CN113559839B - Preparation method of paper mill coagulation solid waste-based catalyst, product and application thereof - Google Patents
Preparation method of paper mill coagulation solid waste-based catalyst, product and application thereof Download PDFInfo
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- CN113559839B CN113559839B CN202110900660.5A CN202110900660A CN113559839B CN 113559839 B CN113559839 B CN 113559839B CN 202110900660 A CN202110900660 A CN 202110900660A CN 113559839 B CN113559839 B CN 113559839B
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
- C02F1/766—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens by means of halogens other than chlorine or of halogenated compounds containing halogen other than chlorine
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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
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Abstract
The invention relates to the technical field of catalysts, in particular to a preparation method of a concrete solid waste-based catalyst in a paper mill, a product and application thereof. The preparation method specifically comprises the steps of drying and anoxic cracking of the solid waste coagulated by the paper mill, and grinding to obtain the solid waste coagulated by the paper mill based catalyst. The invention takes the solid waste of the paper mill as the raw material to prepare the carbon-based catalyst material similar to graphite through anoxic pyrolysis, and has the excellent characteristics of acid and alkali resistance, adjustable electronic structure, low cost, high conductivity and the like; the catalytic material has very good purifying effect on micro pollutants in water, especially sulfadiazine, and the removal rate can reach 99%.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to a preparation method and application of a concrete solid waste-based catalyst in a paper mill.
Background
With the deterioration of the environment and the rapid development of civilization, the discharge of the organic degradation-resistant wastewater brings great difficulty to the environmental management. Sulfonamides are the most widely detected and earliest synthetic antibiotics in medical and veterinary practice. However, most antibiotics taken into the body are not absorbed, but are excreted into the environment. Even low concentrations of antibiotics can alter the microbiota, induce antibiotic-resistant bacteria, cause serious human health problems, and present unpredictable environmental risks. As a broad-spectrum antibiotic, the sulfonamide is difficult to remove by biological methods, and conventional chemical processes adopted by sewage treatment plants cannot be completely removed, and trace residues still remain in aquatic environments, so that efficient removal of micro-organic pollutants in water bodies becomes a technical problem to be solved by those skilled in the art.
Because the traditional biological treatment technology has very limited capability of removing organic refractory pollutants in water, advanced oxidation technology becomes a main means for people to treat the wastewater. Advanced oxidation processes create strong active species that attack persistent contaminants through the use of strong oxidants, among which periodate is of increasing interest due to its stability, ease of transportation and storage, and in some cases priority. However, periodate ions are relatively stable when present alone in an aqueous environment, and are difficult to directly oxidize and degrade organic pollutants in a water body, and rapid reaction efficacy is usually required under the condition of catalyst activation. The activation method of periodate is various and includes bimetallic activation, metal compound activation, freeze activation, ultrasonic treatment, alkali activation, ultraviolet activation and the like. Among them, the transition metal activation is one of the most promising choices, because no extra energy input is needed, the use condition is mild, the cost is low. However, the use of metals is limited by the excessive consumption of chemicals and the generation of metal mud, and therefore, there is a need to develop more environmentally friendly, highly active catalytic materials that further enhance the ability of the catalyst to activate periodate to remove different contaminants.
The paper industry is one of the fastest growing industries, and a large amount of coagulation waste generated in the production process also causes potential harm to the environment. The iron-based coagulant is widely used because of the advantages of wide pH value range, low cost, quick sedimentation and the like, so that the coagulating waste of the paper mill often contains a large amount of lignocellulose, iron and nitrogen elements, and therefore, if the catalyst for preparing the activated periodate by taking the coagulating waste of the paper mill as a raw material can be provided, the catalyst has important significance for efficiently removing micro-organic pollutants in water.
Disclosure of Invention
Based on the above, the invention provides a preparation method of a concrete solid waste-based catalyst for a paper mill, and a preparation method and application thereof.
A preparation method of a concrete solid waste-based catalyst for a paper mill comprises the following steps:
drying and anoxic cracking the solid waste of the paper mill, and grinding to obtain the solid waste-based catalyst of the paper mill.
Further, the coagulant of the solid waste coagulated in the paper mill is polymeric ferric sulfate.
Further, the drying specifically comprises: drying at 60-80 ℃ to constant weight, wherein the anoxic pyrolysis specifically comprises the following steps: under the condition of nitrogen, the temperature is 500-600 ℃ and the time is 1.5-2h.
Further, the grinding is specifically grinding through a 200-mesh sieve.
