Preparation of high-performance reactive polyurethane flame retardant compounded by triphosphonic acid containing melamine ring and derivatives of triphosphonic acid
A technology of polyurethane flame retardant and triphosphonate, which is applied in the fields of periodic table group 5/15 element compounds, chemical instruments and methods, organic chemistry, etc. Complex synthesis process and other issues
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Embodiment 1
[0045] [Example 1]: Preparation of 1,3,5-triazine-2,4,6-triphosphate (TPE)
[0046] Take 60mL of triethyl phosphite (TEP, 0.34mol) into a 200mL three-neck round bottom flask. Under magnetic stirring, divide 11.1g of cyanuric chloride (TCT, 0.06mol) into three batches, and slowly add it to triethyl phosphite within 1 hour at room temperature, TCT will gradually dissolve, the reaction will exotherm, and ethyl chloride will be released gas, a yellow transparent solution was obtained. After adding TCT, raise the temperature to 100-105°C for 8 hours, cool to 50°C, slowly add 35 mL of petroleum ether (boiling range 60-90°C), continue to stir and cool to room temperature, stir overnight, a large amount of colorless crystals precipitate , filtered with suction, washed 3 times with 20mL petroleum ether, removed unreacted TEP and TCT, and obtained 22.9g of colorless crystals, that is, ethyl 1,3,5-triazine-2,4,6-triphosphate (TPE, Yield: 78%).
[0047] Using the above method, just rep...
Embodiment 2
[0048] [Example 2]: Preparation of 1,3,5-triazine-2,4,6-triphosphate (TPA)
[0049] Add 19.6g TPE (0.04mol) into 130mL concentrated hydrochloric acid, reflux for 36h under magnetic stirring, cool to 50~, evaporate HCl under reduced pressure, concentrate to 40mL, extract three times with 90mL ethyl acetate to remove unhydrolyzed TPE. The aqueous phase was concentrated to nearly dryness, and dried in a vacuum oven at 120°C for 12 hours to obtain 12.3 g of white solid, namely 1,3,5-triazine-2,4,6-triphosphoric acid (TPA, yield: 96% ).
[0050] Adopt same reaction step, with different phosphites or under different reflux times, the productive rate of reaction is summarized as shown in table 1:
[0051] Table 1 The reaction conditions and yields of different phosphite reactions to prepare TPA
[0052]
Embodiment 3
[0053] [Example 3]: Preparation of 1,3,5-triazine-2,4,6-triphosphate (MTPA)
[0054] Take 9.63g TPA (0.03mol) and add it into 20mL deionized water, stir at room temperature for 30min to fully dissolve it. Get 4.05g ferric chloride hexahydrate (0.015mol) and dissolve in 30mL0.1mol L -1 In dilute hydrochloric acid (to avoid hydrolysis to generate insoluble ferric hydroxide). Add the hydrochloric acid solution of ferric chloride dropwise to the aqueous solution of TPA, and stir at room temperature for 12 hours to make the phosphonic acid group on TPA and Fe 3+ The polymerization reaction was fully carried out in between, and a yellow suspension was obtained. Suction filtration, washing with deionized water until the filtrate pH = 7 to fully remove unreacted raw materials, and drying at 120 ° C for 12 hours to obtain 6.0 g of yellow solid (yield 51%), namely 1,3,5-triazine - 2,4,6-iron triphosphate, wherein the molar ratio of iron and TPA is 1:2, so the product is recorded as F...
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