CN111453836A - Microbial filler for modified waste lotus seedpod shells and preparation method thereof - Google Patents
Microbial filler for modified waste lotus seedpod shells and preparation method thereof Download PDFInfo
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- CN111453836A CN111453836A CN202010422663.8A CN202010422663A CN111453836A CN 111453836 A CN111453836 A CN 111453836A CN 202010422663 A CN202010422663 A CN 202010422663A CN 111453836 A CN111453836 A CN 111453836A
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- lotus
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- seedpod
- lotus seedpod
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/14—NH3-N
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/16—Total nitrogen (tkN-N)
Abstract
The invention provides a microbial filler for modifying a waste lotus seedpod shell and a preparation method thereof. The microbial filler of the modified waste lotus seedpod shells is prepared by modifying and processing lotus seedpods after fruits of the lotus seedpods are removed. The preparation method of the microbial filler for modifying the waste lotus seedpod shells comprises the steps of cleaning the lotus seedpod shells; drying the lotus seed pod shell; heating to form a carbonized shower shell; NH (NH)4H2PO4Soaking in the solution, and heating again to form a porous carbonized lotus seed shell; ti (SO)4)2Soaking in the solution, adding Na2CO3And carrying out ultrasonic reaction on the solution, and heating for the third time to form the microbial filler of the modified waste lotus seedpod. The microbial filler for modifying the waste lotus seedpod shells and the preparation method thereof provided by the invention solve the defects of good biodegradability, short service life, small strength, small specific surface area, low porosity and the like when the lotus seedpod shells are used as the filler.
Description
Technical Field
The invention relates to the field of biological fillers, in particular to a microbial filler for modifying a waste lotus seedpod shell and a preparation method thereof.
Background
The biofilm process is a commonly used process in sewage treatment. Through the contact of sewage and the biomembrane, the organic matters in the sewage are degraded by utilizing the microorganisms in the membrane, so that the sewage is purified, and meanwhile, the microorganisms in the biomembrane continuously grow and reproduce. The key of the biofilm process is to form a good-performance biofilm, and a filler (or a carrier) for attachment, growth and fixation is provided for the biofilm as a core part of the biofilm process, the performance of the filler directly influences the treatment efficiency of the process, and the good biological characteristic is the main performance of the filler as a carrier of microorganisms in the biofilm reactor.
Currently, the fillers used in the biofilm process are mainly classified into two types, inorganic and organic. The inorganic filler mainly comprises zeolite, ceramsite, slag and the like, and generally has the advantages of high mechanical strength, relatively stable chemical properties, large specific surface, wide raw material source and low price. However, the inorganic filler has the defects of high density, high energy consumption for maintaining a fluidized state, easy breakage in the later period and short service life. The organic filler is mainly made of PVC, PE and PP materials, and has the advantages of regular overall dimension, density close to water, easy fluidization, long service life and large specific surface area. However, the organic fillers have the defects of poor biocompatibility, slow attachment of the biological membrane, low total amount of the biological membrane and the like.
The lotus seedpod has wide planting area in southern areas such as Hunan and Hubei, and is an important economic crop in local areas. The lotus seed pod shell is a product of lotus seeds without fruits, and the main component of the lotus seed pod shell is cellulose and has a loose and porous structure. However, most of the lotus seedpod shells are discarded as waste, and cannot be recycled, which causes waste of resources. The lotus seedpod shell as a natural organic filler has the characteristics of good hydrophilicity and biocompatibility, but has the defects of short service life, small strength, small specific surface area, low porosity and the like caused by good biodegradability, and is difficult to be practically applied to a biofilm method as a biological filler. Therefore, the waste shower shells must be modified to improve their biodegradability, strength, specific surface area, porosity, etc.
Disclosure of Invention
In order to overcome the defects of good biodegradability, short service life, small strength, small specific surface area, low porosity and the like when the lotus seedpod shell is used as a filler, the invention provides a microbial filler for modifying a waste lotus seedpod shell and a preparation method thereof.
