CN110787835A - Preparation method of peanut shell melamine biochar composite material - Google Patents
Preparation method of peanut shell melamine biochar composite material Download PDFInfo
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- CN110787835A CN110787835A CN201911117906.0A CN201911117906A CN110787835A CN 110787835 A CN110787835 A CN 110787835A CN 201911117906 A CN201911117906 A CN 201911117906A CN 110787835 A CN110787835 A CN 110787835A
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0234—Nitrogen-, phosphorus-, arsenic- or antimony-containing compounds
- B01J31/0235—Nitrogen containing compounds
- B01J31/0244—Nitrogen containing compounds with nitrogen contained as ring member in aromatic compounds or moieties, e.g. pyridine
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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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- 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
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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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
- C02F2101/306—Pesticides
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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
- C02F2101/34—Organic compounds containing oxygen
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
Abstract
The invention discloses a preparation method of a peanut shell melamine biochar composite material, which comprises the following steps: s1, preparing peanut shell powder; s2, preparing a mixture; s3, drying, grinding and calcining the mixture at high temperature to obtain the melamine composite material of the peanut shell; the invention adopts waste biomass peanut shells as raw materials, and the novel biochar composite material prepared by mixing melamine with the waste biomass peanut shells is applied to the ozone catalysis process, the composite material forms a mutually stacked sheet structure after high-temperature calcination, the specific surface area is enhanced, the aromatization is high, the capability of decomposing ozone to generate hydroxyl radicals is enhanced, the preparation process of the composite catalyst is simple and easy to realize, no metal ions are dissolved out in the catalytic oxidation process, no secondary pollution is caused, and the composite catalyst can be applied to the advanced treatment process of municipal domestic sewage, surface water and industrial reuse water.
Description
Technical Field
The invention belongs to the technical field of organic pollution catalysis, and particularly relates to a preparation method of a peanut shell melamine biochar composite material.
Background
Ozone is an allotrope of oxygen and is an unstable light purple gas at normal temperature and pressure. Owing to its strong oxidizing property, it is widely used for deodorization and sterilization of water and air, as well as for decoloration of waste water and removal of organic matter. Ozone can react with organic substances in two ways, namely directly and indirectly, and firstly, the ozone directly reacts with various pollutants in water, such as odor-generating cyclic aliphatic compounds, trihalomethanes and inactive aromatic compounds; secondly, ozone is decomposed into hydroxyl free radicals (OH) with stronger oxidability in the reaction for indirect oxidation. The single ozone degrades the waste water, and has the defects of low ozone utilization rate, low ozone content, incomplete degradation and the like. In order to solve this problem, catalytic ozonation technology has been in the field of people in recent years, because hydroxyl radicals generated by catalytic ozonation accelerate reaction rate, degrade more thoroughly, and are indiscriminate selective reactions.
Catalytic ozonation techniques can be divided into two categories according to the catalysts used: one is homogeneous ozone oxidation using metal ions as catalyst, and the other is metal oxide (MnO)2、Al2O3、TiO2) And solid materials such as supported metal oxides and carbon materials as catalysts. Due to the problems of low mineralization rate, secondary pollution caused by introduction of metal ions and low utilization efficiency of an oxidant in homogeneous catalysis, certain subsequent treatment needs to be carried out after catalytic oxidation reaction of ozone, so that the catalytic oxidation process is complex and is not suitable for practical application.
Disclosure of Invention
The invention aims to provide a preparation method of a peanut shell melamine biochar composite material, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a peanut shell melamine biochar composite material comprises the following steps:
s1, preparing peanut shell powder: cleaning peanut shells with deionized water, drying the cleaned peanut shells in a drying oven, and crushing and sieving the dried peanut shells with a crusher;
s2, preparing a mixture: the first solution is composed of peanut shell powder, melamine and deionized water, when the first solution is prepared, the peanut shell powder and the melamine with a certain composite ratio are selected, and the first solution is ultrasonically stirred until the peanut shell powder and the melamine are dissolved, so that an even mixture is obtained:
and S3, drying the mixture, grinding and calcining at high temperature to obtain the melamine composite material of the peanut shell.
The present invention is further preferred: in S1, the peanut shells are washed by deionized water until the peanut shells are washed, after washing, the drying temperature of the peanut shells is 80-105 ℃, the drying time is 15-17h, and after drying, the ground and sieved peanut shells have 60-100 meshes.
