Preparation method of inorganic compound sodium selenide and device of preparation method

A technology of inorganic compounds and sodium selenide, applied in the direction of binary selenium/tellurium compounds, etc., to ensure the purity, ensure the safety of the reaction, and prevent the pressure from being too large.

Active Publication Date: 2014-05-28
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the efficiency of preparing sodium selenide is poor, and in-situ drying cannot be realized. For example, a chemical synthesis method of sodium selenide is proposed on page 421 of the first volume of the second edition of "Handbook of Prepared Inorganic Chemistry", but its existing synthesis device is relatively Complicated, it is difficult to precisely prepare raw materials, the preparation speed is slow, the amount of synthesis is small, in-situ drying cannot be achieved, and the requirements for high-temperature vacuum drying ovens are extremely high, etc.

Method used

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  • Preparation method of inorganic compound sodium selenide and device of preparation method
  • Preparation method of inorganic compound sodium selenide and device of preparation method

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Embodiment 1

[0049] Such as figure 1 Shown, a kind of device that is used to prepare inorganic compound sodium selenide comprises spherical reactor 8, and the top of described reactor 8 is connected with main pipeline 4 by flange set 7; The top of described main pipeline 4 is respectively connected with The vacuum pump 12 is connected to the vacuum pipeline 1 for vacuuming and the nitrogen pipeline 2 and the ammonia pipeline 3 for feeding nitrogen and ammonia. The bottom of the main pipeline 4 is provided with a gyrotron 6; The bottoms are respectively located in the first cooling pool 9-1 and the second cooling pool 9-2 filled with cooling liquid; the bottom of the second cooling pool 9-2 is set on the magnetic stirrer 11. The main pipeline 4 is connected with a barometer 13, and the vacuum pipeline 1, the nitrogen pipeline 2 and the ammonia pipeline 3 are respectively provided with a first three-way piston 5-1, a second three-way piston 5-2, and a third three-way piston. Pistons 5-3. ...

Embodiment 2

[0054] The preparation method of inorganic compound sodium selenide comprises the following steps:

[0055] (1) In a vacuum glove box filled with high-purity argon protection, metal sodium and elemental selenium are put into the reactor with a molar ratio of 2:1, and polytetrafluoroethylene magnets are added at the same time, and then the reaction The device is sealed and removed from the vacuum glove box;

[0056] (2) Evacuate the reactor to a high vacuum, then fill it with high-purity nitrogen, and then evacuate to a high vacuum, repeat high vacuum, nitrogen cleaning, and high vacuum three times;

[0057] (3) Immerse the reactor in a cooling pool equipped with dry ice acetone solution, and then feed liquid ammonia into the reactor to completely dissolve the sodium metal in the liquid ammonia;

[0058] (4) Pass high-purity nitrogen into the reactor to discharge the gasified ammonia in the reactor;

[0059] (5) Use a magnetic stirrer to stir the mixed solution in the reactor...

Embodiment 3

[0065] The preparation method of inorganic compound sodium selenide comprises the following steps:

[0066] (1) In a vacuum glove box filled with high-purity argon protection, metal sodium and elemental selenium are put into the reactor with a molar ratio of 2:1, and polytetrafluoroethylene magnets are added at the same time, and then the reaction The device is sealed and removed from the vacuum glove box;

[0067] (2) Evacuate the reactor to a high vacuum, then fill it with high-purity nitrogen, and then evacuate it to a high vacuum, repeat high vacuum pumping, nitrogen cleaning, and high vacuum pumping 4 times;

[0068] (3) Immerse the reactor in a cooling pool filled with liquid nitrogen and ethanol mixed solution, and then feed liquid ammonia into the reactor to completely dissolve the metal sodium in the liquid ammonia;

[0069] (4) Pass high-purity nitrogen into the reactor to discharge the gasified ammonia in the reactor;

[0070] (5) Use a magnetic stirrer to stir th...

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Abstract

The invention discloses a preparation method of an inorganic compound sodium selenide and a device of the preparation method. The preparation method comprises the steps of: (1) putting metallic sodium and elemental selenium in a reactor in a vacuum glove box, (2) highly vacuumizing, charging nitrogen to, cleaning and highly vacuumizing the reactor repeatedly for 3-4 times, (3) charging liquid ammonia to allow metallic sodium to be completely dissolved in liquid ammonia, (4) discharging gasified ammonia from the reactor via high-purity nitrogen, (5) stirring, (6) after gasifying liquid ammonia, vacuumizing the reactor, and (7) heating the reactor, then cooling to the room temperature, and taking a material to obtain a sodium selenide finished product. According to the preparation method, metallic Na and elemental Se are isolated from air all the time from a proportioning stage to a combination reaction course, and the purity of raw materials and synthesized sodium selenide and the safety in a reaction course are effectively ensured. At the same time, the device realizes a complete preparation technical flow of sodium selenide synthesis, ammonia volatilization, in situ synthesized polycrystal drying and the like.

Description

[0001] Technical field: [0002] The invention relates to the field of inorganic compound synthesis, in particular to a method for preparing the inorganic compound sodium selenide and a device thereof. [0003] Background technique: [0004] When a laser with a certain polarization direction enters a non-centrosymmetric crystal in a specific direction, the incident laser frequency will change, and the crystal with this nonlinear optical effect is called a nonlinear crystal. Using nonlinear crystals to realize nonlinear processes such as frequency doubling (SHG), sum frequency (SFG), difference frequency (DFG), and optical parametric oscillation (OPO) can expand existing laser wavelengths and output deep ultraviolet, visible, infrared, etc. Lasers with important value in national defense security, national economy and other fields. In recent years, with the rapid growth of the demand for mid- and long-wave infrared lasers in the fields of national defense, environment, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04
Inventor 王振友吴海信程旭东肖瑞春黄昌保倪友保毛明生
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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