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Purification method of 5-sulfosalicylic acid

A technology of sulfosalicylic acid and purification method, which is applied in the field of purification of 5-sulfosalicylic acid, can solve the problems of cumbersome operation, high cost, and low purity, and achieve the effect of safe and convenient purification process and stable product quality

Active Publication Date: 2014-08-06
TAICANG HUSHI REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by this invention is to provide a kind of purification method of 5-sulfosalicylic acid, to overcome the low purity of 5-sulfosalicylic acid purification product in the prior art, complex operation, large energy consumption and high cost insufficient

Method used

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  • Purification method of 5-sulfosalicylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 350ml of composite purifying agent to 1000g of industrial grade 5-sulfosalicylic acid, heat to 60°C and stir and reflux for 4h, cool to room temperature and then dry and centrifuge to obtain 963g of crude 5-sulfosalicylic acid, the 5-sulfosalicylic acid The crude salicylic acid was dissolved in 500mL of deionized water to make a saturated aqueous solution, then 10g of activated carbon was added and stirred for 3 hours, the activated carbon was removed by filtration, and the filtrate was concentrated under reduced pressure at 70°C to obtain the purified white crystalline product 5-sulfowater Salicylic acid 929g, purity 99.53%;

[0021] The compound cleaning agent used in this embodiment is the mixture of dimethylacetamide, isoamyl acetate, ethyl acetate, butyl acetate, methyl isobutyl ketone and dimethyl phthalate, and its mixing molar ratio is : 0.4:0.3:1:0.7:0.3:0.5.

Embodiment 2

[0023] Add 400ml of composite purifying agent to 1000g of industrial grade 5-sulfosalicylic acid, heat to 65°C and stir and reflux for 5h, cool to room temperature and then drain and centrifuge to obtain 956g of crude 5-sulfosalicylic acid, the 5-sulfosalicylic acid The crude salicylic acid was dissolved in 600mL of deionized water to make a saturated aqueous solution, then 15g of activated carbon was added and stirred for 3.5h, the activated carbon was removed by filtration, and the filtrate was concentrated under reduced pressure at 68°C to obtain the purified white crystalline product 5-sulfo Salicylic acid 917g, purity 99.59%.

[0024] The compound cleaning agent used in this embodiment is the mixture of dimethylacetamide, isoamyl acetate, ethyl acetate, butyl acetate, methyl isobutyl ketone and dimethyl phthalate, and its mixing molar ratio is : 0.3:0.2:1:0.6:0.2:0.4.

Embodiment 3

[0026] Add 450ml of composite purifying agent to 1000g of industrial grade 5-sulfosalicylic acid, heat to 70°C and stir and reflux for 6h, cool to room temperature and then drain and centrifuge to obtain 945g of crude 5-sulfosalicylic acid, the 5-sulfosalicylic acid The crude salicylic acid was dissolved in 700mL of deionized water to make a saturated aqueous solution, then 20g of activated carbon was added and stirred for 4 hours, the activated carbon was removed by filtration, and the filtrate was concentrated under reduced pressure at 65°C to obtain the purified white crystalline product 5-sulfowater Salicylic acid 903g, purity 99.62%.

[0027] The compound cleaning agent used in this embodiment is the mixture of dimethylacetamide, isoamyl acetate, ethyl acetate, butyl acetate, methyl isobutyl ketone and dimethyl phthalate, and its mixing molar ratio is : 0.35:0.25:1:0.65:0.25:0.45.

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Abstract

The invention discloses a purification method of a 5-sulfosalicylic acid. The purification method comprises the following steps: taking industrial-grade 5-sulfosalicylic acid as a raw material, adding a composite cleaning agent made by the company into the raw material, heating, stirring and refluxing, pumping water out and centrifuging after cooling to obtain crude 5-sulfosalicylic acid products, and then obtaining purified 5-sulfosalicylic acid through collecting 5-sulfosalicylic acid products in a conventional method, wherein the purity of the 5-sulfosalicylic acid obtained by the purification method is larger than 99.5%. Compared with the prior art, the purification method has a safe and convenient purification process, saves energy and reduces emission; the composite cleaning agent can be recycled after being activated, so that the requirements of green chemical industry and environment protection are met; and the purified 5-sulfosalicylic acid product is stable in quality, and has an industrial production prospect.

Description

technical field [0001] The invention relates to a method for purifying 5-sulfosalicylic acid. Background technique [0002] 5-sulfosalicylic acid is referred to as sulfosalicylic acid, also known as 2-hydroxy-5-sulfobenzoic acid, the English name is 5-sulphosalicylic acid, mainly used in the manufacture of dyes, surfactants, catalysts, pharmaceutical intermediates Wait. 5-sulfosalicylic acid is used in the dye industry as an intermediate for the manufacture of surfactants; in pharmaceutical intermediates, it is the raw material for various preparations such as doxycycline and methacycline; 5-sulfosalicylic acid Salicylic acid is also a color developer for metal ions, which can be used to determine manganese, lead and other metal ions. [0003] The structural formula of 5-sulfosalicylic acid is as follows: [0004] [0005] In the prior art, there are many reports on the treatment method of 5-sulfosalicylic acid wastewater, but there are few disclosures on its purificat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/44C07C309/60
Inventor 王伟顾小焱吕明王永旗
Owner TAICANG HUSHI REAGENT
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