A kind of synthetic method of sodium polydithiodipropane sulfonate

A technology of sodium polydithiodipropane sulfonate and synthesis method, which is applied in the field of two-step synthesis of sodium polydithiodipropane sulfonate for electroplating brightener, can solve the problem of difficulty in obtaining high-purity products, high production cost and long preparation time and other problems, to achieve the effects of stable yield, effective purity improvement, and simple operation

Active Publication Date: 2019-03-08
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the common SPS synthesis process mostly adopts hydrogen sulfide alkaline sulfonation method. Since hydrogen sulfide in the raw material is a highly toxic gas, there is a great safety hazard. In addition, this process also has long preparation time, many steps, high energy consumption, The defects of high production cost and difficulty in obtaining high-purity products

Method used

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  • A kind of synthetic method of sodium polydithiodipropane sulfonate

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Synthesis of Pent’s salt: Add 155g (0.625mol) sodium thiosulfate and 250ml water into a 1L four-necked bottle, stir until dissolved, cool down to 15°C, and slowly add 76.5g (0.625mol) sodium thiosulfate solution dropwise. mol) 300ml of ethanol solution of 1,3-propane sultone, and the dropping temperature is controlled not to exceed 30°C. After the dropwise addition was completed, the reaction was continued at 15° C. for 2 hours until a large amount of white solid appeared. Continue to stir at this temperature for 1 hour, then filter, wash the bottle with a little ethanol, and dry to obtain a white solid of Pent's salt with a yield of 97%. Wherein, the molar ratio of sodium thiosulfate, 1,3-propane sultone and total solvent participating in the reaction is 1:1:32.

[0019] Synthesis of SPS: Add 35g (0.125mol) of Pendt’s salt and 300ml of methanol into a 500ml reaction flask, stir and heat to reflux, then slowly add 35g of concentrated hydrochloric acid (0.35mol) dropwis...

Embodiment 2

[0021] Synthesis of Pent’s salt: Add 155g (0.625mol) sodium thiosulfate and 250ml water into a 1L four-necked bottle, stir until dissolved, cool down to 15°C, and slowly add 76.5g (0.625mol) sodium thiosulfate solution dropwise. mol) 300ml of methanol solution of 1,3-propane sultone, and the dropping temperature should not exceed 30°C. After the dropwise addition was completed, the reaction was continued at 0-15°C for 2 hours until a large amount of white solid appeared. Continue stirring at this temperature for 1 hour, then filter, wash the bottle with a little methanol, and dry to obtain a white solid of Pent's salt with a yield of 97%. Wherein, the molar ratio of sodium thiosulfate, 1,3-propane sultone and total solvent participating in the reaction is 1:1:37.

[0022] The synthesis of SPS: 35g (0.125mol) Pente salt and 200ml methanol are added in the 500ml reaction bottle, stir and heat to reflux, then slowly add 70g mass fraction is 50% sulfuric acid solution (0.7mol), d...

Embodiment 3

[0024] Synthesis of Pent’s salt: Add 155g (0.625mol) sodium thiosulfate and 125ml water into a 1L four-necked bottle, stir until dissolved, cool down to 15°C, slowly add 38.25g (0.625mol) sodium thiosulfate solution dropwise mol) 125ml of ethanol solution of 1,3-propane sultone, control the dropwise addition temperature not to exceed 30°C. After the dropwise addition was completed, the reaction was continued at 15° C. for 5 hours until a large amount of white solid appeared. Continue to stir at this temperature for 1 hour, then filter, wash the bottle with a little ethanol, and dry to obtain a white solid of Pent's salt with a yield of 97%. Wherein, the molar ratio of sodium thiosulfate, 1,3-propane sultone and total solvent participating in the reaction is 1:1:16.

[0025] The synthesis of SPS: 35g (0.125mol) Pente salt and 100ml methyl alcohol are joined in the 250ml reaction flask, stirring and heating to reflux, then slowly dripping 70g mass fraction is the concentrated s...

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Abstract

The invention relates to a novel synthetic method of bis-(sodium sulfopropyl)-disulfide; the traditional hydrogen sulfide alkalization sulfonation process is abandoned, Bunte salt is generated by the reaction of sodium thiosulfate with 1,3-propanesultone, and the Bunte salt is then subjected to hydrolysis and oxidation two-step process under acid condition to prepare the high-purity bis-(sodium sulfopropyl)-disulfide. The reaction conditions of the method are simple and controllable, no toxic gas is involved in the method, no high-pressure equipment is used, the method is simple to perform, the product yield and purity are high, the method has good repeatability, the reaction process is a common reaction operation with no special reaction equipment involved, little wastewater and solid waste are produced, and the alcohol solvent is recyclable after the reaction.

Description

technical field [0001] The invention belongs to the technical field of fine organic synthesis, and in particular relates to a two-step synthesis method of sodium polydisulfide dipropane sulfonate, an electroplating brightener. Background technique [0002] Sodium polydisulfide dipropane sulfonate, referred to as SPS, is commonly used as acidic copper plating brightener, and decorative and functional coatings can be obtained by using SPS. SPS can be used in combination with non-ionic surfactants, polyamines and hydrogen sulfide, and can also be used with dyes. If SPS is used in combination with DPS and EXP2887, a better coating will be obtained. At present, the common SPS synthesis process mostly adopts the alkali sulfonation method of hydrogen sulfide. Since the hydrogen sulfide in the raw material is a highly toxic gas, there is a great safety hazard. In addition, the process also has long preparation time, many steps, high energy consumption, The production cost is high a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/24C07C323/66
CPCC07C319/24C07C381/02C07C323/66
Inventor 刘治田刘辉张旗
Owner WUHAN INSTITUTE OF TECHNOLOGY
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