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A kind of preparation method of acid dye fixing agent

A technology of acid dyes and fixatives, applied in dyeing, textile and papermaking, etc., can solve the problems of troublesome production, low dyeing rate of reactive dyes, pungent acetic acid smell of fixatives, etc. Control, easy to adjust and control, excellent fixation effect

Active Publication Date: 2020-05-26
约克夏染料(中山)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Acid dyes have complete chromatograms, bright colors, and high dyeing rate. They are often used for dyeing nylon and protein fibers, but the molecular weight of acid dyes is small, and there are water-soluble groups such as carboxylic acid or sulfonic acid groups in the molecular structure. The wet fastness of the dyed fabric is very poor
[0003] There are generally three solutions to the problem of poor wet fastness of acid dyes. One is to let the dyes and metal salts (copper ions, chromium ions, antimony ions, etc.) form acid complex dyes, and then use them for fabric dyeing. The method effectively improves the wet fastness of acid dyes, and has been widely used in the early stage, especially in the dyeing of wool. However, as people pay more and more attention to environmental protection and health, the impact of complex dyes on the environment and human health is also increasing. It is becoming more and more prominent, which limits the development of acid complex dyes to a large extent; the second is to use reactive dyes instead of acid dyes for dyeing. This method can also better improve the wet color fastness of nylon and protein fibers. It is widely used on wool fabrics, but the dyeing rate of reactive dyes is not high, the dyeing process requires a large amount of electrolyte, and the color brightness and dyeing depth are not as good as acid dyes. These shortcomings limit the use of reactive dyes on nylon and protein fibers, especially It is nylon fiber; the third is that after the fabric is dyed with acid dyes, it is post-treated with a color-fixing agent to improve its wet fastness, which is currently the most widely used and common method
European Patent No. EP 1096058A2 discloses a method for synthesizing tannin color fixing agent: mixing 4,4'-dihydroxydiphenylsulfone (bisphenol S), phenylsulfonesulfonic acid, sodium hydroxide, and formaldehyde Afterwards, the high-molecular polymer is obtained by condensation reaction under high temperature conditions above 100°C for a period of time. The raw materials of this synthesis method are easy to obtain and the process is simple, but the pH is high and it is not easy to be adjusted down. The color fixing agent can be obtained when applied to nylon fabrics Good effect, but the effect is poor on nylon / spandex blended fabrics; the US Patent No. US4147512 has announced a synthetic method for synthesizing tannin: bisphenol S reacts with concentrated sulfuric acid in acetic anhydride to generate sulfonated bisphenol phenol S, and then condense with formaldehyde to obtain hydrophilic phenolic resin. Drug-making items, stricter control, will bring some troubles to the production and will make the synthetic color fixing agent have a pungent acetic acid smell

Method used

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  • A kind of preparation method of acid dye fixing agent
  • A kind of preparation method of acid dye fixing agent
  • A kind of preparation method of acid dye fixing agent

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preparation example Construction

[0029] A preparation method of an acid dye fixing agent, specifically comprising the following steps:

[0030] a. Synthesis of sulfonated phenols: Add metered phenols and concentrated sulfuric acid into a reaction kettle with a stirrer, reflux condenser and thermometer, stir and heat to 110-140°C, and keep warm for 2-3 hours to obtain Brown-red sulfonated phenols, cooled to room temperature, and left to stand for use;

[0031] b, pre-condensed part of phenols: add metered phenols and organic solvent to another reaction kettle with stirrer, reflux condenser and thermometer, stir until completely dissolved and then add metered concentration of 37wt% formaldehyde solution and concentrated sulfuric acid, heat up to 90-100°C, keep warm for 2-3 hours, and cool down to 70-80°C;

[0032] c. Polycondensation color-fixing agent: add the product of step b into the reaction kettle of step a, stir and heat up (there may be solid precipitation at this time), as the reaction progresses, the...

