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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

AI Technical Summary

Problems solved by technology

In the above-mentioned related reports, the use time of catalysts is mostly within a few hours to one day, and no industrial application results have been seen yet.

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

Embodiment 1

[0023] Get 0.1kg sodium type MFI microporous structure crystalline aluminosilicate (SiO 2 / Al2 o 3 =55) Cooled after 3 hours of roasting at 1123K, and 4.0×10 -4 m 3 The concentration is 1.0×10 2 mol / m 3 Mix the hydrochloric acid solution, stir at 368K for 1h, filter after cooling, wash the solid with distilled water until no chloride ions are detected in the filtrate, and mix the same hydrochloric acid solution with the solid, repeat the above operation for a total of 4 times, and the obtained solid is dried at 823K Calcined for 4 hours, the catalyst carrier HMFI with 0.2% sodium residue was obtained.

[0024] Take the above catalyst carrier HMFI 5g, 3.54×10 -4 kg Al(NO 3 ) 3 9H 2 O soluble in 4.0×10 -6 m 3 impregnated in distilled water at room temperature, dried at 393K for 2 hours, and roasted at 823K for 3 hours to obtain Al 2 o 3 Catalyst Al-MFI (1.0) at a content of 1.0%.

Embodiment 2

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

Embodiment 3

[0028] Get 0.2kg sodium type BEA microporous structure crystalline aluminosilicate (SiO 2 / Al 2 o 3 =24) Cooled after 3 hours of roasting at 1023K, with 1.0×10 -3 m 3 The concentration is 4.0×10 2 mol / m 3 Mix the hydrochloric acid solution, stir at 363K for 1h, filter, wash the solid with distilled water until no chloride ions are detected in the filtrate, and mix the same hydrochloric acid solution with the solid, repeat the above operation for a total of 5 times, and the obtained solid is dried and roasted 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 soluble in 7.5×10 -6 m 3 impregnated in distilled water at room temperature, dried at 393K for 3 hours, and roasted at 823K for 3 hours to obtain Al 2 o 3 Catalyst Al-BEA-1 (0.5) at 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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