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Preparation method of shape-selective catalyst for synthesizing p-methyl phenol

A p-alkylphenol and catalyst technology, which is applied in the field of preparation of shape-selective catalysts in the process of synthesizing p-cresol, can solve the problems of reducing the para-position shape selectivity of the catalyst, increasing the selectivity of o-cresol, and achieving low cost , high shape-selective performance, and high catalytic activity

Active Publication Date: 2012-06-13
溧阳常大技术转移中心有限公司
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AI Technical Summary

Problems solved by technology

And the newly produced Lewis acid center will cause the increase of o-cresol selectivity in the product, thereby reducing the para-position shape selectivity of the catalyst. A Problem to be Solved by Shape-Selective Catalysts for Phenol-based Processes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take metal lithium nitrate (3.25g), add (39.8ml) in dehydrated alcohol, wherein the mass ratio of metal nitrate and dehydrated alcohol is 1:10, treat that it dissolves completely and then add complex ligand Tetramethyl Ethylenediamine (16.43g), wherein the mol ratio of complex ligand and lithium ion in lithium nitrate is 3:1, stirs with glass rod, then (4.0g) microporous molecular sieve MCM-22 is added wherein, Make the mass ratio of lithium ions in lithium nitrate to microporous molecular sieves 1:13.3, stir evenly, soak at room temperature for 24 hours, dry in a water bath at 60°C, then transfer to an oven to dry at 120°C for 6 hours, and then put Calcined in a muffle furnace, the temperature was raised to 550 °C at 10 °C / min and kept for 6 h to obtain a shape-selective catalyst with a lithium ion loading of 7.5%. The catalyst was used in the process of alkylation of phenol and dimethyl carbonate to synthesize p-cresol, the molar ratio was phenol:dimethyl carbonate 1:...

Embodiment 2

[0018] Compared with Example 1, the molar ratio of lithium ions in the complex ligand tetramethylethylenediamine and lithium nitrate was changed to 1:1, and the others were the same. The catalyst was used in the process of alkylation of phenol and dimethyl carbonate to synthesize p-cresol, the molar ratio was phenol:dimethyl carbonate 1:1, the reaction temperature was 360 °C, and the mass space velocity of the raw material was 2 h －1 , the conversion rate of phenol reached 82.6%, and the selectivity to p-cresol was 70.1%.

Embodiment 3

[0020] Compared with Example 1, the mass ratio of lithium ions to microporous molecular sieves in lithium nitrate was changed to 1:100, that is, the lithium ion loading was 1%, and the others were the same. The catalyst was used in the process of alkylation of phenol and dimethyl carbonate to synthesize p-cresol, the molar ratio was phenol:dimethyl carbonate 1:1, the reaction temperature was 360 °C, and the mass space velocity of the raw material was 2 h －1 , the conversion rate of phenol reaches 90.7%, and the selectivity to p-cresol is 45.2%.

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Abstract

The invention discloses a preparation method of a shape-selective catalyst for synthesizing p-methyl phenol, relating to the technical field of high performance catalyst in alkylating process. The preparation method comprises the following steps of: weighing metal nitrate, and adding the same in anhydrous alcohol, wherein the mass ratio of the metal nitrate to the anhydrous alcohol is 1:10; adding a complex ligand after the metal nitrate is completely dissolved, wherein the mol ratio of the complex ligand to the metal ions in the metal nitrate is 1:1 to 3:1, uniformly stirring the mixture through a glass bar, adding a micro-porous molecular sieve therein, adjusting the mass ratio of the metal ions in the metal nitrate to the micro-porous molecular sieve to 1:100 to 1:5, uniformly stirring, soaking at the room temperature for 24 h, and drying the mixture at water bath of 60 DEG C, transferring the mixture in an oven, and drying the same at 120 DEG C for 6 h, roasting the mixture in a muffle furnace, and heating up to 550 DEG C at a speed of 10 DEG C per minute to obtain the shape-selective catalyst. The invention has the advantages of simple preparation method, low cost and high shape selection performance, etc.

Description

technical field [0001] The invention relates to the technical field of preparation of a high-performance catalyst in an alkylation process, in particular to a preparation method for a shape-selective catalyst in the synthesis of p-cresol. Background technique [0002] P-cresol is widely used as an important raw material for the production of phenolic resins, rubber anti-aging agents, surfactants, etc., and is also an important intermediate for the production of spices and pesticides. The synthesis methods of p-cresol mainly include natural separation method, methylaniline diazotization hydrolysis method, methylbenzene chlorination hydrolysis method and phenol alkylation method. Among them, the first three methods have been gradually eliminated due to the complex process, serious corrosion in the production process and low product quality. The phenol alkylation method is a hot research topic at present. [0003] The result of the phenol alkylation reaction is often a mixture...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40B01J29/70C07C39/07C07C37/16
CPCY02P20/52
Inventor 薛冰李永昕许杰刘平张卫红
Owner 溧阳常大技术转移中心有限公司
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