CN103721677A - Preparation method of biomass carbon composite material for removing phosphorus in wastewater - Google Patents
Preparation method of biomass carbon composite material for removing phosphorus in wastewater Download PDFInfo
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- CN103721677A CN103721677A CN201410013467.XA CN201410013467A CN103721677A CN 103721677 A CN103721677 A CN 103721677A CN 201410013467 A CN201410013467 A CN 201410013467A CN 103721677 A CN103721677 A CN 103721677A
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Abstract
The invention provides a preparation method of a biomass carbon composite material for removing phosphorus in wastewater. The preparation method comprises the steps of adding waste biomass into a metal salt solution to stir and mix evenly, then adding an alkali solution to continuously stir for 30-120 minutes, then performing hydrothermal carbonization, cooling a product to room temperature after reaction is ended, filtering, washing unreacted substances on the surface by using water and/or ethyl alcohol, then drying to constant weight at a temperature of 60-120 DEG C and sieving through a sieve with 40-180 meshes to obtain the biomass carbon composite material. According to the preparation method, the waste biomass serves as the raw material, so that the preparation method is low in cost; due to the adoption of hydrothermal carbonization, the preparation method is warm in reaction condition and simple in whole preparation process; and the prepared biomass carbon composite material is good in stability and efficient in phosphorus removal effect.
Description
Technical field
The invention belongs to sorbing material technical field, relate to a kind of preparation method of biomass carbon composite, particularly a kind of method that adopts hydrothermal carbonization legal system to be ready for use on the biomass carbon composite of waste water dephosphorization.
Background technology
Phosphorus is the one of the chief elements that causes body eutrophication, controls P elements than controlling nitrogen element and more can effectively control body eutrophication, the water body being polluted by phosphorus, algal bloom, dissolved oxygen falls sharply, and water quality fouls, and has a strong impact on the hydrobiological existence such as fish; Phosphorus is also the stable restriction factor of water distribution system water quality biological, and its removal in giving water treatment also receives increasing concern.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, when removing the phosphorus in water, recycled, will be had important Significance for Environment.Conventional biological dephosphorization and chemical dephosphorization method exist operating condition strict, produce secondary pollution and can not reclaim the shortcomings such as phosphor resource, and absorption method is because floor space is little, technique is simple, easy to operate, be easy to phosphorus recovery and extremely people pay close attention to.
Adsorbent is comparatively extensive in removal and the application aspect recovery of phosphorus, but traditional adsorbent is often received phosphorus back and forth by chemical deposition and desorb, this has caused lower phosphorus organic efficiency, but biomass carbon composite can directly be used for agricultural production as phosphate fertilizer after phosphorus absorption, also can obtain by burning the phosphate ash content of high concentration, thereby realize the recovery of phosphorus.
Hydrothermal carbonization is that the heat chemistry of living beings under the pressure condition of relatively mild temperature and steam formation changes.Although hydrothermal carbonization is aspect the preparation of the materials such as solid material with carbon element, catalyst, fuel cell, bio-imaging, drug delivery, sensor and water treatment in recent years, and be used widely aspect the high heating value transformation of abandoned biomass (as stalk, changing food waste etc.), but the application aspect preparing has not yet to see report at dephosphorization material.The elements such as calcium, iron, magnesium, aluminium and lanthanum have obtained a large amount of application in the preparation of efficient phosphorus sorbing material, in at present efficient phosphorus sorbing material, mixing of these elements is mainly by biomass high-temperature thermal cracking, yet high temperature pyrolytic cracking exists, reaction temperature is high, condition is harsh,, high in cost of production defect high to equipment requirement.
Summary of the invention
The object of the invention is the problem existing for prior art, provide that a kind of reaction condition is gentle, preparation technology is simple, with low cost, good stability, there is the preparation method of the biomass carbon composite of controllability.This preparation method comprises abandoned biomass is joined in metal salt solution, stir and evenly mix, then add aqueous slkali, continue to stir 30-120min, it is fully reacted, then carry out hydrothermal carbonization, after question response is complete, products therefrom is cooled to room temperature, suction filtration, water and/or ethanol wash away surperficial unreacting substance again, then under 60-120 ℃ of temperature conditions, be dried to constant weight, cross 40-180 mesh sieve, obtain.
The present invention is by joining abandoned biomass in metal salt solution and soak, after fully soaking, add again aqueous slkali, thereby realize hydroxide in the load on living beings surface, hydrothermal carbonization load the surface of biomass carbon of hydroxide possess abundant oxy radical, and some metallic elements have higher affinity to these oxy radicals, therefore the surface that these metallic elements can mix biomass carbon, forms composite, can synchronously realize carbonization and the functionalization of living beings.
Preferably, the temperature of hydrothermal carbonization is 140-280 ℃, and the time is 4-48 hour.
