Preparation method of cyclodextrin derivatives capable of grafting silk fabric

A technology of cyclodextrin and derivatives, applied in the direction of animal fiber, textile and papermaking, fiber processing, etc., can solve the problems of low grafting rate and silk damage, and achieve the effect of good grafting effect.

Inactive Publication Date: 2010-03-17
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, cyclodextrin derivative finishing agents for silk, such as aldehyde compounds, and chlorotriazine cyclodextrin derivatives will cause certain damage to silk when grafted, and the grafting rate is not high

Method used

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  • Preparation method of cyclodextrin derivatives capable of grafting silk fabric
  • Preparation method of cyclodextrin derivatives capable of grafting silk fabric
  • Preparation method of cyclodextrin derivatives capable of grafting silk fabric

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Synthesis of 2-tosylated-β-cyclodextrin (β-CD-2-OTs): add 8g β-CD (approx. 7.06mmol) and 300ml of 0.15mol / L NaOH aqueous solution, fully stirred to dissolve. Dissolve 6g of p-toluenesulfonyl chloride in a small amount of acetonitrile, and slowly drop it into the three-necked flask within 2 hours, and continuously replenish 1mol / L NaOH aqueous solution during the dropping process to ensure that the pH of the reaction solution is ≥ 12.5. After p-toluenesulfonyl chloride was dropped, the stirring reaction was continued for 2 hours. After the reaction is completed, neutralize to neutral with 1mol / L hydrochloric acid, filter off a small amount of unreacted p-toluenesulfonyl chloride. Vacuum rotary evaporate the filtrate to dryness, and obtain a white solid. Then desalt the solid twice with 200ml of anhydrous methanol, reflux The liquid is cooled, filtered, and evaporated to obtain the white powder product β-CD-2-OTs.

[0033] Synthesis of 2-ethylenediamine-β-cyclodextrin (...

Embodiment 2

[0036] Synthesis of 2-tosylated-β-cyclodextrin (β-CD-2-OTs): 8gβ-CD (approximately 7.06 mmol) and 300ml of 0.15mol / L NaOH aqueous solution, fully stirred to dissolve. Dissolve 8 g of p-toluenesulfonyl chloride in a small amount of acetonitrile, and slowly drop it into the three-necked flask within 3 hours. During the dropping process, 1 mol / L NaOH aqueous solution is continuously added to ensure that the pH of the reaction solution is ≥ 12.5. After p-toluenesulfonyl chloride was dropped, the stirring reaction was continued for 3 hours. After the reaction is completed, neutralize to neutral with 1mol / L hydrochloric acid, filter off a small amount of unreacted p-toluenesulfonyl chloride. Vacuum rotary evaporate the filtrate to dryness, and obtain a white solid. Then desalt the solid twice with 200ml of anhydrous methanol, reflux The liquid is cooled, filtered, and evaporated to obtain the white powder product β-CD-2-OTs.

[0037] Synthesis of 2-ethylenediamine-β-cyclodextrin (...

Embodiment 3

[0040] Synthesis of 2-tosylated-β-cyclodextrin (β-CD-2-OTs): 8gβ-CD (approximately 7.06 mmol) and 300ml of 0.15mol / L NaOH aqueous solution, fully stirred to dissolve. Dissolve 10 g of p-toluenesulfonyl chloride in a small amount of acetonitrile, and slowly drop it into the three-necked flask within 4 hours, and continuously replenish 1 mol / L NaOH aqueous solution during the dropping process to ensure that the pH of the reaction solution is ≥ 12.5. After p-toluenesulfonyl chloride was dropped, the stirring reaction was continued for 4 hours. After the reaction is completed, neutralize to neutral with 1mol / L hydrochloric acid, filter off a small amount of unreacted p-toluenesulfonyl chloride. Vacuum rotary evaporate the filtrate to dryness, and obtain a white solid. Then desalt the solid twice with 200ml of anhydrous methanol, reflux The liquid is cooled, filtered, and evaporated to obtain the white powder product β-CD-2-OTs.

[0041] Synthesis of 2-ethylenediamine-β-cyclodext...

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PUM

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Abstract

The invention relates to a preparation method of cyclodextrin derivatives capable of grafting silk fabric, which comprises the following steps: (1) dissolving beta-CD into NaOH water solution, addingdropwise paratoluensulfonyl chloride, and stirring for reaction; (2) uniformly mixing ethylene diamine and beta-CD-2-OTs in a container for reaction for 5h at the temperature of 65-75 DEG C, filteringand dispersing the mixture in an acetone solution, and separating products out; and (3) dissolving the products into N,N'-dimethyl formamide, adding dropwise 2,3-dibromopropionyl chloride at the temperature of 0-5 DEG C for reaction, and using acetone for depositing and filtering. The preparation method of the invention is simple, the yield is 70.39-85.90%, and the method has better grafting effect on real silk fabric.

Description

technical field [0001] The invention belongs to the field of preparation of cyclodextrin derivatives, in particular to a preparation method of cyclodextrin derivatives capable of grafting silk fabrics. Background technique [0002] Silk, known as the "fiber queen", has now become the pursuit of people who yearn for a better life. People increasingly hope that silk fabrics can have various additional functions, such as health care, in addition to the functions of body covering, cold protection, and beauty. , can release fragrance, can last antibacterial when preserved, and so on. Since cyclodextrins have a special molecular structure with a hydrophilic outer cavity and a hydrophobic inner cavity, they can contain various active substances such as drugs, flavors, anti-ultraviolet agents, antibacterial agents, etc., and slowly release various active substances during use to achieve long-lasting Therefore, the use of cyclodextrins to finish silk has broad application prospects....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16D06M15/03D06M101/10
Inventor 赵曙辉黄良晨
Owner DONGHUA UNIV
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