Activated carbon-loaded tetrasulfo cobalt phthalocyanine and application thereof in preparing dimethyl disulfide as catalyst
A technology of dimethyl disulfide and tetrasulfonyl chloride cobalt phthalocyanine, which is applied in the chemical field, can solve the problems of complex route process, reduced catalytic efficiency, limitation and the like, and achieves the effects of wide sources, stable catalyst structure and low price.
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Embodiment 1
[0079] Example 1 Preparation of catalyst AC-CoPcS
[0080] 1. Preparation of ethylenediamine modified activated carbon (AC-E)
[0081] Weigh 10g of dried activated carbon powder (AC) with concentrated nitric acid aqueous solution V (HNO 3 ):V(H 2 O)=1:2 immersed in a 250mL beaker at 60℃ for 24h, then washed with deionized water to neutrality, dried in an oven at 60℃, and then placed in a vacuum drying oven at 105℃ and dried under vacuum to obtain nitric acid treated Activated carbon (AC-T), spare.
[0082] Accurately weigh 2.0g of activated carbon (AC-T) after nitrification and drying, and add 5mL SOCl 2 Reflux for 12 hours at 80°C, after the reaction, heat to 130°C and evaporate to dry the remaining unreacted SOCl 2 , Cool to room temperature to obtain acyl chloride activated carbon. Dissolve 5mL ethylenediamine (EDA) in 100mL DMF, add the above acyl chloride AC, react at 50℃ for 8h, cool to room temperature, use deionized water, DMF and absolute ethanol to remove the remaining unr...
Embodiment 2
[0085] Example 2 Apparatus and method for preparing dimethyl disulfide with AC-CoPcS as a catalyst
[0086] The production device for preparing dimethyl disulfide includes a reactor 4, a high-purity oxygen device 1, a temperature controller 6 and a speed controller 7; the high-purity oxygen device 1 is connected to the top of the reactor 4 through a pipeline, and The pipeline is also provided with an oxygen pressure reducing valve 2 and an oxygen pressure gauge 3; the reactor 4 is equipped with a stirring and heating device, and the speed and temperature in the reactor are controlled by the temperature controller 6 and the speed controller 7; the reaction The top of the kettle 4 is also provided with a feed port, a feed port, an exhaust port and a cooling water circulation pipeline. The cooling water circulation pipeline regulates the temperature in the reactor by circulating cooling water. The schematic flow chart of the production device is as figure 1 Shown.
[0087] The metho...
Embodiment 3
[0088] Example 3 Method for preparing dimethyl disulfide
[0089] Take 400mL sodium methyl mercaptan solution (the mass fraction of sodium methyl mercaptan is 18%) and 0.1g AC-CoPcS in a reaction device with an oxygen pressure of 0.6MPa and a temperature of 55°C to undergo oxidation reaction for 80 minutes to obtain dimethyl bis- Thioether. The single-pass conversion rate of sodium methyl mercaptan reached 93.8%, the single-pass yield of dimethyl disulfide reached 66.2%, and the product purity was 100%.
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