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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 catalytic activity, outstanding thermal stability, high mechanical strength and anti-sintering ability It also has the advantages of cheap and easy-to-obtain raw materials, green environmental protection, and long service life.

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

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] The preparation method of the phenolic ortho-targeted methylation catalyst provided in this example comprises the following steps:

[0056] 1) Dissolve 148.6g of ferric sulfate, 1.06g of sodium silicate and 1.5g of copper nitrate in 250mL of deionized water to make a solution, adjust the pH to 8 with 12.5% ​​sodium hydroxide and keep stirring to obtain iron-based precursor A.

[0057] 2) Dissolve 6.2g of cobalt chloride hexahydrate and 5.2g of potassium chromate in 100mL of deionized water to form a solution. After it is completely dissolved, adjust the pH to 8 with 12.5% ​​sodium hydroxide and continue stirring to obtain chromium-cobalt Crystalline precursor B;

[0058] 3) The chromium-cobalt crystal precursor B and 7.2gTiO 2 Add the carrier to the iron-based precursor A, stir vigorously at a speed of 0.10Kr / min after mixing, ultrasonically in a constant temperature water bath, transfer to a polytetrafluoroethylene-lined reactor, and place it in an oven at 120°C for 5...

Embodiment 2

[0062] The preparation method of the phenolic ortho-targeted methylation catalyst provided in this example comprises the following steps:

[0063] 1) Dissolve 148.6g of ferric sulfate, 1.06g of sodium silicate and 1.5g of copper nitrate in 250mL of deionized water to make a solution, adjust the pH to 9 with 12.5% ​​potassium hydroxide and keep stirring to obtain iron-based precursor A;

[0064] 2) Dissolve 6.2g of cobalt chloride hexahydrate and 5.2g of potassium chromate in 100mL of deionized water to form a solution. After it is completely dissolved, adjust the pH to 9 with 12.5% ​​potassium hydroxide and continue stirring to obtain chromium-cobalt Crystalline precursor B;

[0065] 3) The chromium-cobalt crystal precursor B and 5.2gTiO 2 The carrier is added to the iron-based precursor A. After mixing, stir vigorously at a speed of 0.10Kr / min, ultrasonically in a constant temperature water bath, transfer to a polytetrafluoroethylene-lined reaction kettle, and place in a 12...

Embodiment 3

[0069]The preparation method of the phenolic ortho-targeted methylation catalyst provided in this example comprises the following steps:

[0070] 1) Dissolve 150.2g ferric nitrate nonahydrate, 1.06g sodium silicate nonahydrate and 1.5g copper nitrate hexahydrate in 250mL deionized water, adjust the pH to 8 with 25% ammonium hydroxide and keep stirring to obtain an iron-based precursor A;

[0071] 2) Dissolve 8.2g of cobalt nitrate hexahydrate and 7.2g of potassium chromate in 100mL of deionized water to form a solution, and keep stirring for 5 minutes. After it is completely dissolved, adjust the pH to 8 with 25% ammonium hydroxide and keep stirring. Obtain chromium-cobalt crystal precursor B;

[0072] 3) The chromium-cobalt crystal precursor B and 8.2gTiO 2 The carrier is added to the iron-based precursor A. After mixing, stir vigorously at a speed of 0.15Kr / min, ultrasonically in a constant temperature water bath, transfer to a polytetrafluoroethylene-lined reaction kettl...

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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
CPCB01J23/002B01J23/868C07C37/16B01J2523/00B01J35/40B01J2523/13B01J2523/17B01J2523/41B01J2523/47B01J2523/842C07C39/07
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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