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Method for preparing phenol from benzene by hydroxylation at one step

A technology for benzene one-step hydroxyl and phenol, applied in the field of phenol synthesis, can solve the problems of complex process, many reaction steps, low benzene conversion rate and the like, and achieve the effects of simple reaction equipment, short reaction time and convenient operation.

Inactive Publication Date: 2013-12-04
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process route overcomes the disadvantages of the traditional phenol synthesis route, such as many reaction steps and complex process, and the disadvantage of low benzene conversion rate in the existing phenol one-step synthesis process route

Method used

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  • Method for preparing phenol from benzene by hydroxylation at one step
  • Method for preparing phenol from benzene by hydroxylation at one step

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 0.25g catalyst (NH 4 ) 6 Mo 7 o 24 4H 2 O (the catalyst is 1.42mmol in terms of molybdenum atoms), 1.85g of hydroxylamine sulfate (22.50mmol in terms of hydroxylamine) is placed in a 100ml three-necked flask, and then 20ml of acidic medium is added. In this acidic medium, glacial acetic acid: water: concentrated sulfuric acid (98% ) at a volume ratio of 15:4:1, stirred at 30°C for 20 minutes at a constant temperature; then 1.0ml of benzene (11.25mmol) was added, the reaction solution was heated to 70°C, refluxed, stirred at constant temperature, and reacted at normal pressure for 5h.

[0029] The organic phase in the reaction solution is separated to obtain the target product phenol, and by-product aniline and the like. Utilize the retention value method of pure substance, and chromatograph-mass spectrometer to qualitatively analyze the composition of organic phase, adopt gas chromatography to quantitatively analyze the conversion rate of benzene and the selec...

Embodiment 2

[0031] Weigh 0.24g catalyst Na2 MoO 4 2H 2 O (the catalyst is 1.00mmol in terms of molybdenum atoms), 1.85g hydroxylamine sulfate (22.50mmol in terms of hydroxylamine) is placed in a 100ml three-necked flask, and then 20ml of acidic medium is added. In this acidic medium, glacial acetic acid: water: concentrated sulfuric acid (98% ) at a volume ratio of 15:3.5:1.5, stirred at 30°C for 20 minutes at a constant temperature; then 1.0ml of benzene (11.25mmol) was added, the reaction solution was heated to 70°C, refluxed, stirred at constant temperature, and reacted at normal pressure for 5h. The experimental results are shown in Table 1.

Embodiment 3

[0033] Weigh 5g carrier SiO 2 , placed in a 100ml evaporating dish, the volume required for equal-volume immersion was measured with deionized water to be 18.5ml; weigh 1.08g (NH 4 ) 6 Mo 7 o 24 4H 2 O was dissolved in 18.5ml deionized water to form a colorless and transparent impregnating solution; the impregnating solution was added dropwise to 5 g of the above carrier SiO 2 After impregnating for 24h, the impregnated catalyst was dried in an oven at 100°C for 1h, and then calcined at 500°C for 3h in an air atmosphere to prepare 1# supported catalyst.

[0034] Weigh 0.20g of the above-mentioned 1# supported catalyst (catalyst is 0.24mmol in terms of molybdenum atoms), 1.85g of hydroxylamine sulfate (22.50mmol in terms of hydroxylamine) and place it in a three-necked bottle, and then add 20ml of acidic medium, in which glacial acetic acid : water: the volume ratio of concentrated sulfuric acid (98%) is 15: 3.5: 1.5, 30 ℃ of constant temperature stirring 20min; Then add 1...

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Abstract

The invention relates to a method for preparing phenol from benzene by hydroxylation at one step. The method comprises the following steps of: placing a catalyst and a hydroxylammonium salt into a reactor, then adding an acid medium containing a lower fatty acid and an inorganic acid water solution and stirring for 20min at constant temperature of 30 DEG C; then adding benzene, stirring under normal pressure to the pressure of 0.4MPa and constant temperature of 60-90 DEG C for reacting for 3-6h, and then separating an organic phase in the reaction liquid to obtain the phenol as a product, wherein the proportions of the materials are as follows: the molar ratio of the benzene to hydroxylamine is 1:(0.5-4), the molar ratio of the catalyst (based on Mo atoms) to the benzene is 1:(0.8-140), the catalyst is sodium molybdate, ammonium molybdate or a supported catalyst taking molybdena as an active component, and the acid medium contains lower fatty acid, water and inorganic acid. The method for synthesizing the phenol has the advantages of simple process route and reaction equipment, simplicity and convenience for operation, mild reaction conditions, short reaction time and high conversion ratio of benzene and selectivity of phenol respectively up to 20-76 percent and 30-75 percent.

Description

technical field [0001] The invention relates to the synthesis of phenol, in particular to a method for preparing phenol by one-step hydroxylation of benzene. Background technique [0002] Phenol, commonly known as carbolic acid and hydroxybenzene, is the simplest phenolic organic compound. Phenol is an important organic chemical raw material, mainly used in the synthesis of bisphenol A, caprolactam, adipic acid and salicylic acid. In addition, phenol can also be used as a solvent, reagent, and disinfectant, and it is also widely used in synthetic fibers, synthetic rubber, plastics, medicine, pesticides, spices, dyes, and coatings. [0003] Since the discovery of phenol from coal tar in 1834, a great deal of research has been done on the synthesis of phenol. At present, the industrial route of phenol synthesis mainly includes benzene sulfonation method, chlorobenzene method, toluene-benzoic acid method, cyclohexanone-cyclohexanol method, cumene method, etc. (Li Hongyan, Yan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/04C07C37/00
CPCY02P20/52
Inventor 王延吉李佳张东升高丽雅安华良邢宪军薛伟
Owner HEBEI UNIV OF TECH