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Method for synthesizing epoxy styrene by catalytic oxidation of phenylethylene

A technology for ethylene oxide and catalytic oxidation, which is applied in chemical instruments and methods, molecular sieve catalysts, catalysts for physical/chemical processes, etc., and can solve problems such as no research reports on ethylene oxide.

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

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Problems solved by technology

However, there is no research report on the application in the preparation of styrene oxide by oxidizing styrene

Method used

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  • Method for synthesizing epoxy styrene by catalytic oxidation of phenylethylene
  • Method for synthesizing epoxy styrene by catalytic oxidation of phenylethylene
  • Method for synthesizing epoxy styrene by catalytic oxidation of phenylethylene

Examples

Experimental program
Comparison scheme
Effect test

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 the precious metal-containing microparticles. Porous titanium silicon material A. After characterization, its composition can be e...

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 method for catalyzing phenylethylene oxide to synthesize epoxy ethylbenzene, which is characterized in that under the condition of the temperature of 0 DEG C to 180 DEG C and the pressure of 0.1MPa to 3.0MPa, phenylethylene, oxygen, hydrogen, diluents, a solvent and a catalyst are mixed and contacted for reaction; the mole ratio of the phenylethylene, the oxygen, the hydrogen and the diluents is 1 : (0.1 to 10) : (0.1 to 10 ): (0 to 100); the mass ratio between the phenylethylene 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 refers to a cellular titanium silicon material or a composition containing the cellular titanium silicon material; the composition of the cellular titanium silicon material expressed in the manner of oxides is xTiO2 question mark 100SiO2 question mark yEmOn question mark zE, wherein, the value of X is between 0.001 and 50.0; the value of (y plus z) is between 0.005 and 20.0 and y / z is less than 1; E represents one or more noble metals selected from Ru, Rh, Pd, Re, Os, Ir, Pt and Au; m and n are numbers meeting the need of E at oxidation state; and the grains of the material are partially hollow and completely hollow.

Description

technical field [0001] The invention relates to a method for catalyzing the oxidation of styrene, and more particularly relates to a method for catalyzing the oxidation of styrene to synthesize styrene oxide by using titanium silicon material as a catalyst. Background technique [0002] Styrene oxide can be used as a diluent, UV absorber, and flavor enhancer for epoxy resins, and is also an important intermediate in organic synthesis, pharmaceuticals, and fragrance industries, such as β-phenylethanol produced by hydrogenation of styrene oxide It is the main component of rose oil, clove oil and neroli oil, and is widely used in the preparation of food, tobacco, soap and cosmetic essence. In recent years, the demand for β-phenylethyl alcohol and medicine levamisole has increased sharply at home and abroad, resulting in a situation in which the supply of styrene oxide is in short supply in the domestic and foreign markets, which has brought broad opportunities for the research ...

Claims

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Application Information

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IPC IPC(8): C07D301/12C07D303/04B01J29/89
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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