CN116712980B - Chitosan modified tiamulin waste salt activated carbon as well as preparation method and application thereof - Google Patents
Chitosan modified tiamulin waste salt activated carbon as well as preparation method and application thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 130
- UURAUHCOJAIIRQ-QGLSALSOSA-N tiamulin Chemical class CCN(CC)CCSCC(=O)O[C@@H]1C[C@@](C)(C=C)[C@@H](O)[C@H](C)[C@@]23CC[C@@H](C)[C@]1(C)[C@@H]2C(=O)CC3 UURAUHCOJAIIRQ-QGLSALSOSA-N 0.000 title claims abstract description 78
- 239000002699 waste material Substances 0.000 title claims abstract description 77
- 150000003839 salts Chemical class 0.000 title claims abstract description 70
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229960004885 tiamulin Drugs 0.000 claims abstract description 38
- HOQPTLCRWVZIQZ-UHFFFAOYSA-H bis[[2-(5-hydroxy-4,7-dioxo-1,3,2$l^{2}-dioxaplumbepan-5-yl)acetyl]oxy]lead Chemical compound [Pb+2].[Pb+2].[Pb+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HOQPTLCRWVZIQZ-UHFFFAOYSA-H 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 238000004321 preservation Methods 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000007833 carbon precursor Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 12
- 238000005470 impregnation Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000012986 modification Methods 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 9
- 238000010000 carbonizing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 238000000197 pyrolysis Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 23
- 230000000694 effects Effects 0.000 abstract description 20
- 238000000034 method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 7
- KVCGISUBCHHTDD-UHFFFAOYSA-M sodium;4-methylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1 KVCGISUBCHHTDD-UHFFFAOYSA-M 0.000 description 6
- ZRZNJUXESFHSIO-UHFFFAOYSA-N Pleuromutilin Natural products CC1C(O)C(C)(C=C)CC(OC(=O)CO)C2(C)C(C)CCC31C2C(=O)CC3 ZRZNJUXESFHSIO-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- ZRZNJUXESFHSIO-VYTKZBNOSA-N pleuromutilin Chemical compound C([C@H]([C@]1(C)[C@@H](C[C@@](C)(C=C)[C@@H](O)[C@@H]2C)OC(=O)CO)C)C[C@]32[C@H]1C(=O)CC3 ZRZNJUXESFHSIO-VYTKZBNOSA-N 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004176 ammonification Methods 0.000 description 2
- 238000011067 equilibration Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- YBDSNEVSFQMCTL-UHFFFAOYSA-N 2-(diethylamino)ethanethiol Chemical compound CCN(CC)CCS YBDSNEVSFQMCTL-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical class OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241000222350 Pleurotus Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229930004069 diterpene Natural products 0.000 description 1
- 150000004141 diterpene derivatives Chemical class 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- -1 p-toluenesulfonyl Chemical group 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
-
- 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
-
- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
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- Hydrology & Water Resources (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The application discloses chitosan modified tiamulin waste salt activated carbon and a preparation method and application thereof, and belongs to the technical field of wastewater treatment and adsorption materials. In the process of treating lead in different complex states by using tiamulin waste salt activated carbon, the adsorption effects of the tiamulin waste salt activated carbon are obviously different. Aiming at the problem that the adsorption effect of tiamulin waste salt activated carbon on lead citrate and the like is poor, the application provides chitosan modified tiamulin waste salt activated carbon, and a preparation method and application thereof. According to the method, the chitosan is utilized to modify the tiamulin waste salt activated carbon, so that the chitosan modified tiamulin waste salt activated carbon (CFAC) is prepared, and is used for adsorbing complex lead, so that the adsorption effect is remarkably improved.
Description
Technical Field
The application belongs to the technical field of wastewater treatment and adsorption materials, and particularly relates to chitosan modified tiamulin waste salt activated carbon, and a preparation method and application thereof.
Background
The tiamulin is prepared by fermenting higher fungus basidiomycete Pleurotus Pleurotus mutilus to obtain pleuromutilin, and then chemically synthesizing to obtain hydrogenated fumarate, and is a diterpene special antibiotic for livestock and poultry. The first proposal in 1951 by Kavangh in Australia, the beginning of the extensive study in 60 s, is one of ten animals in the world. At present, when tiamulin is synthesized at home and abroad, the tiamulin is synthesized by firstly performing p-toluenesulfonylation on pleuromutilin to form pleuromutilin sulfonate and then reacting the pleuromutilin sulfonate with diethylaminoethanethiol (ammoniation reaction). In the ammonification reaction process, due to substitution reaction, p-toluenesulfonyl reacts with sodium hydroxide to generate a large amount of byproducts, namely sodium p-toluenesulfonate, so that the ammonification wastewater has a high COD value.
