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A kind of cross-linked chitosan microsphere and its preparation method and application

A technology for cross-linking chitosan and chitosan, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of difficult removal of dye pollutants, narrow pH value range, poor mechanical properties, etc. Stability, low equipment requirements, good adsorption performance

Active Publication Date: 2019-03-29
ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in practical applications, chitosan, as a dye adsorbent, still has shortcomings such as easy swelling, soluble in dilute acid, poor mechanical properties, weak bridging ability, and narrow applicable pH range, making it difficult to be directly used as a dye adsorbent. Applied to the removal of dye pollutants in wastewater, chitosan generally needs to be physically or chemically modified to overcome its shortcomings

Method used

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  • A kind of cross-linked chitosan microsphere and its preparation method and application
  • A kind of cross-linked chitosan microsphere and its preparation method and application
  • A kind of cross-linked chitosan microsphere and its preparation method and application

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Embodiment 1

[0040] 1. Preparation of cross-linked chitosan microspheres

[0041] 1) Preparation of chitosan acetic acid solution: prepare 2% (vt) acetic acid solution with glacial acetic acid, get a certain amount of 2% acetic acid solution to be mixed with 3% (wt) chitosan acetic acid solution and magnetically stir at room temperature to dissolve completely After standing still, obtain uniform light brown viscous solution;

[0042]2) Preparation of oil phase and surfactant: use 3% chitosan acetic acid solution as water phase, liquid paraffin as oil phase, add oil phase: water phase = 3:1 volume ratio; use Span80 as surface active agent, the added volume ratio is 1 / 10 of the water phase;

[0043] 3) The preparation process of cross-linked chitosan microspheres: at room temperature, use a syringe to draw 10 mL of 3% chitosan acetic acid solution (chitosan mass is about 0.3 g) in step 1) and add it to the preparation in step 2). In a 250mL flat-bottomed flask with 30mL of liquid paraffin ...

Embodiment 2

[0048] 1. Preparation of cross-linked chitosan microspheres

[0049] 1) Preparation of chitosan acetic acid solution: prepare 2% (vt) acetic acid solution with glacial acetic acid, get a certain amount of 2% acetic acid solution to be mixed with 3% (wt) chitosan acetic acid solution and magnetically stir at room temperature to dissolve completely After standing still, obtain uniform light brown viscous solution;

[0050] 2) Preparation of oil phase and surfactant: use 3% chitosan acetic acid solution as water phase, liquid paraffin as oil phase, add oil phase: water phase = 3:1 volume ratio; use Span80 as surface active agent, the added volume ratio is 1 / 10 of the water phase;

[0051] 3) The preparation process of cross-linked chitosan microspheres: at room temperature, use a syringe to draw 10 mL of 3% chitosan acetic acid solution (chitosan mass is about 0.3 g) in step 1) and add it to the preparation in step 2). In a 250mL flat-bottomed flask with 30mL of liquid paraffin...

Embodiment 3

[0055] 1. Preparation of cross-linked chitosan microspheres

[0056] 1) Preparation of chitosan acetic acid solution: prepare 2% (vt) acetic acid solution with glacial acetic acid, get a certain amount of 2% acetic acid solution to be mixed with 3% (wt) chitosan acetic acid solution and magnetically stir at room temperature to dissolve completely After standing still, obtain uniform light brown viscous solution;

[0057] 2) Preparation of oil phase and surfactant: use 3% chitosan acetic acid solution as water phase, liquid paraffin as oil phase, add oil phase: water phase = 3:1 volume ratio; use Span80 as surface active agent, the added volume ratio is 1 / 10 of the water phase;

[0058] 3) The preparation process of cross-linked chitosan microspheres: draw 10 mL of 3% chitosan acetic acid solution (chitosan mass is about 0.3 g) in step 1) with a syringe at room temperature In a 250mL flat-bottomed flask with 30mL of liquid paraffin and 1mL of Span80, stir at a stirring rate o...

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Abstract

The invention discloses cross-linked chitosan microspheres, and a preparation method and application thereof, and belongs to the field of high polymer materials. The preparation method comprises the following steps: (1) dissolving chitosan powder in acetic acid solution to form an aqueous phase, adding an emulsifying agent into liquid paraffin, and mixing uniformly to form an oil phase; (2) injecting the aqueous phase into the oil phase, and stirring to form a water-in-oil type emulsion; (3) adding benzaldehyde into the water-in-oil type emulsion to generate Schiff alkali for protecting amino, adding a pore-foaming agent and stirring, adjusting the pH to be 9 to 10, and then adding epichlorohydrin and diethylenetriamine in sequence to perform cross-linking reaction; (4) after the cross-linking reaction is ended, separating to obtain a reaction product; (5) removing the oil phase and protecting groups from the reaction product, reducing to generate the amino, and washing and drying to obtain the cross-linked chitosan microspheres. The cross-linked chitosan microspheres prepared by the preparation method are small in particle size and high in dispersibility, and can be used as an adsorption agent for a dye, namely, Congo red; the chemical stability is improved.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a cross-linked chitosan microsphere and a preparation method and application thereof. Background technique [0002] Chitosan (chitosan) is the product of deacetylation of chitin, also known as chitosan, deacetylated chitin, etc., its scientific name is β-1,4-poly-D-glucosamine, and its molecular formula is (C 6 h 11 NO 4 ) n . Chitosan is white or off-white, amorphous, translucent, pearlescent flaky or powdery solid, insoluble in water and alkaline solution, soluble in inorganic acids such as dilute hydrochloric acid and nitric acid, and most organic acids such as acetic acid. Compared with other polysaccharides such as cellulose and starch, chitosan has higher chemical activity. Chitosan is widely used in textile, printing and dyeing, medicine, environmental protection and other industries. [0003] In printing and dyeing, chitosan is mainly used for the treatment of print...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/24C08J3/09B01J20/24C08L5/08
CPCB01J20/24C08J3/098C08J3/24C08J2305/08
Inventor 黄俊林越呈毛建卫梅乐和胡升王宏鹏龚金炎张祥谢东芳
Owner ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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