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
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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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