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Catalyst for improving para-selectivity of phenol hydroxylation reaction product, preparation method and application thereof

A technology of phenol hydroxylation and reaction product is applied in the field of catalyst preparation for improving the para-selectivity of phenol hydroxylation reaction product, and can solve serious environmental pollution, small production scale, and low yields of catechol and hydroquinone. And other issues

Active Publication Date: 2021-04-23
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

In the traditional process, the yield of catechol and hydroquinone is low, the production scale is small, the environmental pollution is serious, and it has been eliminated abroad

Method used

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  • Catalyst for improving para-selectivity of phenol hydroxylation reaction product, preparation method and application thereof
  • Catalyst for improving para-selectivity of phenol hydroxylation reaction product, preparation method and application thereof
  • Catalyst for improving para-selectivity of phenol hydroxylation reaction product, preparation method and application thereof

Examples

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Effect test

preparation example Construction

[0038] Preparation of Extruded Ti-Si Molecular Sieve Catalyst

[0039] The above molecular sieve mother liquor was centrifuged, dried and calcined at 540° C. for 4 hours to obtain a titanium silicon molecular sieve. Weigh 500g of titanium-silicon molecular sieve, 446g of silica sol (28wt%) and 20g of scallop powder, mix them uniformly, add appropriate amount of deionized water, fully knead and shape in extruder. Place at room temperature for 12h. Then it was dried at 100°C for 12h, and then calcined at 540°C for 3h.

[0040] Preparation of Microspherical Ti-Si Molecular Sieve Catalyst

[0041]Weigh 1000g of titanium-silicon molecular sieve mother liquor, the molecular sieve solid content is 12%, add 250g of silica sol (28wt%), stir for 24h, and adopt spray drying to form. The spray drying molding conditions are: inlet temperature: 200°C, outlet temperature: 110°C. After molding, it is dried at 35-120°C and calcined at 500-600°C to obtain microspherical titanium-silicon mol...

Embodiment 1

[0043] Mix 5.1 g of ferric nitrate with 15 ml of deionized water to obtain an iron-containing impregnation solution. 20 g of the extruded titanium-silicon molecular sieve catalyst was impregnated with the above impregnating solution at room temperature for 12 hours. Dry at 100°C for 12h, and bake at 540°C for 4h. Then 1.1 g of lanthanum nitrate, 0.4 g of diammonium hydrogen phosphate and 15 ml of deionized water were mixed. The above catalyst was placed in the impregnation solution for 12h. Dry at 100°C for 12h, and bake at 540°C for 4h. The catalyst was then immersed in 15 mL of a cyclohexane solution containing 0.3 g of tetraethylorthosilicate. Immerse at room temperature for 6h, dry at 100°C for 12h, and bake at 540°C for 4h. Catalyst A is obtained.

Embodiment 2

[0045] Mix 6.0 g of ferric chloride with 15 ml of deionized water to obtain an iron-containing impregnation solution. 20 g of the extruded titanium-silicon molecular sieve catalyst was impregnated with the above impregnating solution at room temperature for 12 hours. Dry at 100°C for 14h, and bake at 550°C for 4h. Then 1.5 g of lanthanum nitrate, 1.5 g of diammonium hydrogen phosphate and 15 ml of deionized water were mixed. The above catalyst was placed in the impregnation solution for 12h. Dry at 100°C for 16h, and bake at 550°C for 6h. The catalyst was then immersed in 15 mL of a cyclohexane solution containing 0.7 g of tetraethylorthosilicate. Immerse at room temperature for 6h, dry at 100°C for 12h, and bake at 540°C for 4h. Catalyst B is obtained.

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Abstract

The invention provides a catalyst for improving the para-selectivity of a phenol hydroxylation reaction product, a preparation method and an application thereof. The catalyst uses titanium-silicon molecular sieve as a catalyst, and uses silicon oxide or aluminum oxide as a binder to extrude or spray. Supplemented with iron as the first modification component, lanthanum and phosphorus as the second modification component. The catalyst is then silanized to obtain the phenol hydroxylation catalyst. Based on the weight of the catalyst, the content of iron oxide is 0.5% to 10%, the content of auxiliary agent lanthanum oxide is 0.5% to 5%, the content of auxiliary agent phosphorus oxide is 0.5% to 5%, and the content of silicon oxide is 0.5%. ~2%. Catalyst preparation adopts the equal volume impregnation method to load and introduce the active component iron, after drying and roasting, the second modified component lanthanum and phosphorus are loaded by the equal volume impregnation method, after drying and roasting again, the silanization treatment is carried out to obtain the target catalyst. The catalyst provided by the invention has high low-temperature phenol hydroxylation activity, high para-product selectivity and good catalyst stability.

Description

technical field [0001] The invention belongs to the field of preparation method and application of petrochemical catalysts, in particular to a preparation method and application of a catalyst for improving para-selectivity of phenol hydroxylation reaction products. Background technique [0002] Hydroquinone (catechol and hydroquinone) is an important chemical product with an extremely wide range of applications. Catechol is an important pesticide and pharmaceutical intermediate, which can be used to prepare spices, dyes and photosensitive materials. Hydroquinone is mainly used in photographic film developer, anthraquinone dyes, azo dyes, auxiliary solvent for synthetic ammonia desulfurization process, rubber antioxidant, gasoline antioxidant, etc. [0003] The traditional quinone synthesis process basically produces a single catechol or hydroquinone product. Including the production of catechol by chlorination and hydrolysis of phenol, the production of hydroquinone by the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89C07C37/60C07C39/08
CPCB01J29/89B01J2229/18B01J2229/32C07C37/60C07C39/08Y02P20/52
Inventor 黄家辉龙化云吕强贾玉华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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