Synthesis method of phosphate

A synthesis method and phosphoric acid ester technology, which are applied in the fields of phosphorus organic compounds, chemical instruments and methods, and compounds of Group 5/15 elements of the periodic table, etc. Problems such as poor reproducibility of color and luster products, to achieve the effects of product stability, mild conditions and high esterification rate

Pending Publication Date: 2021-02-26
四川科宏达集团有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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

Method used

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  • Synthesis method of phosphate

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Example Embodiment

[0028]Example 1

[0029]A method for synthesizing phosphate ester, including the following steps: 15kg fatty alcohol polyoxyethylene ether (C12H25(OC2H4)2OH) into the reaction kettle, add 2.7kg P2O5Add the feeding box, set the temperature of the reactor to 40℃, set the feeding box rotation speed 25r / s through the smart display 7, and complete the feeding in 2 hours.2O5During the feeding process, the circulating pump is started at the same time, and the intelligent display 11 controls the speed of the circulating liquid to circulate at 8ml / s, P2O5After the addition, the temperature of the reaction kettle was increased to 70°C, and the reaction was continued for 6 hours, and the reaction was ended to obtain a colorless transparent phosphate.

[0030]QB / T 2949-2008 phosphate ester was used to determine the content of phosphate ester active substance, and the content of phosphate monoester and diester in phosphate ester was detected by potentiometric titration method in "Synthesis of Fatty Al...

Example Embodiment

[0031]Example 2

[0032]A method for synthesizing phosphate ester, including the following steps: 6.25kg fatty alcohol polyoxyethylene ether (C12H25(OC2H4)2OH) into the reactor, add 1.25kg P2O5Add the feeding box, set the temperature of the reaction kettle to 50℃, set the feeding box rotation speed 12r / s through the smart display 7, and complete the feeding in 2 hours.2O5During the feeding process, the circulating pump is started at the same time, and the intelligent display screen 11 controls the circulating fluid external circulation speed of 4ml / s, P2O5After the addition, the temperature of the reaction kettle was increased to 80° C., and the reaction was continued for 5 hours to complete the reaction to obtain a colorless phosphate.

[0033]After testing, the obtained phosphoric ester active matter content is 98.2%, of which the phosphoric acid monoester content is 33.4%, the phosphoric acid diester content is 62.7%, and the obtained phosphoric acid ester product is a colorless and tr...

Example Embodiment

[0034]Example 3

[0035]A method for synthesizing phosphate esters, including the following steps: 10kg of tristyrenol polyoxyethylene ether (C50H82O17) Into the reactor, add 2kg P2O5Add the feeding box, set the temperature of the reactor to 55℃, set the feeding box rotation speed to 18r / s through the smart display 7, and the feeding is completed in 2 hours.2O5During the feeding process, the circulating pump is activated at the same time, and the intelligent display screen 11 controls the circulating fluid external circulation speed of 6ml / s, P2O5After the addition, the temperature of the reaction kettle was increased to 85°C, and the reaction was continued for 7 hours to complete the reaction to obtain a light yellow phosphate.

[0036]After testing, the obtained phosphoric acid ester active matter content is 83.2%, of which the phosphoric acid monoester content is 27.4%, the phosphoric acid diester content is 52.1%, and the obtained phosphoric acid ester product is a light yellow soluti...

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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 ...

Claims

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Application Information

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IPC IPC(8): C07F9/09B01J19/18
CPCC07F9/091B01J19/1881
Inventor 龙平陈海刚漆锐姚永毅张豫红
Owner 四川科宏达集团有限责任公司
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