The present invention is further preferred: in S2, the composite ratio of the peanut shell powder to the melamine is 1: 0.25-5.
The present invention is further preferred: the ultrasonic stirring time of the peanut shell powder and melamine is 60-120 min, and the frequency is 70-80 Hz.
The present invention is further preferred: in S3, the mixture is dried for 15-18h at 80-105 deg.C.
The present invention is further preferred: and after the mixture is dried, grinding the mixture into powder at the rotating speed of 20-30 r/min.
The present invention is further preferred: after the mixture is ground, the mixture is calcined at high temperature, the heating rate is 3-6 ℃/min, the temperature is 550-650 ℃, and the heat preservation time is 2-4 h.
The invention also provides an application of the peanut shell melamine biochar composite material, and the biochar composite material is used for catalyzing ozone to oxidize organic pollutants.
The invention has the technical effects and advantages that: compared with the prior art, the preparation method of the peanut shell melamine biochar composite material provided by the invention has the following advantages:
the method adopts waste biomass peanut shells as raw materials, and prepares a novel biochar composite material by mixing melamine with the raw materials, the biochar composite material is applied to the ozone catalytic process, the composite material forms a mutually-stacked sheet structure after high-temperature calcination, the specific surface area is enhanced, the aromatization is high, the capability of decomposing ozone to generate hydroxyl radicals is enhanced, the preparation process of the composite catalyst is simple and easy to realize, no metal ions are dissolved out in the catalytic oxidation process, no secondary pollution is caused, and the method can be applied to the advanced treatment process of municipal domestic sewage, surface water and industrial reuse water.
Drawings
FIG. 1 is a flow chart of the method of the present invention;
FIG. 2 is a graph showing the degradation profile of Dimethoate in various catalytic oxidation systems according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The specific embodiments described herein are merely illustrative of the invention and do not delimit the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a peanut shell melamine biochar composite material as shown in figure 1, which comprises the following steps:
s1, preparing peanut shell powder: cleaning peanut shells with deionized water, drying the cleaned peanut shells in a drying oven, and crushing and sieving the dried peanut shells with a crusher;
s2, preparing a mixture: the first solution consists of peanut shell powder, melamine and deionized water, and when the first solution is prepared, the peanut shell powder and the melamine with a certain composite ratio are selected and ultrasonically stirred until dissolved, so that a uniform mixture is obtained;
and S3, drying the mixture, grinding and calcining at high temperature to obtain the melamine composite material of the peanut shell.
In this embodiment, specifically: in S1, the peanut shells are washed by deionized water until the peanut shells are washed, after washing, the drying temperature of the peanut shells is 80-105 ℃, the drying time is 15-17h, and after drying, the ground and sieved peanut shells have 60-100 meshes.
By adopting the technical scheme, the drying temperature and time of the peanut shells and the crushing and sieving mesh number of the peanut shells can be determined, so that qualified peanut shell powder can be produced without wasting resources
In this embodiment, specifically: in S2, the composite ratio of the peanut shell powder to the melamine is 1: 0.25-5.
By adopting the technical scheme, the composite ratio of the peanut shell powder and the melamine can be determined.
In this embodiment, specifically: the ultrasonic stirring time of the peanut shell powder and melamine is 60-120 min, and the frequency is 70-80 Hz.
By adopting the technical scheme, the peanut shell powder and the melamine can be stirred until being dissolved.
In this embodiment, specifically: in S3, the mixture is dried for 15-18h at 80-105 deg.C.
By adopting the technical scheme, the drying time and the temperature of the mixture can be controlled.
In this embodiment, specifically: and after the mixture is dried, grinding the mixture into powder at the rotating speed of 25-30 r/min.
By adopting the technical scheme, the grinding time of the mixture can be determined.
In this embodiment, specifically: after the mixture is ground, the mixture is calcined at high temperature, the heating rate is 3-6 ℃/min, the temperature is 550-650 ℃, and the heat preservation time is 2-4 h.
By adopting the technical scheme, the mixture can be quickly calcined under the condition of not influencing the chemical and physical effects of the mixture.
The invention also provides an application of the peanut shell melamine biochar composite material, and the biochar composite material is used for catalyzing ozone to oxidize organic pollutants.
