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.

Inactive Publication Date: 2017-07-28
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the process of this route is relatively complicated, and the requirements for technical equipment are relatively high. There are not many domestic factories that can meet the technical requirements, and further improvement is needed.
Disadvantages: The raw material methyl mercaptan is not easy to obtain, it is gaseous at normal temperature and pressure, and has a foul smell. At present, there are few domestic factories producing methyl mercaptan, which limits the promotion of this process
Previous studies have shown that the degree of association of phthalocyanine molecules in the reaction medium has a great influence on its catalytic performance. As a catalyst, it is easy to form dimers or even polymers in solution, making the large planar axial coordination of metal phthalocyanines The active sites of the sites are reduced, resulting in a decrease in catalytic efficiency

Method used

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  • Activated carbon-loaded tetrasulfo cobalt phthalocyanine and application thereof in preparing dimethyl disulfide as catalyst
  • Activated carbon-loaded tetrasulfo cobalt phthalocyanine and application thereof in preparing dimethyl disulfide as catalyst
  • Activated carbon-loaded tetrasulfo cobalt phthalocyanine and application thereof in preparing dimethyl disulfide as catalyst

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention belongs to the field of chemical engineering and in particular to activated carbon-loaded tetrasulfo cobalt phthalocyanine and an application thereof in preparing dimethyl disulfide as a catalyst. The preparation method of the activated carbon-loaded tetrasulfo cobalt phthalocyanine comprises the following step: loading tetrasulfo cobalt phthalocyanine to modified activated carbon by means of a chemical grafting method to obtain activated carbon-loaded tetrasulfo cobalt phthalocyanine (AC-CoPcS), wherein the modified activated carbon is ethidene diamine modified activated carbon. The catalyst is stable in structure, can be repeatedly used, and can realize effective catalytic oxidation of thiomethoxide to prepare dimethyl disulfide in a reaction system in an alkali-resistant, pressure-resistant and high-temperature-resistant manner. By taking AC-CoPcS as the catalyst, the catalyst can be better separated from a product in a process of preparing the dimethyl disulfide, and the product yield and DMDS purity are higher than those obtained by catalysis of free state CoPcS. The DMDS yield of the obtained product can reach 86.8%, and the product purity can reach 100%.

Description

Technical field [0001] The invention belongs to the field of chemical industry, and specifically relates to an activated carbon supported cobalt phthalocyanine tetrasulfonate and its application as a catalyst in the preparation of dimethyl disulfide. Background technique [0002] Dimethyl disulfide (DMDS) has become an important chemical raw material due to its wide range of uses, with high economic value and good market prospects. However, due to the harsh production and synthesis conditions, malodorous and highly toxic raw materials, and the difficulty of obtaining raw materials, many restrictions have led to fewer domestic manufacturers today. [0003] The synthesis methods of dimethyl disulfide mainly include: methanol sulfurization method, methyl mercaptan sulfurization method, methyl mercaptan oxidation method, and dimethyl sulfate method. [0004] 1. Dimethyl sulfate method [0005] The dimethyl sulfate method uses sulfur and sodium sulfide as raw materials to first prepare so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C319/24C07C321/14C07C319/28
CPCB01J31/1825B01J2231/70B01J2531/025B01J2531/845C07C319/24C07C319/28C07C321/14
Inventor 全学军代明星郑道敏李硕柳亚玲程治良姚如杰
Owner CHONGQING UNISPLENDOUR CHEM
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