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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 phosphorus trichloride to generate phosphorus oxychloride intermediate or phosphorous oxychloride intermediate and hydrogen chloride, and the second step is the intermediate body and metal alkoxide reaction to generate cyclic phosphoric acid ester or cyclic phosphite and metal chloride salt, the hydrogen chloride and metal chloride salt produced by this method need to be post-treated, and the process route is complicated

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

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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

technical field [0001] The invention relates to a preparation method of cyclic phosphate or cyclic phosphite. Background technique [0002] At present, organophosphorus flame retardants have the advantages of high efficiency, low smoke, low toxicity, etc., and have dual functions of flame retardancy and plasticization. In addition to the advantages of high efficiency and no pollution to the environment, cyclic phosphate flame retardants or cyclic phosphite flame retardants also have high thermal stability due to the ring structure in the molecule. At the same time, it is beneficial to the formation of the carbon layer, so it has great development prospects. Such cyclic phosphates or cyclic phosphites can be widely used in epoxy resins such as ABS, polycarbonate, epoxy resin and polyethylene terephthalate. As a flame retardant, it has remarkable flame retardant effect and good plasticizing effect. In addition, it can also be used as lubricant, high temperature lubricating a...

Claims

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Application Information

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IPC IPC(8): C07F9/6571C07F9/6574
CPCC07F9/6571C07F9/65742
Inventor 杨锦飞谢唯佳职慧珍黄小冬赵新叶
Owner NANJING NORMAL UNIV CHANGZHOU INST OF INNOVATION & DEV
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