CN110270310A - A kind of synchronous high-efficiency recycles the preparation method and applications of the rich magnesium charcoal of nitrogen and phosphorus nutrient in farm's waste liquid - Google Patents
A kind of synchronous high-efficiency recycles the preparation method and applications of the rich magnesium charcoal of nitrogen and phosphorus nutrient in farm's waste liquid Download PDFInfo
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- CN110270310A CN110270310A CN201910678241.4A CN201910678241A CN110270310A CN 110270310 A CN110270310 A CN 110270310A CN 201910678241 A CN201910678241 A CN 201910678241A CN 110270310 A CN110270310 A CN 110270310A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D3/00—Calcareous fertilisers
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/20—Nature of the water, waste water, sewage or sludge to be treated from animal husbandry
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
Abstract
The invention discloses the preparation method and applications of the rich magnesium charcoal of nitrogen and phosphorus nutrient in a kind of synchronous high-efficiency recycling farm's waste liquid.The preparation method of the rich magnesium charcoal of nitrogen and phosphorus nutrient in a kind of synchronous high-efficiency recycling farm's waste liquid of the invention, include the following steps: that (1) powdered biomass is added in magnesium chloride solution to mix well, has been dispersed the magnesium chloride solution of biomass after mixing through microwave treatment；(2) then above-mentioned solution is stirred after a certain period of time, filtering, drying obtain rich magnesium biomass；Finally rich magnesium biomass is transferred in anoxic atmosphere, thermal cracking under the conditions of 450-700 DEG C of temperature, the rich magnesium charcoal of nitrogen and phosphorus nutrient in synchronous high-efficiency recycling farm's waste liquid is made.Gained Carbon Materials of the invention, which can not only be realized, recycles the synchronous high-efficiency of nitrogen and phosphorus nutrient in farm's waste liquid, and recycling the charcoal fertilizer after nitrogen phosphorus is the control slow release fertilizer that a kind of pair of soil has improving effect.
Description
Technical field
Waste biologic recycling belonging to the present invention utilizes and the technical field of green agriculture, and in particular to a kind of to synchronize height
The preparation method and applications of the rich magnesium charcoal of nitrogen and phosphorus nutrient in effect recycling farm's waste liquid.
Technical background
The scale and intensivization development of farm in recent years makes livestock and poultry feces become the main next of agricultural non-point source pollution
Source.Although as the popularization construction of biogas project, the organic carbon in livestock and poultry feces is converted to clean energy resource by anaerobic fermentation
CH4, but a large amount of nitrogen, phosphorus substance are still with NH4 +、NO3 -And PO4 3-Form remain in biogas slurry.The unprocessed direct emission of biogas slurry
It can aggravate environmental degradation, and the new source of current agricultural non-point source pollution.In particular, the excess of Water phosphorus substance can accelerate
The outburst of hydration phenomena, constitutes a serious threat to the ecosystem and aquatic animals and plants.However, nitrogen, phosphorus are also to promote crops raw
Long required nutrient.If the nitrogen, phosphorus in polluted-water are used appropriately, it can not only reduce the wasting of resources, promote nature
Good nutrient cycle in boundary, moreover it is possible to alleviate environmental problem caused by the unbalanced accumulation of nitrogen phosphorus.Therefore, it finds and develops and is rationally effective
Method, realize most important to the synchronous recycling of nitrogen in polluted-water, phosphorus nutrient.
