Nickel-based halloysite nanotube hydrogenation catalyst and preparation and application thereof

A technology of halloysite nanotubes and hydrogenation catalysts, applied in the direction of metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, preparation of organic compounds, etc. volume, non-renewable and other issues

Active Publication Date: 2021-06-08
河南天宁新材料科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

my country is rich in naphthalene resources, and its price has a cost advantage over o-xylene, which dominates the market for raw materials for the production of o-phenylene ring carboxylates. Using protonic acid sulfuric acid as a catalyst for esterification reaction, these two factors will lead to trace sulfur (about 100-200μg / g) in the finished product of naphthalene-based o-phenylene ring carboxylate
This means that when the naphthalene-based o-benzene ring carboxylate is used as raw material to hydrogenate cyclohexane carboxylate, the noble metal catalyst will be poisoned and deactivated and cannot be regenerated.

Method used

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  • Nickel-based halloysite nanotube hydrogenation catalyst and preparation and application thereof
  • Nickel-based halloysite nanotube hydrogenation catalyst and preparation and application thereof
  • Nickel-based halloysite nanotube hydrogenation catalyst and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Adopt the in-situ growth preparation method, dissolve 132.5g of nickel nitrate in 400ml of deionized water as solution A, and put 120g of halloysite powder in 500ml of absolute ethanol, stir and ultrasonically disperse for 5h to prepare uniformly dispersed suspension B . Mix solution A and suspension B, stir evenly to obtain solution C, control the temperature of solution C to 85°C, add urea to slowly hydrolyze it in the solution system, adjust the pH value of the mixed solution to 12, stir for 16 hours, and the stirring speed is 100r / min, during which the active components grow slowly and controllably on the halloysite nanotubes in situ, and the resulting green precipitate undergoes solid-liquid separation. The separated solid was washed five times with deionized water and ethanol in turn to obtain a nickel-based catalyst precursor. Place the precursor in a vacuum drying oven at 110°C for 10 hours, then place it in a muffle furnace, and then heat it up to 500°C for 6...

Embodiment 2

[0046] Dissolve 128.2g of nickel nitrate, 2.6g of cerium nitrate, and 3.8g of praseodymium carbonate in 400ml of deionized water to obtain solution A, and put 138g of halloysite powder in 500ml of absolute ethanol, stir and ultrasonically disperse for 5 hours to prepare a uniformly dispersed Suspension B. Mix solution A and suspension B, stir evenly, control the temperature of the solution at 85°C, add urea to slowly hydrolyze it in the solution system, adjust the pH value of the mixed solution to 12, stir for 16 hours, and the stirring speed is 100r / min. The active components grow slowly and controllably on the halloysite nanotubes in situ, and the resulting green precipitate undergoes solid-liquid separation. The separated solid was washed alternately with deionized water and ethanol five times each to obtain a nickel-based catalyst precursor. Place the precursor in a vacuum drying oven at 110°C for 10 hours, then place it in a muffle furnace, and then heat it up to 500°C f...

Embodiment 3

[0048] Dissolve 138.5g of nickel nitrate and 5.5g of cerium carbonate in 400ml of deionized water to form solution A, and put 126.1g of halloysite powder in 500ml of absolute ethanol, stir and ultrasonically disperse for 5h, and prepare uniformly dispersed suspension B . Mix solution A and suspension B, stir evenly, slowly (80-100ml / h) add ammonia water to adjust the pH value of the mixed solution to 12, stir for 16h, and separate the solid-liquid of the obtained green precipitate. The separated solid was washed five times with deionized water and ethanol alternately to obtain a nickel-based catalyst precursor. Place the precursor in a vacuum drying oven at 110°C for 10 hours, then place it in a muffle furnace, and then heat it up to 500°C for 6 hours in a nitrogen atmosphere at a rate of 10°C / min to obtain a nickel-based halloysite nanotube hydrogenation catalyst. .

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Abstract

The invention belongs to the field of cyclohexane carboxylate preparation, and particularly relates to a nickel-based halloysite nanotube hydrogenation catalyst and preparation and application thereof. According to the nickel-based halloysite nanotube hydrogenation catalyst, a halloysite nanotube serves as a carrier, an active component is loaded on the halloysite nanotube in an in-situ growth mode, and the active component is nickel or a combination of nickel and one or more of the following metal elements: Cu, W, Ce, Al, Pr, Y and B. The nickel-based halloysite nanotube hydrogenation catalyst provided by the invention has high activity and good selectivity, is suitable for hydrogenation production with naphthalene orthophthalic acid esters as raw materials, has a great cost advantage of the catalyst per unit product, and can also realize a very high raw material conversion rate after being repeatedly used for many times. Besides, according to the production process provided by the invention, the orthophthalic acid ester raw material in the final finished product is reduced to the ppm level, the refining cost of the product is greatly reduced, and the production process has a remarkable market cost advantage.

Description

technical field [0001] The invention belongs to the field of cyclohexane carboxylate preparation, in particular to a nickel-based halloysite nanotube hydrogenation catalyst and its preparation and application. Background technique [0002] In recent years, scientific research has found that o-benzene ring carboxylate plasticizers harm male reproductive ability and promote female sexual precocity, especially potentially harmful to infants. In December 2018, the European Commission promulgated Regulation 2018 / 2015, Article 51 of REACH Annex XVII related to phthalates, for 4 kinds of phthalates (DEHP, DBP, DIBP and BBP) The limit is increased from less than 0.1% for each item to less than 0.1% for the sum of all items, and the product range is expanded from toys that are placed in the mouth under the age of 3 to all toys and child care products under the age of 12; and it is clearly stipulated that in July 2020 After 7 days, if the limit values ​​of 4 phthalates (DEHP, DBP, DI...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/83C07C67/303C07C69/753
CPCB01J23/755B01J23/83C07C67/303C07C69/753Y02P20/52
Inventor 刘国际姚宁李小聪李俊华徐丽
Owner 河南天宁新材料科技有限公司
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