CN108585101A Recovery method of porous biomass microsphere hybridized with inorganic materials

and used for heavy metal sewage treatment

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1.A method for recovering porous biomass microspheres hybridized with inorganic materials for Cu2+ heavy
metal sewage treatment, characterized in that porous inorganic microspheres hybridized with inorganic materials
are collected by filtration and placed in a 2 mol/L hydrochloric acid aqueous solution at 50 Ultrasonic 2 ° was
carried out at ° C, the desorption rate of Cu2+ heavy metal ions was measured, and the desorbed adsorbent was
vacuum dried at 50 ° C to a constant weight to obtain the recovered inorganic material hybrid porous
microspheres;

The recovered inorganic material hybrid porous biomass microspheres can be used for adsorbing Cu2+
wastewater in a pH environment of 7.0;

The inorganic material hybrid porous microspheres are prepared by the following preparation methods:

1） Modification of sorghum terrier:

a) pulverization process: sorghum stalks are dried and pulverized to a sorghum stalk biomass particle having a
particle size of 200 mesh or less;

b) acid-base treatment process: 100g of sorghum stem biomass particles were placed in 200ml 3wt% phosphoric
acid aqueous solution and stirred for 30min, then immersed in 200ml 5wt% potassium hydroxide aqueous
solution at 50 ° C for 10min, filtered, washed with tap water until The filtrate is made into a neutral acid-base
modified biomass particle;

c) oxidation process: the acid-base modified biomass particles are placed in a concentration of 5 wt% potassium
permanganate aqueous solution at 10-20 ° C for 1-2 h to obtain an oxidized biomass dispersion; potassium
permanganate The dosage is 0.10 times the weight of the sorghum stem biomass particles;

d) grafting reaction: then adding N-(tert-butoxycarbonyl)aminoacetic acid and concentrated sulfuric acid for
reaction at 40 ° C for 2 h, then at 70 ° C for 2 h; filtering, washing with water until the filtrate is neutral, drying
to obtain aminoglycol Branched biomass; N-(tert-butoxycarbonyl)glycine in the grafting reaction is used in an
amount of 0.26 times the weight of the sorghum biomass particles;

2） Preparation of composite modified hectorite:

（1）Quaternization of hectorite: 100 g of hectorite having a particle size of 200 mesh or less is placed in an
aqueous solution of octadecyldimethylbenzylammonium chloride for 48 h to obtain a quaternized saltex
dispersion. 0.15 g of octadecyldimethylbenzylammonium chloride per gram of hectorite;

（2）Complexation of hectorite: Add ethylenediamine to the hectorite dispersion, 0.08 g of ethylenediamine

per gram of hectorite is used for complexation, stir at 40 ° C for 12 h, then filter to filtrate and detect chlorine
free with silver nitrate Ion, dried at 70 ° C to obtain composite modified hectorite;

（3）Preparation of porous biomass microspheres hybridized with inorganic materials:

The biomass grafted with 10 g of the composite modified hectorite and 8 g of glycine was uniformly stirred in
an aqueous solution of 100 ml of ethanol, 0.1 g of triethylamine was added, and then 0.4 g of a crosslinking
agent glutaraldehyde was added thereto for reflux for 2 hours, followed by filtration. It is washed with water and
dried at 65 ° C to a constant weight to obtain porous microspheres in which the inorganic material is hybridized.

2.A method for recovering porous biomass microspheres hybridized with inorganic materials for Ni2+ heavy
metal sewage treatment, characterized in that porous inorganic microspheres hybridized with inorganic materials
are collected by filtration and placed in a 2 mol/L hydrochloric acid aqueous solution at 50 Ultrasonic 2 h was
measured at ° C, the desorption rate of Ni2+ heavy metal ions was measured, and the desorbed adsorbent was
vacuum dried at 50 ° C to a constant weight to obtain the recovered inorganic material hybrid porous
microspheres;

The recovered inorganic material hybrid porous biomass microspheres can be used for adsorbing Ni2+
wastewater in a pH of 4.5;

The inorganic material hybrid porous microspheres are prepared by the following preparation methods:

1） Modification of sorghum terrier:

a) pulverization process: sorghum stalks are dried and pulverized to a sorghum stalk biomass particle having a
particle size of 200 mesh or less;

b) acid-base treatment process: 100g of sorghum stem biomass particles were placed in 200ml 3wt% phosphoric
acid aqueous solution and stirred for 30min, then immersed in 200ml 5wt% potassium hydroxide aqueous
solution at 50 ° C for 10min, filtered, washed with tap water until The filtrate is made into a neutral acid-base
modified biomass particle;

c) oxidation process: the acid-base modified biomass particles are placed in a concentration of 5 wt% potassium
permanganate aqueous solution at 10-20 ° C for 1-2 h to obtain an oxidized biomass dispersion; potassium
permanganate The dosage is 0.10 times the weight of the sorghum stem biomass particles;

d) grafting reaction: then adding N-(tert-butoxycarbonyl)aminoacetic acid and concentrated sulfuric acid for
reaction at 40 ° C for 2 h, then at 70 ° C for 2 h; filtering, washing with water until the filtrate is neutral, drying
to obtain aminoglycol Branched biomass; N-(tert-butoxycarbonyl)glycine in the grafting reaction is used in an
amount of 0.26 times the weight of the sorghum biomass particles;

2） Preparation of composite modified hectorite:

（1）Quaternization of hectorite: 100 g of hectorite having a particle size of 200 mesh or less is placed in an
aqueous solution of octadecyldimethylbenzylammonium chloride for 48 h to obtain a quaternized saltex
dispersion. 0.15 g of octadecyldimethylbenzylammonium chloride per gram of hectorite;

（2）Complexation of hectorite: Add ethylenediamine to the hectorite dispersion, 0.08 g of ethylenediamine

per gram of hectorite is used for complexation, stir at 40 ° C for 12 h, then filter to filtrate and detect chlorine
free with silver nitrate Ion, dried at 70 ° C to obtain composite modified hectorite;

（3）Preparation of porous biomass microspheres hybridized with inorganic materials:

The biomass grafted with 10 g of the composite modified hectorite and 8 g of glycine was uniformly stirred in
an aqueous solution of 100 ml of ethanol, 0.1 g of triethylamine was added, and then 0.4 g of a crosslinking
agent glutaraldehyde was added thereto for reflux for 2 hours, followed by filtration. It is washed with water and
dried at 65 ° C to a constant weight to obtain porous microspheres in which the inorganic material is hybridized.