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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

Inactive Publication Date: 2015-04-15
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention aims to overcome the defect that the current preparation of sodium hydride needs to be carried out under high temperature and high pressure conditions, and provides a method capable of preparing sodium hydride at a lower temperature and in a normal pressure hydrogen atmosphere

Method used

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Examples

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Effect test

preparation example Construction

[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

The invention discloses a method for preparing sodium hydride. The method for preparing sodium hydride comprises the following steps: firstly, in an inert gas atmosphere, mixing metallic sodium and a surfactant into mineral oil to form a mixed reactant, wherein concentration of the metallic sodium in the mineral oil is 60-150g / L, addition amount of the surfactant accounts for 0.5-2.40% of the weight of the mineral oil; secondly, heating the mixed reactant to the temperature of 100-110 DEG C, and insulating for 0.5-2 hours, so as to obtain a metallic sodium dispersion liquid; thirdly, heating the metallic sodium dispersion liquid to the temperature of 200-220 DEG C, introducing hydrogen and carrying out a hydrogenation reaction for 1-6 hours at the temperature of 220-350 DEG C and the pressure of 0.001-0.02MPa, so as to obtain sodium hydride dispersed in the mineral oil. The method for preparing sodium hydride is simple in preparation technology, and a reaction can be carried out at a lower reaction temperature and in normal-pressure hydrogen atmosphere, so that requirement on equipment is reduced and further, production cost of the sodium hydride product is reduced.

Description

technical field [0001] The present invention relates to the preparation technology of sodium hydride. Background technique [0002] Sodium hydride is a high value-added fine chemical product, which can be used as condensing agent, reducing agent, alkylating agent, hydrogenation catalyst, Claisen reagent, rust remover and hydrogen releasing agent in organic synthesis; it can also be widely used in In medicine, spices, pesticides, dye brighteners, rust removers and other organic synthesis; as a hydrogen storage material, it can be used to manufacture high-energy fuels and hydrogen source fuel cells, and is a new energy raw material. [0003] Currently, there are two types of techniques for synthesizing sodium hydride: dry method and wet method. The dry method is to directly react sodium metal with hydrogen, or disperse sodium metal in a solid dispersant to prepare sodium hydride. This type of method has not been applied in industry due to the low dispersion of sodium metal, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B6/04
Inventor 侯殿保李海民党亚杨海云
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI