Method for manufacturing acrylonitrile-based copolymer for carbon fiber
A type of copolymer and acrylonitrile technology, which is applied in the field of preparation of acrylonitrile copolymers, can solve the problems of increased manufacturing costs, minimize side reactions, and achieve the effects of excellent spinnability
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[0028] 1. Preparation method of acrylonitrile copolymer for carbon fiber
[0029] A method for preparing an acrylonitrile-based copolymer for carbon fibers according to an embodiment of the present invention includes the following steps: 1) preparing a reaction solution comprising a monomer mixture comprising a compound represented by the following chemical formula 1 and an organic solvent sulfonate-based monomer, carboxylic acid-based monomer, and acrylonitrile-based monomer; and 2) polymerizing the reaction solution, wherein the monomer mixture contains 0.55 mol% to 1.6 mol% of the chemical formula Sulfonate monomer represented by 1:
[0030]
[0031]
[0032] In Chemical Formula 1,
[0033] R is hydrogen or C 1 to C 3 linear alkyl,
[0034] L is C 1 to C 3 linear alkylene,
[0035] X is an alkali metal.
[0036] Hereinafter, each step of a method for preparing an acrylonitrile-based copolymer for carbon fibers according to an embodiment of the present invention...
Embodiment 1 to Embodiment 8 and comparative example 1 to comparative example 8
[0064] 100 parts by weight of a monomer mixture comprising sodium methallyl sulfonate (SMAS), itaconic acid (IA) and acrylonitrile (AN) at the contents shown in Table 1 and Table 2 below are listed in Table 1 below. and contents shown in Table 2 were uniformly dissolved in dimethyl sulfoxide (DMSO) to prepare a reaction solution.
[0065] Each reaction solution was charged into a reactor equipped with a stirrer, the inside of the reactor was filled with nitrogen, and then the temperature inside the reactor was raised at a rate of 10° C. / hour to the values shown in Table 1 and Table 2 below. first temperature. Azobisisobutyronitrile (AIBN) was added at the content shown in Table 1 and Table 2 below, and the first solution polymerization was performed at the time of the first polymerization shown in Table 1 below. After that, the temperature inside the reactor was raised to the second temperature shown in Table 1 and Table 2 below at a rate of 10° C. / hour, and then carried ou...
experiment example 1
[0074] The material properties of the acrylonitrile-based copolymer solutions of Examples and Comparative Examples were measured by the methods described below, and the results are shown in Table 1 and Table 2 below.
[0075] (1) Polymerization conversion rate (%): Coagulate while immersing 0.5 g of an acrylonitrile-based copolymer solution in water to produce a film, then dry and weigh the film, and compare the obtained weight with that at the time of polymerization. The determined weight percentages of the copolymers were compared to calculate the polymerization conversion.
[0076] (2) Weight-average molecular weight (g / mol) and molecular weight distribution (polydispersity index (PDI)): Use gel permeation chromatography (GPC) to measure the weight-average molecular weight of 1 g of acrylonitrile copolymer solution under the following conditions ( Mw) and number average molecular weight (Mn) to calculate the molecular weight distribution.
[0077] Column: PLmixed B×2, solv...
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