CN112142015A - High-purity hydrogen selenide purification process using carbon nano tube - Google Patents
High-purity hydrogen selenide purification process using carbon nano tube Download PDFInfo
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- CN112142015A CN112142015A CN202011057821.0A CN202011057821A CN112142015A CN 112142015 A CN112142015 A CN 112142015A CN 202011057821 A CN202011057821 A CN 202011057821A CN 112142015 A CN112142015 A CN 112142015A
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Abstract
The invention discloses a high-purity hydrogen selenide purification process by utilizing carbon nano tubes, which comprises the following steps: s1, introducing the hydrogen selenide raw material into a primary rectifying tower in a liquid state, and carrying out primary rectification; s2, introducing the hydrogen selenide material subjected to the primary rectification in the step S1 into a secondary rectification tower for secondary rectification; s3, enabling the hydrogen selenide material subjected to secondary rectification in the step S2 to pass through an adsorption column in a gaseous state, and filling a mixture of carbon nanotubes and activated carbon in the adsorption column for adsorption treatment; and S4, pressurizing the hydrogen selenide material subjected to adsorption treatment in the step S3 to 1.5Mpa through pressurization treatment of a compressor, cooling to-10 ℃, cooling, liquefying and storing the hydrogen selenide material in a storage tank, and finally filling the hydrogen selenide material by using a filling pipeline. The process realizes the separation of hydrogen selenide and hydrogen sulfide by regulating the pipe diameter of the carbon nano tube, and can obtain high-purity hydrogen selenide materials.
Description
Technical Field
The invention relates to the technical field of hydrogen selenide purification, in particular to a high-purity hydrogen selenide purification process by utilizing carbon nano tubes.
Background
Solar energy is inexhaustible as a renewable energy source, and a photovoltaic technology of converting solar energy into electric energy is widely used as a way of obtaining and using solar energy. In the years 2000-2016, the global accumulated installed capacity is dramatically increased from 1250MW to 304300MW, and under the trend that the global greenhouse effect is more and more serious, the growth potential of the solar photovoltaic industry is huge.
Electronic grade hydrogen selenide is used as a key basic raw material for preparing a key CIGS light absorption layer in a solar cell, and has an irreplaceable effect in an inorganic solar thin film cell. In the preparation process of the solar cell, sulfur element is used as a few semiconductor doping reagents, and the introduction of the sulfur element can cause the change of the semiconductor energy gap of the CIGS light absorption layer, thereby greatly influencing the photoelectric conversion efficiency of the material.
In the production process of electronic grade hydrogen selenide, a small amount of hydrogen sulfide is generated. A difficulty in the purification of electronic grade hydrogen selenide is the removal of small amounts of hydrogen sulfide impurities formed from sulfur in the starting materials of the preparation. The property of hydrogen sulfide is close to that of hydrogen selenide, and the hydrogen sulfide is difficult to be removed to below 10ppm by a conventional rectification method. When the traditional hydrogen sulfide adsorbent is used for adsorption, the reaction activity of hydrogen selenide is greater than that of hydrogen sulfide, so that the traditional adsorption material can preferentially adsorb the hydrogen selenide, and the traditional hydrogen sulfide adsorbent is inactivated under the condition. How to obtain high-purity hydrogen selenide becomes a technical problem to be solved by the application.
Disclosure of Invention
The invention aims to: provides a high-purity hydrogen selenide purification process by utilizing carbon nano tubes, which aims to solve the problems in the background technology.
The technical scheme of the invention is as follows: a high-purity hydrogen selenide purification process utilizing carbon nano tubes comprises the following steps:
s1, introducing the hydrogen selenide raw material into a primary rectifying tower in a liquid state, and carrying out primary rectification; removal of CS from the feedstock2、SO2、H2Heavy component impurities such as O;
s2, introducing the hydrogen selenide material subjected to the primary rectification in the step S1 into a secondary rectification tower for secondary rectification; removing light component impurities such as oxygen, nitrogen, carbon dioxide, methane and the like in the material;
s3, enabling the hydrogen selenide material subjected to secondary rectification in the step S2 to pass through an adsorption column in a gaseous state, and filling a mixture of carbon nanotubes and activated carbon in the adsorption column for adsorption treatment; hydrogen sulfide is absorbed by the aperture of the carbon nano tube, and the purpose of adding the activated carbon is mainly to reduce the pressure drop of gas passing through the adsorption column;
and S4, pressurizing the hydrogen selenide material subjected to adsorption treatment in the step S3 to 1.5Mpa through pressurization treatment of a compressor, cooling to-10 ℃, cooling, liquefying and storing the hydrogen selenide material in a storage tank, and finally filling the hydrogen selenide material by using a filling pipeline.
As a further scheme of the present invention, the operating conditions of the preliminary distillation in the step S1 are: the internal pressure is 0.1-2 MPa, the temperature is-10 ℃, and the reflux ratio is 5: 1.
As a further aspect of the present invention, the operating conditions of the secondary rectification in step S2 are: the internal pressure is 0.5-2 MPa, the temperature is-15 ℃, and the reflux ratio is 9: 1.
According to a further scheme of the invention, the mass ratio of the carbon nanotubes filled in the adsorption column in the step S3 to the activated carbon is 1: 1-10.
As a further scheme of the present invention, in the step S3, the inner diameter of the carbon nanotube is 1-15 nm, the outer diameter of the carbon nanotube is 5-40 nm, and the length of the carbon nanotube is 10-30 μm.
As a further aspect of the present invention, the operating conditions of the adsorption process in step S3 are: the internal pressure is 0.1-1 MPa, the temperature is 50 ℃, and the airspeed is 50-3000 h-1。
The invention has the advantages that: the molecular radius of hydrogen sulfide is 134pm, the molecular radius of hydrogen selenide is 146pm, the separation of hydrogen selenide and hydrogen sulfide is realized by regulating and controlling the pipe diameter of the carbon nano tube, hydrogen sulfide with smaller molecular radius can easily enter the inside of the carbon nano tube, and a large amount of hydrogen selenide molecules are outside the carbon nano tube, so that the deep separation of hydrogen selenide and hydrogen sulfide is realized; the pressure drop of gas passing through the adsorption column can be reduced by adding the activated carbon, and the purification effect is improved.
Drawings
The invention is further described with reference to the following figures and examples:
fig. 1 is a schematic flow chart of a process for purifying high-purity hydrogen selenide by using carbon nanotubes.
Detailed Description
Example 1:
a high-purity hydrogen selenide purification process utilizing carbon nano tubes comprises the following steps:
s1, introducing the hydrogen selenide raw material into a primary rectifying tower in a liquid state, and carrying out primary rectification;
s2, introducing the hydrogen selenide material subjected to the primary rectification in the step S1 into a secondary rectification tower for secondary rectification;
s3, enabling the hydrogen selenide material subjected to secondary rectification in the step S2 to pass through an adsorption column in a gaseous state, and filling a mixture of carbon nanotubes and activated carbon in the adsorption column for adsorption treatment;
and S4, pressurizing the hydrogen selenide material subjected to adsorption treatment in the step S3 to 1.5Mpa through pressurization treatment of a compressor, cooling to-10 ℃, cooling, liquefying and storing the hydrogen selenide material in a storage tank, and finally filling the hydrogen selenide material by using a filling pipeline.
Wherein, the working conditions of the preliminary distillation in the step S1 are as follows: the internal pressure is 0.1-0.6 MPa, the temperature is-10 ℃, and the reflux ratio is 5: 1. The working conditions of the secondary rectification in the step S2 are as follows: the internal pressure is 0.5-2 MPa, the temperature is-15 ℃, and the reflux ratio is 9: 1.
The mass ratio of the carbon nanotubes filled in the adsorption column in the step S3 to the activated carbon is 1: 1. In the step S3, the inner diameter of the carbon nano tube is 1-15 nm, the outer diameter of the carbon nano tube is 5-40 nm, and the length of the carbon nano tube is 10-30 microns. The operating conditions of the adsorption process in step S3 are: the internal pressure is 0.1-0.3 MPa, the temperature is 50 ℃, and the airspeed is 50-1100 h-1。
Example 2:
a high-purity hydrogen selenide purification process utilizing carbon nano tubes comprises the following steps:
s1, introducing the hydrogen selenide raw material into a primary rectifying tower in a liquid state, and carrying out primary rectification;
s2, introducing the hydrogen selenide material subjected to the primary rectification in the step S1 into a secondary rectification tower for secondary rectification;
s3, enabling the hydrogen selenide material subjected to secondary rectification in the step S2 to pass through an adsorption column in a gaseous state, and filling a mixture of carbon nanotubes and activated carbon in the adsorption column for adsorption treatment;
and S4, pressurizing the hydrogen selenide material subjected to adsorption treatment in the step S3 to 1.5Mpa through pressurization treatment of a compressor, cooling to-10 ℃, cooling, liquefying and storing the hydrogen selenide material in a storage tank, and finally filling the hydrogen selenide material by using a filling pipeline.
Wherein, the working conditions of the preliminary distillation in the step S1 are as follows: the internal pressure is 0.6-1.3 MPa, the temperature is-10 ℃, and the reflux ratio is 5: 1. The working conditions of the secondary rectification in the step S2 are as follows: the internal pressure is 0.5-2 MPa, the temperature is-15 ℃, and the reflux ratio is 9: 1.
