Solid base catalyst and preparation process of 4-(2-furyl)-3-buten-2-one

A technology of solid base catalyst and production method, which is applied in the direction of molecular sieve catalyst, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., and can solve the problem of FA yield less than 60%, rapid decline in catalyst activity, Problems such as poor recycling performance, to achieve the effects of improving selectivity and yield, avoiding multiple condensation side reactions, and making the preparation method easy to achieve

Active Publication Date: 2019-04-12
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, the activity of the catalyst decreases rapidly, and the yield of FA is less than 60% after 5 times of application
The main reason is that the contact time of the reactants in the reactor is long, which is easy to cause multiple condensation side reactions, and the water generated during the aldol condensation process is likely to cause poisoning and loss of the active sites of the catalyst, resulting in a rapid decline in catalyst activity and poor recycling performance. good

Method used

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  • Solid base catalyst and preparation process of 4-(2-furyl)-3-buten-2-one
  • Solid base catalyst and preparation process of 4-(2-furyl)-3-buten-2-one
  • Solid base catalyst and preparation process of 4-(2-furyl)-3-buten-2-one

Examples

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Effect test

Embodiment 1

[0044] Preparation of 2% NaOH-0.5% Nb 2 o 5 / anion resin catalyst

[0045] Dissolve 6.07g of niobium oxalate in 500mL of absolute ethanol, and adjust the stirring speed to 100 r / min at 30°C. After the metal salt is completely dissolved, 300g of anion exchange resin (specific surface area 180m 2 / g, average pore diameter 3nm, Dandong Mingzhu Special Resin Co., Ltd.) was slowly added to the above salt solution, ammonia water was added dropwise and the pH of the solution was kept between 8.5 and 9.0, and stirring was continued for 1h. Subsequently, after filtering and washing with deionized water, it was dried in an oven at 80°C for 6 hours to form solid particles.

[0046] Dissolve 6.00g of sodium hydroxide in 500mL of deionized water, and adjust the stirring speed to 100r / min at room temperature. After completely dissolving, slowly add the above-mentioned dried solid particles into the above-mentioned lye, and continue stirring for 1 h. Subsequently, the deionized water wa...

Embodiment 2

[0048] Preparation of 5%KOH-1%TiO 2 / magnesium oxide catalyst

[0049] Dissolve 12.78g of tetrabutyl titanate in 500mL of absolute ethanol, and adjust the stirring speed to 100r / min at 35°C. After the metal salt is completely dissolved, 300g of magnesium oxide (specific surface area 160m 2 / g, average pore diameter 2.5nm, Weifang Haililong Magnesium Industry Co., Ltd.) was slowly added to the above salt solution, ammonia water was added dropwise and the pH of the solution was kept between 8.0 and 8.5, and the stirring was continued for 2h. Subsequently, after filtering and washing with deionized water, it was dried in an oven at 80°C for 6 hours to form solid particles.

[0050] Dissolve 15.00 g of potassium hydroxide in 500 mL of deionized water, and adjust the stirring speed to 100 r / min at room temperature. After completely dissolving, slowly add the above-mentioned dried solid particles into the above-mentioned lye, and continue stirring for 1 h. Subsequently, the deio...

Embodiment 3

[0052] Preparation of 3%CsOH-2%ZrO 2 / Magnesium aluminum hydrotalcite catalyst

[0053] Dissolve 13.79g of zirconium hydrogen phosphate in 500mL of absolute ethanol, and adjust the stirring speed to 100r / min at 35°C. After the metal salt is completely dissolved, 300g magnesium aluminum hydrotalcite (specific surface area 200m 2 / g, with an average pore size of 2nm, Beijing Aili Wensen Chemical Co., Ltd.) was slowly added to the above salt solution, ammonia water was added dropwise and the pH of the solution was kept between 8.5 and 9.0, and stirring was continued for 1h. Subsequently, it was filtered, washed with deionized water, and dried in an oven at 80 °C for 6 h.

[0054] Dissolve 9.00 g of cesium hydroxide in 500 mL of deionized water, and adjust the stirring speed to 100 r / min at room temperature. After completely dissolving, slowly add the above-mentioned dried solid particles into the above-mentioned lye, and continue stirring for 1 h. Subsequently, the deionized...

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Abstract

The invention provides a solid base catalyst and a preparation process for preparing 4-(2-furyl)-3-buten-2-one. The catalyst comprises an alkaline carrier, an activated auxiliary agent and a water-resistant auxiliary agent. The catalyst has the characteristics of easy preparation and low preparation cost. The continuous production process is particularly suitable for condensation of furfural withacetone to prepare 4-(2-furyl)-3-buten-2-one, can effectively inhibit occurrence of multi-condensation side reactions, and has a high product yield. At the same time, the catalyst under the process has the characteristics of high activity, high product selectivity, good water resistance and uneasiness to deactivate.

Description

technical field [0001] The invention belongs to the technical field of comprehensive utilization of biomass furfural, and specifically relates to a catalyst and a production process that are especially suitable for preparing 4-(2-furyl)-3-buten-2-one. Background technique [0002] As a common biomass-based platform compound, furfural can be hydrolyzed to xylose from hemicellulose or pentosan under the action of acid, and then prepared from xylose by cyclodehydration. The production process is simple and easy, and has basically realized industrialization at present, and the main raw materials are agricultural and sideline products such as corncobs. The molecular formula of furfural contains a furan ring and an aldehyde group. The furan ring contains double bonds and is a conjugated system. The hydrogen atom at the α position is affected by the oxygen atom and becomes more active. Such structural characteristics determine that it has a strong Subsequent reactivity, so furfura...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/10B01J23/04B01J29/08B01J31/36B01J35/10C07D307/46
CPCC07D307/46B01J23/04B01J29/084B01J31/36B01J35/1019
Inventor 靳少华王明永胡江林刘运海王磊杨恒东宋延方黎源
Owner WANHUA CHEM GRP CO LTD
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