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Environmental response type cationic polymer for active dye salt-free dyeing and preparation method thereof

A cationic polymer, salt-free dyeing technology, applied in the field of textile chemistry and dyeing and finishing engineering, to achieve high commercialization potential, reduced sensitivity, and the effect of solving uneven dyeing

Active Publication Date: 2017-03-15
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide an environment-responsive cationic polymer and a preparation method thereof for salt-free dyeing of reactive dyes. By screening suitable responsive monomers, alkyl halides are used as initiators, ascorbic acid, Glucose and other biological agents are used as reducing agents, and the ppm-level high-valent metal halides and nitrogen-containing ligands are used as catalysts for polymerization, and then modified by quaternization to prepare environment-responsive cationic polymers; the quaternization obtained by this method The molecular weight of the polymer is controllable, the molecular weight distribution is narrow, and the percentage content of quaternary ammonium salt can be effectively controlled. When it is used for cationic modification of cellulose fiber, it can improve the problems of poor level dyeing and uneven shade of modified cotton fiber. high commercial potential

Method used

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  • Environmental response type cationic polymer for active dye salt-free dyeing and preparation method thereof
  • Environmental response type cationic polymer for active dye salt-free dyeing and preparation method thereof
  • Environmental response type cationic polymer for active dye salt-free dyeing and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Glucose (0.05mmol) was dissolved in 10ml ethyl acetate at room temperature, and monomer DEAEMA (25mmol), catalyst CuBr 2 (0.05mmol) and complexing agent PMDETA (1mmol) were added to a 100mL reaction eggplant bottle in turn, and the initiator ECP (64μL) was added under nitrogen protection. Magnetic stirring to make it fully mixed, repeated freezing and vacuuming three times, passing nitrogen gas, reacting in an oil bath at 25°C for 60 minutes, taking out the reaction eggplant bottle and adding ethyl acetate to dilute, then passing the reaction solution in the bottle through a neutral alumina column, The Cu complex in the reaction system was removed, and the filtrate was distilled under reduced pressure to remove the ethyl acetate solvent, precipitated in cold petroleum ether, and dried in vacuum to constant weight to obtain a colorless and transparent polymer product PDEAEMA polymer, which was dissolved in an appropriate amount of Freeze-dry in 1,4-dioxane for later use....

Embodiment 2

[0037] Take ascorbic acid (0.05mmol) and dissolve in 20ml tetrahydrofuran at room temperature, then monomer DMAEMA (25mmol), catalyst CuCl 2 (0.05mmol), complexing agent PMDETA (0.8mmol) were sequentially added to a 100mL reaction eggplant bottle, and the initiator EBiB (64μL) was added under nitrogen protection. Magnetic stirring to make it fully mixed, repeated freezing and vacuuming three times, passing nitrogen gas, reacting in an oil bath at 100°C for 60 minutes, taking out the reaction eggplant bottle and adding tetrahydrofuran to dilute, passing the reaction solution in the bottle through a neutral alumina column to remove the reaction solution. Cu complex in the system, the filtrate was distilled under reduced pressure to remove the tetrahydrofuran solvent, precipitated in cold petroleum ether, and dried in vacuum to constant weight to obtain a colorless and transparent polymer product, which was dissolved in an appropriate amount of 1,4-dioxane Freeze dry in a ring fo...

Embodiment 3

[0040] Get initiator p-TsCl (64 μ L) to be dissolved in 10ml ethyl acetate at room temperature, then add reducing agent AA (0.05mmol) successively to reaction eggplant bottle, complexing agent PMDETA (1.2mmol), solvent ethyl acetate ( 10ml), monomer DMAEMA (25mmol) and catalyst CuCl 2 (0.5 mmol). Magnetic stirring to make it fully mixed, repeated freezing and vacuuming twice, passing nitrogen gas, reacting in an oil bath at 60°C for 60 minutes, taking out the reaction eggplant bottle and exposing it to air to terminate the reaction, passing the reaction solution in the bottle through a neutral alumina column , to remove the Cu complex in the reaction system, the filtrate was distilled under reduced pressure to remove the organic solvent, precipitated in cold petroleum ether, and dried in vacuo to constant weight to obtain a colorless transparent polymer product, which was dissolved in an appropriate amount of 1,4- Freeze-dry in dioxane for later use.

[0041] Add 1g of PDMAE...

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Abstract

The invention relates to an environmental response type cationic polymer for active dye salt-free dyeing and a preparation method thereof. The polymer has the structure (the structure is shown in the description), wherein R1 is CH3 or CH2CH3, R2 is CH3 or phenyl, n ranges from 40 to 1,000, and p ranges from 20% to 70%. The preparation method comprises the steps that an ATRP initiating agent, a monomer, a nitrogen-containing ligand, a catalyst and a reducing agent are mixed in a solvent, reacting is conducted for 0.5 h to 15 h at the temperature of 20 DEG C to 100 DEG C under the oxygen-free condition, then the system is inactivated, impurities and the solvent are removed, and precipitating and drying are conducted to obtain a response type polymer; the polymer is dissolved into an organic solvent, a quaternization reagent is dropwise added, reacting is conducted for 24 h to 48 h at the temperature of 20 DEG C to 100 DEG C, impurities are removed, drying is conducted, and the environmental response type cationic polymer is obtained. The environmental response type cationic polymer which is controllable in molecular weight and uniform in molecular weight distribution is used for salt-free dyeing, so that the problems that modified cotton fiber is poor in levelling property and uneven in color light are solved, and high commercial potential is achieved.

Description

technical field [0001] The invention belongs to the fields of textile chemistry and dyeing and finishing engineering, in particular to an environment-responsive cationic polymer used for salt-free dyeing of reactive dyes and a preparation method thereof. Background technique [0002] The traditional salt dyeing process of reactive dyes needs to add a large amount of inorganic salts to eliminate the electrostatic repulsion between anionic reactive dyes and cotton fibers, and improve the dyeing rate and color fixing rate. After dyeing, inorganic salts remain in the dyeing wastewater and are difficult to degrade. The burden of wastewater treatment is heavy and it is easy to cause environmental pollution. Cationic modification of cotton fibers can effectively improve the affinity between cotton fibers and reactive dyes, improve the dyeing rate and fixation rate of reactive dyes, so as to achieve the purpose of reducing or not using inorganic salts during dyeing. [0003] Howeve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/34C08F8/44D06P1/38D06P1/52D06P3/66
CPCC08F8/44C08F120/34C08F2438/01C08F2500/03D06P1/38D06P1/5257D06P3/66
Inventor 蔡再生王俊崔培红阚逸青
Owner DONGHUA UNIV
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