Charcoal is the new material of exploitation during agricultural wastes resource utilization, in environmental contaminants reparation and soil
Earth improvement aspect all has huge application potential.However, charcoal is because of surface OH rich in-Equal negative electrical charges, to phosphorus
Absorption property is poor, while pure charcoal itself is also relatively weak to the absorption of nitrogen.It therefore, can be effective by functional modification
The structure and surface characteristic for improving charcoal, to improve charcoal to the absorption property of phosphorus.Such as Chinese patent CN
108636351 A, it is entitled " it is a kind of for phosphorus-containing wastewater or the adsorbent of eutrophication water dephosphorization and preparation method thereof with answer
With ", the adsorption capacity to phosphorus is improved using the loaded modified reed charcoal of iron chloride.Although the material can be effectively in adsorbed water body
Phosphorus, but ferric ion can be converted to ferrous ion and dissolve in practical applications, to lose adsorption capacity；And
Have no that the patented technology improves absorption of the biological carbon materials to nitrogen.For another example 109169572 A of patent CN, a kind of entitled " use
The preparation method of the magnesium-modified charcoal of nitrogen P elements in recycling urine ", is prepared using magnesium acetate modified peanut and sawdust
Magnesium-modified charcoal, the recycling for nitrogen P elements in urine.The magnesium-modified biological carbon materials of patented technology method preparation exist
It is almost nil to the absorption of nitrogen in the actual use of urine, guanite ingredient is not detected, only generates magnesium phosphate crystallization, and
It is also only 30.1% to the removal rate of phosphorus；In addition, biological carbon materials are fired using Muffle furnace in this method, due to that cannot be formed
Stringent anaerobic environment easily causes the volatilization of organic carbon constituents to burn, so that ideal biological carbon structure cannot be obtained, influences
Material property.It can be seen that lack in the prior art effective method of modifying and can synchronize recycling Water and phosphorus support
The biological carbon materials divided.In particular, even more requiring material pair for this constituents such as biogas slurry multiplicity, complicated farm's waste liquid
Nitrogen phosphorus composition all has higher recycling ability.
China is the maximum country of agricultural wastes quantum of output in the world, but since its Processes For Effective Conversion is few, comprehensive benefit
With low efficiency, environmental pollution is easily caused while causing resource largely to waste, especially because of crop straw burning bring environmental problem,
Seem in recent years especially prominent.Therefore, the technology of the present invention is alleviating agricultural non-point source pollution, is promoting stalk and feces of farm waste liquid
Innoxious use, nutrient benign cycle and the exploitation of new slow release fertilizer etc. all have significance.
Summary of the invention
For effective material is lacked at present, nitrogen and phosphorus nutrient in farm's waste liquid can be recycled simultaneously and is being returned
It is used as slow release fertilizer to be used for agricultural planting after receiving nitrogen phosphorus, the present invention provides a kind of prepare using cheap agricultural biomass can be simultaneously
Recycle the preparation method and applications of the biological carbon materials of nitrogen and phosphorus nutrient in farm's waste liquid.
To achieve the goals above, the present invention is achieved through the following technical solutions: a kind of synchronous high-efficiency recycling of the invention
The preparation method of the rich magnesium charcoal of nitrogen and phosphorus nutrient, includes the following steps: that (1) powdered biomass is added in farm's waste liquid
It is mixed well in magnesium chloride solution, has been dispersed the magnesium chloride solution of biomass after mixing through microwave treatment；
(2) then above-mentioned solution is stirred after a certain period of time, filtering, drying obtain rich magnesium biomass；It is finally that rich magnesium is raw
Substance is transferred in anoxic atmosphere, thermal cracking under the conditions of 450-700 DEG C of temperature, is made in synchronous high-efficiency recycling farm's waste liquid
The rich magnesium charcoal of nitrogen and phosphorus nutrient.
Further, in step (1), the dry powdered biomass of 1-10g microwave-assisted dipping: is added to 100mL
Concentration is to handle 5-30min after mixing well in microwave environment, and continue at 300- in the magnesium chloride solution of 1-4mol/L
500rpm magnetic agitation 1-8h obtains the biomass mixed solution for being sufficiently impregnated magnesium chloride；
In step (2), thermal cracking: the resulting biomass solution for being sufficiently impregnated magnesium chloride of step (1) is filtered, filtering
Object is dried under the conditions of 80-105 DEG C of temperature, and is transferred in anoxic atmosphere, is warming up at 450-700 DEG C with 10-15 DEG C/min
It is pyrolyzed 1-3h, the rich magnesium charcoal of nitrogen and phosphorus nutrient in synchronous high-efficiency recycling farm's waste liquid is made.
