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Method for catalytically oxidizing organic matter by solid superacid and by taking potassium ferrate as oxidizing agent

A technology of solid superacid and potassium ferrate, which is applied in the fields of oxidative preparation of carbonyl compounds, chemical instruments and methods, organic chemistry, etc., which can solve the problems of fast reaction speed, shortened reaction time, difficult oxidation reaction, etc., to improve oxidation activity , shorten the reaction time, improve the effect of reaction speed

Inactive Publication Date: 2010-03-17
DAQING GASOLINEEUM INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of the oxidation reaction carried out by alkaline aqueous solution as a solvent is that the reaction speed is extremely fast, the selectivity is not easy to control, and it is not suitable for oxidation of compounds sensitive to alkalinity, especially for organic substances that are difficult to dissolve in water, and the oxidation reaction is more difficult to carry out.
When organic matter is used as a solvent, since potassium ferrate is insoluble in organic matter, its activity cannot be fully exerted, the reaction time is long, and the yield is very low
In 1996, Lionel proposed an oxidation synthesis method using montmorillonite as a solid catalyst and potassium ferrate as an oxidant in an organic solvent. For the first time, the selective oxidation of organic matter was realized at room temperature, although this method can improve oxidation synthesis. The final yield, but the method has the disadvantages of long reaction time, high consumption of potassium ferrate and organic solvent
In 2007, we proposed a new method for improving the oxidation activity of potassium ferrate (Song Hua et al., Chinese patent ZL200510053372.1). This method is to increase the oxidation activity of potassium ferrate by adding a small amount of aqueous acid solution to the organic solvent. Oxidation activity, thereby achieving the purpose of greatly shortening the reaction time, but the disadvantage of this method is the addition of liquid acid

Method used

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  • Method for catalytically oxidizing organic matter by solid superacid and by taking potassium ferrate as oxidizing agent
  • Method for catalytically oxidizing organic matter by solid superacid and by taking potassium ferrate as oxidizing agent
  • Method for catalytically oxidizing organic matter by solid superacid and by taking potassium ferrate as oxidizing agent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: add solid catalyst SO in 50mL volumetric flask 4 2- / Al 2 o 3 -ZrO 2 0.5g, 0.2mL benzyl alcohol, 0.8g potassium ferrate, reaction temperature 30°C, reaction time 2h, change the amount of cyclohexane solvent, and investigate the influence of solvent amount. Filter reaction solution, filtrate is carried out chromatographic analysis, result is as table 1 and figure 1 shown.

[0016] Table 1

[0017]

[0018] Conclusion: As can be seen from the data in Table 1, the conversion rate of benzyl alcohol and the production rate of benzaldehyde first increased and then decreased with the increase of solvent consumption. When the solvent consumption was 20 mL, the conversion rate of benzyl alcohol and the yield of benzaldehyde were the highest.

Embodiment 2

[0019] Embodiment 2: add solid catalyst SO in 50mL volumetric flask 4 2- / Al 2 o 3 -ZrO 2 0.5g, benzyl alcohol 0.2mL, solvent cyclohexane 20mL, potassium ferrate 0.8g, reaction time 2h, change the reaction temperature, investigate the influence of temperature. Filter reaction solution, filtrate is carried out chromatographic analysis, result is as table 2 and figure 2 shown.

[0020] Table 2

[0021]

[0022] Conclusion: As can be seen from the data in Table 2, within a given temperature range, as the reaction temperature increases, the conversion rate of benzyl alcohol and the yield of benzaldehyde do not change much, and the law of change of the yield of benzaldehyde increases first and then decreases , when the temperature is 40℃, the yield of benzaldehyde is the highest.

Embodiment 3

[0023] Embodiment 3: add solid catalyst SO in 50mL volumetric flask 4 2- / Al 2 o 3 -ZrO 2 0.5g, 0.2mL benzyl alcohol, 20mL solvent cyclohexane, reaction temperature 40°C, reaction time 2h, change the amount of potassium ferrate, and investigate the effect of the amount of oxidant. Filter reaction solution, filtrate is carried out chromatographic analysis, result is as table 3 and image 3 shown.

[0024] table 3

[0025]

[0026] Conclusion: As can be seen from the data in Table 3, the conversion of benzyl alcohol increases rapidly as the amount of potassium ferrate increases. After the amount of potassium ferrate is 0.7, the conversion rate of benzyl alcohol increases slowly as the amount of potassium ferrate increases. . With the increase of the dosage of potassium ferrate, the benzaldehyde production first increased and then decreased. When the solvent dosage was 0.8g, the benzaldehyde yield was the highest.

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Abstract

The invention relates to a method for catalytically oxidizing organic matter by solid superacid and by taking potassium ferrate as an oxidizing agent. The method comprises the following steps: placing the solid catalyst into a flat bottom beaker, adding organic matter to be oxidized, then adding solvent, adding the potassium ferrate under stirring, and controlling the reaction temperature to 20-70 DEG C and the reaction time to 2-12 hours to obtain the products. The invention provides a method for catalytically oxidizing organic matter by the solid superacid and by taking the potassium ferrate as the oxidizing agent; the adding of solid superacid greatly improves the reaction speed of potassium ferrate for oxidizing organic matter and shortens the reaction time; and the method does not use any liquid acid catalyst, and is characterized by simple operation, economy, green initiative and the like and can be widely applied to the synthetic field of organic chemicals.

Description

Technical field: [0001] The invention relates to a method for catalyzing and oxidizing organic matter with potassium ferrate as an oxidizing agent, specifically a new method for oxidizing organic matter with potassium ferrate under the action of a solid superacid catalyst in an organic system. Background technique: [0002] The invention relates to a method for catalyzing and oxidizing organic matter with potassium ferrate as an oxidizing agent, specifically a new method for oxidizing organic matter with potassium ferrate under the action of a solid superacid catalyst in an organic system. [0003] The general valence states of iron are II and III, while the valence states of high-valent iron-based complexes are IV-VI. The main feature is extremely high oxidation, which is a kind of KMnO 3 , O 2 and Cl 2 It is a strong oxidizing agent with strong oxidizing ability, which can oxidize most organic matter. The simple iron-based compound of VI has up to 3 electron transfer n...

Claims

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Application Information

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IPC IPC(8): C07C47/54C07C45/29B01J27/053B01J35/02
Inventor 宋华王宝辉柳艳修张娇静李锋汪怀远
Owner DAQING GASOLINEEUM INST