Preferably, described abandoned biomass is with the m/v of metal salt solution than being 5-20%, and the concentration of metal salt solution is 0.01-0.2mol/L, to prepare the biological carbon composite that contains best metal element ratio by hydrothermal carbonization.
Preferably, the volume ratio of described aqueous slkali and metal salt solution is 1-25%, and the concentration of aqueous slkali is 1-6mol/L, and the volume ratio of metal salt solution of the present invention and aqueous slkali is comparatively suitable, can make metal ion all form hydroxide.
Preferably, the metallic element in described metal salt solution is at least one in iron, aluminium, calcium, magnesium and lanthanum.The metallic elements such as iron, aluminium, calcium, magnesium and lanthanum possess abundant oxy radical to the surface of biomass carbon and have higher affinity, so these elements can mix the surface of biomass carbon, formation composite.
Preferably, described abandoned biomass is selected from least one in agricultural wastes, forestry waste, breeding waste and changing food waste.Abandoned biomass wide material sources, cheap, can greatly reduce the cost of this composite.
The biomass carbon composite that another object of the present invention provides a kind of above-mentioned preparation method to make.
Another object of the present invention is to provide the application of above-mentioned biomass carbon composite in waste water dephosphorization.
Preferably, described application is in waste water, to add biomass carbon composite described in 1-5 g/L, and adsorption time is 2-24 hour.
Preferably, described application be collect adsorbed phosphorus biomass carbon composite as phosphate fertilizer for agricultural production, or burn, remove organic moiety, obtain the ash content of high phosphate content, thereby realize the recovery of phosphorus.
The present invention compared with prior art, has following remarkable advantage:
The present invention adopts abandoned biomass as raw material, and wide material sources are with low cost; Adopt hydrothermal carbonization legal system for biomass carbon composite, reaction condition is gentle, environmental protection; Preparation process is simple, and good stability operates controlledly, can realize industrialization.The biomass carbon composite that the present invention makes has efficient phosphor-removing effect, and under alkalescence or anion existence condition, the phosphorus removal property range of decrease is faint, is significantly better than traditional dephosphorization material.The biomass carbon composite that has adsorbed phosphorus can be used as phosphate fertilizer for agricultural production, or burns, and removes organic moiety, obtains the ash content of high phosphate content, thereby realizes effective recovery of phosphorus.
accompanying drawing explanation:
Fig. 1 is the SEM figure of prepared biomass carbon composite in embodiment 1;
Fig. 2 is the FTIR spectrogram of prepared biomass carbon composite in embodiment 1;
Fig. 3 is the XRD figure of prepared biomass carbon composite in embodiment 1.
The specific embodiment
Below by embodiment, the present invention is specifically described; be necessary to be pointed out that at this following examples are just for being further detailed the present invention; can not be interpreted as limiting the scope of the invention; some nonessential improvement and adjustment that the person skilled in the art in this field makes according to foregoing invention content, still belong to protection scope of the present invention.
The preparation of biomass composite:
Embodiment 1
The LaCl that adds 30mL 0.01M in the polytetrafluoroethyltank tank of 50 mL
3solution, then add 1.5g rice straw, fully stir after 30min, add 0.3mL 1M KOH, continue to stir 30min, finally at 140 ℃ of hot carbonization 4h of Water Under.After hydrothermal carbonization completes, hydrothermal reaction kettle is taken out from baking oven, in air, be cooled to room temperature, with 0.45 μ m filter membrane, products therefrom is filtered, with deionized water and ethanol, respectively clean 2 times respectively again, then under 60 ℃ of conditions, dry to constant weight, cross 40 mesh sieves standby.
Embodiment 2
The LaCl that adds 30 mL 0.1 M in the polytetrafluoroethyltank tank of 50 mL
3solution, then add 4.5 g rice straws, adds 4.5 mL 3M KOH after fully stirring 30 min, continues to stir 80 min, finally 200 ℃ of hot carbonizations of Water Under 30 hours.After hydrothermal carbonization completes, hydrothermal reaction kettle is taken out from baking oven, in air, be cooled to room temperature, with 0.45 μ m filter membrane, products therefrom is filtered, with deionized water and ethanol, respectively clean 2 times respectively again, then under 105 ℃ of conditions, dry to constant weight, cross 120 mesh sieves standby.
Embodiment 3
The CaCl that adds 30mL 0.2 M in the polytetrafluoroethyltank tank of 50 mL
2solution, then add 6g garbage, adds 7.5 mL 6M KOH after fully stirring 30min, continues to stir 120min, finally 280 ℃ of hot carbonizations of Water Under 48 hours.After hydrothermal carbonization completes, hydrothermal reaction kettle is taken out from baking oven, in air, be cooled to room temperature, with 0.45 μ m filter membrane, products therefrom is filtered, with deionized water and ethanol, respectively clean 2 times respectively again, then under 120 ℃ of conditions, dry to constant weight, cross 180 mesh sieves standby.
