CN110921896A - Method for preparing nano charcoal balls from syrup wastewater - Google Patents
Method for preparing nano charcoal balls from syrup wastewater Download PDFInfo
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- CN110921896A CN110921896A CN201911193572.5A CN201911193572A CN110921896A CN 110921896 A CN110921896 A CN 110921896A CN 201911193572 A CN201911193572 A CN 201911193572A CN 110921896 A CN110921896 A CN 110921896A
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- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- 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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Abstract
The invention relates to the technical field of wastewater resource utilization, and discloses a method for preparing nano biochar balls from syrup wastewater. The invention provides a new way for solving the treatment problem and resource utilization of the syrup wastewater, realizes the resource utilization of the syrup wastewater, and reduces the treatment cost and environmental pollution of the syrup wastewater as sewage; the method has the advantages of simple process, controllable process, no need of additional modification and modification of new groups, material saving, and preparation cost reduction, and simultaneously, the surface of the prepared nano biological carbon ball has positive and negative potentials and an amphoteric state, so that the adsorption and removal of heavy metals, sulfanilamide antibiotics and nitrosamine disinfection byproducts are facilitated; the invention can also realize the removal effect of the nano biological carbon spheres on anions and cations such as heavy metals, sulfonamides antibiotics and nitrosamine disinfection byproducts by regulating and controlling the pH.
Description
Technical Field
The invention relates to the technical field of wastewater resource utilization, in particular to a method for preparing nano biochar balls from syrup wastewater.
Background
The syrup wastewater is the wastewater generated in the food, particularly the preserve processing industry, the CODcr content of the wastewater reaches more than 100000mg/L, and the wastewater contains high-concentration TN (>1000mg/L) and TP. The wastewater is high in organic load, a large amount of medicaments and energy are consumed in the treatment process, and the treated solution still contains a large amount of COD and N, P, so that the wastewater cannot reach the wastewater discharge standard, and the problems of eutrophication and secondary pollution of a water body are easily caused. Therefore, the treatment of the syrup wastewater at present becomes a difficult problem, but because the generation amount of the syrup wastewater at present is extremely large, the resource utilization of the syrup wastewater has a great application prospect.
The nano charcoal ball has a large amount of active functional groups on the surface, has excellent hydrophilicity and surface reaction activity, can be applied to the fields of biochemistry, biological diagnosis and drug delivery, can also be used as a template for preparing core-shell structure materials or porous materials and the like, has excellent application prospect, is spread in industries such as rubber and plastic, environmental protection, chemical engineering, electronics, daily chemicals, functional materials and the like, and has the main functions of strong adsorbability, high activeness, good dispersibility, quick odor removal and good effect.
The syrup wastewater contains a large amount of carbon sources, exists in the forms of glucose and fructose, and can be prepared into biochar, C, N, P contained in the syrup wastewater can be converted into hydroxyl, carboxyl, amino, phosphate and other groups in situ in the preparation process, so that the prepared nano carbon material has amphoteric properties, and the prepared nano biochar sphere can be applied to the fields of pollutant treatment and soil remediation.
Disclosure of Invention
Based on the problems, the invention provides a method for preparing nano biochar balls from syrup wastewater, which realizes resource utilization of the syrup wastewater, and the prepared carbon balls have the advantages that the surface groups are native groups, no additional modified groups are needed, the materials are saved, the preparation cost is low, and the method can be used for adsorbing and removing heavy metals, sulfanilamide antibiotics and nitrosamine disinfection byproducts.
In order to solve the technical problems, the invention provides the following technical scheme:
a method for preparing nano biochar balls by using syrup wastewater comprises the following steps:
s1: putting the syrup waste liquid, the lauryl sodium sulfate and the ultrapure water into a beaker, and stirring for 30min at the temperature of 40 ℃ at the speed of 300r/min for later use;
s2: transferring the solution treated in the step S1 to a high-pressure reaction kettle, carrying out high-pressure reaction for 2-8h at the temperature of 180-240 ℃, taking out and cooling to room temperature;
s3: and (4) performing suction filtration on the product treated in the step S2 by using a 0.22um water system filter membrane, washing the product subjected to suction filtration by using distilled water and absolute ethyl alcohol for three times, and performing vacuum drying at 80 ℃ for more than 12 hours to obtain the carbon nanospheres.
Further, the mass ratio of fructose, ultrapure water and sodium dodecyl sulfate in the syrup waste liquid in the step S1 is (100-200): 200: 1.
further, the mass of the syrup waste liquid and the mass of the sodium dodecyl sulfate in the step S1 are 10g and 0.05g, respectively, wherein the fructose content in the syrup waste liquid is 60 wt%, and the amount of the ultrapure water used in the step S1 is 10ml/g fructose.
