A kind of anti-ultraviolet treatment agent based on disperse dye modification and preparation method thereof

A technology of disperse dyes and treatment agents, applied in the direction of nitro/nitroso dyes, amino-hydroxyanthraquinone dyes, anthracene dyes, etc., can solve the problems of fiber initial strength decline, spinneret hole clogging, and failure to meet the use requirements, etc. , to achieve a high affinity effect

Active Publication Date: 2019-06-28
CHENGDU TEXTILE COLLEGE
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AI Technical Summary

Problems solved by technology

Although this treatment method improves the retention rate of fiber strength, its anti-ultraviolet performance is equivalent to that of uncoated fibers after three times of washing (Dong Linan. Research on photoaging and stabilization of aromatic polyoxadiazole fibers [D] .Chengdu: Sichuan University, 2010; Yang Xiao. Poly 1,3,4-oxadiazole (POD) aging and protection research [D]. Chengdu: Sichuan University, 2011); Azo structure substances that selectively absorb light to protect the heterocyclic structure in the macromolecular chain, but these azo structure substances not only easily cause spinneret hole blockage during spinning, but also reduce the initial strength of the fiber (Zhou W, Yang X, Jia E, Wang X, Xu J, Ye G.Ultraviolet resistance of azo-containing poly(1,3,4-oxadiazole) fibers[J].Polymer Degradation and Stability,2013,98(3 ):691-696); (3) choose disperse dyes containing azo structure to dye the fiber
However, due to the limited effect of the azo group in the dye, the anti-ultraviolet performance of the fiber can only be improved by about 30%, which is far from meeting the requirements of use (Ji Changqing, Zhang Zaixing, Li Wentao, Xing Tieling, Chen Guoqiang. Influence of Fiber Light Stability[J]. Printing and Dyeing, 2014,40(9):1-4); (4) Direct finishing method, that is, water-soluble eight(γ-aminopropyl) with anti-ultraviolet function Silsesquioxane as a finishing agent for surface treatment of fibers
Although the method is simple to operate and requires less equipment, since the method uses water-soluble POSS with amino groups, after the fibers are treated by padding, baking, etc., the POSS molecules can only be adsorbed. The van der Waals force fixes the defects on the fiber surface and the gaps of the fibrils

Method used

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  • A kind of anti-ultraviolet treatment agent based on disperse dye modification and preparation method thereof
  • A kind of anti-ultraviolet treatment agent based on disperse dye modification and preparation method thereof
  • A kind of anti-ultraviolet treatment agent based on disperse dye modification and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Mix 0.3 part of octavinyl silsesquioxane, 0.3 part of octapropenyl silsesquioxane and 0.8 part of disperse red 60 dye, which are respectively ground into powders with a particle size of 0.5-1 μm, under nitrogen atmosphere, together with 0.15 part of Parts of anhydrous aluminum chloride were added together in 60 parts of carbon disulfide and 60 parts of carbon tetrachloride and stirred until fully dissolved, then heated to the boiling point of the mixed solvent, and the reaction was kept under reflux for 24 hours; after the heating was stopped, the mixed solution was cooled to 0 with ice water. ℃, then add 0.4 parts of triethylamine and 0.3 parts of diethylamine mixture and stir evenly, filter under reduced pressure to remove insoluble catalyst, and remove the solvent from the filtrate under reduced pressure to obtain a crude product of anti-ultraviolet treatment agent; add 250 parts of the crude product to the In dichloromethane, reflux extraction is performed in a Soxhl...

Embodiment 2

[0038] Mix 0.6 parts of octapropenyl silsesquioxane and 1.2 parts of disperse red 60 dye, respectively ground into powders with a particle size of 0.5-1 μm, and add 60 parts of benzene together with 0.15 parts of anhydrous ferric chloride under nitrogen atmosphere. Stir in medium until fully dissolved, then heat up to the boiling point of the mixed solvent, keep warm and reflux for 30 hours; after stopping heating, cool the mixture to 2°C with ice water, then add 1.9 parts of diethylamine, stir evenly, filter under reduced pressure, remove Insoluble catalyst, the filtrate was evaporated under reduced pressure to remove the solvent to obtain the crude product of anti-ultraviolet treatment agent; the crude product was added to 65 parts of methylene chloride and 65 parts of toluene, refluxed in a Soxhlet extractor for 30 hours, and then filtered under reduced pressure, The undissolved original dye is removed, and finally the filtrate is distilled under reduced pressure to obtain a...

