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Method for preparing pyridine N-oxide

A technology for oxidizing pyridine and pyridine, which is applied in chemical instruments and methods, organic chemistry, molecular sieve catalysts, etc., and can solve problems such as high on-site production costs, high cost, and economic obstacles

Active Publication Date: 2009-11-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Limited by cost and safety issues, and the preparation of H 2 o 2 Separate equipment and circulation system are required, which cost a lot, and the on-site production cost is very high. Before the introduction of stricter environmental protection regulations, H 2 o 2 There are certain economic barriers to the industrialization of the craft

Method used

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  • Method for preparing pyridine N-oxide
  • Method for preparing pyridine N-oxide
  • Method for preparing pyridine N-oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0069]Get 20 grams of titanium-silicon molecular sieve TS-1, concentration is 0.01 g / ml (as palladium atom) ammonium nitrate palladium complex solution and appropriate amount of hydrazine hydrate and cetyltrimethylammonium bromide are added to tetrapropyl Aqueous solution of ammonium hydroxide (mass percentage concentration 10%) stirs and mixes evenly, wherein titanium silicon molecular sieve (gram): hexadecyltrimethylammonium bromide (mole): tetrapropyl ammonium hydroxide (mole): hydrated Hydrazine (mol): ammonium nitrate palladium complex (g, calculated as 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 ...

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 ...

Embodiment 3

[0073] Tetraethyl orthosilicate, tetrabutyl titanate, palladium acetate solution and Tween 80 with a concentration of 0.01 g / ml (as palladium atom) 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: tetrapropylammonium 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 72 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 hydrothermal ...

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Abstract

The invention discloses a method for preparing pyridine N-oxide, which is characterized in that the pyridine N-oxide is prepared by mixing pyridine, oxygen, hydrogen, diluent gas, solvent and catalyst for contact reaction at 0-180 DEG C and 0.1-3.0 MPa, wherein the mol ratio of the pyridine to the oxygen to the hydrogen to the diluent gas is 1:0.1-10:0.1-10:0-100, the mass ratio of the pyridine to the catalyst is 0.5-50:1, and the mass ratio of the solvent to the catalyst is 20-1000:1, and in addition, the catalyst is microporous titanium silicon material or compound containing the microporous titanium silicon material, an oxide formed by the microporous titanium silicon material has the formula of xTio2.100SiO2.yEmOn.zE, wherein x is equal to 0.001-50.0, y+z is equal to 0.005-20.0, y / z is less than 5, E can be one or more of such noble metals as Ru, Rh, Pd, Re, Os, Ir, Ag, Pt and Au, and both m and n are the numbers meeting the need of the oxidation of the E. The grains of the epoxy propanol can be in hollow structures or concavo-convex structures, and the method ensures the high conversion rate, the good selectivity and the long operation period of the pyridine.

Description

technical field [0001] The present invention relates to a method for producing pyridine N-oxide, and more particularly the present invention relates to a method for producing pyridine N-oxide by oxidation of pyridine. Background technique [0002] Pyridine N-oxide is a commonly used intermediate of pharmaceutical and chemical products. As a new type of nonionic surfactant, it can increase surface adsorption, reduce surface viscosity and stabilize foam. According to different reaction mechanisms, the preparation of pyridine N-oxide can be divided into direct oxidation method and catalytic oxidation method. Commonly used oxidants in the direct oxidation method are hydrogen peroxide and peracetic acid. Hydrogen peroxide oxidation has the advantages of simple process, mild conditions and high yield. The disadvantage is that the demand for glacial acetic acid as a medium is large, and the operation is cumbersome, and a large amount of sodium hydroxide must be added for neutral...

Claims

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Application Information

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IPC IPC(8): C07D213/89B01J29/89
Inventor 朱斌史春风林民舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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