According to the second technical scheme, the preparation method of the paper mill coagulated solid waste-based catalyst is used for preparing the paper mill coagulated solid waste-based catalyst.
In a third technical scheme of the invention, the application of the papermaking factory coagulation solid waste-based catalyst in the treatment of water bodies containing micro-organic pollutants by activating periodate.
Further, the micro-organic pollutant is a sulfonamide, and the pH value of the water body containing the micro-organic pollutant is less than 8.
The fourth technical scheme of the invention is a method for degrading waste water containing micro-organic pollutants, which takes the solid waste-based catalyst coagulated in the paper mill as a catalyst and specifically comprises the following steps:
the catalyst is placed in waste water containing micro-organic pollutants, stirred and mixed uniformly, periodate is added under the stirring condition for reaction, and then the mixture is filtered.
Further, the concentration of the catalyst in the wastewater containing the micro-organic pollutants is 0.25-0.75g/L, the concentration of periodate in the wastewater containing the micro-organic pollutants is 1-7.5mM, the stirring speed is 350-450rpm, and the reaction time is 10-90min.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes the solid waste of the paper mill as the raw material to prepare the carbon-based catalyst material similar to graphite through anoxic pyrolysis, and has the excellent characteristics of acid and alkali resistance, adjustable electronic structure, low cost, high conductivity and the like; in a further preferred scheme, coagulant is used as a raw material of the solid waste coagulated in the paper mill of polymeric ferric sulfate, so that iron and nitrogen elements are introduced into an iron-nitrogen co-doped carbon-based catalyst material prepared from the carbon-based material, the iron-nitrogen co-doped carbon-based catalyst can provide more catalytic activation sites, thereby promoting an electron transfer mechanism and facilitating the degradation of pollutants, and simultaneously, the introduction of heteroatoms can change the electron distribution of the carbon-based material, destroy the chemical inertness of the carbon-based material and introduce active sites; and the iron can be used as an activator of periodate, so that the degradation of pollutants is promoted; in the degradation process, iron atoms and nitrogen atoms can absorb electrons from adjacent carbon atoms to form electron-rich centers, periodate ions are easy to adsorb, electrons are further promoted to be transferred to periodate, and for sulfadiazine wastewater, the electrons are finally promoted to be transferred to periodate through a catalyst by sulfadiazine due to the fact that the ammonium radical of the sulfadiazine is easy to lose electrons, a closed electronic ring is formed, the effect of a non-free radical degradation mechanism leading to the transfer of electrons is promoted, and therefore the performance of catalytic degradation of pollutants is improved, and the sulfadiazine wastewater has a good application prospect in the fields of water purification and the like.
The catalytic material has very good purifying effect on micro pollutants in water, especially sulfadiazine, and the removal rate can reach 99%.
Drawings
FIG. 1 is a scanning electron microscope image of a paper mill coagulated solid waste-based catalyst in example 1 of the present invention;
FIG. 2 is a high resolution transmission electron microscope image of a paper mill coagulated solid waste-based catalyst in example 1 of the present invention;
FIG. 3 is an X-ray diffraction spectrum of a solid waste-based catalyst for paper mill coagulation in example 1 of the present invention;
FIG. 4 is a graph showing the result of X-ray photoelectron spectroscopy analysis of a solid waste-based catalyst coagulated in a paper mill in example 1 of the present invention, wherein (a) is a Fe2p spectrum and (b) is an N1s spectrum;
FIG. 5 is a plot of the effect of CWBC/PI on sulfadiazine degradation rate at different catalyst concentrations in an efficacy verification example of the present invention;
FIG. 6 is a plot of the effect of CWBC catalytic material on sulfadiazine degradation rate at different pH values in an effect verification example of the present invention;
FIG. 7 is a line graph showing the effect of CWBC catalytic materials on sulfadiazine degradation rate at different PI concentrations in an efficacy verification example of the present invention.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, 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 invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
Example 1
Drying 20g of paper mill coagulated solid waste (coagulant is polymeric ferric sulfate) taking rice straw as a raw material in a vacuum drying oven at 60 ℃ for 12 hours to obtain the coagulated solid waste dried to constant weight; putting a certain amount of solid waste into a porcelain boat, and cracking in a vacuum tube furnace under the nitrogen atmosphere, wherein the reaction condition is 550 ℃ for 2 hours; grinding the composite material generated after the reaction in a porcelain boat, and sieving the ground composite material with a 200-mesh sieve to obtain 6g of a paper mill-based concrete solid waste-based catalyst material (CWBC).