Further, in step (1), the powdered biomass is one of lignocellulose-like biomass or several
The mixed-powder of kind；Lignocellulose-like biomass powder is lignocellulose-like biomass by 60-105 DEG C of drying, crushing
And the sieving powder sieved with 100 mesh sieve.
Further, in step (1), the lignocellulose-like biomass be corn stover, corncob, rice husk,
Any one in wheat stalk, bagasse, sawdust, maize leaves, rice straw, broomcorn straw, cotton stalk or soybean stalk
Or several combination.
Further, in step (1), the magnesium chloride solution of the 1-4mol/L is by MgCl2·6H2O is dissolved in water system
?.
Further, in step (1), the microwave environment microwave frequency is 2.45GHz, microwave power 100-
800W。
The rich magnesium charcoal that preparation method of the present invention prepares.
Application of the rich magnesium charcoal of the present invention in farm's waste liquid in synchronous recycling nitrogen and phosphorus nutrient.
Rich magnesium charcoal of the present invention is used as control sustained release charcoal after synchronous recycling nitrogen and phosphorus nutrient in farm's waste liquid
The application of fertilizer.
Further, farm's waste liquid is for the liquid after livestock and poultry feces separation of solid and liquid and by various waste biogas
The biogas slurry obtained after fermentation.
The utility model has the advantages that it is raw materials used from a wealth of sources, cheap and easy to get in the present invention, it is that a kind of controllability is strong, easy to operate
Preparation method.Gained Carbon Materials of the invention, which can not only be realized, recycles the synchronous high-efficiency of nitrogen and phosphorus nutrient in farm's waste liquid,
And recycling the charcoal fertilizer after nitrogen phosphorus is the control slow release fertilizer that a kind of pair of soil has improving effect, in environmental improvement and soil
Reparation field has broad application prospects.
Compared with the prior art, the invention has the following advantages:
(1) present invention is directed to the agricultural biomass (lignocellulose) from plant, especially stalk biomass,
The charcoal fertilizer formed after rich magnesium charcoal recycling nitrogen phosphorus can be used for agricultural planting, on the one hand a variety of rich in C, N, P and Mg etc.
Plant growth element, on the other hand these nutrients can slowly be discharged from the cellular structure of charcoal fertilizer, reach slow
The effect released.In addition, charcoal itself also has the advantages that improvement soil, improvement plant rhizosphere environment.Therefore, the technology of the present invention exists
The fields such as stover, water pollution control and green agriculture are promoted to all have wide application prospect.
(2) the rich magnesium charcoal of the method for the present invention preparation, has a performance of synchronous recycling Water and phosphorus, especially pair
The biogas slurry of feces of farm filtered fluid and separate sources all has higher synchronous nitrogen and phosphorus recovery efficiency.Since this method is
Agricultural biomass derived from plant organism is raw material, using microwave-assisted magnesium salts infusion process and thermal cracking process, acquisition pair
Nitrogen has the rich magnesium charcoal of synchronous recycling ability with phosphorus nutrient.
(3) by the method for microwave-assisted dipping, largely increase the accessibility of biomass material, promote divalent magnesium from
Dip time is shortened in infiltration and deposition of the son in biomass structure；By the dipping of magnesium chloride, charcoal hole is on the one hand improved
Road structure and the magnesium density on surface, another aspect magnesium chloride can be improved the efficiency of subsequent thermal cracking, protected as activator
Hold the rich magnesium charcoal of the biomass natural hole structure such as stalk.
Detailed description of the invention:
Fig. 1 is the SEM spectrum of different biological carbon materials: common charcoal (A, B)；Rich magnesium charcoal recycling in the present invention
It is (C, D) and rear (E, F) before the biogas slurry nitrogen phosphorus of pig farm.
Fig. 2 is the XRD spectrum before and after rich magnesium charcoal recycling farm's waste liquid in the present invention: common charcoal recycles nitrogen
It is (A) and rear (B) before phosphorus；It is (C) and rear (D) before rich magnesium charcoal recycling nitrogen phosphorus in the present invention.
