Method for preparing sodium hydride
A technology of sodium hydride and metal sodium, applied in the direction of alkali metal/alkaline earth metal/beryllium/magnesium hydride, etc., to achieve the effect of reducing requirements, reducing production costs, and simple preparation process
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[0019] The invention provides a method for preparing sodium hydride with simple process and low cost, which solves the problems of high cost, harsh operating conditions and high requirements for equipment in the prior art preparation process of sodium hydride.
[0020] The preparation method of sodium hydride provided by the present invention mainly includes three steps of raw material mixing, melt dispersion and hydrogenation reaction, and these three steps are described respectively below.
[0021] Raw material mixing step S1: mixing metal sodium and surfactant into mineral oil in an inert atmosphere to form a mixed reactant.
[0022] Sodium metal is stored in mineral oil (usually liquid paraffin, kerosene, etc.), mineral oil can disperse sodium metal, and can also be used as a heat conduction agent to absorb excess reaction heat and maintain an appropriate reaction temperature. Avoid decomposition of sodium hydride at too high a temperature. The dispersion effect will dire...
Embodiment 1
[0041] Under the protection of nitrogen, 150ml of liquid paraffin, 12.13g of sodium metal from which mineral oil has been removed, 1g of oleic acid, and 1.8g of potassium hydroxide (14.8% of the weight of sodium metal) were quickly added to a 500ml four-neck flask. After the feeding is completed, start stirring, seal, and ventilate, and heat up to 100-110°C to melt metal sodium in a hydrogen atmosphere, and the melting time is 0.5 hours. Then, under the protection of 0.02MPa hydrogen, when the temperature was raised to 200-220°C at 3°C / min, the hydrogenation reaction started, and hydrogen was passed at a flow rate of 0.14L / min, and the temperature was continued to rise to 290°C. After 1 hour, the hydrogenation was completed.
[0042] Cool to room temperature under nitrogen atmosphere. Filter to obtain off-white powdery sodium hydride,
[0043] Average particle size ≤ 20 microns. Product quality 14g, product content 57.88%; product purity 98.02%, product yield 65.08%.
[004...
Embodiment 2
[0046] Under the protection of nitrogen, 150ml of liquid paraffin, 18g of sodium metal from which mineral oil has been removed, 1g of lauric acid, and sodium hydride accounting for 5% of the amount of sodium metal charged were quickly added to a 500ml four-necked flask. After the feeding is completed, start stirring, seal, and ventilate, and heat up to 100-110°C to melt metal sodium in a hydrogen atmosphere, and the melting time is 1 hour. Then, under the protection of 0.005MPa hydrogen, when the temperature is raised to 200-220°C at 6°C / min, the hydrogenation reaction starts, and hydrogen is passed at a flow rate of 0.4L / min, and the temperature is continued to rise to 300°C. After 2 hours, the hydrogenation is completed.
[0047] Cool to room temperature under nitrogen atmosphere. Filter to obtain off-white powdery sodium hydride.
[0048] Average particle size ≤ 20 microns. Product quality 26.1g, product content 49.55%, product purity 97.88%, product yield 70%.
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Abstract
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