CN113772634A - Preparation method of 5N high-purity selenium granules - Google Patents
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- CN113772634A CN113772634A CN202111083280.3A CN202111083280A CN113772634A CN 113772634 A CN113772634 A CN 113772634A CN 202111083280 A CN202111083280 A CN 202111083280A CN 113772634 A CN113772634 A CN 113772634A
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- C01B19/02—Elemental selenium or tellurium
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Abstract
The invention provides a preparation method of 5N high-purity selenium granules, and relates to the technical field of metallurgy. The preparation method of the 5N high-purity selenium particles provided by the invention comprises the following steps: (1) placing a selenium block with the purity of 4N as a raw material in a quartz tube of a quartz distillation furnace, and vacuumizing the tube; (2) controlling the temperature of the upper section of the quartz tube at 280-; (3) adjusting the temperature of the upper section of the quartz tube to 200-260 ℃ and the temperature of the lower section to 220-280 ℃ to obtain molten selenium liquid; (4) and transferring the molten selenium liquid into a granulating furnace for heating, stirring, dredging slag, cooling and granulating to obtain the 5N high-purity selenium granules. According to the invention, the 5N high-purity selenium particles are prepared by adopting a pyrometallurgy method, and in the preparation steps, the target impurity content can be effectively controlled by strictly controlling the distillation temperature, so that the prepared 5N high-purity selenium particles have low impurity content, and the requirement of preparing infrared chalcogenide glass at downstream can be met.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a preparation method of 5N high-purity selenium particles.
Background
With the development of aerospace science and technology and infrared technology application, the requirements on the performance of infrared optical materials are higher and higher. On one hand, the high-end infrared optical system needs to work in a wider wave band, such as a forward-looking infrared thermal imaging system, a night vision system, infrared guidance and the like, and the used infrared optical material needs to have good light transmittance in the wave band ranges of 3-5 microns and 8-12 microns; on the other hand, in modern military and space technologies, the service environment of infrared light elements becomes more and more demanding, for example, optical window materials of high-speed flight objects will be subjected to severe tests of high temperature, high pressure, thermal shock, impact of solid particles and raindrops in the atmosphere, and the infrared optical materials need to have better mechanical and thermal properties and environmental adaptability.
The infrared chalcogenide glass is a multi-component compound glass formed by combining three oxygen group elements of sulfur, selenium and tellurium and other glass network bodies (such as arsenic, antimony, germanium and the like). Chalcogenide glass has excellent middle and far infrared transmission performance, good thermal stability and chemical stability, and higher nonlinear refractive index coefficient and refractive index, is one of the more ideal infrared optical materials at present, and is considered as a core material of a new-generation temperature self-adaptive infrared optical system. The infrared imaging system has wide application prospect in the fields of military infrared detection, infrared imaging guidance, civil vehicle-mounted night vision, interstellar life detection, other top infrared thermal imaging optical systems and the like.
Selenium is one of main elements for preparing infrared chalcogenide glass, the quality of selenium has great influence on the preparation of the infrared chalcogenide glass, such as the yield of demoulding and annealing, internal impurity points, internal stripes, transmittance and the like, the chalcogenide glass requires that the contents of carbon, oxygen and moisture are all less than 5ppm, but the impurity components of the currently produced 5N high-purity selenium grain product are difficult to meet the requirements of downstream chalcogenide glass application.
Disclosure of Invention
The invention mainly aims to provide a preparation method of 5N high-purity selenium particles, and aims to control the contents of metal impurities, carbon and oxygen in the selenium particles by a pyrometallurgical method so as to prepare the high-purity selenium particles meeting the requirements of the field of chalcogenide glass.
