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A kind of novel green solid superacid catalyst and application thereof for self-condensation reaction of cyclohexanone

A technology of solid super acid and cyclohexanone, applied in the field of catalysis, can solve the problems of difficult disposal of waste liquid, low dimer yield and increased reaction yield, etc.

Inactive Publication Date: 2017-03-01
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0026] The present invention aims at problems such as low conversion rate of cyclohexanone, low yield of dimer, difficult treatment of waste liquid in production, etc., and proposes a SO 4 2- ·xLa 3+ ·yCe 3+ / zZrO 2 Catalyst, by adding the solid superacid catalyst in the reaction system, to increase the activity of the reaction, reduce side reactions, and increase the yield of the reaction

Method used

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  • A kind of novel green solid superacid catalyst and application thereof for self-condensation reaction of cyclohexanone
  • A kind of novel green solid superacid catalyst and application thereof for self-condensation reaction of cyclohexanone
  • A kind of novel green solid superacid catalyst and application thereof for self-condensation reaction of cyclohexanone

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Embodiment 1

[0033] Embodiment 1: first 1gLa (NO 3 ) 3 ·6H 2 O, 1gCe (NO 3 ) 3 ·6H2 O, 100g (NH 4 ) 2 SO 4 Dissolve in distilled water, then put 10g nanometer ZrO 2 , impregnated at 20°C for 36h, dried to anhydrous, and calcined at 550°C for 5h to obtain the catalyst SO 4 2- ·xLa 3+ ·yCe 3+ / zZrO 2 . Add 1.3L of cyclohexanone into a 2L reaction flask, add the prepared catalyst to be 5% of the quality of cyclohexanone, react at 160°C for 2.5h, analyze the reaction solution by gas chromatography to obtain a conversion rate of cyclohexanone of 85%, Dimer selectivity was 96.5%.

Embodiment 2

[0034] Embodiment 2: earlier 2gLa (NO 3 ) 3 ·6H 2 O, 2gCe (NO 3 ) 3 ·6H 2 O, 100g (NH 4 ) 2 SO 4 Dissolve in distilled water, then put 25g nanometer ZrO 2 , impregnated at 20°C for 36h, dried to anhydrous, and calcined at 550°C for 5h to obtain the catalyst SO 4 2- ·xLa 3+ ·yCe 3+ / zZrO 2 . Add 1.3L cyclohexanone into a 2L reaction flask, add the prepared catalyst to be 5% of the quality of cyclohexanone, react at 160°C for 2.5h, analyze the reaction solution by gas chromatography, and obtain a conversion rate of cyclohexanone of 93.2%. Dimer selectivity was 97.1%.

Embodiment 3

[0035] Embodiment 3: first with 5gLa (NO 3 ) 3 ·6H 2 O, 5gCe (NO 3 ) 3 ·6H 2 O, 100g (NH 4 ) 2 SO 4 Dissolve in distilled water, then put 100g nano ZrO 2 , impregnated at 20°C for 36h, dried to anhydrous, and calcined at 550°C for 5h to obtain the catalyst SO 4 2- ·xLa 3+ ·yCe 3+ / zZrO 2 . Add 1.3L cyclohexanone into a 2L reaction flask, add the prepared catalyst to be 5% of the quality of cyclohexanone, react at 160°C for 2.5h, analyze the reaction solution by gas chromatography to obtain a conversion rate of cyclohexanone of 98.3%, Dimer selectivity was 98.7%.

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Abstract

The invention discloses a novel green solid super acidic catalyst for cyclohexanone self-condensing reaction and an application thereof. The catalyst is applied to the reaction for generating two resonant isomers A2 and A3 through cyclohexanone self-condensation, wherein A2 and A3 are 2-(1-cyclohexenyl) cyclohexanone and 2-hexamethylene alkylene cyclohexanone respectively, belonging to the technical field of catalysis. An impregnation method is adopted to prepare the catalyst and comprises the steps of dissolving La(NO3)3.6H2O, Ce(NO3)3.6H2O and (NH4)2SO4 in distilled water, then placing the required nano ZrO2, impregnating, drying until being anhydrous, and calcining to obtain SO4<2->xLa<3+>yCe<3+> / zZrO2. The catalyst is applied to the cyclohexanone self-condensation reaction, the reaction temperature is 130-170 DEG C, the using amount of the catalyst SO4<2->xLa<3+>yCe<3+> / zZrO2 is 1-10%, the reaction time is 1-3h, the conversion rate of the cyclohexanone can reach more than 80%, and the biopolymer selectivity can reach more than 95%.

Description

technical field [0001] The invention introduces a preparation method and application of a novel green solid superacid catalyst used in the cyclohexanone self-condensation reaction. The catalyst is used in the cyclohexanone condensation reaction and belongs to the technical field of catalysis. [0002] technical background [0003] 2-(1-Cyclohexenyl)cyclohexanone and its resonance isomers are important intermediates for the two-step synthesis of o-phenylphenol. O-phenylphenol is an important fine chemical intermediate in industry and has been widely used in the chemical industry. With the rapid development of economy, the amount of o-phenylphenol is also increasing. In view of the important use of o-phenylphenol and the problems existing in the current production, research and development of a new environmentally safe o-phenylphenol production process has become a top priority. It is also very important to continue to carry out in-depth work in this area and strive for early i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/053C07C49/653C07C45/74
Inventor 孙国新程沙沙崔玉
Owner UNIV OF JINAN
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