The mass ratio of the carbon nanotubes filled in the adsorption column in the step S3 to the activated carbon is 1: 4. In the step S3, the inner diameter of the carbon nano tube is 1-15 nm, the outer diameter of the carbon nano tube is 5-40 nm, and the length of the carbon nano tube is 10-30 microns. The operating conditions of the adsorption process in step S3 are: the internal pressure is 0.3-0.7 MPa, the temperature is 50 ℃, and the airspeed is 1100-2300 h-1。
Example 3:
a high-purity hydrogen selenide purification process utilizing carbon nano tubes comprises the following steps:
s1, introducing the hydrogen selenide raw material into a primary rectifying tower in a liquid state, and carrying out primary rectification;
s2, introducing the hydrogen selenide material subjected to the primary rectification in the step S1 into a secondary rectification tower for secondary rectification;
s3, enabling the hydrogen selenide material subjected to secondary rectification in the step S2 to pass through an adsorption column in a gaseous state, and filling a mixture of carbon nanotubes and activated carbon in the adsorption column for adsorption treatment;
and S4, pressurizing the hydrogen selenide material subjected to adsorption treatment in the step S3 to 1.5Mpa through pressurization treatment of a compressor, cooling to-10 ℃, cooling, liquefying and storing the hydrogen selenide material in a storage tank, and finally filling the hydrogen selenide material by using a filling pipeline.
Wherein, the working conditions of the preliminary distillation in the step S1 are as follows: the internal pressure is 1.3-2 MPa, the temperature is-10 ℃, and the reflux ratio is 5: 1. The working conditions of the secondary rectification in the step S2 are as follows: the internal pressure is 0.5-2 MPa, the temperature is-15 ℃, and the reflux ratio is 9: 1.
The mass ratio of the carbon nanotubes filled in the adsorption column in the step S3 to the activated carbon is 1: 10. In the step S3, the inner diameter of the carbon nano tube is 1-15 nm, the outer diameter of the carbon nano tube is 5-40 nm, and the length of the carbon nano tube is 10-30 microns. The operating conditions of the adsorption process in step S3 are: the internal pressure is 0.7-1 MPa, the temperature is 50 ℃, and the airspeed is 2300-3000 h-1。
The performance of the hydrogen selenide material products purified by the process methods of the embodiments 1 to 3 is tested, and the final results all conform to the parameters of the following table 1.
Table 1: hydrogen selenide material product final performance table
| Total purity of | 5N |
| Carbon dioxide | <1ppm |
| Hydrogen sulfide | <1ppm |
| Nitrogen gas | <5ppm |
| Oxygen gas | <1ppm |
| Methane | <1ppm |
| Water (W) | <1ppm |
It should be understood that the above-mentioned embodiments are only illustrative of the technical concepts and features of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All modifications made according to the spirit of the main technical scheme of the invention are covered in the protection scope of the invention.
Claims (6)
1. A high-purity hydrogen selenide purification process by utilizing carbon nano tubes is characterized in that: the method comprises the following steps:
s1, introducing the hydrogen selenide raw material into a primary rectifying tower in a liquid state, and carrying out primary rectification;
s2, introducing the hydrogen selenide material subjected to the primary rectification in the step S1 into a secondary rectification tower for secondary rectification;
s3, enabling the hydrogen selenide material subjected to secondary rectification in the step S2 to pass through an adsorption column in a gaseous state, and filling a mixture of carbon nanotubes and activated carbon in the adsorption column for adsorption treatment;
and S4, pressurizing the hydrogen selenide material subjected to adsorption treatment in the step S3 to 1.5Mpa through pressurization treatment of a compressor, cooling to-10 ℃, cooling, liquefying and storing the hydrogen selenide material in a storage tank, and finally filling the hydrogen selenide material by using a filling pipeline.
2. The process of claim 1, wherein the carbon nanotubes are used for purifying hydrogen selenide, and the process comprises the following steps: the working conditions of the preliminary distillation in the step S1 are as follows: the internal pressure is 0.1-2 MPa, the temperature is-10 ℃, and the reflux ratio is 5: 1.
3. The process of claim 1, wherein the carbon nanotubes are used for purifying hydrogen selenide, and the process comprises the following steps: the working conditions of the secondary rectification in the step S2 are as follows: the internal pressure is 0.5-2 MPa, the temperature is-15 ℃, and the reflux ratio is 9: 1.
4. the process of claim 1, wherein the carbon nanotubes are used for purifying hydrogen selenide, and the process comprises the following steps: the mass ratio of the carbon nanotubes filled in the adsorption column in the step S3 to the activated carbon is 1: 1-10.
5. The process of claim 1, wherein the carbon nanotubes are used for purifying hydrogen selenide, and the process comprises the following steps: in the step S3, the inner diameter of the carbon nano tube is 1-15 nm, the outer diameter of the carbon nano tube is 5-40 nm, and the length of the carbon nano tube is 10-30 microns.
6. The process of claim 1, wherein the carbon nanotubes are used for purifying hydrogen selenide, and the process comprises the following steps: the operating conditions of the adsorption process in step S3 are: the internal pressure is 0.1-1 MPa, the temperature is 50 ℃, and the airspeed is 50-3000 h-1。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113816346A (en) * | 2021-08-30 | 2021-12-21 | 苏州金宏气体股份有限公司 | Process for purifying hydrogen selenide by using modified metal organic framework |
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