Further, the nano carbon spheres prepared in the step S3 are put into a tube furnace, and N is introduced into the tube furnace2Calcining for 1-4h at the temperature of 300-600 ℃ in the atmosphere.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a new way for solving the treatment problem and resource utilization of the syrup wastewater, realizes the resource utilization of the syrup wastewater, and reduces the treatment cost and environmental pollution of the syrup wastewater as sewage; the invention prepares the nano-scale biological carbon spheres by a simple one-step method, has simple process and controllable process, and prepares the nano-scale biological carbon spheres which have large specific surface area (>924.5m2/g), micropores (2.13nm) and high microporosity (89.54%) and are more beneficial to adsorbing and removing pollutants by controlling reaction factors; according to the invention, C, N, P element existing in the syrup wastewater is utilized to convert the syrup wastewater into abundant surface hydroxyl, carboxyl, amino and phosphate groups in the preparation process of the nano biological carbon spheres, and no additional modification and modification of new groups are needed, so that the material can be saved, the preparation cost is reduced, the preparation cost is about 2000 yuan/ton according to the calculation of the inventor, and meanwhile, the surface of the prepared nano biological carbon spheres has positive and negative potentials and an amphoteric state, so that the adsorption and removal of heavy metals, sulfanilamide antibiotics and nitrosamine disinfection byproducts are facilitated; the invention can also realize the removal effect of the nano biological carbon spheres on anions and cations such as heavy metals, sulfonamide antibiotics and nitrosamine disinfection byproducts by regulating and controlling pH, and practice proves that the removal rates of the carbon spheres on lead ions and sulfadiazine are respectively as high as 99.1 percent and 98.65 percent.
Drawings
FIG. 1 is SEM images of nano bio-carbon spheres prepared under different conditions in example 1 of the present invention;
FIG. 2 is an XRD pattern of the nanobubble carbon spheres prepared under different conditions in example 1 of the present invention;
fig. 3 is a raman spectrum of the nanobiocarbon spheres prepared in example 1 of the present invention;
FIG. 4 is a FT-IR spectrum of the nanocarbon beads prepared in example 1 of the present invention;
FIG. 5 is an XPS spectrum of the nano bio-carbon spheres prepared in example 1 of the present invention;
FIG. 6 is a zeta potential diagram of the nanobiocarbon spheres prepared in example 1 of the present invention;
fig. 7 is a BET diagram of the nanobiocarbon spheres prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1:
a method for preparing nano biochar balls by using syrup wastewater comprises the following steps:
s1: putting the syrup waste liquid, the sodium dodecyl sulfate and the ultrapure water into a beaker, and stirring for 30min at the constant temperature of 40 ℃ at 300r/min for later use, wherein the mass of the syrup waste liquid and the mass of the sodium dodecyl sulfate are respectively 10g and 0.05g, the fructose content in the syrup waste liquid is 60 wt%, and the using amount of the ultrapure water is 10ml/g fructose;
s2: transferring the solution treated in the step S1 to a 100mL high-pressure reaction kettle, carrying out high-pressure reaction for 2-8h at the temperature of 180-240 ℃, taking out, and cooling to room temperature;
s3: performing suction filtration on the product treated in the step S2 by using a 0.22um water system filter membrane, cleaning the product after suction filtration by using distilled water and absolute ethyl alcohol for three times, and performing vacuum drying for more than 12 hours at the temperature of 80 ℃ to prepare carbon nanospheres;
s4: in order to further increase the number of surface groups and the specific surface area of the nanocarbon spheres, in this embodiment, the nanocarbon spheres prepared in step S3 are placed in a tube furnace, and N is introduced into the tube furnace2Calcining for 1-4h at the temperature of 300-600 ℃ in the atmosphere.
