Microchannel reaction equipment and preparation method of halogen-free organophosphorus flame retardant
A technology of microchannel reaction and organic phosphorus, which is applied in organic chemistry, chemical instruments and methods, chemical/physical/physical chemical reactors, etc., can solve the problems of consumption of product phosphorus oxychloride, extended reaction cycle, and long time consumption. Achieve the effects of no amplification effect, shortened reaction cycle, and high mass and heat transfer efficiency
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Embodiment 1
[0051] Embodiment 1, weigh 1.5g titanium tetrachloride and join in 150g phosphorus oxychloride bottle, take 378g isooctanol in the second bottle, use diaphragm pump to 15g / min, use Hanbang pump to 37.8g The speed of / min was injected into the module of the microchannel reactor, and the temperature of the reaction module was set to 40 °C. After 5 reaction modules, it was collected into a closed container, and subjected to alkali washing, water washing, steam distillation, and filtration. 99.8%, yield 94%.
Embodiment 2
[0052] Embodiment 2, weigh 1.5g titanium tetrachloride and join in 150g phosphorus oxychloride bottle, take 382g isooctanol in the second bottle, use diaphragm pump at 20g / min, use Hanbang pump at 50.93 g The speed of / min was injected into the module of the microchannel reactor. The temperature of the reaction module was set to 60 °C. After 5 reaction modules, it was collected into a closed container, and subjected to alkali washing, water washing, steam distillation, and filtration. 99.7%, yield 98.5%.
Embodiment 3
[0053] Embodiment 3, get 1.5g titanium tetrachloride and join in 150g phosphorus oxychloride bottle, take 390g isooctanol in the second bottle, use diaphragm pump at 30g / min, use Hanbang pump at 78g / min. The speed of min is injected into the module of the microchannel reactor, the temperature of the reaction module is set to 70 °C, after 5 reaction modules, it is collected in a closed container, and after alkali washing, water washing, steam distillation, and filtration, the content is 99.5 %, the yield is 96.5%.
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