Preparation method of polyamideimide fine powder
A technology of polyamideimide and polyamic acid amic acid is applied in the field of preparation of polyamideimide fine powder, and can solve the problems of preparing polyamideimide fine powder, unable to adopt solution precipitation method, etc.
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Embodiment 1
[0019] Under the protection of nitrogen, the N-methylpyrrolidone solution of 20L of polyamic acid with an apparent viscosity of 500mPas was pressurized to 1MPa through a booster pump, and the compressed nitrogen of 1MPa was mixed with the pressurized polyamic acid solution at the same time. Spray from the spout. The atomized droplets enter the spray precipitation tower equipped with 50L of vigorously stirred methanol solution, and the stirring rate is controlled at 600rpm. After the spraying was completed, the above mixture was added into the washing and filtering tower for washing and filtering twice, and the residual amount of NMP solvent was 3.9 wt%. The obtained polyamide-amic acid powder was vacuum-dried at 80° C. for 12 hours, and thermally imidized at 200° C. for 4 hours to obtain a polyamide-imide fine powder with a D50 particle size of 32.6 μm.
Embodiment 2
[0021] Under the protection of nitrogen, 20L of N,N-dimethylacetamide solution of polyamic acid with an apparent viscosity of 2000mPas is pressurized to 5MPa through a booster pump, and at the same time, the compressed air of 5MPa is mixed with the pressurized polyamideamide The acid solution is mixed and sprayed from the spout. The atomized droplets enter the spray precipitation tower equipped with 100L of vigorously stirred ethanol solution, and the stirring rate is controlled at 600rpm. After the spraying is completed, the above mixture is added into the washing and filtering tower for washing and filtering twice, and the residual amount of DMAc solvent is 3.1 wt%. The obtained polyamide-amic acid powder was vacuum-dried at 120° C. for 8 hours, and heat-treated at 230° C. for 3 hours to obtain a polyamide-imide fine powder with a D50 particle size of 28.2 μm.
Embodiment 3
[0023] Under the protection of nitrogen, pressurize 20L of DMAc solution of polyamic acid with an apparent viscosity of 10000mPas to 0.5MPa through a booster pump, and at the same time mix 0.5MPa compressed air with the pressurized polyamic acid solution and send it from the nozzle squirt. The atomized droplets enter the spray precipitation tower equipped with 100L of vigorously stirred ethanol solution, and the stirring rate is controlled at 600rpm. After the spraying was completed, the above mixture was added into the washing and filtering tower for washing and filtering twice, and the residual amount of DMAc solvent was 9.2wt%. The obtained polyamide-amic acid powder was vacuum-dried at 150° C. for 8 hours, and heat-treated at 230° C. for 3 hours to obtain a polyamide-imide fine powder with a D50 particle size of 487 μm.
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