Perhalide-type ionic liquid solvents for metals and metal compounds
一种离子液体、金属的技术,应用在卤化汞、有机化学、散装化学品生产等方向,能够解决危险、困难等问题
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Embodiment 1
[0113] Embodiment 1: the synthesis of perhalide ionic liquid
[0114] Ionic liquids with mixed perhalogen anions ([XY 2 ] - , wherein X=Cl or Br, and Y=Br or I) according to literature method with dialkylimidazolium (dialkylimidazolium), tetraalkylammonium (tetraalkylammonium), tetraalkylphosphonium (tetraalkylphosphonium) and alkylpicoline Onium (alkylmethylpyridinium) cation (see Table 1) preparation. Briefly, liquid bromine or solid iodine is added to an appropriate amount of an organic halide salt to achieve the desired 1:1 molar stoichiometry, yielding a perhalide anion. The mixture was mixed overnight at room temperature to yield the respective perhalide ionic liquids, which were characterized by mass spectrometry and thermogravimetric analysis (TGA).
[0115] Mass spectrometric identification of cations in each case ([Q] + ) and perhalogen anions ([XY 2 ] - ) in the presence of ionic masses. TGA showed that the volatilization of halogens was significantly reduced...
Embodiment 3
[0121] Example 3: Dissolution of metals
[0122]A series of powdered elemental metal samples (approximately 0.1 g each, accurately measured) were mixed with 1-butyl-3-methylimidazoliumtribromide (1.0 mL) to produce Mixture of approximately 5 wt% metal in ionic liquid. The mixture was stirred and heated to 60 °C for 72 h, then cooled to room temperature and filtered through a 2 micron nylon filter. For each sample, approximately 0.1 g of filtrate was accurately weighed and digested in 50 ml of 5% w / w nitric acid, and the metal content was determined by inductively coupled plasma (ICP) analysis. The percentage of metal samples dissolved in ionic liquids in each test is shown in Table 2.
[0123] Table 2. Metal Dissolution Test Results
[0124]
Embodiment 4
[0125] Example 4: Qualitative Screening for Mercury Solubilization
[0126] Qualitative screening of the solubility of elemental mercury in ionic liquid systems has been performed by visually observing the state of individual mercury droplets (approximately 0.05 g) stirred in approximately 1-2 mL of ionic liquid at room temperature and 60°C. Complete dissolution under these conditions would result in a mercury loading of about 25-50,000 ppm (about 5 mol%).
[0127] Table 3. Screened perhalide ionic liquids and observations on mercury solubility
[0128]
[0129]
[0130] a [C 4 mim] + =1-butyl-3-methylimidazolium; [P 6,6,6,14 ] + = Trihexyltetradecylphosphonium; [C 2 C 2 mim] + =1,3-diethylimidazolium; [N 4,4,4,1 ] + = Tributylmethylammonium; [C 4 4 pic] + = 1-butyl-4-methylpyridinium (4-picolinium) (4-picolinium).
[0131] b About 0.05g of mercury is in contact with 1-2mL of ionic liquid, and the mercury solubility is at least 25,000ppm.
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