Application examples 1
The removal of the biomass carbon composite that under condition of different pH, embodiment 1 makes to phosphorus
In 5 50mL polyethylene centrifuge tubes, add 0.03g biomass carbon composite respectively, then add 30mL 100 mg P/L KH
2pO
4solution, pH is adjusted to respectively 2.5,4.5,6.5,8.5 and 10.5, the 24h that vibrates under the condition of 25 ℃ and 150 rpm, then with 0.45 μ m filter membrane, suspension is filtered, gained filtrate is for phosphate determination.Before and after reaction, the difference of phosphate concn 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, the biological carbon composite that embodiment 1 makes can efficiently be removed the phosphorus in water body, although its ability decreases under alkali condition, compare with traditional dephosphorization material, its range of decrease is lower, can efficient dephosphorization within the scope of wider pH.
Phosphorus adsorbance and the clearance of biological carbon composite 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 removal of the biomass carbon composite that under different anions existence condition, embodiment 1 makes to phosphorus
Configure respectively KCl, the K of 0.01M
2sO
4, KNO
3with KH
2pO
4mixed solution and KCl, the K of 0.1M
2sO
4, KNO3 and KH
2pO
4mixed solution, phosphorus concentration is 100mg P/L, then in 6 50mL polyethylene centrifuge tubes, adds 0.03g biomass carbon composite respectively, wherein 3 add respectively 30mL0.01M KCl, K
2sO
4and KNO
3100 mg P/L KH
2pO
4mixed solution, other 3 add respectively 30mL 0.1M KCl, K
2sO
4and KNO
3100 mg P/L KH
2pO
4mixed solution, the 24h that vibrates under the condition of 25 ℃ and 150rpm, then with 0.45 μ m filter membrane, suspension is filtered, gained filtrate is used for phosphate determination.Biological carbon composite is not adding the KH of anion
2pO
4absorption in solution is processed in contrast.Before and after reaction, the difference of phosphate concn is for calculating composite to the adsorbance of phosphorus and clearance.Result from table 2 can find out, the competition anion of higher concentration and low concentration can not obviously weaken biological carbon composite to phosphatic adsorption effect, illustrates that this material has the selective of height to phosphatic absorption.
Phosphorus adsorbance and the clearance of biomass carbon composite under table 2 different anions existence condition
Claims (10)
1. for a preparation method for the biomass carbon composite of waste water dephosphorization, it is characterized in that, this preparation method comprises abandoned biomass is joined in metal salt solution, stir and evenly mix, add again aqueous slkali, continue to stir 30-120min, then carry out hydrothermal carbonization, after question response is complete, products therefrom is cooled to room temperature, suction filtration, then water and/or ethanol washes away surperficial unreacting substance, then under 60-120 ℃ of temperature conditions, is dried to constant weight, cross 40-180 mesh sieve, obtain.
2. the preparation method of biomass carbon composite according to claim 1, is characterized in that, the temperature of hydrothermal carbonization is 140-280 ℃, and the time is 4-48 hour.
3. the preparation method of biomass carbon composite according to claim 1 and 2, is characterized in that, described abandoned biomass is with the m/v of metal salt solution than being 5-20%, and the concentration of metal salt solution is 0.01-0.2mol/L.
4. according to the preparation method of biomass carbon composite according to claim 3, it is characterized in that, the volume ratio of described aqueous slkali and metal salt solution is 1-25%, and the concentration of aqueous slkali is 1-6mol/L.
5. the preparation method of biomass carbon composite according to claim 1 and 2, is characterized in that, the metallic element in described metal salt solution is at least one in iron, aluminium, calcium, magnesium and lanthanum.
6. the preparation method of biomass carbon composite according to claim 1 and 2, is characterized in that, described abandoned biomass is selected from least one in agricultural wastes, forestry waste, breeding waste and changing food waste.
7. the biomass carbon composite making according to the preparation method described in any one in claim 1-6.
8. the application of biomass carbon composite according to claim 7 in waste water dephosphorization.
9. application according to claim 8, is characterized in that, to adding biomass carbon composite described in 1-5 g/L in waste water, adsorption time is 2-24 hour.
10. application according to claim 8 or claim 9, is characterized in that, collect adsorbed phosphorus biomass carbon composite as phosphate fertilizer for agricultural production, or burn.
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| CN116903414A (en) * | 2023-09-13 | 2023-10-20 | 江苏省农业科学院 | Automatic conditioner capable of continuously treating agricultural non-point source phosphorus pollution and preparation method and application thereof |
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