Activated carbon carried cuprous iodide catalyst, and its preparing method and use

A technology of cuprous iodide and activated carbon, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problems of high production cost ratio, photosensitive decomposition loss, serious problems, etc., to improve recycling efficiency, High uniform dispersion and simplification of separation process

Inactive Publication Date: 2008-11-12
HUAIHAI INST OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cuprous iodide catalyst is a photosensitive compound, and the photosensitive decomposition loss of the fine powder cuprous iodide in the two processes of pulverization and catalytic application is relatively serious
The price of cuprous iodide is relatively high, so the loss of cuprous iodide as a catalyst is high, accounting for 2,4-diamino-3,5-dimethylthiotoluene and 2,6-diamino-3,5 - high proportion of production cost of dimethylthiotoluene mixture

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Activated carbon supported cuprous iodide catalyst and preparation method

[0011] In the reaction flask equipped with stirrer, reflux condenser, and dropping funnel, add 0.21 mole of copper sulfate pentahydrate, 0.2 mole of potassium iodide, 200 grams of 60 mesh activated carbon, and 200 milliliters of deionized water. Hour. Cool to room temperature, stir and drop 0.22 mole of sodium sulfite in a saturated aqueous solution, react for 1 hour, collect the filter cake, wash the filter cake with deionized water for 3 to 5 times, then wash with absolute ethanol for 3 to 5 times, and vacuum dry. The activated carbon-supported cuprous iodide catalyst can be prepared.

Embodiment 2

[0013] Activated carbon supported cuprous iodide catalyst and preparation method

[0014] In a reaction flask equipped with a stirrer, a reflux condenser, and a dropping funnel, add 0.21 moles of copper sulfate pentahydrate, 0.2 moles of iodine iodine, 200 grams of 60-mesh activated carbon, 100 milliliters of ethanol, and 100 milliliters of deionized water. , heated to boiling for 2 hours. Cool to room temperature, stir and drop in 20 grams of 37% formaldehyde solution, react for 1 hour, collect the filter cake, wash the filter cake with deionized water for 3 to 5 times, then wash with absolute ethanol for 3 to 5 times, and then vacuum dry , the activated carbon-supported cuprous iodide catalyst can be prepared.

Embodiment 3

[0016] Application of Activated Carbon Supported Cuprous Iodide Catalyst

[0017] In the reaction flask equipped with agitator, reflux condenser and dropping funnel, add 100 grams of 2,4-diaminotoluene and 2,6-diaminotoluene mixture (80:20) and Example 1 Prepared activated carbon supported cuprous iodide catalyst 30 grams. N 2 Under protection, the temperature was raised to 130-135°C with stirring, and 160 grams of dimethyl disulfide was added dropwise within 3 hours, and the reaction was continued at 130-135°C for 2 hours after the dripping of dimethyl disulfide was completed. Cool to around 50°C, vacuum filter, and vacuum distill the filtrate to separate the mixture of 2,4-diamino-3,5-dimethylthiotoluene and 2,6-diamino-3,5-dimethylthiotoluene 231 g, 94.4% yield. The filter cake can be recycled for more than 8 times and still maintain a high yield.

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PUM

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Abstract

The active carbon loaded cuprous iodide provided in this invention can be used as the catalyst of sulfur-alkylation reaction between dialkyldithio and aromatic compound, which is processed by dipping active carbon in ethanol / hydrosolvent of bluestone and iodine or bluestone and potassium iodide then to be recovered by formaldehyde, SO, H2SO3 or sodium hyposulfite.

Description

technical field [0001] The invention belongs to the field of chemical reaction catalysts. In particular, it relates to an active carbon supported cuprous iodide catalyst used for the reaction of dialkyl disulfide and aromatic compound to prepare alkylthio aromatic compound. technical background [0002] Many alkylthioaromatics (such as sulfide anisole, p-methylthiophenol, 2,4-diamino-3,5-dimethylthiotoluene, 2,6-diamino-3,5-dimethylthio Toluene, etc.) are important fine synthetic intermediate raw materials, widely used in the synthesis of pesticides and rubber and plastic additives. The electrophilic substitution reaction between dialkyl disulfide and arene is one of the important methods to prepare alkylthio arene, wherein dialkyl disulfide mainly includes dimethyl disulfide, diethyl disulfide, dibenzyl disulfide , dicyclohexyl disulfide, etc. Aromatics mainly include aromatic compounds activated by electron-pushing groups, such as phenol, aniline, 2,4-diaminotoluene, 2,6...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/122B01J21/18B01J35/02C07C321/28
Inventor 张田林潘汉春
Owner HUAIHAI INST OF TECH
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