In-situ phosphorized catalyst for preparing cycloalkane from lignin as well as preparation method and application of catalyst
An in-situ phosphating and cycloalkane production technology, which is applied in the field of lignin conversion, can solve the problems of increased catalyst washing costs, harsh phosphating conditions, and poor economic efficiency, and achieves the effects of easy operation, mild phosphating conditions, and low cost
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[0037] The present invention also provides a preparation method of the in-situ phosphatized lignin catalyst for preparing naphthenic hydrocarbons, comprising:
[0038] (1) Under stirring, the Cu-containing 2+ , Mg 2+ , Al 3+ The mixed solution and NaOH solution were dropped into Na 2 CO 3 In the solution, control the temperature and pH of the mixed solution to precipitate it;
[0039] (2) after the dropwise addition is completed, the mixed solution is aged under stirring, and then the Cu-Mg-Al hydrotalcite precursor is obtained after filtering, washing and drying;
[0040] (3) grinding the precursor into powder, and then calcining to obtain a metal oxide;
[0041] (4) reducing and activating the metal oxide to obtain Cu / CuMgAlO x intermediate, and then uniformly mix red phosphorus and intermediate to obtain mixed powder;
[0042] (5) Phosphating the mixed powder in-situ in an inert atmosphere to obtain the catalyst.
Embodiment 1
[0056] 0.072mol Mg(N0 3 ) 2 ·6H 2 0.0.025mol Al(NO 3 ) 3 ·9H 2 O, 0.003mol Cu (NO 3 ) 2 ·3H 2 O was dissolved in 150mL deionized water to form a mixed solution of metal ions; 0.25mol NaOH was dissolved in 250mL deionized water, 0.025mol Na 2 CO 3 Dissolved in 187.5mL deionized water;
[0057] will Na 2 CO 3 The solution was transferred to a 1L beaker, heated to 55°C by a water bath under stirring, and the metal ion mixed solution and NaOH solution were slowly dropped into the beaker by a peristaltic pump, and the temperature of the mixture was kept at 55°C and pH 10;
[0058] After the titration, the mixed solution was transferred to a 1L sealed glass bottle, and aged at 55°C under stirring;
[0059] After the aging, the mixed solution was filtered with a Buchner funnel (the same below), and the filtered solid was redispersed in 150mL containing 15gNa 2 CO 3 The solution was poured back into the glass bottle and stirred at 55°C for 1 h; the mixture was filtered aga...
Embodiment 2
[0064] The steps are the same as in Example 1, except that the mass ratio of red phosphorus to the intermediate is 0.04:1, and the conditions such as the dosage of other reagents are the same as those in Example 1; the catalyst is marked as B.
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