CN114162912B - Preparation method of high {001} crystal face-loaded titanium dioxide particle electrode - Google Patents
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Abstract
A method for preparing a high {001} crystal face-supported titanium dioxide particle electrode composed of a granular activated carbon and titanium dioxide having a high {001} crystal face supported on the granular activated carbon, comprising the steps of: the preparation method comprises the steps of pretreatment of activated carbon, hydrothermal reaction of a mixture of powdered activated carbon and titanium tetrafluoride, high-temperature heat treatment, extrusion molding of granular activated carbon and the like, wherein titanium tetrafluoride is adopted as a titanium source, and titanium dioxide can stably grow a {001} crystal face with high surface energy under a fluorine environment by utilizing high bonding energy between fluorine and titanium, so that the prepared particle electrode can remarkably improve electrocatalytic oxidation activity, promote degradation of difficult-to-biochemically-organic pollutants, reduce treatment time and prolong service life in a three-dimensional electrolysis system applied by the particle electrode; and (3) filling the mixture into a fixed bed of an up-flow three-dimensional electrode reactor for electrolytic oxidation experiment of the acid orange 7, wherein the removal rate of the acid orange 7 can reach 91.2% after 5min of electrolysis.
Description
Technical Field
The application belongs to the field of particle electrode preparation, and particularly relates to a preparation method of a titanium dioxide particle electrode with a high {001} crystal face.
Background
The industrial development of China is rapid, the national economy development and the improvement of the material civilization are greatly driven, but at the same time, the direct discharge or the substandard discharge of the industrial wastewater not only causes serious environmental pollution, but also endangers the physical health of people. According to the statistics of the ecological environment department of China, the discharge amount of industrial wastewater in 2018 China is still up to 175 hundred million tons, and the industrial wastewater comprises a plurality of industries such as papermaking, printing and dyeing, pharmacy, chemical industry and the like. The industrial wastewater has the characteristics of large water quantity, complex components, and various organic pollutants difficult to biochemically degrade, such as colorants, dyes, organic raw materials, auxiliary agents and the like.
At present, the method for treating the organic pollutants in the industrial wastewater mainly comprises flocculation, membrane separation, photocatalysis, laser catalysis, advanced oxidation technology and electrochemical catalytic oxidation technology, wherein the electrochemical catalytic oxidation technology has the advantages of good treatment effect, simple process flow and small occupied area, and is widely applied. The three-dimensional electrode method is to fill granular electrode materials, namely a third electrode, on the basis of the two-dimensional electrolytic tank, and has the advantages of reducing mass transfer resistance, improving current efficiency and space-time yield, reducing energy consumption and the like compared with the two-dimensional electrode method. The particle electrode is polarized in the electric field, so that particles with opposite charges are enriched on two different surfaces of the particles, thereby forming a micro-electrolytic cell, and further improving the efficiency of directly oxidizing organic matters in the electrolytic cell; secondly, the particle electrode has larger specific surface area, and can effectively carry out physical adsorption and electric adsorption on organic pollutants; the particle electrode is carried with a catalyst, water or oxygen is catalyzed by the catalyst to generate hydroxyl free radicals, the concentration of the hydroxyl free radicals in the system is improved, and the indirect catalytic effect on organic pollutants is enhanced.
Anatase type TiO 2 The crystal has important application value in photocatalytic water decomposition and photocatalytic degradation of organic pollutants, but has little application research on electrocatalytic oxidation of organic pollutants, and the main reason is that TiO prepared by the prior art 2 The crystal surface is usually composed of thermodynamically stable {101} planes (94%), and contains only a small amount of {001} crystal planes, resulting in poor electrical conductivity and low electrocatalytic activity. Thus, how to accurately and controllably prepare TiO 2 The specific crystal face of the crystal has important significance for developing high-performance particle electrodes for treating industrial wastewater.
Disclosure of Invention
The application aims to overcome the defects of the prior art and provide a preparation method of a titanium dioxide particle electrode with a high {001} crystal face.
