Novel catalyst for synthesizing tertiary-butyl substituted benzene phenols and its preparation process

A technology of tert-butyl group and catalyst is applied in the field of a new method for synthesizing tert-butyl substituted phenol and related solid acid catalysts, which can solve problems such as no industrial application results, and achieves convenient product separation and purification, simple process and convenient preparation. Effect

Inactive Publication Date: 2004-11-17
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the above-mentioned related reports, the use time of catalysts is mostly within

Method used

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  • Novel catalyst for synthesizing tertiary-butyl substituted benzene phenols and its preparation process
  • Novel catalyst for synthesizing tertiary-butyl substituted benzene phenols and its preparation process
  • Novel catalyst for synthesizing tertiary-butyl substituted benzene phenols and its preparation process

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0022] Example 1:

[0023] Take 0.1 kg of sodium-type MFI microporous structure crystalline aluminosilicate (SiO 2 / Al2 O 3 = 55) calcined at 1123K for 3 hours and cooled down, with 4.0×10 -4 m 3 Concentration is 1.0×10 2 mol / m 3 mixed with the same hydrochloric acid solution, stirred for 1h at 368K, filtered after cooling, washed the solid with distilled water until no chloride ion was detected in the filtrate, took the same hydrochloric acid solution and mixed with the solid, repeated the above operation for a total of 4 times, the obtained solid was dried at 823K After calcination for 4 hours, a catalyst carrier HMFI with a residual sodium content of 0.2% was obtained.

[0024] Take the above catalyst carrier HMFI 5g, 3.54×10 -4 kg Al(NO 3 ) 3 ·9H 2 O dissolves in 4.0×10 -6 m 3 Distilled water was immersed at room temperature, dried at 393K for 2 hours, and calcined at 823K for 3 hours to obtain Al 2 O 3 1.0% catalyst Al-MFI(1.0).

Example Embodiment

[0025] Example 2:

[0026] Take the catalyst Al-MFI (1.0) prepared according to the method of Example 1 and press it into tablets, pulverize it into 20-30 mesh, and take 1 g of it and put it into a fixed-bed continuous flow reaction device. The molar ratio of phenol to isobutylene is 1:1.2, and the weight hourly space velocity is 2.5h -1 Introduce the pre-device to preheat at 393K, and then flow through the catalyst Al-MFI (1.0) with a bed temperature of 393K. Take the online reaction time of 3 hours for product analysis, and the results are as follows: phenol conversion rate 37.2%; phenol alkylation In the product, the selectivity of o-TBP was 19.2%, the selectivity of p-TBP was 57.8%, and the selectivity of 2,4-DTBP was 23.0%.

Example Embodiment

[0027] Example 3:

[0028] Take 0.2kg sodium-type BEA microporous structure crystalline aluminosilicate (SiO 2 / Al 2 O 3 = 24) after calcining at 1023K for 3 hours and cooling, with 1.0×10 -3 m 3 Concentration is 4.0×10 2 mol / m 3 mixed with the same hydrochloric acid solution, stirred at 363K for 1h, filtered, washed the solid with distilled water until no chloride ion was detected in the filtrate, took the same hydrochloric acid solution and mixed it with the solid, repeated the above operation for a total of 5 times, and the obtained solid was dried and calcined at 823K for 3 hours, the catalyst carrier HBEA-1 with a residual sodium content of 0.05% was obtained.

[0029] Take the above catalyst carrier HBEA-110g, 3.54×10 -4 kg Al(NO 3 ) 3 ·9H 2 O dissolves in 7.5×10 -6 m 3 Distilled water was dipped at room temperature, dried at 393K for 3 hours, and calcined at 823K for 3 hours to obtain Al 2 O 3 0.5% catalyst Al-BEA-1 (0.5).

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Abstract

The invention is a new catalyst for synthesizing tert-butyl to replace phenol and the process, belongs to the synthesizing method for tert-butyl to replace phenol and relative solid acid catalyst, which refers to crystal silicon aluminum acid salt catalyst and the process. the catalyst is made up mainly by micropore aluminosilicate, and loads one to three kinds of elements of boracium, magnesium, aluminum, phosphorus, calcium, titanium, zinc, molybdenum as active components, the process is convenient, the activity and the selectivity are high, can be sued repeatedly; the reaction uses moderate operation condition and continuous flow method, the tert-butyl replaced phenol can be produced by putting phenols and alkylation agent through the catalyst bed; the environment of the process is friendly, the side product is little, the process is simple.

Description

technical field [0001] The invention belongs to the field of a new method for synthesizing tert-butyl-substituted phenol and related solid acid catalysts, and relates to a catalyst based on crystalline aluminosilicate, a preparation method thereof and a process for synthesizing the phenols by catalytic alkylation reaction. The catalyst is mainly composed of microporous crystalline aluminosilicate, which is prepared after physical and chemical treatment; the catalytic alkylation reaction process adopts relatively mild operating conditions and continuous flow mode, and phenols and alkylating reagents Through the catalyst bed, selectively catalyze the reaction of phenols and alkylating reagents to synthesize tert-butyl substituted phenol in one step. technical background [0002] Tert-butyl substituted phenol is an important industrial raw material and organic synthesis intermediate, widely used in synthetic resin, rubber, dye, paint, medicine, pesticide and other industries, w...

Claims

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Application Information

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IPC IPC(8): B01J29/06C07C37/11C07C39/06
CPCY02P20/52
Inventor 唐祥海张爱萍刘杰符新亮
Owner NANKAI UNIV
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