to these oxy radicals, therefore these metallic elements
The surface of biomass carbon can be mixed, form composite, can synchronize to realize carbonization and the functionalization of biomass.
Preferably, the temperature of hydrothermal carbonization is 140-280 DEG C, and the time is 4-48 hour.
Preferably, the m/v of described abandoned biomass and metal salt solution is than for 5-20%, and the concentration of metal salt solution is
0.01-0.2mol/L, to contain the biological carbon composite of best metal element ratio by hydrothermal carbonization preparation.
Preferably, described aqueous slkali is 1-25% with the volume ratio of metal salt solution, and the concentration of aqueous slkali is 1-6mol/L,
Metal salt solution of the present invention is the most suitable with the volume ratio of aqueous slkali, it is possible to make metal ion be completely formed hydroxide
Thing.
Preferably, the described metallic element in metal salt solution is at least one in ferrum, aluminum, calcium, magnesium and lanthanum.Ferrum,
The metallic elements such as aluminum, calcium, magnesium and lanthanum possess abundant oxy radical and have higher affinity, therefore the surface of biomass carbon
These elements can mix the surface of biomass carbon, forms composite.
Preferably, described abandoned biomass is in agricultural wastes, forestry waste, breeding waste and changing food waste
At least one.Abandoned biomass wide material sources, cheap, the cost of this composite can be substantially reduced.
Another object of the present invention provides the biomass carbon composite that a kind of above-mentioned preparation method prepares.
A further object of the present invention is to provide the application in waste water dephosphorization of the above-mentioned biomass carbon composite.
Preferably, described application is to add biomass carbon composite described in 1-5 g/L in waste water, and adsorption time is
2-24 hour.
Preferably, described application is that the biomass carbon composite collected and adsorbed phosphorus is raw for agricultural as phosphate fertilizer
Produce, or burn, remove organic moiety, obtain the ash of high phosphate levels, thus realize the recovery of phosphorus.
The present invention compared with prior art, has a following remarkable advantage:
The present invention use abandoned biomass as raw material, wide material sources, with low cost；Use hydrothermal carbonization method preparation biology
Matter carbon composite, reaction condition is gentle, environmental protection；Preparation process is simple, and good stability operates controlled, can realize
Industrialization.The biomass carbon composite that the present invention prepares has efficient phosphor-removing effect, and there is bar in alkalescence or anion
Under part, the phosphorus removal property range of decrease is faint, is significantly better than traditional dephosphorization material.The biomass carbon composite having adsorbed phosphorus can conduct
Phosphate fertilizer is used for agricultural production, or burns, and removes organic moiety, obtains the ash of high phosphate levels, thus realize
The efficient recovery of phosphorus.
Accompanying drawing illustrates:
Fig. 1 is the SEM figure of prepared biomass carbon composite in embodiment 1；
Fig. 2 is the FTIR spectrum figure of prepared biomass carbon composite in embodiment 1；
Fig. 3 is the XRD figure of prepared biomass carbon composite in embodiment 1.
Detailed description of the invention
Below by embodiment, the present invention is specifically described, it is necessary to it is pointed out here that be that following example are simply used
In the present invention is further detailed, it is impossible to be interpreted as limiting the scope of the invention, being skilled in technique of this field
Some nonessential improvement and adjustment that personnel are made according to foregoing invention content, still fall within protection scope of the present invention.
The preparation of biomass composite:
Embodiment 1
The LaCl of 30mL 0.01M is added in the polytetrafluoroethyltank tank of 50 mL3Solution, adds 1.5g rice straw,
After being sufficiently stirred for 30min, add 0.3mL 1M KOH, continue stirring 30min, finally hydrothermal carbonization 4h under the conditions of 140 DEG C.Hydro-thermal
After carbonization completes, hydrothermal reaction kettle is taken out from baking oven, be cooled to room temperature in atmosphere, with 0.45 μm filter membrane to products therefrom
Filter, respectively clean 2 times with deionized water and ethanol respectively, then dry under the conditions of 60 DEG C to constant weight, cross 40 mesh sieves
Standby.
Embodiment 2
The LaCl of 30 mL 0.1 M is added in the polytetrafluoroethyltank tank of 50 mL3Solution, adds 4.5 g Oryza sativa L. straw
Stalk, adds 4.5 mL 3M KOH after being sufficiently stirred for 30 min, continue stirring 80 min, finally hydrothermal carbonization under the conditions of 200 DEG C
30 hours.After hydrothermal carbonization completes, hydrothermal reaction kettle is taken out from baking oven, be cooled to room temperature in atmosphere, with 0.45 μm filter
Products therefrom is filtered by film, respectively cleans 2 times with deionized water and ethanol respectively, then dry under the conditions of 105 DEG C to
Constant weight, crosses 120 mesh sieves standby.
