CN113663652A - Preparation method of UIO-66 modified cotton fabric and adsorption of active dye by UIO-66 modified cotton fabric - Google Patents
Preparation method of UIO-66 modified cotton fabric and adsorption of active dye by UIO-66 modified cotton fabric Download PDFInfo
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Abstract
The invention relates to an in-situ growth preparation method of UIO-66-cotton fabric and research application thereof in the field of reactive dyes in adsorption printing wastewater, wherein the technical scheme is as follows: putting the carboxymethylated cotton fabric in low-concentration alkaline solution, zirconium chloride, terephthalic acid, an organic solvent and a pH regulator into a round-bottom flask, heating in a water bath, stirring, washing and airing. Compared with other adsorbents, MOFs have the advantages of higher specific surface area, large porosity, pore size adjustability and the like, but most MOFs have lower stability in water, so UIO-66 is selected. Compared with other MOFs, the UIO-66 has excellent thermal stability and chemical stability, keeps the structure complete in strong acid and strong alkali, and has wide application fields. Meanwhile, the main component of the cotton fiber is cellulose, and the cotton fiber contains big hydroxyl groups and is easy to modify; the structure of the cotton fiber is difficult to be damaged when the cotton fiber absorbs the dye wastewater. The UIO-66 modified cotton fabric is relatively simple in subsequent recovery, the reuse rate of the fabric is improved, and the stability is good.
Description
Technical Field
The invention relates to the field of environmental protection, in particular to a preparation method of UIO-66 modified cotton fabric and adsorption of the fabric on reactive dye.
Background
The textile industry is an important part of the world's economy, where the printing and dyeing industry has developed rapidly in recent years, producing large amounts of dye waste water, both during the production of the dyes and during the use of the dyes. The dye wastewater has complex organic matter components, deep chromaticity, large alkalinity, strong toxicity, high total carbon content and chemical oxygen demand of the organic matters in the water and poor biodegradability, is difficult to self-degrade, needs special purification treatment before discharge, and otherwise can affect human health and bring environmental pollution problems. The reactive dye has relatively good color and luster, convenient use and low cost, and is widely applied at present. Therefore, adsorption of reactive dyes becomes an important part of the treatment of dye wastewater. At present, the treatment technology of dye wastewater mainly comprises physical treatment, biological treatment, chemical treatment and combined treatment process thereof. The physical treatment mainly comprises adsorption and membrane filtration, the adsorption mainly adopts materials with large specific surface area and porous structure or polar groups such as active carbon, clay minerals, industrial waste, metal oxides or layered double hydroxides and agricultural wastes, and the like, and the common adsorption materials have the problems of low capacity, poor mixing property, low cyclic utilization rate and the like, so the application of the adsorption technology in the dye wastewater treatment is limited. The membrane filtration is to remove pollutants by utilizing the selective separation of the membrane on molecules, and comprises the processes of microfiltration, ultrafiltration, nanofiltration, reverse osmosis and the like. However, the membrane separation technique with better separation results is also correspondingly more costly, limiting its application for back-end processing. The biological treatment mainly comprises anaerobic treatment, aerobic treatment and anaerobic-aerobic combined treatment. Although the biological treatment has low cost and easy operation, the removal effect is not ideal and the removal rate is low. The chemical treatment comprises coagulation-flocculation, electric flocculation and advanced oxidation, and the chemical treatment needs a large amount of consumed chemical agents, needs special equipment and has higher operation cost. Wangsheng et al use waste straw powder to prepare modified biochar and remove methylene blue dye in wastewater by photocatalysis, although the method has low cost, the removed dye is single and cannot meet the practical application. Linwenxin et al provide a method for preparing Fe-MOFs and fiber composite materials for adsorbing dye wastewater, but the stability of the MOFs in water is poor, and the adsorption effect of the MOFs can be influenced. In recent years, the metal organic framework as a porous adsorption material is gradually becoming a research hotspot. Metal-Organic Frameworks (MOFs) are solid porous materials formed by the assembly of Metal nodes and multidentate Organic ligands through coordination bonds. The high selectivity and different connection modes of the metal and the organic ligand enable the metal and the organic ligand to show structural and functional diversity. In addition, the MOFs have channel adjustability, huge specific surface area and special metal center, so that the MOFs have wide application prospect as an adsorbent. Although the MOFs can effectively treat the printing and dyeing wastewater, some MOFs have poor stability in water, and further influence the adsorption effect.
