CN112458747A - Loaded TiO (titanium dioxide)2Preparation method of functional fabric of iron-based MOF - Google Patents

Loaded TiO (titanium dioxide)2Preparation method of functional fabric of iron-based MOF Download PDF

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CN112458747A
CN112458747A CN202010979826.2A CN202010979826A CN112458747A CN 112458747 A CN112458747 A CN 112458747A CN 202010979826 A CN202010979826 A CN 202010979826A CN 112458747 A CN112458747 A CN 112458747A
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fabric
solution
tio
iron
based mof
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王春梅
王静
娄娅娅
徐康景
顾振宇
李龙飞
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Nantong University
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    • D—TEXTILES; PAPER
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
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    • B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
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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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
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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
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Abstract

The invention discloses a loaded TiO2The preparation method of the functional fabric of the Fe-based MOF comprises the steps of adding 2-4 mmol of trimesic acid into 10-25 mL of 1M sodium hydroxide, treating for 10-20 min by ultrasonic waves to dissolve the trimesic acid, adjusting the pH value to obtain a solution A, and mixing 0.2-0.4 g of the fabric and 10% -30% of nano TiO based on the weight of the fabric2Adding the solution A into the solution A, carrying out ultrasonic treatment for 10-20 min, adding 3-6 mmol of ferrous sulfate heptahydrate into 30-40 mL of distilled water, carrying out ultrasonic treatment for 5-10 min to obtain a solution B, dropwise adding the solution B into the solution A soaked with the fabric, carrying out oscillation reaction at room temperature for 12-16 h, taking out the fabric after the reaction is finished, washing with water, and drying to obtain the functional fabric.

Description

Loaded TiO (titanium dioxide)2Preparation method of functional fabric of iron-based MOF
Technical Field
The invention relates to the technical field of functional fiber materials, in particular to a TiO-loaded material2Preparation method of functional fabric of iron-based MOF.
Background
In the world, water resource shortage becomes one of the problems to be solved urgently, along with the development of industry, a large amount of organic matters enter a water body, and the high-efficiency treatment of the organic matters becomes a difficult point in the environmental field. The printing and dyeing industry is an industrial wastewater discharge large-scale household, and has the disadvantages of large total pollution discharge amount, heavy pollution, deep chroma, large pH value change and large treatment difficulty. In order to better reduce the influence of the printing and dyeing wastewater on the environment, a more efficient and environment-friendly method for treating the printing and dyeing wastewater is needed.
TiO2As a semiconductor type photocatalyst with wide application, a plurality of organic matters can be effectively degraded into biodegradable compounds, and even can be mineralized into harmless carbon dioxide and water. TiO 22The stability is good, and the mechanical property is excellent, so that the method is widely researched. However, TiO2The forbidden band width is large (3.2 eV), and the photocatalyst shows strong photocatalytic activity only in an ultraviolet light wave band, thereby generating application of the photocatalystCertain limitations. Metal organic framework Materials (MOFs) are a class of materials that form periodic network structures from organic ligands and metal ions through self-assembly. Compared with the traditional inorganic materials, the MOFs have the advantages of large specific surface area, strong structure and function controllability, large unsaturated coordination quantity and the like, have higher catalytic activity, and have attracted wide attention in the field of photocatalysis. In order to further improve the utilization efficiency of the photocatalyst on solar energy, the MOFs can be used as a substrate to construct the composite photocatalyst. CN109289927A provides a preparation method and application of a nano titanium dioxide @ iron-based MOF visible light composite catalyst, and the nano titanium dioxide @ iron-based MOF visible light composite catalyst is constructed to reduce the electron-hole recombination rate and improve the photocatalytic performance, but has the defects of easy agglomeration, difficult recovery and the like.
To solve the above problems, the present invention provides TiO2The Fe-based MOF is loaded on the nylon fabric with light and thin texture, high strength and lower cost, and the prepared functional material can solve the problem of powdery TiO2The method has the advantages of simple and safe operation, good reuse effect and wide application prospect in the aspect of printing and dyeing wastewater treatment.
