A kind of polyvinylamine-co-acrylonitrile type self-crosslinking dye, its preparation method and application

A polyvinylamine and acrylonitrile technology, applied in dyeing methods, organic dyes, textiles and papermaking, etc., can solve the problems of low light fastness, low fixation rate of cross-linked dyes, complicated dyeing process, etc., and achieve simplified coloring. process, reduce production costs, and solve the effect of complex dyeing process

Active Publication Date: 2015-12-30
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to solve the above problems such as low color fixation rate of cross-linked dyes, low light fastness, complex dyeing process and the need for cross-linking agents, the present invention provides an aminovinyl-acrylonitrile copolymer with amino and cyano groups as the main chain, A macromolecular self-crosslinking dye with a dichloro-s-triazine type small molecule color body is partially introduced into its amino group, and its preparation method is disclosed; the color fixation rate and light fastness of the crosslinking dye prepared by the present invention are good, And no cross-linking agent is needed to fix the color, which simplifies the dyeing process and reduces the cost

Method used

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  • A kind of polyvinylamine-co-acrylonitrile type self-crosslinking dye, its preparation method and application
  • A kind of polyvinylamine-co-acrylonitrile type self-crosslinking dye, its preparation method and application
  • A kind of polyvinylamine-co-acrylonitrile type self-crosslinking dye, its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] In a four-necked flask equipped with a thermometer, reflux condenser and mechanical stirring, add 10 g monomeric N-vinylformamide (NVF), 10 g monomeric acrylonitrile (AN) and N,N-dimethylformamide ( DMF) under nitrogen gas for 30 min with stirring. Raise the temperature to 60°C, add azobisisobutyronitrile (AIBN) with 10% of the total mass of the two monomers under nitrogen protection to initiate polymerization, react for 10 hours, precipitate solids from the reaction solution in water, filter and dry to obtain the product, and the obtained product Infrared spectrum such as figure 1 shown at 2243cm -1 The characteristic peak of cyano group was detected at 1667cm -1 The amide carbonyl absorption peak was detected at 2820cm -1 The aldehyde group absorption peak was detected at , indicating that the copolymerization occurred, and the corresponding non-hydrolyzed polyvinylamine-co-acrylonitrile copolymer was obtained.

[0063] Weigh 10 g of the above-prepared polyvinyla...

Embodiment 2～5

[0065] Preparation of 1#~4# pyrazolone-type small molecule yellow color body:

[0066] Add 1.90g of cyanuric chloride (0.0103mol), 20g of ice and 2mL of water into a 100mL beaker, and beat for 30 minutes. Slowly add 20 mL of an aqueous solution (0.01 mol) containing 1.84 g of m-phenylenediamine monosulfonic acid into the above-mentioned beating liquid dropwise, and the reaction temperature is 0-5°C. During the dropwise addition process, adjust the pH value of the reaction to 4-5 with 10% sodium carbonate solution, and detect the end point of the reaction with thin-layer chromatography (TLC). The developer is isobutanol:n-propanol:ethyl acetate:water=2 :4:1:3, the Rf value of the product is 0.65.

[0067] Add 2.5mL concentrated hydrochloric acid (36%) to the above-mentioned cyanuric chloride condensation product, cool to 0-5°C and add 0.71g sodium nitrite (0.0103mol), the solution after the addition can make the starch potassium iodide test paper turn blue color. After 30 mi...

Embodiment 6～15

[0069] Preparation of 5#~10#, 15#~18# small molecule color bodies:

[0070] The method is the same as that in Example 2, that is, the pyrazolone chromophoric matrix in Example 2 is replaced by the chromophore pyridone, H acid and its derivatives, and J acid to obtain corresponding small molecule chromophores 5# to 10# , 15#~18#, other conditions are consistent with embodiment 2.

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Abstract

The invention provides a polyvinylamine-co-acrylonitrile self-crosslinking dye as well as a preparation method and application thereof and particularly provides a preparation method of a macromolecular self-crosslinking dye formed by partially introducing dichloro-s-triazine micromolecular chromogens to an amino group of an aminoethenyl and acrylonitrile copolymer as a main chain. A macromolecular side chain of the dye contains amino, imide, cyano and dichloro-s-triazine micromolecular chromogens, and the dye has a self-crosslinking characteristic after dyeing fiber. The developed dye is suitable for dyeing cellulosic fiber, free of a crosslinking agent in a dyeing process and capable of reducing the production cost, simplifying the dyeing process and improving the light fastness of the dyed fiber.

Description

technical field [0001] The present invention relates to a dye, in particular to a water-soluble polymer dye whose main chain is a hydrocarbon chain, and the side chain contains a primary amino group and a cyano-reactive group directly connected to the main chain methine group. It particularly relates to a polyvinylamine-co-acrylonitrile type self-crosslinking dye which contains cyano group in molecular structure and retains a chlorine atom on the triazine ring. Background technique [0002] The active groups of reactive dyes are prone to hydrolysis during transportation, storage and dyeing, resulting in the loss of dyes. Due to the hydrolysis of active groups, the loss rate of reactive dyes is between 20% and 50%. These hydrolyzed dyes exist in the dyeing residue, which increases the difficulty of wastewater treatment. It was found that some reactive groups such as -NH 2 ,-SO 2 NH 2 Introduced into the molecular structure of the dye, through the cross-linking reaction be...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B69/10C08F226/02C08F220/44C08F8/00D06P1/00D06P3/60
Inventor 张淑芬唐炳涛
Owner DALIAN UNIV OF TECH
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