Barium dibenzofuranoate compound and its preparation method, anion initiating system and preparation method of conjugated diene polymer
A technology of benzofuran carboxylic acid and furan carboxylic acid, which is applied in directions such as organic chemistry, can solve problems such as the recovery of polymer solvents with high trans structure content, and can shorten the polymerization reaction time, promote the polymerization reaction, and achieve low prices. Effect
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preparation example Construction
[0057] According to the fourth aspect of the present invention, the preparation method of the conjugated diene polymer comprises: in the presence of the above-mentioned anion initiating system, performing anionic polymerization reaction of the polymerizable monomer containing conjugated diene in a solvent.
[0058] According to the present invention, the amount of the anion initiating system can be reasonably selected according to the expected molecular weight (design molecular weight) of the conjugated diene polymer. Generally, the amount of the anion initiating system can make the conjugated diene The designed molecular weight of the polymer is 50000-80000, preferably 55000-65000.
[0059] The present invention has no particular limitation on the anionic polymerization reaction conditions, for example, generally, the polymerization temperature may be 50-120°C, preferably 50-90°C; the polymerization time may be 0.5-4 hours, preferably 0.5-3 hours. In addition, in the process ...
preparation example 1
[0093] This preparation example is used to illustrate the preparation method of the barium dibenzofuranoate compound provided by the present invention.
[0094] 0.05mol of 1-benzofuran-6-carboxylic acid (purchased from Shanghai Keplin Fine Chemical Co., Ltd., has the structure shown in formula (II), R 1 and R 2 For H, the same below), 0.02mol barium hydroxide and 150mL ethylbenzene were added to a 250mL two-necked flask equipped with a water separator, under the protection of high-purity nitrogen, placed in an oil bath at 130°C to maintain boiling and reflux reaction , Stop the reaction until there is basically no liquid separated from the water separator, and the product is washed with water to obtain barium dibenzofuranoate compound (marked as B1). Through infrared and nuclear magnetic detection, the barium dibenzofuranoate compound has the structure shown in formula (I), and R 1 -R 4 Both are H.
preparation example 2
[0096] This preparation example is used to illustrate the preparation method of the barium dibenzofuranoate compound provided by the present invention.
[0097] 0.05mol of 1-benzohexylfuran-6-carboxylic acid (purchased from Shanghai Caplin Fine Chemical Co., Ltd., has the structure shown in formula (II), R 1 for H, R 2 is n-hexyl), 0.17mol barium hydroxide and 150mL ethylbenzene were added to a 250mL two-necked flask, and under the protection of high-purity nitrogen, they were placed in an oil bath at 100°C to keep boiling and reflux until there was almost no The reaction was stopped until the liquid was separated, and the product was washed with water to obtain a barium dibenzofuranoate compound (referred to as B2). Through infrared and nuclear magnetic detection, the barium dibenzofuranoate compound has the structure shown in formula (I), and R 1 and R 3 for H, R 2 and R 4 For n-hexyl.
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