Specific embodiment
The present invention selectively provides embodiment, gives detailed embodiment and specific operation process, is only to illustrate this
The part important value of invention, but protection scope of the present invention is not limited to following embodiments, person skilled in the art's root in the field
The nonessential modifications and adaptations made according to foregoing invention content, still fall within protection scope of the present invention.
Embodiment 1
The preparation method of the rich magnesium charcoal of nitrogen and phosphorus nutrient in a kind of synchronous high-efficiency recycling farm's waste liquid of the invention,
Include the following steps: that (1) powdered biomass is added in magnesium chloride solution to mix well, be dispersed after mixing through microwave treatment
The magnesium chloride solution of biomass；
(2) then above-mentioned solution is stirred after a certain period of time, filtering, drying obtain rich magnesium biomass；It is finally that rich magnesium is raw
Substance is transferred in anoxic atmosphere, thermal cracking under the conditions of 450-700 DEG C of temperature, is made in synchronous high-efficiency recycling farm's waste liquid
The rich magnesium charcoal of nitrogen and phosphorus nutrient.
The rich magnesium charcoal that preparation method of the present invention prepares.
Application of the rich magnesium charcoal of the present invention in farm's waste liquid in synchronous recycling nitrogen and phosphorus nutrient.
Rich magnesium charcoal of the present invention is used as control sustained release charcoal after synchronous recycling nitrogen and phosphorus nutrient in farm's waste liquid
The application of fertilizer.Farm's waste liquid is for the liquid after livestock and poultry feces separation of solid and liquid and by obtaining after various waste biogas fermentations
The biogas slurry arrived.
Embodiment 2
Embodiment 2 the difference from embodiment 1 is that: in step (1), microwave-assisted dipping: by the biomass that 9g is dry
Powder is added in the magnesium chloride solution that 100mL concentration is 1mol/L, handles 30min after mixing well in microwave environment, and
500rpm magnetic agitation 8h is continued at, the biomass mixed solution for being sufficiently impregnated magnesium chloride is obtained；
Lignocellulose-like biomass powder is that lignocellulose-like biomass passes through 60-105 DEG C of drying, crushing and mistake
The sieving powder of 100 meshes.The lignocellulose-like biomass is the combination of corn stover and broomcorn straw.Described
The magnesium chloride solution of 1mol/L is by MgCl2·6H2O is dissolved in water and is made.The microwave environment microwave frequency is 2.45GHz, micro-
Wave power is 100W.
In step (2), thermal cracking: the resulting biomass solution for being sufficiently impregnated magnesium chloride of step (1) is filtered, filtering
Object is dried under the conditions of 100 DEG C of temperature, and is transferred in anoxic atmosphere, is warming up at 450 DEG C with 12 DEG C/min and is pyrolyzed 1h, is made
Synchronous high-efficiency recycles the rich magnesium charcoal of nitrogen and phosphorus nutrient in farm's waste liquid.
Embodiment 3
Rich magnesium charcoal is prepared by raw material of corn stover
The preparation method of the rich magnesium charcoal of nitrogen and phosphorus nutrient in a kind of synchronous high-efficiency recycling farm's waste liquid of the invention,
Include the following steps: in step (1), microwave-assisted dipping: collecting the corn stover that big Tanaka tests in Agricultural University Of Anhui, clearly
It is dried after washing in 90 DEG C and crushes, smash it through 100 meshes and collect the maize straw powder of sieving.Take 6g maize straw powder
It is added to the MgCl of 100mL 1.5mol/L2In solution, 20min is handled in the case where power is the microwave environment of 100W after mixing, and
300rpm magnetic agitation 4h is continued at, the MgCl of maize straw powder has been dispersed2Solution.The microwave environment Microwave Frequency
Rate is 2.45GHz, microwave power 800W.
