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Preparation method of high-efficiency low-cost acidic color fixing agent

An acid color fixing agent, low-cost technology, applied in the preparation of sulfonic acid, preparation of organic compounds, dyeing method, etc., can solve the problems of poor water fastness, high production cost of raw materials, high processing cost, etc., to achieve production cost reduction , Good color fixing effect and less by-products

Active Publication Date: 2021-02-05
WUYI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The acid color fixing agent commonly used in the market is synthesized mainly through the condensation of 4,4'-dihydroxydiphenyl sulfone, 4-hydroxybenzenesulfonic acid and formaldehyde under alkaline conditions; or through the condensation of 4,4'- Dihydroxydiphenylsulfone, acetic anhydride, concentrated sulfuric acid and formaldehyde are condensed polymer products under acidic conditions. Both synthetic routes use 4,4'-dihydroxydiphenylsulfone as raw materials, and require high purity. The purity is required to be above 90-99%. The production of high-purity 4,4'-dihydroxydiphenyl sulfone will produce a large amount of wastewater containing phenol, and the treatment cost is high, resulting in a high production cost of this raw material. Under the strict national environmental protection policy Under the request, the price of 4,4'-dihydroxydiphenyl sulfone has tripled, which is difficult for color-fixing agent manufacturers to accept
In addition, the comprehensive performance of color fixing agents currently on the market is not high, and the fastness to alkali and perspiration is poor, which is difficult to meet the needs of printing and dyeing factories, especially for the current new blister fastness.

Method used

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  • Preparation method of high-efficiency low-cost acidic color fixing agent
  • Preparation method of high-efficiency low-cost acidic color fixing agent
  • Preparation method of high-efficiency low-cost acidic color fixing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] This embodiment provides a method for preparing an acidic color fixing agent with high efficiency and low cost, comprising the following steps:

[0033] The first step intermediate synthesis:

[0034] Sulfonation reaction: phenol: 188g (2mol); concentrated H 2 SO 4 : 200g (2.04mol);

[0035] Sulfonation reaction: phenol: 178.6g (1.9mol);

[0036] Synthetic steps:

[0037] (1) Put 188g of phenol into a four-necked flask, heat up to 95°C, and slowly add 200g of concentrated H 2 SO 4 , control the dropping speed, so that the temperature is controlled at 95-100 °C, after the dropping is completed, start the heat preservation timer for 3 hours, record the temperature every 30 minutes, and observe the experimental phenomenon;

[0038] (2) The sulfonation is finished, and the acidity is measured, and the correct value is 27;

[0039] (3) Raise the temperature to 130°C, add 89.3g of phenol and continue to heat up to 165°C, start the heat preservation timer, start vacuumi...

Embodiment 2

[0047] This embodiment provides a method for preparing an acidic color fixing agent with high efficiency and low cost, comprising the following steps:

[0048] The first step intermediate synthesis:

[0049]Sulfonation reaction: phenol: 200g; concentrated H 2 SO 4 : 210g;

[0050] Sulfonation reaction: phenol: 188.6g;

[0051] Synthetic steps:

[0052] (1) Put 200g of phenol into a four-neck flask, heat up to 95°C, and slowly add 210g of concentrated H 2 SO 4 , control the dropping speed, so that the temperature is controlled at 95-100 °C, after the dropping is completed, start the heat preservation timer for 3 hours, record the temperature every 30 minutes, and observe the experimental phenomenon;

[0053] (2) The sulfonation is finished, and the acidity is measured, and the correct value is 27;

[0054] (3) Heat up to 130°C, add 94.3g of phenol and continue to heat up to 165°C, start the heat preservation timer, start vacuuming after 20 minutes, increase the vacuum de...

Embodiment 3

[0062] This embodiment provides a method for preparing an acidic color fixing agent with high efficiency and low cost, comprising the following steps:

[0063] The first step intermediate synthesis:

[0064] Sulfonation reaction: phenol: 180g; concentrated H 2 SO 4 : 195g;

[0065] Sulfonation reaction: phenol: 170g;

[0066] Synthetic steps:

[0067] (1) Put 180g of phenol into a four-necked flask, heat up to 95°C, and slowly add 195g of concentrated H 2 SO 4 , control the dropping speed, so that the temperature is controlled at 95-100 °C, after the dropping is completed, start the heat preservation timer for 3 hours, record the temperature every 30 minutes, and observe the experimental phenomenon;

[0068] (2) The sulfonation is finished, and the acidity is measured, and the correct value is 28;

[0069] (3) Raise the temperature to 130°C, add 85g of phenol and continue to heat up to 165°C, start the heat preservation timer, start vacuuming after 20 minutes, increase ...

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Abstract

According to the preparation method, phenol, concentrated sulfuric acid and formaldehyde are used as raw materials to synthesize an intermediate, 4, 4'-dihydroxy diphenyl sulfone and 4-hydroxy benzenesulfonic acid are used as main mixtures, the pH value is adjusted to 8-9 by using an alkaline substance, a 37% formaldehyde solution is added for a condensation reaction to obtain the acidic color fixing agent, and acetic acid is used for adjusting the acid when the acidic color fixing agent is used. The acidic color fixing agent prepared by the method has the advantages of short synthesis route,no need of purification of the produced intermediate, low manufacturing cost, and satisfaction of market demands on use performance, can save cost for printing and dyeing enterprises, can greatly reduce sewage discharge, especially phenol-containing sewage discharge, and has the advantages of energy saving and emission reduction. The acid color fixing agent synthesized by the invention is small incolor change, the soaping fastness can reach 4-5 level, especially the alkali perspiration fastness can reach 4 level or above, and the acid color fixing agent can completely replace an acid color fixing agent prepared by a condensation reaction method of high-purity 4, 4'-dihydroxy diphenyl sulfone, 4-hydroxy benzenesulfonic acid and the formaldehyde solution.

Description

technical field [0001] The invention relates to the technical field of acidic color fixing agents, in particular to a preparation method of an acidic color fixing agent with high efficiency and low cost. Background technique [0002] Acid color fixing agent is mainly used to improve the wet treatment fastness of acid dyes, acid mordant dyes dyed nylon, nylon / spandex fabrics, generally it includes color fastness to soaping, color fastness to water stains, color fastness to acid perspiration Degree, color fastness to alkali perspiration, color fastness to chlorine, color fastness to rubbing and color fastness to sea water. Acid dyes are dyed on nylon, nylon / spandex fabrics, mainly under acidic conditions, the terminal amino groups of nylon and nylon / spandex fibers absorb hydrogen ions to become cationic, and acid dyes are anionic, and are adsorbed by anions and cations On nylon, nylon / spandex fabrics, this acid dye, which is adsorbed on the fabric through anionic and cationic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C08G8/08C08G8/10D06P5/08C07C315/00C07C317/22C07C303/06C07C309/42
CPCC08G8/28C08G8/08C08G8/10D06P5/08C07C315/00C07C303/06C07C309/42C07C317/22
Inventor 李峥嵘刘昊吴均鑫王康康黄钢李养令郑丹纯唐秋杏张浩峰邹洁
Owner WUYI UNIV
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