Preparation method for supported solid-acid catalyst for synthesising 2-isonaphthol via one-step hydroxylation of naphthalene

A solid acid catalyst, a naphthalene one-step hydroxyl technology, which is applied in the field of preparation of solid acid catalysts, can solve the problems of difficult separation and recovery of catalysts, difficult continuous production of processes, poor dispersion of active components, etc. low conversion rate

Inactive Publication Date: 2013-04-24
天津市中云慧德科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the one-step hydroxylation of naphthalene to synthesize 2-naphthol, there are mainly acid catalysis and metal oxide catalysis, among which: acid catalysis mainly uses liquid superacid HF as the catalyst, which makes the process have a homogeneous catalytic reaction itself Difficult to overcome shortcomings: poor product selectivity, difficulty in catalyst separation and recovery, serious corrosion of equipment, difficult continuous production of the process
In addition, the acidity of the catalyst is too strong, so that the generated naphthol is further hydroxylated to generate polyhydroxynaphthalene, and the product selectivity is poor
[0006] The metal oxide catalysis method uses solid acid as a catalyst for the hydroxylation reaction. For example, in the literature Yang Huiqiong "Jiangsu Chemical Industry", the study of spinel-type magnesium ferrite as

Method used

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  • Preparation method for supported solid-acid catalyst for synthesising 2-isonaphthol via one-step hydroxylation of naphthalene
  • Preparation method for supported solid-acid catalyst for synthesising 2-isonaphthol via one-step hydroxylation of naphthalene

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0033] Embodiment 1 Catalyst ZrSO4.nH 2 Preparation of O / HY (n=3)

[0034] Accurately weigh 1g of the carrier HY and transfer it to a suction filter bottle, degas and dehydrate under a vacuum of 650mmHg; at the same time, accurately weigh 0.5g of zirconium sulfate, dissolve it in 6ML of deionized water, add a solution volume of 3% surfactant AEO- 9. Configure as impregnating liquid, transfer the impregnating liquid to the funnel integrated with the suction filter bottle, after the catalyst carrier is evacuated for 2 hours, turn on the switch of the funnel, quickly add the prepared impregnating liquid into the carrier, and impregnate the obtained The suspension was stirred for 2 hours, and then shaken by a low-temperature water bath oscillator at 40°C until the water was evaporated to dryness and the powder was cracked. The obtained powder was ground and baked at 110°C for 2 hours to obtain a supported solid acid catalyst ZrSO4.nH 2 O / HY, denoted as CAT-1, its XRD characteriza...

Example Embodiment

[0035] Embodiment 2 Catalyst ZrSO4.mH 2 Preparation of O / HY (m=1)

[0036] Accurately weigh 1g of the carrier HY and transfer it to a suction filter bottle, degas and dehydrate under a vacuum of 650mmHg; at the same time, accurately weigh 0.5g of zirconium sulfate, dissolve it in 6ML of deionized water, add a solution volume of 3% surfactant AEO- 9. Configure as impregnating liquid, transfer the impregnating liquid to the funnel integrated with the suction filter bottle, after the catalyst carrier is evacuated for 2 hours, turn on the switch of the funnel, quickly add the prepared impregnating liquid into the carrier, and impregnate the obtained The suspension was stirred for 2 hours, and then shaken by a low-temperature water bath oscillator at 40°C until the water was evaporated to dryness and the powder was cracked. Grind the obtained powder and dry it at 200°C for 2 hours to obtain a supported solid acid catalyst ZrSO4.mH 2 O / HY, denoted as CAT-2 (m≠n), its XRD characteri...

Example Embodiment

[0037] Embodiment 3 Catalyst CoO-ZrSO4.mH 2 Preparation of O / HY(m=1)

[0038] Accurately weigh 1g of the carrier HY and transfer it to a suction filter bottle, degas and dehydrate under a vacuum of 650mmHg; at the same time, accurately weigh 0.07g of cobalt nitrate and dissolve it in 6ML of deionized water, add 1% of the solution volume Surfactant AEO-9 , configured as an impregnating liquid, and transferred the impregnating liquid to a funnel integrated with the suction filter bottle. After the catalyst carrier was evacuated for 1 hour, the switch of the funnel was turned on, and the prepared impregnating liquid was quickly added to the carrier, and the impregnated The suspension was stirred for 2 hours, then shaken by a low-temperature water bath oscillator at 40°C until the water was evaporated to dryness and the powder was cracked, the obtained powder was ground, and then put in a muffle furnace for calcination at 400°C for 2 hours to prepare a Auxiliary solid acid cataly...

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Abstract

The invention discloses a preparation method for a supported solid-acid catalyst for synthesising 2-isonaphthol via the one-step hydroxylation of naphthalene, belonging to the technical field of supported solid-acid catalysts, wherein via the technical scheme of soaking a supporter in a solution containing an auxiliary constituent precursor in a vacuum condition, vibrating and drying in a low-temperature water bath, and calcining for 1-3 hours at 400-600 DEG C at first, and then soaking the calcined powder in the solution containing an auxiliary constituent precursor in a vacuum condition, vibrating and drying in the low-temperature water bath, and baking in an airflow at 110-300 DEG C, a solid-acid catalyst which is adjustable in surface acidity and high in the dispersibility of active constituents is prepared. With the adoption of the method, the various problems existing in the prior art are effectively solved, the conversion rate of naphthalene and the selectivity of 2-isonaphthol are greatly increased, and good effects are obtained.

Description

technical field [0001] The invention belongs to the technical field of supported solid acid catalysts, is applied to the hydroxylation reaction of polycyclic aromatic hydrocarbons (PAHs), and specifically relates to a preparation method of a solid acid catalyst exclusively used for one-step hydroxylation of naphthalene to synthesize 2-naphthol. Background technique [0002] 2-naphthol, also known as β-naphthol, ethyl naphthol or 2-hydroxynaphthalene, is an important organic chemical raw material and synthetic intermediate. There are more than 130 kinds of dyes and pigments directly synthesized from it, and more than 20 dye intermediates indivual. It is also widely used in medicine, pesticides, rubber additives, spices, leather tanning, textile printing and dyeing additives, and mineral processing agents. [0003] The traditional production techniques of 2-naphthol are: 1. Sulfonated alkali fusion method. The sulfonation alkali fusion method is the main method of industrial...

Claims

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Application Information

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IPC IPC(8): B01J29/08B01J29/14C07C39/14C07C37/60
CPCY02P20/50
Inventor 刘聪张敬畅刘海峰
Owner 天津市中云慧德科技有限公司
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