Method for preparing 2,3,6-trimethylphenol by using 2,5-dimethylphenol

A technology of tricresol and xylenol, which is applied in the field of organic compound synthesis, can solve the problems of short service life, low repeatability, and high operating temperature, and achieve the effects of reducing energy and material consumption, reducing equipment costs, and simplifying reaction pathways

Inactive Publication Date: 2010-09-29
台州太祥化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second-generation magnesium oxide catalyst has the characteristics of good activity and high selectivity, but the operating temperature is 400-600 ° C, high energy consumption, easy to form carbon, and short service life, such as USP3446856, USP7972836, USP4041085, USP4201880, USP4554267, CN1066263A
On the one hand, these catalysts have low reproducibility or short service life; on the other hand, there are problems of poor selectivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0021] Weigh 55Kg Fe(NO 3 ) 3 9H 2 O, 880gCr(NO 3 )·9H 2 O, 320gGeCl 4 , 630gMn(NO 3 ) 2 4H 2 O, 730gNa 2 SiO 3 9H 2 O, 3.5KgInCl 3 4H 2 O, dissolved in 1000L of water, first dropwise add 10% ammonia water to neutralize the solution to pH = 7.0, and heat to 90°C, then continue to neutralize with 10% ammonia water to pH = 7.5-8.0, stir for 1 hour, and Precipitate for 12 hours, filter the filter cake, wash and filter it repeatedly with deionized water, dry at 120°C for 24 hours, crush it into 30-80 mesh particles, put it into 20L of 1.0% K 2 CO 3 Immerse in the solution for 24 hours, filter and separate, dry the obtained particles at 120°C for 14 hours, and then bake them in a roasting furnace at 470°C for 5 hours. A catalyst composed of iron, indium oxide, silicon dioxide, chromium oxide, manganese dioxide, germanium oxide and potassium oxide, the molar ratio of each component in the catalyst is:

[0022] Fe 2 o 3 : In 2 o 3 : SiO 2 :Cr 2 o 3 :MnO 2 :GeO ...

example 2

[0026] A preparation method of 2,3,6-tricresol, 2,5-xylenol is gasified with methanol and water, mixed with nitrogen, and carried out in a fixed-bed reactor in the presence of an iron oxide catalyst. Catalytic reaction, one-step synthesis of 2,3,6-tricresol, the reaction temperature is 300 ~ 450 ° C; the reaction pressure is 0 ~ 0.1Mpa; the molar ratio of the 2,5-xylenol, methanol, water, nitrogen is : 1: (2~5): (8~10): (8~12). After the gas-phase catalytic reaction is completed, cool down, separate unreacted methanol and water, and rectify to obtain the finished product of 2,3,6-tricresol. The iron oxide-based catalyst is: mainly iron oxide and contains promoters: chromium oxide, germanium oxide, manganese oxide, indium oxide, silicon oxide, and potassium oxide; the molar ratio of each component in the iron oxide-based catalyst is: Iron: chromium oxide: germanium oxide: manganese oxide: indium oxide: silicon oxide: potassium oxide = 100: 0.5~5: 0.1~6: 0.1~3: 0.1~9: 0.5~3: 0....

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PUM

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Abstract

The invention discloses a method for preparing 2,3,6-trimethylphenol by using 2,5-dimethylphenol. In the method, the 2,5-dimethylphenol, methanol, water and nitrogen in a certain ratio perform a gas phase reaction in a fixed bed reactor in the presence of an iron oxide catalyst so as to synthesize the 2,3,6-trimethylphenol by one step. In the preparation method, the easily obtained 2,5-dimethylphenol is used as a raw material, so that the problem of raw material resource for industrial preparation of the 2,3,6-trimethylphenol is solved; a novel iron oxide catalyst is used so that continuous synthesis time of the 2,3,6-trimethylphenol is prolonged; the conversion rate and the selectivity of the reaction are improved; a material feeding temperature is reduced; and equipment cost is reduced due to the adoption of a fixed adiabatic bed reactor. Therefore, the manufacturing cost of a product is reduced greatly; and the method has very good economic benefits and social benefits.

Description

technical field [0001] The invention relates to the field of synthesis of organic matter, more specifically a method for preparing 2,3,6-tricresol by performing gas-phase catalysis with 2,5-xylenol and methanol under the action of an iron oxide catalyst. Background technique [0002] 2,3,6-Tricresol is used in a wide range of fields. In addition to being synthesized with the main ring of vitamin E, it is also used as a monomer and a raw material for the production of heat-resistant polyphenylene ether engineering plastics and plastic alloys. In addition, it is used in some pesticides and disinfectants. It is also an indispensable intermediate and medium in production and organic chemical reactions. [0003] There are many processes for synthesizing 2,3,6-tricresol, and there are two that are suitable for large-scale industrialization: 1. The synthesis technology commonly used at home and abroad is to use m-cresol as a raw material, methanol as a methylating agent, and in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/10C07C37/16B01J23/889
CPCY02P20/52
Inventor 徐友剑王健随学强杨德校倪夕松罗晓东倪之兴王鹏
Owner 台州太祥化工有限公司
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