Supercharge Your Innovation With Domain-Expert AI Agents!

Preparation method of aluminum diethylphosphinate

A technology of aluminum dipropyl phosphinate and dipropyl phosphinic acid is applied in the field of preparation of green and environment-friendly dipropyl phosphinate flame retardants, which can solve the problems of high energy consumption, high temperature and affecting product quality. and initial decomposition temperature, etc., to achieve the effects of low energy consumption, temperature reduction, and low cost

Active Publication Date: 2014-05-07
山东兄弟科技股份有限公司
View PDF8 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the temperature required for the reaction system is generally high, and the energy consumption is large. At the same time, due to the high pressure, the polymerization reaction occurs. For example, by-products such as butylphosphinic acid or salt are easily produced when ethylene is used as the raw material. These impurities will seriously affect the product. Performance indicators such as quality and initial decomposition temperature

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A preparation method for aluminum dipropylphosphinate, comprising the steps of:

[0018] 1) Dissolve 106g of sodium hypophosphite monohydrate in 600ml of acetic acid and stir thoroughly to obtain an acetic acid solution of sodium hypophosphite, then move it to a 2L photoreactor, add 0.2g of nano-ZnO and vigorously stir, pass through at 50°C Add propylene, and reach saturation, then turn on the ultraviolet lamp, react for 15h, the resulting reaction mixture is carried out 31 P NMR spectrum (CDCCl 3 ) characterization analysis, the data show that the content of sodium di-n-propylphosphinate reaches 90% (molar percentage), the content of sodium diisopropylphosphinate reaches 6.7%, and the content of sodium mono-n-propylphosphinate is 2.6%. Sodium isopropylphosphinate is 0.7%, no sodium hypophosphite;

[0019] 2) Dilute the above mixed solution with water to a concentration of 0.5 mol / L containing sodium dipropylphosphinate (including sodium di-n-propylphosphinate and sod...

Embodiment 2

[0024] A preparation method for aluminum dipropylphosphinate, comprising the steps of:

[0025] 1) Dissolve 212g of sodium hypophosphite monohydrate in 1200ml of acetic acid and stir thoroughly to obtain an acetic acid solution of sodium hypophosphite, then move it to a 2L photoreactor and add 1.2g of nano-WO 3 And carry out vigorous stirring, pass through propylene at 60 ° C, and reach saturation, then turn on the ultraviolet lamp, react for 18 hours, and the obtained reaction mixture is subjected to 31P nuclear magnetic resonance spectrum (CDCCl 3 ) characterization analysis, the data show that the content of sodium di-n-propylphosphinate reaches 92% (molar percentage), the content of sodium diisopropylphosphinate reaches 6.2%, and the content of sodium mono-n-propylphosphinate is 1.6%. Sodium isopropylphosphinate is 0.2%, no sodium hypophosphite;

[0026] 2) Dilute the above mixed solution with water to a concentration of 0.25mol / L containing sodium dipropylphosphinate (in...

Embodiment 3

[0031] A preparation method for aluminum dipropylphosphinate, comprising the steps of:

[0032] 1) Dissolve 212g of sodium hypophosphite monohydrate in 1200ml of acetic acid and stir thoroughly to obtain an acetic acid solution of sodium hypophosphite, then move it to a 2L photoreactor and add 2.0g of nano-ZrO 2 and vigorously stirred, propylene was introduced at 60°C, and reached saturation, and then the ultraviolet lamp was turned on, and the reaction was carried out for 20 hours, and the obtained reaction mixture was carried out 31 P NMR spectrum (CDCCl 3 ) characterization analysis, the data show that the content of sodium di-n-propylphosphinate reaches 94.5% (molar percentage), the content of sodium diisopropylphosphinate reaches 3.8%, and the content of sodium mono-n-propylphosphinate is 1.2%. Sodium isopropylphosphinate is 0.5%, no sodium hypophosphite;

[0033] 2) Dilute the above mixed solution with water to a concentration of 0.3mol / L containing sodium dipropylphos...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Initial decomposition temperatureaaaaaaaaaa
Initial decomposition temperatureaaaaaaaaaa
Login to View More

Abstract

The invention relates to a preparation method of aluminum diethylphosphinate. Sodium hypophosphite and propylene are adopted as reaction raw materials, acetic acid is adopted as solvent, nano metal oxide is adopted as a catalyst to catalyze the addition reaction of the sodium hypophosphite and propylene so as to synthesize high-purity sodium diethylphosphinate, and then the high-purity sodium aluminum diethylphosphinate has the replacement reaction with aluminum salt to generate the aluminum diethyphosphinate. The preparation method has the advantages that due to the concerted catalysis effect of the nano metal oxide, the photoreaction is carried out under the condition of low temperature and normal pressure, so that the safety is high, the energy consumption is low, the conversion rate of the sodium diethylphosphinate is high, and fewer byproducts are produced; less catalyst is consumed, the catalyst can be repeatedly utilized, and the cost is low; the conversion rate of the sodium diethylphosphinate in the photoreaction is high, so that fewer byproducts are produced, the temperature for the replacement reaction and washing is greatly lowered, and the white solid product with high purity and good thermal stability can be obtained.

Description

technical field [0001] The invention relates to the preparation of a green and environment-friendly dipropylphosphinate flame retardant, in particular to a preparation method of aluminum dipropylphosphinate. Background technique [0002] With the rapid development of the polymer material industry and the continuous improvement and improvement of flame retardant regulations, the demand for non-toxic, smoke-suppressing, environmentally friendly, halogen-free flame retardants is becoming more and more urgent at home and abroad. Alkyl phosphinate is a new generation of green and environmentally friendly phosphorus-based flame retardants developed in recent years. It has good compatibility with high-molecular polymer materials. This type of flame-retardant products has a low density and requires less flame retardants. , better mechanical properties, better color, lower smoke density, higher relative tracking index. In particular, aluminum dipropylphosphinate is a flame retardant...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07F9/30
Inventor 张宝贵唐雪娇杨喜生赵震郭建树
Owner 山东兄弟科技股份有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com