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Additive phosphorus-containing polysiloxane compound for thermosetting resins, flame retardant composition comprising same, and articles made therefrom
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A kind of flame retardant composition, polysiloxane technology, applied in the field of flame retardants
Inactive Publication Date: 2020-09-11
爱思乐艾博美国有限公司
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[0008] Although Chernyy, Sergey described in Journal of Applied Polymer Science, 132(19), 41955 / 1-41955 / 9; 2015 by 10-(2-trimethoxysilyl-ethyl)-9-hydrogen-9 - Copolymer of oxa-10-phosphaphenanthrene-10-oxide (DOPO) and tetraethyl orthosilicate, but it is only described as a flame retardant for cotton fibers
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Embodiment 1
[0097] Example 1 : Synthesis of DOPO-siloxane
[0098] 10-(2-Trimethoxysilyl-ethyl)-9-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO-H) (432.4g, 2.0mol) and ethylene Vyltriethoxysilane (VTES) (399.7 g, 2.1 mol) was mixed together. The suspension was heated to 120°C and a heterogeneous solution formed (molten DOPO-H layer at the bottom). tert-Butyl peroxide (4 mL) was added dropwise to the reaction mixture over 30 minutes, producing fine bubbles as the peroxide reached solution and a homogeneous solution formed within a short time. The mixture was stirred at 120°C for another 2 hours. At the end of the reaction, 31 P NMR showed less than 1 mol% DOPO-H remaining. The product DOPO-triethoxysilane (DOPO-TES) was a clear liquid. 31 P NMR (121MHz, CDCl 3 , ppm) δ40. 1 H NMR (300MHz, CDCl 3 , ppm) δ7.0-8.0 (m, 8H), 3.3-3.5 (m, 9H), 1.8-2.3 (m, 2H), 0.6-1.1 (m, 2H).
[0099] 3.3 g of methanol, 0.6 g of water, and 2.0 g of acetic acid were mixed together and added drop...
Embodiment 2
[0100] Example 2 : Synthesis of DOPO-siloxane
[0101] The DOPO-siloxane was prepared using the procedure in Example 1. The product was then heated at 165°C for 2 hours to completely react any remaining Si-OH groups. After heating, TGA 95wt% at 359°C.
Embodiment 3
[0102] Example 3 : Synthesis of DOPO-vinyl-siloxane
[0103] DOPO-TES was prepared using the procedure in Example 1. 3.3 g of methanol, 0.6 g of water and 2 g of acetic acid were mixed together and added dropwise to a mixture of 10 g of DOPO-TES and 1.3 g of VTES at 0° C. within 15 minutes. The reaction mixture was stirred at 100°C for 4 hours. The solvent was removed and the product was a white foam. 31 P NMR (121MHz, CDCl 3 , ppm) δ37-42 (product). 1 HNMR (300MHz, CDCl 3 , ppm) δ7.0-8.0 (m, 8H), 5.3-6.0 (m, 1.8), 1.8-2.3 (m, 2H), 0.6-1.1 (m, 2H). Proton-based ( 1 H) The ratio between DOPO- and vinyl-groups determined by NMR is 5:3. The product was then heated at 150 °C for 2 hours to completely react any remaining Si-OH groups. After heating, TGA 95wt% at 318°C.
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Abstract
There is provided herein a flame retardant composition containing a thermosetting resin and a phosphorus-containing polysiloxane flame retardant, which flame retardant composition can be used in prepregs, laminate, bonding sheets and printed wiring boards.
Description
[0001] This application claims priority to U.S. Provisional Application No. 62 / 595,334, filed December 6, 2017, the entire contents of which are incorporated herein by reference. technical field [0002] The present invention relates to the field of flame retardants, especially phosphorus-containing flame retardants for electronic applications such as printed circuit boards. Background technique [0003] The fast-growing electronics industry, especially consumer electronics, requires products with light weight, high density, high reliability, high functionality and low power consumption. This requires electronic components with higher signal transmission speed and transmission efficiency, as well as high signal integrity and very low power loss. This requires significant improvements in the performance of printed circuit board carriers. In addition, high speed and multifunctionalization of electronic products require improvements in dimensional stability and thermal stabili...
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