The MOF material UIO-66 is selected, and compared with other metal organic frameworks, the UIO-66 has extremely strong stability, excellent thermal stability and obvious tolerance to the widest pH value in water; the UIO-66 is grown on the cotton fabric in situ, the cotton fiber is a natural fiber, the main component is cellulose, and the cellulose contains big hydroxyl groups and is easy to modify; most of the dye wastewater is alkaline environment, and the cotton fiber is difficult to damage when absorbing the dye due to the extremely strong alkali resistance. The UIO-66 grows on the cotton fabric in situ, so that the stability is high, the recovery is easy, the reuse rate is improved, the use cost is reduced, and the method has important significance for treatment of printing and dyeing wastewater, water body environment and soil treatment in China.
Disclosure of Invention
In order to improve the removal efficiency of reactive dyes in printing and dyeing wastewater, the stability of an adsorbent and the recycling rate of the adsorbent, carboxymethylated cotton fabrics in low-concentration alkaline liquor, zirconium chloride, terephthalic acid, an organic solvent and a pH regulator are placed in a round-bottom flask for water bath heating and stirring, and then the cotton fabrics are washed and dried. By comparing the adsorption effect of the UIO-66 powder and the adsorption effect of the UIO-66 modified cotton fabric on the dye, the adsorption rate of the UIO-66 modified cotton fabric is over 90 percent, and the stability of the invention in practical cycle application is greatly improved.
In order to achieve the purpose, the technical scheme of the invention is as follows:
putting the carboxymethylated cotton fabric in low-concentration alkaline solution, zirconium chloride, terephthalic acid, an organic solvent and a pH regulator into a round-bottom flask, heating in a water bath, stirring, washing and airing.
Preferably, the UIO-66-cotton fabric in-situ growth preparation method comprises the following steps of pretreating the cotton fabric, wherein the pretreatment conditions are as follows: soaking the cotton fabric in deionized water containing 0.1-0.3% of sodium hydroxide, 0.1-0.6% of non-ionic surfactant Triton X-100 and 0.1-0.3% of acetic acid at 80-120 deg.c for 1-3 hr, and hanging and drying at 25-45 deg.c.
Preferably, the UIO-66-cotton fabric in-situ growth preparation method comprises the following steps of carboxymethylation of the cotton fabric in low-concentration alkali liquor: soaking the washed cotton fabric in isopropanol, adding weak base, and stirring at 25-45 deg.C for 1-3 h. Then heating the solution to 35-65 ℃, adding sodium chloroacetate, stirring strongly for 1-5h, and then baking at 60-100 ℃ for 20-60 min. Then soaking the cotton fabric in weak acid solution for 5-20min, washing with deionized water, and hanging and drying at 25-45 deg.C.
Preferably, the treatment method of carboxymethylation of the cotton fabric under the condition of low-concentration alkali liquor is characterized in that the weak base is sodium hydroxide or sodium carbonate.
Preferably, the processing method of carboxymethylation of the cotton fabric under the condition of low-concentration alkali liquor is characterized in that the content of sodium hydroxide is 0.1-0.3 percent by mass percent.
Preferably, the treatment method of carboxymethylation of the cotton fabric under the condition of low-concentration alkali liquor is characterized in that the weak acid is carbonic acid or acetic acid.
Preferably, the method for processing the carboxymethylation of the cotton fabric under the condition of low-concentration alkali liquor is characterized by comprising the following components in percentage by mass, 0.1-0.3% of acetic acid and 2.5-6% of sodium chloroacetate.
Preferably, the UIO-66-cotton fabric in-situ growth preparation method is characterized in that zirconium chloride is dissolved in a mixed solution of an organic solvent and a pH regulator, and ultrasonic action is carried out for 10-30min to obtain a metal precursor solution; dissolving terephthalic acid in an organic solvent in another beaker, then uniformly mixing the terephthalic acid with a metal precursor solution, adding a cotton fabric into the solution, carrying out water bath heating reaction for 10-24h at 60-120 ℃, then washing for 3-5 times by using the organic solvent, and finally carrying out vacuum drying for 12-24 h.
Preferably, the UIO-66-cotton fabric in-situ growth preparation method is characterized in that the organic solvent is N, N-dimethylformamide or methanol, and the pH regulator is concentrated hydrochloric acid.
