Preparation method of ethyl methylethyl phosphinate

A technology of ethyl methyl ethyl phosphinate and diethyl methyl phosphinate, which is applied in the field of preparation of ethyl methyl ethyl phosphinate, can solve the problem of slow reaction rate and efficiency and difficulties in scale-up , high safety risks and other issues, to achieve safe operation, facilitate large-scale industrial production, and increase the effect of warming probability

Active Publication Date: 2020-07-10
LIER CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the above problems, the invention provides a preparation method of ethyl methyl ethyl phosphinate, which has the advantages of safety and simple operation, and can be large-scale industrialized production, and solves the problems in the traditional isomerization preparation method. , Diethyl methylphosphonite is usually converted by one-pot method for isomerization. There are safety hazards in the one-pot conversion process, and the reaction rate and efficiency are relatively slow, high safety risks, and difficult to scale up.

Method used

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  • Preparation method of ethyl methylethyl phosphinate
  • Preparation method of ethyl methylethyl phosphinate
  • Preparation method of ethyl methylethyl phosphinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] MDEP: Diethyl methyl phosphonite

[0035] Using the one-pot method:

[0036] 1-0#, replace the four-necked flask with nitrogen three times, keep the bottle dry, add 80g of diethyl methylphosphinate and 80g of trimethylbenzene into the four-necked flask, take 2.4g of iodoethane with a syringe, add In the four-necked flask, the catalyst content in the system is 1.48wt%, pay attention to nitrogen protection during the process, set the temperature of the oil bath to 140°C, gradually heat up, and start timing after the temperature of the reaction system in the bottle rises to 130°C, and maintain this state About 3 hours, detected at 1 hour, the target product was 89%; detected at 2 hours, the target product was 95%; detected at 3 hours, the reactants were completely converted, and the target product was 97%. There was no obvious temperature rise during the reaction, the highest The temperature was 142°C.

[0037] For 1-1#, the proportion of catalyst content in the system w...

Embodiment 2

[0044] Add dropwise in batches, there is trimethylbenzene:

[0045] The four-neck flask was replaced with nitrogen three times to keep the inside of the flask dry. Divide 1100g of diethyl methylphosphonite into 5 parts (0#, 1#, 2#, 3#, 4#), each with an average of 220g. Add diethyl methylphosphonite 0# and 440g trimethylbenzene into the four-necked flask, take 6.6g iodoethane with a syringe, and add it into the four-necked flask, pay attention to nitrogen protection during the process. Set the temperature of the oil bath to 140°C, gradually heat up, and start timing after the temperature of the reaction system in the bottle rises to 130°C, and maintain this state for about 2 hours.

[0046] Subsequently, maintain the internal temperature of the reaction system at 130-140°C, and continuously drop diethyl methylphosphonite 1# to 4# into the reaction system using a syringe pump. Each batch of drops takes 1 hour, and each batch Start timing when dropping, and detect the content ...

Embodiment 3

[0051] Add dropwise, without trimethylbenzene, ethyl methyl ethyl phosphinate as substrate:

[0052] The four-neck flask was replaced with nitrogen three times to keep the inside of the flask dry. Divide 700g of diethyl methylphosphonite into 7 parts (0#, 1#, 2#, 3#, 4#, 5#, 8#), with an average of 100g each; in addition, prepare 2 additional parts of methylphosphonite Diethyl phosphonate, respectively 800g diethyl methylphosphonite 6# and 1500g diethyl methylphosphonite 7#. Add 100 g of ethyl methyl ethyl phosphinate into the four-necked flask, take 3 g of ethyl iodide with a syringe, and add it into the four-necked flask, paying attention to nitrogen protection during the process. Set the temperature of the oil bath to 140°C, gradually heat up until the temperature of the reaction system in the bottle rises to 130°C, then start timing, maintain the internal temperature of the reaction system at 130-140°C, and continuously add methylphosphine into the reaction system with a ...

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Abstract

The invention relates to the technical field of methyl phosphinate, and discloses a preparation method of ethyl methylethyl phosphinate. The method comprises the following steps: mixing a substrate with a catalyst, then adding diethyl methylphosphite dropwise into the reaction system, and carrying out reaction to generate ethyl methylethyl phosphinate. According to the preparation method of ethylmethylethyl phosphinate, through a dropwise adding method, the probability of temperature rush due to rising of a highest temperature can be prevented from increasing, the safety risk is effectively reduced, and large-scale industrial production is facilitated. According to the method, while the usage amount of the catalyst is effectively reduced, the reaction rate does not show a decreasing trend, the advantages of safety, simple operation and the like are achieved, the purpose of large-scale industrial production can be achieved, and the problems that potential safety hazards exist in a one-pot method conversion process, the one-pot method reaction rate and efficiency are relatively low, the safety risk is high, and large-scale amplification is difficult are solved.

Description

technical field [0001] The invention relates to the technical field of organic phosphinates, in particular to a preparation method of ethyl methyl ethyl phosphinate. Background technique [0002] Due to the high phosphorus content, organic phosphinates have good flame retardancy. At the same time, due to the introduction of alkyl groups in the molecular structure, compared with inorganic hypophosphites, their hydrophobicity and thermal decomposition temperature are greatly improved. Among molecular materials, it will not migrate and absorb moisture, can withstand high processing temperature, and will not cause the insulation performance of the material to decrease. The compatibility with the matrix resin can maintain the mechanical properties of the matrix material. Due to these characteristics as an excellent flame retardant, it has been widely used in the field of engineering plastics such as high processing temperature, high shear strength and high CTI value, especially i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/32
CPCC07F9/3264C07F9/3205Y02P20/584
Inventor 岳杰何达何航左翔程柯
Owner LIER CHEM CO LTD
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