CN114505077A - Composite catalyst for treating sewage and preparation method thereof - Google Patents

Composite catalyst for treating sewage and preparation method thereof Download PDF

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Publication number
CN114505077A
CN114505077A CN202210107796.5A CN202210107796A CN114505077A CN 114505077 A CN114505077 A CN 114505077A CN 202210107796 A CN202210107796 A CN 202210107796A CN 114505077 A CN114505077 A CN 114505077A
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nano
cellulose
composite catalyst
organic framework
metal organic
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CN114505077B (en
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邓洁
邓玉梅
张纯
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Hunan City University
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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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
    • 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
    • C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/10—Biological treatment of water, waste water, or sewage
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

A composite catalyst for treating sewage comprises a metal organic framework and nanocellulose; the metal organic framework is loaded on the nano-cellulose, the metal organic framework is loaded on the carrier, and the nano-cellulose is hybridized by a metal active component-polypropylene imine dendritic polymer. In the invention, the metal active component is loaded on the nano-cellulose modified by the polypropylene imine dendrimer, and the nano-cellulose and the metal organic framework form complexation; this avoids agglomeration of the metal active component on the metal organic framework, resulting in a large amount of metal active component being uniformly distributed on the catalyst. The catalyst of the invention has good treatment effect on low-concentration organic pollutants.

