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Preparation method of low-stain dispersant MF

A dispersant and staining technology, which is applied in the preparation of sulfonic acid, sulfonate, organic chemistry, etc., can solve the problems of serious staining, deep color of MF, etc., achieve easy control of reaction conditions, and improve the degree of sulfonation , good thermal stability

Active Publication Date: 2019-04-05
ZHEJIANG LONGSHENG CHEM RES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The MF obtained by conventional methods is not only dark in color, but also has serious staining properties

Method used

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  • Preparation method of low-stain dispersant MF
  • Preparation method of low-stain dispersant MF

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Sulfonation: Add 71g (0.5mol, all calculated as methylnaphthalene, the same below) of methylnaphthalene to the four-necked flask, and start to add 60g (0.6mol) of 98% sulfuric acid dropwise after the material is heated to 100°C , control the dropping temperature at 115°C, and control the acid dropping time at 20-30min. After the dropwise addition, the temperature was raised to 121° C. and kept at this temperature for 3 hours. At the end of the reaction, 15 g of water was added to control the acidity of the feed solution at 30%, to obtain the sulfonated feed.

[0027] 2. Condensation: adjust the acidity of the sulfonated material to 24.5% by adding 30g of water. After the temperature of the material drops to 85°C, start to add 27g (0.32mol) of 37% formaldehyde solution dropwise. , and kept at this temperature for 3.5h.

[0028] 3. Neutralization: Add 75g of water to the condensed material after heat preservation and stir evenly, then pre-neutralize with 15g of lime, ...

Embodiment 2

[0030] 1. Sulfonation: Add 75g (0.53mol) of methylnaphthalene to a four-necked flask, and when the temperature of the material rises to 100°C, start to add 65g (0.65mol) of 98% sulfuric acid dropwise, and control the dropping temperature to 125°C. The time is controlled at 20-30min. After the dropwise addition, the temperature was raised to 130° C. and kept at this temperature for 3 hours. At the end of the reaction, 18 g of water was added to control the acidity of the feed solution at 30%, to obtain the sulfonated feed.

[0031] 2. Condensation: Adjust the acidity of the sulfonated material to 26% by adding 30g of water. After the temperature of the material drops to 85°C, start to add 27g (0.32mol) of 37% formaldehyde solution dropwise. After the dropwise addition, heat up to 110°C and start to keep warm , and kept at this temperature for 3.5h.

[0032] 3. Neutralization: Add 79.5g of water to the condensed material after heat preservation and stir evenly, then pre-neutral...

Embodiment 3

[0034] 1. Sulfonation: Add 70g (0.49mol) of methylnaphthalene to the four-necked flask, and when the temperature of the material reaches 100°C, start to add 68g (0.62mol) of 90% sulfuric acid dropwise, and control the dropping temperature to 125°C. The time is controlled at 20-30min. After the dropwise addition, the temperature was raised to 127° C. and kept at this temperature for 3 hours. At the end of the reaction, 13 g of water was added to control the acidity of the feed solution at 31%, to obtain the sulfonated feed.

[0035] 2. Condensation: adjust the acidity of the sulfonated material to 25% by adding 37g of water. After the material temperature drops to 85°C, start to add 27g (0.32mol) of 37% formaldehyde solution dropwise. After the dropwise addition, raise the temperature to 110°C and start to keep warm , and kept at this temperature for 3.5h.

[0036] 3. Neutralization: Add 79g of water to the condensed material after heat preservation and stir evenly, then pre-n...

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Abstract

A preparation method of a low-stain dispersant MF includes adding methylnaphthalene in a reaction container, rising the temperature to 80-100 DEG C, dropping in sulphuric acid while controlling the system temperature to be 100-130 DEG C, rising the temperature to be 120-140 DEG C after finishing dropping, performing thermal reaction for 3 to 5 hours, adding water to control acidity of the feed liquor to be 29-31% at the reaction endpoint, so as to obtain a sulfonated material; further, regulating acidity of the sulfonated material to be 24-27% by adding water, adding formaldehyde dropwisely when the temperature of the material is reduced to be 80-90 DEG C, after finishing dropping, rising the temperature to be 105-125 DEG C and then performing thermal reaction for 3-5 hours, so as to obtain a condensed material; diluting the condensed material with water, performing pre-neutralization with lime, adding in alkali liquor to neutralize the pH value to be 7.0-9.0, finally filtering in heatto obtain the dispersant MF. The dispersant MF prepared by the method is light in color, good in heat stability and low in stain.

Description

(1) Technical field [0001] The invention relates to a preparation method of a dispersant MF, in particular to a preparation method of a low-contamination dispersant MF. (2) Background technology [0002] Dispersant MF is a widely used dye auxiliaries. Its preparation method is to use industrial methylnaphthalene or washing oil as raw material, obtain methylnaphthalenesulfonic acid through sulfonation, and then condense with formaldehyde, and then neutralize, Spray dry to get powdery finished product. [0003] The technology of producing MF both at home and abroad is mainly divided into two kinds at present: one is main raw material with the methyl naphthalene that is processed or not through processing, then is the sulfuric acid of 98% with concentration as sulfonating agent, adopts methyl naphthalene: The mass ratio of sulfuric acid is 1:(1-1.1) for sulfonation, and condensation with formaldehyde under high acidity (27-32%), and then neutralized by lime and liquid caustic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C309/36
CPCC07C303/22C07C303/32C07C309/36
Inventor 何旭斌徐伟朱敬鑫张桂香王森峰吴建伟
Owner ZHEJIANG LONGSHENG CHEM RES