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Preparation method of cellulose adsorbent for adsorbing heavy metal cations

A technology for adsorbing heavy metals and cellulose, applied in chemical instruments and methods, adsorption water/sewage treatment, water/sludge/sewage treatment, etc., to achieve the effects of wide sources, mild catalytic reaction conditions and low cost

Inactive Publication Date: 2013-04-03
MINNAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention aims at the problems existing in the current cellulose amination modification route and provides a preparation method of cellulose adsorbent for heavy metal cation adsorption

Method used

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  • Preparation method of cellulose adsorbent for adsorbing heavy metal cations
  • Preparation method of cellulose adsorbent for adsorbing heavy metal cations
  • Preparation method of cellulose adsorbent for adsorbing heavy metal cations

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preparation example Construction

[0026] The present invention discloses a method for preparing a cellulose adsorbent for adsorbing heavy metal cations. The cellulose is a natural renewable and environmentally compatible cellulose. The specific preparation steps include:

[0027] Step 1. After crushing the cellulose to a particle size of less than 80 mesh, soak it in 15% sodium hydroxide solution at 60°C for 2 hours; the cellulose is microcrystalline cellulose, quantitative filter paper or cellulose ester; the hydroxide The dosage of sodium solution is 20~50 times of the mass of cellulose.

[0028] Step 2, adding dimethyl sulfoxide, using azeotropic distillation to remove excess water to obtain cellulose sol; wherein the mass of dimethyl sulfoxide added is 5 to 20 times the mass of cellulose; and azeotropic The entrainer for rectification is isobutanol, and the mass of the entrainer is 5 to 10 times that of dimethyl sulfoxide.

[0029] Step 3. In the presence of nitrogen medium, react the sol with diimidazole...

Embodiment 1

[0040] (1) Weigh 2g of quantitative filter paper, break it to a particle size of 80-100 mesh, put it in a 250mL three-neck flask, add 40g of sodium hydroxide solution with a mass percentage of 15%, stir and swell at 60°C for 2 hours to obtain a fiber slurry 24g.

[0041] (2) Weigh 10 g of dimethyl sulfoxide and 80 g of isobutanol in a flask, stir evenly, heat and distill, and remove the water at a distillation temperature of 89.5°C to obtain cellulose sol.

[0042] (3) Infuse high-purity nitrogen gas into the three-neck flask, weigh 150 mg of 1,1'-oxalyldiimidazole and add it to the flask. After activation at 50°C for 2 hours, add 10 mL of isobutanol, stir and filter immediately, and add to the filtrate 60mg of ethylenediamine was added to it, and the reaction was carried out at 60°C for 2h.

[0043] (4) The product was reflux washed with toluene for 12 hours, filtered, and the filter cake was vacuum-dried at 50°C for 12 hours to obtain the cellulose adsorbent. The obtained ...

Embodiment 2

[0045] (1) Weigh 2g of microcrystalline cellulose, crush it to a particle size of 200 mesh, put it in a 250mL three-necked flask, add 50g of sodium hydroxide solution with a mass percentage of 18%, stir and swell at 60°C for 2h to obtain a fiber slurry 32g.

[0046] (2) Weigh 20 g of dimethyl sulfoxide and 110 g of isobutanol in a flask, stir evenly, heat and distill, and remove the water at a distillation temperature of 89.5°C to obtain cellulose sol.

[0047] (3) Infuse high-purity nitrogen gas into the three-necked flask, weigh 100 mg of 1,1'-carbonyldiimidazole and add it to the flask. After activation at 50°C for 2 hours, add 10 mL of isobutanol, stir and filter immediately, and add 120 mg of melamine was reacted at 60°C for 2h.

[0048] (4) The product was reflux washed with toluene for 12 hours, filtered, and the filter cake was vacuum-dried at 50°C for 12 hours to obtain the cellulose adsorbent. The obtained product is to Cr 3+ The adsorption capacity is 57.7 mg·g ...

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Abstract

The invention discloses a preparation method of a cellulose adsorbent for adsorbing heavy metal cations. The preparation method comprises the following steps: 1) crushing cellulose till the grain diameter is smaller than 80 meshes, putting the cellulose into 15-30% of sodium hydroxide solution, and soaking for 2 hours at 60 DEG C; 2) adding dimethyl sulfoxide, and removing excessive water through azeotropic distillation to obtain a cellulose sol; 3) in the presence of a nitrogen medium, reacting the sol with a diimidazole catalyst and dihydric or polyhydric amine sequentially; and 4) reflowing a reaction product with methylbenzene for 12 hours, filtering, and performing vacuum drying for 12 hours at 50 DEG C to obtain the cellulose adsorbent. The preparation method has the characteristics of mild catalytic reaction conditions, low cost and the like; and the prepared adsorbent is good in effect of adsorbing the heavy metal cations, wide in application range and recyclable.

Description

technical field [0001] The invention relates to a preparation method of a heavy metal cation adsorption material, in particular to a preparation method of a cellulose adsorbent applied to heavy metal cation adsorption. Background technique [0002] With the rapid development of society and economy, human's demand for water resources has increased sharply. At the same time, the waste water produced by human industry, agriculture and life is discharged directly without treatment, resulting in serious pollution of water bodies and directly affecting the safety of human drinking water. , and the heavy metal pollutants in these water bodies enter the human body through drinking water and accumulate in the body, causing the body's metabolic pathways to be blocked and endangering human health. Therefore, corresponding measures must be taken to effectively deal with these heavy metal pollutants. Advanced treatment and reuse of heavy metal wastewater can not only reduce the dischar...

Claims

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Application Information

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IPC IPC(8): B01J20/24B01J20/30C02F1/28C02F1/62
Inventor 吴文炳王艳
Owner MINNAN NORMAL UNIV
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