In step (2), thermal cracking: the resulting biomass solution for being sufficiently impregnated magnesium chloride of step (1) is filtered, is obtained
Filtrate in 80 DEG C drying after, be transferred in anoxic atmosphere, be warming up at 500 DEG C with 10 DEG C/min and be pyrolyzed 1h, obtain rich magnesium
Charcoal.
Embodiment 4
Rich magnesium charcoal is prepared by raw material of rice husk
Embodiment 4 and the difference of embodiment 3 are: nitrogen and phosphorus in a kind of synchronous high-efficiency recycling farm's waste liquid of the invention
The preparation method of the rich magnesium charcoal of nutrient includes the following steps: microwave-assisted dipping: to collect this seminar in step (1)
Big Tanaka harvesting is tested treated rice husk, is dried after cleaning in 100 DEG C and crush, smash it through 100 meshes and collect sieving
Powdered rice hulls.4g rice husk powder is taken to be added to the MgCl of 100mL 2mol/L2In solution, in the microwave that power is 500W after mixing
10min is handled under environment, and continues at 300rpm magnetic agitation 6h, has been dispersed the MgCl of rice husk powder2Solution.Described
Microwave environment microwave frequency is 2.45GHz, microwave power 600W.
In step (2), thermal cracking: the resulting biomass solution for being sufficiently impregnated magnesium chloride of step (1) is filtered, by this
Solution filtering, obtained filtrate are transferred in anoxic atmosphere after 105 DEG C of drying, are warming up at 700 DEG C with 15 DEG C/min hot
3h is solved, rich magnesium charcoal is obtained.
Embodiment 5
Rich magnesium charcoal is prepared by biomass of wheat stalk
Embodiment 5 and the difference of embodiment 3 are: nitrogen and phosphorus in a kind of synchronous high-efficiency recycling farm's waste liquid of the invention
The preparation method of the rich magnesium charcoal of nutrient includes the following steps: microwave-assisted dipping: to collect this seminar in step (1)
The wheat stalk for testing big Tanaka dries in 105 DEG C after cleaning and crushes, smash it through 100 meshes and collect the wheat of sieving
Straw powder.8g wheat stalk powder is taken to be added to the MgCl of 100mL3mol/L2In solution, after mixing power be 100W it is micro-
25min is handled under wave environment, and continues at 300rpm magnetic agitation 6h, has been dispersed the MgCl of wheat stalk powder2Solution.
In step (2), thermal cracking: the resulting biomass solution for being sufficiently impregnated magnesium chloride of step (1) is filtered, by this
Solution filtering, obtained filtrate are transferred in anoxic atmosphere after 105 DEG C of drying, are warming up at 600 DEG C with 15 DEG C/min hot
2h is solved, rich magnesium charcoal is obtained.
Embodiment 6
Rich magnesium charcoal is prepared by biomass of sawdust
Embodiment 6 and the difference of embodiment 3 are: nitrogen and phosphorus in a kind of synchronous high-efficiency recycling farm's waste liquid of the invention
The preparation method of the rich magnesium charcoal of nutrient includes the following steps: in step (1), microwave-assisted dipping: by the sawdust of collection
It is dried after cleaning in 100 DEG C and crushes, smash it through 100 meshes and collect the wood dust of sieving, 3g sawdust powder is taken to be added to
The MgCl of 100mL 1.5mol/L2In solution, 15min is handled in the case where power is the microwave environment of 300W after mixing, and continue at
400rpm magnetic agitation 7h, has been dispersed the MgCl of sawdust powder2Solution.
In step (2), thermal cracking: the resulting biomass solution for being sufficiently impregnated magnesium chloride of step (1) is filtered, by this
Solution filtering, obtained filtrate are transferred in anoxic atmosphere after 100 DEG C of drying, are warming up at 700 DEG C with 10 DEG C/min hot
1h is solved, rich magnesium charcoal is obtained.
