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Preparation method of ketone anhydride-polyphenolic acid active oxygen molecule finishing agent

A technology of polyphenolic acid and active oxygen, applied in the field of textile processing, can solve the problems of high activity and poor stability of active oxygen components, and achieve efficient killing effect

Active Publication Date: 2021-10-22
安徽三宝棉纺针织投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the development of the above-mentioned active oxygen antibacterial and anti-mite finishing agents is still in the laboratory stage, and the technical bottleneck of batch synthesis has not yet been overcome. At the same time, the high activity and poor stability of active oxygen components make it difficult to carry out stable immobilization on the surface of textile materials. Therefore, how to realize the batch synthesis of active oxygen antibacterial and anti-mite finishing agents and the efficient immobilization of active oxygen molecules is still a key problem to be solved.

Method used

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  • Preparation method of ketone anhydride-polyphenolic acid active oxygen molecule finishing agent
  • Preparation method of ketone anhydride-polyphenolic acid active oxygen molecule finishing agent
  • Preparation method of ketone anhydride-polyphenolic acid active oxygen molecule finishing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Synthesis of active oxygen molecules of ketone anhydride-polyphenolic acid:

[0026] Add 0.05mol BDTA to THF, add 0.05g DMAP after complete dissolution, then dropwise add 0.1mol caffeic acid THF solution, heat to reflux state, keep it warm for 5 hours, and when the reaction is complete, add water and ethyl acetate at a volume ratio of 1:1 Ester extraction, take the organic layer, distill under reduced pressure to recover ethyl acetate, vacuum dry, and column chromatography to obtain BDTA-caffeic acid compound. 1 H NMR(DMSO-d6,400MHz),δ:13.22(s,2H),12.05(s,2H),9.46(s,2H),8.41-8.21(m,6H),7.45(d,2H),7.28 -7.26(m,6H), 6.28(d,2H); ESI-MS: m / z=683.1[M+1] + .

[0027]

[0028] 2. Preparation of ketone anhydride-polyphenolic acid reactive oxygen molecule finishing agent:

[0029] Add ketone anhydride-polyphenolic acid active oxygen molecules to the mixed solvent of ethanol and water with a volume ratio of 2:1, the mass concentration of the ketone anhydride-polyphenolic...

Embodiment 2

[0031] 1. Synthesis of active oxygen molecules of ketone anhydride-polyphenolic acid:

[0032] Add 0.05mol IDPA to tetrahydrofuran, add 0.08g DMAP after the dissolution is complete, then add dropwise 0.1mol gallic acid tetrahydrofuran solution, heat to reflux state and keep it warm for 5 hours. After the reaction is completed, add water and ethyl acetate with a volume ratio of 1:1 Ester extraction, take the organic layer, distill under reduced pressure to recover ethyl acetate, vacuum dry, and column chromatography to obtain IDPA-gallic acid compound. 1 H NMR(DMSO-d6,400MHz),δ:13.20(s,2H),12.75(s,2H),9.47(s,4H),8.40-8.22(m,6H),7.54-7.47(m,4H) ,7.15(s,4H); ESI-MS: m / z=767.08[M+1] + .

[0033]

[0034] 2. Preparation of ketone anhydride-polyphenolic acid reactive oxygen molecule finishing agent:

[0035] Add ketone anhydride-polyphenolic acid active oxygen molecules to a mixed solvent of acetone and water with a volume ratio of 1:1, the mass concentration of ketone anhydri...

Embodiment 3

[0037] 1. Synthesis of active oxygen molecules of ketone anhydride-polyphenolic acid:

[0038] Add 0.05mol BDTA to tetrahydrofuran, add 0.05g DMAP after complete dissolution, then dropwise add 0.1mol chlorogenic acid tetrahydrofuran solution, heat to reflux state and keep it warm for 5 hours. After the reaction is completed, add water and acetic acid with a volume ratio of 1:1 Extract with ethyl ester, take the organic layer, distill under reduced pressure to recover ethyl acetate, dry in vacuum, and perform column chromatography to obtain BDTA-chlorogenic acid compound. 1 H NMR(DMSO-d6,400MHz),δ:13.22(s,2H),12.85(s,2H),9.46(s,2H),8.41-8.21(m,6H),7.45(d,2H),7.28 -7.26(m,6H),6.31(d,2H),5.91(s,2H),4.62-4.61(m,4H),4.39(s,2H),4.12(m,2H),3.54(m,2H ),1.94-1.85(m,8H); ESI-MS: m / z=1031.2[M+1] + .

[0039]

[0040] 2. Preparation of ketone anhydride-polyphenolic acid reactive oxygen molecule finishing agent:

[0041]Add ketone anhydride-polyphenolic acid active oxygen molecules ...

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Abstract

The invention discloses a preparation method of a ketone anhydride-polyphenolic acid active oxygen molecule finishing agent, and relates to the technical field of textile processing. According to the invention, a ketone anhydride-polyphenolic acid compound is synthesized and added into a finishing agent as an antibacterial and anti-mite effective component, and a fiber base cloth is endowed with excellent antibacterial and anti-mite performance through an after-finishing procedure, wherein the antibacterial and anti-mite performance is achieved by releasing active oxygen through the ketone anhydride-polyphenolic acid compound so as to achieve efficient killing of bacteria and mites, the finishing agent is safe, non-toxic, colorless and odorless and belongs to a green antibacterial and anti-mite agent, the bacteria killing rate can be larger than or equal to 99%, the mite repelling rate can be larger than or equal to 80%, and the antibacterial and anti-mite performance of the fiber base cloth is not obviously attenuated after the fiber base cloth is dried and stored in a dark place at 37 DEG C for 3 months.

Description

Technical field: [0001] The invention relates to the technical field of textile processing, in particular to a preparation method of a ketone anhydride-polyphenolic acid reactive oxygen molecule finishing agent. Background technique: [0002] There are many harmful microorganisms (bacteria, fungi, etc.) and mites in people's living environment. These substances invade the human body and can cause diseases such as meningitis, psoriasis, allergic dermatitis, allergic rhinitis, and seriously affect people's health. In daily life, textiles are the items that have been in contact with human skin for the longest time, such as clothing and home textiles. However, during use, textiles tend to absorb water, accumulate dander shed by human metabolism, and trap fine particles in the air. An excellent place for the growth and reproduction of Staphylococcus aureus, Candida albicans, dust mites, etc. Therefore, the development of antibacterial and anti-mite textiles has very important pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/89A01N43/12A01P3/00A01P1/00D06M13/224D06M23/04
CPCC07D307/89A01N43/12D06M13/2246D06M13/224D06M23/04D06M16/00
Inventor 张丽马晓飞张志成
Owner 安徽三宝棉纺针织投资有限公司
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