CN106904581A - The preparation method of hydrogen selenide - Google Patents
The preparation method of hydrogen selenide Download PDFInfo
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- CN106904581A CN106904581A CN201710244129.0A CN201710244129A CN106904581A CN 106904581 A CN106904581 A CN 106904581A CN 201710244129 A CN201710244129 A CN 201710244129A CN 106904581 A CN106904581 A CN 106904581A
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- hydrogen
- selenizing
- selenium
- selenide
- hydrogen selenide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/04—Binary compounds including binary selenium-tellurium compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention relates to a kind of preparation method of hydrogen selenide, comprise the following steps：S1：The selenium raw material of sulfur-bearing is added in reacting furnace；S2：Hydrogen after heating is passed into reacting furnace；S3：Selenium generates hydrogen selenide with hydrogen chemical combination under heating condition in reacting furnace, and hydrogen selenide is mixed into gaseous mixture；S4：Go out the gaseous mixture of reacting furnace through cooling, and isolate selenium steam；S5：Gaseous mixture after cooling is in condenser inner condensat liquid；S6：When 5 15% selenium raw material is consumed, liquefied hydrogen selenide is carried out to fill collection；S7：Continue to react, when 40% 60% selenium raw material is consumed, liquefied hydrogen selenide is carried out to fill collection；S8：Continue to react, when 85% 95% selenium raw material is consumed, liquefied hydrogen selenide is carried out to fill collection；S9：Repeat S2 S8 operations.The preparation method of hydrogen selenide of the present invention obtains the selenizing hydrogen production of hydrogen sulfide content different size by way of Fractional Collections, meets the different demands of different clients.
Description
Technical field
The present invention relates to a kind of preparation field of hydrogen selenide, more particularly to a kind of preparation method of hydrogen selenide.
Background technology
Hydrogen selenide is the important source material for making Infrared Material Zinc Selenide eyeglass and preparing other metal selenides, is still used for
The raw material of solar cell, the extension, ion implanting and doping of semiconductor and IC production.With selenium and hydrogen as raw material
In the technique of direct chemical combination generation hydrogen selenide, because the sulfur impurity in selenium equally can generate hydrogen sulfide with hydrogen reaction, it is blended in
In hydrogen selenide, it is difficult to remove, therefore, sulphur turns into the difficult impurity for removing in hydrogen selenide.In the prior art, general use removes in advance
The method of sulfur impurity solves the above problems, however, the program of do so is complex, can also be readily incorporated other problems (such as
Block), and sulfur impurity is not divisible, and expense is high.
Thus, it is necessary to design a kind of preparation method of new hydrogen selenide to solve above-mentioned technical problem.
The content of the invention
Object of the present invention is to provide a kind of preparation method of hydrogen selenide.
To realize object defined above, the present invention is adopted the following technical scheme that：A kind of preparation method of hydrogen selenide, including following step
Suddenly：
S1：Using charging device, the selenium raw material of sulfur-bearing 0.1-100ppm is added in reacting furnace；
S2：Path is passed through using hydrogen, the hydrogen after heating is passed into reacting furnace；
S3：Selenium generates hydrogen selenide with hydrogen chemical combination under heating condition in reacting furnace, and hydrogen selenide is mixed into gaseous mixture；
S4：Go out the gaseous mixture of reacting furnace through cooling, and isolate selenium steam；
S5：Gaseous mixture after cooling in condenser inner condensat liquid, uncollected hydrogen through recycle compressor be back to S2 with it is new
The hydrogen being passed through together participates in reaction；
S6：When the selenium raw material of 5-15% is consumed, liquefied hydrogen selenide in condenser is carried out filling collection, obtain first
Selenizing hydrogen production；
S7：Continue to react, when the selenium raw material of 40%-60% is consumed, liquefied hydrogen selenide in condenser is carried out filling receipts
Collection, obtains the second selenizing hydrogen production；
S8：Continue to react, when the selenium raw material of 85%-95% is consumed, liquefied hydrogen selenide in condenser is carried out filling receipts
Collection, obtains the 3rd selenizing hydrogen production；
S9：Before selenium runs out of in the reacting furnace, next group selenium raw material is added, repeat S2-S8 operations, continuous output hydrogen selenide is produced
Product.
As a further improvement on the present invention, the heating-up temperature in the S3 in reacting furnace is between 400-700 DEG C.
As a further improvement on the present invention, the S4 cools to 20-50 DEG C.
As a further improvement on the present invention, the temperature in the S5 in condenser is -40~-60 DEG C, in condenser
Pressure is 5-10 atmospheric pressure.
As a further improvement on the present invention, the content of hydrogen sulfide is higher than the second hydrogen selenide in the first selenizing hydrogen production
Product, the 3rd selenizing hydrogen production.
