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

A technology of dimethyl disulfide and activated carbon, which is applied in the chemical industry, can solve problems such as limitations, high technical equipment requirements, and low product purity, and achieve the effects of increased effective contact area, high purity of DMDS, and wide sources

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

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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
The study found that cobalt tetraaminophthalocyanine can effectively catalyze the oxidation of methyl mercaptide to prepare dimethyl disulfide (DMDS). However, the catalyst is easily soluble in the product dimethyl disulfide, so that the catalyst and the product cannot be separated well. Product purity is not high, thus need further improvement

Method used

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

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Experimental program
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Effect test

Embodiment 1

[0077] The preparation of embodiment 1 catalyst AC-CoTAPc

[0078] 1. Preparation of 1,5-dibromopentane modified activated carbon (AC-Br)

[0079] Weigh the dried 10g activated carbon powder (AC) with concentrated nitric acid aqueous solution V (HNO 3 ):V(H 2 (0)=1:2 was immersed in a 250mL beaker at 60°C for 24h, then washed with deionized water until neutral, dried in a 60°C oven, and then placed in a vacuum oven and dried under vacuum at 105°C to obtain nitric acid-treated Activated carbon (AC-T), spare.

[0080] Accurately weigh 2.0 g of activated carbon after nitrification and drying into a 100 mL round bottom flask, add 50 mL of DMF after redistillation, K 2 CO 3 2.0g, add 2g NaH to react in ice bath for 8h, add 2.0g 1,5-dibromopentane to react at room temperature for 1h, then react at 80°C for 24 hours. After cooling, suction filtration, washing and drying, 2.03 g of activated carbon modified by 1,5-dibromopentane was obtained.

[0081] 2. Preparation of activate...

Embodiment 2

[0083] Example 2 AC-CoTAPc as a catalyst for the preparation of dimethyl disulfide device and method

[0084] 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 The pipeline is also provided with an oxygen pressure reducing valve 2 and an oxygen pressure gauge 3; the reactor 4 is provided with a stirring and heating device, and the temperature controller 6 and the speed controller 7 are used to control the speed and temperature in the reactor; The top of the kettle 4 is also provided with a feed inlet, a feed outlet, an exhaust outlet and cooling water circulation pipes. The cooling water circulation pipeline adjusts the temperature in the reactor by circulating cooling water. The schematic flow chart of the production device is as figure 1 shown.

[0085] The method...

Embodiment 3

[0086] Embodiment 3 prepares the method for dimethyl disulfide

[0087] Take 400mL sodium methyl mercaptide solution (mass fraction of sodium methyl mercaptide is 18%) and 0.1g AC-CoTAPc in a reaction device where the oxygen pressure is 0.6MPa and the temperature is 55°C for 80min to produce dimethyl disulfide ether. The one-way conversion rate of sodium methyl mercaptide reaches 89.7%, the one-way yield of dimethyl disulfide reaches 38.7%, and the product purity is 100%.

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Abstract

The invention belongs to the field of chemical engineering and in particular to activated carbon-loaded tetraamino cobalt phthalocyanine and an application thereof in preparing dimethyl disulfide as a catalyst. The preparation method of the activated carbon-loaded tetraamino cobalt phthalocyanine comprises the following step: loading tetraamino cobalt phthalocyanine to modified activated carbon by means of a chemical grafting method to obtain activated carbon-loaded tetraamino cobalt phthalocyanine, wherein the modified activated carbon is 1,5-dibromopentane 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-CoTAPc 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 CoTAPc. The DMDS yield of the obtained product can reach 87.4%, and the product purity can reach 100%.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to activated carbon-supported cobalt tetraaminophthalocyanine 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 because of its wide application, high economic value and good market prospect. However, due to the relatively harsh production and synthesis conditions, the raw materials are odorous and highly toxic, and the raw materials are not easy to obtain, many restrictions have led to fewer domestic manufacturers. [0003] The synthesis methods of dimethyl disulfide mainly include: methanol vulcanization method, methyl mercaptan vulcanization 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 prepare...

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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