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Method for preparing naphthalene series additive from low-acidity process waste water

A low-acidity, wastewater technology, applied in chemical instruments and methods, water/sewage multi-stage treatment, water/sludge/sewage treatment, etc., can solve the problems of waste, unused effective components of process wastewater, and high treatment costs. To achieve the effect of saving consumption, reducing subsequent treatment costs and saving water resources

Inactive Publication Date: 2013-06-12
通辽市龙盛化工有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In chemical production, especially in the production of dyes and their intermediates, a large amount of acid-containing process wastewater is often produced. At present, most manufacturers adopt first treatment before discharge, such as chemical oxidation method, coagulation precipitation method, adsorption method reported in the literature. method, electrochemical method, biochemical method, etc. to discharge after treatment. The above-mentioned methods not only have high treatment costs, but also do not utilize the active ingredients in the process wastewater, resulting in waste; in addition, there are also literatures on the recycling of the process wastewater. However, it is only limited to the reuse and washing of the same type of products, and there is no report on the synthesis of auxiliary agents for this process wastewater

Method used

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  • Method for preparing naphthalene series additive from low-acidity process waste water
  • Method for preparing naphthalene series additive from low-acidity process waste water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 256 grams of industrial naphthalene and place it in a reactor, heat up to 100°C to 120°C, slowly add 224 grams of 105% sulfuric acid (oleum) dropwise, heat up and control it at 160°C to 165°C for sulfonation reaction 2 hour, cool down to 110°C, add C.I. disperse blue 79 dyes to prepare the process wastewater (through biochemical and oxidation treatment) produced by the filtration and washing process, adjust the acidity of the reaction system material at 25% to 29%, and control the temperature at 110°C to carry out the hydrolysis reaction for 0.5 hour, after the hydrolysis reaction was completed, then add the above-mentioned process wastewater to adjust the acidity of the reaction system material to be 22%~27%, then add 160 grams of formaldehyde solution of 37% (w / w) in the reactor to carry out the condensation reaction, and the temperature is controlled at 105 ~110°C, condensation time 7 hours, lower the temperature to below 80°C, add 30% (w / w) liquid caustic dropw...

Embodiment 2

[0018] Add 173.9 grams of industrial naphthalene and 82.4 grams of methylnaphthalene to the reactor, heat up to 100-120°C, slowly add 225.8 grams of 105% sulfuric acid (oleum) dropwise, heat up and control it at 160-165°C for sulfonation reaction 2.5 Hour. Cool down to 110°C after the reaction is over, add C.I. Process waste water (acidity is 11.51%, chloride ion content is 0.28%) produced in the preparation process of C.I. ℃~115℃ for 0.5 hours of hydrolysis reaction, after the hydrolysis reaction is completed, then add the above process wastewater to adjust the acidity of the reaction system material to 23~27%, then add 161 grams of 37% formaldehyde solution dropwise in the reactor to carry out condensation reaction, temperature control Condensation reaction at 105-110°C for 5 hours, lower the temperature to below 80°C, add 30% (w / w) liquid alkali dropwise to adjust the pH value to 7-9, and stir for 1 hour to obtain the naphthalene-based water reducer.

Embodiment 3

[0020] Add 128 grams of industrial naphthalene to the reactor, raise the temperature to 130°C, slowly add 89 grams of 98% sulfuric acid and 18 grams of sulfur trioxide dropwise while stirring, raise the temperature to about 160°C for sulfonation reaction for 3 hours, and cool down after the reaction To 110 DEG C, add the process waste water (acidity is 8.61%, chloride ion content is 0.27%) that C.I. Disperse Orange 30 dyestuff preparation process produces, adjust reaction system material acidity at 24%~27%, carry out hydrolysis at 110 DEG C for 45 minutes, After the hydrolysis, add the above-mentioned process wastewater to adjust the acidity of the reaction system material to 21-25%, then add 82.2 grams of 37% formaldehyde solution dropwise, control the temperature at 105-110°C for 4 hours, and start to cool down to about 80°C Add 30% (w / w) liquid alkali dropwise to adjust the pH value to 7-9, and stir for 30 minutes to obtain the naphthalene-based water reducer.

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Abstract

The invention provides a method for preparing a naphthalene series additive from low-acidity process waste water. The method comprises the following steps of: firstly, carrying out a sulfonation reaction on naphthalene or naphthalene series derivatives at the temperature of 80-200DEG C in the presence of a sulfonating agent; secondly, after the sulfonation reaction is ended, adding the low-acidity process waste water and carrying out a hydrolysis reaction at the temperature of 100-130DEG C under the condition that the total acidity of a reaction system is controlled to be 20-30 percent; and thirdly, after the hydrolysis is ended, adding formaldehyde, raising the temperature and controlling the temperature to be 100-150DEG C for a condensation reaction, adding the low-acidity process wastewater in the condensation process and adjusting the acidity of a material system to be 10-30 percent; and after the condensation is ended, adding an alkali liquor and adjusting the pH value to be 5-9to obtain the naphthalene series additive. According to the method disclosed by the invention, dye and process waste water in the preparation process of a dye intermediate can be recycled; the subsequent treatment cost can be reduced; the consumption of the sulfonating agent in the preparation process of the naphthalene series additive can be reduced; the production cost is reduced; meanwhile, the addition amount of fresh water in the condensation reaction of the naphthalene series additive is reduced, so that water resources are saved; and better economic benefit and social benefit are obtained.

Description

(1) Technical field [0001] The invention relates to a method for recycling low-acidity process wastewater, in particular to a method for preparing naphthalene-based additives from low-acidity process wastewater. (2) Background technology [0002] In chemical production, especially in the production of dyes and their intermediates, a large amount of acid-containing process wastewater is often produced. At present, most manufacturers adopt first treatment before discharge, such as chemical oxidation method, coagulation precipitation method, adsorption method reported in the literature. method, electrochemical method, biochemical method, etc. to discharge after treatment. The above-mentioned methods not only have high treatment costs, but also do not utilize the active ingredients in the process wastewater, resulting in waste; in addition, there are also literatures on the recycling of the process wastewater. It is reported, but only limited to the recycling washing of the same...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B24/20C04B24/22C02F9/04C04B103/30
Inventor 高怀庆余青结张海斌钟玉霞蒋应海
Owner 通辽市龙盛化工有限公司
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