Phosphor-contained fire-retardant with two spirane structure and preparation method
A technology of flame retardants and double spiro rings, which is applied in the field of phosphorus-containing flame retardants with a double-spiro ring structure and its preparation. Simple method, easy to use effect
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Embodiment 1
[0032] The reaction equation of the present embodiment is as follows:
[0033]
[0034] Among them, the monomer 3,9-dichloro 2,4,8,10-tetrachloro-3,9-diphosphorous spiro-3,9 dioxo[5.5]-undecane (referred to as double spiro, SPDPC) The synthesis of is prepared by referring to the method disclosed in US Pat. No. 3,169,863.
[0035] In the 50ml polymerization bottle that nitrogen inlet and outlet and mechanical stirrer are housed, add 12.5g bisphenol S (SDP) and 9.95g double spiro ring and 0.05g zinc chloride as catalyst; Under nitrogen flow protection, slowly heat up to 170°C, at this time, hydrogen chloride gas is generated, and the system is in a solid phase reaction; when kept at 170°C for 2 hours, the system gradually softens, and the system becomes liquid after about 20 minutes, continue to maintain the temperature until the rod climbing phenomenon occurs, and then Then raise the temperature to 220° C. and continue the reaction for 3 hours to obtain 18.5 g of light yell...
Embodiment 2
[0037] The reaction equation of the present embodiment is as follows:
[0038]
[0039] Among them, the monomer 3,9-dichloro 2,4,8,10-tetrachloro-3,9-diphosphorous spiro-3,9 dioxo[5.5]-undecane (referred to as double spiro, SPDPC) The synthetic method is with embodiment 1.
[0040] In a 50ml polymerization bottle equipped with a nitrogen inlet and outlet and a mechanical stirrer, add 28.5g of bisphenol A and 29.6g of double spiro rings; under the protection of nitrogen flow, slowly heat up to 180°C, at which point hydrogen chloride gas begins to be produced, And the system is in a solid phase reaction; when kept at 180°C for 2 hours, the system softens slowly, and after about 20 minutes the system becomes liquid, continue to maintain the temperature until the rod climbing phenomenon occurs, and then raise the temperature to 210°C and continue the reaction for 5 hours 46 g of light yellow solid product was obtained. The hydrogen chloride gas discharged from the system can ...
Embodiment 3
[0042] The reaction equation of the present embodiment is as follows:
[0043]
[0044] Among them, the monomer 3,9-dichloro 2,4,8,10-tetrachloro-3,9-diphosphorous spiro-3,9 dioxo[5.5]-undecane (referred to as double spiro, SPDPC) The synthetic method is with embodiment 1.
[0045] In the 50ml polymerization bottle equipped with nitrogen inlet and outlet and mechanical stirrer, add 14.2g bisphenol S (SDP), 14.8g double spiro ring and 25ml acetonitrile; Hydrogen chloride gas began to be generated; when the temperature was continued to rise to 76°C for 2 hours, the system gradually softened, and then the temperature was maintained for 4 hours, and the solvent was removed to obtain 22.5 g of a light yellow solid product. The hydrogen chloride gas discharged from the system can be absorbed by sodium hydroxide solution. The solid product was dissolved in 50ml of chloroform, then added with 300ml of methanol and stirred to precipitate a pure white precipitate, then filtered, an...
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Abstract
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