Preparation method for flame retardant diethyl allylphosphonate

A technology of diethyl allyl phosphonate and flame retardant, which is applied in the field of preparation of flame retardant diethyl allyl phosphonate, can solve problems such as inability to be widely used, no suitable preparation method, etc., and achieves easy scale Chemical production, good application and development prospects, and the effect of improving the reaction yield

Active Publication Date: 2014-06-25
SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it cannot be widely used because there is no preparation method suitable for industrialization.

Method used

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  • Preparation method for flame retardant diethyl allylphosphonate
  • Preparation method for flame retardant diethyl allylphosphonate
  • Preparation method for flame retardant diethyl allylphosphonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1 Set up the device of the 250mL four-neck flask equipped with agitator, thermometer, high-efficiency reflux condenser and ethyl chloride collector, replace the air in the device with nitrogen, add 150ml of chlorobenzene, 16.6g (0.1mol) Triethyl phosphite, 0.1g KI and 0.01g hydroquinone, raise the temperature to 130°C, within 5h, uniformly inject 9.2g (0.12mol) of allyl chloride with a micropump under the liquid surface. After the injection is completed, keep the reaction at 130°C for 4 hours, distill and recover the excess chloropropene, and then distill off the solvent under reduced pressure (for recycling) to obtain the product diethyl allyl phosphonate. Its yield is 74.7%, boiling point: 223°C, refractive index: n D 20 =1.4340, density (25°C): 1.035g / cm 3 .

Embodiment 2

[0027] Example 2 Set up a 250mL four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and an ethyl chloride collector, replace the air in the device with nitrogen, add 150ml of diethylene glycol dimethyl ether, 16.6 g (0.1mol) triethyl phosphite, 0.1g NaI and 0.01g hydroquinone, raise the temperature to 130°C, within 5h, uniformly inject 10.72g (0.14mol) allyl chloride with a micropump under the liquid surface. After the injection is completed, raise the temperature to 140°C, keep it warm for 4 hours, recover excess chloropropene by distillation, and then remove the solvent by distillation under reduced pressure (for recycling) to obtain the product diethyl allyl phosphonate. Its yield is 82.5%, boiling point: 223°C, refractive index: n D 20 =1.4340, density (25°C): 1.035g / cm 3 .

Embodiment 3

[0028] Embodiment 3 Set up the device of the 250mL four-neck flask equipped with agitator, thermometer, high-efficiency reflux condenser and ethyl chloride collector, replace the air in the device with nitrogen, add 100mlDMF, 16.6g (0.1mol) phosphorous acid Triethyl ester, 0.2g CuCl and 0.01g hydroquinone, raise the temperature to 130°C, within 6h, uniformly inject 12.25g (0.16mol) of chloropropene with a micropump under the liquid surface. After the injection is completed, raise the temperature to 150°C, keep the temperature for 5 hours, and recover excess chloropropene by distillation, and then remove the solvent by distillation under reduced pressure (recycling) to obtain the product diethyl allyl phosphonate. Its yield is 85.6%, boiling point: 223°C, refractive index: n D 20 =1.4340, density (25°C): 1.035g / cm3 .

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Abstract

The invention relates to a preparation method for a flame retardant diethyl allylphosphonate. The method comprises the following steps: adding an organic solvent, triethyl phosphate, an appropriate amount of catalyst and trace polymerization inhibitor hydroquinone into a reaction device, rising a temperature to 130 DEG C, uniformly injecting chloropropene with a molar weight which is 1-2 times of the molar weight of triethyl phosphate in a micro pump under a liquid level within 5-7 hours, after the injection is finished, rising the system temperature to 130-170 DEG C, carrying out thermal reaction for 4-6 hours, distilling to recover excessive chloropropene, and then carrying out reduced pressure distillation to remove the solvent, so as to obtain the product, namely diethyl allylphosphonate. The preparation method for the flame retardant diethyl allylphosphonate disclosed by the invention is high in product yield, capable of realizing a normal-pressure reaction, simple to operate, easy in product separation and purification, low in equipment investment, easy for large-scale production, and great in application and development prospect.

Description

technical field [0001] The invention relates to a method for preparing a flame retardant diethyl allyl phosphonate. The compound is a reactive organic phosphine flame retardant and is suitable for use as a flame retardant for materials such as unsaturated resins and polyolefins. Background technique [0002] In recent years, with the enhancement of people's awareness of fire safety and the increasing requirements for flame retardant materials, the development of flame retardants and flame retardant materials has been promoted. Its development trend is to improve the flame retardant performance while also requiring good mechanical properties of the material, and paying more attention to environmental protection and ecological safety. [0003] At present, halogen-based flame retardants and phosphorus-based flame retardants are the two types of flame retardants with the widest application range and high comprehensive cost performance. However, when a fire occurs, halogen-contai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40C08K5/5333C08L101/02
Inventor 王彦林俞春雷顾勇燕
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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