Preparation method of flame retardant TCPP (testosterone cyclopentylpropionate)

Abstract

The invention discloses a preparation method of a TCPP (testosterone cyclopentylpropionate) flame retardant, which is characterized in that a programmed heating method is used in the reaction process of phosphorus oxychloride and propylene oxide, thus obtaining an intermediate product of which the product mass yield is above 93% and the impurity content is below 3.0%; in the post-treatment process, the intermediate product is treated by organic peroxide, thus ensuring that aldehyde substances in the intermediate product are oxidized into acidic substances through the oxidizability of the peroxide; and in the subsequent treatment process, procedures of alkali washing, water washing, dewatering under reduced pressure and the like are performed to obtain a low-odor product. According to the invention, process conditions and flows of the reaction are optimized, and the acidic products obtained through oxidization and the residual peroxide have good water solubility, so that the acidic products and the peroxide can be easily removed in the subsequent procedures, thereby achieving the purpose of effectively removing odor and impurities; and the consumption of washing water can be reduced, thereby decreasing the discharge of waste water. Through the subsequent procedures of alkali washing, water washing, dewatering, filtering and the like, the content of aldehyde substances can be optimally reduced to 10ppm or below, and the product almost has no odor.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a preparation method of a flame retardant TCPP, in particular to a preparation method capable of effectively removing odorous aldehyde compounds in the phosphorus flame retardant TCPP. Background technique [0002] Tris-(2-chloroisopropyl) phosphate (TCPP) is a phosphorus-halogen flame retardant, mainly used for flame retardant of soft and hard polyurethane foam, epoxy resin, polystyrene, phenolic plastic and other materials, and its production process The crude product is obtained by reacting phosphorus oxychloride with propylene oxide at 20-80°C under the catalysis of Lewis acid such as titanium tetrachloride. The crude product is washed with acid and alkali to remove the catalyst, then washed with water and decompressed. Obtained after dehydration. During the reaction process, some propylene oxide will be oxidized into aldehyde compounds. The content of these aldehyde com...

AI Technical Summary

Problems solved by technology

When these products are added as additives to polyurethane foam or plastics, it can cause products made of these materials to emit an unpleasant smell that cannot be easily removed for a long time

[0003] In the existing disclosed technology, such as CN101007952A, utilize hydroxylamine hydrochloride as a deodorant to remove the odor in TCPP, the hydroxylamine hydrochloride that this method adopts is incompatible with the product, resulting in slow reaction and incomplete deodorization; CN101775031A uses The aqueous solution of high-valence oxides or peroxides and their salts composed of Mn, Cr, Fe, O, S, Cl, Br, I and other elements removes the odor in TCPP. The peroxides used in this method are Inorganic substances are also incompatible with the product, resulting in slow reaction and incomplete deodorization; CN102002068A directly uses ozone to oxidize odorous aldehydes to achieve the purpose of deodorization. This method requires a special ozone generator, increasing The equipment investment increases the production cost, and the compatibility between gaseous ozone and the product is also poor, and the dosage is not easy to control, which affects the deodorization effect to a certain extent