In the related art, for example, the Chinese patent publication No. CN104262210A describes a method for extracting sodium paratoluenesulfonate from tiamulin synthetic wastewater, and the sodium paratoluenesulfonate is extracted and recovered, so that waste is changed into valuable and available resources are increased.
However, the inventor finds that even though the components contained in the waste liquid are too complex, the sodium paratoluenesulfonate still needs to be subjected to a time-consuming and labor-consuming purification process in the later stage, otherwise, the recovered sodium paratoluenesulfonate basically belongs to a waste salt line, and no mature purification process exists in the prior research, so that the recovery of the sodium paratoluenesulfonate from the waste liquid in the tiamulin production process is actually impractical. The Chinese patent publication No. CN112919463A describes an activated carbon prepared by using tiamulin waste salt and a preparation method thereof, wherein the activated carbon is prepared by calcining the tiamulin waste salt serving as a raw material, namely the tiamulin waste salt activated carbon (FAC).
In the subsequent further research, the adsorption effect of the tiamulin waste salt activated carbon is found to be obviously different when the tiamulin waste salt activated carbon adsorbs lead in different complex states, for example, the adsorption effect of the tiamulin waste salt activated carbon on lead Citrate (Citrate-Pb (II)) is poor.
Disclosure of Invention
1. Problems to be solved
Aiming at the problem that the adsorption effect of the tiamulin waste salt activated carbon on part of complex lead is poor, the application provides the chitosan modified tiamulin waste salt activated carbon, the preparation method and the application thereof, the chitosan is utilized to modify the tiamulin waste salt activated carbon (FAC) to prepare the chitosan modified tiamulin waste salt activated carbon (CFAC), and the chitosan modified tiamulin waste salt activated carbon (CFAC) is used for adsorbing the complex lead, so that the adsorption effect is obviously improved.
2. Technical proposal
In order to solve the problems, the technical scheme adopted by the application is as follows:
the application provides a preparation method of chitosan modified tiamulin waste salt activated carbon, which refers to Chinese patent invention with publication number of CN112919463A, and the method utilizes chitosan to modify the tiamulin waste salt activated carbon and specifically comprises the following steps:
s1, concentrating tiamulin production waste liquid, separating to obtain a solid raw material, and concentrating the solid raw material, wherein the concentrating comprises high-temperature evaporation at 95-115 ℃;
s2, carbonizing the solid raw materials to obtain a carbon precursor A, wherein the carbonizing treatment comprises a heating stage and a heat preservation stage, the heating speed is 4-10 ℃/min, the heat preservation temperature is 400-500 ℃, and the heat preservation time is 60-180 min;
s3, carrying out pyrolysis treatment on the carbon precursor A to obtain a carbon precursor B; the pyrolysis treatment comprises a heating stage and a heat preservation stage, wherein the heating speed is 4-10 ℃/min, the heat preservation temperature is 600-900 ℃, and the heat preservation time is 90-180 min;
s4, washing the carbon precursor B to be neutral by pure water, and drying to obtain tiamulin waste salt activated carbon FAC;
s5, dissolving chitosan in acetic acid solution to prepare a modifier, carrying out impregnation modification on the tiamulin waste salt activated carbon FAC obtained in the S4, carrying out impregnation treatment by using NaOH solution after filtering, repeatedly washing to be neutral by using deionized water, and drying to obtain the chitosan modified tiamulin waste salt CFAC.
Further, in the above S2, the temperature rising rate is 10 ℃/min.
Further, in the above step S2, the temperature is 500℃and the time is 120 minutes.
Further, in the above S3, the temperature rising rate is 10 ℃/min.
Further, in the above step S3, the temperature is 800℃and the time is 150 minutes.
Further, in S5, the chitosan is used in an amount of 2 to 4g per 50mL of 1% acetic acid solution. Further, the chitosan was used in an amount of 3g.
