Preparation method and application of solid super acidic catalyst
A solid superacid and catalyst technology, which is applied in the preparation of organic compounds, carboxylic acid ester preparation, molecular sieve catalysts, etc., to achieve the effects of high conversion rate and purity, mild reaction conditions, and high catalytic activity
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[0041] A kind of preparation method of solid superacid catalyst of the present invention, comprises the steps:
[0042](1) Preparation of iron-neodymium cross-linking agent: prepare iron solution, neodymium nitrate solution and sodium hydroxide solution; add the prepared sodium hydroxide solution dropwise to the mixture of iron solution and neodymium nitrate at a rate of 2 to 4ml / min In the solution, add distilled water dropwise to adjust the pH to 8-9, keep the temperature at 35-55°C, stir at a constant temperature for 8.5-11 hours, keep the temperature at 15-25°C for aging, and the aging time is 25-45min to obtain Iron-neodymium crosslinking agent; comprising the following components in parts by volume:
[0043] 12-18 parts of iron solution,
[0044] 15-20 parts of neodymium nitrate solution,
[0045] 18-25 parts of sodium hydroxide solution.
[0046] (2) Acidification of titanium-silicon molecular sieve: prepare sulfuric acid with a mass concentration of 8-20%, acidify t...
Embodiment 1
[0061] Such as figure 1 and figure 2 as shown, figure 1 There are two characteristic absorption peaks in the IR analysis: 1040~1080cm -1 And 1200~1280cm -1 , of which 1050cm -1 The absorption peak at is stronger, and the 1210cm -1 The absorption peak is weak, and the infrared absorption spectrum is at 1058cm -1 The strong characteristic absorption peaks appearing nearby indicate that SO 4 2- It has been supported on the surface of the catalyst, and it can be seen from the above characteristics that the prepared catalyst is a solid superacid. Compared with the catalyst before the reaction, the catalyst was recycled 5 times, at 2928cm -1 、2863cm -1 The absorption vibration peak is the absorption of acetyl tributyl citrate after the reaction, and the appearance of CH 3 and CH 2 The C-H stretching vibration in .
[0062] figure 2 It can be seen that the microstructure of the solid superacid catalyst is loose and fragmented, which increases its specific surface area,...
Embodiment 2
[0086] The difference between embodiment 2 and embodiment 1 is: the preparation method of a kind of solid superacid catalyst of the present invention, comprises the steps:
[0087] In step (1), the preparation of iron-neodymium cross-linking agent: prepare iron solution, neodymium nitrate solution and sodium hydroxide solution; Add the prepared sodium hydroxide solution dropwise to iron solution and neodymium nitrate at a rate of 3ml / min Add distilled water dropwise to the mixed solution to adjust the pH to 8.5, control the temperature to 45°C, stir at a constant temperature for 10 hours, and age at a temperature of 20°C for 35 minutes to obtain an iron-neodymium crosslinking agent; including The following components in parts by volume:
[0088] 16 parts of iron solution,
[0089]17 parts of neodymium nitrate solution,
[0090] 20 parts of sodium hydroxide solution.
[0091] The solute in the iron solution is ferric chloride. The concentration of the iron solution is 0.7mo...
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