A microbial filler for modifying waste lotus seedpods is prepared by the following steps:
step 1, cleaning a shower nozzle shell;
step 2, drying the lotus seedpod shells;
step 3, heating the dried lotus seedpod shell to 600-1000 ℃ at a constant heating rate in a protective atmosphere, and carrying out heat preservation reaction for a period of time to form a carbonized lotus seedpod shell;
step 4, placing the carbonized shower nozzle shell in NH4H2PO4Soaking in the solution for a period of time, then heating to 600-1000 ℃ at a constant heating rate in a protective atmosphere, and carrying out heat preservation reaction for a period of time to form a porous carbonized lotus seed shell;
step 5, placing the porous carbonized shower nozzle shell in Ti (SO)4)2Soaking in the solution for a period of time, and adding Na2CO3The solution is filled with Ti (SO)4)2Porous carbonized lotus seed pod shell and Na2CO3The container is placed in an ultrasonic reactor, and ultrasonic reaction is carried out for a period of time; and heating the porous carbonized lotus seedpod shells subjected to the ultrasonic reaction to 600-1000 ℃ at a constant heating rate in a protective atmosphere, and carrying out heat preservation reaction for a period of time to form the microbial filler of the modified waste lotus seedpod shells.
In a preferred embodiment of the preparation method of the microbial filler for the modified waste lotus seedpod, step 1, the lotus seedpod is placed in an ultrasonic cleaner filled with pure water and is ultrasonically cleaned for 2 hours; step 2, placing the lotus seedpod shells subjected to ultrasonic cleaning in a vacuum drying box at the temperature of 80 ℃ for vacuum drying for 48 hours; step 5, Ti (SO) is filled in the solution4)2Porous carbonized lotus seed pod shell and Na2CO3The beaker is placed in an ultrasonic reactor for ultrasonic reaction for 1 hour.
In the invention providedIn a preferred embodiment of the method for preparing the microbial filler for modifying the waste lotus seedpod, in step 3, or step 4, or step 5, the lotus seedpod, the carbonized lotus pod and the porous carbonized lotus pod are all put into a tube furnace in an N-shaped furnace2Heating at a heating rate of 5-20 ℃/min in the atmosphere, and carrying out heat preservation reaction for 120 min.
In a preferred embodiment of the method for preparing the microbial filler for modifying the waste lotus seedpod provided by the invention, NH is performed in the step 44H2PO4The concentration of the solution is 0.1-0.6 mol/L, and Ti (SO) is added in the step 54)2The concentration of the solution is 0.1-0.6 mol/L, and Na is added in the step 52CO3The concentration of the solution is 0.2-1.2 mol/L, and the solution is added to Ti (SO) according to the volume ratio of 1:54)2In solution.
Compared with the prior art, the modified microbial filler for the waste lotus seedpod shells, provided by the invention, takes the waste lotus seedpod shells as the raw material, so that the treatment cost generated by treating the waste lotus seedpod shells is avoided, the resource utilization of the lotus seedpod shells is realized, and the cost is reduced from the source of filler production. The microbial filler of the modified waste lotus seedpod shell provided by the invention can be used for treating COD and NH in domestic sewage under the same conditions3The treatment effects of-N, TN and TP are better than those of commercial fillers such as zeolite, ceramsite, slag and the like, the sewage treatment efficiency is higher, and the effluent index reaches the first-class A standard.
In the preparation method of the microbial filler for the modified waste lotus seedpod provided by the invention, NH is added4H2PO4Then pyrolyzed at high temperature to make NH4H2PO4P atoms formed by thermal decomposition are doped into the lotus seedpod shell structure and condensed with hydroxyl groups in the lotus seedpod shell structure to form phosphate ester bonds, and the cross-linking among the phosphate ester bonds effectively inhibits the breakage of carbon-carbon bonds, so that the stability and the ageing resistance of the lotus seedpod shell can be improved, and the service life of the modified biological filler is longer. And NH formed during decomposition3、O2、H2When gas such as O and the like overflows from the shower nozzle shell, pores can be formed in the inner part and the surface of the shower nozzle shell, the specific surface area of the shower nozzle shell is greatly increased, and more growth is provided for the attachment, growth and propagation of microorganismsA living place.
In the preparation method of the microbial filler for modifying the waste lotus seedpod provided by the invention, Ti (SO) is added4)2With Na2CO3Reacting Ti (SO)4)2With Na2CO3Reaction to produce Ti (OH)4Then calcining at high temperature in the presence of Ti (OH)4Decomposition by heating to form TiO2，TiO2Is absorbed in the surface pore structure inside the shower nozzle shell. TiO 22The introduction of the compound makes the surface of the lotus seedpod filler have positive charge in the water solution, and the surface of the microorganism has negative charge, so that the combination between the microorganism and the lotus seedpod filler is facilitated, the film hanging stability of the microorganism on the lotus seedpod filler is accelerated, and the starting time of the sewage treatment reactor is shortened.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1:
(1) the lotus seedpod shells are placed in an ultrasonic cleaner filled with pure water and cleaned for 2 hours by ultrasonic.
