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Catalyst for continuously preparing cis-p-tert-butylcyclohexanol, and preparation method and application

A p-tert-butyl catalyst technology, applied in the continuous preparation of cis-p-tert-butyl cyclohexanol catalyst and preparation field, can solve the problems of uneven concentration, long auxiliary operation time, slow mass transfer and heat transfer, etc.

Active Publication Date: 2020-02-04
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the above kettle-type process, the selectivity of cis-to-tert-butylcyclohexanol is improved by adding hydrochloric acid in the reaction system. The hydrochloric acid added in the reaction process will corrode the equipment, increase the difficulty of separation, and increase the cost of acid liquid treatment
In addition, the kettle-type process is intermittently operated, the catalyst is repeatedly applied, the catalyst precious metal is severely worn, the mass transfer and heat transfer are slow during the reaction process, and it is easy to cause reaction temperature, concentration unevenness, low space-time yield, poor stability of batch products, and difficulty in accurate reaction process. Control and safety hazards are great; the obtained products need to be separated and purified, and the auxiliary operation time is long and labor-intensive

Method used

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  • Catalyst for continuously preparing cis-p-tert-butylcyclohexanol, and preparation method and application
  • Catalyst for continuously preparing cis-p-tert-butylcyclohexanol, and preparation method and application
  • Catalyst for continuously preparing cis-p-tert-butylcyclohexanol, and preparation method and application

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Experimental program
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Embodiment 1

[0057] The preparation method of the pretreated catalyst carrier in this embodiment includes acid-treating the porous material carrier to obtain the pretreated carrier, and the porous material carrier is γ-Al 2 o 3 , the acid treatment is pickling treatment, and the pickling treatment comprises:

[0058] γ-Al 2 o 3 Dry at 120°C to constant weight, and dry the γ-Al 2 o 3 Soak in a mineral acid solution with a mass concentration of 10% for 4 hours, filter, wash the filtered retentate with water until the pH is 4, dry the washed retentate at 100°C for 4 hours, and roast the dried retentate at 400°C 3h, to obtain the pretreatment carrier; the inorganic acid solution is a sulfuric acid solution, and the volume of the sulfuric acid solution is γ-Al 2 o 3 6 times the mass, the unit of volume of sulfuric acid solution is mL, γ-Al 2 o 3 The unit of mass is g; γ-Al 2 o 3 The shape is spherical, the γ-Al 2 o 3 The specific surface area is 268.47m 2 / g, particle size 1.5mm, p...

Embodiment 2

[0060] The preparation method of the pretreated catalyst carrier in this embodiment includes acid-treating the porous material carrier to obtain the pretreated carrier, and the porous material carrier is γ-Al 2 o 3 , the acid treatment is pickling treatment, and the pickling treatment comprises:

[0061] γ-Al 2 o 3 Dry at 100°C to constant weight, and dry the γ-Al 2 o 3 Soak in a mineral acid solution with a mass concentration of 5% for 8 hours, filter, wash the filtered retentate to a pH of 3, dry the washed retentate at 70°C for 7 hours, and roast the dried retentate at 500°C 2h, to obtain the pretreatment carrier; the inorganic acid solution is a hydrochloric acid solution, and the volume of the hydrochloric acid solution is γ-Al after drying 2 o 3 3 times the mass, the unit of volume of hydrochloric acid solution is mL, γ-Al 2 o 3 The unit of mass is g; the γ-Al 2 o 3 The shape is sheet-like, the γ-Al 2 o 3 The specific surface area is 319.96m 2 / g, particle s...

Embodiment 3

[0063] The preparation method of the pretreated catalyst carrier in this embodiment includes acid-treating the porous material carrier to obtain the pretreated carrier, and the porous material carrier is γ-Al 2 o 3 , the acid treatment is pickling treatment, and the pickling treatment comprises:

[0064] γ-Al 2 o 3 Dry at 110°C to constant weight, and dry the γ-Al 2 o 3 Soak in a mineral acid solution with a mass concentration of 20% for 2 hours, filter, wash the filtered retentate with water until the pH is 5, dry the washed retentate at 120°C for 2 hours, and roast the dried retentate at 180°C 6h, to obtain the pretreatment carrier; the inorganic acid solution is a nitric acid solution, and the volume of the nitric acid solution is γ-Al 2 o 3 8 times the mass, the unit of volume of nitric acid solution is mL, γ-Al 2 o 3 The unit of mass is g; the γ-Al 2 o 3 The shape is cylindrical, the γ-Al 2 o 3 The specific surface area is 119.85m 2 / g, particle size 2.49mm, ...

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Abstract

The invention discloses a catalyst for continuously preparing cis-p-tert-butylcyclohexanol. The catalyst comprises a porous material carrier, Pd, Ru, a non-metal auxiliary agent component, and a metalauxiliary agent component, wherein a mass percentage of Pd is 0.05%-1%, a mass percentage of Ru is 0.2%-3%, a mass percentage of the non-metal auxiliary agent component is 0.01%-0.5%, a mass percentage of the metal auxiliary agent component is 0.05%-0.8%, the non-metal auxiliary agent component is one or more of P, F and B, and the metal auxiliary agent component is one or more of Mn, Zr, Wu, V,Nb and Ti. In addition, the invention also provides a preparation method and application of the catalyst. The catalyst can significantly improve the selectivity of continuously preparing cis-p-tert-butylcyclohexanol, a molar conversion rate of p-tert-butylphenol exceeds 99.5%, the selectivity of p-tert-butylcyclohexanol exceeds 99%, and the selectivity of cis-p-tert-butylcyclohexanol exceeds 80%.

Description

technical field [0001] The invention belongs to the technical field of chemical product preparation, and in particular relates to a catalyst for continuously preparing cis-p-tert-butylcyclohexanol, a preparation method and an application. Background technique [0002] 4-tert-butylcyclohexanol is an important intermediate for fragrances, medicines and pesticides. Among them, the most widely used is its cis (cis) isomer, which is mainly used as a raw material for fragrances to produce high-grade spices such as soaps and shampoos. p-tert-butylcyclohexyl ester. In the current industrial production, the corresponding alcohol can be prepared by direct hydrogenation of p-tert-butylphenol, but the content of trans isomer in the mixture of cis and trans isomers in the product is high, which affects the fragrance of subsequent products. At present, the catalysts for the hydrogenation of p-tert-butylphenol to prepare cis-p-tert-butylcyclohexanol include Pd / C, Pt / C, and Pd / Al 2 o 3 ,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/656B01J23/648B01J27/16B01J23/46B01J27/12B01J23/652B01J29/00C07C29/20C07C35/08
CPCB01J23/6562B01J23/6482B01J23/6484B01J27/16B01J23/462B01J27/12B01J23/6527B01J29/00C07C29/20C07C35/08C07C2601/14C07B2200/09
Inventor 万克柔高明明程杰林涛张力张炳亮赵茁然
Owner XIAN CATALYST NEW MATERIALS CO LTD
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