Description

Composite catalyst for treating sewage and preparation method thereof
Technical Field
The invention relates to a catalyst for treating sewage, in particular to a composite catalyst based on metal oxide-nanocellulose-metal organic framework and a preparation method thereof.
Background
At present, the lack of water resources has become one of the major problems which plague human development. With the continuous improvement of the requirement of process water, the deep purification and reuse process of the sewage becomes a shortcut for realizing the purposes of water saving and emission reduction.
Domestic sewage generally contains a large amount of suspended matters, N-containing pollutants, P-containing pollutants, persistent organic pollutants, pathogenic microorganisms and the like. At present, the sewage is generally discharged completely directly or after being treated by a sewage treatment plant. The method not only discharges a large amount of sewage into a natural system and increases the environmental pollution, but also the related water resources are primary resources, and the use efficiency cannot be improved. The prior sewage treatment uses a catalyst to improve the treatment efficiency, but the traditional catalyst has poor catalytic effect when the pollutant content is low, which is probably caused by the uneven distribution of the adsorption capacity of the catalyst and the active sites on the catalyst.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide a composite catalyst based on metal oxide-nanocellulose-metal organic framework and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a composite catalyst for treating sewage comprises a metal organic framework and nanocellulose; the metal organic framework is loaded on the nano-cellulose, the metal organic framework is loaded on the carrier, and the nano-cellulose is hybridized by a metal active component-polypropylene imine dendritic polymer.
Preferably, the metal active component comprises CuOXAnd ZnO; x =1 or 2. In the present invention, CuOXZnO can be uniformly attached to the nano-cellulose modified by the polypropyleneimine dendrimer, and the nano-cellulose has large surface area and CuOXAnd ZnO is easily supported on activated carbon particles. Enough CuO can be loaded on the nano-celluloseXAnd ZnO, which provides enough reactive sites for the reaction of the wastewater. The polypropylene imine tree-shaped macromolecule can effectively capture pollutant molecules or microorganisms in sewage, and the metal organic framework can effectively absorb the pollutant molecules or microorganisms in low-concentration pollutant sewage by virtue of synergistic adsorption of the pollutant molecules or microorganisms, so that the sewage treatment is more thorough.
In the invention, the nanocellulose and the metal organic framework form complexation, so that the nanocellulose has good dispersibility and stability in sewage.
Preferably, the weight of the nano-cellulose is 15-30% of the metal organic framework.
Preferably, the nano-cellulose is cellulose nano-fiber prepared by performing acidolysis, centrifugation and high-pressure homogenization on bleached wood pulp.
A preparation method of a composite catalyst for sewage treatment comprises the following steps,
1) modifying the nano-cellulose by using the polypropylene imine dendrimer;
2) loading metal oxide on the modified nano-cellulose in the step 1);
Figure DEST_PATH_IMAGE002
soaking the nano-cellulose into the precursor solution, uniformly stirring, and then preserving heat for more than 2 hours at the temperature of 50-80 ℃; the precursor solution comprises ZnCO with the mass concentration of 2-6%3Suspension or CuCO with mass concentration of 2-6%3One or two of the suspensions are mixed;
Figure DEST_PATH_IMAGE004
taking the nano-cellulose in the step 1) out of the precursor solution, and drying;
Figure DEST_PATH_IMAGE006
calcining the nano-cellulose in the step 2) for 1-3 h under the protection of vacuum or inert gas, wherein the calcining temperature is 200-400 ℃; obtaining nano-cellulose loaded with metal oxide;
3) adding the nano-cellulose loaded with the metal oxide in the step 2) into the suspension of the metal organic framework, and stirring for more than 2 hours at the temperature of 50-80 ℃;
4) and 3) carrying out solid-liquid separation on the suspension liquid obtained in the step 3), sequentially using DMF (dimethyl formamide), methanol and deionized water to clean the obtained precipitate, and drying to obtain the composite catalyst for treating sewage.
In the preparation method of the composite catalyst for sewage treatment, preferably, the modification of the nanocellulose by the polypropyleneimine dendrimer in the step 1) comprises the following steps;
Figure DEST_PATH_IMAGE008
soaking the nano-cellulose in the polypropylene imine dendrimer solution for 5-20min, and taking out;
Figure DEST_PATH_IMAGE010
will be described in detail
Figure 225518DEST_PATH_IMAGE008
The nano-cellulose is annealed at the temperature of 150-300 ℃ for 20-60 min; obtaining the nano-cellulose modified by the polypropylene imine dendrimer. In the invention, during annealing treatment, amidation reaction is carried out between the amine-base end of the polypropylene imine dendrimer and the carboxyl end of the nano-cellulose, so that the polypropylene imine dendrimer is grafted on the nano-cellulose.
In the present invention, under acidic conditions, the primary amine-terminal end and the internal tertiary amino group on the polypropyleneimine dendrimer are protonated; after protonation, strong repulsion force between the base end of the primary amine and the tertiary amino group in the primary amine is generated, so that the diameter of the polypropylene imine dendrimer is increased, the size of the cavity of the polypropylene imine dendrimer is increased, and the capacity of capturing pollutant molecules or microorganisms by the internal cavity of the polypropylene imine dendrimer is realized.
In the invention, under an acidic condition, the primary amine terminal end on the polypropyleneimine dendrimer and the tertiary amino group in the polypropyleneimine dendrimer are protonated, so that the nano-cellulose modified by the polypropyleneimine dendrimer is positively charged, and the capability of the catalyst for adsorbing anionic pollutants is enhanced.
In the preparation method of the composite catalyst for sewage treatment, preferably, the preparation of the nanocellulose comprises the following steps: using bleached wood pulp as a raw material, hydrolyzing for 0.5-1.5h by using sulfuric acid with the weight concentration of 40-55%, cleaning by using distilled water, centrifuging for three times, centrifuging to remove the distilled water to obtain highly purified nano-cellulose, and mechanically opening the suspension by using a high-pressure homogenizer to obtain nano-cellulose suspension; drying to obtain the nano-cellulose.
In the preparation method of the composite catalyst for sewage treatment, preferably, the homogenization speed in the high-pressure homogenizer is controlled at 150-250 ml/min; homogenizing for 6-8 times.
Compared with the prior art, the invention has the advantages that: in the invention, the metal active component is loaded on the nano-cellulose modified by the polypropylene imine dendrimer, and the nano-cellulose and the metal organic framework form complexation; thus avoiding the agglomeration of the metal active component on the metal organic framework and leading a large amount of the metal active component to be uniformly distributed on the catalyst. The catalyst of the invention has good treatment effect on low-concentration organic pollutants.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