Embodiment 7
Rich magnesium charcoal is prepared by biomass of corncob
Embodiment 7 and the difference of embodiment 3 are: nitrogen and phosphorus in a kind of synchronous high-efficiency recycling farm's waste liquid of the invention
The preparation method of the rich magnesium charcoal of nutrient includes the following steps: microwave-assisted dipping: to collect this seminar in step (1)
The corncob for testing big Tanaka dries in 90 DEG C after cleaning and crushes, smash it through 100 meshes and collect the maize leaves of sieving
Powder takes 3g corncob powder to be added to the MgCl of 100mL 1mol/L2In solution, in the microwave environment that power is 300W after mixing
Lower processing 5min, and 500rpm magnetic agitation 2h is continued at, dispersed the MgCl of corncob powder2Solution.
In step (2), thermal cracking: the resulting biomass solution for being sufficiently impregnated magnesium chloride of step (1) is filtered, by this
Solution filtering, obtained filtrate are transferred in anoxic atmosphere after 80 DEG C of drying, are warming up at 600 DEG C with 10 DEG C/min hot
1h is solved, rich magnesium charcoal is obtained.
Embodiment 8
Carbon-based magnetic adsorptive material is prepared by biomass of rice straw
Embodiment 8 and the difference of embodiment 3 are: nitrogen and phosphorus in a kind of synchronous high-efficiency recycling farm's waste liquid of the invention
The preparation method of the rich magnesium charcoal of nutrient includes the following steps: microwave-assisted dipping: to collect this seminar in step (1)
The rice straw for testing big Tanaka dries in 105 DEG C after cleaning and crushes, smash it through 100 meshes and collect the rice of sieving
Straw powder takes 10g rice straw powder to be added to the MgCl of 100mL4mol/L2In solution, after mixing power be 500W it is micro-
15min is handled under wave environment, and continues at 300rpm magnetic agitation 3h, has been dispersed the MgCl of rice straw powder2Solution.
In step (2), thermal cracking: the resulting biomass solution for being sufficiently impregnated magnesium chloride of step (1) is filtered, by this
Solution filtering, obtained filtrate are transferred in anoxic atmosphere after 105 DEG C of drying, are warming up at 600 DEG C with 15 DEG C/min hot
2h is solved, rich magnesium charcoal is obtained.
Embodiment 9
Rich magnesium charcoal is prepared using cotton stalk and bagasse as raw material
Embodiment 9 and the difference of embodiment 3 are: nitrogen and phosphorus in a kind of synchronous high-efficiency recycling farm's waste liquid of the invention
The preparation method of the rich magnesium charcoal of nutrient includes the following steps: microwave-assisted dipping: to collect experimental plot in step (1)
Cotton stalk dries in 90 DEG C after cleaning and crushes, smash it through 100 meshes and collect the cotton stalk powder of sieving；It collects
Bagasse in the market dries in 90 DEG C after cleaning and crushes, smash it through 100 meshes and collect the bagasse powder of sieving.It takes
3g cotton stalk and 2g bagasse powder are added to the MgCl of 100mL 2mol/L2It in power is 600W after mixing in solution
5min is handled under microwave environment, and continues at 500rpm magnetic agitation 5h, has been dispersed cotton stalk and bagasse mixed powder
The MgCl at end2Solution.
In step (2), thermal cracking: the resulting biomass solution for being sufficiently impregnated magnesium chloride of step (1) is filtered, by this
Solution filtering, obtained filtrate are transferred in anoxic atmosphere after 90 DEG C of drying, are warming up at 700 DEG C with 15 DEG C/min hot
3h is solved, rich magnesium charcoal is obtained.
