Preparation and application of attapulgite-supported chitosan cross-linked cyclodextrin complex

A technology of loading chitosan and cross-linked cyclodextrin, which is applied in the direction of chemical instruments and methods, natural dyes, organic dyes, etc., can solve the high requirements of the refining process and separation technology of macroporous adsorption resins and affect the quality of macroporous adsorption resins. Solve problems such as separation effect and complex process, achieve excellent purification effect, shorten purification process, and simple purification process steps

Active Publication Date: 2020-02-11
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 cross-linked cyclodextrin complex
  • Preparation and application of attapulgite-supported chitosan cross-linked cyclodextrin complex

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 sugar sol was 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...

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 oxalate acetate shell at a solid-to-liquid ratio of 5g: 3.5ml The polysaccharide 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 th...

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Abstract

The invention relates to the field of chemical synthesis, and discloses the preparation and application of an attapulgite-loaded chitosan cross-linked cyclodextrin complex, which is prepared by the following method: acid-activated attapulgite and oxalic acid-acetic acid chitosan with a volume of V Mix sugar sol evenly, centrifuge, filter, and vacuum dry to constant weight to obtain attapulgite once loaded with chitosan; after standing, remove the supernatant, add alkaline water to the residue until the pH value is 6.8~7.2, centrifuge, wash with water , suction filtration, and vacuum drying to constant weight to obtain the attapulgite-loaded chitosan; evenly pour the cyclodextrin aqueous solution into the attapulgite-loaded chitosan, stir quickly and evenly, and slowly add a crosslinking agent dropwise therein, After fully reacting, it is filtered, and the filtrate is washed with water to neutrality, and then washed with ketone, alcohol, suction filtered and dried to obtain the attapulgite-loaded chitosan cross-linked cyclodextrin complex. Compared with the macroporous resin, the complex has better adsorption effect on 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 Patents(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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