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Catalyst for hydroxylation reaction of phenol and preparation method thereof

A phenol hydroxylation and catalyst technology, applied in the field of chemical engineering, can solve problems such as corrosive environment, many by-products, and many production steps, and achieve the effects of good pore order, mild reaction conditions and high reaction activity

Inactive Publication Date: 2013-05-08
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Catechol and hydroquinone are important chemical raw materials. The traditional production methods of catechol include o-chlorophenol, o-dichlorobenzene hydrolysis and 1-phenol-2-sulfonate sodium alkali fusion or alkaline hydrolysis. Catechol is obtained; hydroquinone is produced by oxidation of aniline or oxidative acidolysis of p-dicumene. The problems in these processes are many production steps, many by-products, serious corrosion and environmental pollution, and low production capacity
Relatively speaking, this preparation method is relatively simple, but since hexadecylchlorocopper phthalocyanine has no water-soluble groups, phthalocyanine molecules are prone to aggregation, and the phthalocyanine on the surface of the molecular sieve is not easy to remove
[0009] In addition, the above three methods all use microporous molecular sieves. Due to the small aperture, the molecules of phthalocyanine are relatively large, and the molecular space structure of phthalocyanine may be distorted in the pores of microporous molecular sieves; Diffusion speed is slow in smaller pores; the phthalocyanine used does not contain water-soluble groups, and phthalocyanine molecules are easy to aggregate in molecular sieves, and at the same time, it also increases the difficulty of catalyst post-treatment

Method used

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  • Catalyst for hydroxylation reaction of phenol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Dissolve 0.1 g of tetrasulfonate iron phthalocyanine in 10 mL of deionized water, add 3.72 g of CTMAB, fully oscillate and dissolve in ultrasonic waves, and form a micellar solution for later use. Take 12.1g Na 2 SiO 3 9H 2 O was dissolved in 18.1mL deionized water, and the pH of the solution was adjusted to 10.5 with 4.0M sulfuric acid. After stirring at room temperature for 0.5 hours, the above-mentioned micellar solution was slowly poured into the sodium silicate solution with adjusted pH, and after stirring evenly, the Aged at room temperature for 1 hour, then moved into a stainless steel autoclave, and crystallized at 120°C for 24 hours. After cooling, filter with suction and wash with deionized water until the filtrate is colorless. The obtained solid was added to a mixture of 2.5 mL of concentrated hydrochloric acid and 300 mL of absolute ethanol (the concentration of HCl was 0.1 M), and heated to reflux for 6 hours. Then suction filter, wash with deionized w...

Embodiment 2

[0021] The preparation method is the same as Example 1, except that the amount of tetrasulfonate iron phthalocyanine added is 0.5 g. The prepared catalyst detects the metal content therein with an inductively coupled plasma emission spectrometer (ICP), and calculates that the loading capacity of the tetrasulfonic acid base iron phthalocyanine in the catalyst is 1.59 × 10 -5 mol / g.

Embodiment 3

[0023] The preparation method is the same as Example 1, except that the amount of tetrasulfonate iron phthalocyanine added is 0.9 g. The prepared catalyst detects the metal content therein with an inductively coupled plasma emission spectrometer (ICP), and calculates that the loading capacity of the tetrasulfonic acid base iron phthalocyanine in the catalyst is 2.15 × 10 -5 mol / g.

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Abstract

The invention provides a catalyst for hydroxylation reaction of phenol and a preparation method thereof, belonging to the technical field of chemical engineering and relating to phenol hydroxylation co-production catechol and hydroquinone catalyzer as well as a preparation method thereof. The preparation method of the catalyst is characterized by comprising the following steps: adopting a hydrothermal synthesis method, and packaging phthalocyanine containing water-soluble groups in an MCM-41 channel in the form of molecule to prepare an immobilized homogeneous catalyst. The effects and the benefits of the invention are as follows: the preparation process of the catalyst is simple and has good repeatability; the phthalocyanine packaged in the MCM-41 channel exists in the form of molecule; metal ions or ligands without being subject to complexation do not exit in the MCM-41 channel; the phthalocyanine on the outer surface of the MCM-41 channel is easy to be eliminated; and the prepared catalyst has high capacity and good ordered channel. The catalyst has the advantages that the homogeneous catalyst has mild reaction conditions, high reactivity and good selectivity, and heterogeneouscatalyst is easy to be separated from a product and can be used repeatedly.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and relates to a catalyst and a preparation method thereof, in particular to a catalyst for hydroxylation of phenol and co-production of catechol and hydroquinone and a preparation method thereof. Background technique [0002] Catechol and hydroquinone are important chemical raw materials. The traditional production methods of catechol include o-chlorophenol, o-dichlorobenzene hydrolysis and 1-phenol-2-sulfonate sodium alkali fusion or alkaline hydrolysis. Catechol is taken; hydroquinone is produced by oxidation of aniline or oxidative acidolysis of p-dicumene. The problems in these processes are many production steps, many by-products, serious corrosion and environmental pollution, and low production capacity. [0003] The process of using hydrogen peroxide and phenol as raw materials to carry out hydroxylation reaction to co-produce catechol and hydroquinone plays an important role...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/26B01J31/22B01J37/10C07C39/08C07C37/60
CPCY02P20/52
Inventor 王梅严理徐绍平
Owner DALIAN UNIV OF TECH
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