In order to achieve the above object, in a first aspect, the present invention provides a method for preparing 5N high-purity selenium granules, comprising the following steps:
(1) placing a selenium block with the purity of 4N as a raw material in a quartz tube of a quartz distillation furnace, and vacuumizing the tube;
(2) controlling the temperature of the upper section of the quartz tube at 280-;
(3) adjusting the temperature of the upper section of the quartz tube to 200-260 ℃ and the temperature of the lower section to 220-280 ℃ to obtain molten selenium liquid;
(4) and transferring the molten selenium liquid into a granulating furnace for heating, stirring, dredging slag, cooling and granulating to obtain the 5N high-purity selenium granules.
According to the technical scheme, the 4N selenium block is sequentially subjected to heat preservation distillation in a quartz distillation furnace and heated and granulated in a granulating smelting furnace, and the specific device structure is the application of the patent (application number 200610122508.4), wherein in the step (1), the selenium block is placed in a quartz tube of the quartz distillation furnace, a quartz tower head is installed, a quartz distillation furnace cover and a gasket are cleaned, and the quartz distillation furnace cover is covered; in the step (2), the 4N selenium blocks are heated and evaporated at the upper end of the quartz tube, selenium steam is condensed and then enters the lower section of the quartz tube, the temperature of the upper section and the lower section of the quartz tube is adjusted after the heat preservation and distillation are continued for a period of time, and the temperature is reduced and the quartz tube is discharged; and (4) transferring the selenium liquid to a granulating furnace for granulation to obtain 5N high-purity selenium granules.
(selenium is melted by heating, and the evaporation temperature of selenium is reduced by vacuum to achieve the effect of separating selenium from impurities)
According to the invention, the 5N high-purity selenium particles are prepared by adopting a pyrometallurgy method, and in the preparation steps, the target impurity content can be effectively controlled by strictly controlling the distillation temperature, so that the prepared 5N high-purity selenium particles have low impurity content, and the requirement of preparing infrared chalcogenide glass at downstream can be met.
As a preferred embodiment of the preparation method of the 5N high-purity selenium granules, the granulation furnace in the step (4) is divided into an upper section, a middle section and a lower section for controlling the temperature, and the heating process is divided into two stages, wherein the temperature of the upper section, the middle section and the lower section of the furnace is controlled to be 280-shaped and 360 ℃, and the temperature of the upper section, the middle section and the lower section of the furnace is controlled to be 200-shaped and 250 ℃ in the second stage.
(in the granulation, because the heating mode of the granulation furnace is heating from the periphery to the inside, the actual temperature of the selenium melt is above the melting point, so the heating temperature needs to be set to 280-360 ℃, and the selenium is kept in the molten state, thereby ensuring the normal granulation.
As a preferred embodiment of the method for preparing 5N high-purity selenium granules according to the present invention, the cooling granulation in the step (4) comprises the following steps: and putting the granulating funnel into a heating sleeve device, controlling the temperature of the heating sleeve to be 200-250 ℃, and starting a granulating water tank to cool pure water for casting and granulating.
In the technical scheme of the invention, pure water is adopted for extreme cooling during granulation, so that the selenium solution can be rapidly cooled and formed, the introduction of oxygen element oxide and other metal elements in the selenium granules can be prevented, and finally the 5N high-purity selenium granules with low carbon, low oxygen and low impurities are obtained.
As a preferred embodiment of the method for preparing 5N high-purity selenium particles according to the present invention, in the step (1), vacuum is applied until the degree of vacuum in the quartz tube is not higher than 10 Pa.
The invention can reduce the evaporation temperature of selenium by vacuumizing, thereby achieving the effect of separating selenium from impurities.
As a preferred embodiment of the preparation method of the 5N high-purity selenium granules, the heat preservation and distillation time in the step (2) is 18-36 h.
In the technical scheme of the invention, the heat preservation distillation time is strictly controlled, and the residual metal impurities in the 4N selenium block can be effectively removed.
As a preferred embodiment of the method for preparing 5N high-purity selenium granules, the molten selenium liquid in step (4) is transferred by using a stainless steel disc; the granulating smelting furnace and the granulating funnel in the step (4) are made of quartz materials; and (4) stirring and fishing the slag by adopting a quartz rod.
