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Synthetic method of o-phenylphenol

A technology of o-phenylphenol and catalyst, which is applied in the field of synthetic compounds, can solve the problems of increased separation and purification tasks, increased costs, and low industrial value, and achieves the effects of high production efficiency, improved selectivity, and convenient recovery

Inactive Publication Date: 2012-07-25
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the addition of hydrogen acceptors and solvents to the reactants, the cost is increased, the subsequent separation and purification tasks are increased, and the industrialization value is not great.

Method used

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  • Synthetic method of o-phenylphenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Dilute 50g with Na 2 CO 3 Add the modified 1% Pt / C catalyst and 500g of cyclohexanone dimer together into the reactor, fill it with nitrogen for replacement 3 times, heat it to 370-380°C under stirring, and release the hydrogen generated by the reaction in time to maintain the pressure At 1.0~1.2MPa. Sampling analysis, when the o-cyclohexylphenol content in the reaction solution is less than 2%, the reaction is stopped. The reaction liquid was cooled to 70° C. and filtered to obtain a total of 442 g of filtrate. Gas chromatography analysis showed that the content of o-phenylphenol in the reaction liquid was 90.6%, and the conversion rate of cyclohexanone dimer was 100%.

Embodiment 2

[0021] 30g with K 2 CO 3 Add the modified 3% Pt / C catalyst and 500g of cyclohexanone dimer together into the reactor, fill it with nitrogen for replacement 3 times, heat it to 390-400°C under stirring, release the hydrogen generated by the reaction in time to maintain the pressure 1.9-2.0MPa. Sampling analysis, when the o-cyclohexylphenol content in the reaction solution is less than 2%, the reaction is stopped. The reaction solution was cooled to 60° C. and filtered to obtain a total of 449 g of filtrate. Gas chromatography analysis showed that the o-phenylphenol content in the reaction solution was 91.3%, and the conversion rate of cyclohexanone dimer was 100%.

Embodiment 3

[0023] 20g with CaCO 3 Add the modified 5% Pt / C catalyst and 500g of cyclohexanone dimer together into the reactor, fill it with nitrogen for replacement 3 times, heat it to 320-330°C under stirring, release the hydrogen generated by the reaction in time to maintain the pressure It is 0.6-0.7MPa. Sampling analysis, when the o-cyclohexylphenol content in the reaction solution is less than 2%, the reaction is stopped. The reaction solution was cooled to below 65° C. and filtered to obtain a total of 451 g of the filtrate. Gas chromatography analysis showed that the content of o-phenylphenol in the reaction solution was 90%, and the conversion rate of cyclohexanone dimer was 100%.

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Abstract

The invention discloses a synthetic method of o-phenylphenol. The method comprises the following steps: Pt / C catalyst modified by alkali metal carbonate or alkali earth metal carbonate and cyclohexanone dimer are added in a reaction vessel, nitrogen is charged for 2-3 times to replace the air in the reaction vessel, and then heating is conducted under stirring to temperature of 320 to 400 DEG C ;the reaction pressure is 0.6 to 2MPa, the reaction is stopped when the content of intermediate o-cyclohexyl alkylphenol in the reaction liquid is less than 2 percent, and the reaction liquid is cooledto the temperature of 60 to 70 DEG C and filtered to obtain the filtrate containing o-phenylphenol. The core of the method is that the active carbon carrier is modified by alkali metal carbonate or alkali earth metal carbonate so as to inhibit the promotion action of the acid center on the active carbon to the decomposition of the reaction material, namely, cyclohexanone dimer, and simultaneouslyprovide proper alkaline condition for the generation of the o-phenylphenol, therefore, the selectivity of the catalyst is greatly improved. Moreover, the production efficiency of the catalyst in process unit is high, the recovery of the catalyst is convenient, and the method is beneficial to industrialization.

Description

technical field [0001] The invention relates to a method for synthesizing compounds, in particular to a method for synthesizing o-phenylphenol. Background technique [0002] Ortho-phenylphenol (OPP) is an organic chemical product with a wide range of uses. It is widely used in sterilization and anticorrosion, printing and dyeing auxiliaries and surfactants, synthetic new plastics, stabilizers and flame retardants for resins and polymer materials, etc. field. [0003] OPP and its sodium salt have a broad-spectrum bactericidal and mildew-removing ability, and are low-toxic and tasteless. They are good preservatives and can be used for anti-mold and preservation of fruits and vegetables, especially for citrus anti-mold, and can also be used to treat lemons. , pineapples, pears, peaches, tomatoes, cucumbers, etc., can minimize rot. Britain, the United States, Canada and other countries allow a wider range of fruits to use OPP. OPP and its sodium salt can also be used as a pre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/15C07C37/06C07C37/07B01J27/232B01J23/42
CPCY02P20/52
Inventor 陈业强陈志荣毛春强袁慎峰
Owner ZHEJIANG UNIV
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