Catalyst for diphenylguanidine (DPG) serving as accelerating agent in oxygen oxidation synthesis production process, and preparation method thereof

A technology of oxygen oxidation and production process, which is applied to the preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc. It can solve the problems of human and environmental hazards and elimination, and achieve the goal of using The effect of small amount, reduced dosage, and improved reaction speed

Inactive Publication Date: 2012-02-15
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the use of heavy metal Pb in this method, which is very harmful to human body and environment, this method has basically stopped using in the late 1990s
In the mid-1990s, there were reports of zinc oxide and iron oxide methods in China, but they were not popularized due to various reasons and have been eliminated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Measure dry SiO 2 The saturated adsorption capacity of the carrier (80 mesh) is 0.9mL / g, weigh 100g of the carrier, and put it in a crucible for subsequent use; dissolve 0.2g of copper acetate in 90mL of distilled water, and stir to make it all dissolve to form an aqueous solution of copper acetate; Slowly pour the copper aqueous solution into the crucible containing the carrier, stir while pouring, and continue stirring after pouring to make it fully and evenly mixed; place it at room temperature for 8 hours to fully infiltrate the copper acetate solution and the carrier; after infiltration, put the mixture at 100 ℃ oven for 8 hours, and then placed in a muffle furnace for roasting, the roasting temperature is 400 °C, and the roasting time is 4 hours; 80-mesh sieve, put the sieved catalyst in a sealed bag, and put it in a desiccator for subsequent use.

[0023] This catalyst is used in the reaction of oxygen oxidation to synthesize DPG. The amount of catalyst used is ...

Embodiment 2

[0025] Measure the saturated adsorption capacity of dry activated carbon (200 mesh) to be 1.1mL / g, weigh 100g of this carrier, and put it in a crucible for later use; dissolve 5g of cobalt acetate in 110mL of ethanol, stir to make it completely dissolve to form ethanol of cobalt acetate solution; slowly pour the alcohol solution of cobalt acetate into the crucible containing the carrier, stir while pouring, and continue to stir after pouring to make it fully mixed; place it at room temperature for 24 hours, and the cobalt acetate solution and the carrier are fully infiltrated; After infiltration, dry the mixture in an oven at 100°C for 8 hours, and then place it in a muffle furnace for calcination at a temperature of 800°C and a calcination time of 12 hours; After the large particles are crushed, pass through a 200-mesh sieve, put the sieved catalyst in a sealed bag, and put it in a desiccator for later use.

[0026] Dissolve 5g of copper sulfate in 110mL of ethanol, stir to m...

Embodiment 3

[0029] Measure dry TiO 2 The saturated adsorption capacity of carrier (240 order) is 1.3mL / g, weighs this carrier 100g, puts in the crucible for subsequent use; Dissolve 10g manganese sulfate in 130mL distilled water, stir to make it all dissolve and form manganese sulfate aqueous solution; Manganese sulfate Slowly pour the aqueous solution into the crucible containing the carrier, stir while pouring, and continue to stir after pouring to make it fully and evenly mixed; place it at room temperature for 36 hours to fully infiltrate the manganese sulfate solution and the carrier; Roasting in a Furnace at a temperature of 550°C and a calcination time of 24 hours; after the calcination, place the crucible in a desiccator to cool down to room temperature, then crush the sintered large particles and pass through a 240-mesh sieve, and the sieved catalyst Put it in a sealed bag and put it in a desiccator for later use.

[0030] This catalyst is used in the reaction of oxygen oxidatio...

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Abstract

The invention relates to a catalyst for diphenylguanidine (DPG) serving as an accelerating agent in an oxygen oxidation synthesis production process and a preparation method thereof. The catalyst is one or more of metal salts, such as copper acetate, copper sulfate, copper nitrate, cobalt acetate, cobalt sulfate, cobalt linoleate, cobalt nitrate, cerium acetate, cerium sulfate, cerium nitrate, manganese acetate, manganese sulfate, manganese nitrate and the like; and a carrier of the catalyst is one or more of active carbon, SiO2, Al2O3, TiO2, a mesoporous material molecular sieve, a micropore material molecular sieve and the like. The prepared catalyst is used in reaction of synthesizing the DPG by oxygen oxidation; and the reaction is used for reflecting the performance of the catalyst. The use amount of the catalyst is 0.02 to 0.1 percent of the weight of reactants. The catalyst provided by the invention has the advantages of rational formula, small use amount and good catalysis effect, and contains active ingredients and the carrier; furthermore, the dispersion area of the active ingredients is enlarged, so the contact area between the active ingredients and the reactants is enlarged and the reaction speed is increased; meanwhile, the use amount of the catalyst is reduced; and yield of CBS is up to over 97 percent under the optimized reaction conditions.

Description

technical field [0001] The present invention relates to a catalyst used in the oxygen oxidation synthesis process of a rubber vulcanization accelerator DPG (chemical name is diphenylguanidine), specifically, it relates to the composition and preparation of a catalyst used in the DPG oxygen oxidation process method. Background technique [0002] Accelerator Diphenylguanidine (DPG) is a medium-speed accelerator for natural rubber and synthetic rubber, and also an activator for thiazoles, thiurams, and sulfenamides. There are plasticizers and peptizers in neoprene. It is mainly used in the manufacture of rubber products such as tires and rubber soles. It is mentioned in US1,422,506 that as early as 1869, there was a report on the preparation of accelerator DPG by PbO method, and the Pb method was also improved in the literature. However, because this method uses heavy metal Pb, it is very harmful to human body and environment, and this method has basically stopped using in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J23/75B01J23/34B01J29/48B01J29/46B01J27/25B01J27/053C07C279/18C07C277/08C08K5/31C08L21/00
Inventor 尹红伟
Owner KEMAI CHEM
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