A kind of hydrotalcite-based composite catalyst and its preparation method and application
A composite catalyst, hydrotalcite-based technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of difficult separation and reuse of homogeneous catalysts, and unsatisfactory catalytic effect
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[0046] The present invention provides a method for preparing the hydrotalcite-based composite catalyst described in the technical solution, comprising the steps of:
[0047] (1) Mix the multivalent metal salt solution with an organic base to obtain an alkaline mixed solution; the multivalent metal salt solution includes divalent metal cations and trivalent metal cations, and the divalent metal cations and trivalent metal cations are The molar ratio is 2~3.5:1;
[0048] The pH value of the alkaline mixed solution is 8-9;
[0049] (2) Under a protective atmosphere, mix the alkaline mixed solution obtained in the step (1) with the ammonium hexamolybdate salt solution to obtain a pre-reaction solution; The molar ratio is 4~7:1;
[0050] (3) Under a protective atmosphere, the pre-reaction liquid obtained in the step (2) is subjected to a hydrothermal reaction to obtain a hydrotalcite-based composite catalyst; the temperature of the hydrothermal reaction is 70 to 90°C, and the hyd...
Embodiment 1
[0086] Dissolve 1.25g of sodium molybdate in 3mL of water, and use 1.0mL6mol·L -1 The HCl solution was adjusted to pH 4.5, and then 0.80 g (n-C 4 h 9 ) 4 NCl, filter; wash twice with distilled water, ethanol respectively, obtain the isopolyacid of molybdenum ([n-(C 4 h 9 ) 4 N] 4 [Mo 8 o 26 ]). Take 0.56g[n-(C 4 h 9 ) 4 N] 4 [Mo 8 o 26 ] was dissolved in 30mL acetonitrile, and 0.17gBiCl was added 3 , reflux at 70°C for 20min, cool and stand for 10h to obtain yellow crystals, filter and wash twice with distilled water to obtain tetrabutylamine hexamolybdate ([n-(C 4 h 9 ) 4 N] 2 [Mo 6 o 19 ], abbreviated (TBA) 2 [Mo 6 o 19 ]). Under nitrogen protection, 0.96g [n-(C 4 h 9 )4 N] 2 [Mo 6 o 19 ] was dissolved in 20mL of ethanol to obtain a polymolybdate solution.
[0087] Under nitrogen protection, magnesium nitrate and aluminum nitrate were dissolved in deionized water according to the molar ratio of magnesium ions and aluminum ions in the amount of 3...
Embodiment 2
[0092] Using the hydrotalcite-based composite catalyst obtained in Example 1, the catalytic performance of the hydrotalcite-based composite catalyst was tested according to the conditions of Example 1, except that the amount of the hydrotalcite-based composite catalyst was 0.02 g.
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