The application adopts the following technical scheme:
a method for preparing a high {001} crystal face-supported titanium dioxide particle electrode composed of a granular activated carbon and titanium dioxide having a high {001} crystal face supported on the granular activated carbon, comprising the steps of:
step one, pretreatment of activated carbon: boiling powdered activated carbon and dilute hydrochloric acid solution at 100 ℃ for 2 hours, cooling, filtering, washing with deionized water until the pH value of the filtrate is neutral, and then vacuum drying at 110 ℃ for 24 hours;
step two, hydrothermal reaction: dissolving titanium tetrafluoride in deionized water, adding hydrochloric acid solution and sodium chloride solid particles, stirring uniformly, adding the powdered activated carbon obtained in the first step, mixing uniformly, pouring into a reaction kettle with polytetrafluoroethylene, and treating for 2-6 hours at 200 ℃, wherein the molar ratio of the titanium tetrafluoride to the hydrochloric acid solution to the sodium chloride is 3-5:1:80, and the mass ratio of the titanium tetrafluoride to the powdered activated carbon is 1-2:30;
step three, high-temperature heat treatment: filtering the mixed solution obtained in the second reaction, washing with deionized water for 5-6 times, vacuum drying at 110 ℃ for 20 hours, and heat treating at 450 ℃ for 2 hours to obtain modified activated carbon;
and step four, uniformly mixing and stirring the modified activated carbon obtained in the step three with coal tar, extruding and molding, drying at 110 ℃, and carbonizing at 400 ℃ for 2 hours to obtain the particle electrode loaded with high {001} crystal face titanium dioxide.
Further, the powdered activated carbon is made from coconut shells, fruit shells, wood or coal based.
Further, the particle size of the powdered activated carbon is smaller than 200 meshes, the iodine adsorption value is larger than 950mg/L, and the methylene blue adsorption value is 10-15ml.
Further, in the first step, the concentration of the dilute hydrochloric acid aqueous solution is 0.05-0.1mol/L.
Further, in the second step, the concentration of the hydrochloric acid solution is 0.1mol/L.
Further, in the fourth step, the content of the coal tar is 5-10% of the mass of the modified activated carbon.
Further, the titanium dioxide crystal form is anatase.
As can be seen from the above description of the present application, compared with the prior art, the present application has the following beneficial effects:
firstly, the titanium tetrafluoride is adopted as a titanium source, and the titanium dioxide can stably grow a {001} crystal face with high surface energy under a fluorine environment by utilizing higher bonding energy between fluorine and titanium, so that the prepared particle electrode can remarkably improve electrocatalytic oxidation activity, promote degradation of organic pollutants difficult to biochemically produce, reduce treatment time and prolong service life in a three-dimensional electrolysis system to which the particle electrode is applied; filling the mixture into a fixed bed of an up-flow three-dimensional electrode reactor for electrolytic oxidation experiment of the acid orange 7, wherein the removal rate of the acid orange 7 can reach 91.2% after 5min of electrolysis;
secondly, adding sodium chloride solid particles to provide a stable environment for the {001} crystal face with high surface energy for the stable growth of titanium dioxide, so as to ensure the characteristics of the prepared particle electrode;
thirdly, coal tar is used as an adhesive to prepare the formed active carbon electrode particles, so that the mechanical strength is high, and the water outlet is not lost or blocked due to crushing in the actual application process;
fourth, the powdered activated carbon is washed by dilute hydrochloric acid, so that inorganic ash and organic impurities in the activated carbon pore canal are effectively removed, the load rate of titanium dioxide is improved, and the titanium dioxide is firmly fixed in the pore canal.
Detailed Description
The application is further described below by means of specific embodiments.
A titanium dioxide particle electrode loaded with a high {001} crystal face consists of granular active carbon and titanium dioxide loaded on the granular active carbon and having the high {001} crystal face, wherein the crystal form of the titanium dioxide is anatase; specifically, the powdered activated carbon is prepared from coconut shells, fruit shells, woodiness or coal base, the grain diameter is smaller than 200 meshes, the iodine adsorption value is larger than 950mg/L, and the methylene blue adsorption value is 10-15ml.
