Preparation method of long-acting p-phenylenediamine anti-aging agent

Abstract

The invention discloses a preparation method of a long-acting p-phenylenediamine anti-aging agent. The preparation method comprises the following steps: (1) mixing a silane coupling agent with N-phenyl-p-phenylenediamine according to a ratio of (0.6-1.4):1 to obtain a mixed solution A; (2) mixing the mixed solution A, an organic solvent and a catalyst according to a weight ratio of 1:(5-10):(0.0005-0.005), then carrying out heating to 50-80 DEG C, and carrying out a reaction for 15-60 minutes to obtain a mixed solution B; (3) mixing the mixed solution B with inorganic filler at a high mixing rate according to a weight ratio of (0.1-1):1 to obtain a mixture C; and (4) drying the mixture C to obtain a final product. The long-acting p-phenylenediamine anti-aging agent prepared by the method provided by the invention is connected to inorganic filler through chemical bonds, and the long-term protective effect is excellent; the silane coupling agent exists on the inorganic filler, and unevendistribution is avoided; and the reaction time of the silane coupling agent with the N-phenyl-p-phenylenediamine is short, and is only 15-60 minutes.

Description

technical field [0001] The invention belongs to the field of rubber antiaging agents, and in particular relates to a preparation method of long-acting p-phenylenediamine antiaging agents. Background technique [0002] Traditional anti-aging agents are all small molecules, which are volatile and easy to migrate during processing and use, resulting in a decrease in the concentration of effective anti-aging agents in the product, which is not conducive to the long-term protection of rubber products, and the migration of anti-aging agents It also pollutes the environment and endangers human health. In view of the above-mentioned shortcomings of traditional small molecule antiaging agents, long-acting antiaging agents have attracted people's attention. There are several ways to prepare long-acting antiaging agents: (1) increase the molecular weight of antiaging agents, (2) ) Grafting the anti-aging agent on the molecular chain of the polymer matrix, and (3) grafting the anti-agi...

AI Technical Summary

Problems solved by technology

These three methods have their own shortcomings and problems: simply increasing the molecular weight of the anti-aging agent will reduce the proportion of effective anti-aging groups and is not conducive to the uniform dispersion of the anti-aging agent, resulting in a decrease in the protective efficiency of the anti-aging agent; Branching on the molecular chain of the polymer matrix will not only affect the uniform dispersion of the anti-aging agent, but also affect the network structure of the rubber, so the anti-aging efficiency is not high, and it will also affect the performance of the rubber; grafting the anti-aging agent on the surface of the filler, this This method will affect the interaction of rubber and filler to a certain extent

[0003] Patent CN 107118391 A discloses a preparation method of a modified anti-aging agent, which is to mix the anti-aging agent with activated carbon, which is just a simple physical adsorption, and the anti-aging agent is easy to detach when the rubber is mixed and sheared at high speed. Attached, resulting in poor long-term protection effect; patent CN 104877178 A and patent CN 106084353 A disclose the use of halloysite and carbon nanotubes to absorb anti-aging agents, halloysite and carbon nanotubes are nano-scale tubular structures, completely entering the The anti-aging dose in the anti-aging agent is relatively small, and the long-term protection effect is not good; patent CN 106750523 A and patent CN 107641325 A disclose anti-aging agent to increase the molecular weight of anti-aging agent by chemical method, which is not conducive to the uniform dispersion of anti-aging agent, resulting in anti-aging agent The protection efficiency is reduced; the patent CN 103396592 A discloses a load-type anti-aging agent, the anti-aging agent is connected to the inorganic filler through chemical bonds, and the long-term protection effect is excellent, but the preparation process is cumbersome and takes a long time, and only the reaction time requires 10~20h