Method for rectifying dimethyl phosphite

A dimethyl phosphite and rectification technology, which is applied in the field of synthesis and preparation of pharmaceutical intermediates, can solve problems such as difficult industrial production, complex reactant components, and low equipment utilization, and achieve good product quality and low cost , the effect of short production time

Active Publication Date: 2018-02-23
HENAN HDF CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The specific methods are: solvent reaction and solvent-free reaction. The specific methods include vapor-liquid reaction, vapor-vapor reaction, discontinuous method, continuous method, etc. Since the reaction is a violent exothermic reaction, the reaction speed is fast, and it is completed in an instant. Discontinuous method operation Frequent, labor-intensive, long production cycle, low equipment utilization, limited production capacity
Due to the complex components of reactants, high boiling point of the mixture, strong corrosiveness, difficult separation, high energy consumption, low processing capacity, and complicated equipment, it is difficult to adapt to large-scale industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of rectification method of dimethyl phosphite,

[0019] Specific steps are as follows:

[0020] Add methanol 1800L and phosphorus trichloride 1620 into the esterification reaction kettle at a volume ratio of 1:0.9 at a flow rate of 71L / min and 50L / min respectively, start stirring, and slowly heat up. After a period of reaction, pass a sampling port and take a sample for TLC Detect until the raw materials are completely reacted, and the crude product of dimethyl phosphite is obtained after the reaction is completed.

[0021] Put the reacted crude ester into the rectification kettle for rectification. (The height of the first rectification tower is 4m, and the height of the second rectification tower is 8m). Turn on the stirring and slowly raise the temperature. When the first rectification tower and the second rectification tower reach the set temperature, turn on the condensate gas At the same time, open the circulating hot water for cooling of the top condense...

Embodiment 2

[0023] A kind of rectification method of dimethyl phosphite,

[0024] Specific steps are as follows:

[0025] Add methanol 1800L and phosphorus trichloride 1620L phosphorus trichloride to the esterification reactor at a flow rate of 71L / min and 50L / min respectively according to the volume ratio of 1:0.9, start stirring, slowly raise the temperature, and after a period of reaction, pass a sample Take a sample for TLC detection until the reaction of the raw materials is complete, and the crude product of dimethyl phosphite is obtained after the reaction ends.

[0026] Put the reacted crude ester into the rectification kettle for rectification. (The height of the first rectification tower is 5m, and the height of the second rectification tower is 9m). Turn on the stirring and slowly raise the temperature. At the same time, open the circulating hot water for cooling of the top condenser of the second rectification tower, start the vacuum system, open the reflux ratio regulator o...

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Abstract

The invention relates to a method for rectifying dimethyl phosphite. The method comprises the following steps that after raw materials are fully reacted in an esterification reaction kettle, crude ester enters the rectification kettle, a first rectifying tower and a second rectifying tower are arranged at the top of the rectifying kettle, and the first rectifying tower and the second rectifying tower are continuously heated; the first rectifying tower firstly collects low-boiling-point substances in the materials into a low-boiling-point substance storage tank, and tower bottom discharge liquid enters the second rectification tower for further separation; a vacuum unit is started for vacuum concentration, high-purity dimethyl phosphate is collected into a product storage tank, and tower bottom residual liquid is high-boiling-point substances. The technical process is simple, the production time is short, the product purity is high, the yield is high, continuous production can be achieved, the cost is low, the fuel utilization rate is high, emission is basically avoided, the environmental pollution is small, the reaction operation safety is high, the labor intensity is low, the labor efficiency is high, the product quality is good, and industrialization is facilitated.

Description

technical field [0001] The invention belongs to the field of synthesis and preparation of pharmaceutical intermediates, in particular to a rectification method of dimethyl phosphite. Background technique [0002] Dimethyl phosphite, molecular formula C 2 h 7 o 3 P, molecular weight 110.05, appearance is a colorless transparent liquid with a slight fragrance, boiling point is 170°C, relative density is 1.20, soluble in water, easily soluble in most organic solvents such as alcohol and ether. Commonly used as lubricating oil additives, adhesives and some organic synthesis intermediates. It is used in the synthesis of insecticides omethoate, methylthiocyclophos and herbicide glyphosate, etc. It has a wide range of uses. With the continuous expansion of domestic production scale of alkyl ester method glyphosate, the demand for dimethyl phosphite increases sharply. The traditional refining method of batch distillation is facing a severe test. [0003] The synthesis of dime...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/142
CPCC07F9/142
Inventor 韩永胜徐建生孙晓峰范红奎韩金豹
Owner HENAN HDF CHEM CO LTD
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