Method for producing hydrogen phosphide by utilizing phosphorous acid pyrolysis
A technology of phosphine and phosphorous acid, applied in phosphine and other directions, can solve problems such as strong corrosion of reaction equipment, and achieve the effects of low reaction temperature, high product recovery rate and low energy consumption
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Embodiment 1
[0022] Preparation of Platinum Carbon Catalyst
[0023] 1) Preparation of activated carbon support
[0024] Sieve 200-300 mesh activated carbon, add 5g of activated carbon and 45ml17%HNO into a three-necked flask 3 The solution (solid-liquid mass ratio is 1:10) was stirred and refluxed at 90-100°C for 3 hours, washed with distilled water until neutral, filtered, and dried at 110°C to obtain the activated carbon carrier.
[0025] 2) Preparation of platinum-carbon catalyst
[0026] Add 0.12g of carrier and 1.8ml of distilled water into a 50ml three-necked flask, add 0.19ml of chloroplatinic acid solution (31.65mg / ml (c=0.0772mol / l) equivalent to 5%Pt / Ac) under stirring, and heat up to 80°C Stir for 2 hours, then cool down to 40°C, add 0.2ml of formic acid, stir for 0.5h; dropwise add NaOH solution (0.1ml / L) to pH=8~9, raise the temperature to 80°C to promote the reduction; until Pt (IV ) was completely reduced; the reducing solution was filtered and washed several times with ...
Embodiment 2
[0028] In a 250ml three-necked flask, add 200g of phosphorous acid raw material (1mol) with a purity of 93%, and add 0.372g of a platinum carbon catalyst with a platinum content of 5w / w% prepared in Example 1. The weight ratio of platinum and phosphorous acid is 1 / 10,000 one. After purging the reaction system thoroughly with nitrogen, maintain a small nitrogen flow rate, and raise the temperature to 200 °C under stirring. Phosphine begins to be produced and enters the collection bottle along with the nitrogen flow. The collection bottle is filled with 1000ml of absorption solution (composed of 37w / w% formaldehyde and 10w / w% hydrochloric acid). After the collection bottle absorbs all the phosphine produced, its total phosphorus content is determined to be 5.1 g of phosphorus. In theory, 1 mol of phosphorous acid can generate 0.25 mol of phosphine, containing 7.75 g of phosphorus, which indicates that the yield of phosphine is 65.8%.
Embodiment 3
[0030] In a 250ml three-necked flask, add 84g of phosphorous acid raw material (1mol) with a purity of 98%, and add 1.64g of the platinum carbon catalyst with a platinum content of 5w / w% prepared in Example 1. The weight ratio of platinum and phosphorous acid is 1 / 1000 one. After purging the reaction system thoroughly with nitrogen, maintain a small nitrogen flow rate, and raise the temperature to 160°C under stirring. Phosphine begins to be produced and enters the collection bottle along with the nitrogen flow. The collection bottle is filled with 1000ml of absorption solution (composed of 37w / w% formaldehyde and 10w / w% hydrochloric acid). After the collection bottle absorbed all the phosphine produced, its total phosphorus content was determined to be 6.3g phosphorus. In theory, 1 mol of phosphorous acid can generate 0.25 mol of phosphine, containing 7.75 g of phosphorus, which indicates that the yield of phosphine is 81.3%.
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