In this example, the prepared nano charcoal spheres were analyzed as follows:
(1) scanning Electron Microscope (SEM) analysis
When the inventor obtains the optimal reaction conditions, the inventor also forms uniform nano biological carbon spheres with different sizes by controlling different reaction conditions, the minimum size is about 200-300nm, and SEM images of the nano biological carbon spheres prepared under different conditions are shown in figure 1;
(2) x-ray diffraction (XRD) analysis
The crystal structure of the nano biological carbon spheres prepared by utilizing the syrup wastewater is analyzed through XRD, the XRD spectrum is shown in figure 2, and the carbon spheres have a wider peak at the position of 2 theta (21.56 degrees), which indicates the amorphous state of the spheres; a small peak also exists at the position of 43.57 degrees 2 theta, which corresponds to the (100) crystal face of the graphite carbon, and shows that the graphitization of the sphere shows that the nano biological carbon sphere prepared by the invention has strong adsorption capacity;
(3) raman spectroscopy (Raman) analysis
See FIG. 3, which shows that the depth is 1365cm-1And 1595cm-1Two obvious absorption peaks exist at the position, which are respectively attributed to the defects of C atom crystal lattices and the in-plane stretching vibration of C atom sp2 hybridization, the R value of the sphere is low, the graphitization degree is enhanced, and the adsorption capacity of the prepared nano biological carbon sphere is strong;
(4) infrared spectral analysis (FT-IR)
Referring to the attached figure 4, the infrared absorption peaks of the syrup wastewater nano biological carbon spheres are as follows: 3392cm-1Spectral band of (B) is due to O-H vibration, 1698cm-1Corresponding to an absorption peak of C ═ O, 1650cm-1Corresponds to δ NH2Absorption peak of (5), 1070cm-1And 1019cm-1Corresponding to C-O and P+-O-FT-IR results show that a large amount of-OH, -COOH, -NH2 and-PO (OH) exist on the surface of the prepared nano biological carbon spheres2The groups are beneficial to the adsorption of anions and cations in water by the nano biological carbon spheres;
(5) x-ray photoelectron spectroscopy (XPS) analysis
Referring to fig. 5, XPS spectrum shows that the prepared nano biological carbon spheres contain C, N, O, P elements, and the contents of C, N, O are 63.69%, 19.31% and 17%, respectively; FIG. 5b is an XPS peak separation plot of N1s, which plot can be divided into two peaks, 400.8eV and 399.3eV, with the peak at 400.8eV assigned to the C-N bond of N and the peak at 399.3eV assigned to the N-H bond of N; figure 5C reveals a high resolution XPS spectrum of C1s in the carbon sphere, with the peak at 290.4eV assigned to COOR bond, the peak at 288.1eV assigned to C ═ O bond of graphitic sp2 hybridized C, the peak at 286.3eV assigned to C-O bond of sp3 hybridized C, and the peak at 284.8eV assigned to C-C bond of sp3 hybridized C; FIG. 5d is an XPS peak separation plot of O1s in carbon spheres, which can be separated into three peaks 533.2eV, 532.9eV and 531.7eV, corresponding to C-O, C ═ O and O-H bonds, respectively; XPS spectrogram shows that a large amount of functional groups containing oxygen, nitrogen and phosphorus, such as hydroxyl, carboxyl, amino, phosphate and the like, exist on the surface of the nano biological carbon spheres of the syrup wastewater;
(6) zeta potential analysis
Referring to the attached figure 6, the Zeta potential diagram shows that the pH value of the prepared nano biological carbon sphere at the zero potential point is 4.1, and when the pH value is less than 4.1, the charge on the surface of the spherical nano biological carbon sphere is positive; when the pH value is more than 4.1, the charge on the surface of the spherical nano biological carbon sphere is negative; the nano biological carbon spheres prepared by the embodiment can remove anions and cations such as heavy metals, sulfanilamide antibiotics and nitrosamine disinfection byproducts by regulating and controlling pH;
(7) specific surface area (BET) analysis
Referring to FIG. 7 and Table 1, the specific surface area of the nano biological carbon spheres prepared from the syrup wastewater is 924.528m2·g-1Pore volume of 0.4915cm3·g-1The average pore size is 2.127nm, and the microporosity is 89.54%; the specific surface area result shows that the high specific surface area and the pore size of the nano biological carbon spheres in the syrup wastewater are beneficial to the adsorption of the nano biological carbon spheres to remove heavy metals, sulfanilamide antibiotics and nitrosamine disinfection byproducts.
TABLE 1 physical parameters of Nanobiotic carbon spheres
The invention provides a new way for solving the treatment problem and resource utilization of the syrup wastewater, realizes the resource utilization of the syrup wastewater, and reduces the treatment cost and environmental pollution of the syrup wastewater as sewage; the preparation method prepares the nano-scale carbon spheres by a simple one-step method, has simple process and controllable process, and prepares the nano-scale carbon spheres with large specific surface area (>924.5m2/g), micropores (2.13nm) and high microporosity (89.54 percent) by controlling reaction factors, and is more favorable for adsorbing and removing pollutants; according to the invention, C, N, P element existing in the syrup wastewater is utilized to convert the syrup wastewater into abundant surface hydroxyl, carboxyl, amino and phosphate groups in the preparation process of the nano biological carbon spheres, and no additional modification and modification of new groups are needed, so that the material can be saved, the preparation cost is reduced, the preparation cost is about 2000 yuan/ton according to the calculation of the inventor, and meanwhile, the surface of the prepared nano biological carbon spheres has positive and negative potentials and an amphoteric state, so that the adsorption and removal of heavy metals, sulfanilamide antibiotics and nitrosamine disinfection byproducts are facilitated; the invention can realize the removal effect of the nano biological carbon spheres on anions and cations such as heavy metals, sulfonamide antibiotics and nitrosamine disinfection byproducts by regulating and controlling pH, and practice proves that the removal rates of the carbon spheres on lead ions and sulfadiazine are respectively as high as 99.1 percent and 98.65 percent.