Further, in the above step S5, the immersion modification time is 12 to 36 hours. Further, the dip modification time was 24 hours.
Further, in the above S5, the NaOH solution impregnation treatment includes an impregnation treatment with 1mol/L NaOH solution for 12 to 36 hours. Further, the dipping treatment was carried out for 24 hours.
The application also provides the chitosan modified tiamulin waste salt activated carbon prepared by the preparation method of the chitosan modified tiamulin waste salt activated carbon.
The invention also provides application of the chitosan modified tiamulin waste salt activated carbon in adsorption removal of complex lead in the environment.
Further, the complex lead includes lead Citrate (Citrate-Pb (II)).
Further, the above application includes adjusting the pH of the environment to 2 to 10. Further, the pH of the environment was adjusted to 4.
Further, the environment includes a water environment.
3. Advantageous effects
Compared with the prior art, the application has the beneficial effects that:
(1) According to the chitosan modified tiamulin waste salt activated carbon, the preparation method and the application thereof, the chitosan is used for modifying the tiamulin waste salt activated carbon, and the prepared chitosan modified tiamulin waste salt activated carbon has high pore volume and high specific surface area, so that more adsorption sites are provided for adsorbing complex lead.
(2) The chitosan modified tiamulin waste salt activated carbon and the preparation method and application thereof are used for adsorbing and removing complex lead, particularly Citrack-Pb (II), the adsorption effect is improved to 99.6% from 33.4% of the tiamulin waste salt activated carbon, and the adsorption effect is remarkably improved.
Drawings
Fig. 1 is an SEM image of chitosan modified tiamulin waste salt activated carbon CFAC prepared herein.
Fig. 2 is an SEM image of chitosan modified tiamulin waste salt activated carbon CFAC prepared herein.
Fig. 3 is an SEM image of chitosan modified tiamulin waste salt activated carbon CFAC prepared herein.
Fig. 4 is a graph showing the effect of tiamulin waste salt activated carbon FAC on adsorbing lead in different complex states.
FIG. 5 is a comparison of the effect of the chitosan modified tiamulin waste salt activated carbon CFAC prepared in the present application on adsorption of Citrite-Pb and NAT-Pb (II) by tiamulin waste salt activated carbon FAC.
FIG. 6 is a comparison of the effect of chitosan modified tiamulin waste salt activated carbon CFAC on adsorption of Citrack-Pb under different pH conditions.
Detailed Description
The present application is further described below in connection with specific embodiments.
The terms such as "upper", "lower", "left", "right", "middle" and the like referred to in the present specification are also for convenience of description, and are not intended to limit the scope of the present invention, but rather to limit the scope of the present invention, and the changes or modifications of the relative relationship are considered to be within the scope of the present invention without substantial modification of the technical content.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
As used herein, the term "about" is used to provide the flexibility and inaccuracy associated with a given term, metric or value. The degree of flexibility of a particular variable can be readily determined by one skilled in the art.
As used herein, the term "is intended to be synonymous with" one or more of ". For example, "at least one of A, B and C" expressly includes a only, B only, C only, and respective combinations thereof.
Concentrations, amounts, and other numerical data may be presented herein in a range format. It is to be understood that such range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, a numerical range of about 1 to about 4.5 should be interpreted to include not only the explicitly recited limits of 1 to about 4.5, but also include individual numbers (such as 2, 3, 4) and subranges (such as 1 to 3, 2 to 4, etc.). The same principles apply to ranges reciting only one numerical value, such as "less than about 4.5," which should be construed to include all such values and ranges. Moreover, such an interpretation should apply regardless of the breadth of the range or the characteristics being described.