Devices (such as a distillation furnace, a granulating funnel, a quartz rod and the like) which are required to be contacted with the selenium in the whole process of the preparation method disclosed by the invention are made of quartz materials, and meanwhile, molten selenium liquid is transferred by adopting a stainless steel disc, so that the introduction of a carbon source can be avoided, and the purity of selenium particles is ensured.
As a preferred embodiment of the preparation method of the 5N high-purity selenium granules, after the casting granulation in the step (4), the selenium granules are placed in a stainless steel sieve for draining, and are heated and dried by hot air at 40 ℃ for 18-24h to obtain the 5N high-purity selenium granules.
In a second aspect, the invention also provides application of the 5N high-purity selenium particles in preparation of infrared chalcogenide glass.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts a pyrometallurgical method to prepare 5N high-purity selenium granules, the equipment adopted in the production process is simple to operate, the safety coefficient is higher, the target impurity content can be effectively controlled, the prepared selenium granules have lower impurity content, the product quality is stable, and the requirements of downstream preparation of infrared chalcogenide glass can be met.
Drawings
FIG. 1 is a schematic diagram of a process for preparing 5N high-purity selenium granules according to an embodiment of the present invention.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
The preparation process of the 5N high-purity selenium granules of the embodiment is shown in fig. 1, and the specific preparation method comprises the following steps:
(1) taking a selenium block with the purity of 4N as a raw material, putting 8kg of the 4N selenium block into a quartz tube in a quartz distillation furnace, cleaning a quartz distillation furnace cover and a gasket, installing a quartz tower head, covering the quartz distillation furnace cover, and starting a vacuum pump to pump the vacuum degree in the quartz tube to be below 10 Pa;
(2) controlling the temperature of the upper section of the quartz tube to be 280 ℃ and the temperature of the lower section of the quartz tube to be 240 ℃, and carrying out heat preservation distillation for 18 h;
(3) after the heat preservation is finished, the temperature of the upper section of the quartz tube is adjusted to be 200 ℃, and the temperature of the lower section of the quartz tube is adjusted to be 220 ℃, so that molten selenium liquid is obtained;
(4) after the temperature is stable, transferring the selenium solution in the furnace into a granulating smelting furnace by using a stainless steel disc for heating, controlling the temperatures of the upper section, the middle section and the lower section of the granulating smelting furnace to be 280 ℃ in the first stage, and completely melting; in the second stage, the temperature of the upper section, the middle section and the lower section of the granulating smelting furnace are controlled to be 200 ℃, a clean quartz rod is used for stirring and fishing slag, a granulating funnel is placed into a heating sleeve device, the temperature of the heating sleeve device is controlled to be 200 ℃, and a granulating water tank is opened to take cooling pure water for casting and granulating;
(5) and (3) catching the selenium particles by using a stainless steel screen mesh, draining the water, putting the drained selenium particles into a hot air circulation oven tray, controlling the temperature to be 40 ℃, and performing heat preservation and drying for 20 hours to obtain the 5N high-purity selenium particles.
