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Preparation method of catalyst for preparing cyclohexanol from cyclohexene and application of catalyst

A catalyst, cyclohexene technology, applied in catalyst activation/preparation, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of short catalyst service life, complex product recovery, poor thermal stability, etc., achieve high conversion rate, preparation Advanced technology, strong water-oil amphiphilic effect

Inactive Publication Date: 2018-06-29
山东亚科环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction of cyclohexene with water is a typical acid-catalyzed reaction. The liquid acid catalyst (such as sulfuric acid) used in the early stage has defects such as complicated product recovery, easy corrosion, and high energy consumption; in order to overcome the problem of product recovery, ion-exchange resin catalysts have been developed and utilized, but There are still shortcomings such as short service life of the catalyst, poor thermal stability, and easy swelling in organic solvents, and the high price also limits its further application

Method used

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  • Preparation method of catalyst for preparing cyclohexanol from cyclohexene and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 1.0g of WO 3 Soaked in organic acid A for 30min, filtered to obtain acidified solid WO 3 . 1.0 g acidified solid WO 3 , 300.0g polyvinylpyrrolidone (PVP), 500.0g ZSM-5 molecular sieve, mix well, place the mixture in a microwave reactor with a power of 300W, heat it to 250°C under microwave radiation, and obtain a tungsten catalyst carrier W / ZSM- 5.

[0031] Put 10g of W / ZSM-5 catalyst into 100ml of 0.1g / ml triethylchlorosilane-toluene solution, put it in a microwave reactor, and under the action of nitrogen flow, radiate and heat to 55°C, radiate for 15min, and filter , The solid was calcined at 120°C for 3h. The obtained heterogeneous supported catalyst is designated as TECS-W / ZSM-5.

[0032] Add 10g of titanium-loaded TECS-W / ZSM-5 catalyst, 120g of cyclohexene, and 110g of water into a 500ml autoclave, close the autoclave, replace the air with high-purity nitrogen, heat to 120°C, stir, and react for 2h , filtered, the organic phase was analyzed by gas chro...

Embodiment 2

[0034] Weigh 1.0g of WO 3 Soaked in organic acid A for 40min, filtered to obtain acidified solid WO 3 . 1.0 g acidified solid WO 3 , 350.0g polyvinylpyrrolidone (PVP), 550.0g ZSM-5 molecular sieve, mix well, place the mixture in a microwave reactor with a power of 300W, heat it to 250°C under microwave radiation, and obtain a tungsten catalyst carrier W / ZSM- 5.

[0035] Put 10g of W / ZSM-5 catalyst into 50ml of 0.1g / ml hexamethyldisilazane-toluene solution, put it in a microwave reactor, and heat it to 50°C under the action of nitrogen flow, and radiate for 20min , filtered, and the solid was calcined at 110°C for 4h. The obtained heterogeneous supported catalyst is designated as HMDSZ-W / ZSM-5.

[0036] Add 10g of titanium-loaded HMDSZ-W / ZSM-5 catalyst, 120g of cyclohexene, and 100g of water into a 500ml autoclave, close the autoclave, replace the air with high-purity nitrogen, heat to 150°C, stir, and react for 2h , filtered, the organic phase was analyzed by gas chromat...

Embodiment 3

[0038] Weigh 1.0g of WO 3 Soaked in organic acid A for 50min, filtered to obtain acidified solid WO 3 . 1.0 g acidified solid WO 3 , 400.0g polyvinylpyrrolidone (PVP), 500.0gHZSM-5 molecular sieve, mix well, place the mixture in a microwave reactor with a power of 300W, and heat it to 250°C under microwave radiation. After 15min, the supported tungsten catalyst carrier W / HZSM- 5.

[0039] Put 10g of W / ZSM-5 catalyst into 6ml of 1.0g / ml hexamethyldisilazane-toluene solution, put it in a microwave reactor, and heat it to 40°C under the action of nitrogen flow for 15 minutes , filtered, and the solid was calcined at 90°C for 5h. The obtained heterogeneous supported catalyst is designated as HMDSZ-W / HZSM-5.

[0040] Add 10g of titanium-loaded HMDSZ-W / HZSM-5 catalyst, 100g of cyclohexene, and 200g of water into a 500ml autoclave, close the autoclave, replace the air with high-purity nitrogen, heat to 150°C, stir, and react for 2h , filtered, the organic phase was analyzed by ...

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Abstract

The invention discloses a preparation method of a catalyst for preparing cyclohexanol from cyclohexene and application of the catalyst in preparing cyclohexanol from cyclohexene. The catalyst adopts amicrowave radiation method for loading an active ingredient tungsten and a silanization reagent on a molecular sieve ZSM-5. The catalyst provided by the invention has relatively strong water-oil amphipathy, so that reaction activity is improved. Meanwhile, the catalyst prepared by the microwave radiation method has higher mechanical strength and a longer service life. Selectivity of the catalystprovided by the invention for preparing cyclohexanol from cyclohexene hydration reaches 99%. The catalyst is prepared by an advanced process, and has great industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of synthesis of cyclohexanol, in particular to a preparation method and application of a catalyst for preparing cyclohexanol from cyclohexene. Background technique [0002] At present, cyclohexanol is usually prepared from cyclohexene by hydration reaction. The reaction of cyclohexene with water is a typical acid-catalyzed reaction. The liquid acid catalyst (such as sulfuric acid) used in the early stage has defects such as complicated product recovery, easy corrosion, and high energy consumption; in order to overcome the problem of product recovery, ion-exchange resin catalysts have been developed and utilized, but There are still shortcomings such as short service life of the catalyst, poor thermal stability, and easy swelling in organic solvents, and the high price also limits its further application. [0003] Molecular sieve catalyst is a solid acid catalyst widely used in industry at present. It has th...

Claims

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Application Information

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IPC IPC(8): B01J29/48B01J37/34C07C29/04C07C35/08
CPCB01J29/48B01J37/346B01J2229/18B01J2229/32C07C29/04C07C35/08
Inventor 王月昶柳金林张志宏訾文礼闵庆绍
Owner 山东亚科环保科技有限公司
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