Embodiment 1

[0035] Add 250g of bisphenol S and 200g of concentrated sulfuric acid into a 2L reaction kettle equipped with a stirrer, reflux condenser and thermometer, heat to 125°C while stirring, keep warm for 3.5 hours to obtain sulfonated bisphenol S, cool to room temperature, and statically put aside;

[0036] Add 140g of bisphenol S and 280g of n-butanol into another 1L reaction kettle with agitator, reflux condenser and thermometer, stir to make it dissolve completely, then add 110g of 37% formaldehyde solution and 20g of concentrated sulfuric acid, and heat up to 100 ℃, keep warm for 2 hours, then cool down to 80℃;

[0037] Pour the product in the second step into the reaction kettle of the first step, stir and heat up (solids will precipitate out at this time), as the reaction progresses, the system gradually becomes transparent and the viscosity increases slowly, keeping the final temperature at 100 React at -105°C for 6 hours, cool down and discharge.

Embodiment 2

[0039] Add 250g of bisphenol S and 200g of concentrated sulfuric acid into a 2L reaction kettle equipped with a stirrer, reflux condenser and thermometer, heat to 120°C while stirring, keep warm for 3 hours to obtain sulfonated bisphenol S, cool to room temperature, and statically put aside;

[0040] Add 160g of bisphenol S and 300g of n-butanol into another 1L reaction kettle with a stirrer, reflux condenser and thermometer, stir to make it completely dissolve, then add 120g of 37% formaldehyde solution and 20g of concentrated sulfuric acid, and heat up to 100 ℃, keep warm for 2 hours, then cool down to 80℃;

[0041] Pour the product in the second step into the reaction kettle of the first step, stir and heat up (solids will precipitate out at this time), as the reaction progresses, the system gradually becomes transparent and the viscosity increases slowly, keeping the final temperature at 100 React at -105°C for 5 hours, cool down and discharge.

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Abstract

The invention discloses a preparation method of an acid dye color fixing agent. The preparation method comprises the following steps of enabling concentrated sulfuric acid to sulfonate one part of phenolic substance, so as to obtain the phenolic substance with sulfonic group; concentrating the other part of phenolic substance and formaldehyde in an organic solvent under the condition of acid neutralizing and catalyzing, so as to obtain a precondensate; mixing the products, and performing condensation reaction, so as to obtain a viscous color fixing agent. The preparation method has the advantages that the acid dye color fixing agent is synthesized by three steps; one part of phenolic substance firstly generates the sulfonating reaction with the concentrated sulfuric acid, the product generates the condensation reaction with the other part of sulfonated phenol and the formaldehyde in the organic solvent, the sulfonating degree and water dissolvability of the final product are controlled, and the color fixing effect of the final product is adjusted; the use of acetic anhydride is avoided, the synthesized product has no irritative odor of acetic acid, the final pH (potential of hydrogen) value of the product can be easily adjusted and controlled, the influence to the water dissolvability of the product is avoided, and the acid dye color fixing agent can be directly applied to thecolor fixing of chinlon and chinlon / spandex fabrics.

Description

【Technical field】 [0001] The invention relates to a preparation method of an acid dye fixing agent, belonging to the technical field of textile auxiliaries. 【Background technique】 [0002] Acid dyes have complete chromatograms, bright colors, and high dyeing rate. They are often used for dyeing nylon and protein fibers, but the molecular weight of acid dyes is small, and there are water-soluble groups such as carboxylic acid or sulfonic acid groups in the molecular structure. The wet fastness of the dyed fabric after dyeing is very poor. [0003] There are generally three solutions to the problem of poor wet fastness of acid dyes. One is to let the dyes and metal salts (copper ions, chromium ions, antimony ions, etc.) form acid complex dyes, and then use them for fabric dyeing. The method effectively improves the wet fastness of acid dyes, and has been widely used in the early stage, especially in the dyeing of wool. However, as people pay more and more attention to environ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D06P5/08D06P1/39C08G8/24
CPCC08G8/24D06P1/39D06P5/08
Inventor 李峥嵘邹洁李不韪张鑫宇冉巍巍张智慧
Owner 约克夏染料(中山)有限公司
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