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Phthalic Anhydride by Air Oxidation of Naphthalene: Gibbs and Conover, 1918
Harry D. Gibbs and Courtney Conover patented this in 1918, US 1,285,117 (filed 1917), and dedicated it to the public. Phthalic anhydride had been made by oxidising naphthalene with sulphuric acid in the presence of mercury sulphate; they used air instead. Naphthalene vapour mixed with plenty of air is passed over finely divided oxides of vanadium at 350–550 °C, and the phthalic anhydride formed is condensed and separated by fractional sublimation.
高级
Works process
说明
1
1
Melt and vaporise the naphthalene
Melt and vaporise the naphthalene
Melt the naphthalene and let it flow continuously, at a measured rate, into a heated chamber where it is volatilised.
此步骤所需材料:
萘1 as required所需工具:
铸铁熔锅
汽化室
温度计2
2
Mix the vapour with air
Mix the vapour with air
Mix the naphthalene vapour with air in excess of the amount needed to oxidise it to phthalic anhydride, preferably at least four times the amount theoretically required.
所需工具:
鼓风机
汽化室3
3
Pass it over vanadium oxide at 350–550 °C
Pass it over vanadium oxide at 350–550 °C
Pass the mixture into a reaction chamber kept at 350–550 °C, preferably 500 °C. There it is forced into close contact with oxides of vanadium in the form of a fine powder, supported on trays, with baffle plates forcing the gas current through it. Keep the gases under pressure only sufficient to make them flow continuously through the chamber. The naphthalene is oxidised to phthalic anhydride, with carbon dioxide and water.
所需工具:
托盘式催化室
氧化钒
高温计
鼓风机4
4
Condense the products
Condense the products
Condense the products of the reaction, phthalic anhydride with small portions of other oxidation products of naphthalene, together with the unchanged naphthalene.
所需工具:
冷凝室5
5
Separate by fractional sublimation
Separate by fractional sublimation
Separate the phthalic anhydride from the other oxidation products and the unchanged naphthalene by fractional sublimation.
所需工具:
升华装置
温度计6
6
How much air
How much air
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