Preparation method for bamboo pulp cellulose-based integrated Fenton catalyst Fe<3+>C2O4/R

An integrated Fenton and cellulose-based technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve high oxidation cost, low degradation efficiency, Fenton To solve the problems such as the difficulty of recycling the reagents, to expand the range of raw materials and increase economic income

Inactive Publication Date: 2015-05-27
ZHEJIANG SCI-TECH UNIV
9 Cites 17 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0005] In order to overcome the traditional Fenton oxidation process of industrial wastewater treatment, the Fenton reagent is difficult to recycle and cause secondary pollution, high oxidation cost, low degradation efficiency and other problems, and at the same time ...
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Method used

[0028] Determination of the water absorption rate and ferric iron loading rate of the cellulose-based porous resin R prepared in Examples 1, 2, and 3. Table 1 shows the water absorption capacity of the cellulose-based porous resin R prepared in Examples 1, 2, and 3, and the measurement results of the loading ra...
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Abstract

The invention discloses a preparation method for a bamboo pulp cellulose-based integrated Fenton catalyst Fe<3+>C2O4/R. The preparation method is characterized in that tri-valent iron and oxalic acid are subjected to coordination to form a complex Fe<3+>C2O4, and the complex Fe<3+>C2O4 is loaded on bamboo pulp cellulose-based porous resin R synthesized by bamboo pulp to form the integrated Fenton catalyst Fe<3+>C2O4/R; under visible light, hydrogen peroxide can be catalyzed in an acceleration manner to degrade dye type organic pollutants in printing and dyeing wastewater. A product prepared by the method is high in efficiency, environment-friendly and low in cost; the problems of secondary pollution, high oxidization cost, low degrading efficiency and the like which are caused by a fact that the Fenton reagent cannot be repeatedly used in the conventional dye type organic pollutant Fenton oxidization degrading are solved, and the creation concept of using bamboo resources in China in a high value is provided, and thus the preparation method has obvious environmental and social significance.

Application Domain

Technology Topic

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  • Preparation method for bamboo pulp cellulose-based integrated Fenton catalyst Fe&lt;3+&gt;C2O4/R
  • Preparation method for bamboo pulp cellulose-based integrated Fenton catalyst Fe&lt;3+&gt;C2O4/R
  • Preparation method for bamboo pulp cellulose-based integrated Fenton catalyst Fe&lt;3+&gt;C2O4/R

Examples

  • Experimental program(3)

Example Embodiment

[0016] Example 1:
[0017] 1) The light bamboo pulp board is pulverized by a plant grinder, filtered through a 100-mesh screen to obtain bamboo pulp powder with a particle size of 0.15 mm or less, added with an alkaline solution pre-frozen to -10 ℃, stirred vigorously for 4 min, and left to react 120 min, the alkaline solution is a mixed solution of sodium hydroxide and urea. The mass percentages of sodium hydroxide, urea and deionized water are 6 wt%, 11 wt% and 83 wt%, respectively. The bamboo pulp powder and the mixed solution are 2 g : 70 mL for mixing and reaction, then take it out and stir in an ice bath to obtain a uniform transparent bamboo pulp cellulose solution;
[0018] 2) Under the action of mechanical stirring, heat the bamboo pulp cellulose solution obtained in step 1) to 70℃ in a water bath, bubbling with nitrogen for 20 minutes, adding 0.1 g/g bamboo pulp powder of ammonium persulfate for 20 minutes, adding 0.5 in sequence g/g bamboo pulp powder of acrylamide, 2.0 g/g bamboo pulp powder of acrylic acid and 15 mg/g bamboo pulp powder of N-N'-methylenebisacrylamide neutralized by sodium hydroxide, continue to pass nitrogen After reacting for 1 h, the product was washed with deionized water to neutrality, dehydrated with absolute ethanol for 12 h, and freeze-dried to obtain bamboo pulp cellulose-based porous resin R;
[0019] 3) Add 0.1 mol/L Na 2 C 2 O 4 And Fe(NO 3 ) 3 Take 10 mL of each solution and mix and react for 20 minutes, add 40 mg of the bamboo pulp cellulose-based porous resin R obtained in step 2) to the above mixed solution, and shake and react for 24 hours under the conditions of a constant temperature water bath shaker at 40°C and 100 r/min. The product is washed with deionized water to neutrality and dried in vacuum to obtain integrated Fenton catalyst Fe 3+ C 2 O 4 /R product (a).

