A preparation method of titanium dioxide/13X molecular sieves compound materials used for treating dyestuff waste water

Abstract

The invention discloses a method for preparation of TiO2 molecular screen compound material for treating dyes waste water, comprising: a. preparing titanium tetrachloride / absolute ethyl alcohol solution; b. weighing 13X molecular screen of 80 mesh-100 mesh into the solution; c. adding dilute HNO3 solution dropwise and adding with deionized water after agitating; d. sealing and aging at normal temperature and vacuum extraction filtering; e. drying; f. calcining the sample at 200 DEG C. finally to obtain an end product. The invention has 13X molecular screen as substrate, and titanium tetrachloride as titanium source, introduces Ti in TiO2 anatase crystal form into frame of the molecular screen through liquid-solid reaction and partly adsorbs Ti on surface and in hollow space of the molecular screen, thereby, the composite material has adsorbability and ion-exchange property of the 13X molecular screen, as well as has photocatalysis activity of the TiO2, which preparing method is simple in operation, less consumption in energy and low in cost.

Description

technical field

[0001] The present invention relates to a kind of preparation method of molecular sieve composite material, more specifically relate to a kind of TiO used for dye wastewater treatment 2 / 13X molecular sieve composite material preparation method. Background technique

[0002] The world's annual output of dyes is about 700,000 tons, of which about 10-15% is discharged into the environment in the form of wastewater. Dye wastewater is characterized by high chroma, high toxicity, COD Cr (chemical oxygen demand) high, low biodegradability (BOD 5 / COD<0.1), most dyes are resistant to photolysis, oxidation, and biodegradation, and are persistent organic pollutants. These dye wastewater often cause serious water pollution and become a difficult point in environmental restoration. At present, the treatment of dye wastewater commonly used at home and abroad is generally non-destructive technology, such as physical adsorption method, coagulation method, air flotat...

Examples

Embodiment 1

[0023] 1. Measure 8ml of titanium tetrachloride solution in a beaker filled with 40ml of absolute ethanol to make a titanium tetrachloride / absolute ethanol solution, and stir vigorously at a constant speed.

[0024] 2. Weigh 10g of 13X molecular sieve with a particle size of 100 mesh, add it into a beaker filled with titanium tetrachloride solution, and stir vigorously at a constant speed for 3 hours.

[0025] 3. Then add dilute HNO dropwise into the beaker 3 Solution 10ml, stir for 2-3min, slowly add about 3ml of deionized water, stop stirring.

[0026] 4. After airtight aging at room temperature for 48 hours, the vacuum pump is used for suction filtration, and the filtrate is washed several times with absolute ethanol and deionized water.

[0027] 5. Put the filtered sample into a constant temperature blast drying oven, adjust the temperature to 110°C, and dry for 3 hours.

[0028] 6. Put the dried sample into a muffle furnace and bake it at 200°C for 4h.

[0029] 7. Get Ti...

Embodiment 2

[0031] 1. Measure 6ml of titanium tetrachloride solution in a beaker filled with 35ml of absolute ethanol to make a titanium tetrachloride / absolute ethanol solution, and stir vigorously at a constant speed.

[0032] 2. Weigh 10g of 13X molecular sieve with a particle size of about 100 mesh, add it into a beaker filled with titanium tetrachloride solution, and stir vigorously at a constant speed for 2 hours.

[0033] 3. Then add dilute HNO dropwise into the beaker 3 Solution 5ml, stir for 2-3min, slowly add about 2ml of deionized water, stop stirring.

[0034] 4. After airtight aging at room temperature for 40 hours, the vacuum pump is used for suction filtration, and the filtrate is washed several times with absolute ethanol and deionized water.

[0035] 5. Put the filtered sample into a constant temperature blast drying oven, adjust the temperature to 110°C, and dry for 2 hours.

[0036] 6. Put the dried sample into a muffle furnace and bake it at 200°C for 4h.

[0037] 7....

Embodiment 3

[0039] 1. Measure 10ml of titanium tetrachloride solution in a beaker filled with 45ml of absolute ethanol to make a titanium tetrachloride / absolute ethanol solution, and stir vigorously at a constant speed.

[0040] 2. Weigh 10 g of 13X molecular sieve with a particle size of 80 mesh, add it to a beaker containing a titanium tetrachloride solution, and stir vigorously at a constant speed for 3 hours.

