A novel bio-based phosphazene epoxy resin monomer and its prepared bio-based phosphorus nitrogen flame retardant epoxy resin
A technology of nitrile epoxy resin and epoxy resin is applied in the field of bio-based phosphorus nitrogen flame retardant epoxy resin to achieve the effects of abundant raw materials, low price and improved mechanical properties
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0039]Take 7.44g of sodium hydride, 45.55g of eugenol, and 18.87g of hexachlorocyclotriphosphazene into 140mL of tetrahydrofuran, blow nitrogen at 50°C, and react for 36 hours to obtain a flame-retardant intermediate. Add 200mL ethanol to the system to complete the reaction of sodium hydride. The crude product was transferred to a single-necked flask, and excess tetrahydrofuran and ethanol were spin-dried with a rotary evaporator to obtain a brown-yellow viscous oily liquid. Then add chloroform to the system to dissolve evenly. After that, deionized water was used to extract three times, and the organic layer was spin-dried again. The viscous liquid obtained after spin-drying was added to the ethanol solution while stirring at 60°C, and a small amount of water was added (ethanol:water ≈10:1). After cooling to room temperature, put it in the refrigerator to cool, and you can get light yellow crystals. Filter under reduced pressure to collect the upper solid. The crystals we...
Embodiment 2
[0042] 10 g of HEP prepared in Example 1 and 8 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) were dissolved in tetrahydrofuran, stirred evenly and heated to 60°C. Add 0.1 g of azobisisobutyronitrile and react for 2 days. After the crude product was spin-dried, ethanol was added, and the precipitate was filtered off. Then spin dry ethanol to obtain the intermediate of novel bio-based phosphazene epoxy resin monomer, abbreviated as QDEP.
[0043] For the above obtained QDEP 1 The characterization result of H-NMR is: the absorption peak is δ=7.2ppm-8.2ppm (five kinds of hydrogen atoms on the phosphaphenanthrene ring). δ = 7.0 ppm, δ = 6.7 ppm, δ = 6.6 ppm (hydrogen on the benzene ring). δ = 2.5 ppm, δ = 2.8 ppm, δ = 3.1 ppm (3 hydrogens on glycidyl). δ = 4.0 ppm (hydrogen of methoxy). δ = 3.9 ppm, δ = 2.7 ppm, δ = 2.0 ppm (methylene groups on aliphatic chains). δ = 5.9 ppm, δ = 5.0 ppm, δ = 3.3 ppm (three different hydrogens on the allyl groups).
Embodiment 3
[0045] Get 10g of QDEP prepared in Example 2, dissolve in 100ml of dichloromethane, and stir evenly. Add 20 g of peracetic acid dropwise, keep the temperature below 5° C., pass nitrogen gas, and react for 4 days to obtain the crude product of novel bio-based phosphazene epoxy resin monomer (abbreviated as EQDEP). Wash once with aqueous sodium thiosulfate and three times with aqueous sodium bicarbonate. After drying with anhydrous sulfuric acid for 8 hours, it was spin-dried to synthesize the epoxide (EQDEP) of the tetraphosphaphenanthrene adduct of six [(4-allyl-2-methoxy) phenoxy] cyclotriphosphazene, Its molecular structure is as Figure 4 shown.
[0046] of the above derived EQDEP 1 The characterization result of H-NMR is: the absorption peak is δ=7.2ppm-8.2ppm (five kinds of hydrogen atoms on the phosphaphenanthrene ring). δ = 7.0 ppm, δ = 6.7 ppm, δ = 6.6 ppm (hydrogen on the benzene ring). δ = 2.5 ppm, δ = 2.8 ppm, δ = 3.1 ppm (3 hydrogens on glycidyl). δ = 4.0 ppm...
PUM
| Property | Measurement | Unit |
|---|---|---|
| limiting oxygen index | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More