Example 2:
a method for preparing nano biochar balls by using syrup wastewater comprises the following steps:
s1: putting the syrup waste liquid, the sodium dodecyl sulfate and the ultrapure water into a beaker, stirring for 30min at the constant temperature of 40 ℃ at 300r/min, and keeping for later use, wherein the mass ratio of the fructose, the ultrapure water and the sodium dodecyl sulfate in the syrup waste liquid in the embodiment is (100-200): 200: 1;
s2: transferring the solution treated in the step S1 to a 100mL high-pressure reaction kettle, carrying out high-pressure reaction for 2-8h at the temperature of 180-240 ℃, taking out, and cooling to room temperature;
s3: performing suction filtration on the product treated in the step S2 by using a 0.22um water system filter membrane, cleaning the product after suction filtration by using distilled water and absolute ethyl alcohol for three times, and performing vacuum drying for more than 12 hours at the temperature of 80 ℃ to prepare carbon nanospheres;
s4: in order to further increase the number of surface groups and the specific surface area of the nanocarbon spheres, in this embodiment, the nanocarbon spheres prepared in step S3 are placed in a tube furnace, and N is introduced into the tube furnace2Calcining for 1-4h at the temperature of 300-600 ℃ in the atmosphere.
The above is an embodiment of the present invention. The embodiments and specific parameters in the embodiments are only for the purpose of clearly illustrating the verification process of the invention and are not intended to limit the scope of the invention, which is defined by the claims, and all equivalent structural changes made by using the contents of the specification and the drawings of the present invention should be covered by the scope of the present invention.
Claims (4)
1. The method for preparing the nano biochar balls by using the syrup wastewater is characterized by comprising the following steps of:
s1: putting the syrup waste liquid, the lauryl sodium sulfate and the ultrapure water into a beaker, and stirring for 30min at the temperature of 40 ℃ at the speed of 300r/min for later use;
s2: transferring the solution treated in the step S1 to a high-pressure reaction kettle, carrying out high-pressure reaction for 2-8h at the temperature of 180-240 ℃, taking out and cooling to room temperature;
s3: and (4) performing suction filtration on the product treated in the step S2 by using a 0.22um water system filter membrane, washing the product subjected to suction filtration by using distilled water and absolute ethyl alcohol for three times, and performing vacuum drying at 80 ℃ for more than 12 hours to obtain the carbon nanospheres.
2. The method for preparing nano biochar pellets from syrup wastewater as claimed in claim 1, wherein the mass ratio of fructose, ultrapure water and sodium dodecyl sulfate in the syrup wastewater in the step S1 is (100-200): 200: 1.
3. the method for preparing nano biochar pellets from syrup wastewater as claimed in claim 1, wherein the mass of the syrup wastewater and the mass of the sodium dodecyl sulfate in the step S1 are 10g and 0.05g respectively, wherein the fructose content in the syrup wastewater is 60 wt%, and the amount of the ultrapure water used in the step S1 is 10ml/g fructose.
4. The method for preparing nano biochar pellets by using syrup wastewater as claimed in claim 1, wherein the nano biochar pellets prepared in the step S3 are placed in a tube furnace, and N is introduced into the tube furnace2Calcining for 1-4h at the temperature of 300-600 ℃ in the atmosphere.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113120989A (en) * | 2021-05-25 | 2021-07-16 | 中国电建集团江西省电力建设有限公司 | Method for treating antibiotic-polluted water body by using functional green carbon material |
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| KR20100138212A (en) * | 2009-06-24 | 2010-12-31 | 한국과학기술연구원 | Method for preparing porous carbon ball from sugar with hydrothermal treatment |
| US20140021096A1 (en) * | 2010-12-22 | 2014-01-23 | Centre National De La Recherche Scientifique | Process for preparing a spherical material with a hierarchical porosity comprising metallic particles trapped in a mesostructured matrix |
| CN106082160A (en) * | 2016-06-02 | 2016-11-09 | 浙江大学 | Preparation method of Carbon Hollow material and products thereof |
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