Example 2
The preparation process of the 5N high-purity selenium granules of the embodiment is shown in fig. 1, and the specific preparation method comprises the following steps:
(1) taking a selenium block with the purity of 4N as a raw material, putting 8kg of the 4N selenium block into a quartz tube in a quartz distillation furnace, cleaning a quartz distillation furnace cover and a gasket, installing a quartz tower head, covering the quartz distillation furnace cover, and starting a vacuum pump to pump the vacuum degree in the quartz tube to be below 10 Pa;
(2) controlling the temperature of the upper section of the quartz tube to be 300 ℃ and the temperature of the lower section of the quartz tube to be 250 ℃, and carrying out heat preservation distillation for 18 h;
(3) after the heat preservation is finished, the temperature of the upper section of the quartz tube is adjusted to 230 ℃, and the temperature of the lower section of the quartz tube is adjusted to 250 ℃, so that molten selenium liquid is obtained;
(4) after the temperature is stable, transferring the selenium solution in the furnace into a granulating smelting furnace by using a stainless steel disc for heating, controlling the temperatures of the upper section, the middle section and the lower section of the granulating smelting furnace to be 320 ℃ in the first stage, and completely melting; in the second stage, the temperature of the upper section, the middle section and the lower section of the granulating smelting furnace are controlled to be 220 ℃, a clean quartz rod is used for stirring and fishing slag, a granulating funnel is placed into a heating sleeve device, the temperature of the heating sleeve device is controlled to be 220 ℃, and a granulating water tank is opened to take cooling pure water for casting and granulating;
(5) and (3) catching the selenium particles by using a stainless steel screen mesh, draining the water, putting the drained selenium particles into a hot air circulation oven tray, controlling the temperature to be 40 ℃, and performing heat preservation and drying for 20 hours to obtain the 5N high-purity selenium particles.
Example 3
The preparation process of the 5N high-purity selenium granules of the embodiment is shown in fig. 1, and the specific preparation method comprises the following steps:
(1) taking a selenium block with the purity of 4N as a raw material, putting 8kg of the 4N selenium block into a quartz tube in a quartz distillation furnace, cleaning a quartz distillation furnace cover and a gasket, installing a quartz tower head, covering the quartz distillation furnace cover, and starting a vacuum pump to pump the vacuum degree in the quartz tube to be below 10 Pa;
(2) controlling the temperature of the upper section of the quartz tube to be 360 ℃ and the temperature of the lower section of the quartz tube to be 260 ℃, and carrying out heat preservation distillation for 18 h;
(3) after the heat preservation is finished, adjusting the temperature of the upper section of the quartz tube to be 260 ℃ and the temperature of the lower section of the quartz tube to be 280 ℃ to obtain molten selenium liquid;
(4) after the temperature is stable, transferring the selenium solution in the furnace into a granulating smelting furnace by using a stainless steel disc for heating, controlling the temperature of the upper section, the middle section and the lower section of the granulating smelting furnace to be 360 ℃ in the first stage, and completely melting; in the second stage, the temperature of the upper section, the middle section and the lower section of the granulating smelting furnace are controlled to be 250 ℃, a clean quartz rod is used for stirring and fishing slag, a granulating funnel is placed into a heating sleeve device, the temperature of the heating sleeve device is controlled to be 250 ℃, and a granulating water tank is opened to take cooling pure water for casting and granulating;
(5) and (3) catching the selenium particles by using a stainless steel screen mesh, draining the water, putting the drained selenium particles into a hot air circulation oven tray, controlling the temperature to be 40 ℃, and performing heat preservation and drying for 20 hours to obtain the 5N high-purity selenium particles.
Comparative example 1
This comparative example was prepared in substantially the same manner as example 1, except that: in the step (2), the temperature of the upper section of the quartz tube is controlled to be 270 ℃, the temperature of the lower section of the quartz tube is controlled to be 260 ℃, the heat preservation distillation is carried out for 18h, and the vacuum degree is pumped to be below 10 Pa.
Comparative example 2
This comparative example was prepared in substantially the same manner as example 1, except that: and (4) after the heat preservation in the step (3) is finished, adjusting the temperature of the upper section of the quartz tube to be 290 ℃ and the temperature of the lower section of the quartz tube to be 250 ℃ to obtain the molten selenium liquid.
Comparative example 3
This comparative example was prepared in substantially the same manner as example 1, except that: in the first stage of the step (4), the temperatures of the upper section, the middle section and the lower section of the granulating smelting furnace are controlled to be 270 ℃, and the granulating smelting furnace is completely melted; in the second stage, the temperature of the upper section, the middle section and the lower section of the granulating smelting furnace are controlled to be 260 ℃.