Example 1
The embodiment provides a preparation method of chitosan modified tiamulin waste salt activated carbon CFAC and the chitosan modified tiamulin waste salt activated carbon prepared by the method, which comprises the following steps:
s1, concentrating tiamulin production waste liquid, separating to obtain a solid raw material, and concentrating the solid raw material, wherein the concentrating comprises high-temperature evaporation at 95-115 ℃;
s2, carbonizing the solid raw material to obtain a carbon precursor A, wherein the carbonizing treatment comprises a heating stage and a heat preservation stage, the heating speed is 10 ℃/min, the heat preservation temperature is 500 ℃, and the heat preservation time is 120min;
s3, carrying out pyrolysis treatment on the carbon precursor A to obtain a carbon precursor B, wherein the pyrolysis treatment comprises a heating stage and a heat preservation stage, the heating speed is 10 ℃/min, the heat preservation temperature is 800 ℃, and the heat preservation time is 150min;
s4, washing the carbon precursor B to be neutral by pure water, and drying to obtain tiamulin waste salt activated carbon FAC;
s5, dissolving 3g of chitosan in 50mL of 1% acetic acid solution to prepare a modifier, carrying out impregnation modification on the tiamulin waste salt activated carbon FAC obtained in the S4 for 24 hours, carrying out impregnation treatment on the obtained product by 1mol/L NaOH solution after filtration for 24 hours, repeatedly washing the product to be neutral by deionized water, and drying the product to obtain the chitosan modified tiamulin waste salt CFAC.
Analysis of results:
fig. 1 to 3 are SEM images of the chitosan-modified tiamulin waste salt activated carbon CFAC prepared in this example, and it can be seen from the images that the chitosan-modified tiamulin waste salt activated carbon CFAC has developed pore structures of different sizes, and the specific surface area thereof is increased.
Example 2
This example provides the use of tiamulin waste salt activated carbon FAC prepared in example 1 for adsorbing Pb (ii) in complex form bound to different ligands, comprising in particular the following steps:
s1: 40mg of tiamulin waste salt activated carbon FAC prepared in example 1 is added into 50mL of 20ppm different Pb complex solutions with the pH value adjusted to 2, wherein the solutions are EDTA-Pb (II), NTA-Pb (II), DTPA-Pb (II) and Citite-Pb (II) respectively, and the solutions are placed into a shaking table with the temperature of 25 ℃ and the rotating speed of 200 r/min;
s2: during the reaction, 1.5mL of the mixture is sampled in 5, 15, 30, 60, 120 and 360min respectively, and the mixture is filtered by a water phase filter head with the diameter of 0.22 mu m;
s3: the concentration of Pb (II) complex remaining in the solution was determined by ICP-OES, and a reaction curve was drawn.
As shown in the figure 4, the tiamulin waste salt activated carbon FAC has good adsorption effect on EDTA-Pb (II) and DTPA-Pb (II); the adsorption effect on NTA-Pb (II) and Citite-Pb (II) is poor.
Example 3
The embodiment provides application of the chitosan modified tiamulin waste salt activated carbon CFAC prepared in the embodiment 1, which is used for adsorbing NTA-Pb (II) and Citrack-Pb (II), and specifically comprises the following steps:
s1: 40mg of the chitosan modified tiamulin waste salt activated carbon CFAC prepared in the example 1 is respectively added into 50mL of 20ppm of solution of Citrite-Pb (II) and NTA-Pb (II), and the mixture is placed into a shaking table with the temperature of 25 ℃ and the rotating speed of 200 r/min;
s2: after equilibration, 1.5mL of sample was taken and filtered through a 0.22 μm aqueous filter;
s3: the concentration of Pb remaining in the solution was determined by ICP-OES.
As shown in figure 5, the adsorption effect of the chitosan modified tiamulin waste salt activated carbon CFAC on Citrite-Pb (II) can reach 99.6%, and compared with the adsorption effect of the tiamulin waste salt activated carbon FAC, the adsorption effect is remarkably improved. Correspondingly, the adsorption effect of the chitosan modified tiamulin waste salt activated carbon CFAC on NTA-Pb (II) is not improved, but is reduced compared with that before being modified.
Example 4
This example provides the application of chitosan modified tiamulin waste salt activated carbon CFAC prepared in example 1 to adsorption of Citrack-Pb (II) solutions with different initial pH values, comprising the following steps:
s1: 40mg of chitosan modified tiamulin waste salt activated carbon CFAC prepared in example 1 is added into 50mL of 20ppm Citrate-Pb (II) solution with pH adjusted to 2, 4, 6, 8 and 10, and the solution is placed into a shaking table with the temperature of 25 ℃ and the rotating speed of 200 r/min;
s2: after equilibration, 1.5mL of sample was taken and filtered through a 0.22 μm aqueous filter;
s3: the concentration of residual Citrite-Pb (II) in the solution was determined by ICP-OES.
As shown in FIG. 6, the chitosan modified tiamulin waste salt activated carbon CFAC can adsorb Citrate-Pb (II) at pH 2-10, and the adsorption effect is optimal when pH=4.