Embodiment 3

[0041] Mix 0.6 parts of octabutenyl silsesquioxane and 3.2 parts of disperse yellow 42 dye, which are respectively ground into powders with a particle size of 0.5-1 μm, together with 0.22 parts of anhydrous ferric chloride and 0.23 parts of anhydrous under nitrogen atmosphere. Magnesium chloride was added to 300 parts of carbon disulfide and 200 parts of benzene and stirred until fully dissolved, then heated to the boiling point of the mixed solvent, and the reaction was kept under reflux for 18 hours; after the heating was stopped, the mixture was cooled to 4°C with ice water, and then 1.5 parts of diethyl The mixture of amine and 1.5 parts of dichloromethane was stirred evenly, filtered under reduced pressure to remove the insoluble catalyst, and the filtrate was distilled under reduced pressure to remove the solvent to obtain a crude product of anti-ultraviolet treatment agent; the crude product was added to 450 parts of dichloromethane and 340 parts of trichloromethane In m...

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Abstract

The invention discloses an ultraviolet resistant treatment agent based on disperse dye modification. The general structural formula of the ultraviolet resistant treatment agent is as shown in the specification. Stretching vibration peaks representing Si-O-Si and Si-C respectively appear at 588cm<1>, 1109cm<1> and 782cm<1> positions of an infrared absorption spectrum of the ultraviolet resistant treatment agent, stretching and bending vibration peaks representing -CH2-CH2-, -CH2-CH2-CH2- or -CH2-CH2-CH2-CH2 respectively appear at 3068cm<1>, 2962cm<1> and 1460cm<1> positions of the infrared absorption spectrum of the ultraviolet resistant treatment agent, a vibration peak representing silicon atoms in a POSS (polyhedral oligomeric silsesquioxane) structure appears at a -109.63ppm position of <29>Si NMR (nuclear magnetic resonance) spectrogram, and absorption peaks appear below 300nm wavelength of ultraviolet-visible absorption spectra of solution. The invention further discloses a preparation method of the ultraviolet resistant treatment agent. The ultraviolet resistant treatment agent can be firmly inlaid into a shallow fiber layer by the aid of dye molecules by a high-temperature high-pressure treatment method and fixed onto fibers, durable ultraviolet resistant functions are achieved, and the synthetic fibers can be simultaneously dyed.

Description

technical field [0001] The invention belongs to the technical field of an anti-ultraviolet agent treatment agent and its preparation, in particular to an anti-ultraviolet treatment agent based on disperse dye modification and a preparation method thereof. Background technique [0002] Aromatic high-performance fibers such as wholly aromatic polyamide (aramid) and polyparaphenylene 1,3,4-oxadiazole (p-POD) have excellent physical and mechanical, thermal stability, electrical insulation, Solvent resistance, special electrical conductivity and electroluminescence properties are often used as high temperature resistant filter cloths, permeable membranes and insulating protective materials (Zhang Z, Ye G, Li W, Li T, Xu J. Influence of sulfuric acid bath on morphological structure and mechanicalproperties of poly(p-phenylene-1,3,4-oxadiazole)fibers[J].Journal of AppliedPolymer Science,2009,114(3):1485-1493;Schulz B, Bruma M, Brehmer L. AromaticPoly(1,3,4-Oxadiazoe)s as Advanced ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21C09B1/54C09B51/00D06M13/513D06M23/00D06P3/26D06P1/16D06M101/36
CPCC07F7/21C09B1/547C09B51/00D06M13/5135D06M23/00D06M2101/36D06M2200/25D06P1/16D06P3/004D06P3/26
Inventor 冒亚红管宇
Owner CHENGDU TEXTILE COLLEGE
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