Silica gel loaded polyamine and carboxyl bifunctional group composite adsorbing material and preparation method thereof

A composite adsorption material and composite material technology, which are applied in the field of heavy metal adsorption materials, can solve the problems that the polymer chain of polyamine cannot be fully expanded in solution, reduce the bonding amount of polyamine, and cannot diffuse uniformly, so as to overcome steric hindrance. effect, improve adsorption performance, improve adsorption capacity

Active Publication Date: 2012-09-26
陕西水木云旗实业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Furthermore, if the organic modification is not infiltrated with a solvent in advance, adding the mixed solution of the coupling agent to the humidified silica gel will lead to insufficient solvent in the initial stage of the reaction, so that the coupling agent cannot be uniformly diffused after adding, resulting in a rapid reaction of the coupling agent. Hydrolysis, reaction with the surrounding silica gel, blocking the pore size, the coupling agent overlaps on the silica gel surface, and the bond is not strong
Fourth, the bonded polymeric amine is not infiltrated with an organic solvent and stirred at low temperature in advance, but the mixture of the polymeric amine and deionized water is directly added to the modified silica gel. Since the modified silica gel and deionized water cannot be infiltrated in this step, the , the modified silica gel is coated with polymeric amine, and the intertwining of polymer chains increases the steric hindrance and reduces the bonding amount of polymeric amine
Fifth, the polymeric amine / silica gel composite material is directly mixed with chloroacetate, and the polymeric amine / silica gel composite material is not swollen, so that the polymeric amine polymer chain cannot be fully expanded in the solution, which is not conducive to the introduction of carboxyl groups

Method used

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  • Silica gel loaded polyamine and carboxyl bifunctional group composite adsorbing material and preparation method thereof
  • Silica gel loaded polyamine and carboxyl bifunctional group composite adsorbing material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Pre-humidify the spherical macroporous silica gel until the silica gel is slightly translucent. Among them, the index of the above-mentioned spherical macroporous silica gel is spherical, the particle size is 300um~850um, and the specific surface area is 300m 2 / g~350m 2 / g, aperture The pore volume is 0.8mL / g~1.2mL / g, and the bulk density is 0.4g / mL~0.45g / mL. Humidification is done by electromagnetically atomized water vapor. Put the humidified silica gel into a three-necked flask, and add 1.2mol / L hydrochloric acid twice the mass of silica gel. Start stirring, control the stirring speed to 30r / min, heat in an oil bath, raise the temperature to 90°C, condense and reflux, absorb tail gas, react for 3h, naturally cool down to below 40°C after the reaction, filter, and collect the mother liquor for recycling. Then, the silica gel was washed with deionized water until it was neutral, and dried, and the silica gel was transferred to a drying oven at 80° C. and dried to ...

Embodiment 2

[0059] Pre-humidify the spherical macroporous silica gel until the silica gel is slightly translucent. Among them, the index of the above-mentioned spherical macroporous silica gel is spherical, the particle size is 180um~300um, and the specific surface area is 350m 2 / g~450m 2 / g, aperture The pore volume is 1.2mL / g~1.5mL / g, and the bulk density is 0.45g / mL~0.5g / mL. Humidification can be done with steam. Put the humidified silica gel into a three-necked flask, and add 2 mol / L sulfuric acid which is 6 times the mass of silica gel. Start stirring, control the stirring speed to 120r / min, heat in an oil bath, raise the temperature to 120°C, condense and reflux, absorb tail gas, and react for 8h. After the reaction, naturally cool down to below 40°C, filter, and collect the mother liquor for recycling. Then, the silica gel was washed with deionized water until it was neutral, and dried, and the silica gel was transferred to a drying oven at 140° C. and dried to a constant wei...

Embodiment 3

[0061] Pre-humidify the spherical macroporous silica gel until the silica gel is slightly translucent. Among them, the index of the above-mentioned spherical macroporous silica gel is spherical, with a particle size of 120um~180um and a specific surface area of ​​450m 2 / g~500m 2 / g, aperture The pore volume is 1.5mL / g~2mL / g, and the bulk density is 0.5g / mL~0.6g / mL. Humidification Humidification through water mist. Add the humidified silica gel into a three-necked flask, and add 1.4 mol / L benzenesulfonic acid that is three times the mass of silica gel. Start stirring, control the stirring speed to 60r / min, heat in an oil bath, raise the temperature to 100°C, condense and reflux, absorb tail gas, react for 5h, naturally cool down to below 40°C after the reaction, filter, and collect the mother liquor for recycling. Then, the silica gel was washed with deionized water until it was neutral, and dried, and the silica gel was transferred to a drying oven at 110° C. to dry to co...

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Abstract

The invention discloses a silica gel loaded polyamine and carboxyl bifunctional group composite adsorbing material. The bifunctional group composite adsorbing material comprises the following components in percentage by mass: 60.2-86.2% of silica gel, 6.1-24.0% of coupling agent, 1.7-14.5% of polyamine, and 1.7-14.5% of carboxyl, wherein the total mass of all the components is 100%. The invention further comprises a preparation method of the adsorbing material. The method comprises the step as follows: the porous silica gel is taken as a nonpolar rigid skeleton, activated, humidified, modified with the coupling agent, bonded with high molecular polyamine, and is grafted with carboxyl to obtain the bifunctional radical composite adsorbing material. The prepared adsorbing material has an excellent adsorptive property to heavy metal ions and can be used repeatedly after being regenerated; and the adsorbing material has a simple preparation technology, is easy to realize industrialization, is free from toxic solvent, is extensive in sources of raw material, can be applied to adsorption, separation and enrichment of heavy metal in water body, and realizes harmless treatment of waste water polluted by heavy metal.

Description

technical field [0001] The invention belongs to the technical field of heavy metal adsorption materials, and relates to a silica gel-loaded polymeric amine and carboxyl bifunctional group composite adsorption material. The invention also relates to a preparation method of the composite adsorption material, which is applied to the treatment of heavy metal pollution and wastewater. Background technique [0002] While the progress of society and the improvement of productivity have accelerated the development of industrialization, it has also led to a sharp increase in industrial pollutant discharge, and a large amount of heavy metal pollutants have been discharged into the environment, causing serious harm to the ecological environment. Heavy metal ions can accumulate in the soil and cannot be degraded by microorganisms. No matter what method is used, they can only transfer the location of heavy metal ions or change their physical and chemical forms, but cannot decompose and de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/30C02F1/28C02F1/62
Inventor 陈博烟小亿陈雷
Owner 陕西水木云旗实业有限公司
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