The prepared solid waste-based catalyst material for paper mill coagulation was subjected to surface scanning electron microscopy (fig. 1), transmission electron microscopy (fig. 2), X-ray diffraction spectroscopy (fig. 3) and X-ray photoelectron spectroscopy (fig. 4).
As can be seen from fig. 1, the CWBC has a fluffy structure with iron and nitrogen materials distributed on a carbon-based material, indicating that iron and nitrogen are co-doped in the CWBC, wherein the Si element originates from the paper making process.
As can be seen from FIG. 2, the CWBC catalyst has an irregular multi-layer structure, a plurality of spherical black particles are uniformly dispersed in a carbon matrix, and the calculated lattice distance of the black particles is 0.221nm, corresponding to Fe 2 O 3 The (113) crystal plane of (b) indicates the presence of Fe oxide. Further, the transmission electron microscope image showed that the lattice spacing calculated for the carbon matrix was 0.337nm, and the lattice spacing (sp 2 Hybrid) indicating the presence of graphitic carbon.
As can be seen from fig. 3, the CWBC is an amorphous structure, and has a wide dispersion peak at 2θ=23°, corresponding to the (002) diffraction plane of the structure of six Fang Danmo, and the peak of the spectrum may be due to the presence of an inorganic phase in the papermaking solid waste, such as silicon, sodium, iron, and the like. No characteristic peak of iron was observed in XRD due to the small content of iron in the material.
As can be seen from fig. 4 (a): fe2p spectrum at 711.35eV,719.46eV,723.19eV and 732.9eV corresponds to Fe2p of Fe (III), respectively 3/2 And Fe2p 1/2 And their satellite peaks. 714.97eV and 728.1eV correspond to Fe (II) 2p 1/2 Spectrum and satellite peaks. Thus, XPS iron spectrum shows iron as FeO and Fe 2 O 3 Is present in CWBC. The peak splitting results of XPS N1s spectrum (FIG. 4 (b)) are 398.29eV,400.48eV,403.72eV and 408.02eV for pyridine nitrogen, pyrrole nitrogen, graphite nitrogen and nitrogen oxide, respectively.
Effect verification example
Taking Sulfadiazine (SDZ) as an example, the technical effect of the product of the example 1 on removing pollutants by activating periodate is verified, and the specific test method is as follows:
the catalytic material of example 1 was uniformly suspended in a 250mL beaker containing 100mL of SDZ solution (40. Mu.M) with the catalyst concentration (0.25 g/L, 0.50g/L, 0.75 g/L), the pH of the sulfadiazine solution (3, 5, 7, 9, 11), and the periodate concentration (1.0 mM, 2.5mM, 5.0mM, 7.5 mM) as variables, respectively. The mixed suspension was stirred at 400rpm on a magnetic stirrer, and then sodium Periodate (PI) was added to a concentration of 5mM. At specific time intervals, 1mL of the solution was extracted from the reactor, filtered through a 0.22 μm aqueous filter, and immediately thereafter, 20. Mu.L of Na was used 2 S 2 O 3 (1M) after quenching, the SDZ removal effect was examined.
FIG. 5 is a plot showing the effect of CWBC/PI on sulfadiazine degradation at various catalyst concentrations, as seen from the graph, when the catalyst level was varied from 0.25 to 0.25g L -1 Increased to 0.50g L -1 When SDZ degradation efficiency is improved, the corresponding pseudo first order reaction rate constant (k obs ) 0.0219min respectively -1 And 0.0586min -1 . However, as the catalyst concentration further increased to 0.75g L -1 At the time, the reaction rate constant k obs Reducing to 0.0319min -1 . This phenomenon may be due to the limitation of PI concentration, resulting in a higher concentration of catalyst that cannot further increase the reaction rate. Thus, 0.5. 0.5g L is selected -1 The optimal dosage of the CWBC catalyst is obtained.
FIG. 6 is a plot of the effect of CWBC catalytic materials on sulfadiazine degradation rate at different pH values; as seen from the figure, SDZ can degrade rapidly under strongly acidic and near neutral pH conditions, achieving optimal removal at pH3.0 (98.94% removal in 90 minutes). Since the zero charge point of CWBC is between 3.0 and 5.0, at ph=3.0, the potential of CWBC is positive, reducing electrostatic repulsion between periodate anions and positively charged catalyst surface, contributing to CWBC activation of PI. In contrast, when the pH was increased above 3.12, the CWBC surface was negatively charged due to the decrease in zeta potential of CWBC, indicating that the increased pH caused electrostatic repulsion between CWBC and PI, resulting in suppressed dynamic SDZ degradation. In addition, the seven-valent iodine ions have different existence forms under different pH values, and IO is lower than 8.0 4 - The material predominates and, at a pH of 8.0, dimerizes to form (H 3 IO 6 2- ) Is the main substance. And IO (input/output) 4 - /IO 3 - (1.298V) reduction potential compared with H 3 IO 6 2- /IO 3 - The lower reduction potential of (0.686V) may also be the reason for the relatively low degradation efficiency of SDZ at higher pH values.
