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Preparation method of amino-terminated hyperbranched polymer grafted chitosan microsphere heavy metal ion adsorbent

An amino-terminated hyperbranched, chitosan microsphere technology, applied in the directions of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve the problem of increasing the preparation cost of adsorbents, affecting the adsorption capacity of heavy metals, It does not achieve the adsorption effect and other problems, and achieves the effect of excellent heavy metal ion adsorption performance, good biocompatibility and non-toxicity, good non-toxic effect

Active Publication Date: 2017-06-30
OCEAN UNIV OF CHINA +1
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AI Technical Summary

Problems solved by technology

The study found that, whether it is chitosan powder or chitosan particles, when heavy metal ions are adsorbed in acidic medium, the –NH in the molecule will 2 is protonated to form –NH 3 + Dissolving in water causes the loss of the adsorbent, which limits its application range
Adding a cross-linking agent can enhance the mechanical strength of chitosan and its stability in acidic medium, but the cross-linking agent will affect its adsorption capacity for heavy metals by occupying the functional groups of chitosan
In order to overcome the above defects, many studies have focused on grafting chitosan with functional groups and then crosslinking, which has increased the stability and adsorption performance of the product to a certain extent, but there are still certain defects: (1) Part of the grafted functional groups still participated in the cross-linking; (2) only part of the functional groups were exposed on the surface of the microspheres to play an adsorption role, and most of the functional groups were embedded in the interior of the microspheres; (3) when increasing While reducing the cost of adsorbent preparation, the ideal adsorption effect was not achieved

Method used

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preparation example Construction

[0013] A method for preparing an amino-terminated hyperbranched polymer grafted chitosan microsphere heavy metal ion adsorbent, which is characterized in that it comprises the following steps: 5 Da, chitosan with a deacetylation degree of 75%~97% is dissolved in 1%~2% (v / v) acetic acid or lactic acid aqueous solution to obtain a concentration of 1%~3% (w / v) chitosan Chitosan solution, the unit is g / mL; the chitosan solution is spray-dried at an inlet temperature of 160-220°C and an outlet temperature of 80-100°C to prepare chitosan microspheres; (2) With methanol as the medium, in N 2 Under the conditions of protection, constant temperature of 40-60°C, and stirring speed of 400-1000 rpm, the Michael addition reaction between chitosan microspheres and methyl acrylate occurred, and the reaction time was 36-60 h. The microspheres were collected and washed with absolute ethanol for 3 ~6 times, drying in an oven at 30~70°C to obtain the intermediate product methyl acrylate grafte...

Embodiment 2

[0019] The viscosity average molecular weight is 6×10 5 Da, 10 g of chitosan with a deacetylation degree of 85%, was dissolved in 500 mL of 2% (v / v) acetic acid aqueous solution to obtain a 2% (w / v) chitosan solution; The chitosan solution was spray-dried under the condition that the inlet temperature was 180° C. and the outlet temperature was 90° C., and chitosan microspheres were collected. Take 6 g of chitosan microspheres and add them to 100 mL of methanol, 2 Under the conditions of protection, constant temperature at 60°C, and stirring speed of 1000 rpm, 18 mL of methyl acrylate was added, reacted for 40 h, collected microspheres, washed with absolute ethanol three times, and dried in an oven at 70°C to obtain the intermediate product methyl acrylate. branched chitosan microspheres. Take 3 g of methyl acrylate grafted chitosan microspheres into 100 mL of methanol, 2 protection, at a constant temperature of 60°C and a stirring speed of 1000 rpm, 30 mL of diethylenetria...

Embodiment 3

[0021] The viscosity average molecular weight is 5×10 5 Da, 20 g of chitosan with a deacetylation degree of 93%, was dissolved in 1000 mL of lactic acid aqueous solution with a concentration of 2% (v / v) to obtain a chitosan solution with a concentration of 2% (w / v); The chitosan solution was spray-dried under the condition that the inlet temperature was 210° C. and the outlet temperature was 100° C., and chitosan microspheres were collected. Take 10 g of chitosan microspheres and add them to 1000 mL of methanol, 2 Under the conditions of protection, constant temperature at 60°C, and stirring speed of 1000 rpm, 60 mL of methyl acrylate was added, reacted for 60 h, collected microspheres, washed with absolute ethanol three times, and dried in an oven at 60°C to obtain the intermediate product methyl acrylate. branched chitosan microspheres. Take 5 g of methyl acrylate grafted chitosan microspheres into 500 mL of methanol, 2 protection, at a constant temperature of 60 °C and a ...

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Abstract

The invention discloses a preparation method of an amino-terminated hyperbranched polymer grafted chitosan microsphere heavy metal ion adsorbent, and belongs to the field of water environment protection. The preparation method comprises the steps: firstly, preparing chitosan microspheres by a spray drying method; then grafting the surface of the chitosan microspheres with methacrylate through Michael addition to prepare methacrylate-grafted chitosan microspheres; and finally, grafting the surface of the methacrylate-grafted chitosan microspheres with diethylenetriamine by a substitution reaction, separating, washing and drying to obtain the heavy metal ion adsorbent. The amino-terminated hyperbranched polymer grafting method, the surface of the adsorbent is grafted with a large number of amide and amino functional groups, at the same time, the strategy of firstly preparing the microspheres and then grafting with the functional groups makes the functional groups exposed on the adsorbent surface to the greatest extent, and the adsorption effect of the heavy metal ion adsorbent is enhanced.

Description

technical field [0001] The invention belongs to the field of water environment protection, and relates to a preparation method of an amino-terminated hyperbranched polymer grafted chitosan microsphere heavy metal ion adsorbent. Background technique [0002] Because heavy metal ions are highly toxic, non-degradable, and enriched in organisms, they accumulate continuously after entering the natural environment, and are further transferred to the human body through the food chain, causing serious harm to the natural environment and human health. Therefore, it is an urgent task to develop environmentally safe and efficient methods for the treatment of heavy metal ions. [0003] Chitosan is the second largest natural polysaccharide in nature after cellulose. It is obtained by deacetylation of chitin. It is widely distributed and cheap. Chitosan has the advantages of good biocompatibility, biodegradability, and non-toxicity. In addition, chitosan molecules contain a large number...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F8/32C08F251/00C08F220/14B01J20/26B01J20/28B01J20/30
CPCB01J20/24B01J20/265B01J20/28004B01J20/28019C08F8/32C08F251/00C08F220/14
Inventor 刘成圣党奇峰张海峰刘恺高辉
Owner OCEAN UNIV OF CHINA
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