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Process for preparing 4,5-dihydroxy-phenyl-sodium-disulfonate

A technology of sodium benzenedisulfonate and a manufacturing method, which is applied in the fields of sulfonic acid preparation and organic chemistry, can solve the problems of serious environmental pollution, cumbersome treatment process, and excessive sulfuric acid, and achieve low environmental pollution, high purity, and reduced Effects of Environmental Pollution

Active Publication Date: 2010-05-19
XILONG SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The excess of oleum used in this method is relatively large, which is 5 times the quality of catechol; sodium chloride is used to react with 4,5-dihydroxy-1,3-benzenedisulfonic acid, and the reaction product contains a higher proportion The by-products of sodium sulfate, sodium bisulfate and unreacted sodium chloride and hydrogen chloride have complex components, complicated treatment process, low purity (about 80%) of the finished product, a lot of waste water in the treatment process, serious environmental pollution, and high cost

Method used

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  • Process for preparing 4,5-dihydroxy-phenyl-sodium-disulfonate
  • Process for preparing 4,5-dihydroxy-phenyl-sodium-disulfonate

Examples

Experimental program
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Effect test

Embodiment 1

[0029] In a 1000ml three-neck round-bottom flask, add 110 grams of catechol (1.0 mol), cool in a water bath, and slowly add 484 grams of 20% oleum (5.16 mol) dropwise with stirring, white smoke is produced immediately, control The temperature of the reactant is about 40°C to suppress the amount of white smoke produced. After adding fuming sulfuric acid, the reaction solution was heated to 70°C and reacted for 3 hours. A large amount of solid 4,5-dihydroxy-1,3-benzenedisulfonic acid was produced in the reaction solution. Cool to room temperature.

[0030] An aqueous sodium hydroxide solution was prepared with 72.1 g of 96% sodium hydroxide (1.73 mol) and 125 ml of pure water, and the solution was slowly added dropwise to the above reaction solution under water bath cooling. After the addition, the reaction solution was heated to 70°C for 1.5 hours, then cooled to room temperature, poured into a beaker containing 1200ml of pure water, heated to 80°C, added with a small amount ...

Embodiment 2

[0032] According to the operation steps of Example 1, change the following parameters:

[0033] 1. Amount of 20% oleum: 440g; after adding oleum, the reaction temperature was controlled at 80°C;

[0034] 2. Amount of sodium hydroxide: 78.6 g; after adding sodium hydroxide, the reaction temperature was controlled at 80°C.

[0035] The weight of the crystal obtained in this example is 204.1 g, the content of sodium 4,5-dihydroxy-1,3-benzenedisulfonate is 99.6%, and the yield is 65%.

Embodiment 3

[0037] According to the operation steps of Example 1, change the following parameters:

[0038] The dosage of 25% oleum is 440g; after adding the oleum, the reaction temperature is controlled at 90°C;

[0039] The amount of sodium hydroxide was 83.3g; after adding sodium hydroxide, the reaction temperature was controlled at 90°C;

[0040] The weight of the crystal obtained in this example is 216.5 g, the content of sodium 4,5-dihydroxy-1,3-benzenedisulfonate is 99.8%, and the yield is 68.9%.

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Abstract

This invention relates to preparation method of a high-purity,low cost, simple handleing 4,5-dioxy-1,3-benzene disulfoacid sodium. The invention takes two steps synthetic process: first adopts brenzcatechin as raw meterial, use fuming sulfuric acid to proceed sulfonating, then takes reaction with caustic soda.

Description

technical field [0001] The present invention relates to a method for producing sodium 4,5-dihydroxy-1,3-benzenedisulfonate. Background technique: [0002] 4. Sodium 5-dihydroxy-1,3-benzenedisulfonate is used in spectrophotometer as a color developer for the determination of rare earth elements, manganese, titanium, cerium, niobium, molybdenum and other elements, and also used for coordination titration indicator and masking agent for metal ions. [0003] The synthetic method of this substance is mentioned in Article 03235 on page 450 of the first edition of "Commonly used reagents and high-purity substances" published by Chemical Industry Press in January 2003. Diphenol is sulfonated, the resulting sulfonated product is dissolved in water, sodium chloride is added, the precipitated crystals are dissolved in pure water, activated carbon is added to heat for decolorization, barium carbonate is added to the filtrate, the precipitate is removed by filtration, then sodium carbon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/42C07C303/06
Inventor 庄景发黄益祥王立林
Owner XILONG SCI CO LTD
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