FIG. 7 is a plot of the effect of CWBC catalytic material on sulfadiazine degradation rate at different PI concentrations; as seen from the graph, the removal rate of SDZ was significantly improved with increasing PI concentration (1 mM, 2.5mM, 5.0mM and 7.5 mM). Higher concentrations of PI may produce more active species, resulting in a SDZ degradation rate of from 0.0097min when PI concentration is increased from 1.0mM to 5.0mM -1 Increase to 0.0586min -1 . However, as the PI concentration was increased from 5.0mM to 7.5mM, although the final removal efficiency was hardly changed, the reaction rate constant k was obs The increase rate of (1) is greatly slowed down (from 0.0586 to 0.0601 min) -1 ). This phenomenon can be explained in the following way: firstly, excessive PI can compete with SDZ for reactive free radicals, and secondly, when PI concentration is below 5.0mM, the amount of CWBC administered is excessive relative to PI concentration, however, as PI concentration increases further above 5mM, higher concentrations of PI cannot be fully activated due to CWBC dose limitations, and thus the magnitude of SDZ removal is not great.
The test results show that the catalytic material based on the paper mill coagulation solid waste prepared by the method can activate PI and has high-efficiency catalytic oxidation performance on sulfadiazine. The catalytic material can purify other organic matters in the solution by a catalytic oxidation method, and has good application prospect and significance in reducing the pollution of organic pollutants in wastewater.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (3)
1. The application of the paper mill coagulated solid waste-based catalyst in the treatment of water bodies containing sulfonamides by activated periodate is characterized in that the paper mill coagulated solid waste-based catalyst is prepared by the following steps: drying and performing anoxic pyrolysis on the solid waste coagulated by the paper mill, and grinding to obtain a solid waste coagulated catalyst;
the coagulant of the solid waste coagulated in the paper mill is polymeric ferric sulfate;
the drying is specifically as follows: drying at 60-80 ℃ to constant weight, wherein the anoxic pyrolysis specifically comprises the following steps: under the condition of nitrogen, the temperature is 500-600 ℃ for 1.5-2h;
the sulfadiazine is sulfadiazine.
2. Use according to claim 1, wherein the grinding is in particular grinding through a 200 mesh screen.
3. The use according to claim 1, characterized in that it comprises in particular the following steps:
placing the catalyst into waste water containing micro-organic pollutants, stirring and uniformly mixing, adding periodate under the stirring condition for reaction, and filtering;
the concentration of the catalyst in the wastewater containing the micro-organic pollutants is 0.5g/L, the concentration of periodate in the wastewater containing the micro-organic pollutants is 5-7.5mM, the stirring speed is 350-450rpm, and the reaction time is 10-90min;
the micro-organic pollutant is sulfadiazine, and the pH value of the wastewater containing the micro-organic pollutant is 3.
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| CN107265606A (en) * | 2017-07-21 | 2017-10-20 | 中国地质大学（武汉） | A kind of method that removal organic polluter is removed based on periodate oxidation |
| CN109179626A (en) * | 2018-10-15 | 2019-01-11 | 南京师范大学 | A method of utilizing sulphadiazine in coagulation sludge activation persulfate degradation water |
| CN110227534A (en) * | 2019-07-16 | 2019-09-13 | 河南省科学院化学研究所有限公司 | A kind of magnetic N doping biology Pd/carbon catalyst and preparation method thereof based on sludge |
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| CN107265606A (en) * | 2017-07-21 | 2017-10-20 | 中国地质大学（武汉） | A kind of method that removal organic polluter is removed based on periodate oxidation |
| CN109179626A (en) * | 2018-10-15 | 2019-01-11 | 南京师范大学 | A method of utilizing sulphadiazine in coagulation sludge activation persulfate degradation water |
| CN110227534A (en) * | 2019-07-16 | 2019-09-13 | 河南省科学院化学研究所有限公司 | A kind of magnetic N doping biology Pd/carbon catalyst and preparation method thereof based on sludge |
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