Technology for purifying poly(ether-ketone-ketone) crude product by using amino tris(methylene phosphonic acid)
A technology of aminotrimethylene phosphonic acid and crude polyether ketone ketone, which is applied in the field of polymer materials, can solve the problems of polyether ketone ketone viscosity decrease, product structure change, molecular weight decrease, etc., and achieve low cost, energy saving and environmental protection of the process, less toxic effect
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Embodiment 1
[0023] Take Al 3+ To 50 g of crude polyether ketone ketone with a content of 4300 ppm, 500 g of an aqueous solution of aminotrimethylene phosphonic acid with a mass concentration of 20% was added thereto, refluxed and stirred at 100° C. for 6 hours, cooled and filtered to obtain a primary purified product.
[0024] Add the primary purified product to 1000ml of aqueous solution with a pH of 8 adjusted by ammonia water, under the action of ultraviolet light with a wavelength of 280nm and 20KHZ ultrasonic waves, pass through ozone at a rate of 1L / h and reflux for 3 hours, cool down and filter to obtain the following Grade Purity.
[0025] The secondary purified product was added to 1000g of water, washed by reflux, filtered and dried to obtain pure white polyether ketone ketone. As detected by ICP, its Al 3+ The content is 23ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.
Embodiment 2
[0027] Take Al 3+ To 50 g of crude polyether ketone ketone with a content of 4300 ppm, 750 g of an aqueous solution of aminotrimethylenephosphonic acid with a mass concentration of 10% was added thereto, stirred at reflux at 100°C for 8 hours, cooled and filtered to obtain a primary purified product.
[0028] The primary purified product was added to 750ml of aqueous solution with a pH of 9 adjusted by ammonia water, and under the action of ultraviolet light with a wavelength of 290nm and 20KHZ ultrasonic waves, ozone was refluxed at a rate of 0.5L / h for 4 hours, cooled and filtered to obtain Secondary purification.
[0029] The secondary purified product was added to 1250 g of water, washed by reflux, filtered and dried to obtain pure white polyether ketone ketone. As detected by ICP, its Al 3+ The content is 18ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.
Embodiment 3
[0031] Take Al 3+ To 50 g of crude polyether ketone ketone with a content of 4300 ppm, 1000 g of an aqueous solution of amino trimethylene phosphonic acid with a mass concentration of 1% was added thereto, refluxed and stirred at 100° C. for 10 hours, cooled and filtered to obtain a primary purified product.
[0032] The primary purified product was added to 500ml of aqueous solution with a pH of 10 adjusted by ammonia water, and under the action of ultraviolet light with a wavelength of 320nm and 20KHZ ultrasonic waves, ozone was refluxed at a rate of 0.1L / h for 5 hours, cooled and filtered to obtain Secondary purification.
[0033] The secondary purified product was added to 1500g of water, washed by reflux, filtered and dried to obtain pure white polyether ketone ketone. As detected by ICP, its Al 3+ The content is 28ppm, which meets the high-temperature use and processing requirements of polyether ketone ketone.
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