A method for preparing high ortho thermosetting phenolic fiber by wet spinning
A wet spinning and phenolic fiber technology, applied in the field of flame retardant, can solve the problems of pollution electrospinning, difficult mass production, etc., and achieve the effects of reducing energy consumption, simple processing and high molecular weight
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Embodiment 1
[0024] A method for preparing high-ortho position thermosetting phenolic fibers by wet spinning, specifically comprising the following steps:
[0025] (1) Heat phenol and formaldehyde (the molar ratio of phenol to formaldehyde is 1:0.8) under the action of zinc acetate (100 parts by mass of phenol, 1 part by mass of zinc acetate), heat to boiling for 2 hours, add concentrated Sulfuric acid (the mass ratio of phenol to concentrated sulfuric acid is 100:0.2), continue to react for 0.5h, carry out dehydration under reduced pressure, and lower the temperature to 40°C, then raise the temperature to 105°C at 1°C / min, vacuum degree is 8500Pa, react for 0.1h, Obtain high ortho-position thermoplastic phenolic resin until the solution is viscous;
[0026] (2) The obtained high-ortho-position thermoplastic phenolic resin is dissolved in ethanol (the mass ratio of high-ortho-position thermoplastic phenolic resin to absolute ethanol is 3:4), and in triethanolamine (the mass ratio of trieth...
Embodiment 2
[0030] A method for preparing high-ortho position thermosetting phenolic fibers by wet spinning, specifically comprising the following steps:
[0031] (1) Heat phenol and acetaldehyde (the molar ratio of phenol to acetaldehyde is 1:1) under the action of cadmium acetate (phenol is calculated as 100, cadmium acetate is 3), and heated to boiling for 6 hours, and hydrochloric acid (phenol The mass ratio with hydrochloric acid is 100:2), continue to react for 4h, carry out dehydration under reduced pressure, and lower the temperature to 85°C, then raise the temperature to 170°C at 1°C / min, keep the temperature at 8500Pa for 4h to react until the solution is viscous, and get High ortho thermoplastic phenolic resin;
[0032] (2) The obtained high-ortho-position thermoplastic phenolic resin is dissolved in ethanol (the mass ratio of high-ortho-position thermoplastic phenolic resin to absolute ethanol is 3:9), and in ammonium hydroxide (ammonium hydroxide and high-ortho-position therm...
Embodiment 3
[0036] A method for preparing high-ortho position thermosetting phenolic fibers by wet spinning, specifically comprising the following steps:
[0037] (1) Heat phenol and furfural (the molar ratio of phenol to furfural is 1:0.9) under the action of cobalt acetate (phenol is calculated as 100, cobalt acetate is 2), and heated to boiling for 3 hours, then dropwise add phosphoric acid (phenol and phosphoric acid The mass ratio of 100:1), continue to react for 2h, carry out dehydration under reduced pressure, and lower the temperature to 70°C, then raise the temperature to 130°C at 0.5°C / min, vacuum degree is 8500Pa, keep constant temperature for 3h to react until the solution becomes viscous High ortho thermoplastic phenolic resin;
[0038] (2) The obtained high-ortho-position thermoplastic phenolic resin is dissolved in ethanol (the mass ratio of high-ortho-position thermoplastic phenolic resin to absolute ethanol is 3:7), and in ammonium hydroxide (ammonium hydroxide and high-o...
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