Preparation method for anhydrous formaldehyde
An anhydrous formaldehyde and methanol technology, applied in the preparation of organic compounds, the preparation of carbon-based compounds, chemical instruments and methods, etc., can solve the problems of low catalyst activity and stability, poor reaction selectivity, and high reaction temperature, and achieve selective High, mild reaction conditions, simple preparation effect
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Embodiment 1
[0017] Weigh 100 g of ZSM-5 molecular sieve, the molecular sieve has a silicon-aluminum ratio of 25, perform proton exchange three times in 0.5 M ammonium nitrate, and roast at 600° C. for 4 hours. Immerse it in a mixed solution of palladium chloride and zinc chloride, dry it, roast it at 350°C for 1 hour, and reduce it under a hydrogen atmosphere at 400°C for 3 hours to obtain the main active metal (Pd:molecular sieve:promoter (Zn)=20:100: 5 (mass ratio) supported molecular sieve catalyst, filled into a reaction tube after molding, and filled with a 5mm bed layer. Under normal pressure, nitrogen gas is used as a carrier gas, methanol is injected by a micropump, reacted at 250 ° C, and the feed The space velocity was 35ml / (g·s), the conversion rate of methanol was 80% and the yield of formaldehyde was 50% as detected by gas chromatography on-line.
Embodiment 2
[0019] Weigh 100g Y molecular sieve, the molecular sieve has a silicon-aluminum ratio of 2.7, perform proton exchange in 1.0M ammonium nitrate for 3 times, and calcinate at 500°C for 4h. Immerse it in a mixed solution of chloroauric acid and ferric chloride, dry it, roast it at 450°C for 3 hours, and reduce it under a hydrogen atmosphere at 450°C for 2 hours to obtain the main active metal (Au):molecular sieve:promoter (Fe)=15:100 : 15 (mass ratio) supported molecular sieve catalyst, filled into a reaction tube after molding, filled with a 5mm bed, under normal pressure, argon gas as a carrier gas, injected by a micropump, reacted at 450 ° C, and injected The material space velocity was 35ml / (g·s), the conversion rate of methanol was 75% and the yield of formaldehyde was 70% as detected by gas chromatography on-line.
Embodiment 3
[0021] Weigh 100g Y molecular sieve, the molecular sieve has a silicon-aluminum ratio of 5.6, perform proton exchange in 1.0M ammonium nitrate for 3 times, and calcinate at 500°C for 4h. Immerse it in a mixed solution of chloroauric acid and ferric chloride, dry it, roast it at 450°C for 3 hours, and reduce it under a hydrogen atmosphere at 450°C for 2 hours to obtain the main active metal (Au):molecular sieve:promoter (Fe)=15:100 : 15 (mass ratio) supported molecular sieve catalyst, filled into a reaction tube after molding, and filled with a 5mm bed layer, under normal pressure, argon gas as a carrier gas, methanol was injected by a micropump, and reacted at 450 ° C. The feed space velocity was 35ml / (g·s), the conversion rate of methanol was 55% and the yield of formaldehyde was 45% as detected by gas chromatography on-line.
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