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Synthesis method of diethyl phosphite

A technology of diethyl phosphite and triethyl phosphite, which is applied in the field of synthesis of diethyl phosphite, can solve problems such as affecting product yield, increasing production cost, and increasing operational difficulties, so as to achieve low cost and avoid impurities , the effect of good purity

Pending Publication Date: 2020-11-27
LIAONING DOPP WEINONG CHEM & INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] So far, the preparation method of diethyl phosphite mainly contains two kinds, phosphorous acid and ethanol direct esterification method, phosphorus trichloride and anhydrous ethanol reaction synthesis diethyl phosphite, the first method esterification yield Low, restricted by various factors, not suitable for industrialization, the second method requires a large amount of solvent or synthesizes the target product under acidic conditions, and this method has been industrialized on a large scale, but the method is harmful to raw material PCl 3 The purity requirement is high, otherwise it will cause safety hazards; and in the production process, side reactions will occur. Therefore, after the synthesis is completed, desorption and distillation are required, which affects the yield of the product, and increases the difficulty of operation and increases the production cost.

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  • Synthesis method of diethyl phosphite

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Experimental program
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Effect test

Embodiment 1

[0022] The specific operation process of this embodiment is shown in Table 1. Take 41.5 g of triethyl phosphite and put it into a four-necked flask at room temperature of 24 ° C, and put the four-necked flask into a water bath. Add four times to the four-neck flask, the temperature of the first phosphorous acid addition is 24°C, and the amount of phosphorous acid added is 1.025g and stir for 15 minutes; due to the exothermic reaction, when the first addition and the reaction is completed, the temperature of the reaction system rises to 27°C, add 2.05g of phosphorous acid for the second time and stir for 15 minutes, the reaction system will heat up to 32°C due to the exothermic reaction, and cool down with cold water; For the third time, 3.075 g of phosphorous acid was added, and stirred for 15 minutes. The reaction system heated up to 33°C due to the exothermic reaction, and the temperature was lowered with cold water; Add 4.1g of phosphorous acid four times, and stir for 15 m...

Embodiment 2

[0026] The specific operation process of this embodiment is shown in Table 2. Take 41.5 g of triethyl phosphite and put it into a four-necked flask at room temperature of 24 ° C, and put the four-necked flask into a water bath. Add four times to the four-necked flask, the temperature of phosphorous acid added for the first time is 24°C, and the amount of phosphorous acid added is 2g and stirred for 15 minutes; due to the exothermic reaction, when the first addition and reaction are completed, the temperature of the reaction system rises to 28°C, add 2g of phosphorous acid for the second time and stir the reaction for 15 minutes, the reaction system will heat up to 33°C due to the exothermic reaction, and cool down with cold water; Add 2g of phosphorous acid three times, and stir for 15 minutes. The reaction system is heated to 33°C due to the exothermic reaction, and the temperature is lowered with cold water. When the third addition and the reaction is completed, the reaction ...

Embodiment 3

[0031] The specific operation process of this embodiment is shown in Table 3. Take 41.5 g of triethyl phosphite and put it into a four-necked flask at room temperature of 24 ° C, and put the four-necked flask into a water bath. Add four times to the four-necked flask, the temperature of phosphorous acid added for the first time is 24°C, and the amount of phosphorous acid added is 2g and stirred for 15 minutes; due to the exothermic reaction, when the first addition and reaction are completed, the temperature of the reaction system rises to 28°C, add 2g of phosphorous acid for the second time and stir the reaction for 15 minutes, the reaction system will heat up to 33°C due to the exothermic reaction, and cool down with cold water; Add 2g of phosphorous acid three times, and stir for 15 minutes. The reaction system is heated to 33°C due to the exothermic reaction, and the temperature is lowered with cold water. When the third addition and the reaction is completed, the reaction ...

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Abstract

The invention relates to a synthesis method of diethyl phosphite. The method comprises the following steps: putting triethyl phosphite into a stirring reactor; adding phosphorous acid into the stirring reactor in batches under a stirring condition; wherein the batch adding frequency is 4-5 times, the temperature is controlled to be less than or equal to 35 DEG C in the phosphorous acid batch adding process, the temperature is kept at 50-60 DEG C for 30 minutes after phosphorous acid is added, then the temperature is increased at 2.5-5 DEG C / h, the temperature is gradually increased at 60-90 DEG C, and the reaction is carried out for 3-5 hours to obtain diethyl phosphite. The method is prepared by directly reacting triethyl phosphite with phosphorous acid, does not need a solvent or a catalyst in comparison with the traditional process, and is mild in reaction and higher in yield, and the yield can reach 97-99%; no side reaction occurs in the reaction process, the product purity is goodand can reach 99% or above, and the method is low in cost, safe, environmentally friendly and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of organic synthesis of fine chemical intermediates, in particular to a method for synthesizing diethyl phosphite. Background technique [0002] Diethyl phosphite is an important organic synthesis intermediate, which can be used as an intermediate to make flame-retardant plasticizers; it can also be used to prepare organophosphorus insecticides and acaricides; it can also be used to prepare phosphate esters and Made of metal corrosion inhibitor. [0003] So far, the preparation method of diethyl phosphite mainly contains two kinds, phosphorous acid and ethanol direct esterification method, phosphorus trichloride and anhydrous ethanol reaction synthesis diethyl phosphite, the first method esterification yield Low, restricted by various factors, not suitable for industrialization, the second method requires a large amount of solvent or synthesizes the target product under acidic conditions, and this method has been ind...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/142
CPCC07F9/142
Inventor 姜长新费存
Owner LIAONING DOPP WEINONG CHEM & INDAL
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