Catalyst for synthesizing benzaldehyde and benzyl alcohol from toluol, the preparation process and application thereof

A catalyst, a technology of benzaldehyde, applied in the preparation of the above-mentioned catalyst, and the application field of the above-mentioned catalyst in the catalytic oxidation of toluene to synthesize benzaldehyde and benzyl alcohol, can solve problems such as difficulty in recycling, increase separation difficulty, etc., and achieve production cost saving, The effect of high selectivity and mild reaction conditions

Inactive Publication Date: 2004-03-31
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction conditions are milder and the selectivity is higher, but the use of a homogeneous catalyst is not easy to recycle; the use of solvents and additives increases the difficulty of separation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 177.3gZrOCl 2 ·8H 2 O was dissolved in deionized water to make a 500mL solution (ZrO 2+ The molar concentration is 1.1mol / L), stirring while heating, the temperature is kept at about 60°C, and 210mL of sodium hydroxide solution with a concentration of 5.5mol / L is added dropwise to the above solution to produce precipitation, and the pH value at the end of the solution is maintained at 7. After the dropwise addition was completed, the precipitate was filtered out, and washed with 300 mL of deionized water for 6 times to remove Cl - ions, using silver nitrate solution (0.1mol / L) to detect Cl - ion. Then dry at 100°C for 12 hours, burn at 650°C for 3 hours, cool down, and weigh 60g. Grind, sieve, and take 80-100 mesh granules for reaction evaluation. The catalyst designation is Cat-01.

[0028] The toluene oxidation reaction was carried out in a 1.0L reaction kettle, and 60g of toluene and 1.6g of catalyst Cat-01 were added; the top of the kettle was sealed, stirred...

Embodiment 2

[0030] 177.3gZrOCl 2 ·8H 2 O and 89.3gFeCl 3·6H 2 O was dissolved in deionized water to make a 500mL solution (ZrO 2+ and Fe 3+ The molar concentrations are 1.1mol / L and 0.66mol / L respectively), while heating and stirring, the temperature is kept at about 75°C, 390mL sodium hydroxide solution (5.5mol / L) is added dropwise to the above solution, and the final pH of the solution is Keep it at 7. After the precipitation was completed, the precipitate was filtered out, and washed with 300 mL of deionized water for 6 times to remove Cl. - ions, using silver nitrate solution (0.1mol / L) to detect Cl - ion. Then dry at 110°C for 12 hours, burn at 650°C for 3 hours, cool, grind, sieve, and take 80-100 mesh particles for reaction evaluation. The catalyst designation is Cat-02. The composition ratio (mol / mol) of the active components is Fe:Zr=0.6:1. Except that using Cat-02 catalyst and reaction pressure is 0.1MPa, other reaction conditions and analysis method are the same as em...

Embodiment 3

[0032] 177.3gZrOCl 2 ·8H 2 O and 109.6gCo(CH 3 COO) 2 4H 2 O was dissolved in deionized water to make a 500mL solution (ZrO 2+ and Co 2+ The molar concentrations are respectively 1.1mol / L and 0.44mol / L), while heating and stirring, the temperature is maintained at about 50°C, and 370mL of sodium hydroxide solution with a concentration of 5.5mol / L is added dropwise to the above solution to produce precipitation. The final pH of the solution was maintained at 7. After the dropwise addition was completed, the precipitate was filtered out, and washed with 300 mL of deionized water for 6 times to remove Cl - ions, using silver nitrate solution (0.1mol / L) to detect Cl - ion. Then dry at 120°C for 12 hours, burn at 550°C for 3 hours, cool, grind, sieve, and take 80-100 mesh particles for reaction evaluation. The catalyst designation is Cat-03, and the composition ratio of active components (mol / mol): Co:Zr=0.8:1. Except that using Cat-03 catalyst and reaction pressure is 1....

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PUM

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Abstract

A catalyst of synthesizing benzaldehyde and benzyl alcohol by methylbenzene, its manufacturing method and application. The active component is zirconium, or transit metals, alkaline metal, alkaline-earth metals, metals of IIIAíóIVA and VA Group in the Periodic Table. The method comprises solving a zirconium compound or a zirconium compound and a compound of an element as the active component, adding a precipitator; drying, burning, pulverizing to particles. In reactions, a gas containing oxygen is the oxygen source, such as oxygen and air, an organic solution wouldn't be used. The catalyzing reaction is 180-195 degree C, the pressure is 0.8-1.2Mpa. when the conversion rate of methylbenzene is 13.0úÑ, the total selectivity of benzaldehyde and benzyl alcohol is 86.6úÑ. In the method, the catalyst is easy to be separated and could be recyclable, the reaction condition is mild.

Description

technical field [0001] The invention relates to a catalyst for directly catalyzing the oxidation of toluene to synthesize benzaldehyde and benzyl alcohol. [0002] The present invention also relates to a method for preparing the above-mentioned catalyst. [0003] The present invention also relates to the application of the above-mentioned catalyst in the synthesis of benzaldehyde and benzyl alcohol by catalytic oxidation of toluene. Background technique [0004] Benzaldehyde and benzyl alcohol are important fine chemical intermediates, widely used in medicine, pesticide, food and other fields. The production of benzaldehyde and benzyl alcohol can adopt the method of toluene chlorination-hydrolysis; but this method equipment corrosion is serious, produces chlorine-containing waste water and pollutes the environment, and it is difficult to separate a small amount of chlorine-containing impurities in the product, which cannot meet the requirements of medicine, food and other f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/02B01J23/06B01J23/50B01J23/72B01J23/75B01J23/76C07C33/22C07C45/27C07C47/34
Inventor 徐杰王峰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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