(2) And (3) placing the lotus seed pod shells subjected to ultrasonic cleaning in a vacuum drying box at the temperature of 80 ℃ and drying for 48 hours in vacuum.
(3) Putting the lotus seed pod shell after vacuum drying into a tube furnace in N2Heating to 600 ℃ at the heating rate of 5 ℃/min in the atmosphere, then carrying out heat preservation reaction for 120min, cooling to room temperature, and taking out the product from the tubular furnace, wherein the product is marked as a carbonized lotus seed shell.
(4) Soaking the carbonized lotus seed pod shell in NH4H2PO4In a beaker of solution, NH4H2PO4Is 0.2 mol/L, the carbonized shower nozzle shell after soaking is put into a tube furnace after soaking for 2 hours, and then the carbonized shower nozzle shell is soaked in N2Heating to 600 ℃ at the heating rate of 5 ℃/min in the atmosphere, then carrying out heat preservation reaction for 120min, cooling to room temperature, taking out the product from the tubular furnace, and marking as the porous carbonized lotus seed shell.
(5) Soaking porous carbonized lotus seed pod shell in Ti (SO)4)2In a beaker of solution, Ti (SO)4)2Is 0.1 mol/L, is soaked for 2 hours, and then 0.2 mol/L of Na is added2CO3The solution was added to the above Ti (SO) in a volume ratio of 1:54)2Putting the beaker into an ultrasonic reactor for ultrasonic reaction for 1 hour, and finally putting the porous carbonized shower nozzle shell after the ultrasonic reaction is completed into a tube furnace in N2Heating to 600 ℃ at the heating rate of 5 ℃/min in the atmosphere, then carrying out heat preservation reaction for 120min, cooling to room temperature, and taking out the product from the tubular furnace to obtain the microbial filler of the modified waste lotus seedpod shell.
Example 2:
(1) the lotus seedpod shells are placed in an ultrasonic cleaner filled with pure water and cleaned for 2 hours by ultrasonic.
(2) And (3) placing the lotus seed pod shells subjected to ultrasonic cleaning in a vacuum drying box at the temperature of 80 ℃ and drying for 48 hours in vacuum.
(3) Putting the lotus seed pod shell after vacuum drying into a tube furnace in N2Heating to 800 ℃ at the heating rate of 10 ℃/min in the atmosphere, then carrying out heat preservation reaction for 120min, cooling to room temperature, and taking out the product from the tubular furnace, wherein the product is marked as a carbonized lotus seed shell.
(4) Soaking the carbonized lotus seed pod shell in NH4H2PO4In a beaker of solution, NH4H2PO4Is 0.4 mol/L, the carbonized shower nozzle shell after soaking is put into a tube furnace after soaking for 2 hours, and then the carbonized shower nozzle shell is soaked in N2Heating to 800 ℃ at the heating rate of 10 ℃/min in the atmosphere, then carrying out heat preservation reaction for 120min, cooling to room temperature, taking out the product from the tubular furnace, and marking as the porous carbonized lotus seed shell.
(5) Soaking porous carbonized lotus seed pod shell in Ti (SO)4)2In a beaker of solution, Ti (SO)4)2Is 0.2 mol/L, is soaked for 2 hours, and then 0.2 mol/L of Na is added2CO3The solution was added to the above Ti (SO) in a volume ratio of 1:54)2A beaker of the solution, then the beaker is placed in an ultrasonic reactor,ultrasonic reaction for 1 hr, and finally putting the porous carbonized shower nozzle shell into a tubular furnace in N2Heating to 800 ℃ at the heating rate of 10 ℃/min in the atmosphere, then carrying out heat preservation reaction for 120min, cooling to room temperature, and taking out the product from the tubular furnace to obtain the microbial filler of the modified waste lotus seedpod shell.
Example 3:
(1) the lotus seedpod shells are placed in an ultrasonic cleaner filled with pure water and cleaned for 2 hours by ultrasonic.
(2) And (3) placing the lotus seed pod shells subjected to ultrasonic cleaning in a vacuum drying box at 60 ℃ and drying for 48 hours in vacuum.
