Method for preparing polyacrylonitrile spinning solution

Abstract

The invention relates to a method for preparing polyacrylonitrile spinning solution, which mainly solves the problem that a reactor easily has phenomena of adhesion, gelation and shake in the late period of polymerization in the reaction process of preparing the polyacrylonitrile spinning solution in the prior art. The problem is better solved by a technical scheme that a reactor with a double helical ribbon stirring blade is adopted in the process of preparing the polyacrylonitrile spinning solution, the lower part of the reactor has a truncated cone shape, and the double helical ribbon stirring blade corresponding to the lower part is a conical double helical ribbon stirring blade. The method can be applied to industrial production of the polyacrylonitrile spinning solution.

Description

technical field

[0001] The invention relates to a method for preparing polyacrylonitrile spinning dope. Background technique

[0002] There are many ways to polymerize acrylonitrile. Free radical polymerization mainly includes solution polymerization (SL), emulsion polymerization, suspension polymerization (SP) and bulk polymerization; it can be divided into homopolymerization or copolymerization according to the ratio of polymerized monomers; it can be divided into organic solvents and inorganic solvents according to the solvent used in polymerization ; According to the polymerization and spinning process, it can be divided into one-step method and two-step method. The so-called one-step method is that the solvent used can dissolve both the monomer and the polymer resin. The solution after polymerization can be directly used for spinning. Polymerization and spinning are a complete production line. The chain transfer constants of acrylonitrile radicals in different solvent...

Examples

Embodiment 1

[0017] use figure 1 Described 10 liters of mechanically stirred tanks (the height of the round table part accounts for about 33% of the total tank height, the volume accounts for 30% of the total tank volume, and the inclination angle θ is 50 °, wherein the outer edge of the double-screw ribbon stirring blade and the inner wall of the reactor The distance is 10 millimeters), dimethyl sulfoxide (DMSO), acrylonitrile (AN), itaconic acid (IA), initiator azobisisobutyronitrile altogether 5 kilograms add in the reactor successively, and wherein ratio is dimethyl Base sulfoxide: acrylonitrile: itaconic acid=80: 19.6: 0.4, and the initiator consumption is 0.55% of the monomer. Stir until it becomes a uniform solution, first vacuumize the system with a vacuum pump, then protect it with nitrogen, slowly heat up to the target temperature, the initial solution is colorless and transparent, stir and react at 150 rpm, as the reaction time prolongs , the viscosity of the system increases g...

Embodiment 2

[0019] use figure 1 Described 10 liters of mechanically stirred tank (the height of the round table part accounts for about 40% of the total tank height, the volume accounts for about 35% of the total tank volume, and the inclination angle θ is 60°, wherein the outer edge of the double-screw ribbon agitator and the inner wall of the reactor The distance is 8 millimeters), dimethyl sulfoxide (DMSO), acrylonitrile (AN), itaconic acid (IA), methyl acrylate (MA), and initiator azobisisobutyronitrile in turn for a total of 5 kg Add it into the reaction kettle, wherein the ratio is dimethyl sulfoxide: acrylonitrile: itaconic acid: methyl acrylate = 80: 19.6: 0.2: 0.2, and the amount of the initiator is 0.6% of the monomer. Stir until it becomes a uniform solution, first vacuumize the system with a vacuum pump, then protect it with nitrogen, slowly heat up to the target temperature, the initial solution is colorless and transparent, stir and react at 150 rpm, as the reaction time pro...

Embodiment 3

[0021] use figure 1Described 10 liters of mechanically stirred tank (the height of the round table part accounts for about 25% of the total tank height, the volume accounts for about 28% of the total tank volume, and the inclination angle θ is 40°, wherein the outer edge of the double-screw ribbon agitator and the inner wall of the reactor The distance is 6 millimeters), dimethylsulfoxide (DMSO), acrylonitrile (AN), itaconic acid (IA), initiator azobisisoheptanonitrile total 5 kilograms are added in the reactor successively, and wherein ratio is Dimethyl sulfoxide: acrylonitrile: itaconic acid=82:17.6:0.4, the amount of initiator is 0.5% of the monomer. Stir until it becomes a uniform solution, first vacuumize the system with a vacuum pump, then protect it with nitrogen, slowly heat up to the target temperature, the initial solution is colorless and transparent, stir and react at 150 rpm, as the reaction time prolongs , the viscosity of the system rises gradually, the torque ...

