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Environment-friendly type preparing method for H2O2 low-temperature bleaching assistant

A kind of H2O2, environment-friendly technology, applied in the direction of sulfonic acid preparation, organic chemistry, etc., to achieve the effect of simple and easy to obtain raw materials, simple operation and high product yield

Inactive Publication Date: 2008-10-29
HUZHOU ZHILI CHILDRENS CLOTHING DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solve the shortcomings of using organic solvents xylene and tetrahydrofuran as reaction solvents in the existing synthesis methods, and realize the environmental protection requirements of the synthesis process

Method used

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  • Environment-friendly type preparing method for H2O2 low-temperature bleaching assistant
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  • Environment-friendly type preparing method for H2O2 low-temperature bleaching assistant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～9

[0027] Add 15.82g (0.1mol) isononanoic acid in the there-necked flask that reflux condenser, constant pressure dropping funnel and thermometer are housed, start to stir, slowly drip the sulfur oxychloride ( See Table 1 for details), control the rate of addition to complete the dropwise addition in about 1 hour; allow it to react for 30 minutes, then raise the temperature to 40°C for reflux reaction for 2.5 hours. Then carry out normal pressure distillation to remove excess thionyl chloride, and vacuum distillation collects the product isononanoyl chloride. The test results are shown in Table 1.

[0028] Table I

[0029]

[0030] 2. The influence of reaction temperature on the synthesis of isononanoyl chloride

Embodiment 10～15

[0032] Add 15.82g (0.1mol) isononanoic acid to a three-necked flask equipped with a reflux condenser, a constant pressure dropping funnel and a thermometer, start stirring, and slowly add 15.47g (0.13mol) thionyl chloride dropwise at room temperature to control the rate of addition The dropwise addition was completed in about 1 hour; after allowing it to react for 30 minutes, the temperature was raised to the temperature shown in Table 2 for reflux reaction for 2.5 hours. Then carry out normal pressure distillation to remove excess thionyl chloride, and vacuum distillation collects the product isononanoyl chloride. The test results are shown in Table II.

[0033]

[0034] 3. The influence of the amount ratio of raw materials on the synthesis of sodium nonanoyl chloride benzene sulfonate

Embodiment 16～21

[0036] Prepare a certain amount of lye with a pH value of 11 with the mixture of sodium hydroxide, sodium carbonate, and sodium bicarbonate with the same mass fraction and volume ratio of 1:4:1, and 1.96g (0.01mol) of p-hydroxybenzenesulfonic acid Sodium was added wherein, stirred and dissolved, then added 5% phase-transfer catalyst tetrabutylammonium bromide, continued to stir for 5 minutes and then added dropwise nonanoyl chloride (see Table 3) in different molar ratios with sodium p-hydroxybenzenesulfonate, and the reaction Carried out at normal temperature (25°C). After reacting for 40 minutes, the reaction solution was evaporated by rotary evaporation, centrifugally filtered and vacuum-dried to obtain the product sodium isononanoyloxybenzenesulfonate.

[0037] Table three

[0038]

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PUM

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Abstract

The invention relates to an environmentally friendly preparation method of a series of H2O2 low temperature bleaching assistants. The assistant is mainly composed of acyloxybenzene sulfonate (AOBS) salts. The preparation method is characterized in that no common toxic or explosive organic synthesis solvents such as tetrahydrofuran and xylene are used by controlling reaction conditions, so as to ensure no toxicity and good safety during synthetic process, and meet environmentally friendly requirements of synthetic process. The series of H2O2 low temperature bleaching assistants are prepared by reaction of organic carboxylic acids (including linear chain carboxylic acids and branch chain carboxylic acids) and acylating agents such as phenolsulfonate and thionyl chloride under specific conditions, and by means such as atmospheric distillation, vacuum distillation, rotary evaporation and vacuum drying. The inventive method has the advantages of easily accessible raw materials, high utilization rate of raw materials, easily fulfilled reaction conditions, short reaction time, low cost, easy operation, and high product yield.

Description

technical field [0001] The invention relates to the field of textile auxiliaries, in particular to a H 2 o 2 The preparation method of low-temperature bleaching assistants. Background technique [0002] Hydrogen peroxide, also known as hydrogen peroxide, is a strong oxidizing bleach. The effect of hydrogen peroxide bleaching and the stability after bleaching are good, the whiteness is pure, it will not make the fabric yellow, and it is non-toxic, odorless, and has little environmental pollution. It is suitable for bleaching of various fibers and their blended fabrics. Moreover, it has no corrosive effect on equipment and is suitable for large-scale industrial production. In the development of a new process of chlorine-free bleaching H 2 o 2 has become one of the most important bleaching [0003] There are also certain problems in the practical application of hydrogen peroxide bleaching. Generally, the hydrogen peroxide bleaching of textiles needs to be carried out at a...

Claims

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Application Information

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IPC IPC(8): C07C309/42C07C303/02
Inventor 邵建中王锋夏敏董利敏黄益
Owner HUZHOU ZHILI CHILDRENS CLOTHING DEV
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