Embodiment 3
The CaCl of 30mL 0.2 M is added in the polytetrafluoroethyltank tank of 50 mL2Solution, adds 6g garbage, fills
Adding 7.5 mL 6M KOH after dividing stirring 30min, continue stirring 120min, finally under the conditions of 280 DEG C, hydrothermal carbonization 48 is little
Time.After hydrothermal carbonization completes, hydrothermal reaction kettle is taken out from baking oven, be cooled to room temperature in atmosphere, with 0.45 μm filter membrane pair
Products therefrom filters, respectively cleans 2 times with deionized water and ethanol respectively, then dries to constant weight under the conditions of 120 DEG C,
Cross 180 mesh sieves standby.
Application examples 1
The biomass carbon composite that under condition of different pH, embodiment 1 the prepares removal to phosphorus
In 5 50mL polyethylene centrifuge tube, add 0.03g biomass carbon composite respectively, add 30mL 100
mg P/L KH2PO4Solution, pH is adjusted to 2.5,4.5,6.5,8.5 and 10.5 respectively, shakes under conditions of 25 DEG C and 150 rpm
Swinging 24h, then filter suspension with 0.45 μm filter membrane, gained filtrate is used for phosphate determination.Before and after reaction, phosphate is dense
The difference of degree is for calculating composite to the adsorbance of phosphorus and clearance.As can be seen from Table 1, in the scope of pH2.5-10.5
In, the biological carbon composite that embodiment 1 prepares can efficiently remove the phosphorus in water body, although its ability has in the basic conditions
Being reduced, compared with traditional dephosphorization material, its range of decrease is relatively low, can efficient dephosphorization in the range of wider pH.
The phosphorus adsorbance of biological carbon composite and clearance under table 1 condition of different pH
| pH | 2.5 | 4.5 | 6.5 | 8.5 | 10.5 |
| Adsorbance (mg/g) | 58.244 | 60.76 | 57.79 | 53.50 | 51.64 |
| Clearance (%) | 58.244 | 60.76 | 57.79 | 53.50 | 51.64 |
Application examples 2
The biomass carbon composite that under different anions existence condition, embodiment 1 the prepares removal to phosphorus
It is respectively configured KCl, K of 0.01M2SO4、KNO3With KH2PO4 Mixed solution and KCl, K of 0.1M2SO4、KNO3
With KH2PO4 Mixed solution, phosphorus concentration is 100mg P/L, the most respectively in 6 50mL polyethylene centrifuge tube add 0.03g
Biomass carbon composite, wherein 3 are separately added into 30mL0.01M KCl, K2SO4And KNO3100 mg P/L KH2PO4Mixed
Closing solution, other 3 are separately added into 30mL 0.1M KCl, K2SO4And KNO3100 mg P/L KH2PO4Mixed solution, 25
DEG C and 150rpm under conditions of vibrate 24h, then with 0.45 μm filter membrane, suspension is filtered, gained filtrate is for phosphate survey
Fixed.Biological carbon composite is not adding the KH of anion2PO4Absorption in solution is as control treatment.Phosphoric acid before and after reaction
The difference of salinity is for calculating composite to the adsorbance of phosphorus and clearance.It can be seen from the results in table 2 it is more highly concentrated
The competition anion of degree and low concentration can not substantially weaken biological carbon composite to phosphatic adsorption effect, explanation
This material has the selectivity of height to phosphatic absorption.
The phosphorus adsorbance of biomass carbon composite and clearance under table 2 different anions existence condition
Claims (7)
1. the preparation method for the biomass carbon composite of waste water dephosphorization, it is characterised in that this preparation method includes
Abandoned biomass is joined in metal salt solution, stirring and evenly mixing, add aqueous slkali, continue stirring 30-120min, then enter
Row hydrothermal carbonization, is cooled to products therefrom room temperature, sucking filtration, then it is the most anti-to wash away surface with water and/or ethanol after question response is complete
Answer material, be then dried under 60-120 DEG C of temperature conditions to constant weight, cross 40-180 mesh sieve, to obtain final product；Wherein, described waste biomass
The m/v of matter and metal salt solution is than for 5-20:100g/mL, and the concentration of metal salt solution is 0.01-0.2mol/L；Described alkali is molten
Liquid is 1-25:100 with the volume ratio of metal salt solution, and the concentration of aqueous slkali is 1-6mol/L；Described abandoned biomass is selected from agriculture
At least one in industry garbage, forestry waste, breeding waste and changing food waste.
The preparation method of biomass carbon composite the most according to claim 1, it is characterised in that the temperature of hydrothermal carbonization
For 140-280 DEG C, the time is 4-48 hour.
The preparation method of biomass carbon composite the most according to claim 1 and 2, it is characterised in that described metal
Metallic element in saline solution is at least one in ferrum, aluminum, calcium, magnesium and lanthanum.
4. the biomass carbon composite prepared according to the preparation method according to any one of claim 1-3.
The biomass carbon composite the most according to claim 4 application in waste water dephosphorization.
Application the most according to claim 5, it is characterised in that add biomass carbon composite wood described in 1-5g/L in waste water
Material, adsorption time is 2-24 hour.
7. according to the application described in claim 5 or 6, it is characterised in that collect the biomass carbon composite work having adsorbed phosphorus
For phosphate fertilizer for agricultural production, or burn.
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