In this embodiment: the organic contaminant comprises Dimethoate
By adopting the scheme, the dimethoate is used as a degradation object in the research, is an organophosphorus pesticide which is widely used and has strong volatility, can pollute the environment when being volatilized to the atmosphere and deposited in soil, and is finally transferred to a human body through the enrichment effect of a food chain to cause harm. It has been shown that even a low dose of intake can cause many chronic adverse effects on the human body, such as carcinogenesis, teratogenicity, disorders of the nervous system, and the like. Therefore, the research on the degradation of dimethoate is of great significance and is a non-negligible component in water treatment. The degradation research on the pollutant can provide a degradation mode for the degradation of other pollutants of the same type.
The preparation method and application of the peanut shell melamine biochar composite material are described in detail below with reference to specific examples.
Example one
The embodiment provides a preparation method of a peanut shell melamine biochar composite, which is shown in fig. 1 and comprises the following steps:
firstly, washing waste biomass peanut shells by clear water and a little detergent, spreading the waste biomass peanut shells on a tray, placing the tray in an oven, drying the waste biomass peanut shells at a set temperature of 100 ℃, crushing the peanut shells into powder by a crusher, sieving the powder by a 80-mesh sieve to prepare peanut shell powder, and weighing the peanut shell powder in a ratio of 1: 0.25: putting melamine in a beaker, adding water, stirring, performing ultrasonic treatment until the melamine is dissolved, putting the melamine in an oven, drying at 100 ℃, taking out the melamine, and grinding the melamine into powder to obtain a uniformly mixed peanut shell powder/melamine compound; and then placing the composite material in a tubular furnace, heating the composite material to 600 ℃ at the heating rate of 5 ℃/min under the inert atmosphere, preserving the heat for 4h, and grinding to obtain the required catalyst.
Example two
The embodiment provides a preparation method of a peanut shell melamine biochar composite, which is shown in fig. 1 and comprises the following steps:
firstly, washing waste biomass peanut shells by clear water and a little detergent, spreading the waste biomass peanut shells on a tray, placing the tray in an oven, drying the waste biomass peanut shells at a set temperature of 80 ℃, crushing the peanut shells into powder by a crusher, sieving the powder by a 60-mesh sieve to prepare peanut shell powder, and weighing the peanut shell powder in a ratio of 1: 0.25: putting melamine in a beaker, adding water, stirring, performing ultrasonic treatment until the melamine is dissolved, putting the melamine in an oven, drying at 80 ℃, taking out the melamine, and grinding the melamine into powder to obtain a uniformly mixed peanut shell powder/melamine compound; and then placing the composite material in a tubular furnace, heating the composite material to 550 ℃ at the heating rate of 3 ℃/min under the inert atmosphere, preserving the heat for 2 hours, and grinding to obtain the required catalyst.
EXAMPLE III
Firstly, washing waste biomass peanut shells by clear water and a little detergent, spreading the waste biomass peanut shells on a tray, placing the tray in an oven, drying the waste biomass peanut shells at a set temperature of 108 ℃, crushing the peanut shells into powder by a crusher, sieving the powder by a 100-mesh sieve to prepare peanut shell powder, and weighing the peanut shell powder in a ratio of 1: 5: putting melamine in a beaker, adding water, stirring, performing ultrasonic treatment until the melamine is dissolved, putting the melamine in an oven, drying at 108 ℃, taking out the melamine, and grinding the melamine into powder to obtain a uniformly mixed peanut shell powder/melamine compound; and then placing the composite material in a tubular furnace, heating the composite material to 650 ℃ at the heating rate of 6 ℃/min under the inert atmosphere, preserving the heat for 4h, and grinding to obtain the required catalyst.
Experimental example 1
Dimethoate was catalyzed with the catalysts prepared in examples one to three to test catalytic efficiency and catalytic stability, and the test results are shown in Table 1:
the experimental conditions are as follows: the ozone concentration is 5mg/min (ozone flow is 0.5L/min), the [ dimethoate ]0 is 5mg/L, (peanut shell-melamine) is added at 600 ℃ of 500mg/L, the peanut shell is added at 600 ℃ of 500mg/L, the [ pH ]0 is 6.0, and the temperature is 20 ℃.