The preparation method comprises the following steps:
step one, pretreatment of activated carbon: boiling powdered activated carbon and dilute hydrochloric acid solution at 100 ℃ for 2 hours, cooling, filtering, washing with deionized water until the pH value of the filtrate is neutral, and then vacuum drying at 110 ℃ for 24 hours;
step two, hydrothermal reaction: dissolving titanium tetrafluoride in deionized water, adding 0.1mol/L hydrochloric acid solution and sodium chloride solid particles, stirring uniformly, adding the powdered activated carbon obtained in the first step, mixing and stirring uniformly, pouring into a reaction kettle with polytetrafluoroethylene, and treating for 2-6 hours at 200 ℃, wherein the molar ratio of the titanium tetrafluoride to the hydrochloric acid solution to the sodium chloride is 3-5:1:80, and the mass ratio of the titanium tetrafluoride to the powdered activated carbon is 1-2:30;
step three, high-temperature heat treatment: filtering the mixed solution obtained in the second reaction, washing with deionized water for 5-6 times, vacuum drying at 110 ℃ for 20 hours, and heat treating at 450 ℃ for 2 hours to obtain modified activated carbon;
and step four, uniformly mixing and stirring the modified activated carbon obtained in the step three with coal tar, extruding and molding, drying at 110 ℃, and carbonizing at 400 ℃ for 2 hours to obtain the particle electrode loaded with high {001} crystal face titanium dioxide.
Specifically, in the first step, the concentration of the dilute hydrochloric acid aqueous solution is 0.05-0.1mol/L.
In the fourth step, the content of the coal tar is 5-10% of the mass of the modified activated carbon.
Example 1
A titanium dioxide particle electrode loaded with high {001} crystal face is composed of granular active carbon and titanium dioxide loaded on the granular active carbon and having high {001} crystal face, and the titanium dioxide crystal form is anatase.
The preparation method comprises the following steps:
step one, pretreatment of activated carbon: boiling powdered activated carbon and dilute hydrochloric acid solution at 100 ℃ for 2 hours, cooling, filtering, washing with deionized water until the pH value of the filtrate is neutral, and then vacuum drying at 110 ℃ for 24 hours;
step two, hydrothermal reaction: dissolving 0.3g of titanium tetrafluoride in 100ml of deionized water, adding 8ml of hydrochloric acid solution with the concentration of 0.1mol/L and 3.77g of sodium chloride solid particles, uniformly stirring, adding 9g of powdered activated carbon obtained by the treatment in the step one, uniformly mixing, pouring into a reaction kettle with polytetrafluoroethylene, and treating for 2 hours at the temperature of 200 ℃, wherein the molar ratio of the titanium tetrafluoride to the hydrochloric acid solution to the sodium chloride is 3:1:80, and the mass ratio of the titanium tetrafluoride to the powdered activated carbon is 1:30;
step three, high-temperature heat treatment: filtering the mixed solution obtained in the second reaction, washing with deionized water for 5-6 times, vacuum drying at 110 ℃ for 20 hours, and heat treating at 450 ℃ for 2 hours to obtain modified activated carbon;
and step four, uniformly mixing and stirring the modified activated carbon obtained in the step three with coal tar, extruding and molding, drying at 110 ℃, and carbonizing at 400 ℃ for 2 hours to obtain the particle electrode loaded with high {001} crystal face titanium dioxide.
Specifically, in the first step, the concentration of the dilute hydrochloric acid aqueous solution is 0.05mol/L.
In the fourth step, the content of the coal tar is 5% of the mass of the modified activated carbon.
The particle electrode prepared in the embodiment is filled into a fixed bed of an up-flow three-dimensional electrode reactor for electrolytic oxidation experiment of the acid orange 7, wherein an electrolyte is Na2SO4 solution with the concentration of 10g/L, both anode and cathode adopt graphite, the working voltage is 10V, and the removal rate of the acid orange 7 reaches 88.3% after 5min of electrolysis.
Example 2
A titanium dioxide particle electrode loaded with high {001} crystal face is composed of granular active carbon and titanium dioxide loaded on the granular active carbon and having high {001} crystal face, and the titanium dioxide crystal form is anatase.