Disclosure of Invention
The invention provides a supported TiO2The preparation method of the iron-based MOF functional fabric is used for decoloring organic dyes in printing and dyeing wastewater, solves the problems of chromaticity problem, easy agglomeration, difficult recovery and the like caused by the organic dyes in the prior art, is beneficial to the recovery and reuse of the wastewater, and achieves the aim of reducing the emission of pollutants.
The invention adopts the following technical scheme: loaded TiO (titanium dioxide)2A preparation method of a functional fabric of iron-based MOF comprises the following specific steps:
the first step is as follows: adding 2-4 mmol of trimesic acid into 10-25 mL of 1M sodium hydroxide, treating with 40KHZ ultrasonic waves for 10-20 min to dissolve the trimesic acid, and adjusting the pH value to obtain a solution A;
the second step is that: 0.2-0.4 g of fabric and 10-30% of nano TiO based on the weight of the fabric2Is added toTreating the solution A with 40KHZ ultrasonic wave for 10-20 min;
the third step: adding 3-6 mmol of ferrous sulfate heptahydrate into 30-40 mL of distilled water, and treating with 40KHZ ultrasonic waves for 5-10 min to obtain a solution B;
the fourth step: and dropwise adding the solution B into the solution A soaked with the fabric, carrying out oscillation reaction at room temperature for 12-16 h, taking out the fabric after the reaction is finished, washing with water, and drying to obtain the functional fabric.
As a preferred technical scheme of the invention: and adjusting the pH range to 6-8 in the first step.
As a preferred technical scheme of the invention: the fabrics used in the second step are nylon woven fabrics and knitted fabrics; the nano TiO is used2The particle size is 30 to 50 nm.
As a preferred technical scheme of the invention: and in the fourth step, the dropping speed is 50-60 drops/min.
Has the advantages that:
the invention relates to a TiO-loaded material2Compared with the prior art, the preparation method of the functional fabric of the iron-based MOF has the following technical effects:
1. the invention provides an in-situ grown TiO2The iron-based MOF obtains a functional fiber material for catalyzing and degrading dyes under simulated sunlight.
2. Adding TiO into the mixture2The Fe-based MOF is loaded on the nylon fabric with light and thin texture, high strength and lower cost, and the prepared functional material can solve the problem of powdery TiO2The iron-based MOF is easy to agglomerate and is not easy to recover;
3. the method is simple and safe to operate, has good repeating effect, and has wide application prospect in the aspect of printing and dyeing wastewater treatment;
4. the problems of chromaticity problem, easy agglomeration, difficult recovery and the like caused by organic dyes in the prior art are solved, the recovery and the reuse of waste water are facilitated, and the aim of reducing pollutant discharge is fulfilled.
5. The technical scheme provided by the invention is to use TiO with large specific surface area, strong structure controllability and large unsaturated coordination quantity2Iron-based MOF composite photocatalystThe functional fabric is prepared by being carried on the fabric with excellent performance and low cost.
6. The method has simple process and low cost of raw materials, and can comprehensively utilize polyamide fabric and TiO2The iron-based MOF has excellent performance and excellent decolorizing effect on high-concentration organic dye in printing and dyeing wastewater.
7. Adding TiO into the mixture2The/iron-based MOF is loaded on the nylon fabric and can solve the problem of powdery TiO2The iron-based MOF is difficult to recover in water treatment, can reduce the electron-hole recombination rate and improve the photocatalytic performance, and has wide application prospect.
8. Supported TiO2Compared with the unloaded fabric, the iron-based MOF polyamide fabric has the advantages that the decolorization rate under the dark condition can be improved by 51.3% to the maximum extent, and the decolorization rate under the illumination condition can be improved by 57.0% to the maximum extent.
Drawings
FIG. 1 shows the TiO loading of the present application2The decolorization effect of the nylon fabric of the iron-based MOF on the active black KN-B dye under the dark condition is shown.
