A kind of reuse method of benzene hydrogenation sulfur-containing wastewater
A technology for benzene hydrogenation and wastewater, which is applied in chemical instruments and methods, gaseous discharge wastewater treatment, hydrogenated polysulfide/polysulfide preparation, etc., can solve problems such as environmental pollution and waste, and achieve high purity and stable quality. , the effect of avoiding emissions
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Embodiment 1
[0030] Example 1 Preparation of dimethyl disulfide by utilizing benzene hydrogenation sulfur-containing wastewater
[0031] (1) vulcanization: in the vulcanization still, add 40g sodium hydroxide in the benzene hydrogenation sulfur-containing waste water 147g that is 38% in the calibration sodium hydrosulfide content, the gained solution is diluted with water and is that the mass fraction is 17% sodium sulfide solution, will The solution was heated to 65°C, and then 32g of pulverized sublimed sulfur was added to the solution in batches, and the mixture was stirred and reacted at 65°C for 1 hour to obtain a sodium disulfide solution with a mass fraction of 22.4%.
[0032] (2) Alkylation: transfer the above solution to an alkylation kettle, and vacuumize to 1-2×10 4 Pa, followed by the introduction of methyl chloride gas, the system pressure is maintained at 0.5MPa, the system temperature is maintained at 65 ~ 70 ° C, through metering, the feed amount of methyl chloride reaches ...
Embodiment 2
[0036] Example 2 Preparation of diethyl disulfide by utilizing benzene hydrogenation sulfur-containing wastewater
[0037] (1) vulcanization: put into the sodium disulfide solution 100g that contains 20% in the round bottom flask of 250mL, the preparation method of sodium disulfide is with embodiment 1;
[0038] (2) Alkylation: place a tee and a simple gas distributor, after vacuuming to 0.2 atm, start vigorously stirring and feed ethyl chloride gas, use a mass flow meter to control the flow rate and amount of ethyl chloride, and react Keep a slight positive pressure and control the reaction temperature at 80-90°C. When the feed rate reaches the feed ratio (molar ratio) of sodium disulfide: ethyl chloride = 1:2, or when the water phase changes from dark red to light yellow , stop feeding ethyl chloride. The reaction was cooled to room temperature;
[0039] (3) Purification and waste water treatment: stand to separate the oil phase, a small amount of oil-water mixed layer is ...
Embodiment 3
[0040] Example 3 Preparation of dicyclohexyl disulfide by utilizing benzene hydrogenation sulfur-containing wastewater
[0041]The preparation method of sodium disulfide is the same as in Example 1. At room temperature, 100 g of sodium disulfide solution is added to a 250 mL four-neck flask, and then, under nitrogen protection, 0.472 mol of chlorocyclohexane is slowly added dropwise, and the reaction mixture is refluxed. React for 4 to 6 hours. The progress of the reaction is detected by thin-layer chromatography. After the reaction, the oil phase is separated by standing, and a small amount of oil-water mixed layer is reused for the next reaction. The water phase is left to be distilled for diluting sodium sulfide or preparing liquid caustic soda, and recycled to benzene The hydrogenation section is used for the absorption of hydrogen sulfide. The oil phase was distilled under reduced pressure to obtain 44.0 g of a yellow oily liquid with a yield of 80.9%. 1 H-NMR (400MHz, ...
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