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Catalyst for synthesizing 2,3,6-trimethylphenol from m-cresol and preparation method thereof

A technology of trimethylphenol and m-cresol is applied in the field of catalysts and their preparation, which can solve the problems of high cost of iron-based composite oxide catalysts, toxic metals and the like, and achieve the effects of high selectivity, low cost and simple preparation method.

Inactive Publication Date: 2020-07-17
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of high cost of iron-based composite oxide catalysts and the use of toxic metals in the preparation process of the above-mentioned 2,3,6-trimethylphenol, and provide a cheap, environmentally friendly, high-activity and high-selectivity catalyst Catalyst for synthesizing 2,3,6-trimethylphenol from m-cresol and preparation method thereof

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 36.36g Fe(NO 3 ) 3 9H 2 O was dissolved in 150g of deionized water at a temperature of 60°C, and then 0.639g of Na 2 SiO 3 9H 2 O and 0.109g Cu(NO 3 ) 2 ·3H 2 O, after it dissolves, add 25 g of 25% ammonia solution to the solution, keep the temperature at 60° C., and continue to stir for 1 h to age it. After cooling to room temperature, suction filtration was performed, and the filter cake was dried at 100°C for 12 hours. The dried solid was calcined at 550°C for 5 hours to obtain the catalyst. The molar ratio of each component of the catalyst is Fe 2 o 3 : SiO 2 :CuO=100:5:1. The specific surface area of ​​the catalyst determined by the low-temperature nitrogen adsorption-desorption method is 53m 2 / g, the pore volume is 0.180cm 3 / g.

[0017] The prepared catalyst (20-40) mesh is packed in a fixed-bed reactor with an internal diameter of 8 mm, and the catalyst loading is 3.5 ml. m-cresol, methanol and water are mixed in a molar ratio of 1:5:1.5, and inj...

Embodiment 2

[0019] 36.36g Fe(NO 3 ) 3 9H 2 O was dissolved in 150g of deionized water at a temperature of 40°C, and then 1.279g of Na 2 SiO 3 9H 2 O and 0.545g Cu(NO 3 ) 2 ·3H 2 O, after it dissolves, add 20.3 g of 25% ammonia solution to the solution, keep the temperature at 40° C., continue to stir for 3 h to age it. After cooling to room temperature, suction filtration was performed, and the filter cake was dried at 100°C for 12 hours. The dried solid was calcined at 500°C for 5 hours to obtain the catalyst. The molar ratio of each component of the catalyst is Fe 2 o 3 : SiO 2 :CuO=100:10:5. The specific surface area of ​​the catalyst is 54m 2 / g, the pore volume is 0.183cm 3 / g.

[0020] The prepared catalyst (20-40) mesh is packed in a fixed-bed reactor with an inner diameter of 8mm, and the catalyst loading amount is 3.5ml. m-cresol, methanol and water are mixed in a molar ratio of 1:4:1, and injected via microinjection. Pump into the reactor, at normal pressure, 320...

Embodiment 3

[0022] 36.36g Fe(NO 3 ) 3 9H 2 O was dissolved in 150g of deionized water at a temperature of 60°C, and 1.023g of Na 2 SiO 3 9H 2 O and 0.0545g Cu(NO 3 ) 2 ·3H 2 O, after it dissolves, add 27.5 g of 25% ammonia solution to the solution, keep the temperature at 60° C., and continue stirring for 5 h to age it. After cooling to room temperature, filter with suction, and dry the filter cake at 100°C for 12 hours. The dried solid was calcined at 600°C for 3 hours to obtain the catalyst. The molar ratio of each component of the catalyst is Fe 2 o 3 : SiO 2 :CuO=100:8:0.5. The specific surface area of ​​the catalyst is 50m 2 / g, the pore volume is 0.170cm 3 / g.

[0023]The prepared catalyst (20-40) mesh is packed in a fixed-bed reactor with an inner diameter of 8mm, and the catalyst loading amount is 3.5ml. m-cresol, methanol and water are mixed in a molar ratio of 1:7:2, and injected via microinjection Pump into the reactor, at normal pressure, 360°C and liquid hourl...

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Abstract

A catalyst for synthesizing 2,3,6-trimethylphenol from m-cresol and a preparation method thereof, and relates to a catalyst and a preparation method thereof. The composition of the catalyst used to synthesize 2,3,6-trimethylphenol from m-cresol is Fe 2 O 3 ,SiO 2 and CuO. During preparation, Fe(NO 3 ) 3 ·9H 2 Dissolve O in deionized water, then add Na in sequence 2 SiO 3 ·9H 2 O and Cu(NO 3 ) 2 ·3H 2 O, after dissolving, mixture A is obtained; add ammonia water to mixture A, stir and age, then cool to room temperature and filter with suction, dry the filter cake and calcine, to obtain a mixture that can be used to synthesize 2,3,6-trimethyl from m-cresol Phenol catalyst. The catalyst does not contain precious metals and toxic heavy metals, is low-cost, environmentally friendly, has a simple preparation method, good catalytic activity and high selectivity. The conversion rate of m-cresol can reach 100%, and the selectivity of 2,3,6-trimethylphenol can reach up to 100%. 97.9%.

Description

technical field [0001] The invention relates to a catalyst and a preparation method thereof, in particular to a catalyst for synthesizing 2,3,6-trimethylphenol from m-cresol and a preparation method thereof. Background technique [0002] 2,3,6-Trimethylphenol is an important chemical intermediate, mainly used in the synthesis of vitamin E intermediate 2,3,5-trimethylhydroquinone. In addition, 2,3,6-trimethylphenol is also widely used in the production of materials, pesticides, cosmetics, food antioxidants and disinfectants, and the market demand prospect is good. [0003] According to different raw materials, there are three main methods for industrially synthesizing 2,3,6-trimethylphenol: one is to synthesize 2,3,6-trimethylphenol by using phenol and methanol as raw materials, under the action of a catalyst, and using a two-stage synthesis method of gas-solid phase reaction , 3,6-Trimethylphenol, patent CN 102976903B discloses a method of synthesizing 2,3,6-trimethylphenol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/11C07C39/07B01J23/745B01J37/08B01J37/03B01J35/10
CPCC07C37/11B01J23/002B01J23/745B01J37/031B01J37/082B01J37/088B01J2523/00B01J35/613B01J35/633B01J2523/17B01J2523/41B01J2523/842C07C39/07
Inventor 黎四芳邓小玲
Owner XIAMEN UNIV