Preferably, the UIO-66-cotton fabric in-situ growth preparation method is characterized by comprising, by mass, 0.5% -1.5% of zirconium chloride, 0.5% -1.5% of terephthalic acid, 5% -12% of concentrated hydrochloric acid and the balance of DMF.
An application of UIO-66-cotton fabric in adsorption of reactive dye in printing and dyeing wastewater.
Preferably, the application of the UIO-66-cotton fabric in adsorbing the reactive dye in the printing and dyeing wastewater is characterized in that the adsorbed reactive dye is vinyl maple type reactive dye, monochlorotriazine type reactive dye and dichloros-triazine type reactive dye
The beneficial effect that adopts foretell technical scheme to produce lies in:
(1) compared with other porous adsorbents, the MOF material has the advantages of higher specific surface area, large porosity, pore size adjustability and the like, but most MOFs have lower stability in water, so the UIO-66 is adopted in the invention to solve the problem. Compared with other MOFs, the UIO-66 has excellent thermal stability and chemical stability besides common structural advantages, keeps the structure complete in strong acid, strong alkali and various organic solvents, and is very wide in application field.
(2) The cotton fiber is a natural fiber, the main component of the cotton fiber is cellulose, and the cotton fiber contains big hydroxyl groups and is easy to modify; most of the dye wastewater is alkaline environment, and the cotton fiber is difficult to damage when absorbing the dye due to the extremely strong alkali resistance.
(3) In order to improve the reutilization rate, the obtained UIO-66 modified cotton fabric is relatively simple in subsequent recovery, the reutilization rate is improved, and the stability is good.
(4) The UIO-66 modified cotton fabric used in the invention is prepared by a one-bath method, the production flow is simple, the operation is convenient, the production cost is reduced, and the energy consumption is saved.
Drawings
FIG. 1: aUIO-66SEM picture; b, taking an SEM image of the cotton fabric; c UIO-66 modified Cotton Fabric SEM Picture
FIG. 2: the effect of a time on the adsorption capacity of UIO-66 to reactive orange 16; influence of b time on adsorption quantity of reactive orange 16 adsorbed by UIO-66 modified cotton fabric
FIG. 3: the effect of a time on the adsorption capacity of UIO-66 for active violet 5; influence of b time on adsorption activity of violet 5 on UIO-66 modified cotton fabric
FIG. 4: the effect of a time on the adsorption capacity of UIO-66 adsorptive active red X-3B; influence of B time on adsorption capacity of active Red X-3B for adsorption of UIO-66 modified Cotton Fabric
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
Example 1 preparation of UIO-66 modified Cotton Fabric
Pretreating cotton fabrics: 0.5g of sodium hydroxide, 1.5g of a nonionic surfactant Triton X-100 and 0.75g of acetic acid were dissolved in 500mL of deionized water to prepare a refined solution. Soaking the cotton fabric in a refining solution at 100 ℃ for washing for 1h, and hanging and airing at room temperature.
(II) carboxymethylation of cotton sample: the washed cotton fabric was soaked in 200mL of isopropanol, 20mL of 7.5% (w/v) sodium hydroxide was added and stirred at room temperature for 1 h. Then the solution is heated to 45 ℃, 12g of sodium chloroacetate is added into a reaction bottle, strong stirring is carried out for 3h, and then the cotton fabric is baked for 60min at 85 ℃. Then, the cotton fabric is soaked in acetic acid solution for 5min, washed by water and hung and dried at room temperature.
(III) preparation of UIO-66 modified cotton fabric: dissolving zirconium chloride (1510mg, 6.48mmol) in a mixed solution of 60mLDMF and 12mL concentrated hydrochloric acid, and performing ultrasonic action for 10min to obtain a metal precursor solution; in a separate beaker, dissolving terephthalic acid (1495mg, 9mmol) in 120mLDMF, adding the solution into the precursor solution, uniformly mixing, adding the cotton fabric into the solution, heating in a water bath to 80 ℃ for reaction for 12h, washing 3 times with DMF and methanol solution respectively after the reaction is finished, and finally drying in vacuum for 24 h.
As shown in figure 1, a figure UIO-66SEM figure is formed by agglomeration of a plurality of octahedral small crystals, a figure b is a cotton fabric SEM figure with smooth surface, and a figure c is a UIO-66 modified cotton fabric SEM figure, so that compared with a cotton fabric raw cloth in a figure b, the modified cotton fabric surface has obvious small particles, which indicates that UIO-66 successfully grows on the cotton fabric in situ, and the cotton fabric has wide application prospect in the aspect of dye adsorption.