TABLE 1
| Degradation rate of Dimethoate (min)-1) | |
| Example one | 0.6342 |
| Example two | 0.8839 |
| EXAMPLE III | 0.3497 |
Experimental example 2
Catalyzing dimethoate by taking ozone oxidation without adding any catalyst as a catalyst;
the experimental conditions are as follows: the ozone concentration is 5mg/min, [ dimethoate ]0 is 5mg/L, (peanut shell-melamine) is 500mg/L at 600 ℃, the peanut shell is 500mg/L at 600 ℃, pH 0 is 6.0, and the temperature is 20 ℃.
The test results are shown in fig. 2.
Comparing the first experimental example with the second experimental example, the melamine biochar composite material of the peanut shell is prepared by a high-temperature calcination method. When the mass ratio of the peanut shell powder to the melamine is 1: 0.25, the peanut shell melamine catalyst is heated to 600 ℃ at a speed of 5 ℃/min under inert gas, and the heat preservation time is 4 hours, the prepared peanut shell melamine catalyst has the optimal catalytic effect, the degradation rate of the dimethoate within 3 minutes can reach 95%, the rapid and high-efficiency catalytic ozone degradation of trace pollutant dimethoate in water can be realized, and the ozone oxidation rate is improved by 7 times compared with that of single ozone.
The working principle is as follows: the melamine biochar composite material with the peanut shells is prepared by a high-temperature calcination method, and the peanut shells are waste biomass materials, so that the melamine biochar composite material has the characteristics of no toxicity, no harm, stable chemical structure and the like, has no pollution problems of metal ion dissolution and the like in the water treatment process, is simple in preparation process and easy to realize, and can be applied to the advanced treatment process of urban domestic sewage, surface water and industrial reuse water; the peanut shell and the melamine are creatively used as a composite material in the ozone catalysis process, the catalyst at 600 ℃ of the peanut shell-melamine improves the efficiency of generating hydroxyl free radicals (OH) by ozone decomposition, so that the degradation and removal of dimethoate in water are accelerated, the catalytic ozone system can be used for degrading and removing various organic matters which are difficult to degrade in the future, and the catalytic ozone system has wide application prospect in drinking water, reuse water and even industrial wastewater treatment.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (8)
1. The preparation method of the peanut shell melamine biochar composite material is characterized by comprising the following steps:
s1, preparing peanut shell powder: cleaning peanut shells with deionized water, drying the cleaned peanut shells in a drying oven, and crushing and sieving the dried peanut shells with a crusher;
s2, preparing a mixture: the first solution is composed of peanut shell powder, melamine and deionized water, when the first solution is prepared, the peanut shell powder and the melamine with a certain composite ratio are selected, and the first solution is ultrasonically stirred until the peanut shell powder and the melamine are dissolved, so that an even mixture is obtained:
and S3, drying the mixture, grinding and calcining at high temperature to obtain the melamine composite material of the peanut shell.
2. The preparation method of the peanut shell melamine biochar composite material as claimed in claim 1, characterized in that: in S1, the peanut shells are washed by deionized water until the peanut shells are washed, after washing, the drying temperature of the peanut shells is 80-105 ℃, the drying time is 15-17h, and after drying, the ground and sieved peanut shells have 60-100 meshes.
3. The preparation method of the peanut shell melamine biochar composite material as claimed in claim 1, characterized in that: in S2, the composite ratio of the peanut shell powder to the melamine is 1: 0.25-5.
4. The preparation method of the peanut shell melamine biochar composite material as claimed in claim 3, characterized in that: the ultrasonic stirring time of the peanut shell powder and melamine is 60-120 min, and the frequency is 70-80 Hz.
5. The preparation method of the peanut shell melamine biochar composite material as claimed in claim 1, characterized in that: in S3, the mixture is dried for 15-18h at 80-105 deg.C.
6. The preparation method of the peanut shell melamine biochar composite material as claimed in claim 5, characterized in that: and after the mixture is dried, grinding the mixture into powder at the rotating speed of 20-30 r/min.
7. The method for preparing the peanut shell melamine biochar composite material as claimed in claim 6, wherein the method comprises the following steps: after the mixture is ground, the mixture is calcined at high temperature, the heating rate is 3-6 ℃/min, the temperature is 550-650 ℃, and the heat preservation time is 2-4 h.
8. Use of a peanut shell melamine biochar composite according to any one of claims 1-7, characterized in that: the biochar composite material is used for catalyzing ozone to oxidize organic pollutants.
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