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Catalyst for synthesizing 2,6-xylenol as well as preparation method of catalyst and method for synthesizing 2,6-xylenol

A dimethylphenol and catalyst technology, which is applied to the catalyst for synthesizing 2,6-dimethylphenol and the fields of its preparation and synthesis of 2,6-dimethylphenol, can solve the problem of many catalyst components, complicated preparation and initial The problem of high reaction temperature can improve the activity and stability, the preparation method is simple, and the low temperature activity is high.

Active Publication Date: 2013-05-08
HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the catalyst has many components, the preparation is complicated, and the initial reaction temperature is high.

Method used

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  • Catalyst for synthesizing 2,6-xylenol as well as preparation method of catalyst and method for synthesizing 2,6-xylenol
  • Catalyst for synthesizing 2,6-xylenol as well as preparation method of catalyst and method for synthesizing 2,6-xylenol
  • Catalyst for synthesizing 2,6-xylenol as well as preparation method of catalyst and method for synthesizing 2,6-xylenol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh Fe(NO 3 ) 3 9H 2 O404g, Mg(NO 3 ) 2 ·6H 2 O12.82g and 28.80g of phosphotungstic acid were mixed and dissolved in 800mL of ethanol, and then slowly mixed with 28% 700mL of concentrated ammonia water containing 4gPEG in a co-current manner under normal temperature ultrasonic conditions, and continued to stir for 30min after the addition was completed. Then the precipitate was filtered, washed, and baked at 120°C for 6h. The obtained solid is calcined at 450°C for 8 hours, and finally the solid is ground into fine particles, and then crushed into small particles of 10-20 meshes, which is the obtained catalyst FeMg. 0.05 PW 0.01 (PW stands for phosphotungstic acid).

[0025] Pack 40mL of the above catalyst into a stainless steel fixed-bed reactor, the raw material is phenol:methanol:water=1:5:1 (molar ratio), and the mass space velocity is 0.4 hr -1 , the carrier gas is N 2 The flow rate is 20 mL / min, the reaction pressure is normal, and the catalyst runs st...

Embodiment 2

[0028] Weigh Fe(OAc) 3 233.05g, Mg(OAc) 2 1.42g and 94.55g of silicomolybdic acid were mixed and dissolved in 800mL of ethanol, and then slowly mixed with 700mL of 28% concentrated ammonia water containing 8gPEG in a co-current manner under ultrasonic conditions at room temperature. The precipitate was filtered, washed, and baked at 120°C for 6h. The obtained solid is calcined at 450°C for 8 hours, and finally the solid is ground into fine particles, and then crushed into small particles of 10-20 meshes, which is the obtained catalyst FeMg. 0.01 SM 0.04 (SM stands for silicomomolybdic acid).

[0029] Pack 40mL of the above catalyst into a stainless steel fixed-bed reactor, the raw material is phenol:methanol:water=1:4:0.5 (molar ratio), and the mass space velocity is 0.5 hr -1 , the carrier gas is N 2 The flow rate is 15 mL / min, the reaction pressure is 0.2 MPa, and the catalyst runs stably for 2000 h in one pass. The reaction results are shown in the table below.

[00...

Embodiment 3

[0032] Weigh FeCl 3 162.21g, MgCl 2 ·6H 2 O6.10g and 37.82g of sodium phosphomolybdate were mixed and dissolved in 800mL of ethanol, and then slowly mixed with 28% 700mL of concentrated ammonia water containing 4gPEG in a co-current manner under normal temperature ultrasonic conditions, and continued to stir for 30min after the addition was complete , and then the precipitate was filtered, washed, and baked at 120°C for 6h. The obtained solid is calcined at 450°C for 8 hours, and finally the solid is ground into fine particles, and then crushed into small particles of 10-20 meshes, which is the obtained catalyst FeMg. 0.03 (PMNa) 0.02 (PMNa stands for sodium phosphomolybdate).

[0033] Pack 40mL of catalyst into a stainless steel fixed bed reactor, the raw material is phenol:methanol:water=1:3:0.5 (molar ratio), and the mass space velocity is 1.0 hr -1 , the carrier gas is N 2 The flow rate is 10 mL / min, the reaction pressure is 0.2MPa, and the catalyst runs stably for ...

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Abstract

The invention discloses a catalyst for synthesizing 2,6-xylenol as well as a preparation method of the catalyst and a method for synthesizing 2,6-xylenol. The catalyst is a composite oxide of Fe, Mg and heteropolyacid / salt with a molar ratio of 1:(0.01-0.05):(0.01-0.04). The preparation method of the catalyst comprises the following steps of: mixing and dissolving soluble iron slat, magnesium salt and heteropolyacid / salt into an alcohol solvent in proportion to obtain a solution A; adding polyethylene glycol to stronger ammonia water to obtain a solution B; slowly mixing the solution A with the solution B under a normal-temperature ultrasonic condition in a cocurrent flow mode, and continuously stirring for 30 minutes after the polyethylene glycol is added; filtering, washing and drying the obtained precipitates; and grinding and tabletting the roasted solid to obtain the catalyst. The preparation method of the catalyst disclosed by the invention is adopted, so that the phenol conversion rate is as high as 99%, the ortho-position selectivity is as high as 99%, and the service life of the catalyst is more than 2000 hours. Moreover, the catalyst is high in low-temperature activity, simple in preparation method, non-toxic and good in stability.

Description

technical field [0001] The invention relates to a catalyst for synthesizing 2,6-dimethylphenol, a preparation method thereof and a method for synthesizing 2,6-dimethylphenol using the catalyst. Background technique [0002] 2,6-Dimethylphenol is a raw material for the synthesis of polyphenylene ether resin (PPE), photographic agents, pesticides, medicines, polyester and polyether resins, and is widely used. [0003] In the early stage, 2,6-dimethylphenol was isolated from coal tar and petroleum cracking products, with low yield and poor quality. In 1945, N. Cullinane et al first used phenol and methanol for gas-phase catalytic methylation to synthesize 2,6-dimethylphenol. The improvement of synthesis selectivity and conversion of 2,6-dimethylphenol mainly depends on the continuous improvement of its ortho-methylation catalyst. [0004] The earliest used catalyst for ortho-methylation of phenol was Al 2 o 3 , due to its low catalytic activity and low selectivity of ortho-...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J31/16C07C39/07C07C37/16
Inventor 黄华衷晟佘喜春徐斌谢琼玉郑香兰
Owner HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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