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Chitosan single guanidine hydrochloride loaded nanometer titanium dioxide compound and preparation method thereof

A technology of nano-titanium dioxide and chitosan, which is applied in textiles, papermaking, fiber treatment, etc., can solve the problems of limited application of pH sensitivity and low antibacterial activity of chitosan, and achieve high continuous antibacterial effect, excellent anti-ultraviolet radiation, The effect of high-efficiency broad-spectrum antibacterial properties

Active Publication Date: 2014-03-12
科凯精细化工(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chitosan has become the most commonly used natural antibacterial agent because of its cheap and easy to obtain, easy to process, non-toxic, tasteless, good biodegradation, regeneration, antibacterial and antiseptic properties, but compared with traditional antibacterial agents, The antibacterial activity of chitosan is low, and its pH sensitivity limits its application under alkaline conditions

Method used

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  • Chitosan single guanidine hydrochloride loaded nanometer titanium dioxide compound and preparation method thereof
  • Chitosan single guanidine hydrochloride loaded nanometer titanium dioxide compound and preparation method thereof
  • Chitosan single guanidine hydrochloride loaded nanometer titanium dioxide compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 8mL of hydrogen peroxide in a beaker, add 0.4mL of concentrated sulfuric acid, stir, and make a hydrogen peroxide acidic solution, then weigh 5g of thiourea dioxide, and alternately put the hydrogen peroxide acidic solution and thiourea dioxide into the Erlenmeyer flask, and control the reaction temperature at 50-55°C. After stirring for 2 hours, filter to obtain smooth and shiny thiourea trioxide hydrate crystals; figure 1 is the FT-IR map of thiourea trioxide, where 1230 and 1050cm - The strong absorption peak at , evidenced the formation of thiourea trioxide.

[0026] Weigh 5g of chitosan, add 200mL of hydrochloric acid solution with a concentration of 0.2mol / L, stir thoroughly for 4h; use 50g / L of sodium carbonate solution to adjust the pH of the chitosan solution to 8-9, then wash with distilled water to pH When the value is 7.0 to 7.5, centrifuge, drain part of the upper layer of clear water, put it into a three-hole flask, and start heating to 50°C; add 3.8...

Embodiment 2

[0029] The preparation of chitosan monoguanidine hydrochloride is the same as in Example 1.

[0030] Take a certain amount of chitosan monoguanidine hydrochloride and dissolve it in water, stir and dissolve, and prepare a chitosan monoguanidine hydrochloride solution with a mass percentage of 5%, take 15mL of the above-mentioned chitosan monoguanidine hydrochloride solution and 0.145g nano-TiO 2Place in a beaker, ultrasonically disperse for 1 hour, then add 0.15mL Tween80 to obtain a pre-emulsified aqueous phase mixture; add 100mL petroleum ether, 50mL liquid paraffin and 7.5mL Span8080 to a three-necked flask, and stir evenly to obtain an oil phase mixture. Add the pre-emulsified water phase mixture to the oil phase mixture by spraying within 30min, control the reaction temperature at 30°C, stir for 0.5h, add 0.75mL glutaraldehyde, continue stirring for 4h, let stand, filter with suction, wash, sample Vacuum drying for 12 hours to obtain chitosan monoguanidine hydrochloride ...

Embodiment 3

[0032] The preparation of chitosan monoguanidine hydrochloride is the same as in Example 1.

[0033] Take a certain amount of chitosan monoguanidine hydrochloride and dissolve it in water, stir and dissolve, and prepare a chitosan monoguanidine hydrochloride solution with a mass percentage of 5%, take 15mL of the above-mentioned chitosan monoguanidine hydrochloride solution and 0.072g nano-TiO 2 Place in a beaker, ultrasonically disperse for 1 hour, then add 0.15mL Tween80 to obtain a pre-emulsified aqueous phase mixture; add 100mL petroleum ether, 50mL liquid paraffin and 7.5mL Span80 to a three-necked flask, and stir mechanically to obtain an oil phase mixture. Add the pre-emulsified water phase mixture to the oil phase mixture by spraying within 30min, control the reaction temperature at 30°C, stir for 0.5h, add 0.75mL glutaraldehyde, continue stirring for 4h, let stand, filter with suction, wash, sample Vacuum drying for 12 hours to obtain chitosan monoguanidine hydrochlo...

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Abstract

The invention discloses a chitosan single guanidine hydrochloride loaded nanometer titanium dioxide compound and a preparation method thereof. The preparation method comprises the following steps: using a natural antibacterial agent namely chitosan as a skeleton, and chemically modifying the chitosan; using aminoiminomethanesulfonic acid to inoculate a single guanidine groups on the chitosan through reaction to obtain chitosan single guanidine hydrochloride; using glutaraldehyde as a cross-linking agent, and coating the nanometer titanium dioxide particles with glutaraldehyde to obtain a chitosan single guanidine hydrochloride loaded nanometer titanium dioxide microspheric antibacterial agent. The prepared compound comprises natural, organic and inorganic antibacterial agents, has a broad-spectrum and efficient antibacterial performance, can ensure that finished textiles can still keep a better antibacterial effect in more and wider environments, and is suitable for antibiotic finish of various textiles.

Description

technical field [0001] The invention relates to the preparation of a textile antibacterial agent, in particular to a chitosan monoguanidine hydrochloride loaded nano-titanium dioxide composite and a preparation method thereof. technical background [0002] There are two production methods for antibacterial fabrics: one method is to add antibacterial agents to fiber-forming polymers and make antibacterial fibers after spinning; the other method is to use antibacterial finishing methods, which are currently the most commonly used The method is the antibacterial finishing method, which is realized by adding antibacterial agents to textiles; there are many antibacterial finishing agents applied to textiles, and traditional antibacterial finishing agents mainly include natural antibacterial agents, inorganic, organic and polymer antibacterial agents. Four categories of agents. Comparing and analyzing all types of antibacterial agents shows that although various types of antibact...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M11/46D06M15/03D06M23/12C08B37/08
Inventor 任一波周文张萍武小荣张乃超戚文迎俞成丙
Owner 科凯精细化工(上海)有限公司
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