Phenol ortho-position targeted methylation catalyst as well as preparation method and application thereof

A catalyst and methylation technology, applied in physical/chemical process catalysts, chemical instruments and methods, preparation of organic compounds, etc., to achieve high reactivity, good selectivity, and improved heat resistance

Active Publication Date: 2021-11-02
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the technical problems existing in the existing methylation catalysts, the present invention provides a phenolic ortho-targeted methylation catalyst and a preparation method thereof. The catalyst has high cat

Method used

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  • Phenol ortho-position targeted methylation catalyst as well as preparation method and application thereof
  • Phenol ortho-position targeted methylation catalyst as well as preparation method and application thereof
  • Phenol ortho-position targeted methylation catalyst as well as preparation method and application thereof

Examples

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Example Embodiment

[0054] Example 1

[0055] The preparation method of the phenolic neighboring a targeting methylated catalyst provided in this embodiment includes the following steps:

[0056] 1) 148.6 g of iron sulfate, 1.06 g sodium silicate and 1.5 g of nitrate were dissolved in 250 ml of deionized water, and the pH was adjusted to a solution, and the pH was 8 and continued to stir, and the iron-based precursor A.

[0057] 2) 6.2 g of cobalt chloride and 5.2 g of potassium chromate were dissolved in 100 ml of deionized water, and the pH was adjusted with 12.5% ​​sodium hydroxide to adjust the pH 8 and continuously stirred with 12.5% ​​sodium hydroxide. Crystalline precursor B;

[0058] 3) Chromium cobalt-type precursor B and 7.2GTIO 2 The carrier is added to the iron-based precursor A. After mixing, the rotational speed is 0.10 kR / min, the constant temperature water bath is ultrasound, and the polytetrafluoroethylene liner is transferred to the polytetrafluoride, and the reaction is placed in...

Example Embodiment

[0061] Example 2

[0062] The preparation method of the phenolic neighboring a targeting methylated catalyst provided in this embodiment includes the following steps:

[0063] 1) 148.6 g of iron sulfate, 1.06 g of sodium silicate and 1.5 g of nitrate is dissolved in 250 mL deionized water, and the pH is adjusted to a solution, and the pH is 9 and continuously stirred, and the iron-based precursor A;

[0064] 2) 6.2 g of cobalt chloride and 5.2 g of potassium chromate were dissolved in 100 ml of deionized water, and after completion of a solution, it was completely dissolved, and the pH was adjusted with 12.5% ​​of the potassium hydroxide, and continued to stir, and chromium cobalt. Crystalline precursor B;

[0065] 3) Chromium cobalt-type precursor B and 5.2GTIO 2 The carrier is added to the iron-based precursor A. After mixing, the rotational speed was 0.10 kR / min, and the constant temperature water bath was ultrasound, and the polytetrafluoroethylene liner is transferred to th...

Example Embodiment

[0068] Example 3

[0069]The preparation method of the phenolic neighboring a targeting methylated catalyst provided in this embodiment includes the following steps:

[0070] 1) 150.2 g of nine hydrogen nitrate, 1.06 g of nine hydrated sodium silicate and 1.5 g of hexahydrate copper is dissolved in 250 ml of deionized water, and the pH is 8 and the pH is 8 and continuously stirred, and the iron-based precursor is obtained. A;

[0071] 2) 8.2 g of cobalt nitrate and 7.2 g of potassium chromate were dissolved in 100 ml of deionized water, and the mixture was stirred for 5 min. After completion of it, the pH was adjusted with 25% ammonium hydroxide to be 8 and continued to stir. Glycohoidal cobalt-type precursor B;

[0072] 3) Chromium cobalt-type precursor B and 8.2GTIO 2 The carrier is added to the iron-based precursor A. After mixing, the rotational speed was 0.15 km agharge, the constant temperature water bath was ultrasound, and the polytetrafluoroethylene liner was transferred ...

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Abstract

The invention belongs to the technical field of catalysts, and relates to a phenol ortho-position targeted methylation catalyst and a preparation method and application thereof, and the method comprises the following steps: 1) preparing an iron-based precursor A; preparing a chromium-cobalt crystal form precursor B; 3) preparing a catalyst precursor from the iron-based precursor A, the chromium-cobalt crystal precursor B and a TiO2 carrier; 4) modifying the catalyst precursor by adopting a potassium solution; obtaining a catalyst; and 5) carrying out primary screening, tabletting and multi-stage screening on the catalyst to obtain the phenol ortho-position targeted methylation catalyst. The catalyst provided by the invention has the characteristics of high catalytic activity, outstanding thermal stability, high mechanical strength and sintering resistance, and also has the advantages of cheap and easily available raw materials, environmental protection, long service life and the like; meanwhile, when the catalyst is used as a medium and low temperature coal tar phenolic compound catalyst, the selectivity on ortho-targeted methylation is good, the number of catalyst sites is large, and the conversion rate is high.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and relates to a phenolic ortho-targeted methylation catalyst and a preparation method and application thereof. Background technique [0002] In recent years, my country's coal tar output has basically stabilized at 2500×10 4 About t, of which high-temperature tar accounts for 1000×10 4 Above t, the content of phenol oil is very small, while low-temperature or medium-low temperature tar contains more phenolic oil; the phenolic compounds in medium-low temperature coal tar are mainly low-level phenols (accounting for about 9.8% of the total mass of tar, mainly including phenol, cresol, di Cresol), C 3 ~C 4 Alkylphenols and indenols, etc., phenolic compounds accounted for about 50.33%, of which phenol accounted for about 2.51%, m-cresol about 9.32%, p-cresol about 7.32%, 2,5-xylenol about 2.16% %, 3,5-xylenol accounts for about 1.34%. The existence of phenolic compounds leads to additional co...

Claims

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Application Information

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IPC IPC(8): B01J23/86B01J35/02C07C37/16C07C39/07
CPCB01J35/023B01J23/002B01J23/868C07C37/16B01J2523/00B01J2523/13B01J2523/17B01J2523/41B01J2523/47B01J2523/842C07C39/07
Inventor 李冬田佳勇施俊合徐贤崔楼伟刘杰杜崇鹏朱永红
Owner NORTHWEST UNIV
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