The preparation method comprises the following steps:
step one, pretreatment of activated carbon: boiling powdered activated carbon and dilute hydrochloric acid solution at 100 ℃ for 2 hours, cooling, filtering, washing with deionized water until the pH value of the filtrate is neutral, and then vacuum drying at 110 ℃ for 24 hours;
step two, hydrothermal reaction: dissolving 0.3g of titanium tetrafluoride in 100ml of deionized water, adding 8ml of hydrochloric acid solution with the concentration of 0.1mol/L and 3.77g of sodium chloride solid particles, uniformly stirring, adding 9g of powdered activated carbon obtained by the treatment in the step one, uniformly mixing, pouring into a reaction kettle with polytetrafluoroethylene, and treating for 4 hours at 200 ℃, wherein the molar ratio of the titanium tetrafluoride to the hydrochloric acid solution to the sodium chloride is 3:1:80, and the mass ratio of the titanium tetrafluoride to the powdered activated carbon is 1:30;
step three, high-temperature heat treatment: filtering the mixed solution obtained in the second reaction, washing with deionized water for 5-6 times, vacuum drying at 110 ℃ for 20 hours, and heat treating at 450 ℃ for 2 hours to obtain modified activated carbon;
and step four, uniformly mixing and stirring the modified activated carbon obtained in the step three with coal tar, extruding and molding, drying at 110 ℃, and carbonizing at 400 ℃ for 2 hours to obtain the particle electrode loaded with high {001} crystal face titanium dioxide.
Specifically, in the first step, the concentration of the dilute hydrochloric acid aqueous solution is 0.1mol/L.
In the fourth step, the content of the coal tar is 10% of the mass of the modified activated carbon.
The particle electrode prepared in the embodiment is filled into a fixed bed of an up-flow three-dimensional electrode reactor for electrolytic oxidation experiment of the acid orange 7, wherein an electrolyte is Na2SO4 solution with the concentration of 10g/L, both anode and cathode adopt graphite, the working voltage is 10V, and the removal rate of the acid orange 7 reaches 89.7% after 5min of electrolysis.
Example 3
A titanium dioxide particle electrode loaded with high {001} crystal face is composed of granular active carbon and titanium dioxide loaded on the granular active carbon and having high {001} crystal face, and the titanium dioxide crystal form is anatase.
The preparation method comprises the following steps:
step one, pretreatment of activated carbon: boiling powdered activated carbon and dilute hydrochloric acid solution at 100 ℃ for 2 hours, cooling, filtering, washing with deionized water until the pH value of the filtrate is neutral, and then vacuum drying at 110 ℃ for 24 hours;
step two, hydrothermal reaction: dissolving 0.3g of titanium tetrafluoride in deionized water, adding 8ml of hydrochloric acid solution with the concentration of 0.1mol/L and 3.77g of sodium chloride solid particles, uniformly stirring, adding 9g of powdered activated carbon obtained in the first step, uniformly mixing, pouring into a reaction kettle with polytetrafluoroethylene, and treating for 6 hours at 200 ℃, wherein the molar ratio of the titanium tetrafluoride to the hydrochloric acid solution to the sodium chloride is 3:1:80, and the mass ratio of the titanium tetrafluoride to the powdered activated carbon is 1:30;
step three, high-temperature heat treatment: filtering the mixed solution obtained in the second reaction, washing with deionized water for 5-6 times, vacuum drying at 110 ℃ for 20 hours, and heat treating at 450 ℃ for 2 hours to obtain modified activated carbon;
and step four, uniformly mixing and stirring the modified activated carbon obtained in the step three with coal tar, extruding and molding, drying at 110 ℃, and carbonizing at 400 ℃ for 2 hours to obtain the particle electrode loaded with high {001} crystal face titanium dioxide.
Specifically, in the first step, the concentration of the dilute hydrochloric acid aqueous solution is 0.08mol/L.
In the fourth step, the content of the coal tar is 8% of the mass of the modified activated carbon.
The particle electrode prepared in the embodiment is filled into a fixed bed of an up-flow three-dimensional electrode reactor for electrolytic oxidation experiment of the acid orange 7, wherein an electrolyte is Na2SO4 solution with the concentration of 10g/L, both anode and cathode adopt graphite, the working voltage is 10V, and the removal rate of the acid orange 7 reaches 91.2% after 5min of electrolysis.
