Homogeneous phase dual-function catalyst for synthesizing p-aminophenol and preparation and use method thereof
A bifunctional catalyst and p-aminophenol technology, which is applied in the preparation of amino hydroxyl compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of wastewater discharge environmental pollution, harsh reaction conditions, and non-reusable use, etc., and achieve stability Good performance, simple preparation method, and no reduction in catalytic activity
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Embodiment 1
[0032] Synthesis of acidic ionic liquid N,N,N-trimethyl-N-sulfobutyl-ammonium bisulfate:
[0033] ①Take 0.50mol trimethylamine aqueous solution and 0.5~0.55mol 1,4-butane sultone, put them in a 250ml three-necked flask, react at room temperature~60℃ for 8~48 hours, then take out the reaction solution Afterwards, the water was distilled off under reduced pressure to obtain a white zwitterionic solid, which was washed sequentially with absolute ethanol, toluene and anhydrous ether, and then vacuum-dried to constant weight at 80°C to obtain the zwitterionic N, N , N-trimethyl-N-sulfobutylammonium ([TMBS]).
[0034] ②Put 0.50mol [TMBS] into a four-neck flask, and slowly add 0.48-0.52mol of concentrated sulfuric acid (95%-98% by mass) dropwise while keeping the temperature below 10°C, and then raise the temperature to 70°C , and reacted for 6 hours to obtain the target product acidic ionic liquid N,N,N-trimethyl-N-sulfobutyl-ammonium bisulfate. FT-IR(KBr): υ max : 3044, 2968, 14...
Embodiment 2
[0038] The first step, according to the molar ratio: the acidic ionic liquid N, N, N-trimethyl-N-sulfobutyl-ammonium bisulfate prepared in Example 1: the ratio of platinum=1000: 1, the acidic ion Liquid N,N,N-trimethyl-N-sulfobutyl-ammonium bisulfate 1.802g and chloroplatinic acid 3.186mg (1.2mg equivalent to metallic platinum) were placed in a three-necked flask, methanol and deionized water were added, and , methanol is 5ml, deionized water is 25ml, and magnetically stirred for 5 hours under reflux to obtain a colloidal dispersion system of Pt nanoparticles under the protection of acidic ionic liquid;
[0039] In the second step, the colloidal dispersion system of Pt nanoparticles under the protection of the acidic ionic liquid prepared in the second step is distilled under reduced pressure (vacuum degree 0.09-0.1MPa), and the target product homogeneous phase of the dark brown transparent state is obtained. Bifunctional catalyst.
Embodiment 3
[0041] The first step, according to the molar ratio: the acidic ionic liquid N, N, N-trimethyl-N-sulfobutyl-ammonium bisulfate prepared in Example 1: the ratio of platinum=6000: 1, the acidic ion Liquid N,N,N-trimethyl-N-sulfobutyl-ammonium bisulfate 10.813g and chloroplatinic acid 3.186mg (equivalent to 1.2mg metal platinum) were placed in a three-necked flask, and absolute ethanol and deionized water were added , wherein, 24ml of absolute ethanol, 8ml of deionized water, and magnetic stirring at 50°C for 0.5 hours, the colloidal dispersion system of Pt nanoparticles under the protection of acidic ionic liquid is obtained;
[0042] In the second step, the colloidal dispersion system of Pt nanoparticles under the protection of the acidic ionic liquid prepared in the second step is distilled under reduced pressure (vacuum degree 0.09-0.1MPa), and the target product homogeneous phase of the dark brown transparent state is obtained. Bifunctional catalyst.
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