It should be particularly noted that when an element is referred to as being "fixed to, connected to or communicated with" another element, it can be directly fixed to, connected to or communicated with the other element or indirectly fixed to, connected to or communicated with the other element through other intermediate connecting components.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Example 1
A composite catalyst for treating sewage comprises a metal organic framework and nanocellulose; the metal organic framework is loaded on the nano-cellulose, the metal organic framework is loaded on the carrier, and the nano-cellulose is polymerized by the metal active componentPropyleneimine dendrimer hybrids. The metal active component comprises CuO2And CuO. The weight of the nanocellulose is 20% of the metal organic framework.
In an embodiment, the metal organic framework is PCN222, and in other embodiments, it may also be PCN224, PCN225, or the like. In this embodiment, when preparing PCN222, porphyrin, zirconium chloride, benzoic acid and N, N-dimethylformamide were mixed under ultrasonic conditions to obtain a mixed solution, the mixed solution was subjected to hydrothermal reaction, and ethanol was centrifuged, washed and dried to obtain a PCN222 metal organic framework material.
A preparation method of a composite catalyst for sewage treatment comprises the following steps,
1) modifying the nano-cellulose by using a polypropyleneimine dendrimer;
2) loading metal oxide on the modified nano-cellulose in the step 1);
Figure 547915DEST_PATH_IMAGE002
soaking the nano-cellulose into the precursor solution, uniformly stirring, and then preserving heat for more than 2 hours at the temperature of 50-80 ℃; the precursor solution is CuCO with the mass concentration of 5 percent3One or two of the suspensions are mixed;
Figure 95571DEST_PATH_IMAGE004
taking the nano-cellulose in the step 1) out of the precursor solution, and drying;
Figure 187024DEST_PATH_IMAGE006
calcining the nano-cellulose in the step 2) for 1-3 h under the protection of vacuum or inert gas, wherein the calcining temperature is 200-400 ℃; obtaining nano-cellulose loaded with metal oxide;
3) adding the nano-cellulose loaded with the metal oxide in the step 2) into the suspension of the metal organic framework, and stirring for more than 2 hours at the temperature of 80 ℃;
4) and 3) carrying out solid-liquid separation on the suspension liquid obtained in the step 3), sequentially using DMF (dimethyl formamide), methanol and deionized water to clean the obtained precipitate, and drying to obtain the composite catalyst for treating sewage.
In this embodiment, the modification of the nanocellulose with the polypropyleneimine dendrimer in step 1) comprises the following steps;
Figure 427512DEST_PATH_IMAGE008
soaking the nano-cellulose in the polypropylene imine dendrimer solution for 20min, and taking out;
Figure 470161DEST_PATH_IMAGE010
will be described in detail
Figure 821508DEST_PATH_IMAGE008
The nano-cellulose is annealed at the temperature of 300 ℃ for 30 min; obtaining the nano-cellulose modified by the polypropyleneimine dendrimer;
in this example, the preparation of nanocellulose comprises the following steps: hydrolyzing bleached wood pulp serving as a raw material by using 50% sulfuric acid by weight for 1h, cleaning by using distilled water, centrifuging for three times, centrifuging to remove the distilled water to obtain high-purification nano cellulose, and mechanically opening the suspension by using a high-pressure homogenizer to obtain nano cellulose suspension; drying to obtain the nano-cellulose. The homogenizing speed in the high-pressure homogenizer is controlled at 200 ml/min; homogenizing for 8 times.
Example 2
A composite catalyst for treating sewage comprises a metal organic framework and nanocellulose; the metal organic framework is loaded on the nano-cellulose, the metal organic framework is loaded on the carrier, and the nano-cellulose is hybridized by a metal active component-polypropylene imine dendritic polymer. The metal active component comprises CuO2A mixture of CuO and ZnO. The weight of the nanocellulose is 20% of the metal organic framework.
In an embodiment, the metal organic framework is PCN 222. In this embodiment, when preparing PCN222, porphyrin, zirconium chloride, benzoic acid and N, N-dimethylformamide were mixed under ultrasonic conditions to obtain a mixed solution, the mixed solution was subjected to hydrothermal reaction, and ethanol was centrifuged, washed and dried to obtain a PCN222 metal organic framework material.
A preparation method of a composite catalyst for sewage treatment comprises the following steps,
1) modifying the nano-cellulose by using a polypropyleneimine dendrimer;
2) loading metal oxide on the modified nano-cellulose in the step 1);
Figure 908413DEST_PATH_IMAGE002
soaking the nano-cellulose into the precursor solution, uniformly stirring, and then preserving heat for more than 2 hours at the temperature of 50-80 ℃; the precursor solution is CuCO with the mass concentration of 2%3And ZnCO with the mass concentration of 2%3Mixing the suspension;
Figure 178857DEST_PATH_IMAGE004
taking the nano-cellulose in the step 1) out of the precursor solution, and drying;
Figure 351212DEST_PATH_IMAGE006
calcining the nano-cellulose obtained in the step 2) for 1-3 hours under the protection of vacuum or inert gas, wherein the calcining temperature is 200 ℃; obtaining nano-cellulose loaded with metal oxide;
3) adding the nano-cellulose loaded with the metal oxide in the step 2) into the suspension of the metal organic framework, and stirring for more than 2 hours at the temperature of 80 ℃;
4) and 3) carrying out solid-liquid separation on the suspension liquid obtained in the step 3), sequentially using DMF (dimethyl formamide), methanol and deionized water to clean the obtained precipitate, and drying to obtain the composite catalyst for treating sewage.
In this embodiment, the modification of the nanocellulose with the polypropyleneimine dendrimer in step 1) comprises the following steps;
Figure 365305DEST_PATH_IMAGE008
soaking the nano-cellulose in the polypropylene imine dendrimer solution for 10min, and taking out;
Figure 306716DEST_PATH_IMAGE010
will be described in detail
Figure 13641DEST_PATH_IMAGE008
The nano-cellulose is annealed at the temperature of 200 ℃ for 60 min; obtaining the nano-cellulose modified by the polypropyleneimine dendrimer;
in this example, the preparation of nanocellulose comprises the following steps: hydrolyzing bleached wood pulp serving as a raw material by using 50% sulfuric acid by weight for 1h, cleaning by using distilled water, centrifuging for three times, centrifuging to remove the distilled water to obtain high-purification nano cellulose, and mechanically opening the suspension by using a high-pressure homogenizer to obtain nano cellulose suspension; drying to obtain the nano-cellulose. The homogenizing speed in the high-pressure homogenizer is controlled at 200 ml/min; homogenizing for 8 times.
The composite catalysts of example 1 and example 2 are respectively used for treating sewage containing COD and bacteria, and ozone is introduced into the sewage for 30min during treatment so that the COD is subjected to oxidative decomposition. The original COD content in the sewage is about 450 mg/L. In example 1, the COD concentration after the treatment with ozone and catalyst was about 25 mg/L, and the removal rate reached 94.6%. After the composite catalyst and ozone treatment in example 2, the COD concentration was about 32 mg/L, and the removal rate reached 92.9%. And the removal of COD of the common catalyst on the market does not exceed 60 percent under the same condition.
The content of bacteria in the sewage is about 3.4 multiplied by 106About per liter, when the sewage is treated in the embodiment 1 and the embodiment 2, after the sewage is treated by ozone and a catalyst, the bacteria in the sewage are removedThe content is 1.5X 103About L/L, it can be seen that the catalyst in this example can substantially remove bacteria from water.