Comparative example 4
This comparative example was prepared in substantially the same manner as example 1, except that: in the first stage of the step (4), the temperatures of the upper section, the middle section and the lower section of the granulating smelting furnace are controlled to be 380 ℃, and the granulating smelting furnace is completely melted; in the second stage, the temperature of the upper section, the middle section and the lower section of the granulating furnace are controlled to be 240 ℃.
Comparative example 5
This comparative example was prepared in substantially the same manner as example 1, except that: and (2) starting a vacuum pump in the step (1) to pump the vacuum degree in the quartz tube to 11 Pa.
Comparative example 6
This comparative example was prepared in substantially the same manner as example 1, except that: and (2) starting a vacuum pump in the step (1) to pump the vacuum degree in the quartz tube to 15 Pa.
Experimental example 1
Impurity elements and moisture contents of the selenium particles prepared in examples 1 to 3 and comparative examples 1 to 4 were measured, wherein metal impurity elements were measured by Agilent 7700x ICP-MS, element C was measured by a carbon sulfur instrument, moisture was measured by a coulometer, element O was measured by a chemical method, and the measurement results are shown in table 1 below.
TABLE 1 impurity test results of selenium pellets prepared in examples 1-3 and comparative examples 1-4
As can be seen from Table 1, the contents of each impurity in the high-purity selenium granules prepared in examples 1-3 are lower than the standard content, while the contents of C element in the selenium granules prepared in comparative examples 1-6 are significantly higher than those in examples 1-3, and the contents of the other impurity elements cannot be distinguished at present due to the detection limit of the corresponding detection equipment.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of 5N high-purity selenium particles is characterized by comprising the following steps:
(1) placing a selenium block with the purity of 4N as a raw material in a quartz tube of a quartz distillation furnace, and vacuumizing the tube;
(2) controlling the temperature of the upper section of the quartz tube at 280-;
(3) adjusting the temperature of the upper section of the quartz tube to 200-260 ℃ and the temperature of the lower section to 220-280 ℃ to obtain molten selenium liquid;
(4) and transferring the molten selenium liquid into a granulating furnace for heating, stirring, dredging slag, cooling and granulating to obtain the 5N high-purity selenium granules.
2. The method as claimed in claim 1, wherein the temperature of the granulating furnace in step (4) is controlled by an upper section, a middle section and a lower section, and the heating process is divided into two stages, wherein the temperature of the upper section, the middle section and the lower section of the furnace is controlled by 280-360 ℃ in the first stage, and the temperature of the upper section, the middle section and the lower section of the furnace is controlled by 200-250 ℃ in the second stage.
3. The method of claim 1, wherein the cooling granulation in the step (4) comprises the steps of: and putting the granulating funnel into a heating sleeve device, controlling the temperature of the heating sleeve to be 200-250 ℃, and starting a granulating water tank to cool pure water for casting and granulating.
4. The method according to claim 1, wherein in the step (1), the vacuum is applied until the degree of vacuum in the quartz tube is not higher than 10 Pa.
5. The method according to claim 1, wherein the distillation time in the step (2) is 18 to 36 hours.
6. The method according to claim 1, wherein the molten selenium solution in the step (4) is transferred using a stainless steel plate.
7. The method according to claim 3, wherein the granulating furnace and the granulating funnel in step (4) are made of quartz.
8. The preparation method according to claim 1, wherein the quartz rod is used for stirring and slag removal in the step (4).
9. The preparation method of claim 3, wherein after the casting granulation in the step (4), the selenium granules are placed in a stainless steel sieve for draining, and are subjected to heat preservation and drying at 40 ℃ for 18-24h to obtain the 5N high-purity selenium granules.
10. Use of the 5N high purity selenium granulate prepared by the method of preparing 5N high purity selenium granulate of any of claims 1 to 9 in the preparation of infrared chalcogenide glass.
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