Reaction accelerator, and method for producing urethane compound, thiocarbamate compound, amide compound, or urea compound using same
A technology of reaction accelerators and compounds, applied in the field of manufacture of reaction accelerators and carbamate compounds, thiocarbamate compounds, amide compounds or urea compounds using them, capable of solving physical properties of cured products Adverse effects, insufficient promotion effects, etc.
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[0151] Hereinafter, the present invention will be described in detail through examples, but the present invention is not limited by these examples.
[0152] In the following examples, unless otherwise specified, "%" means mass% (wt%), and "ppm" means mass ppm (wtppm).
[0153] The conditions of liquid chromatography analysis (hereinafter referred to as "LC analysis") are as follows.
[0154] Columns: 4 manufactured by Showa Denko Co., Ltd., brand name "Shodex (registered trademark) KF-801",
[0155] Eluent: Tetrahydrofuran (THF),
[0156] Flow rate: 0.8mL / min,
[0157] Oven temperature: 40℃,
[0158] Detector: Differential refractive index (RI)·UV (wavelength 210nm)
[0159] (Preparation method of reaction accelerator)
Synthetic example 1
[0161] Into a 100 mL three-necked flask, 10.0 g of methacryloyloxyethyl isocyanate (Karensun MOI (registered trademark), manufactured by Showa Denko Corporation. Hereinafter referred to as "MOI") was placed, and the inner temperature was cooled to 15°C while 2.58 g of dry hydrogen chloride was bubbled into methacryloxyethyl isocyanate through an inner cannula to obtain 12.6 g of methacryloxyethylcarbamoyl chloride (hereinafter referred to as "MOC"). The purity is 100%.
Synthetic example 2
[0163] 110 g of aminoethyl methacrylate hydrochloride (hereinafter referred to as "AEMHCl") was put into 200 g of toluene, and 110 g of phosgene was supplied in a state where AEMHCl was melted at an internal temperature of 85°C to synthesize MOI. The dissolved phosgene was removed by bubbling nitrogen gas into the reaction liquid, and then toluene as a solvent was distilled off under reduced pressure to obtain 110 g of crude MOI.
[0164] The MOC content in the crude MOI was confirmed by silver nitrate titration, and the result was 10.8%.
[0165] (Accelerating effect of urethanization reaction based on reaction accelerator addition)
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