Example 2 Effect of time on adsorption absorption energy of UIO-66, UIO-66 modified Cotton fabrics adsorbing reactive orange 16
Method 1-UIO-66: preparing 100mL of active orange 16 dye solution with the concentration of 60mg/L into a conical flask, weighing 50mg of UIO-66 powder, putting into the conical flask, oscillating and adsorbing at room temperature at the rotating speed of 200r/min every 10min, 20min, 30min, 40min, 60min, 90min, 120min, 150min and 180min, and measuring the absorbance and calculating the adsorption capacity by analogy.
Method 2-UIO-66 modified cotton fabric: preparing 30mL of active orange 16 dye solution with the concentration of 60mg/L into a conical flask, weighing 0.9g of UIO-66 modified cotton fabric, putting the cotton fabric into the conical flask, carrying out oscillation adsorption at room temperature at the rotating speed of 200r/min every 10min, 20min, 30min, 40min, 60min, 90min, 120min, 150min and 180min, and measuring the absorbance and calculating the adsorption capacity by analogy.
As shown in fig. 2, analysis of the graph of change of adsorption amount with time shows that UIO-66 powder reaches adsorption equilibrium in 1 hour, the maximum adsorption amount is 118mg/g, the removal rate reaches 98%, and the UIO-66 powder has a higher adsorption rate for reactive orange 16 and a better adsorption effect; the UIO-66 modified cotton fabric reaches the adsorption balance in 3 hours, the maximum adsorption capacity is 1.79mg/g, and the removal rate reaches 89%.
EXAMPLE 3 Effect of time on adsorption energy of adsorption of active Violet 5 on UIO-66, UIO-66 modified Cotton fabrics
Method 1-UIO-66: preparing 100mL of active violet 5 dye solution with the concentration of 60mg/L into a conical flask, weighing 50mg of UIO-66 powder, putting into the conical flask, oscillating and adsorbing at room temperature at the rotating speed of 200r/min every 10min, 20min, 30min, 40min, 60min, 90min, 120min, 150min and 180min, and measuring the absorbance and calculating the adsorption capacity by analogy.
Method 2-UIO-66 modified cotton fabric: preparing 30mL of active violet 5 dye solution with the concentration of 60mg/L into a conical flask, weighing 0.9g of UIO-66 modified cotton fabric, putting the cotton fabric into the conical flask, carrying out oscillation adsorption at room temperature at the rotating speed of 200r/min every 10min, 20min, 30min, 40min, 60min, 90min, 120min, 150m n min and 180min, and measuring the absorbance and calculating the adsorption capacity by analogy.
As shown in fig. 3, according to the trend analysis of the change of the adsorption amount with time, the UIO-66 powder reaches the adsorption equilibrium within 2 hours, the maximum adsorption amount is 114mg/g, the removal rate reaches 95%, and the UIO-66 powder has a high adsorption rate for active violet 5 and a good adsorption effect; the UIO-66 modified cotton fabric reaches adsorption balance in 3.5 hours, the maximum adsorption capacity is 1.5mg/g, and the removal rate reaches 70%.
EXAMPLE 4 Effect of time on the adsorption Capacity of the adsorption-active Red X-3B of UIO-66, UIO-66 modified Cotton fabrics
Method 1-UIO-66: preparing 100mL of active red X-3B dye solution with the concentration of 60mg/L into a conical flask, weighing 50mg of UIO-66 powder, putting into the conical flask, carrying out oscillation adsorption at room temperature at the rotation speed of 200r/min every 10min, 20min, 30min, 40min, 60min, 90min, 120min, 150min and 180min, and repeating the steps, measuring the absorbance, and calculating the adsorption capacity.
Method 2-UIO-66 modified cotton fabric: preparing 30mL of active red X-3B dye solution with the concentration of 60mg/L into a conical flask, weighing 0.9g of UIO-66 modified cotton fabric, putting the cotton fabric into the conical flask, carrying out oscillation adsorption at room temperature at the rotating speed of 200r/min, and measuring the absorbance and calculating the adsorption capacity of the cotton fabric at intervals of 10min, 20min, 30min, 40min, 60min, 90min, 120min, 150min and 180min by analogy.
As shown in FIG. 4, from the analysis of the graph of the change of the adsorption amount with time, the UIO-66 powder reached the adsorption equilibrium within 2 hours, the maximum adsorption amount was 120mg/g, and the removal rate reached 100%; the UIO-66 modified cotton fabric reaches adsorption balance in 3 hours, the maximum adsorption capacity is 1.93mg/g, and the removal rate reaches 96%.
