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Catalyst for preparing bridged tetrahydrodicyclopentadiene, preparation method and application

A technology of tetrahydrodicyclopentadiene and dicyclopentadiene is applied in the field of preparation of diene hydrogenation catalysts, which can solve the problems that the selectivity and stability need to be improved and the reaction temperature is high, and achieve the elimination of nickel-aluminum spinel. Tendency, high reduction degree, good effect of low temperature hydrogenation activity

Active Publication Date: 2021-07-27
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] It can be seen that the supported nickel-based catalyst still has the problems of high reaction temperature, selectivity and stability in the process of diene hydrogenation reaction.

Method used

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  • Catalyst for preparing bridged tetrahydrodicyclopentadiene, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh an appropriate amount of γ-Al 2 o 3 The carrier was subjected to vacuum treatment at 100° C. for 2 hours, and then cooled to room temperature for use. Weigh 0.01gLiNO 3 Add 10ml of deionized water, impregnate 10.0g of carrier after vacuum treatment, dry in the shade naturally, dry at 120°C for 12 hours, and bake at 400°C for 6 hours.

[0031] Weigh 12.72g Ni(NO 3 ) 2 ·6H 2 O and 0.472g (NH 4 ) 6 Mo 7 o 24 4H 2 Add O and 0.22g ethylene glycol to 30ml deionized water, mix well and impregnate the modified γ-Al 2 o 3 The carrier was dried naturally in the shade, dried at 120°C for 12 hours, reduced at 400°C for 6 hours in a hydrogen atmosphere, and cooled to room temperature, in 0.5% O 2 / N 2 Passivation in the atmosphere for 3 hours, the prepared catalyst is 20%Ni-2%Mo-0.1%Li / γ-Al 2 o 3 .

Embodiment 2

[0033] Adopt the γ-Al of vacuum pretreatment in embodiment 1 2 o 3 carrier.

[0034] Weigh 0.156gCa(NO 3 ) 2 4H 2 O Add 10ml of deionized water, impregnate into 10.0g of vacuum-treated carrier, dry in the shade naturally, dry at 120°C for 12 hours, and bake at 400°C for 6 hours.

[0035] Weigh 13.07g Ni(NO 3 ) 2 ·6H 2 O and 0.971g (NH 4 ) 6 Mo 7 o 24 4H 2 Add O and 0.22g ethylene glycol to 30ml deionized water, mix well and impregnate the modified γ-Al 2 o 3 The carrier was dried naturally in the shade, dried at 120°C for 12 hours, reduced at 400°C for 6 hours in a hydrogen atmosphere, and cooled to room temperature, in 0.5% O 2 / N 2 Passivation in the atmosphere for 3 hours, the prepared catalyst is 20%Ni-4%Mo-0.2%Ca / γ-Al 2 o 3 .

Embodiment 3

[0037] Adopt the γ-Al of vacuum pretreatment in embodiment 1 2 o 3 carrier.

[0038] Weigh 0.189g KNO 3 Add 10ml of deionized water, impregnate into 10.0g of vacuum-treated carrier, dry in the shade naturally, dry at 120°C for 12 hours, and bake at 400°C for 6 hours.

[0039] Weigh 18.08g Ni(NO 3 ) 2 ·6H 2 O and 1.612g (NH 4 ) 6 Mo 7 o 24 4H 2 Add O and 0.22g ethylene glycol to 30ml deionized water, mix well and impregnate the modified γ-Al 2 o 3 The carrier was dried naturally in the shade, dried at 120°C for 12 hours, reduced at 400°C for 6 hours in a hydrogen atmosphere, and cooled to room temperature, in 0.5% O 2 / N 2 Passivation in the atmosphere for 3 hours, the prepared catalyst is 25%Ni-6%Mo-0.5%K / γ-Al 2 o 3 .

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Abstract

The invention relates to a catalyst and a preparation method for preparing bridged tetrahydrodicyclopentadiene. The catalyst is composed of a carrier, an active metal, a metal assistant and a carrier promoter. The carrier is alumina, the active component is metal Ni, the metal additive is one of Mo and W, and the carrier promoter is one or more of alkaline earth oxide, alkali metal oxide and rare earth oxide. The mass fraction of the active metal in the catalyst is 5-30%, the mass fraction of the metal additive in the catalyst is 1-10%, the mass fraction of the carrier accelerator in the catalyst is 0.01-1%, and the balance is the carrier. The supported catalyst is used in the reaction of dicyclopentadiene hydrogenation to prepare bridged tetrahydrodicyclopentadiene. It has high hydrogenation activity and selectivity at relatively low temperature and pressure, and has good stability. Continuous production is realized, which is suitable for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of preparation of diene hydrogenation catalysts, in particular to a catalyst and a preparation method for preparing bridged tetrahydrodicyclopentadiene by catalytic hydrogenation of dicyclopentadiene. Background technique [0002] Dicyclopentadiene (DCPD) is a by-product of ethylene cracking C 5 The main component of the distillate, with the rapid development of my country's petroleum and chemical industries, especially the rapid increase in ethylene production capacity, the source of DCPD will be more abundant. DCPD is an important chemical raw material. Due to its unique structure and high reactivity, DCPD has been widely used in the fields of medicine, pesticides, rubber, leather, synthetic fragrances, and unsaturated resins. In recent years, in the field of new polymer materials and fine chemicals, the application of DCPD has attracted people's attention. Among them, DCPD can prepare a bridged tetrahydr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/887B01J23/888C07C5/03C07C13/61
CPCB01J23/8871B01J23/8872B01J23/888B01J37/0203B01J37/18C07C5/03C07C2521/10C07C2523/02C07C2523/04C07C2523/10C07C2523/28C07C2523/30C07C2523/755C07C2523/887C07C2523/888C07C13/61
Inventor 王涛丁云杰董文达卢巍马立新
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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