Reactive flame retardant applied to polyurethane materials and preparation method of reactive flame retardant

A technology of reactive flame retardants and polyurethane materials, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve limited flame retardant effects, single flame retardant elements, and synergistic effects No way to play and other problems, to achieve a good flame retardant effect, the effect of a simple synthesis process

Active Publication Date: 2016-06-08
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
View PDF10 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The flame retardant element is single, and the flame retardant effect on polyurethane foam is limited. The synergistic effect of multiple flame retardant elements in composite flame retardants cannot be exerted, and the reactive flame retardants containing multiple flame retardant elements are rarely reported.

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
  • Reactive flame retardant applied to polyurethane materials and preparation method of reactive flame retardant
  • Reactive flame retardant applied to polyurethane materials and preparation method of reactive flame retardant
  • Reactive flame retardant applied to polyurethane materials and preparation method of reactive flame retardant

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0020] A preparation method of a reactive flame retardant applied to polyurethane materials, the specific steps are as follows:

[0021] (1) Add reactant tetrabromophthalic anhydride, N,N-di(2-hydroxyethyl)aminomethylenephosphonic acid diethyl ester (FRC-6) and solvent into the reaction vessel; stir until tetrabromophthalic anhydride is completely dissolved , heated to 60-120°C under stirring conditions, and reacted for 2-12 hours to synthesize tetrabromophthalic acid (2-hydroxyethylphosphonic acid diethyl methylene) aminomono-2-ethyl ester;

[0022] (2) After the reaction, cool down to below 50°C, filter, and distill to recover the solvent to obtain viscous tetrabromophthalic acid (2-hydroxyethylphosphonic acid diethyl methylene) aminomono-2 - Ethyl ester products.

[0023] The reactant tetrabromophthalic anhydride:diethyl N,N-bis(2-hydroxyethyl)aminomethylenephosphonate (FRC-6) has a mass ratio of 3.6:1-0.9:1.

[0024] The solvent is one of benzene, toluene, xylene, cycloh...

Embodiment 1

[0027] Add 100g of tetrabromophthalic anhydride, 50g of FRC-6 and 50mL of benzene in sequence to a 500mL four-neck flask equipped with a stirrer, condenser and thermometer, start stirring until the tetrabromophthalic anhydride is completely dissolved, raise the temperature to 80°C, and react for 10 hours at a constant temperature . Cool down to 20°C, filter, and recover benzene by distillation to obtain a viscous TBPAHM product, which is detected by a NICOLETIS10 Fourier transform infrared spectrometer from Thermo Fisher. The FTIR of this product is as follows: figure 1 shown. The functional group vibrations corresponding to the main absorption peaks in the infrared spectrum are: 3364cm -1 (v-OH), 2981cm -1 (VS-CH3), 2906cm -1 (V-P-CH2), 1736(V-C=O)cm -1 , 1620cm -1 、1532cm -1 、1508cm -1 (Phenyl ring hexasubstituted), 1316cm -1 (V-CH3), 1370cm -1 (V-P=O), 1235cm -1 (V-C-O), 1162cm -1 (V-C-N), 1017cm -1 (V-P-O), 627cm -1 (V-C-Br). Adopt the Agilent400MR nuclear ma...

Embodiment 2

[0029] Add 90g of tetrabromophthalic anhydride, 60g of FRC-6 and 100mL of toluene in sequence to a 500mL four-necked flask equipped with a stirrer, condenser and thermometer, start stirring until the tetrabromophthalic anhydride is completely dissolved, raise the temperature to 95°C, and react for 8 hours at a constant temperature . Cool down to 25°C, filter, and recover toluene by distillation to obtain a viscous TBPAHM product. The content of TBPAHM is 88.3%. It is detected by the LC-1525 high-performance liquid chromatograph of Waters Corporation in the United States. The high-performance liquid chromatogram of the product is Such as image 3 shown.

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 belongs to the field of flame-retardant high molecular materials and relates to a reactive flame retardant applied to polyurethane materials and a preparation method of the reactive flame retardant. The reactive flame retardant is tetrabromophthalate(2-hydroxyethyl phosphate diethyl methylene)amidomono-2-ethyl ester containing bromine, phosphorous and nitrogen. The preparation method particularly includes: adding reactants tetrabromophthalic anhydride, N, N-di(2-ethoxy)amino methylene diethyl phosphite and solvent into a reactor; stirring until tetrabromophthalic anhydride is completely dissolved, heating while stirring to 60-120 DEG C, and allowing reaction for 2-12 h to synthesize TBPAHM; after reaction is finished, cooling to below 50 DEG C, filtering, distilling and recovering the solvent to obtain pasty TBPAHM. The reaction flame retardant is simple in synthesis process, can be directly used only after being filtered and distilling and recovering the solvent, is suitable for industrialized production and has good flame-retardant effect when being applied in polyurethane foamed materials.

Description

technical field [0001] The invention belongs to the field of flame-retardant polymer materials, and relates to a reactive flame retardant applied to polyurethane materials and a preparation method thereof. Background technique [0002] Polyurethane (PU) materials include rigid foam materials, soft foam materials, artificial leather, elastomers and coatings, and are widely used in the fields of building materials, external wall insulation, home appliances, furniture and vehicle decoration. PU materials, especially PU foamed plastics, have a high proportion of hydrocarbons in molecular chains, large specific surface area, and good gas permeability. When burning, they will accelerate the burning speed and loss of quality. The limiting oxygen index (LOI) is between 16% and 18%. It is a flammable material and emits toxic gases such as HCN and CO during combustion. Therefore, it is of great practical significance to carry out research on flame retardant technology of polyurethane...

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): C08G18/38C07F9/40C08G101/00
CPCC07F9/4009C08G18/3889C08G2101/00
Inventor 张忠厚方少明韩琳田俊峰王银涛
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap