Method for preparing tri(1,3-dichloro-2-propyl) phosphonate

Abstract

The invention provides a method for preparing tri(1,3-dichloro-2-propyl) phosphonate, which relates to the technical field of a preparation method of a fire retardant. The method adopts a self-made catalyst, and uses phosphorus oxychloride and 1,3-dichloro-2-propanol as a raw material, and adopts the following steps: phosphorus oxychloride, 1,3-1,3-dichloro-2- propanol and the self-made solid acidcatalyst are added to a reaction kettle, the materials are heated to the temperature of 100-160 DEG C for 4-6 hours, the generated hydrogen chloride gas is distilled under vacuum of -0.2-0 MPa, a crude product is washed with alkali, washed with water, and is subjected to underpressure distillation to remove water. A reaction equation is shown as the specification. The raw materials of the invention are easy to obtain, the catalyst has good catalytic performance, the product has high purity, the yield is high, the reaction is mild, the operation is simple, and the product is more suitable forindustrial production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and specifically relates to a method for synthesizing phosphonic acid tris(1,3-dichloro-2-propyl) by using a self-made solid acid catalyst to catalyze the reaction of phosphorus oxychloride and 1,3-dichloro-2-propanol ) Preparation method of ester. Background technique [0002] Phosphonic acid tris (1,3-dichloro-2-propyl) ester is an additive general-purpose chlorine-containing and phosphorus-containing flame retardant. Compression performance, the halogen atoms generated by decomposition at high temperature have the function of trapping and burning active free radicals, making highly active hydroxyl or hydrogen atoms generate water or hydrogen, thereby interrupting the chain oxidation reaction. And the thermal decomposition of tris(1,3-dichloro-2-propyl) phosphonate can be converted into glassy polymetaphosphonic acid, forming a solid charcoal layer on the surface of the material to insulate a...

AI Technical Summary

Problems solved by technology

This type of preparation method has serious disadvantages: first, the catalyst itself is unstable, easily decomposed in the air, difficult to separate after the reaction, the catalyst cannot be recycled and reused, and pollutes the environment; secondly, epichlorohydrin is 1,3-di The product of cyclization of chloro-2-propanol is volatile, unstable, potentially carcinogenic, and flammable. Its vapor and air can easily form explosive mixtures, and the reaction between epichlorohydrin and phosphorus oxychloride is an exothermic reaction , has higher requirements on temperature, when the temperature is low, it is easy to accumulate, and when it reaches a certain amount, it is easy to react instantaneously and cause bumping phenomenon, and epichlorohydrin is prone to self-polymerization reaction, resulting in high color of the product and more by-products , low raw material utilization

Again, epichlorohydrin is added dropwise, which is complicated to operate

[0004] Yu Chunhong et al. improved the reaction catalyst by using rare earth solid superacid SO 2- 4 / TiO 2 -Al 2 o 3 / La 3+ Catalyst catalyzes the reaction of epichlorohydrin and phosphorus oxychloride to synthesize phosphonic acid tris (1,3-dichloro-2-propyl) ester. The catalyst has good stability, is easy to recycle and can be reused, but epoxy chloride There are many by-products in the reaction between propane and phosphorus oxychloride, the utilization rate of raw materials is low, and the product quality needs to be improved, which is not conducive to industrial production