Preparation method of antibacterial graphene slurry

A production method and graphene technology, applied in the field of textile processing, can solve the problems of poor environmental protection, limited grafting rate of chitosan, and inadaptability to green production concepts, etc.

Pending Publication Date: 2020-10-23
合肥克拉伦斯科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since graphene oxide is electronegative, it has poor adsorption to anionic dyes that are also electronegative
Although the patent CN 102995394A discloses that the dyes contain anionic dyes, and it is theoretically stated that the dyes can produce van der Waals forces, hydrogen bonds, and ionic bonds with chitosan, the chitosan / graphene oxide produced has not been tested. The adsorption capacity of composite materials to anionic dyes, so it cannot objectively reflect that chitosan / graphene oxide composite materials can significantly improve the dyeing effect of anionic dyes on textiles
[0005] Although chitosan is a natural antibacterial agent, the grafting rate of chitosan on graphene oxide is limited due to the large molecular structure of chitosan
Moreover, in order to improve the grafting rate and ensure the antibacterial properties of the finishing agent, it is necessary to make a large excess of chitosan relative to graphene oxide when preparing the chitosan / graphene oxide composite material, so that the chitosan a lot of waste
In addition, chitosan has poor water solubility. Patent CN 102995394A uses dimethylformamide as a solvent, but dimethylformamide has certain toxicity, so its preparation method is less environmentally friendly and does not adapt to the current green production concept

Method used

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  • Preparation method of antibacterial graphene slurry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Production of antibacterial graphene slurry:

[0042] (1) Add 2.50 g of graphene oxide into 500 mL of water, and ultrasonically disperse for 30 min under the conditions of ultrasonic frequency 40 KHz and ultrasonic power 100 W to obtain a graphene oxide solution.

[0043] (2) Add 1.85g 3-amino-1-cyclopropylpyrazole, 3.31g EDC, 0.99gNHS to the graphene oxide solution, ultrasonically dissolve it under the conditions of ultrasonic frequency 40KHz and ultrasonic power 100W, then heat up to 60°C magnetically Stirring and reacting for 5 hours, after the reaction was completed, filtered, the filter residue was washed with water three times, and dried in an oven at 70°C to obtain modified graphene oxide. In the FT-IR spectrum of modified graphene oxide at 1658cm -1 C=O bond stretching vibration peak (amide I band) appears at 1531cm -1 The N-H bond stretching vibration peak (amide II band) appeared at , indicating that 3-amino-1-cyclopropylpyrazole was successfully linked to g...

Embodiment 2

[0047] Production of antibacterial graphene slurry:

[0048] (1) Add 2.50 g of graphene oxide into 500 mL of water, and ultrasonically disperse for 30 min under the conditions of ultrasonic frequency 40 KHz and ultrasonic power 100 W to obtain a graphene oxide solution.

[0049] (2) Add 1.48g 3-amino-1-cyclopropylpyrazole, 3.31g EDC, and 0.99gNHS to the graphene oxide solution, and heat it up to 60°C after ultrasonic dissolution under the conditions of ultrasonic frequency 40KHz and ultrasonic power 100W. Stirring and reacting for 5 hours, after the reaction was completed, filtered, the filter residue was washed with water three times, and dried in an oven at 70°C to obtain modified graphene oxide.

[0050] (3) Add the modified graphene oxide prepared above to 500mL of water, ultrasonically disperse for 30min under the conditions of ultrasonic frequency 40KHz and ultrasonic power 100W, then add 0.65g nanometer zinc oxide, heat up to 75°C for 4h with magnetic stirring, the reac...

Embodiment 3

[0059] Example 3 uses the antibacterial graphene slurry prepared in Example 1 to dye the cellulose fiber fabric.

[0060] Synthesis of histidine hexanediol ester: first dissolve 1.55g L-histidine and 1.18g 1,6-hexanediol in water to form histidine solution and hexanediol solution, and then add L-histidine Add hexanediol solution and 0.2g 98% concentrated sulfuric acid dropwise to the acid solution at the same time. After the dropwise addition, raise the temperature to 75°C and stir for 3 hours. After crystallization under low temperature for 12 hours, suction filtration, the obtained solid was dried at 50° C. to obtain histidine hexanediol ester with a yield of 97.5% and a purity of 99.3%. ESI-MS: m / z=256.18[M+1] + .Elem.C, 56.43; H, 8.29; N, 16.47; O, 18.81.

[0061] Dyeing of cellulose fiber fabrics:

[0062] (1) Add the antibacterial graphene slurry prepared by embodiment 1, Congo red and the histidine hexylene glycol ester prepared in water, the concentration of nano-zi...

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Abstract

The invention discloses a preparation method of antibacterial graphene slurry, and relates to the technical field of textile processing. According to the invention, the antibacterial graphene slurry with antibacterial performance and good adsorption to anionic dyes is prepared through two-step chemical modification treatment of graphene oxide; after an anionic dye is added into the antibacterial graphene slurry, the cellulosic fiber fabric can be efficiently dyed, so that the utilization rate of the dye is remarkably improved, and the cellulosic fiber fabric is endowed with excellent antibacterial performance.

Description

Technical field: [0001] The invention relates to the technical field of textile processing, in particular to a method for preparing an antibacterial graphene slurry. Background technique: [0002] Graphene is a new star carbon-based material developed in recent years. Graphene is a carbon atom with sp 2 The hybridized orbitals form a hexagonal planar film with a honeycomb lattice, a two-dimensional material with a thickness of only one carbon atom. due to sp 2 With the existence of hybrid orbitals, graphene can adsorb aromatic substances through π-π stacking, so it can be used to remove organic dyes with aromatic ring structures. [0003] Graphene oxide is the oxide of graphene, with a large number of carboxyl groups, hydroxyl groups and epoxy groups on the surface, which is electronegativity. Patent CN 102995394A discloses a graphene oxide-based dyeing and antibacterial finishing agent, which is a chitosan / graphene oxide / dye composite material, and the dyes are reactive...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06P1/673D06P1/645D06P3/60
CPCD06P1/673D06P1/645D06P3/60
Inventor 任礼新
Owner 合肥克拉伦斯科技有限公司
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