FIG. 2 shows the TiO loading of the present application2The decolorization effect of the nylon fabric of the iron-based MOF on the active black KN-B dye under the irradiation of visible light is shown.
Detailed Description
The present invention is further described with reference to the following examples, which are intended to be illustrative only and not to be limiting of the scope of the claims, and other alternatives which may occur to those skilled in the art are within the scope of the claims.
Example 1:
loaded TiO (titanium dioxide)2A preparation method of a functional fabric of iron-based MOF comprises the following specific steps:
the first step is as follows: adding 2 mmol of trimesic acid into 10 mL of 1M sodium hydroxide, performing ultrasonic treatment for 10 min by using 40KHZ, and adjusting the pH value to 7 to obtain a solution A;
the second step is that: 0.2 g of nylon fabric and 10 percent of nano TiO based on the weight of the fabric2Is added into the solutionTreating liquid A with 40KHZ ultrasonic wave for 10 min;
the third step: adding 3 mmol ferrous sulfate heptahydrate into 30 mL distilled water, and treating with 40KHZ ultrasonic wave for 5 min to obtain solution B;
the fourth step: and (3) dropwise adding the solution B into the solution A soaked with the nylon fabric at the speed of 50-60 drops/min, carrying out oscillation reaction at room temperature for 12 hours, taking out the nylon fabric after the reaction is finished, washing with water, and drying to obtain the functional fabric.
In order to investigate the adsorption effect of the prepared functional fabric on the dye, an active black KN-B dye is selected as a research object, the adsorption performance of the dye under the dark condition is measured, and the test conditions are as follows: and adsorbing 50mL of active black KN-B dye solution with the mass concentration of 50mg/L for 60 min at room temperature by using 0.25g of functional fabric, and measuring the absorbance of the solution every 10 min. And calculating the decolorization ratio of the dye.
The decolorization ratio of the prepared functional fabric to the active black KN-B dye solution is shown in figure 1. As can be seen from FIG. 1, after 60 min of dark adsorption, the loaded TiO was2Nylon fabric of/iron-based MOF is compared with non-loaded TiO2The decoloring rate of the nylon fabric of the iron-based MOF on the active black KN-B dye liquor is improved by 49.1 percent. Description of the Supported TiO2The nylon fabric of the iron-based MOF has better adsorption effect on the dye.
In order to examine the photocatalytic performance of the prepared functional fabric, 0.25g of the functional fabric was irradiated by a 1000W xenon lamp, and 12uL H was added to 50mL of the functional fabric2O2The active black KN-B dye solution with the concentration of 50mg/L is treated for 60 min at room temperature, the absorbance of the solution is measured every 10 min, and the decolorization rate of the dye is calculated.
The decolorization ratio of the prepared functional material to the active black KN-B dye solution under the irradiation of a 1000W xenon lamp is shown in figure 2. As can be seen from FIG. 2, after 60 min of illumination, the TiO loading2Nylon fabric of/iron-based MOF is compared with non-loaded TiO2The decoloring rate of the nylon fabric of the Fe-based MOF on the active black KN-B dye liquor is improved by 55.5 percent and reaches 95.0 percent. Description of the Supported TiO2The nylon fabric of the iron-based MOF has better photocatalytic color mapping effect on dye.
Example 2:
loaded TiO (titanium dioxide)2A preparation method of a functional fabric of iron-based MOF comprises the following specific steps:
the first step is as follows: adding 3 mmol of trimesic acid into 15 mL of 1M sodium hydroxide, performing ultrasonic treatment for 10 min by using 40KHZ, and adjusting the pH value to 6 to obtain a solution A;
the second step is that: 0.3 g of nylon fabric and 30 percent of nano TiO based on the weight of the fabric2Adding into solution A, and treating with 40KHZ ultrasonic wave for 20 min;
the third step: adding 6 mmol ferrous sulfate heptahydrate into 40 mL distilled water, and treating with 40KHZ ultrasonic wave for 5 min to obtain solution B;
the fourth step: and (3) dropwise adding the solution B into the solution A soaked with the nylon fabric at the speed of 50-60 drops/min, carrying out oscillation reaction at room temperature for 16 h, taking out the nylon fabric after the reaction is finished, washing with water, and drying to obtain the functional fabric.
