Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Phosphor-containing nitrogen-containing structural type flame retardant polyhydric alcohol as well as preparation method and application thereof

A flame-retardant polyol and structural technology, which is applied in the field of phosphorus-containing nitrogen-containing structural flame-retardant polyol and its preparation, can solve the problem that the flame retardant performance of polyurethane rigid foam is not obvious, there is strong irritating hydrogen halide gas, and it is difficult to Meet environmental protection requirements and other issues, and achieve the effects of easy industrial production, easy operation, and strong practicability

Inactive Publication Date: 2014-08-06
XIAMEN UNIV +1
View PDF4 Cites 23 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The Chinese patent with the application number 201210103713.1 introduces a preparation method of phosphorus-halogen synergistic flame-retardant polyether polyol, and applies it to the preparation of flame-retardant polyurethane rigid foam. The result significantly improves the flame retardancy of polyurethane rigid foam (LOI is 30.8), but because the flame-retardant polyether polyol contains halogen, it will produce toxic, harmful and strongly irritating hydrogen halide gas during combustion, so it is difficult to meet environmental protection requirements
[0005] The Chinese patent with the application number 201310414097.6 introduces a preparation method of a reactive Mannich polyether polyol with permanent flame retardant effect. By using the polyether polyol, the benzene ring structure with good thermal stability and flame retardant Elements are introduced into the polyurethane structure, but because the polyether polyol contains a relatively single flame retardant element (only nitrogen elements), the flame retardant performance of the polyurethane rigid foam used for the preparation is not significantly improved (the highest LOI is 26.2) , low flame retardant efficiency

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Phosphor-containing nitrogen-containing structural type flame retardant polyhydric alcohol as well as preparation method and application thereof
  • Phosphor-containing nitrogen-containing structural type flame retardant polyhydric alcohol as well as preparation method and application thereof
  • Phosphor-containing nitrogen-containing structural type flame retardant polyhydric alcohol as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] On a 1000mL three-neck flask, install a constant pressure dropping funnel and a reflux condenser, add 45.00g (1.50mol) of paraformaldehyde and 91.68g (1.50mol) of ethanolamine, stir and react at 20°C for 0.5h, then heat up under nitrogen protection After reacting at 60° C. for 2 hours, 94.11 g (0.50 mol) of phenol-ethanol solution with a mass fraction of 50% was slowly added dropwise, and refluxed for 4 hours to obtain a phenol-based Mannich-based polyol intermediate.

[0038] After the temperature of the system was lowered to 50°C, 207.00g (1.50mol) of diethyl phosphite and 45.00g (1.50mol) of paraformaldehyde were successively added to continue the reaction for 4h. Finally, the ethanol and the water produced by the reaction are removed by vacuum distillation to obtain a light yellow viscous liquid, which is a phosphorus-containing and nitrogen-containing structural flame-retardant polyol.

[0039] The infrared spectrogram of the phosphorus-containing and nitrogen-cont...

Embodiment 2

[0041] On a 1000mL three-neck flask, install a constant pressure dropping funnel and a reflux condenser, 45.00g (1.50mol) of paraformaldehyde and 91.68g (1.50mol) of ethanolamine, stir and react at 20°C for 1.0h, then heat up under nitrogen protection React at 80° C. for 2 hours, slowly drop 165.15 g (0.75 mol) of resorcinol ethanol solution with a mass fraction of 50%, and reflux for 2 hours to obtain a Mannich polyol intermediate.

[0042] After the temperature of the system was lowered to 55°C, 207.00g (1.50mol) of diethyl phosphite and 45.00g (1.50mol) of paraformaldehyde were successively added to continue the reaction for 4h. Finally, the ethanol and the water generated by the reaction are removed by vacuum distillation to obtain a light yellow viscous liquid, which is a phosphorus-containing and nitrogen-containing structure-type flame-retardant polyol.

Embodiment 3

[0044] On a 1000mL three-neck flask, install a constant pressure dropping funnel and a reflux condenser, 45.00g (1.50mol) of paraformaldehyde and 91.68g (1.50mol) of ethanolamine, stir and react at 20°C for 1.0h, then heat up under nitrogen protection After reacting at 70° C. for 2 hours, 297.33 g (1.50 mol) of phenol ethanol solution with a mass fraction of 50% was slowly added dropwise, and refluxed for 3 hours to obtain a Mannich polyol intermediate.

[0045] After the temperature of the system was lowered to 55°C, 207.00g (1.50mol) of diethyl phosphite and 45.00g (1.50mol) of paraformaldehyde were successively added to continue the reaction for 4h. Finally, the ethanol and the water generated by the reaction are removed by vacuum distillation to obtain a light yellow viscous liquid, which is a structural phosphorus-containing nitrogen-containing flame-retardant polyol.

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

No PUM Login to View More

Abstract

The invention discloses a phosphor-containing nitrogen-containing structural type flame retardant polyhydric alcohol as well as a preparation method and application thereof, and relates to a flame retardant polymer. The preparation method comprises the following steps of carrying out heat-up reaction on paraformaldehyde and ethanol amine under protection of a nitrogen gas after mixing and reacting, then, adding alcohol liquor of aromatic phenol compounds, and refluxing and reacting to obtain an Mannich polyhydric alcohol intermediate; adding phosphite ester compounds to continuously react with paraformaldehyde after cooling the temperature of the system to 50 DEG C-55 DEG C, removing alcohol and moisture produced by reaction by distilling under reduced pressure to obtain a product. The phosphor-containing nitrogen-containing structural type flame retardant polyhydric alcohol can be applied to manufacturing hard polyurethane foam plastic. A benzene ring structure with good thermal stability and P, N flame-retardant elements are introduced into a PU (poly urethane) structure by virtue of a chemical bond mode by using the polyhydric alcohol without a mobility problem, so that lasting flame resistance is realized on the condition of ensuring material processing performances. A catalyst is not used for synthesizing the flame retardant polyhydric alcohol, materials are cheap and easily available, process is simple; and the retardant polyhydric alcohol is easy for industrial production without producing pollutants, and satisfies environment-friendly requirements.

Description

technical field [0001] The invention relates to a flame-retardant polymer, in particular to a phosphorus-containing and nitrogen-containing structural flame-retardant polyol and a preparation method and application thereof. Background technique [0002] Rigid polyurethane foam (RPUF), also known as rigid polyurethane foam, has the advantages of light weight, good heat insulation, sound absorption, cushioning and shock resistance, and has excellent mechanical properties and chemical corrosion resistance. The material has strong cohesive force, so it is widely used as thermal insulation material for petrochemical pipelines, refrigeration equipment, transportation equipment and buildings. However, due to the large specific surface area of ​​PU foam plastics, good gas permeability, and high proportion of molecular chain hydrocarbons, the burning speed and quality loss will be accelerated during combustion, so the limiting oxygen index of rigid polyurethane foam plastics without ...

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): C07F9/6574C07F9/40C08G18/32C08G18/66C08G101/00
Inventor 戴李宗陈国荣陈昌禧刘诚陈华泽姜文峰许一婷吴耕何凯斌毛杰
Owner XIAMEN UNIV
Features
  • Generate Ideas
  • 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