Low-chlorine ECH-residue-free TGIC curing agent and preparation method thereof

Abstract

The invention belongs to the technical field of curing agents, and particularly relates to a low-chlorine ECH-residue-free TGIC curing agent and a preparation method thereof. According to the preparation method of the TGIC curing agent, isocyanuric acid, chloropropene, sodium carbonate, an epoxidation solvent, hydrogen peroxide and a metal catalyst are used as raw materials for preparation, TAIC is prepared through a pressurization reaction firstly, then the TAIC is subjected to a reaction in a special circulating separation reactor under the oxidation effect of relatively low-concentration hydrogen peroxide, the generated TGIC product is continuously separated from the system and then eluted with methanol to obtain the low-chlorine electronic-grade TGIC curing agent product, the yield ofthe product finally reaches 90% or above, the total chlorine content of the prepared TGIC curing agent product is 5 ppm or below, ECH residues do not exist, the epoxy equivalent is 100-103 g / mol, andthe method has better quality and application value.

Description

technical field [0001] The invention belongs to the technical field of curing agents, and in particular relates to a low-chlorine and ECH-free TGIC curing agent and a preparation method thereof. Background technique [0002] Triglycidyl isocyanurate, also known as tris (2,3-epoxypropyl) isocyanurate, referred to as TGIC, commonly known as "Bick", is an important cyanuric acid derivative. Since TGIC has three highly active epoxy groups and the triazine ring is also very stable, TGIC not only has the physical and chemical properties of general epoxy resins, but also can be used with epoxy curing agents such as amines, carboxylic acids, phenolic anhydrides, etc. It produces a curing reaction; it can also generate cross-linked insoluble and infusible materials, and the curing reaction speed is faster; and compared with the usual epoxy resin, TGIC has a low epoxy equivalent, small molecular weight, and high epoxy value. Good weather resistance, heat resistance, and adhesion, so ...

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Problems solved by technology

In order to obtain low-chlorine products with better performance, which are used in higher-end electronic packaging, flame-retardant inks and other fields, such as the traditional method of preparing electronic-grade triglycidyl isocyanurate, by using solvents for multiple recrystallization, Although the chlorine content of the product has been reduced to a certain extent, it has led to a sharp drop in product yield, and it is still unable to effectively reduce the total chlorine and ECH to the desired level for high-end electronic grade products

The synthesis method of low-chlorine TGIC that is otherwise reported in the prior art, such as "Synthesis of Triglycidyl Isocyanurate Using Hydrogen Peroxide as Epoxy Agent" in Electroplating and Finishing Magazine in 2017, needs to use concentrations as high as 40%, 50% Hydrogen peroxide solution can reach a relatively good yield (more than 80%), but the most commonly used in industry, the lowest price is that the concentration of hydrogen peroxide solution is basically 27.5% (see GB / T 1616-1988 " Industrial hydrogen peroxide"), generally more than 30% hydrogen peroxide solution is mostly controlled as explosive dangerous goods, and the high-concentration hydrogen peroxide aqueous solution has a high risk factor, which brings danger and inconvenience to industrial production and application. Moreover, The whole process needs to consume a large amount of hydrogen peroxide solution (at least a molar ratio of 1:6 or more), indicating that the utilization rate of hydrogen peroxide is low, which leads to a higher cost of epoxidation

In order to overcome the above-mentioned deficiencies that must be achieved with high-concentration hydrogen peroxide solution to achieve low-chlorinated products, in the "Preparation and Application Research of Low-Chlorine Triglycidyl Isocyanurate" published in the 2020 Coating and Protection Journal, through Use 30% hydrogen peroxide aqueous solution, and prepare under the action of catalyst, but its product yield is still only about 56%, and the required reaction time is as long as 15 hours, and the industrialization cost is relatively high

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