In order to investigate the adsorption effect of the prepared functional fabric on the dye, an active black KN-B dye is selected as a research object, the adsorption performance of the dye under the dark condition is measured, and the test conditions are as follows: and adsorbing 50mL of active black KN-B dye solution with the mass concentration of 50mg/L for 60 min at room temperature by using 0.25g of functional fabric, and measuring the absorbance of the solution every 10 min. And calculating the decolorization ratio of the dye.
The decolorization ratio of the prepared functional fabric to the active black KN-B dye solution is shown in figure 1. As can be seen from FIG. 1, after 60 min of dark adsorption, the loaded TiO was2Nylon fabric of/iron-based MOF is compared with non-loaded TiO2The decoloring rate of the nylon fabric of the Fe-based MOF to the active black KN-B dye liquor is improved by 51.3 percent. Description of the Supported TiO2The nylon fabric of the iron-based MOF has better adsorption effect on the dye.
In order to examine the photocatalytic performance of the prepared functional fabric, 0.25g of the functional fabric was irradiated by a 1000W xenon lamp, and 12uL H was added to 50mL of the functional fabric2O2The active black KN-B dye solution with the concentration of 50mg/L is treated for 60 min at room temperature, the absorbance of the solution is measured every 10 min, and the decolorization rate of the dye is calculated.
The functional material thus obtainedThe decolorization ratio of the material to the active black KN-B dye solution under the irradiation of a xenon lamp of 1000W is shown in figure 2. As can be seen from FIG. 2, after 60 min of illumination, the TiO loading2Nylon fabric of/iron-based MOF is compared with non-loaded TiO2The decoloring rate of the nylon fabric of the Fe-based MOF on the active black KN-B dye liquor is improved by 57.0 percent and reaches 96.5 percent. Description of the Supported TiO2The nylon fabric of the iron-based MOF has better photocatalytic color mapping effect on dye.
Example 3:
loaded TiO (titanium dioxide)2A preparation method of a functional fabric of iron-based MOF comprises the following specific steps:
the first step is as follows: adding 3 mmol of trimesic acid into 20 mL of 1M sodium hydroxide, performing ultrasonic treatment for 10 min by using 40KHZ, and adjusting the pH value to 8 to obtain a solution A;
the second step is that: 0.4 g of nylon fabric and 20 percent of nano TiO based on the weight of the fabric2Adding into solution A, and treating with 40KHZ ultrasonic wave for 20 min;
the third step: adding 4 mmol of ferrous sulfate heptahydrate into 30 mL of distilled water, and performing ultrasonic treatment with 40KHZ for 5 min to obtain a solution B;
the fourth step: and (3) dropwise adding the solution B into the solution A soaked with the nylon fabric at the speed of 50-60 drops/min, carrying out oscillation reaction at room temperature for 16 h, taking out the nylon fabric after the reaction is finished, washing with water, and drying to obtain the functional fabric.
In order to investigate the adsorption effect of the prepared functional fabric on the dye, an active black KN-B dye is selected as a research object, the adsorption performance of the dye under the dark condition is measured, and the test conditions are as follows: and adsorbing 50mL of active black KN-B dye solution with the mass concentration of 50mg/L for 60 min at room temperature by using 0.25g of functional fabric, and measuring the absorbance of the solution every 10 min. And calculating the decolorization ratio of the dye.
The decolorization ratio of the prepared functional fabric to the active black KN-B dye solution is shown in figure 1. As can be seen from FIG. 1, after 60 min of dark adsorption, the loaded TiO was2Nylon fabric of/iron-based MOF is compared with non-loaded TiO2The decoloring rate of the nylon fabric of the Fe-based MOF on the active black KN-B dye liquor is improved by 48.3 percent. Description of the Supported TiO2Method for producing iron-based MOFThe nylon fabric has better adsorption effect on dye.