[0041] 3. Then add dilute HNO dropwise into the beaker 3 Solution 10ml, stir for 2-3min, slowly add about 5ml of deionized water, stop stirring.

[0042] 4. After airtight aging at room temperature for 48 hours, the vacuum pump is used for suction filtration, and the filtrate is washed several times with absolute ethanol and deionized water.

[0043] 5. Put the filtered sample into a constant temperature blast drying oven, adjust the temperature to 110°C, and dry for 3 hours.

[0044] 6. Put the dried sample into a muffle furnace and bake it at 200°C for 4h.

[0045] 7. Get ...

technical field

[0001] The present invention relates to a kind of preparation method of molecular sieve composite material, more specifically relate to a kind of TiO used for dye wastewater treatment 2 / 13X molecular sieve composite material preparation method. Background technique

[0002] The world's annual output of dyes is about 700,000 tons, of which about 10-15% is discharged into the environment in the form of wastewater. Dye wastewater is characterized by high chroma, high toxicity, COD Cr (chemical oxygen demand) high, low biodegradability (BOD 5 / COD<0.1), most dyes are resistant to photolysis, oxidation, and biodegradation, and are persistent organic pollutants. These dye wastewater often cause serious water pollution and become a difficult point in environmental restoration. At present, the treatment of dye wastewater commonly used at home and abroad is generally non-destructive technology, such as physical adsorption method, coagulation method, air flotat...

Examples

Embodiment 1

[0023] 1. Measure 8ml of titanium tetrachloride solution in a beaker filled with 40ml of absolute ethanol to make a titanium tetrachloride / absolute ethanol solution, and stir vigorously at a constant speed.

[0024] 2. Weigh 10g of 13X molecular sieve with a particle size of 100 mesh, add it into a beaker filled with titanium tetrachloride solution, and stir vigorously at a constant speed for 3 hours.

[0025] 3. Then add dilute HNO dropwise into the beaker 3 Solution 10ml, stir for 2-3min, slowly add about 3ml of deionized water, stop stirring.

[0026] 4. After airtight aging at room temperature for 48 hours, the vacuum pump is used for suction filtration, and the filtrate is washed several times with absolute ethanol and deionized water.

[0027] 5. Put the filtered sample into a constant temperature blast drying oven, adjust the temperature to 110°C, and dry for 3 hours.

[0028] 6. Put the dried sample into a muffle furnace and bake it at 200°C for 4h.

[0029] 7. Get Ti...

Embodiment 2

[0031] 1. Measure 6ml of titanium tetrachloride solution in a beaker filled with 35ml of absolute ethanol to make a titanium tetrachloride / absolute ethanol solution, and stir vigorously at a constant speed.

[0032] 2. Weigh 10g of 13X molecular sieve with a particle size of about 100 mesh, add it into a beaker filled with titanium tetrachloride solution, and stir vigorously at a constant speed for 2 hours.

[0033] 3. Then add dilute HNO dropwise into the beaker 3 Solution 5ml, stir for 2-3min, slowly add about 2ml of deionized water, stop stirring.

[0034] 4. After airtight aging at room temperature for 40 hours, the vacuum pump is used for suction filtration, and the filtrate is washed several times with absolute ethanol and deionized water.

[0035] 5. Put the filtered sample into a constant temperature blast drying oven, adjust the temperature to 110°C, and dry for 2 hours.

[0036] 6. Put the dried sample into a muffle furnace and bake it at 200°C for 4h.

[0037] 7....

Embodiment 3

[0039] 1. Measure 10ml of titanium tetrachloride solution in a beaker filled with 45ml of absolute ethanol to make a titanium tetrachloride / absolute ethanol solution, and stir vigorously at a constant speed.

[0040] 2. Weigh 10 g of 13X molecular sieve with a particle size of 80 mesh, add it to a beaker containing a titanium tetrachloride solution, and stir vigorously at a constant speed for 3 hours.

[0041] 3. Then add dilute HNO dropwise into the beaker 3 Solution 10ml, stir for 2-3min, slowly add about 5ml of deionized water, stop stirring.

[0042] 4. After airtight aging at room temperature for 48 hours, the vacuum pump is used for suction filtration, and the filtrate is washed several times with absolute ethanol and deionized water.

[0043] 5. Put the filtered sample into a constant temperature blast drying oven, adjust the temperature to 110°C, and dry for 3 hours.

[0044] 6. Put the dried sample into a muffle furnace and bake it at 200°C for 4h.

[0045] 7. Get ...

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