Example Embodiment

[0020] Example 2:
[0021] 1) The purple bamboo pulp board is pulverized by a plant grinder, filtered through a 100-mesh screen to obtain bamboo pulp powder with a particle size of 0.15 mm or less, add an alkaline solution pre-frozen to -15 ℃ and stir vigorously for 3 min, and let it stand for 90 min, where the alkaline solution is a mixed solution of sodium hydroxide and urea. The mass percentages of sodium hydroxide, urea and deionized water are 5 wt%, 10 wt% and 85 wt%, respectively. The bamboo pulp powder and the mixed solution are 2 g : 60 mL is mixed and reacted, then taken out and placed in an ice bath and stirred to obtain a uniform transparent bamboo pulp cellulose solution;
[0022] 2) Under mechanical stirring, heat the bamboo pulp cellulose solution obtained in step 1) to 60℃ in a water bath, bubbling with nitrogen for 30 minutes, adding 0.15 g/g bamboo pulp powder of ammonium persulfate for 15 minutes, adding 0.75 in sequence g/g bamboo pulp powder of acrylamide, 3.0 g/g bamboo pulp powder of acrylic acid, and 20 mg/g bamboo pulp powder of N-N'-methylenebisacrylamide neutralized by sodium hydroxide, continue to pass nitrogen After reacting for 2 h, the product was washed with deionized water to neutrality, dehydrated with absolute ethanol for 18 h, and freeze-dried to obtain bamboo pulp cellulose-based porous resin R;
[0023] 3) Add 0.15 mol/L Na 2 C 2 O 4 And Fe(NO 3 ) 3 Take 10 mL of each solution and mix and react for 30 min. Add 50 mg of the bamboo pulp cellulose-based porous resin R obtained in step 2) to the above mixed solution, and shake and react for 24 h at a constant temperature water bath shaker at 30°C and 110 r/min. The product is washed with deionized water to neutrality and dried in vacuum to obtain integrated Fenton catalyst Fe 3+ C 2 O 4 /R product (b).

Example Embodiment

[0024] Example 3:
[0025] 1) The purple bamboo pulp board is pulverized by a plant grinder, filtered through a 100-mesh screen to obtain bamboo pulp powder with a particle size of 0.15 mm or less, add an alkaline solution pre-frozen to -25°C, stir vigorously for 2 minutes, and let stand for 60 minutes min, where the alkaline solution is a mixed solution of sodium hydroxide and urea. The mass percentages of sodium hydroxide, urea and deionized water are 4 wt%, 9 wt% and 87 wt%, respectively. The bamboo pulp powder and the mixed solution are 2 g : Mix and react with 50 mL, then take it out and stir in an ice bath to obtain a uniform transparent bamboo pulp cellulose solution;
[0026] 2) Under the action of mechanical stirring, heat the bamboo pulp cellulose solution obtained in step 1) to 50℃ in a water bath, bubbling in nitrogen for 40 minutes, adding 0.2 g/g bamboo pulp powder of ammonium persulfate for 10 minutes, adding 1.0 in sequence g/g bamboo pulp powder of acrylamide, 4.0 g/g bamboo pulp powder of acrylic acid, and 25 mg/g bamboo pulp powder of N-N'-methylenebisacrylamide neutralized by sodium hydroxide, continue to pass nitrogen After 3 hours of reaction, the product was washed with deionized water to neutrality, dehydrated by adding absolute ethanol for 24 hours, and freeze-dried to obtain bamboo pulp cellulose-based porous resin R;
[0027] 3) Add 0.2 mol/L Na 2 C 2 O 4 And Fe(NO 3 ) 3 Take 10 mL of each solution and mix and react for 40 min. Add 60 mg of the bamboo pulp cellulose-based porous resin R obtained in step 2) to the above mixed solution, and shake and react for 24 h at a constant temperature water bath shaker at 20°C and 120 r/min. The product is washed with deionized water to neutrality and dried in vacuum to obtain integrated Fenton catalyst Fe 3+ C 2 O 4 /R product (c).
[0028] The water absorption rate and ferric iron loading rate of the cellulose-based porous resin R prepared in Examples 1, 2, and 3 were measured. Table 1 shows the measurement results of the water absorption rate of the cellulose-based porous resin R and the trivalent iron loading rate on the cellulose-based porous resin R prepared in Examples 1, 2, and 3. It can be seen from the data in Table 1 that the bamboo pulp cellulose-based integrated Fenton catalyst Fe 3+ C 2 O 4 /R integrated Fenton catalyst Fe 3+ C 2 O 4 /R has a high ferric iron loading rate.
[0029] As shown in Figure 1, the integrated Fenton catalyst Fe prepared from Example 1 3+ C 2 O 4 The field emission scanning electron microscope photos of the /R product can be seen, Figure 1a It shows that the morphology of the cellulose-based porous resin is loose and porous, which is conducive to the large load of ferric ions in the later period. Figure 1b Show the prepared integrated Fenton catalyst Fe 3+ C 2 O 4 /R has suitable individual size and specific surface area, suitable for efficient photo-assisted Fenton catalytic oxidation reaction.
[0030] Table 1
[0031]
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