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Azo structure carboxylic amide type dyes for polylactic acid fiber dyeing and preparation method thereof

A technology of polylactic acid fiber and carboxamide type, applied in the field of azo-structure carboxamide type dyes and its preparation, can solve the problems of poor dye uptake and color fastness, and achieve favorable dye uptake and color fastness , increase the dipole force, the effect of simple synthesis process

Inactive Publication Date: 2012-05-09
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] To sum up, polylactic acid (PLA) fiber belongs to a relatively new type of polyester fiber, and many disperse dyes with good dyeing results on PET fibers have poor dyeing rate and color fastness on PLA fibers.

Method used

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  • Azo structure carboxylic amide type dyes for polylactic acid fiber dyeing and preparation method thereof
  • Azo structure carboxylic amide type dyes for polylactic acid fiber dyeing and preparation method thereof
  • Azo structure carboxylic amide type dyes for polylactic acid fiber dyeing and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1, a kind of preparation method of azo structure carboxamide type dyestuff for polyester fiber dyeing, carries out following steps successively:

[0039] 1) Add 3.2g of 1-phenyl-3-methyl-4-(4'-carboxyphenylhydrazone)-5-pyrazole into a three-necked flask equipped with a thermometer, reflux condenser and mechanical stirring device Linone, 20ml benzene, 0.2ml DMF, 2.2ml thionyl chloride, heated to 60°C, reacted for 2h;

[0040] 2) After the reaction is complete, heat the reaction liquid to 90°C, evaporate excess thionyl chloride and solvent under reduced pressure, cool to room temperature, transfer to ice water, filter, wash with ice water until the filtrate is neutral, and dry in vacuum After obtaining the carboxylic acid chloride intermediate;

[0041] 3) In a three-neck flask equipped with a stirrer, a thermometer, and a condenser tube, first add 3.4g of carboxylic acid chloride intermediate and 25ml of acetone as a solvent, and after the carboxylic acid chl...

Embodiment 2

[0043] Embodiment 2, a kind of preparation method of azo structure carboxamide type dyestuff for polyester fiber dyeing, carry out following steps successively:

[0044] 1) Add 6.4g of 1-phenyl-3-methyl-4-(4'-carboxyphenylhydrazone)-5-pyrazole into a three-necked flask equipped with a thermometer, reflux condenser and mechanical stirring device Linone, 60ml benzene, 0.6ml DMF, 6ml thionyl chloride, heated up to 55°C, and reacted for 6h;

[0045] 2), with embodiment 1;

[0046] 3), add 3.4g carboxylic acid chloride intermediate and 25ml of acetone as solvent in the there-necked flask equipped with agitator, thermometer and condenser, after the carboxylic acid chloride intermediate is dissolved in acetone, add 0.87g n-pentylamine and 1.38g powdered K 2 CO3, mixed and stirred at room temperature for 1 hour;

[0047] 4), with embodiment 1, obtain carboxyl n-pentylamine type dye.

Embodiment 3

[0048] Embodiment 3, a kind of preparation method of azo structure carboxamide type dyestuff for polyester fiber dyeing, carry out following steps successively:

[0049] 1) Add 6.4g of 1-phenyl-3-methyl-4-(4'-carboxyphenylhydrazone)-5-pyrazole into a three-necked flask equipped with a thermometer, reflux condenser and mechanical stirring device Linone, 50ml benzene, 0.8ml DMF, 5.5ml thionyl chloride, heated up to 55°C, reacted for 3h;

[0050] 2), with embodiment 1;

[0051] 3), first add 3.4g of carboxylic acid chloride intermediate and 25ml of acetone as solvent in the there-necked flask equipped with agitator, thermometer and condenser tube, after the carboxylic acid chloride intermediate is dissolved in acetone, then add 1.0g of n-hexylamine and 2.5 g powdered K 2 CO 3 , mixed and stirred at room temperature for 1 hour,

[0052] 4), with embodiment 1, get carboxyl n-hexylamine type dye.

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Abstract

The invention discloses a carboxamide type dye which has an azo structure and is used for dyeing polylactic acid fibre. The molecular structure contains a carboxamide group; the general structural formula of the dye is shown above. In the formula, D is a chromogen with the azo structure; m is 1 or 2; X is H or n-CnH2n+1; Y is H, n-CnH2n+1, C6H12 or C6H6; and in the n-CnH2n+1, n meets the following condition: n is more than or equal to 1 and less than or equal to 18, and n is an integer. The invention simultaneously discloses a method for preparing the dye. The dye is used to improve the rate of dye-uptake and color fastness on the PLA fibre.

Description

technical field [0001] The invention relates to an azo-structure carboxamide type dye suitable for dyeing polylactic acid fibers and a preparation method thereof. Background technique [0002] Polyester fibers mainly include polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT), polybutylene terephthalate (PBT) and emerging polylactic acid (PLA) fibers , this type of fiber usually has high crystallinity, and there is no strong hydrophilic group in the main chain of the molecule, so it is hydrophobic. After the polyester fiber is spun and stretched and preheated, there is a molecular layer on the surface that is oriented and difficult to penetrate, and the molecular structure lacks active groups that combine with dyes, so it is difficult to dye. The molecules of polyester fibers are arranged neatly. When the temperature is low, the movement of macromolecular segments is inactive and the gaps are small; in addition, the molecules of disperse dyes suitable for...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B26/02C09B43/40C09B29/01C09B29/50D06P3/54D06P1/18
Inventor 崔志华陈维国郑今欢胡恩岭许建华
Owner ZHEJIANG SCI-TECH UNIV
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