Method for producing high-purity sodium p-styrenesulfonate and method for producing sodium polystyrenesulfonate
A technology of sodium polystyrene sulfonate, sodium styrene sulfonate, applied in chemical instruments and methods, nanotechnology for materials and surface science, conductive coatings, etc., can solve the problems of insufficient conductivity, stability, water resistance, etc. Poor adhesion and other problems, to achieve the effect of improving electrical conductivity
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[0110] The present invention is described more specifically through the following examples, but the present invention is not limited by these examples.
[0111] It should be noted that in the following examples, the analysis, preparation and evaluation of styrene sulfonate, PSS salt, CNT and PEDOT aqueous dispersions were carried out under the following conditions.
[0112]
[0113] A p-styrenesulfonate sample was dissolved in the following eluent A to prepare a solution with a concentration of 0.5 mg / ml, and HPLC analysis was performed. The conditions are as follows.
[0114] Model = LC-8020 manufactured by TOSOH
[0115] (Degasser: SD-8022, Pump: CCPM-II, Thermostat Oven: CO-8020, Ultraviolet Visible Light Detector: UV-8020)
[0116] Column = TSKgel ODS-80TsQA (4.6mm×25cm)
[0117] Eluent=A liquid) water / acetonitrile=95 / 5+0.1% trifluoroacetic acid
[0118] Liquid B) water / acetonitrile=80 / 20+0.1% trifluoroacetic acid
[0119] Gradient conditions = 100% of liquid A unti...
manufacture example 1
[0154] Production Example 1 [Synthesis of Radical Polymerization Initiator (Radical Polymerization Controlling Agent)]
[0155] Under a nitrogen atmosphere, 24 ml of methanol, 4.21 g (55.31 mmol) of carbon disulfide, 1.00 g (3.69 mmol) of an azo initiator V-50 (manufactured by Wako Pure Chemical Industries, Ltd.), and 3.73 g (18.44 mmol) of tri-n-butylphosphine were mixed. The mixture was put into a reaction container made of pressure-resistant glass, and reacted at 50° C. for 72 hours while stirring with a magnet stirrer under a nitrogen atmosphere. After the reaction, methanol and unreacted carbon disulfide were distilled off under reduced pressure to obtain a living radical polymerization control agent.
Embodiment 1
[0156] Embodiment 1 (manufacture example of high-purity PSSNa and CNT dispersion)
[0157] (manufacture of high-purity PSSNa)
[0158] Put 1000 g of commercially available sodium p-styrene sulfonate (SPINOMAR NaSS manufactured by TOSOH Organic Chemicals Co., Ltd.), 950 g of pure water, 40 g of sodium hydroxide, and 1 g of sodium nitrite into a 2L detachable flask, and heat at 60° C. for 1 hour, Dissolve completely while stirring. Subsequently, it was cooled to 10° C. at a rate of 10° C. for 1 hour, crystals were precipitated, and sodium p-styrenesulfonate was recovered by centrifugal filtration. A small amount of sample was accurately weighed, and the water content was calculated from the weight after vacuum drying at 50° C. for 6 hours, and it was 9.2% by weight. Sodium bromide measured with an ion chromatograph was 0.19% by weight, and sodium sulfate was 0.04% by weight. That is, the monomer component to which sodium β-bromoethylbenzenesulfonate was added was 90.57% by we...
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