In the dynamic adsorption process, the UIO-66 shows excellent adsorption performance in the adsorption of the reactive dye due to the large specific surface area, high porosity and electrostatic attraction. Compared with UIO-66 powder, although the adsorption rate of the UIO-66 modified cotton fabric is slightly slow, the cotton fabric is easy to recover relative to the powder, and the removal rate is close to that of the UIO-66 powder, so that the modified cotton fabric obtained by growing the UIO-66 on the cotton fabric has a good adsorption effect and the advantage of easy recovery, and the reuse rate of the modified cotton fabric is improved.
Claims (10)
1. A UIO-66-cotton fabric in-situ growth preparation method is characterized in that carboxymethylated cotton fabric under low-concentration alkaline liquor, zirconium chloride, terephthalic acid, an organic solvent and a pH regulator are placed into a round-bottom flask to be heated in a water bath, stirred, washed and dried.
2. The UIO-66-cotton fabric in-situ growth preparation method of claim 1, wherein the cotton fabric is pretreated under the following pretreatment conditions: soaking the cotton fabric in deionized water containing 0.1-0.3% of sodium hydroxide, 0.1-0.6% of non-ionic surfactant Triton X-100 and 0.1-0.3% of acetic acid at 80-120 deg.c for 1-3 hr, and hanging and drying at 25-45 deg.c.
3. The UIO-66-cotton fabric in-situ growth preparation method according to claim 1, wherein the carboxymethylation treatment conditions of the cotton fabric under low-concentration alkaline solution are as follows: soaking the washed cotton fabric in isopropanol, adding weak base, and stirring at 25-45 deg.C for 1-3 h. Then heating the solution to 35-65 ℃, adding sodium chloroacetate, stirring strongly for 1-5h, and then baking at 60-100 ℃ for 20-60 min. Then soaking the cotton fabric in weak acid solution for 5-20min, washing with deionized water, and hanging and drying at 25-45 deg.C.
4. The carboxymethylation method for the cotton fabrics under the condition of low-concentration alkaline liquor according to claim 3, characterized in that the weak base is sodium hydroxide or sodium carbonate, and the content of the sodium hydroxide is 0.1-0.3% by mass percent.
5. The carboxymethylation method for the cotton fabrics under the condition of low-concentration alkaline liquor according to claim 3, characterized in that the weak acid is carbonic acid or acetic acid, and comprises the following components by mass percent, wherein the acetic acid is 0.1-0.3%, and the sodium chloroacetate is 2.5-6%.
6. The UIO-66-cotton fabric in-situ growth preparation method according to claim 1, wherein zirconium chloride is dissolved in a mixed solution of an organic solvent and a pH regulator, and ultrasonic action is performed for 10-30min to obtain a metal precursor solution; dissolving terephthalic acid in an organic solvent in another beaker, then uniformly mixing the terephthalic acid with a metal precursor solution, adding a cotton fabric into the solution, carrying out water bath heating reaction for 10-24h at 60-120 ℃, then washing for 3-5 times by using the organic solvent, and finally carrying out vacuum drying for 12-24 h.
7. The method of claim 7, wherein the organic solvent is N, N-dimethylformamide or methanol and the pH adjusting agent is concentrated hydrochloric acid.
8. The UIO-66-cotton fabric in-situ growth preparation method according to claim 7, characterized by comprising, by mass, 0.5% -1.5% of zirconium chloride, 0.5% -1.5% of terephthalic acid, 5% -12% of concentrated hydrochloric acid, and the balance of DMF.
9. An application of UIO-66-cotton fabric in adsorption of reactive dye in printing and dyeing wastewater.
10. The use of a UIO-66-cotton fabric for adsorbing reactive dyes from printing and dyeing wastewater as claimed in claim 10, wherein the reactive dyes adsorbed are vinyl maple type reactive dyes, monochlorotriazine type reactive dyes, dichloros-triazine type reactive dyes.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114225913A (en) * | 2022-01-05 | 2022-03-25 | 天津工业大学 | Efficient preparation method of UiO-66 and adsorption of UiO-66 on cationic dye |
| CN114247430A (en) * | 2022-01-05 | 2022-03-29 | 天津工业大学 | Active dye adsorbent and preparation method thereof |
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