Example 5
The embodiment provides a preparation method of chitosan modified tiamulin waste salt activated carbon CFAC and the chitosan modified tiamulin waste salt activated carbon prepared by the method, which comprises the following steps:
s1, concentrating tiamulin production waste liquid, separating to obtain a solid raw material, and concentrating the solid raw material, wherein the concentrating comprises high-temperature evaporation at 95-115 ℃;
s2, carbonizing the solid raw material to obtain a carbon precursor A, wherein the carbonizing treatment comprises a heating stage and a heat preservation stage, the heating speed is 4 ℃/min, the heat preservation temperature is 400 ℃, and the heat preservation time is 60min;
s3, carrying out pyrolysis treatment on the carbon precursor A to obtain a carbon precursor B, wherein the pyrolysis treatment comprises a heating stage and a heat preservation stage, the heating speed is 4 ℃/min, the heat preservation temperature is 600 ℃, and the heat preservation time is 180min;
s4, washing the carbon precursor B to be neutral by pure water, and drying to obtain tiamulin waste salt activated carbon FAC;
s5, dissolving 2g of chitosan in 50mL of 1% acetic acid solution to prepare a modifier, carrying out impregnation modification on the tiamulin waste salt activated carbon FAC obtained in the S4 for 36h, carrying out impregnation treatment on the obtained product by 1mol/L NaOH solution after filtration for 36h, repeatedly washing the product to be neutral by deionized water, and drying the product to obtain the chitosan modified tiamulin waste salt CFAC.
Claims (6)
1. The application of chitosan modified tiamulin waste salt activated carbon in adsorbing and removing complex lead in the environment is characterized in that the complex lead comprises lead citrate;
the preparation method of the chitosan modified tiamulin waste salt activated carbon specifically comprises the following steps:
s1, concentrating tiamulin production waste liquid, separating to obtain a solid raw material, and concentrating the solid raw material, wherein the concentrating comprises high-temperature evaporation at 95-115 ℃;
s2, carbonizing the solid raw material in the step S1 to obtain a carbon precursor A, wherein the carbonizing treatment comprises a heating stage and a heat preservation stage, the heating speed is 4-10 ℃/min, the heat preservation temperature is 400-500 ℃, and the heat preservation time is 60-180 min;
s3, carrying out pyrolysis treatment on the carbon precursor A to obtain a carbon precursor B, wherein the pyrolysis treatment comprises a heating stage and a heat preservation stage, the heating speed is 4-10 ℃/min, the heat preservation temperature is 600-900 ℃, and the heat preservation time is 90-180 min;
s4, washing the carbon precursor B to be neutral by pure water, and drying to obtain tiamulin waste salt activated carbon FAC;
s5, dissolving chitosan in acetic acid solution to prepare a modifier, carrying out impregnation modification on the tiamulin waste salt activated carbon FAC obtained in the S4, carrying out impregnation treatment by using NaOH solution after filtering, repeatedly washing to be neutral by using deionized water, drying to obtain chitosan modified tiamulin waste salt CFAC,
the dipping modification time in the step S5 is 12-36 hours; the NaOH solution dipping treatment comprises the step of using the NaOH solution to dip for 12-36 hours.
2. The use according to claim 1, characterized in that the use comprises adjusting the pH of the environment to 2-10.
3. The use according to claim 1, wherein the holding temperature in S2 is 500 ℃ and the holding time is 120min.
4. The use according to claim 1, wherein the holding temperature in S3 is 800 ℃ and the holding time is 150min.
5. The use according to claim 3 or 4, wherein the heating rate in S2 and S3 is 10 ℃/min.
6. The use according to claim 1, wherein the chitosan is used in an amount of 2-4 g relative to 50mL of 1% acetic acid solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310707045.1A CN116712980B (en) | 2023-06-14 | 2023-06-14 | Chitosan modified tiamulin waste salt activated carbon as well as preparation method and application thereof |
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| CN202310707045.1A CN116712980B (en) | 2023-06-14 | 2023-06-14 | Chitosan modified tiamulin waste salt activated carbon as well as preparation method and application thereof |
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| Publication Number | Publication Date |
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| CN116712980A CN116712980A (en) | 2023-09-08 |
| CN116712980B true CN116712980B (en) | 2024-03-08 |
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