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Preparation and application of attapulgite-supported chitosan crosslinked cyclodextrin composite

A technology of loading chitosan and cross-linked cyclodextrin, which is applied in chemical instruments and methods, natural dyes, organic dyes, etc., can solve the complex process, high requirements and great influence of macroporous adsorption resin refining process and separation technology Pore ​​adsorption resin separation effect and other issues, to achieve the effect of simple purification process steps, excellent purification effect, and shorten the purification process

Active Publication Date: 2017-11-03
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since each operation unit will affect the separation effect of the macroporous adsorption resin, the requirements for the refining process and separation technology of the macroporous adsorption resin are relatively high, and the process is relatively complicated.

Method used

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  • Preparation and application of attapulgite-supported chitosan crosslinked cyclodextrin composite
  • Preparation and application of attapulgite-supported chitosan crosslinked cyclodextrin composite
  • Preparation and application of attapulgite-supported chitosan crosslinked cyclodextrin composite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0019] This embodiment provides an attapulgite-loaded chitosan cross-linked cyclodextrin complex, which is prepared by the following method:

[0020] 1) Preparation of acid-activated attapulgite:

[0021] Attapulgite was calcined at 700°C for 4 h, and after cooling down, it was added to 1 mol / L hydrochloric acid aqueous solution, the concentration of attapulgite in hydrochloric acid aqueous solution was 0.5 g / mL, stirred at 90°C for 4 h, and then centrifuged to collect The solid was washed with water until neutral, then added to 10% oxalic acid aqueous solution, the addition amount was 0.5 g / mL, stirred at room temperature for 2 h, left standing for 5 h, centrifuged, collected solid, washed with water until neutral, 120 °C Dry to obtain acid-activated attapulgite.

[0022] 2) Preparation of chitosan oxalate acetate sol:

[0023] Mix 10wt% oxalic acid aqueous solution and 1wt% acetic acid aqueous solution at a volume ratio of 4:1, then add chitosan with a solution mass of 3%,...

Embodiment approach 2

[0033] This embodiment provides an attapulgite-loaded chitosan cross-linked cyclodextrin complex, which is prepared by the following method:

[0034] 1) Preparation of acid-activated attapulgite:

[0035] The method is the same as that in Embodiment 1.

[0036] 2) Preparation of chitosan oxalate acetate sol:

[0037] The method is the same as that in Embodiment 1.

[0038] 3) Preparation of attapulgite-loaded chitosan:

[0039] a. Take chitosan oxalate acetate sol, dilute it with 2 times the volume of water, heat to 50°C and stir for 1 hour, then cool down to room temperature, and mix acid-activated attapulgite with diluted chitosan oxalate acetate at a solid-to-liquid ratio of 5g:5ml The sols were mixed, stirred for 3 hours, centrifuged, filtered, and vacuum-dried at 55°C to constant weight to obtain attapulgite once loaded with chitosan;

[0040] b. Take the chitosan oxalate acetate sol of the same volume as in a again, dilute it with 2 times the volume of water, mix it ...

Embodiment approach 3

[0046] This embodiment provides a preparation method of attapulgite-loaded chitosan cross-linked cyclodextrin complex, comprising the following steps:

[0047] 1) Preparation of acid-activated attapulgite:

[0048] The method is the same as that in Embodiment 1.

[0049] 2) Preparation of chitosan oxalate acetate sol:

[0050] The method is the same as that in Embodiment 1.

[0051] 3) Preparation of attapulgite-loaded chitosan:

[0052] a. Take chitosan oxalate acetate sol, dilute it with 3 times the volume of water, heat to 50°C and stir for 3 hours, then cool down to room temperature, and mix acid-activated attapulgite with diluted chitosan oxalate acetate at a solid-to-liquid ratio of 5g: 3.5ml The sugar sol was mixed, stirred for 4 hours, centrifuged, filtered, and vacuum-dried at 55°C to constant weight to obtain attapulgite once loaded with chitosan;

[0053] b. Take the chitosan oxalate acetate sol of the same volume as in a again, dilute it with 3 times the volu...

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Abstract

The invention relates to the field of chemical synthesis and discloses preparation and application of attapulgite-supported chitosan crosslinked cyclodextrin composite; the preparation includes mixing well acid-activated attapulgite with chitosan oxaloacetate sol having volume of V, centrifuging the mixture, performing suction filtering, and drying in vacuum to constant weight to obtain primary attapulgite-supported chitosan; allowing standing, removing supernate, adding alkaline liquor into the remainder until pH is 6.8-7.2, centrifuging, washing, performing suction filtering, and drying in vacuum to constant weight to obtain attapulgite-supposed chitosan; pouring cyclodextrin solution evenly into the attapulgite-supported chitosan, stirring fast and well, dropwise adding a crosslinking agent slowly, filtering after full reaction, washing filtered material to neutrality, and performing ketone washing, alcohol washing, suction filtering and drying to obtain the attapulgite-supported chitosan crosslinked cyclodextrin composite. Compared with macroporous resins, the composite of the invention has good adsorbing effect for plant pigments.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to the preparation of an attapulgite-loaded chitosan-crosslinked cyclodextrin compound and its application in extracting pigments. Background technique [0002] Macroporous adsorption resin selectively adsorbs organic substances from the solution through physical adsorption, so as to achieve the purpose of separation and purification. At present, macroporous adsorption resin is also used for separation and purification in the process of extracting pigments from plants. When using macroporous adsorption resin for separation and refining process, the general operation steps are: macroporous adsorption resin pretreatment-resin loading column-medicine solution loading column-desorption of macroporous adsorption resin-macroporous adsorption resin desorption Clean, regenerate. Since each operation unit will affect the separation effect of the macroporous adsorption resin, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L5/16C08L5/08C08K9/02C08K9/04C08K3/34C08J3/24C09B61/00
CPCC08J3/246C08J2305/08C08J2305/16C08J2405/08C08J2405/16C08L5/08C08L5/16C08L2205/02C09B61/00C08K9/02C08K9/04C08K3/346
Inventor 王朝宇毕艳红迟雪文罗洪镇董庆
Owner HUAIYIN INSTITUTE OF TECHNOLOGY
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