Synthesis method of phosphate

Abstract

The invention discloses a synthesis method of phosphate. The method comprises the following steps: (1) adding organic alcohol into a reaction kettle; (2) proportionally adding phosphorus pentoxide into a feeding box, and setting the rotating speed of the feeding box, wherein the adding time of phosphorus pentoxide is controlled to be 1-3 h, a circulating pump is started in the feeding process, thespeed of circulating liquid is controlled, a plurality of small holes are formed in the surface layer of the feeding box, phosphorus pentoxide overflows from the small holes through the rotation of abox body and enters the reaction kettle to react with organic alcohol; and (3) after addition of the phosphorus pentoxide is finished, raising the temperature of the reaction kettle to 70-90 DEG C, and continuing reacting for 5-7 hours to obtain a phosphate product. According to the invention, phosphate is prepared by adopting a solvent-free method; the adding amount and quality of phosphorus pentoxide are guaranteed by controlling the adding mode of phosphorus pentoxide and setting a material circulating device; heat generated by the reaction is discharged in time, so reaction stability is guaranteed, and the prepared phosphate product is stable and high in esterification rate; and the formed system is colorless and transparent, decoloration is not needed, and the product does not contain any decolorizing agent.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing phosphoric acid esters. Background technique [0002] As an important class of surfactants, phosphate esters are widely used in the fields of chemical fiber, textile, leather, plastic, papermaking, printing and dyeing, metal processing and daily chemicals, as detergents, oils, antistatic agents, emulsifiers , liquid ion exchangers and pharmaceuticals, etc. [0003] At present, the preparation of phosphoric acid ester usually adopts the reaction preparation of alcohol and phosphorylation reagent, and the phosphorylation reagent of existing report has phosphorus trichloride, phosphorus pentoxide etc. at present, and wherein the report of phosphorus pentoxide aspect is the most also most commonly used, because five The phosphorus oxide method is simple and easy, and the yield of phosphate ester is high. Because phosphorus pentoxide is a strong ...

AI Technical Summary

Problems solved by technology

Because phosphorus pentoxide is a strong oxidizing agent and strong dehydrating agent, it is easy to produce different degrees of color changes in the reaction process, and it is easy to undergo polymerization reaction to form polyphosphoric acid by-products during the reaction, thereby affecting the use effect of the product; at the same time, Since most of the existing phosphorus pentoxide feeds are manually fed step by step, and because the reaction between organic alcohols and phosphorus pentoxide is an acylation exothermic reaction, the amount of phosphorus pentoxide added each time cannot be guaranteed, resulting in different batches of synthesis The ratio of single and double esters of phosphate esters varies greatly, and the reproducibility is poor, resulting in unstable product quality

[0004] In order to improve the color and luster of phosphate products and the problem of poor product reproducibility, most of the prior art adopts the method of adding solvent, as patent publication number CN1068599C discloses a kind of method for synthesizing colorless fatty alcohol polyoxyethylene ether phosphate, adopts fat Alcohol polyoxyethylene ether is used as a raw material, phosphorus pentoxide is added for esterification, and colorless phosphate is synthesized by adding water before the esterification; however, adding water to the reaction system will increase the phosphoric acid content in the reaction product. Affect the performance and use of phosphoric acid ester; therefore, there is an urgent need to develop a synthetic method of colorless phosphoric acid ester suitable for industrial production and with controllable ratio of single and double esters

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