Phosphorus-containing flame-retardant polybutadiene material and preparation method thereof
A technology of polybutadiene and polybutadiene, which is applied in the field of phosphorus-containing flame-retardant polybutadiene materials and its preparation, can solve the problems of easy loss of flame retardants, poor compatibility between flame retardants and polymers, etc. , to achieve the effect of durable flame retardancy
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Embodiment 1
[0029] In a three-necked flask, add 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) (4mmol) and acrylic acid (6mmol), stir, heat to 80°C, and reflux for 6h , to obtain a light yellow and transparent mixed product; the product was separated by precipitation, dissolved in acetone and then added with 1000 mL of chloroform as a precipitant, filtered to obtain a white solid product, and finally vacuum-dried to obtain DOPO derivative 10-propionic acid-9,10- Dihydro-9-oxa-10-phosphaphenanthrene-10V oxide, yield 80.6%.
Embodiment 2
[0031] Add the DOPO derivative 10-propionic acid-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10V oxide (5.0mmol) and 20ml of anhydrous tetrahydrofuran THF into the reactor until the reaction temperature rises to After 70°C, slowly add SOCl dropwise 2 (5.0mmol), dropwise completed reaction 2h, after finishing reaction, decompression distillation removes SOCl 2 and THF to obtain DOPO derivative 10-propionic acid-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10V oxide acid chloride product.
[0032] Hydroxyl-terminated polybutadiene (50.0mmol) was added to a 50ml Schlenk bottle, and after pumping nitrogen three times, N 2 Under protection, add 30ml of anhydrous toluene into a disposable syringe, raise the temperature to 70°C, inject 1ml of pyridine after the hydroxyl-terminated polybutadiene is completely dissolved, stir for 30min, and add the DOPO derivative 10-propionic acid dissolved in toluene dropwise -9,10-dihydro-9-oxa-10-phosphaphenanthrene-10V oxide acid chloride product, he...
Embodiment 3
[0034] 100 parts by mass of polybutadiene grafted nitrogen-phosphorus flame retardant, 10 parts by mass of anti-dripping agent, 2 parts by mass of composite antioxidant, 3 parts by mass of other additives in a mixer at 25°C at 600 rpm Mix at a high speed for 20 minutes, and the mixed material is extruded through an extruder at 230° C., cooled, dried, and pelletized to obtain a phosphorus-containing flame-retardant polybutadiene material.
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