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Preparation method and application of dipentene dehydrogenation catalyst

A dehydrogenation catalyst and dipentene technology, applied in the chemical industry, can solve the problems of high equipment requirements, high cost, harsh reaction conditions, etc., and achieve the effect of simple preparation process, easy recovery, and mild reaction conditions

Active Publication Date: 2018-08-17
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the gas phase method has higher requirements on equipment and harsh reaction conditions, and the cost is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Mix distilled water and activated carbon at a ratio of 5 mL / g, boil for 1 hour, wash repeatedly with distilled water until the upper liquid is clear, take out the activated carbon and dry it; mix the dried activated carbon with 25% HNO 3 After the solution was mixed at a ratio of 5mL / g, it was heated to boiling and kept stirring until the HNO 3 The solution was completely volatilized, and the acidified activated carbon was washed with distilled water until the filtrate pH=7, and the obtained activated carbon was dried at 100°C;

[0026] (2) Add 1g RuCl 3 ·3H 2 O and 15 mL of absolute ethanol were placed in a three-necked flask and heated at 70 °C until RuCl 3 ·3H 2 O is completely dissolved, slowly drop 1,5-cyclooctadiene into rhodium trichloride ethanol solution, and continue to heat and reflux at 70°C for 4 hours to generate an orange crystal product, which is washed with absolute ethanol, and the washed crystal is put into Into drying oven, wherein the mol ra...

Embodiment 2

[0030] (1) Mix activated carbon and distilled water at a ratio of 3mL / g and boil for 1.5h, wash repeatedly with distilled water until the upper liquid is clear and dry; mix the dried activated carbon with 30% HNO 3 After the solution was mixed at a ratio of 4mL / g, it was heated to boiling and kept stirring until the HNO 3 The solution was completely volatilized, and the acidified activated carbon was washed with distilled water until the filtrate pH=7, and the obtained activated carbon was dried at 100°C;

[0031] (2) Add 1g RuCl 3 ·3H2 O and 18 mL of absolute ethanol were placed in a three-necked flask, and heated to RuCl at 80°C 3 ·3H 2 O is completely dissolved, slowly drop 1,5-cyclooctadiene into rhodium trichloride ethanol solution, continue to heat and reflux at 80°C for 2 hours, and produce an orange crystal product, wash the obtained product with absolute ethanol, and put the filtered crystal into Into drying oven, wherein the mol ratio of 1,5-cyclooctadiene and rho...

Embodiment 3

[0035] (1) Mix activated carbon and distilled water at a ratio of 4 mL / g and boil for 2 hours, then wash repeatedly with distilled water until the upper liquid is clear, then take out the activated carbon and dry it; mix the dried activated carbon with 8% HNO 3 After the solution was mixed at a ratio of 3mL / g, it was heated to boiling and kept stirring until the HNO 3 The solution was completely volatilized, and the acidified activated carbon was washed with distilled water until the filtrate pH=7, and the obtained activated carbon was dried at 105°C;

[0036] (2) Add 1g RuCl 3 ·3H 2 O and 20 mL of absolute ethanol were placed in a three-necked flask, and heated at 90 °C to RuCl 3 ·3H 2 O is completely dissolved, slowly drop 1,5-cyclooctadiene into the ethanol solution of rhodium trichloride, continue to heat and reflux at 60°C for 3 hours, and produce an orange crystal product, wash the obtained product with absolute ethanol, and put the filtered crystal into Into drying ...

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PUM

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Abstract

The invention discloses a reparation method and an application of a dipentene dehydrogenation catalyst. The preparation method includes the steps: preparing [Rh(COD)Cl]2 by a co-heat backflow method of RhCl3*3H2O ethanol solution and 1, 5-cyclooctadiene (COD); mixing the [Rh(COD)Cl]2 and functionalized activated carbon; adding methanol solution; ultrasonically treating, filtering and drying mixture to prepare a [Rh(COD)Cl]2 / C catalyst; applying the prepared catalyst into dipentene dehydrogenation reaction to obtain p-cymene with high yield. The method is simple to operate, low in device condition requirement, mild in condition and high in dipentene conversion rate and p-cymene selectivity.

Description

technical field [0001] The invention relates to a preparation method and application of an industrial dipentene dehydrogenation catalyst, which belongs to the field of chemical industry. Background technique [0002] Dipentene is a by-product obtained when turpentine is used as raw material to produce camphor or terpineol. It is mainly composed of a mixture of double bond isomers of monocyclic monoterpenes. The annual output of dipentene is abundant in my country. Dipentene undergoes dehydrogenation reaction A valuable spice intermediate - p-cymene can be obtained. p-Cymene is the first choice material for polymer and fragrance chemistry. It can be directly used to prepare flavors for food and washing. It can also be used as a medicine for antitussive, expectorant, and chronic bronchitis. Phlegm, reducing and controlling the effect of bacterial growth, in addition, the synthesis of polycyclic musk type precious fragrances such as powdery sandalwood musk and tuna musk is also...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C5/367C07C15/02
CPCC07C5/367B01J31/2295B01J2531/0213B01J2531/822C07C15/02
Inventor 蒋丽红丁雨晴王亚明郑燕娥陈廷辉冉索宇贾庆明陕绍云
Owner KUNMING UNIV OF SCI & TECH
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