Synthetic process of sodium polydithiodipropane sulfonate

A technology of sodium polydisulfide dipropane sulfonate and synthesis process, which is applied in the synthesis field of sodium polydisulfide dipropane sulfonate, can solve the problems of many steps, high production cost, difficulty in obtaining high-purity products, etc., and achieves easy access to raw materials. the effect of fewer synthesis steps

Active Publication Date: 2019-03-08
吉和昌新材料(荆门)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Hydrogen sulfide in this route is a highly toxic gas, and there are great potential safety hazards. Secondly, the process has long production time, many steps, high energy consumption, high production cost, and it is difficult to obtain high-purity products.

Method used

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  • Synthetic process of sodium polydithiodipropane sulfonate
  • Synthetic process of sodium polydithiodipropane sulfonate
  • Synthetic process of sodium polydithiodipropane sulfonate

Examples

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Effect test

Embodiment 1

[0038] The synthetic technique of sodium polydithiodipropane sulfonate, this synthetic technique comprises the following steps:

[0039] 1) Synthesis of Pent’s salt: Add 79g (0.5mol) sodium thiosulfate and 300mL methanol into a 500mL four-neck flask and stir evenly, cool down to 20°C, slowly add 61g (0.5mol) 1,3-propanesulfone dropwise For ester, control the dropwise addition temperature at 20-30°C. After the dropwise addition, continue to react at 20°C for 2 hours to obtain Pent salt;

[0040] 2) Preparation of sodium dithiodipropane sulfonate: after adding 30% sodium hydroxide to the prepared Penter's salt in step 1) to adjust the pH value to 10, add 22.5g (0.25mol) tert-butyl hydroperoxide, Raise the temperature to 55°C for 4 hours, then lower the temperature to 5°C, filter and separate the solid sodium sulfate, and at the same time, concentrate the filtrate until the solid precipitates, filter and dry at 70-80°C to obtain polydithiodipropanesulfonic acid sodium.

[0041]...

Embodiment 2

[0043] The synthetic technique of sodium polydithiodipropane sulfonate, this synthetic technique comprises the following steps:

[0044] 1) Synthesis of Penter's salt: Add 79g (0.5mol) sodium thiosulfate, 200mL isopropanol and 100mL water into a 500mL four-necked bottle and stir evenly, cool down to 20°C, slowly add 61g (0.5mol)1,3 - Propane sultone, control the dropwise addition temperature at 20-30°C, after the dropwise addition, continue to react at 20°C for 2 hours to obtain Pent's salt;

[0045] 2) Preparation of sodium polydisulfide dipropane sulfonate: after adding 30% sodium hydroxide to the prepared Penter's salt in step 1) to adjust the pH value to 10, add 30g (0.25mol) of 28% super Hydrogen oxide, heat up to 50°C and react for 4 hours, then cool down to 5°C, filter and separate solid sodium sulfate, at the same time, concentrate the filtrate until solid precipitates, filter and dry at 70-80°C to obtain polydisulfide Sodium Propane Sulfonate.

[0046] The yield of ...

Embodiment 3

[0048] The synthetic technique of sodium polydithiodipropane sulfonate, this synthetic technique comprises the following steps:

[0049] 1) Synthesis of Penter's salt: Add 79g (0.5mol) sodium thiosulfate, 250mL isopropanol and 50mL water into a 500mL four-necked bottle and stir evenly, cool down to 20°C, slowly add 61g (0.5mol)1,3 - Propane sultone, control the dropwise addition temperature at 20-30°C, after the dropwise addition, continue to react at 20°C for 2 hours to obtain Pent's salt;

[0050] 2) Preparation of sodium polydithiodipropane sulfonate: after adding 30% sodium hydroxide to the prepared Penter's salt in step 1) to adjust the pH value to 10, continue to feed oxygen, raise the temperature to 60°C and react for 4 hours, Then lower the temperature to 5°C, filter and separate the solid sodium sulfate, and at the same time, concentrate the filtrate until the solid precipitates, filter and dry at 70-80°C to obtain sodium polydithiodipropanesulfonate.

[0051] The yi...

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Abstract

The invention discloses a synthetic process for bis-(3-sulfopropyl)disulfide, belonging to the technical field of synthesis of the bis-(3-sulfopropyl)disulfide. The synthetic process provided by the invention comprises the following steps: with 1,3-propanesultone as a raw material, carrying out a reaction with sodium thiosulfate in a mixed solution of an alcohol substance and water so as to prepare bunte salt, then subjecting the prepared bunte salt to alkalization and oxidation, and carrying out purification and concentration so as to prepare the bis-(3-sulfopropyl)disulfide. The bis-(3-sulfopropyl)disulfide prepared by using the method provided by the invention has high yield and purity, wherein the yield can reach 98.1%, and the purity can reach 99.5%; meanwhile, the synthetic process provided by the invention has the advantages of easily available raw materials, less synthetic steps and applicability to industrial production.

Description

technical field [0001] The invention relates to the technical field of synthesis of sodium polydithiodipropane sulfonate, in particular to a synthesis process of sodium polydithiodipropane sulfonate. Background technique [0002] Sodium polydisulfide dipropane sulfonate (bis-(3-sulfopropyl) disulfide, hereinafter referred to as SPS), molecular formula: C 6 h 12 Na 2 o 6 S 4 , Molecular weight: 354.4, CAS No.: 27206-35-5, is white to light yellow solid powder, mainly used for acidic copper plating brightener, is an essential additive in copper plating, it can be used for copper plating to obtain decoration and functional coatings. SPS can also be used in combination with typical copper plating formulations such as non-ionic surfactants, polyamines and other hydrogen sulfide compounds, and can also be used with dyes, if combined with N,N-dimethyl-dithiocarbonylpropanesulfonate Sodium disulfide (DPS), thiourea propyl sulfate (UPS) or 3-(benzothiazole-2-mercapto)-propanesu...

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 杨威冯庆诚周世骏黄开伟宋文华肖忠新郭新乐
Owner 吉和昌新材料(荆门)有限公司
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