In order to examine the photocatalytic performance of the prepared functional fabric, 0.25g of the functional fabric was irradiated by a 1000W xenon lamp, and 12uL H was added to 50mL of the functional fabric2O2The active black KN-B dye solution with the concentration of 50mg/L is treated for 60 min at room temperature, the absorbance of the solution is measured every 10 min, and the decolorization rate of the dye is calculated.
The decolorization ratio of the prepared functional material to the active black KN-B dye solution under the irradiation of a 1000W xenon lamp is shown in figure 2. As can be seen from FIG. 2, after 60 min of illumination, the TiO loading2Nylon fabric of/iron-based MOF is compared with non-loaded TiO2The decoloring rate of the nylon fabric of the Fe-based MOF on the active black KN-B dye liquor is improved by 54.4 percent and reaches 93.9 percent. Description of the Supported TiO2The nylon fabric of the iron-based MOF has better photocatalytic color mapping effect on dye.
As can be seen from FIG. 1, the adsorption time was 60 min under dark conditions, and TiO was not supported2Chinlon fabric of/iron-based MOF has almost no decolorizing effect and is loaded with TiO2The maximum polyamide fabric decoloring rate of the iron-based MOF can reach 51.7% (example 2). As can be seen from FIG. 2, 12uL of H was added2O2Reacting for 60 min under the illumination condition, and not loading TiO2The decolorization rate of the/iron-based MOF polyamide fabric is 39.5 percent, and the polyamide fabric is loaded with TiO2The maximum polyamide fabric decoloring rate of the iron-based MOF can reach 96.5% (example 2). After the reaction time reaches 12 hours, the influence of the length of the reaction time on the decoloring effect is small, the mol ratio of the trimesic acid to the ferrous sulfate has a certain influence on the decoloring, and the higher the ferrous sulfate input ratio is, the better the decoloring rate is. The decolorization rate is from large to small: trimesic acid/ferrous sulfate = 1/2 (example 2) > trimesic acid/ferrous sulfate = 2/3 (example 1) > trimesic acid/ferrous sulfate = 3/4 (example 3).

Claims (4)

1. Loaded TiO (titanium dioxide)2A preparation method of a functional fabric of iron-based MOF is characterized by comprising the following specific steps:
the first step is as follows: adding 2-4 mmol of trimesic acid into 10-25 mL of 1M sodium hydroxide, treating with 40KHZ ultrasonic waves for 10-20 min to dissolve the trimesic acid, and adjusting the pH value to obtain a solution A;
the second step is that: 0.2-0.4 g of fabric and 10-30% of nano TiO based on the weight of the fabric2Adding the mixture into the solution A, and treating the mixture for 10-20 min by using 40KHZ ultrasonic waves;
the third step: adding 3-6 mmol of ferrous sulfate heptahydrate into 30-40 mL of distilled water, and treating with 40KHZ ultrasonic waves for 5-10 min to obtain a solution B;
the fourth step: and dropwise adding the solution B into the solution A soaked with the fabric, carrying out oscillation reaction at room temperature for 12-16 h, taking out the fabric after the reaction is finished, washing with water, and drying to obtain the functional fabric.
2. The TiO-supported catalyst according to claim 12A preparation method of a functional fabric of iron-based MOF is characterized in that: and adjusting the pH range to 6-8 in the first step.
3. The TiO-supported catalyst according to claim 12A preparation method of a functional fabric of iron-based MOF is characterized in that: the fabrics used in the second step are nylon woven fabrics and knitted fabrics; the nano TiO is used2The particle size is 30 to 50 nm.
4. The TiO-supported material according to claim 32A preparation method of a functional fabric of iron-based MOF is characterized in that: and in the fourth step, the dropping speed is 50-60 drops/min.
CN202010979826.2A 2020-09-17 2020-09-17 Loaded TiO (titanium dioxide)2Preparation method of functional fabric of iron-based MOF Pending CN112458747A (en)

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