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Telomer of aluminum diethylphosphinate and preparation method of telomer

A technology of diethylphosphinic acid and phenylethylphosphinate, which is applied in the field of preparation of aluminum diethylphosphinate, can solve the difficulty in meeting the requirements of phosphorus-containing wastewater treatment, low light conversion efficiency, Increase the distillation to remove the acetic acid solvent link and other issues

Pending Publication Date: 2022-05-13
LANZHOU RUIPU TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such a large amount of sulfuric acid leads to a low yield when the intermediate sodium diethyl hypophosphite solution produced by this method reacts with aluminum sulfate, and the filtrate produced contains a large amount of phosphorus-containing compounds, which is difficult to achieve environmental protection for the treatment of phosphorus-containing wastewater. requirements; at the same time, this method has the following problems:
[0005] (2) The second problem with the persulfate initiating system is that its half-life is related to temperature. For example, when the commonly used potassium persulfate is at 70°C, the half-life is 7.7 hours, and at 80°C, the half-life is 1.5 hours.
This method is difficult to implement in production, and the light conversion efficiency is usually low, and it is easy to implement in the laboratory
Once the equipment is enlarged, it will bring many practical problems. For example, the stainless steel reactor needs to use quartz tubes to transmit ultraviolet rays, so sealing and pressure resistance are difficult to solve; at the same time, the system needs to use acetic acid as a solvent, which will bring production problems. Unacceptable odor during the process, increased distillation to remove acetic acid solvent, lower thermal stability of polymers in downstream use, and many other problems

Method used

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  • Telomer of aluminum diethylphosphinate and preparation method of telomer
  • Telomer of aluminum diethylphosphinate and preparation method of telomer
  • Telomer of aluminum diethylphosphinate and preparation method of telomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Sodium hypophosphite solution, configured into 227 grams per liter of solution, heated to 65 ° C, slowly added dropwise 1.5wt% acetophenone (calculated as sodium hypophosphite) and OP-10 mixture (the mixture of acetophenone and OP-10 The mass ratio is 1:1.0), after the air is replaced by nitrogen, ethylene is introduced to keep the pressure at 0.40MPa, and the microwave generator in the reactor is turned on to start the reaction. After reacting for 5 hours, every 30 minutes, start to detect whether the reaction is complete. The obtained reaction solution was raised to 90° C., and the reaction method with aluminum sulfate was the same as that of Comparative Example 1. The yield was 98% (calculated as phosphorus).

Embodiment 2

[0081] Sodium hypophosphite solution, configured into 227 grams per liter of solution, heated to 75 ° C, slowly added dropwise 4.5wt% acetophenone (calculated as sodium hypophosphite) and OP-10 mixture (the mixture of acetophenone and OP-10 The mass ratio is 1:1.0), after the air is replaced by nitrogen, ethylene is introduced to keep the pressure at 0.43MPa, and the microwave generator in the reactor is turned on to start the reaction. After reacting for 5 hours, every 30 minutes, start to detect whether the reaction is complete. The obtained reaction solution was raised to 90° C., and the reaction method with aluminum sulfate was the same as that of Comparative Example 1. The yield was 97% (calculated as phosphorus).

Embodiment 3

[0083] Sodium hypophosphite solution, configured into 227 g / L solution, heated to 85 ° C, slowly added dropwise 2.5wt% isobutyryl phenone (calculated as sodium hypophosphite) and OP-10 mixture (acetophenone and OP- The mass ratio of 10 is 1:1.0), after the air is replaced by nitrogen, ethylene is introduced to keep the pressure at 0.45MPa, and the microwave generator in the reactor is opened to start the reaction. After reacting for 5 hours, every 30 minutes, start to detect whether the reaction is complete. The obtained reaction solution was raised to 90° C., and the reaction method with aluminum sulfate was the same as that of Comparative Example 1. The yield was 98% (calculated as phosphorus).

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Abstract

The invention provides an aluminum diethylphosphinate flame retardant, which contains a telomer as shown in a structure I, in which R1 = CnH2n + 1, n = 1, 2, 3, 4, 5, 6, 7 or 8, R2 = CnH2n + 1, n = 1, 2, 3, 4, 5, 6, 7 or 8, and n = 1, 2, 3, 4, 5, 6, 7 or 8. R2 is phenyl.

Description

technical field [0001] The invention relates to a process for the preparation of aluminum diethylphosphinate which is a telomer containing at least one phenyl substituent. Background technique [0002] Aluminum diethylphosphinate is a halogen-free flame retardant with good flame retardant properties. It is widely used in polyester materials, polyamide materials, EVA materials and TPE materials by coordinating with other flame retardants. In the literature, a large number of preparation methods for this material have been reported. For example, Clariant, Guangzhou Jinkai, Shouguang Weidong Chemical Industry, Jiangsu Liside, etc. have reported a large number of diethylaluminum hypophosphite and its precursor diethyl The synthetic method of phosphinic acid sodium salt. [0003] According to public information and information published by various companies’ patents, Clariant disclosed in early patents the method of using sodium hypophosphite to react with ethylene in acetic aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
CPCC07F9/301C07F9/304
Inventor 窦伟许红卫刘鹏周玉来
Owner LANZHOU RUIPU TECH CO LTD
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