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Novel 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 the problems of low esterification yield, high purity requirements, and inapplicability to industrialization, so as to reduce production costs, The effect of simple operation and low cost

Active Publication Date: 2021-09-14
LIAONING DOPP WEINONG CHEM & INDAL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 and a large amount of by-product hydrochloric acid will be produced. Therefore, after the synthesis is completed, desorption and distillation are required. Incomplete treatment will directly lead to the acid value of the product. Exceeding the standard will affect the yield of the product, and increase the difficulty of operation and increase the production cost

Method used

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  • Novel synthesis method of diethyl phosphite
  • Novel synthesis method of diethyl phosphite

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Effect test

Embodiment 1

[0023] The specific operation process of this embodiment is shown in Table 1. 170 g (1 mol) of triethyl phosphite was put into the reaction flask, heated to 70-80° C., and 18 g (1 mol) of water was added dropwise to carry out the hydrolysis reaction. The dropping rate is controlled at about 1 hour, and the dropwise addition is completed and the temperature is maintained for 1 hour for analysis, and the remaining 0.24% of the raw material is subjected to vacuum distillation. The vacuum degree is 0.095Mpa. When the material temperature in the flask reaches 118°C, the distillation is stopped, and the reaction flask is pressurized to normal pressure with nitrogen. After the completion of the reaction and product recovery, 139.4 g of 99.52% diethyl phosphite was obtained, and the yield was 99.3%. The remaining mother liquor in the bottle is the product except trace impurities. The remaining mother liquor in the bottle is the product except trace impurities. The gas chromatogram o...

Embodiment 2

[0028] In this embodiment, the raw materials are put into the reaction bottle at one time, and the rest of the feeding amount, raw material ratio, etc. are carried out according to the general steps of Example 1. The actual yield of diethyl phosphite was 99.1%, and the purity was 99.11%.

Embodiment 3

[0030] Before dropping into new triethyl phosphite and water in the reaction flask, do not remove the remaining raffinate from the distillation of example 1 from the reaction flask, and the others are carried out by implementing the 2 conditions. The actual yield of diethyl phosphite was 99.2%, and the purity was 99.21%.

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Abstract

The invention relates to a synthesis method of diethyl phosphite. The method comprises the following steps: taking and putting triethyl phosphite into a stirring reactor, heating the stirring reactor to 70-80 DEG C within 30-60 minutes, adding water into the stirring reactor under the stirring condition, raising the temperature, and carrying out a reaction, wherein the molar ratio of the triethyl phosphite to the water is 1:1; keeping the temperature for 60 minutes after the water is completely added, carrying out chromatographic analysis, controlling the triethyl phosphite to be less than or equal to 0.3%, opening a receiving bottle, and carrying out reduced-pressure rectification to remove low-boiling-point ethanol; and stopping rectification, and pressurizing the reaction bottle to normal pressure by using nitrogen to obtain the diethyl phosphite. According to the method, triethyl phosphite and water directly react to prepare triethyl phosphate, compared with a traditional process, a solvent and a catalyst are not needed, the reaction is mild, the yield is high, the yield can be larger than or equal to 99%, raw materials are easily available, and the production cost can be effectively reduced; and the method is easy to operate, free of side reaction in the reaction process, good in product purity, low in cost, safe, environmentally friendly and suitable for industrial production, and the purity of the product can reach 99% or above.

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 费存姜长新
Owner LIAONING DOPP WEINONG CHEM & INDAL