Example 4
A titanium dioxide particle electrode loaded with high {001} crystal face is composed of granular active carbon and titanium dioxide loaded on the granular active carbon and having high {001} crystal face, and the titanium dioxide crystal form is anatase.
The preparation method comprises the following steps:
step one, pretreatment of activated carbon: boiling powdered activated carbon and dilute hydrochloric acid solution at 100 ℃ for 2 hours, cooling, filtering, washing with deionized water until the pH value of the filtrate is neutral, and then vacuum drying at 110 ℃ for 24 hours;
step two, hydrothermal reaction: dissolving 0.4g of titanium tetrafluoride in deionized water, adding 8ml of hydrochloric acid solution with the concentration of 0.1mol/L and 3.77g of sodium chloride solid particles, uniformly stirring, adding 8g of powdered activated carbon obtained in the first step, uniformly mixing, pouring into a reaction kettle with polytetrafluoroethylene, and treating for 2 hours at 200 ℃, wherein the molar ratio of the titanium tetrafluoride to the hydrochloric acid solution to the sodium chloride is 4:1:80, and the mass ratio of the titanium tetrafluoride to the powdered activated carbon is 1.5:30;
step three, high-temperature heat treatment: filtering the mixed solution obtained in the second reaction, washing with deionized water for 5-6 times, vacuum drying at 110 ℃ for 20 hours, and heat treating at 450 ℃ for 2 hours to obtain modified activated carbon;
and step four, uniformly mixing and stirring the modified activated carbon obtained in the step three with coal tar, extruding and molding, drying at 110 ℃, and carbonizing at 400 ℃ for 2 hours to obtain the particle electrode loaded with high {001} crystal face titanium dioxide.
Specifically, in the first step, the concentration of the dilute hydrochloric acid aqueous solution is 0.08mol/L.
In the fourth step, the content of the coal tar is 8% of the mass of the modified activated carbon.
The particle electrode prepared in the embodiment is filled into a fixed bed of an up-flow three-dimensional electrode reactor for electrolytic oxidation experiment of the acid orange 7, wherein an electrolyte is Na2SO4 solution with the concentration of 10g/L, both anode and cathode adopt graphite, the working voltage is 10V, and the removal rate of the acid orange 7 reaches 90.2% after 5min of electrolysis.
Example 5
A titanium dioxide particle electrode loaded with high {001} crystal face is composed of granular active carbon and titanium dioxide loaded on the granular active carbon and having high {001} crystal face, and the titanium dioxide crystal form is anatase.
The preparation method comprises the following steps:
step one, pretreatment of activated carbon: boiling powdered activated carbon and dilute hydrochloric acid solution at 100 ℃ for 2 hours, cooling, filtering, washing with deionized water until the pH value of the filtrate is neutral, and then vacuum drying at 110 ℃ for 24 hours;
step two, hydrothermal reaction: dissolving 0.5g of titanium tetrafluoride in deionized water, adding 8ml of hydrochloric acid solution with the concentration of 0.1mol/L and 3.77g of sodium chloride solid particles, uniformly stirring, adding 7.5g of powdered activated carbon obtained in the first step, uniformly mixing and stirring, pouring into a reaction kettle with polytetrafluoroethylene, and treating for 6 hours at 200 ℃, wherein the molar ratio of the titanium tetrafluoride to the hydrochloric acid solution to the sodium chloride is 5:1:80, and the mass ratio of the titanium tetrafluoride to the powdered activated carbon is 2:30;
step three, high-temperature heat treatment: filtering the mixed solution obtained in the second reaction, washing with deionized water for 5-6 times, vacuum drying at 110 ℃ for 20 hours, and heat treating at 450 ℃ for 2 hours to obtain modified activated carbon;
and step four, uniformly mixing and stirring the modified activated carbon obtained in the step three with coal tar, extruding and molding, drying at 110 ℃, and carbonizing at 400 ℃ for 2 hours to obtain the particle electrode loaded with high {001} crystal face titanium dioxide.