technical field

[0001] The invention relates to a method for preparing polyacrylonitrile spinning dope. Background technique

[0002] There are many ways to polymerize acrylonitrile. Free radical polymerization mainly includes solution polymerization (SL), emulsion polymerization, suspension polymerization (SP) and bulk polymerization; it can be divided into homopolymerization or copolymerization according to the ratio of polymerized monomers; it can be divided into organic solvents and inorganic solvents according to the solvent used in polymerization ; According to the polymerization and spinning process, it can be divided into one-step method and two-step method. The so-called one-step method is that the solvent used can dissolve both the monomer and the polymer resin. The solution after polymerization can be directly used for spinning. Polymerization and spinning are a complete production line. The chain transfer constants of acrylonitrile radicals in different solvent...

Examples

Embodiment 1

[0017] use figure 1 Described 10 liters of mechanically stirred tanks (the height of the round table part accounts for about 33% of the total tank height, the volume accounts for 30% of the total tank volume, and the inclination angle θ is 50 °, wherein the outer edge of the double-screw ribbon stirring blade and the inner wall of the reactor The distance is 10 millimeters), dimethyl sulfoxide (DMSO), acrylonitrile (AN), itaconic acid (IA), initiator azobisisobutyronitrile altogether 5 kilograms add in the reactor successively, and wherein ratio is dimethyl Base sulfoxide: acrylonitrile: itaconic acid=80: 19.6: 0.4, and the initiator consumption is 0.55% of the monomer. Stir until it becomes a uniform solution, first vacuumize the system with a vacuum pump, then protect it with nitrogen, slowly heat up to the target temperature, the initial solution is colorless and transparent, stir and react at 150 rpm, as the reaction time prolongs , the viscosity of the system increases g...

Embodiment 2

[0019] use figure 1 Described 10 liters of mechanically stirred tank (the height of the round table part accounts for about 40% of the total tank height, the volume accounts for about 35% of the total tank volume, and the inclination angle θ is 60°, wherein the outer edge of the double-screw ribbon agitator and the inner wall of the reactor The distance is 8 millimeters), dimethyl sulfoxide (DMSO), acrylonitrile (AN), itaconic acid (IA), methyl acrylate (MA), and initiator azobisisobutyronitrile in turn for a total of 5 kg Add it into the reaction kettle, wherein the ratio is dimethyl sulfoxide: acrylonitrile: itaconic acid: methyl acrylate = 80: 19.6: 0.2: 0.2, and the amount of the initiator is 0.6% of the monomer. Stir until it becomes a uniform solution, first vacuumize the system with a vacuum pump, then protect it with nitrogen, slowly heat up to the target temperature, the initial solution is colorless and transparent, stir and react at 150 rpm, as the reaction time pro...

Embodiment 3

[0021] use figure 1Described 10 liters of mechanically stirred tank (the height of the round table part accounts for about 25% of the total tank height, the volume accounts for about 28% of the total tank volume, and the inclination angle θ is 40°, wherein the outer edge of the double-screw ribbon agitator and the inner wall of the reactor The distance is 6 millimeters), dimethylsulfoxide (DMSO), acrylonitrile (AN), itaconic acid (IA), initiator azobisisoheptanonitrile total 5 kilograms are added in the reactor successively, and wherein ratio is Dimethyl sulfoxide: acrylonitrile: itaconic acid=82:17.6:0.4, the amount of initiator is 0.5% of the monomer. Stir until it becomes a uniform solution, first vacuumize the system with a vacuum pump, then protect it with nitrogen, slowly heat up to the target temperature, the initial solution is colorless and transparent, stir and react at 150 rpm, as the reaction time prolongs , the viscosity of the system rises gradually, the torque ...

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