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Preparation method of halogen-free retardant dimethyl methylphosphonate

A technology of dimethyl methylphosphonate and flame retardant, which is applied in the field of preparation of halogen-free flame retardant dimethyl methylphosphonate, can solve the problems of high toxicity of methyl iodide, restriction of industrialization, and high cost, and achieve raw material Low cost, easy operation and protection, low cost effect

Inactive Publication Date: 2012-10-03
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the toxicity of methyl iodide is relatively large and the cost is high, the industrialization of this method is greatly limited.

Method used

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  • Preparation method of halogen-free retardant dimethyl methylphosphonate
  • Preparation method of halogen-free retardant dimethyl methylphosphonate
  • Preparation method of halogen-free retardant dimethyl methylphosphonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A preparation method of halogen-free flame retardant methyl methyl phosphonate, it comprises the steps:

[0026] Put the three-necked flask and trimethyl phosphite (TMP) into the refrigerator, treat at 0°C, and then add trimethyl phosphite (TMP) and catalyst p-toluenesulfonate to the three-necked flask under the protection of nitrogen Add 50g and 4g of the two (mass ratio is 100:8), put the three-necked flask in an oil bath, install the stirrer, condenser tube and thermometer, start stirring, and the whole reaction is under the protection of nitrogen conduct;

[0027] Under the condition of stirring, when the temperature is gradually raised to 110°C, reflux begins to appear, and a steady and continuous reflux is maintained for 30 minutes; then the reflux gradually subsides, and then the temperature is gradually raised to 150°C, and a stable and continuous reflux continues, and the temperature is maintained at 150°C , continued for 15 minutes, and after the reflux was c...

Embodiment 2

[0030] A preparation method of halogen-free flame retardant methyl methyl phosphonate, it comprises the steps:

[0031] Put the three-necked flask and trimethyl phosphite (TMP) into the refrigerator, treat at 0°C, and then add trimethyl phosphite (TMP) and catalyst p-toluenesulfonate to the three-necked flask under the protection of nitrogen Add 50g and 5g of methyl ester to the two (mass ratio is 100:10), put the three-necked flask in an oil bath, install the stirrer, condenser and thermometer, start stirring, and the whole reaction is under the protection of nitrogen conduct;

[0032] Under the condition of stirring, when the temperature is gradually raised to 115°C, reflux begins to appear and maintains a stable and continuous reflux for 30 minutes; then the reflux gradually subsides, and then gradually increases the temperature to 150°C, and continues to appear stable and continuous reflux, keeping the temperature at 150°C , continued for 15 minutes, and after the reflux ...

Embodiment 3

[0035] A kind of preparation method of halogen-free flame retardant methyl methyl phosphonate, it comprises the steps:

[0036] Put the three-necked flask and trimethyl phosphite (TMP) into the refrigerator, treat at 0°C, and then add trimethyl phosphite (TMP) and catalyst p-toluenesulfonate to the three-necked flask under the protection of nitrogen Add 50g and 6g respectively of the two, (mass ratio is 100:12), put the three-necked flask in an oil bath, install the stirrer, condenser tube and thermometer, start stirring, and the whole reaction is under the protection of nitrogen under;

[0037] Under the condition of stirring, when the temperature is gradually raised to 120°C, reflux begins to appear and maintains a stable and continuous reflux for 30 minutes; then the reflux gradually subsides, and then gradually increases the temperature to 150°C, and then continues to appear stable and continuous reflux, keeping the temperature at 150°C , continued for 15 minutes, and aft...

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Abstract

The invention relates to a preparation method of halogen-free retardant dimethyl methylphosphonate. The preparation method comprises the steps of 1) treating a three-mouth flask and trimethyl phosphate (TMP) at 0 DEG C; adding the trimethyl phosphate (TMP) and the catalyst p-toluenesulfonic acid methyl into the three-mouth flask under protection of nitrogen according to the mass ratio of 100:(8-12); putting the three-mouth flask to oil bath, installing a condenser pipe, starting to stir, performing the whole reaction under protection of nitrogen; 2) heating up to 18-200 DEG C with stirring; reacting for 9-13 hours, cooling to room temperature, using the oil bath to warm; and performing reduced pressure distillation, collecting fraction at 105-110 DEG C, namely, dimethyl methylphosphonate. The catalyst adopted by the method is environment-friendly catalyst p-toluenesulfonic acid methyl, which can be used repeatedly, so that the cost is low; the product dimethyl methylphosphonate is separated easily, so that the yield is high; according to the method, the synthetic process is simple, the material cost is low, and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a preparation method of a halogen-free flame retardant dimethyl methylphosphonate. Background technique [0002] Due to the serious environmental pollution of organic halogen-based flame retardants, new flame retardants have become a hot research topic, among which dimethyl methylphosphonate (DMMP) is a new type of phosphorus-based environmentally friendly flame retardant. Flame retardancy, water solubility and compatibility are good, and it has the advantages of low price and smokeless, so it is favored by people and is widely used in the flame retardant treatment of various polymer materials. Its application range has penetrated into All aspects of commercial entertainment, industrial production and people's life. After the product is added with DMMP, its self-extinguishing property, plasticity, low temperature resistance, ultraviolet stability, water drainage and antistatic property are superior to other commonly used flame...

Claims

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Application Information

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IPC IPC(8): C07F9/40C08L67/06C08K13/04C08K7/14C08K5/5333
Inventor 高山俊车绪新孟泉王柱
Owner WUHAN UNIV OF TECH
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