Piperazine boric acid polymer used as fire retardant and preparation method thereof
A flame retardant and polymer technology, which is applied in the preparation of piperazine boric acid polymers and the preparation of flame retardants, can solve problems such as limiting the application field of compounds, and achieve excellent carbon-forming effect, excellent heat resistance, and manufacturing process. simple effect
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Embodiment 1
[0022] Add 1Kg of piperazine and 10kg of diphenyl ether into the reactor at normal pressure. After stirring for 30 minutes, add 4.3kg of boric acid powder in batches and stir at room temperature for 1-2 hours. When it is small, start to heat up to 250° C. After reacting for 5 hours, suction filter and wash with methanol, and dry in a vacuum oven at 80° C. for 4 hours. The product yield is 93% (theoretical yield is calculated by piperazine).
[0023] In order to explore the influence of the reaction temperature on the synthesis of the sample, the reaction temperature was changed under the condition of other conditions unchanged in the embodiment. It can be seen that the sample was in the range of 150-190°C, and an intermediate was obtained; when the temperature continued to rise to 230°C , the intermediate gradually disappears, and when the temperature exceeds 250°C, the characteristic spectrum of the target product appears ( figure 1 ).
[0024] In addition, the influence of ...
Embodiment 2
[0027] In the high-pressure reactor, add 1Kg piperazine and 12 kg of monobutyl glycol, after stirring for 60 minutes, add 4.2 kg of boric acid powder in batches, and stir at room temperature for 1-2 hours. The viscosity of the reaction material changes greatly in the initial stage of stirring, etc. When the viscosity change is small, start to heat up to 240°C. After reacting for 8 hours, suction filter and wash with methanol, and dry in an oven at 100°C for 12 hours. The product yield is 93% (theoretical yield is calculated by piperazine).
Embodiment 3
[0029] In the high-pressure reactor, add 1Kg piperazine and 5 kg of diphenyl ether, after stirring for 30 minutes, add 3.8 kg of boric acid powder in batches, and stir at room temperature for 1-2 hours. hour, close the loam cake, begin to heat up to 260 DEG C, after reacting for 5 hours, drop to room temperature, add 5L methanol, suction filter and wash with methanol, dry 12h in oven at 100 DEG C, product yield is 90% (calculate theoretically with piperazine Yield).
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