Ignition accelerant for hydrogen peroxide-spontaneous combustion ionic liquid as well as preparation method and application of ignition accelerant
An ignition accelerator, ionic liquid technology, applied in offensive equipment, compressed gas generation, organic chemistry, etc., can solve problems such as difficult spontaneous ignition, and achieve the effect of improving combustion performance and good compatibility
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Embodiment 1
[0032] Preparation of 1-methyl-4,5-diiodoimidazolium iodide salt:
[0033] ;
[0034] At room temperature, add (5.02g, 15.6mmol) 4,5-diiodoimidazole, (4.751g, 34.4mmol) potassium carbonate and 70ml acetonitrile into a 250ml round bottom flask, then react at a constant temperature at 30°C for 4h, and then (4.436 g, 31.2 mmol) methyl iodide was added dropwise within 10 minutes under atmosphere, and the reaction mixture was kept at 30° C. for 72 hours after the addition was complete. After the reaction, the solvent acetonitrile was filtered off with a sand core funnel to obtain the crude product 1-methyl-4,5-diiodoimidazole iodide salt. The crude product was washed with ethyl acetate and cold water, and then vacuum-dried to obtain the product 1-methyl-4,5-diiodoimidazolium iodide salt (4.306 g, yield 82.65%) as a white solid.
Embodiment 2
[0036] Preparation of accelerator 1,3-dimethyl-4,5-diiodoimidazole iodine salt:
[0037] ;
[0038] Add (4g, 11.98mmol) 1-methyl-4,5-diiodoimidazolium iodide salt and 50ml N,N-dimethylformamide to a 100ml round-bottomed flask at room temperature, and then under nitrogen atmosphere for 10 minutes (3.401 g, 23.96 mmol) methyl iodide was added dropwise, and after the addition was complete, the reaction mixture was heated to 50° C. for 24 hours. After the reaction, the solvent N,N-dimethylformamide was filtered off with a sand core funnel to obtain the crude product 1,3-dimethyl-4,5-diiodoimidazolium iodide salt. The crude product was washed with ethanol and diethyl ether, and then vacuum-dried to obtain the product 1,3-dimethyl-4,5-diiodoimidazolium iodide salt (3.785 g, yield 66.40%) as a white solid.
[0039] The test data of accelerator 1,3-dimethyl-4,5-diiodoimidazolium iodide salt is as follows: IR: ν=3134, 3110, 3086, 3045, 2939, 1652, 1553, 1438, 1235, 1192, 1101, 108...
Embodiment 3
[0041] Preparation of accelerator 1,3-dimethyl-4,5-diiodoimidazole triiodide:
[0042] ;
[0043] At room temperature, add (0.267g, 1.05mmol) iodine simple substance and 80ml acetone to a 100ml round bottom flask, then add (0.5g, 1.05mmol) 1,3-dimethyl-4,5-diiodoimidazole iodine salt, after the addition was complete the reaction mixture was warmed to 25°C for 10 hours. After the reaction, the solvent acetone in the system was removed by rotary evaporation, and then vacuum-dried to obtain 1,3-dimethyl-4,5-diiodoimidazole triiodide salt.
[0044] The test data of accelerator 1,3-dimethyl-4,5-diiodoimidazole triiodide salt is as follows: 1H NMR (DMSO-d6): δ 9.42 (1H, s, CH), 3.82 (6H, s, CH3 ). 13C NMR (DMSO-d6): δ38.82, 94.03,140.75. ESI: m / z calcd for anion [M]−: 380.70; found: 380.70; calcd forcation [M]+: 348.89; found: 348.91. Elemental analysis of C5H7I5N2 (729.626). Calcd: C, 8.23; H, 0.967; N, 3.84. Found: C, 8.95; H, 0.95; N, 4.01.
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