(3) Putting the lotus seed pod shell after vacuum drying into a tube furnace in N2Heating to 1000 ℃ at a heating rate of 20 ℃/min in the atmosphere, then carrying out heat preservation reaction for 120min, cooling to room temperature, and taking out the product from the tubular furnace, wherein the product is marked as a carbonized lotus seed shell.
(4) Soaking the carbonized lotus seed pod shell in NH4H2PO4In a beaker of solution, NH4H2PO4Is 0.6 mol/L, the carbonized shower nozzle shell after soaking is put into a tube furnace after soaking for 2 hours, and then the carbonized shower nozzle shell is soaked in N2Heating to 1000 ℃ at a heating rate of 20 ℃/min in the atmosphere, then carrying out heat preservation reaction for 120min, cooling to room temperature, taking out the product from the tubular furnace, and marking as the porous carbonized lotus seed shell.
(5) Soaking porous carbonized lotus seed pod shell in Ti (SO)4)2In a beaker of solution, Ti (SO)4)2Is 0.4 mol/L, is soaked for 2 hours, and then 0.2 mol/L of Na is added2CO3The solution was added to the above Ti (SO) in a volume ratio of 1:54)2Putting the beaker into an ultrasonic reactor for ultrasonic reaction for 1 hour, and finally putting the porous carbonized shower nozzle shell after the ultrasonic reaction is completed into a tube furnace in N2Heating to 1000 ℃ at a heating rate of 20 ℃/min in the atmosphere, then carrying out heat preservation reaction for 120min, cooling to room temperature, and taking out the product from the tubular furnace to obtain the microbial filler of the modified waste lotus seedpod shell.
Example 4:
the microbial fillers of the modified waste lotus seedpod shells prepared in the examples 1, 2 and 3, the commercial biological fillers 1, 2, zeolite and ceramsite were subjected to a sewage treatment test. Respectively adding the 7 fillers into a Sequencing Batch Biofilm Reactor (SBBR), operating under the same condition, and respectively performing biofilm culturing stabilization time, COD (chemical oxygen demand) and NH (NH) on the 7 fillers3The removal performance of-N, TN and TP was investigated experimentally.
The experimental research method comprises the following steps: taking activated sludge of a certain sewage treatment plant, equivalently adding the activated sludge into a Sequencing Batch Biofilm Reactor (SBBR) with 7 fillers, and filling domestic sewage into the Sequencing Batch Biofilm Reactor (SBBR); and starting aeration for 3 days, then culturing the sludge by adopting an intermittent aeration mode, and controlling the aeration and standing time ratio to be 10: 2 (namely aerating 10 hours every day, standing for 2 hours, 2 times a day), replacing the supernatant of 1/5 with domestic sewage after standing is finished, and continuously culturing for 4 days, adding 3 days for starting closed aeration and culturing for 7 days in total; then, the Sequencing Batch Biofilm Reactor (SBBR) is operated according to 4 periods every day, each period consists of five processes of water inlet, aeration, sedimentation, water drainage and standby, the biofilm formation condition of 7 fillers is observed, and COD and NH of water outlet in each period are detected3N, TN and TP, until the effluent pollution index is basically stable in each period, the filler biofilm formation level reaches a stable period. When the film formation level of the 7 fillers reaches a stable period, the average data of continuous operation for 30 days are compared, and the test results are shown in the following table:
the test result shows that: under the same equipment and process conditions, the microbial filler (example 1-3) of the modified waste lotus seedpod shell prepared by the method disclosed by the invention can be subjected to biofilm formation for about 7-10 days faster than the commercial filler 1 and the commercial filler 2; the time is about 10 to 15 days faster than that of zeolite and ceramsite; and finally a Sequencing Batch Biofilm Reactor (SBBR) with microbial fillers (examples 1-3) of modified waste lotus seedpod added in the stable operation stage under the same conditionsTo COD and NH in domestic sewage3The treatment effects of-N, TN and TP are better than those of the filler 1 sold in the market, the filler 2 sold in the market, zeolite and ceramsite, the sewage treatment efficiency is higher, and the effluent index reaches the first-class A standard.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, or direct or indirect applications in other related fields, which are made by the present disclosure, are included in the scope of the present invention.
