Unlock instant, AI-driven research and patent intelligence for your innovation.

Macromolecular flame retardant containing three elements of phosphorus, nitrogen and silicon and synthesis method and application of macromolecular flame retardant

A technology of macromolecules and flame retardants, applied in the field of flame retardants and their preparation, can solve the problems of complex structure and preparation process, poor resin compatibility, no macromolecular flame retardants, etc. Large-scale production, beneficial to environmental protection, and the effect of improving flame retardancy

Active Publication Date: 2015-01-14
BEIJING UNIV OF CHEM TECH
View PDF8 Cites 28 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reports on synergistic flame retardants in the literature mostly focus on phosphorus-nitrogen and phosphorus-silicon flame retardants, and the structure and preparation process are complex, and there are problems such as poor compatibility with resins.
At present, there are no reports on macromolecular flame retardants containing three elements: phosphorus, nitrogen, and silicon.

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
  • Macromolecular flame retardant containing three elements of phosphorus, nitrogen and silicon and synthesis method and application of macromolecular flame retardant
  • Macromolecular flame retardant containing three elements of phosphorus, nitrogen and silicon and synthesis method and application of macromolecular flame retardant
  • Macromolecular flame retardant containing three elements of phosphorus, nitrogen and silicon and synthesis method and application of macromolecular flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 Synthesis of Flame Retardant DPP-Si-1

[0035]

[0036] (Ⅳ)

[0037] The synthesis process of the flame retardant DPP-Si-1 is shown in the above formula (Ⅳ).

[0038] Amino silicone oil (SiONH 2 , 20.0 g, 0.023 mol), p-hydroxybenzaldehyde (5.1 g, 0.041 mol) and 30 mL of dichloromethane, reacted at room temperature under nitrogen protection for 3 hours, added DOPO (8.9 g, 0.041 mol) in batches, continued The reaction was carried out by spotting the plate (developing agent: chloroform / methanol = 4:1) to detect the reaction. After about 6 hours of reaction, DOPO reacted completely. / methanol=10:1), after removing the solvent, 24.8 g of yellow blocky solid DPP-Si-1 was obtained (yield: 79.5 %). IR(KBr) ν max (cm ?1 ) : 3305 (-OH); 2954~2846 (CH3 and CH 2 ); 1606, 1523, 1452 (Ar ring); 1187 (P=O); 1267 (Si-CH 3 ); 1040~1092 (Si-O-Si); 921 (P-O-C). 1 H-NMR (CDCl 3 , 400MHz) δ ppm : -0.14~0.21(-Si-CH 3 ), 0.25~0.35(m, Si-CH 2 ), 1.25~1.39(m, Si...

Embodiment 2

[0039] Example 2 Synthesis of Flame Retardant DPP-Si-2

[0040]

[0041] (V)

[0042] The synthesis process of the flame retardant DPP-Si-2 is shown in the above formula (Ⅴ).

[0043] Amino silicone oil (SiONH 2 ) (20.0g, 0.023mol), benzaldehyde (4.3g, 0.041mol) and 30mL of dichloromethane were added to a 100mL three-necked flask equipped with a condenser, a thermometer and magnetic stirring, and reacted at room temperature for 3 hours under nitrogen protection. Add DOPO (8.9g, 0.041mol), and detect the progress of the reaction by dot plate (developing agent: chloroform / methanol=5:1). After about 8 hours, the reaction of DOPO is complete, and the solvent is removed by rotary evaporation, and purified by column chromatography through a silica gel column. (Eluent: chloroform / methanol=12:1), after removing the solvent, 23.8 g of light yellow viscous DPP-Si-2 was obtained (yield: 77.9 %). IR(KBr) ν max (cm ?1 ) : 3071(Ar-H); 2964~2894 (CH 3 and CH 2 ); 1599,1460 (Ar...

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
thermal decomposition temperatureaaaaaaaaaa
thermal decomposition temperatureaaaaaaaaaa
Login to View More

Abstract

The invention discloses a macromolecular flame retardant containing three elements of phosphorus, nitrogen and silicon and a synthesis method of the macromolecular flame retardant. The synthesis method is characterized in that an organic silicon polymer containing an amino group firstly reacts with an aldehyde type substance and then reacts with 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to prepare novel flame retardant molecules which simultaneously contain three flame retardant elements of phosphorus, nitrogen and silicon in the molecules. The flame retardant disclosed by the invention is simple in a preparation process and has good solubility with resin, and the three flame retardant elements of phosphorus, nitrogen and silicon are synergistic for realizing flame retardance, so that the flame retardant effect of resin added with the flame retardant is significantly improved, and the flame retardant can be used as the additive flame retardant for halogen-free flame retardance of epoxy resin, polyurethane, ABS (acrylonitrile butadiene styrene), nylon and other engineering plastics.

Description

technical field [0001] The invention relates to a class of halogen-free flame retardant and a preparation method thereof, belonging to the technical field of fine organic synthesis. Background technique [0002] With the advancement of industrial technology, more and more organic synthetic polymer materials have entered our daily life. These materials have excellent properties, such as good hardness, high tensile strength, water resistance, corrosion resistance, etc., and have a wide range of applications. . However, since most polymer materials such as epoxy resins, polyesters, and engineering plastics are flammable or combustible substances, and emit a large amount of toxic and corrosive gases when burned, the hazards caused by fires caused by them are also more serious. . Therefore, preventing the fire caused by the burning of polymer materials has become an urgent problem to be solved. [0003] At present, halogenated flame retardants are mostly used in polymer mater...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/30C08L83/08C08L63/00
Inventor 王涛李永杰
Owner BEIJING UNIV OF CHEM TECH