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Method for preparing phenol

A kind of phenol, the said technology is applied in the field of catalyzing the direct hydroxylation of benzene, which can solve the problems of waste, benzene and benzene volatilization loss, etc.

Active Publication Date: 2009-05-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But raw gas H 2 —O 2 The bubbling introduction method will cause H 2 and O 2 A large amount of waste, and the mixed gas in circulation can easily take benzene out of the reactor and cause the volatilization loss of benzene

Method used

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  • Method for preparing phenol
  • Method for preparing phenol
  • Method for preparing phenol

Examples

Experimental program
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Embodiment 1

[0069] Get 20 grams of titanium-silicon molecular sieve TS-1, concentration is 0.01g / ml (as palladium atom) ammonium nitrate palladium complex solution and appropriate amount of hydrazine hydrate and cetyltrimethylammonium bromide are added to tetrapropyl Stir and mix in the aqueous solution of ammonium hydroxide (mass percentage concentration 10%), wherein titanium silicon molecular sieve (gram): hexadecyltrimethylammonium bromide (mole): tetrapropyl ammonium hydroxide (mole): hydrate Hydrazine (mol): ammonium nitrate palladium complex (gram, in palladium): water (mol)=100:0.005:0.5:3.0:2.0:1000. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 150°C and autogenous pressure for 48 hours, filter the resultant, wash with water, dry it naturally, and continue drying at 180°C for 3 hours to obtain micropores containing precious metals Titanium silicon material A. After characterization, its composition can be expressed as 4Ti...

Embodiment 2

[0071] Get 20 grams of titanium-silicon molecular sieve TS-1, a palladium chloride solution with a concentration of 0.01 g / ml (in terms of palladium atoms), and an appropriate amount of hydrazine hydrochloride and polypropylene to join in an aqueous solution of sodium hydroxide (mass percentage concentration 15%) and stir Mix well, wherein titanium silicon molecular sieve (gram): polypropylene (mol): sodium hydroxide (mol): hydrazine hydrochloride (mol): palladium chloride (gram, in palladium): water (mol)=100:0.9: 1.8:0.15:0.1:4600. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 180°C and autogenous pressure for 24 hours, filter the resultant, wash with water, dry it naturally, and continue drying at 110°C for 3 hours to obtain micropores containing precious metals. Titanium silicon material B. After characterization, its composition can be expressed as 8TiO in the form of oxides 2 100SiO2 2 ·0.006PdO·0.008Pd, the ads...

Embodiment 3

[0073] Tetraethyl orthosilicate, tetrabutyl titanate, palladium acetate solution and Tween 80 with a concentration of 0.01 g / ml (in terms of palladium atoms) were added to the aqueous solution of tetrapropylammonium hydroxide and butylenediamine (mass The percentage concentration is 10%) and stir and mix evenly, wherein the molar composition silicon source: titanium source: tetrapropyl ammonium hydroxide: butylenediamine: palladium source: protective agent: water=100:0.03:0.5:0.1:0.05: 0.02:550, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of palladium source in terms of Pd. Then put it into a sealed reactor, hydrothermally treat it at a temperature of 120°C and autogenous pressure for 120 hours, take out the resultant, filter it, dry it, and roast it to obtain an intermediate crystalline material. Transfer the intermediate crystalline material to the above remaining filtrate, add an appropriate amount of hydrazine hydrate, and then conduct a hydroth...

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Abstract

The invention discloses a preparing method of phenol, which is characterized in that in the conditions that the temperature is 0 to 150 DEG C and the pressure is 0.1 to 3.0MPa, benzene, oxygen, hydrogen, diluent gas, a solvent and a catalyst are mixed for contact reaction. The mol ratio of the benzene to the oxygen to the hydrogen to the diluent gas is equal to 1 : (0.1 to 10) : (0.1 to 10) : (0 to 100); the mass ratio between the benzene and the catalyst is (0.5 to 50) : 1; the mass ratio between the solvent and the catalyst is (20 to 1000) : 1; the catalyst is a millipore titanium silicon material or a composition containing the millipore titanium silicon material; and the component of the millipore titanium silicon material can be expressed by oxide as xTiO2 question mark 100SiO2 question mark yEmOn question mark zE, wherein, x is equal to 0.001 to 50.0, (y plus z) is equal to 0.005 to 20.0, y / z is less than 1, E represents one or a plurality of noble metals such as Ru, Rh, Pd, Re, Os, Ir, Pt and Au, m and n are the numbers meeting the oxidation state of E. The crystal grain is completely or partially in hollow-core structure.

Description

technical field [0001] The invention relates to a method for catalyzing the direct hydroxylation of benzene, and more particularly relates to a method for preparing phenol by catalyzing the direct hydroxylation of benzene with a titanium-silicon material containing noble metal as a catalyst. Background technique [0002] Phenol is an important bulk chemical raw material product in the current organic chemical industry. It is mainly used to prepare bisphenol A, phenolic resin and pharmaceutical intermediates. Bisphenol A is the main raw material for the production of polycarbonate and epoxy resins. Polycarbonate is one of the top five engineering plastics today, and plays an important role in the production of electronics and electrical appliances, photographic and optical instruments, office equipment and household goods. Epoxy resins are mainly used to make laminates, varnishes and adhesives. Phenolic resins, especially resins made of phenol and formaldehyde, have greater...

Claims

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Application Information

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IPC IPC(8): C07C39/04C07C37/58B01J29/89
CPCY02P20/52
Inventor 林民史春风朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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