Specifically, in the first step, the concentration of the dilute hydrochloric acid aqueous solution is 0.08mol/L.
In the fourth step, the content of the coal tar is 8% of the mass of the modified activated carbon.
The particle electrode prepared in the embodiment is filled into a fixed bed of an up-flow three-dimensional electrode reactor for electrolytic oxidation experiment of the acid orange 7, wherein an electrolyte is Na2SO4 solution with the concentration of 10g/L, both anode and cathode adopt graphite, the working voltage is 10V, and the removal rate of the acid orange 7 reaches 91.1% after 5min of electrolysis.
According to the application, titanium tetrafluoride is adopted as a titanium source, and titanium dioxide can stably grow a {001} crystal face with high surface energy in a fluorine environment by utilizing higher bonding energy between fluorine and titanium, so that the prepared particle electrode can remarkably improve electrocatalytic oxidation activity, promote degradation of organic pollutants difficult to biochemically produce, reduce treatment time and prolong service life in a three-dimensional electrolysis system to which the particle electrode is applied; and (3) filling the mixture into a fixed bed of an up-flow three-dimensional electrode reactor for electrolytic oxidation experiment of the acid orange 7, wherein the removal rate of the acid orange 7 can reach 91.2% after 5min of electrolysis.
The foregoing description is only illustrative of the preferred embodiments of the present application and is not to be construed as limiting the scope of the application, i.e., the application is not to be limited to the details of the claims and the description, but rather is to cover all modifications which are within the scope of the application.
Claims (4)
1. A preparation method of a titanium dioxide particle electrode with a high {001} crystal face load is characterized by comprising the following steps: the particle electrode consists of granular activated carbon and titanium dioxide with high {001} crystal face loaded on the granular activated carbon, and the preparation method comprises the following steps:
step one, pretreatment of activated carbon: boiling powdered activated carbon and dilute hydrochloric acid solution at 100 ℃ for 2 hours, cooling, filtering, washing with deionized water until the pH value of the filtrate is neutral, and then vacuum drying at 110 ℃ for 24 hours;
step two, hydrothermal reaction: dissolving titanium tetrafluoride in deionized water, adding hydrochloric acid solution and sodium chloride solid particles, stirring uniformly, adding the powdered activated carbon obtained in the first step, mixing uniformly, pouring into a reaction kettle with polytetrafluoroethylene, and treating for 2-6 hours at 200 ℃, wherein the molar ratio of the titanium tetrafluoride to the hydrochloric acid solution to the sodium chloride is 3-5:1:80, and the mass ratio of the titanium tetrafluoride to the powdered activated carbon is 1-2:30;
step three, high-temperature heat treatment: filtering the mixed solution obtained in the second reaction, washing with deionized water for 5-6 times, vacuum drying at 110 ℃ for 20 hours, and heat treating at 450 ℃ for 2 hours to obtain modified activated carbon;
step four, uniformly mixing and stirring the modified activated carbon obtained in the step three with coal tar, extruding and molding, drying at 110 ℃, and carbonizing at 400 ℃ for 2 hours to obtain the particle electrode loaded with high {001} crystal face titanium dioxide;
the powdered activated carbon is prepared from coconut shells, fruit shells, wood or coal base;
the particle size of the powdered activated carbon is smaller than 200 meshes, the iodine adsorption value is larger than 950mg/L, and the methylene blue adsorption value is 10-15ml;
in the fourth step, the content of the coal tar is 5-10% of the mass of the modified activated carbon.
2. The method for preparing the highly {001} crystal face loaded titanium dioxide particle electrode according to claim 1, which is characterized in that: in the first step, the concentration of the dilute hydrochloric acid aqueous solution is 0.05-0.1mol/L.
3. The method for preparing the highly {001} crystal face loaded titanium dioxide particle electrode according to claim 1, which is characterized in that: in the second step, the concentration of the hydrochloric acid solution is 0.1mol/L.
4. The method for preparing the highly {001} crystal face loaded titanium dioxide particle electrode according to claim 1, which is characterized in that: the titanium dioxide crystal form is anatase.
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