废液中六亚甲基1,6-二硫代硫酸二钠二水合物回收工艺研究-study on recovery technology of hexamethylene 1,6 - dithiosulfate dihydrate from waste liquid.docxVIP

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废液中六亚甲基1,6-二硫代硫酸二钠二水合物回收工艺研究-study on recovery technology of hexamethylene 1,6 - dithiosulfate dihydrate from waste liquid.docx

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废液中六亚甲基1,6-二硫代硫酸二钠二水合物回收工艺研究-study on recovery technology of hexamethylene 1,6 - dithiosulfate dihydrate from waste liquid

AbstractSodium hexamethylene-1,6-bisthiosulfate dihydrate (HTS), a post- vulcanisation stabilizer, is used to strengthen the thermal stability and fatigue life of tie rubber. As a high-performance rubber additive, the demand of HTS is increasing with the development of automobile industry. Currently, HTS is synthesized through an one-step reactive crystallization, and the reaction conversion rate is higher than 99% while the yield of it is just 75%. A quarter ofHTS still remains in waste liquid，which not only reduces the utilization rate ofraw materials, but also causes environment pollution. The problem needs to be solved urgently. In this work, systematic experiment has been done to determine the system composition and component content, and study on the system thermodynamics. At last, a cooling crystallization technology with solvent circulation was designed to extract all the HTS from the waste liquid.The composition of waste liquid is detected by liquid chromatograph-mass spectrometer, and then the residue was quantitatively analyzed after the concentration and drying of the waste liquid. Volhard Method was first introduced to analyze content of sodium chloride in the residue quantitatively. Combining with Iodometry Method analyzing the content of sodium thiosulfate in this system, the composition of residue is: sodium chloride 54.10~62.13%, sodium thiosulfate 10.54%~21.72%, HTS 26.4%~33.28%.The solubilities of sodium chloride + sodium thiosulfate + HTS in ethanol + water binary solvent system are measured by the static method at different temperatures with diverse percentage of ethanol. The purity of HTS dissolved outby cooling the 95% ethanol system from 78.15℃ to 20.00℃ can be figure outabove 95%, based on the solute contents at the two temperatures.According to thermodynamic calculation above, a cooling crystallization route was designed. The dry residue was dissolved in 95% ethanol system at78.15 ℃ to reach a saturation state of HTS while the undi