As a further improvement on the present invention, the content of hydrogen sulfide is higher than the 3rd hydrogen selenide in the second selenizing hydrogen production
Product.
As a further improvement on the present invention, repeatedly collection is filled also including hydrogen selenide between the S6-S8.
The preparation method of hydrogen selenide of the present invention obtains the selenizing of hydrogen sulfide content different size by way of Fractional Collections
Hydrogen production, meets the different demands of different clients, to carrying out a small amount of change on the preparation facilities of existing hydrogen selenide, reaches
Expected purpose.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described implementation
Example is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
A kind of preparation method of hydrogen selenide, comprises the following steps：
S1：Using charging device, the selenium raw material of sulfur-bearing 0.1-100ppm is added in reacting furnace；
S2：Path is passed through using hydrogen, the hydrogen after heating is passed into reacting furnace；
S3：Selenium generates hydrogen selenide with hydrogen chemical combination under heating condition in reacting furnace, and hydrogen selenide is mixed into gaseous mixture；
S4：Go out the gaseous mixture of reacting furnace through cooling, and isolate selenium steam；
S5：Gaseous mixture after cooling in condenser inner condensat liquid, uncollected hydrogen through recycle compressor be back to S2 with it is new
The hydrogen being passed through together participates in reaction；
S6：When the selenium raw material of 5-15% is consumed, liquefied hydrogen selenide in condenser is carried out filling collection, obtain first
Selenizing hydrogen production；
S7：Continue to react, when the selenium raw material of 40%-60% is consumed, liquefied hydrogen selenide in condenser is carried out filling receipts
Collection, obtains the second selenizing hydrogen production；
S8：Continue to react, when the selenium raw material of 85%-95% is consumed, liquefied hydrogen selenide in condenser is carried out filling receipts
Collection, obtains the 3rd selenizing hydrogen production；
S9：Before selenium runs out of in the reacting furnace, next group selenium raw material is added, repeat S2-S8 operations, continuous output hydrogen selenide is produced
Product.
In certain embodiments of the present invention, the heating-up temperature in S3 in reacting furnace is between 400-700 DEG C.
In certain embodiments of the present invention, S4 cools to 20-50 DEG C.
In certain embodiments of the present invention, the temperature in S5 in condenser is -40~-60 DEG C, the pressure in condenser
It is 5-10 atmospheric pressure.
In certain embodiments of the present invention, the content of hydrogen sulfide is higher than the second hydrogen selenide in the first selenizing hydrogen production
Product, the 3rd selenizing hydrogen production.
In certain embodiments of the present invention, the content of hydrogen sulfide is higher than the 3rd hydrogen selenide in the second selenizing hydrogen production
Product.
Embodiment 1.
In a selenium reacting furnace, using the selenium powder of charging device input 500kg sulfur-bearings 0.1ppm, sky is displaced with hydrogen
Gas, is added in hydrogen selenide reacting furnace after heating fusing.Reacting furnace is heated to 400 DEG C, is passed through hydrogen reaction.It is mixed that reaction is generated
Close air cooling and isolate selenium steam to 35 DEG C, entering back into the condenser that pressure is 8 atmospheric pressure, temperature is -50 DEG C makes selenizing
Hydrogen condensation liquefaction is simultaneously collected.Uncooled hydrogen is participated in by returning to reacting furnace after compressor boost together with the hydrogen being newly passed through
Reaction.When 10% selenium raw material is consumed, hydrogen selenide in condenser is carried out to fill collection for the first time, obtain the first selenizing
Hydrogen production.When 50% selenium raw material is consumed, collection is filled for the second time to hydrogen selenide in condenser, obtained the second selenium
Change hydrogen production.When 90% selenium raw material is consumed, third time is carried out to hydrogen selenide in condenser and fills collection, obtain the 3rd
Selenizing hydrogen production.Input next group raw material, repeats the above steps, continuous production.
Composition to the first resulting selenizing hydrogen production, the first selenizing hydrogen production, the 3rd selenizing hydrogen production is analyzed
Obtain the result of following table.
Embodiment 2.
In a selenium reacting furnace, using the selenium powder of charging device input 500kg sulfur-bearings 11ppm, sky is displaced with hydrogen
Gas, is added in hydrogen selenide reacting furnace after heating fusing.Reacting furnace is heated to 500 DEG C, is passed through hydrogen reaction.It is mixed that reaction is generated
Close air cooling and isolate selenium steam to 50 DEG C, entering back into the condenser that pressure is 10 atmospheric pressure, temperature is -50 DEG C makes selenizing
Liquefaction of hydrogen is collected.Uncooled hydrogen participates in reaction by returning to reacting furnace after compressor boost together with the hydrogen being newly passed through.
When 5% selenium raw material is consumed, hydrogen selenide in condenser is carried out to fill collection for the first time, obtain the first selenizing hydrogen production.
