Hydrotalcite-like structuring catalyst and method for catalytic synthesis of pseudo-ionone

A hydrotalcite structure and catalyst technology, applied in the field of membrane catalysis, can solve problems such as increasing mass transfer resistance and unfavorable multiphase contact material diffusion

A hydrotalcite structure and catalyst technology, applied in the field of membrane catalysis, can solve problems such as increasing mass transfer resistance and unfavorable multiphase contact material diffusion

CN101816950AInactive Publication Date: 2010-09-01BEIJING UNIV OF CHEM TECH
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  • Hydrotalcite-like structuring catalyst and method for catalytic synthesis of pseudo-ionone
  • Hydrotalcite-like structuring catalyst and method for catalytic synthesis of pseudo-ionone
  • Hydrotalcite-like structuring catalyst and method for catalytic synthesis of pseudo-ionone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A. Sonicate the sheared aluminum sheet with a purity of 99.999% with acetone for 5 minutes, then use 8% sodium hydroxide solution for 10 minutes to remove the surface oxide layer, clean it with deionized water, and put it in an anodizing device for oxidation. Among them, the aluminum sheet is used as the anode, the lead plate is used as the cathode, the electrolyte is 1mol / L sulfuric acid solution, and the oxidation voltage is 2V / cm 2 Aluminum sheet, after anodizing for 75 minutes, take it out and rinse it with deionized water for later use;

[0023] B. Weigh 4.1024g Mg(NO 3 ) 2 ·6H 2 O and 7.6877g urea were dissolved together in 800ml deionized water, and after stirring evenly with a glass rod, put it into a polytetrafluoroethylene container;

[0024] C. Take the aluminum sheet prepared earlier and take an area of ​​0.4m 2 Place the small piece in the mixed solution in the reaction vessel of step B, seal it well, react at a constant temperature at 90° for 3 days, r...

Embodiment 2

[0029] A. Sonicate the sheared aluminum sheet with a purity of 99.999% with acetone for 8 minutes, then use 5% sodium hydroxide solution for 8 minutes to remove the surface oxide layer, clean it with deionized water, and put it in an anodizing device for oxidation. Among them, the aluminum sheet is used as the anode, the lead plate is used as the cathode, the electrolyte is 1mol / L sulfuric acid solution, and the oxidation voltage is 2V / cm 2 Aluminum sheet, after anodizing for 75 minutes, take it out and rinse it with deionized water for later use;

[0030] B. Weigh 2.0512g Mg(NO 3 ) 2 ·6H 2 O and 3.8439g of urea were dissolved in 400ml of deionized water together, and after stirring evenly with a glass rod, put it into a polytetrafluoroethylene container;

[0031] C. Take the aluminum sheet prepared earlier and take an area of ​​0.4m 2 Place the small piece in the mixed solution in the reaction vessel of step B, seal it well, react at a constant temperature at 90° for 3 da...

Embodiment 3

[0036] A. Sonicate the sheared aluminum sheet with a purity of 99.999% with acetone for 9 minutes, then use 10% sodium hydroxide solution for 6 minutes to remove the surface oxide layer, clean it with deionized water, and put it in an anodizing device for oxidation. Among them, the aluminum sheet is used as the anode, the lead plate is used as the cathode, the electrolyte is 1mol / L sulfuric acid solution, and the oxidation voltage is 2V / cm 2 Aluminum sheet, after anodizing for 75 minutes, take it out and rinse it with deionized water for later use;

[0037] B. Weigh 1.282g Mg(NO 3 ) 2 ·6H 2 O and 2.4025g of urea were dissolved in 500ml of deionized water together, and after stirring evenly with a glass rod, put it into a polytetrafluoroethylene container;

[0038] C. Take the aluminum sheet prepared earlier and take an area of ​​0.4m 2 Place the small piece in the mixed solution in the reaction vessel of step B, seal it well, react at a constant temperature at 90° for 3 da...

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Abstract

The invention discloses a hydrotalcite-like thin membrane which is grown on an aluminum substrate with surface anode oxidation and used as a structuring catalyst in the field of membrane catalysis, so as to catalyze the optimal feed ratio of citral to acetone during the aldol condensation reaction of the citral and the acetone. The in-situ synthesis technology is adopted for preparing the hydrotalcite-like thin membrane on an aluminum sheet after the surface anode oxidation, the high-temperature calcination and the re-hydration are further carried out, and the hydrotalcite-like structuring catalyst which takes aluminum as the substrate is finally obtained. The prepared structuring catalyst can be effectively used for the aldol condensation reaction of the citral and the acetone, solve a series of problems caused by a liquid base catalyst and a solid base catalyst and lead the process to meet the requirements on environmental protection and sustainable development; more importantly, the use of the structuring catalyst can effectively reduce the molar ratio of acetone / citral to 1, thereby obtaining great catalytic effect.

Description

technical field [0001] The invention belongs to the field of membrane catalysis, and specifically relates to the optimal feed ratio of citral and acetone when a hydrotalcite-like film grown on an anodized aluminum substrate is used as a structured catalyst to catalyze the aldol condensation reaction of citral and acetone . Background technique [0002] Pseudoionone is a widely used intermediate in the perfume synthesis industry, and it is also an intermediate in the synthesis of vitamin A and β-carotene in the pharmaceutical industry, so it is necessary to further improve its synthesis process. At present, citral and acetone are used as raw materials in the industry, and the aldol condensation reaction is carried out under the action of an alkali catalyst to generate pseudoionone. [0003] There are two very important factors in this process, one is the choice of catalyst: the catalyst commonly used in the traditional process is a liquid alkali catalyst, such as Ba(OH) 2 S...

Claims

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Application Information

Patent Timeline
01 Sep 2010
Publication
CN101816950A
IPC
B01J27/236; B01J37/34; C07C49/203; C07C45/74
Inventors
张法智; 卢伟