N-vinyl amide polymer and production method thereof
A kind of vinyl amide, the technology of the manufacturing method, is applied in the N-vinyl amide polymer and its manufacture field, can solve the problem such as the record that there is no N-vinyl amide polymer manufacture
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[0132] The present invention will be described in more detail with reference to examples below, but the present invention is not limited to these examples. In addition, "part" means "weight part", and "%" means "mass %" unless otherwise specified.
[0133] [K value determination method]
[0134] The relative viscosity of the 1 mass % N-vinylamide polymer aqueous solution was measured with a capillary viscometer at 25° C., and the result was substituted into the following formula for calculation.
[0135] Logη rel / C=[(75K 0 2 ) / (1+1.5K 0 C)]+K 0
[0136] K=1000K 0
[0137] C: grams of N-vinylamide polymer in 100ml solution
[0138] n re1 : relative viscosity
[0139] [Methods for Measuring the Amount of N-Vinylpyrrolidone and the Amount of 2-Pyrrolidone]
[0140] Quantification was performed by liquid chromatography.
[0141] [Ash content determination method]
[0142] Based on the measurement method of the strong heat residue in the Japanese Pharmacopoeia.
[014...
Embodiment 1
[0146] use as figure 1 The polymerization apparatus shown was operated. An aqueous monomer solution containing 60 parts of N-vinylpyrrolidone and 40 parts of ion-exchanged water was prepared, and oxygen dissolved in the aqueous solution was sufficiently removed by bubbling nitrogen bubbles. Nitrogen exchange is performed on the inside of the reaction vessel in advance and the surface is heated to 100°C. The monomer aqueous solution is put into the reaction vessel from the feed port 1, and then the initiator solution is put into the feed port 2. The initiator solution is 0.06 One part of azo initiator V-59 (trade name, produced by Wako Pure Chemical Industries, Ltd., 2,2'-azobis (2-methylbutyronitrile)) was dissolved in 1 part of isopropanol (IPA) to form . The liquid depth of the reaction liquid in the reaction container was 10 mm. The polymerization was carried out under nitrogen flow, and the temperature of the reaction liquid reached 100° C. after about 5 minutes. There...
Embodiment 2
[0149] The reaction was carried out in exactly the same manner as in Example 1 except that the amount of the azo-based initiator was 0.12 parts. After about 5 minutes, the temperature of the reaction liquid reached 100°C. Thereafter, the temperature was maintained at not lower than 100° C. for 12 minutes to obtain a colorless, transparent, slightly soft solid block. As a result of analysis, the K value was 95.3, N-vinylpyrrolidone was 2400 ppm with respect to the resin component, and 0.1 ppm of 2-pyrrolidone was contained. In addition, the APHA of the 10% aqueous solution was 5, and the ash content was 200 ppm. The results are shown in Table 1.
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