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

A technology of trimethylphenol and catalyst, applied in the field of solid catalyst, can solve the problems of high price, short service life of catalyst, use of toxic metals, etc., and achieve the effects of improving purity, avoiding waste and improving production efficiency

Inactive Publication Date: 2014-08-13
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Technical problem: the purpose of the present invention is to solve the problems of short service life of the catalyst, high price and use of toxic metals in the production of 2,3,6-trimethylphenol, and provides a preparation for the synthesis of 2,3,6-trimethylphenol The catalyst method of methyl phenol can prepare a cheap and environment-friendly catalyst, the catalyst has high activity, high selectivity to 2,3,6-trimethylphenol, and the service life can reach more than 3000h

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) Accurately weigh Fe(NO 3 ) 3 9H 2 O20g, FeCl 3 10g, Al(NO 3 ) 3 9H 2 O0.1g, AlCl 3 0.16g, Al(OAC) 3 0.22g and Na 2 SO 4 9H 2 0.06g, it was dissolved in 350ml of deionized water, and then at room temperature and under stirring conditions, slowly dropwise add ammonia solution with a concentration of 1:1 to pH=6, the time for adding was about 1h, and continue to stir for 2h at room temperature age it;

[0025] 2) Then the precipitate was suction filtered and washed three times, baked in an oven at 110°C for 24 hours to remove the moisture, and finally calcined in a muffle furnace at 500°C for 5 hours to obtain a block solid;

[0026] 3) Grind the obtained massive solids to 10-80 meshes, and impregnate the ground particles in a solution containing 0.014g Na 2 CO 3 7mL of deionized aqueous solution, soaked for 24h, then dried the impregnated solid particles at 110°C, and calcined at 500°C for 3h. Catalyst Fe 2 o 3 -SiO 2 -Al 2 o 3 -K 2 O, wherein the r...

Embodiment 2

[0028]1) Accurately weigh Fe(NO 3 ) 2 20g, Fe(C 2 h 4 )15g, FeSO 4 10g, Al(NO 3 ) 3 9H 2 O1.0g, AlCl 3 1.20g and Na 2 SO 4 9H 2 O6.99g, it is dissolved in the deionized water of 350ml, then at room temperature, under stirring condition, slowly add dropwise the molar ratio is sodium hydroxide: ammoniacal liquor=1:1, and the total mass concentration is the solution of 30% to pH=7 , continue to stir at room temperature for 2h to age it;

[0029] 2) Then the precipitate was suction filtered and washed three times, baked at 110°C for 24 hours, and calcined at 500°C for 5 hours to obtain a massive solid;

[0030] 3) Grind the obtained massive solid to 10-80 mesh, and impregnate the ground particles in a solution containing 1.10g Na 2 CO 3 , 0.41g KOH in 8mL of deionized aqueous solution, impregnated for 24h, then dried at 110°C, and calcined at 500°C for 3h to obtain the catalyst FeO-SiO 2 -Al 2 o 3 -K 2 O, wherein the ratio of iron oxide, silicon dioxide, aluminum ...

Embodiment 3

[0032] 1) Accurately weigh Fe(NO 3 ) 3 9H 2 O15g, Fe 2 (SO 4 ) 3 10g, Fe(NO 3 ) 2 12g, FeSO 4 10gAl(NO 3 ) 3 9H 2 O0.4g, AlCl 3 ·6H 2 O0.25g, Al(OH)C 4 h 6 o 4 0.26g and Na 2 SO 4 9H 2 O1.5g, silica gel 0.27g, it is dissolved in the water of 350ml, then under the condition of stirring, slowly add dropwise the molar ratio is NaOH:KOH=1:3, the total mass concentration is 30% solution to pH=5, room temperature Continue to stir for 2h;

[0033] 2) Then the precipitate was suction filtered and washed three times, baked at 110°C for 24 hours, and calcined at 500°C for 5 hours to obtain a massive solid;

[0034] 3) Grind the obtained massive solids to 10-80 meshes, - impregnate the ground particles in a solution containing 0.012g Na 2 CO 3 , 0.05g K 2 CO 3 6.7mL of deionized aqueous solution, soaked for 24h, then dried at 110°C, and calcined at 500°C for 3h to obtain the catalyst Fe 2 o 3 -FeO-SiO 2 -Al 2 o 3 -K 2 O-Na 2 O, wherein the ratio of iron oxid...

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PUM

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Abstract

The invention discloses a method for preparing 2,3,6-trimethylphenol, and the 2,3,6-trimethylphenol is an important intermediate of vitamin E. The method comprises the following steps of: enabling a mixture of metacresol, methanol and water to pass a fixed bed reactor containing an o-position methylation catalyst in a liquid space velocity of 0.4-10 h<-1>, and preparing the 2,3,6-trimethylphenol by carrying out a gas solid phase catalytic reaction under a temperature of 280-450 DEG C and a pressure of 0-10 MPa, wherein the o-position methylation catalyst consists of iron oxide, silicon dioxide and alkali metal oxide, and in the oxides, the metal ion molar ratio of iron, silicon, aluminum and alkali metal is equal to 100:(0.1-10):(0.2-5):(0-1). According to a catalyst for synthesizing the 2,3,6-trimethylphenol and a preparation method thereof, the conversion rate of the metacresol for compounding the 2,3,6-trimethylphenol is 100%, the yield of the 2,3,6-trimethylphenol is above 99.9%, and the service life of the catalyst is longer than 3000 hours.

Description

technical field [0001] The invention belongs to the technical field of solid catalysts, and relates to a catalyst for 2,3,6-trimethylphenol, an important intermediate of vitamin E, and a preparation method of the catalyst. Background technique [0002] 2,3,6-Trimethylphenol, also known as trimethylphenol, 1-hydroxy-2,3,6-trimethylphenol, 3-hydroxypseudocumene, white or light yellow crystal, has a strong phenolic smell , Insoluble in water, has good solubility in alcohol. The basic organic chemical raw material 2,3,6-trimethylphenol has a wide range of applications. In addition to being used in the synthesis of the main ring of vitamin E, it is also used as a monomer for the production of heat-resistant polyphenylene ether engineering plastics and a raw material for plastic alloys. At the same time, this substance has a good antioxidant function and is widely used in food additives, feed additives and cosmetics. In addition, it is also an indispensable intermediate and mediu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/78C07C39/07C07C37/16
Inventor 肖国民李遵陕姜枫牛磊熊振
Owner SOUTHEAST UNIV
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