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Efficient phosphorus-nitrogen type fire retardant and preparation method thereof

A high-efficiency phosphorus-nitrogen system and flame retardant technology, applied in the field of flame retardant materials, can solve the problems of low flame retardant efficiency of halogen-free flame retardants, achieve high char formation rate, improve flame retardant performance, and simple synthesis process

Active Publication Date: 2014-06-18
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the flammability of existing polymer materials and consider the defects of low flame retardant efficiency of existing halogen-free flame retardants, the present invention provides a high-efficiency phosphorus Nitrogen-based flame retardant, preparation method and application, when added in a low amount (phosphorus content 0.75 wt.%), it can reach UL-94 V-0 level

Method used

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  • Efficient phosphorus-nitrogen type fire retardant and preparation method thereof
  • Efficient phosphorus-nitrogen type fire retardant and preparation method thereof
  • Efficient phosphorus-nitrogen type fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The synthesis steps of flame retardant DP-DDM are as follows:

[0034] Add 9.91 g of DDM, 15.22 g of 4-hydroxy-3-methoxybenzaldehyde and 200 mL of absolute ethanol into a three-necked flask with a stirring device. Under stirring, the reaction temperature is 40 ° C for 2 h; the reaction After the end, add 21.62 g DOPO into the three-necked flask (there is a dispersion system containing intermediate products in the three-necked flask), under the action of stirring, the reaction temperature is 60 ° C for 10 h, after the reaction, the reaction mixture is suction filtered , washing, and drying in a vacuum oven at 60°C for 8 h to obtain the required flame retardant DP-DDM with a yield of 89.2%.

[0035] After infrared spectroscopy, NMR, and mass spectrometry tests, the test and analysis results are as follows:

[0036] 1 H NMR (400 MHz, DMSO-d6) δ 8.90 (d, J = 11.4 Hz, 2H), 8.16 (dd, J = 16.3, 9.5 Hz, 4H), 8.01 – 7.94 (m, 1H), 7.79 – 7.63 (m, 3H), 7.52 (t, J = 6.7 Hz,...

Embodiment 2

[0041] The synthetic steps of flame retardant DP-DDE are as follows:

[0042] Add 10.01g DDE, 15.22g 4-hydroxyl-3-methoxybenzaldehyde, 300 mL of dehydrated alcohol and ethyl acetate mixed solvent into a three-necked flask with a stirring device, and under stirring, the reaction temperature is React at 30°C for 4 h; after the reaction, add 21.62 g DOPO into the three-necked flask, under stirring, the reaction temperature is 30°C and react for 15 h. After the reaction, the reaction mixture is suction filtered, washed, and dried in a vacuum oven Dry at 60°C for 8 h to obtain the desired flame retardant DP-DDE with a yield of 90.8%.

[0043] The test analysis results are as follows:

[0044] 1 H NMR (400 MHz, DMSO-d6) δ 9.02 – 8.92 (m, 2H), 8.12 (t, J = 7.3 Hz, 4H), 7.87 (dd, J = 9.8, 6.0 Hz, 1H), 7.66 (dd, J = 14.4, 4.6 Hz, 3H), 7.48 – 7.18 (m, 12H), 7.11 (d, J = 8.1 Hz, 1H), 6.99 (dd, J = 7.8, 3.1 Hz, 1H), 6.91 (d, J = 18.2 Hz, 2H), 6.76 (dt, J = 13.7, 7.8 Hz, 6H...

Embodiment 3

[0049] The synthesis steps of flame retardant DP-DDS are as follows:

[0050] Add 12.42g of DDS, 15.22g of 4-hydroxy-3-methoxybenzaldehyde and 400 mL of ethyl acetate into a three-necked flask with a stirring device. Under stirring, the reaction temperature is 60°C for 3 h, and the reaction After the end, 21.62 g of DOPO was added into the three-necked flask, and under stirring, the reaction temperature was 60°C for 18 h. After the reaction, the reaction mixture was suction filtered, washed, and dried in a vacuum oven at 60°C for 8 h. The desired flame retardant DP-DDS was obtained with a yield of 90.7%.

[0051] The test analysis results are as follows:

[0052] 1 H NMR (400 MHz, DMSO-d6) δ 9.02 – 8.92 (m, 2H), 8.11 (dd, J = 11.5, 4.7 Hz, 4H), 7.85 (d, J = 8.4 Hz, 1H), 7.75 – 7.59 (m, 3H), 7.47 – 7.18 (m, 12H), 7.11 (d, J = 8.1 Hz, 1H), 7.01 – 6.96 (m, 1H), 6.91 (d, J = 17.9 Hz, 2H), 6.74 (dd, J = 15.1, 10.4 Hz, 6H), 6.62 (dd, J = 8.0, 2.2 Hz, 2H), 5.43 (dd, J ...

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Abstract

The invention discloses an efficient phosphorus-nitrogen type fire retardant and preparation method thereof. The method comprises the following steps: firstly performing condensation reaction on aromatic amine and aromatic aldehyde in a solvent, then performing addition reaction together with DOPO, cooling, performing suction filtering and washing, and performing vacuum drying to obtain the phosphorus-nitrogen type fire retardant powder, wherein the fire retardant molecule has high activity and is capable of promoting the solidification of the epoxy resin, the fire retardant powder is added in the epoxy resin, the solidified epoxy condensate has high inflaming retarding, when the phosphorus content of the epoxy solidification system is 0.75wt%, the level can achieve UL-84V-0 in vertical burning.

Description

technical field [0001] The invention belongs to the field of flame-retardant materials, and in particular relates to a high-efficiency phosphorus-nitrogen flame retardant, a preparation method and an application. Background technique [0002] Compounds containing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) group as flame retardant materials have broad application prospects in the halogen-free flame retardant modification of epoxy resins , is a research hotspot in the field of halogen-free flame retardant in recent years. It has been confirmed that some DOPO derivatives play an important role in optimizing the flame retardant efficiency and comprehensive mechanical properties of epoxy resins. However, the research on these phosphorus-containing flame retardants faces two problems: 1. Improve the flame retardant performance of the epoxy curing system to reach the UL-94 V-0 level; 2. Reduce the amount of phosphorus in the system and reduce the possible phosphorus...

Claims

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Application Information

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IPC IPC(8): C08K5/5313C07F9/6574C08L63/00
Inventor 姚有为顾立强
Owner SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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