Claims (8)

1. A composite catalyst for treating sewage is characterized in that: comprises a metal organic framework and nanocellulose; the metal organic framework is loaded on the nano-cellulose, the metal organic framework is loaded on the carrier, and the nano-cellulose is hybridized by a metal active component-polypropylene imine dendritic polymer.
2. The composite catalyst for treating wastewater according to claim 1, wherein: the metal active component comprises CuOXAnd ZnO; x =1 or 2.
3. The composite catalyst for treating wastewater according to claim 1, wherein: the weight of the nano-cellulose is 15-30% of the metal organic framework.
4. The composite catalyst for treating wastewater according to claim 1, wherein: the nano-cellulose is cellulose nano-fiber prepared by carrying out acidolysis, centrifugation and high-pressure homogenization on bleached wood pulp.
5. A preparation method of a composite catalyst for sewage treatment is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
1) modifying the nano-cellulose by using the polypropylene imine dendrimer;
2) loading metal oxide on the modified nano-cellulose in the step 1);
Figure 601823DEST_PATH_IMAGE001
soaking the nano-cellulose into the precursor solution, uniformly stirring, and then preserving heat for more than 2 hours at the temperature of 50-80 ℃; the precursor solution comprises ZnCO with the mass concentration of 2-6%3Suspensions or substancesCuCO in a quantitative concentration of 2-6%3One or two of the suspensions are mixed;
Figure 594049DEST_PATH_IMAGE002
taking the nano-cellulose in the step 1) out of the precursor solution, and drying;
Figure 617369DEST_PATH_IMAGE003
calcining the nano-cellulose in the step 2) for 1-3 h under the protection of vacuum or inert gas, wherein the calcining temperature is 200-400 ℃; obtaining nano-cellulose loaded with metal oxide;
3) adding the nano-cellulose loaded with the metal oxide in the step 2) into the suspension of the metal organic framework, and stirring for more than 2 hours at the temperature of 50-80 ℃;
4) and 3) carrying out solid-liquid separation on the suspension liquid obtained in the step 3), sequentially using DMF (dimethyl formamide), methanol and deionized water to clean the obtained precipitate, and drying to obtain the composite catalyst for treating sewage.
6. The method for preparing the composite catalyst for sewage treatment according to claim 5, characterized in that: the modification of the nano-cellulose by the polypropylene imine dendrimer in the step 1) comprises the following steps;
Figure 327836DEST_PATH_IMAGE004
soaking the nano-cellulose in the polypropylene imine dendrimer solution for 5-20min, and taking out;
Figure 706689DEST_PATH_IMAGE005
will be described in detail
Figure 819001DEST_PATH_IMAGE004
Is removed from the nanocellulosePerforming fire treatment, wherein the temperature of the annealing treatment is 150-300 ℃, and the time is 20-60 min; obtaining the nano-cellulose modified by the polypropyleneimine dendrimer.
7. The method for preparing the composite catalyst for sewage treatment according to claim 5, characterized in that: the preparation of the nano-cellulose comprises the following steps: using bleached wood pulp as a raw material, hydrolyzing for 0.5-1.5h by using sulfuric acid with the weight concentration of 40-55%, cleaning by using distilled water, centrifuging for three times, centrifuging to remove the distilled water to obtain highly purified nano-cellulose, and mechanically opening the suspension by using a high-pressure homogenizer to obtain nano-cellulose suspension; drying to obtain the nano-cellulose.
8. The method for preparing a composite catalyst for sewage treatment according to claim 7, characterized in that: the homogenizing speed in the high-pressure homogenizer is controlled at 150-250 ml/min; homogenizing for 6-8 times.
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