Embodiment 10
Rich magnesium charcoal is prepared by biomass of the mixture of rice husk, sawdust and soybean stalk
Embodiment 10 and the difference of embodiment 3 are: in a kind of synchronous high-efficiency recycling farm's waste liquid of the invention nitrogen and
The preparation method of the rich magnesium charcoal of phosphorus nutrient includes the following steps: in step (1), microwave-assisted dipping: it is big to collect experiment
Tanaka's harvesting treated rice husk, dries in 100 DEG C after cleaning and crushes, smash it through 100 meshes and collect the rice husk of sieving
Powder；It is dried after the sawdust of collection is cleaned in 100 DEG C and crushes, smash it through 100 meshes and collect the wood dust of sieving；It collects
The soybean stalk for testing big Tanaka dries in 100 DEG C after cleaning and crushes, smash it through 100 meshes and collect the sorghum of sieving
Straw powder.4g powdered rice hulls, 2g wood dust and 4g soybean stalk powder is taken to be added to the MgCl of 100mL 4mol/L2In solution, mix
Handle 10min in the case where power is the microwave environment of 800W afterwards, and continue at 500rpm magnetic agitation 6h, dispersed rice husk,
The MgCl of sawdust and soybean stalk mixed-powder2Solution.
In step (2), thermal cracking: the resulting biomass solution for being sufficiently impregnated magnesium chloride of step (1) is filtered, by this
Solution filtering, obtained filtrate are transferred in anoxic atmosphere after 90 DEG C of drying, are warming up at 700 DEG C with 15 DEG C/min hot
3h is solved, rich magnesium charcoal is obtained.
Test 1
The performance evaluation of nitrogen phosphorus in the synchronous recycling farm's biogas slurry of rich magnesium charcoal
(1) the rich magnesium charcoal obtained in 0.1g above-described embodiment 2-10 is weighed respectively, is added in 60mL 1# biogas slurry
(pH:7.5；Total ammonia nitrogen content: 135.0mg/L；Total nitrogen content: 188.8mg/L；Total phosphorus content: 52.8mg/L)；By above-mentioned each group
Mixed liquor concussion recycling 12h under 25 DEG C, the revolving speed of 300rpm；The content of total ammonia nitrogen, total nitrogen and total phosphorus in final sample liquid is measured,
And each group rich magnesium charcoal is calculated to the rate of recovery of nitrogen phosphorus.Concrete outcome sees appendix table 1.
(2) the rich magnesium charcoal obtained in 0.1g above-described embodiment 2-10 is weighed respectively, is added in 100mL2# biogas slurry
(pH:10；Total ammonia nitrogen content: 298.0mg/L；Total nitrogen content: 375.1mg/L；Total phosphorus content: 315.5mg/L)；By above-mentioned each group
Concussion recycling is for 24 hours under 35 DEG C, the revolving speed of 500rpm for mixed liquor；The content of total ammonia nitrogen, total nitrogen and total phosphorus in final sample liquid is measured,
And each group rich magnesium charcoal is calculated to the rate of recovery of nitrogen phosphorus.Concrete outcome sees appendix table 2.Rich magnesium charcoal is to farm's 1# biogas slurry
The recyclability of middle nitrogen phosphorus compares that figure is as shown in table 1, and rich magnesium charcoal compares the recyclability of nitrogen phosphorus in farm's 2# biogas slurry
Figure is as shown in table 2.
Table 1
Table 2
As can be seen from Table 1, according to the present invention the rich magnesium biological carbon materials in the standby embodiment 2~10 of patent system to 1#
Nitrogen and phosphorus nutrient recovery efficiency with higher in biogas slurry, the wherein rate of recovery of the material of embodiment 3 to ammonia nitrogen, total nitrogen and total phosphorus
Highest, respectively 97.4%, 90.7% and 100%.Although the concentration of nitrogen phosphorus is higher than 1# biogas slurry, especially total phosphorus in 2# biogas slurry
Concentration is as many as 6 times of 1# biogas slurry.But as can be seen from Table 2, using in the material recovery 2# biogas slurry in above-described embodiment 2~10
Nitrogen phosphorus, the rate of recovery of total phosphorus are still higher than 95%, and the rate of recovery of total nitrogen and ammonia nitrogen is also maintained at higher level.Mandatory declaration
It is that 2# biogas slurry pH is 10, and rich magnesium biological carbon materials have the recycling of nitrogen phosphorus in waste liquid generate different knots at various ph values
Fruit needs to be adjusted as the case may be.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, the present invention
Claimed range is delineated by the appended claims, the specification and equivalents thereof from the appended claims.
