Method for preparing cyclic phosphate or cyclic phosphite

A technology of cyclic phosphite and cyclic phosphate, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as complex process routes and difficult handling of hydrogen chloride, Achieve the effect of simple process, low cost and high product quality

Inactive Publication Date: 2018-11-30
NANJING NORMAL UNIV CHANGZHOU INST OF INNOVATION & DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Cyclic phosphate or cyclic phosphite currently adopts the following main methods, one of which is the reaction of phosphorus oxychloride or phosphorus trichloride with alcohol to generate cyclic phosphate or cyclic phosphite in two steps and hydrogen chloride, the hydrogen chloride produced by this method is difficult to handle; the second step is that alcohol reacts with phosphorus oxychloride or phosphor

Method used

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  • Method for preparing cyclic phosphate or cyclic phosphite
  • Method for preparing cyclic phosphate or cyclic phosphite
  • Method for preparing cyclic phosphate or cyclic phosphite

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 0.1 mol of phosphoric acid triester and 0.13 mol of neopentyl glycol into a four-necked flask equipped with a thermometer, an electric stirrer, and a reflux condenser, wherein the mass of 0.13 mol of neopentyl glycol is 13.52 g, and the temperature is raised to 140 ° C. Then add 0.068g of catalyst triethylamine, keep warm at 140-150°C for 9h; collect by-products, and distill off unreacted substances under reduced pressure after the reaction to obtain a light yellow liquid product with a yield of 81.3%.

[0026] The structural formula of the product obtained in the present embodiment is as follows:

[0027]

Embodiment 2

[0029] The 0.1 mol phosphotriester in Example 1 was replaced with 0.1 mol phosphite triester, and the others were the same as in Example 1, and the yield was 81.3%.

[0030] The structural formula of the product obtained in the present embodiment is as follows:

[0031]

Embodiment 3

[0033] Add 0.1moL of phosphoric acid triester and 0.10moL of ethylene glycol into a four-neck flask equipped with a thermometer, an electric stirrer, and a reflux condenser. Among them, the mass of 0.10moL of ethylene glycol is 6.21g, raise the temperature to 110°C, and then add Catalyst triethylamine 0.062g, heat preservation reaction at 110-130° C. for 5 hours, collect by-products, remove unreacted substances by vacuum distillation after the reaction, and obtain a light yellow liquid product with a yield of 81.3%.

[0034] The structural formula of the product obtained in the present embodiment is as follows:

[0035]

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Abstract

The invention discloses a method for preparing cyclic phosphate or cyclic phosphite. The method comprises the steps: (1) mixing a substance A with an alcoholic compound so as to obtain a mixture, andthen, heating the temperature of the mixture to 110 DEG C to 150 DEG C, wherein the substance A is triphosphate or triphosphite; (2) adding an organic amine catalyst into the mixture, and carrying outan ester exchange reaction for 5 to 9 hours so as to obtain a prepared substance, wherein the prepared substance is cyclic phosphate when the substance A is triphosphate, and the prepared substance is cyclic phosphite when the substance A is triphosphite; (3) carrying out distillation to remove impurities. According to the method, the cyclic phosphate or cyclic phosphite is synthesized in one step by adopting an ester exchange process by adopting organic amine as the catalyst, a solvent is not used, aftertreatment is not required, byproducts can be recycled, and the process route is simple.

Description

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Claims

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Application Information

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Owner NANJING NORMAL UNIV CHANGZHOU INST OF INNOVATION & DEV
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