Claims (10)
1. The microbial filler for the modified waste lotus seedpod shells is characterized by comprising the following steps:
step 1, cleaning a shower nozzle shell;
step 2, drying the lotus seedpod shells;
step 3, heating the dried lotus seedpod shell to 600-1000 ℃ at a constant heating rate in a protective atmosphere, and carrying out heat preservation reaction for a period of time to form a carbonized lotus seedpod shell;
step 4, placing the carbonized shower nozzle shell in NH4H2PO4Soaking in the solution for a period of time, then heating to 600-1000 ℃ at a constant heating rate in a protective atmosphere, and carrying out heat preservation reaction for a period of time to form a porous carbonized lotus seed shell;
step 5, placing the porous carbonized shower nozzle shell in Ti (SO)4)2Soaking in the solution for a period of time, and adding Na2CO3The solution is filled with Ti (SO)4)2Porous carbonized lotus seed pod shell and Na2CO3The container is placed in an ultrasonic reactor, and ultrasonic reaction is carried out for a period of time; and heating the porous carbonized lotus seedpod shells subjected to the ultrasonic reaction to 600-1000 ℃ at a constant heating rate in a protective atmosphere, and carrying out heat preservation reaction for a period of time to form the microbial filler of the modified waste lotus seedpod shells.
2. The method for preparing the microbial filler for modifying the waste lotus seedpod as claimed in claim 1, wherein the method comprises the following steps: in step 3, or step 4, or step 5, the lotus seed pod shell, the carbonized lotus seed pod shell and the porous carbonized lotus seed pod shell are all put into a tube furnace for heating.
3. The method for preparing the microbial filler for modifying the waste lotus seedpod as claimed in claim 1, wherein the method comprises the following steps: in step 3, or step 4, or step 5, the lotus seed pod, the carbonized lotus seed pod and the porous carbonized lotus seed pod are all in N2Heating is carried out in an atmosphere.
4. The method for preparing the microbial filler for modifying the waste lotus seedpod as claimed in claim 1, wherein the method comprises the following steps: in step 3, or step 4, or step 5, the lotus seed pod, the carbonized lotus seed pod and the porous carbonized lotus seed pod are heated at a heating rate of 5-20 ℃/min.
5. The method for preparing the microbial filler for modifying the waste lotus seedpod as claimed in claim 1, wherein the method comprises the following steps: in step 3, or step 4, or step 5, the lotus seedpod shell, the carbonized lotus seedpod shell and the porous carbonized lotus seedpod shell are all subjected to heat preservation reaction for 120 min.
6. The method for preparing the microbial filler for modifying the waste lotus seedpod as claimed in claim 1, wherein the method comprises the following steps: NH in step 44H2PO4The concentration of the solution is 0.1-0.6 mol/L.
7. The method for preparing the microbial filler for modifying the waste lotus seedpod as claimed in claim 1, wherein the method comprises the following steps: ti (SO) in step 54)2The concentration of the solution is 0.1-0.6 mol/L.
8. The method for preparing the microbial filler for modifying the waste lotus seedpod as claimed in claim 1, wherein the method comprises the following steps: in step 5 Na2CO3The concentration of the solution is 0.2-1.2 mol/L, Na2CO3The solution is added to Ti (SO) according to the volume ratio of 1:54)2In solution.
9. The method for preparing the microbial filler for modifying the waste lotus seedpod as claimed in claim 1, wherein the method comprises the following steps: in the step 1, the lotus seedpod is placed in an ultrasonic cleaner filled with pure water and is cleaned for 2 hours in an ultrasonic mode; in step 2, the lotus seedpod shells after ultrasonic cleaning are placed in a vacuum drying box at 80 ℃ and are dried for 48 hours in vacuum.
10. The method for preparing the microbial filler for modifying the waste lotus seedpod as claimed in claim 1, wherein the method comprises the following steps: in step 5, Ti (SO) is filled in4)2Porous carbonized lotus seed pod shell and Na2CO3The beaker is placed in an ultrasonic reactor and subjected to ultrasonic reaction for 1 hour.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170197192A1 (en) * | 2014-10-01 | 2017-07-13 | Cool Planet Energy Systems, Inc. | Biochar aggregate particles |
| CN109126714A (en) * | 2018-09-26 | 2019-01-04 | 湖南农业大学 | A kind of TiO2/SiO2Banana skin charcoal composite adsorbing material and preparation method thereof |
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2020
- 2020-05-19 CN CN202010422663.8A patent/CN111453836A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170197192A1 (en) * | 2014-10-01 | 2017-07-13 | Cool Planet Energy Systems, Inc. | Biochar aggregate particles |
| CN109126714A (en) * | 2018-09-26 | 2019-01-04 | 湖南农业大学 | A kind of TiO2/SiO2Banana skin charcoal composite adsorbing material and preparation method thereof |
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