Claims (10)
1. the preparation method of the rich magnesium charcoal of nitrogen and phosphorus nutrient in a kind of synchronous high-efficiency recycling farm's waste liquid, it is characterised in that
Include the following steps:
(1) powdered biomass is added in magnesium chloride solution and is mixed well, dispersed biomass through microwave treatment after mixing
Magnesium chloride solution；
(2) then above-mentioned solution is stirred after a certain period of time, filtering, drying obtain rich magnesium biomass；Finally by rich magnesium biomass
Be transferred in anoxic atmosphere, thermal cracking under the conditions of 450-700 DEG C of temperature, be made synchronous high-efficiency recycling farm's waste liquid in nitrogen and
The rich magnesium charcoal of phosphorus nutrient.
2. the preparation of the rich magnesium charcoal of nitrogen and phosphorus nutrient in synchronous high-efficiency recycling farm's waste liquid according to claim 1
Method, it is characterised in that include the following steps:
In step (1), microwave-assisted dipping: it is 1-4mol/L that the dry powdered biomass of 1-10g, which is added to 100mL concentration,
Magnesium chloride solution in, 5-30min is handled after mixing well in microwave environment, and continue at 300-500rpm magnetic agitation 1-
8h obtains the biomass mixed solution for being sufficiently impregnated magnesium chloride；
In step (2), thermal cracking: by step (1) it is resulting be sufficiently impregnated magnesium chloride biomass solution filter, filtrate in
It dries, and is transferred in anoxic atmosphere under the conditions of 80-105 DEG C of temperature, be warming up at 450-700 DEG C and be pyrolyzed with 10-15 DEG C/min
The rich magnesium charcoal of nitrogen and phosphorus nutrient in synchronous high-efficiency recycling farm's waste liquid is made in 1-3h.
3. the preparation of the rich magnesium charcoal of nitrogen and phosphorus nutrient in synchronous high-efficiency recycling farm's waste liquid according to claim 2
Method, it is characterised in that: in step (1), the powdered biomass is one of lignocellulose-like biomass or several
The mixed-powder of kind；Lignocellulose-like biomass powder is lignocellulose-like biomass by 60-105 DEG C of drying, crushing
And the sieving powder sieved with 100 mesh sieve.
4. the preparation of the rich magnesium charcoal of nitrogen and phosphorus nutrient in synchronous high-efficiency recycling farm's waste liquid according to claim 3
Method, it is characterised in that: in step (1), the lignocellulose-like biomass is corn stover, corncob, rice husk, wheat
In stalk, bagasse, sawdust, maize leaves, rice straw, broomcorn straw, cotton stalk or soybean stalk any one or it is several
The combination of kind.
5. the preparation of the rich magnesium charcoal of nitrogen and phosphorus nutrient in synchronous high-efficiency recycling farm's waste liquid according to claim 2
Method, it is characterised in that: in step (1), the magnesium chloride solution of the 1-4mol/L is by MgCl2·6H2O is dissolved in water system
?.
6. the preparation of the rich magnesium charcoal of nitrogen and phosphorus nutrient in synchronous high-efficiency recycling farm's waste liquid according to claim 2
Method, it is characterised in that: in step (1), the microwave environment microwave frequency is 2.45GHz, microwave power 100-
800W。
7. the rich magnesium charcoal that preparation method described in any one of claims 1-6 prepares.
8. application of the rich magnesium charcoal as claimed in claim 7 in farm's waste liquid in synchronous recycling nitrogen and phosphorus nutrient.
9. rich magnesium charcoal as claimed in claim 7 is used as control sustained release charcoal after synchronous recycling nitrogen and phosphorus nutrient in farm's waste liquid
The application of fertilizer.
10. application according to claim 8 or claim 9, it is characterised in that: farm's waste liquid is livestock and poultry feces solid-liquid point
Liquid from after and the biogas slurry by being obtained after various waste biogas fermentations.
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