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A method of co-producing high-purity Schaeffer's salt and g-salt

A technology of Schaeffer's salt and naphthol, which is applied in the field of co-production of Schaeffer's salt and G salt, can solve the problems of low utilization rate of raw materials, difficult purification of finished products, and low yield of G salt, so as to improve the overall utilization rate , Process environmental protection, high product purity effect

Active Publication Date: 2020-10-09
ZHEJIANG LONGSHENG CHEM RES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But even so, the resulting G salt yield is still low (about 70%), and the filter cake still contains more by-products such as Scherrer's salt and R salt, resulting in a purity≤80%. If the G salt of higher purity is to be obtained , it is bound to further affect the yield
However, there is a large amount of R salt in the G salt wastewater, which needs to be extracted by extraction / back extraction, but only poor quality R salt can be obtained.
[0007] In summary, the synthesis of Schaeffer's salt / G salt has disadvantages such as difficult purification of finished products, low yield, low utilization rate of raw materials, and complicated procedures.

Method used

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  • A method of co-producing high-purity Schaeffer's salt and g-salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] This embodiment provides a method for simultaneously preparing and separating high-purity Schaeffer's salt and G salt, comprising the following steps:

[0035] Take 100g of 2-naphthol, add 300g of 98.5% sulfuric acid, react at 50°C for 4 hours, add 130g of water to adjust the acidity for hydrolysis, control the addition temperature at 80-85°C, keep it warm for 2 hours, then add 50g of 20% ammonia water for salting out, Control the addition temperature at 100-105°C, keep warm for 2 hours after the addition, cool down to 40-50°C and press filter to obtain 100g of Schaeffer's salt crude product and 480g of mother liquor, add 100g of water to the Schaeffer's salt crude product for washing, and obtain 88g Schaeffer's salt finished product, purity 99.77%. After mixing the washing water with the mother liquor of Schaeffer's salt, add 150g of 20% ammonia water, keep it at 80°C for 2 hours for salting out, then cool down to 40-50°C and filter and separate to obtain 105g of finis...

Embodiment 2

[0037] This embodiment provides a method for simultaneously preparing and separating high-purity Schaeffer's salt and G salt, comprising the following steps:

[0038] Take 100g of 2-naphthol, add 300g of 98.5% sulfuric acid, react at 65°C for 5 hours, add 150g of water to adjust the acidity for hydrolysis, control the addition temperature at 80-85°C, keep it warm for 2 hours, then add 60g of 20% ammonia water for salting out, Control the addition temperature at 100-105°C, keep warm for 1h after the addition, cool to 40-50°C and press filter to obtain 85g of Schaeffer's salt crude product and 525g of mother liquor, add 280g of water to the Schaeffer's salt crude product for washing, and obtain 70g Schaeffer's salt finished product, purity 99.87%. After mixing the washing water with the mother liquor of Schaeffer's salt, add 150g of 20% ammonia water, incubate at 90°C for 1 hour for salting out, then cool down to 40-50°C and filter and separate to obtain 115g of finished G salt ...

Embodiment 3

[0040] This embodiment provides a method for simultaneously preparing and separating high-purity Schaeffer's salt and G salt, comprising the following steps:

[0041] Take 100g of 2-naphthol, add 300g of 97% sulfuric acid, react at 80°C for 6 hours, add 150g of water to adjust the acidity for hydrolysis, control the addition temperature at 80-85°C, keep it warm for 2 hours, then add 70g of 20% ammonia water for salting out, Control the addition temperature at 100-105°C, keep warm for 2 hours after the addition, cool down to 40-50°C and press filter to obtain 62g of Schaeffer's salt crude product and 558g of mother liquor, add 200g of water to the crude Schaeffer's salt for washing, and obtain 54g Schaeffer's salt finished product, purity 99.8%. After mixing the washing water with the Schaeffer’s salt mother liquor, add 150g of 20% ammonia water, keep it at 100°C for 2h for salting out, then cool down to 40-50°C and filter and separate to obtain 128g of G salt finished product ...

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Abstract

A method of combined production of high-purity Schaffer's salt and G salt comprises the following steps: 1) performing a reaction with 2-naphthol as a raw material and sulfuric acid as a sulfonating agent at 20-90 DEG C for 1-10 h to prepare a sulfonated solution; 2) adding water to the sulfonated solution for hydrolysis at 70-150 DEG C for 1-2 h to obtain a hydrolyzed solution; 3) adding ammoniato the hydrolyzed solution, maintaining temperature at 70-130 DEG C for 1-5 h to perform salting-out; 4) cooling the mixture to 40-50 DEG C and filtering the mixture, water-washing and drying a filtercake to obtain a Schaffer's salt product, mixing the filtrate and washing waste water, adding ammonia or ammonium sulfate and maintaining temperature at 70-130 DEG C for 1-5 h to perform salting-out,and cooling the mixture to 40-50 DEG C and filtering and separating the mixture, and drying a filter cake to obtain a G salt product. The method can achieve combined production of the Schaffer's saltand G salt at high purity; meanwhile, total utilization rate of raw materials and equipment utilization rate are increased. The method has simple processes, is environment-friendly and is economical.

Description

[0001] (1) Technical field [0002] The invention relates to the technical field of chemical industry, in particular to a method for co-producing Schaeffer's salt and G salt. [0003] (2) Background technology [0004] Both Schaeffer's salt (2-naphthol-6-sulfonate) and G salt (2-naphthol-6,8-disulfonate) are important chemical intermediates, and Schaeffer's salt is used to make acid Dye and food dye; G salt is used to produce dyes such as acid scarlet 3R, acid complex violet 5RW and weak acid scarlet G, and can also be used to prepare 2-amino-8-naphthol-6-sulfonic acid and 2-amino-6 , 8-Naphthalene disulfonic acid and other intermediates. [0005] The traditional production of Schaeffer's salt is to use 2-naphthol as raw material, sulfonate concentrated sulfuric acid at 100-120°C for 3-10 hours, and then salt out and filter to obtain the crude product after cooling down, add lye to dissolve, then acidify and salt out to produce have to. There are certain drawbacks in this me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/43C07C303/06C07C303/32
CPCC07C303/06C07C303/32C07C309/43
Inventor 何旭斌徐伟朱敬鑫魏沁
Owner ZHEJIANG LONGSHENG CHEM RES
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