A kind of preparation method of high-grade ultrafine particle aluminum diethylphosphinate

Abstract

The invention relates to a preparation method of top-grade ultrafine particle diethyl aluminum phosphinate. The preparation method comprises the following steps: by taking acetic acid as a solvent, acetone as an initiator and organic alkyl phosphinic ionic liquid modified nano titanium dioxide as a photocatalyst, carrying out concerted catalysis on addition reaction of sodium hypophosphite and ethylene to synthesize high purity diethyl sodium phosphinate; then, acidifying the high purity diethyl sodium phosphinate to obtain diethyl phosphinic acid; and finally, neutralizing the diethyl phosphinic acid by aluminum hydroxide to generate the diethyl aluminum phosphinate. The preparation method provided by the invention has the advantages that the production process comprises two steps: S1, the light-catalyzed reaction is carried out at low temperature and low pressure, so that the safety is high and byproducts are effectively avoided; concerted catalysis is used, so that the reaction time is greatly shortened and the conversion rate is extremely high; filtering is performed for removing sodium salt after acidification, so that the influence on the quality of the product is avoided, and the photocatalyst is recovered; S2, the neutralization reaction is carried out close to a condition of room temperature, so that the neutralization reaction is simple to operate and low in energy consumption; finally, the obtained white solid product is ultrafine in particle, high in purity and good in heat stability.

Description

technical field [0001] The invention relates to the preparation of a green and environment-friendly diethylphosphinate flame retardant, in particular to a preparation method of high-grade ultrafine particle aluminum diethylphosphinate. Background technique [0002] Halogen flame retardants are currently one of the most produced organic flame retardants in the world. Halogen flame retardants have the advantages of high flame retardant efficiency and low cost, but halogen-containing flame retardant materials produce smoke containing toxic and corrosive gases such as hydrogen halides when burned, which can easily poison and suffocate people at the fire scene. With the rapid development of the polymer material industry and the continuous improvement and improvement of flame retardant regulations, the demand for non-toxic, smoke-suppressing, environmentally friendly, halogen-free flame retardants is becoming more and more urgent at home and abroad. [0003] Phosphorous flame ret...

AI Technical Summary

Problems solved by technology

Although this method is compared with US6011172 and CN 1280581 report, dialkyl phosphinic acid or salt productive rate improves to some extent in the product (the molar percentage of dialkyl phosphinic acid or salt reaches about 90%), but still in the product Contains a large number of other by-products that affect the purity of the product, for example, due to the polymerization reaction due to high pressure, ethylene is used as a raw material to easily produce by-products such as butylphosphinic acid or salts

[0005] Aiming at problems such as high energy consumption and reaction system safety, patent CN 101891762A proposes a synthesis method of diethylphosphinate with the characteristics of low temperature and low pressure and high operational safety.

However, the active ingredient of the target product aluminum diethylphosphinate is low, only about 90%. The product contains aluminum monoethylphosphinate and other unidentified compounds, and these impurities will seriously affect product quality and initial decomposition temperature and other performance indicators