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2-tertiary-butyl-4-methyl phenol preparation method

A technology of cresol and p-cresol, which is applied in the field of organic chemical synthesis, can solve problems such as catalyst deactivation, and achieve the effects of low reaction temperature, good selectivity and high conversion rate

Inactive Publication Date: 2006-12-13
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

BijuM.Devassy et al. published the paper "Alkylation of p-cresol with tert-butanolcatalyzed by heteropoly acid supported on zirconia catalyst" in "Journal of Molecular Catalysis: A: Chemical" 210 (2004) 125-130, in liquid time and space Speed ​​4h -1 , the maximum conversion rate was 61%, but the selectivity to 2-tert-butyl-4-methylphenol was 81.4%, and the catalyst deactivated faster

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～5

[0019] Step 1 Catalyst preparation

[0020] 10g SiO 2 / Al 2 o 3 Mix mesoporous molecular sieve NaAlMCM-41 of 20, 50, and 100 with 200mL of 1M ammonium nitrate solution, conduct ion exchange at 70-80°C for 2-6 hours, dry, and roast at 550-600°C for 2-6 hours , making SiO 2 / Al 2 o 3

[0021] Mesoporous molecular sieves HAlMCM-41 8.3g, 8.2g and 8.5g of 20, 50 and 100 respectively, SiO 2 / Al 2 o 3 The mesoporous molecular sieves HAlMCM-41 of 20, 50 and 100 are respectively marked as C 1 、C 2 、C 3 .

[0022] Step 2 Preparation of 2-tert-butyl-4-methylphenol

[0023] Get the prepared mesoporous molecular sieve HAlMCM-41 catalyst C of the first step respectively 1 、C 2 、C 3 Packed in three vertically placed stainless steel tubular reactors with a thermocouple sleeve of φ3mm in the middle and a diameter of φ20mm. The filling thickness of mesoporous molecular sieve HAlMCM-41 catalysts C1, C2, and C3 is 20-30mm ;

Embodiment 1

[0025] In the 2nd step, under normal pressure and the temperature of 120 ℃, methyl tert-butyl ether, that is MTBE: the molar ratio of p-cresol is 1: 1 the mixed solution of MTBE and p-cresol is filled with Catalyst C 1 The top of the reactor at 2.1mL·h -1 The liquid hourly space velocity is injected into the packed catalyst C 1 The reactor; under normal pressure and the temperature of 120 ℃, methyl tert-butyl ether, that is, MTBE: the molar ratio of p-cresol is 1:1 MTBE and p-cresol mixture from the catalyst C 2 The top of the reactor at 1.32mL·h -1 The liquid hourly space velocity is injected into the packed catalyst C 2 The reactor; under normal pressure and the temperature of 100 ℃, methyl tert-butyl ether, that is MTBE: the molar ratio of p-cresol is 1:1 MTBE and the mixture of p-cresol is filled with catalyst C 3 The top of the reactor at 1.32mL·h -1 The liquid hourly space velocity is injected into the packed catalyst C 3 of the reactor. The GC quantitative anal...

Embodiment 2

[0027] In the 2nd step, under normal pressure and the temperature of 120 ℃, methyl tert-butyl ether, that is MTBE: the molar ratio of p-cresol is 1.5:1 MTBE and the mixed solution of p-cresol are filled with Catalyst C 1 The top of the reactor at 2.1mL·h -1 The liquid hourly space velocity is injected into the packed catalyst C 1 The reactor; under normal pressure and the temperature of 90 ℃, methyl tert-butyl ether, namely MTBE: the molar ratio of p-cresol is 1.5: 1 MTBE and the mixture of p-cresol are loaded with catalyst C 2 The top of the reactor at 1.02mL·h -1 The liquid hourly space velocity is injected into the packed catalyst C 2The reactor; under normal pressure and the temperature of 120 ℃, methyl tert-butyl ether, that is, MTBE: the molar ratio of p-cresol is 1:1 MTBE and p-cresol mixture from the catalyst C 3 The top of the reactor at 1.02mL·h -1 The liquid hourly space velocity is injected into the packed catalyst C 3 of the reactor. The results of GC qua...

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PUM

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Abstract

The invention provides a process for preparing 2-tert-butyl-methylphenol by using mesoporous molecular sieve HAlMCM-41 as catalyst, which comprises the following two steps, (1) catalyst preparation by using mesoporous molecular sieve NaAlMCM containing 20-100 SiO2 / Al2O3 as raw material to obtain catalyst of mesoporous molecular sieve HAlMCM-41, (2) preparation of 2-tert-butyl-4-methylphenol by using the obtained mesoporous molecular sieve HAlMCM-41 as catalyst, carrying out synthesizing reaction between alkylating agent and p-methylbenzene, wherein the alkylating agent being tert-butanol or methyl tert-butyl ether.

Description

technical field [0001] The present invention relates to a kind of preparation method of 2-tert-butyl-4-methylphenol, to be precise, relate to a kind of method that prepares 2-tert-butyl-4-methylphenol with mesoporous molecular sieve HAlMCM-41 as catalyst, It belongs to the technical field of organic chemical synthesis. Background technique [0002] 2-tert-butyl-4-methylphenol, also known as o-tert-butyl-p-cresol, commonly known as 2,4-phenol, is an organic intermediate and occupies an important position in the field of organic synthesis. It is widely used in the production of surfactants, antioxidants and UV absorbers. It is mainly used to produce 2246, 2246-S high-grade phenolic antioxidants and light stabilizer UV-326, etc. Compared with BHT (antiaging agent 264), high-grade phenolic antioxidants not only have low toxicity and no pollution, but also have good protective properties against aging caused by oxygen and heat and surface cracks caused by su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/06C07C37/14B01J29/06
CPCY02P20/52
Inventor 杨建国于心玉刘彩华梁学正何鸣元
Owner EAST CHINA NORMAL UNIV