When 40% selenium raw material is consumed, collection is filled for the second time to hydrogen selenide in condenser, obtained the second hydrogen selenide product
Product.When 85% selenium raw material is consumed, third time is carried out to hydrogen selenide in condenser and fills collection, obtain the 3rd hydrogen selenide
Product.Input next group raw material, repeats the above steps, continuous production.
Composition to the first resulting selenizing hydrogen production, the first selenizing hydrogen production, the 3rd selenizing hydrogen production is analyzed
Obtain the result of following table.
Embodiment 3.
In a selenium reacting furnace, using the selenium powder of charging device input 500kg sulfur-bearings 100ppm, sky is displaced with hydrogen
Gas, is added in hydrogen selenide reacting furnace after heating fusing.Reacting furnace is heated to 700 DEG C, is passed through hydrogen reaction.It is mixed that reaction is generated
Close air cooling and isolate selenium steam to 20 DEG C, entering back into the condenser that pressure is 5 atmospheric pressure, temperature is -60 DEG C makes selenizing
Liquefaction of hydrogen is collected.Uncooled hydrogen participates in reaction by returning to reacting furnace after compressor boost together with the hydrogen being newly passed through.
When 15% selenium raw material is consumed, hydrogen selenide in condenser is carried out to fill collection for the first time, obtain the first hydrogen selenide product
Product.When 60% selenium raw material is consumed, collection is filled for the second time to hydrogen selenide in condenser, obtained the second hydrogen selenide
Product.When 95% selenium raw material is consumed, third time is carried out to hydrogen selenide in condenser and fills collection, obtain the 3rd selenizing
Hydrogen production.Input next group raw material, repeats the above steps, continuous production.
Composition to the first resulting selenizing hydrogen production, the first selenizing hydrogen production, the 3rd selenizing hydrogen production is analyzed
Obtain the result of following table.
Data obtained by analysis can be obtained, in the first selenizing hydrogen production the content of hydrogen sulfide really higher than the second selenizing hydrogen production,
3rd selenizing hydrogen production.The content of hydrogen sulfide is also higher than the 3rd selenizing hydrogen production really in second selenizing hydrogen production.Resulting
First selenizing hydrogen production, the second selenizing hydrogen production, the 3rd selenizing hydrogen production can meet the different demands of different clients.
The preparation method of hydrogen selenide of the present invention obtains the selenizing of hydrogen sulfide content different size by way of Fractional Collections
Hydrogen production, meets the different demands of different clients, to carrying out a small amount of change on the preparation facilities of existing hydrogen selenide, reaches
Expected purpose.
Although being example purpose, the preferred embodiment of the present invention, the ordinary skill people of this area are had been disclosed for
Member will be various to change, it is realized that in the case of scope and spirit of the present invention disclosed in not departing from by appending claims
It is possible for entering, increasing and replacing.
Claims (7)
1. a kind of preparation method of hydrogen selenide, it is characterised in that：Comprise the following steps：
S1：Using charging device, the selenium raw material of sulfur-bearing 0.1-100ppm is added in reacting furnace；
S2：Path is passed through using hydrogen, the hydrogen after heating is passed into reacting furnace；
S3：Selenium generates hydrogen selenide with hydrogen chemical combination under heating condition in reacting furnace, and hydrogen selenide is mixed into gaseous mixture；
S4：Go out the gaseous mixture of reacting furnace through cooling, and isolate selenium steam；
S5：Gaseous mixture after cooling in condenser inner condensat liquid, uncollected hydrogen through recycle compressor be back to S2 with it is new
The hydrogen being passed through together participates in reaction；
S6：When the selenium raw material of 5-15% is consumed, liquefied hydrogen selenide in condenser is carried out filling collection, obtain first
Selenizing hydrogen production；
S7：Continue to react, when the selenium raw material of 40%-60% is consumed, liquefied hydrogen selenide in condenser is carried out filling receipts
Collection, obtains the second selenizing hydrogen production；
S8：Continue to react, when the selenium raw material of 85%-95% is consumed, liquefied hydrogen selenide in condenser is carried out filling receipts
Collection, obtains the 3rd selenizing hydrogen production；
S9：Before selenium runs out of in the reacting furnace, next group selenium raw material is added, repeat S2-S8 operations, continuous output hydrogen selenide is produced
Product.
2. the preparation method of the hydrogen selenide according to claim 1, it is characterised in that：Heating in the S3 in reacting furnace
Temperature is between 400-700 DEG C.
3. the preparation method of the hydrogen selenide according to claim 1, it is characterised in that：The S4 cools to 20-50
℃。
4. the preparation method of the hydrogen selenide according to claim 1, it is characterised in that：Temperature in the S5 in condenser
It it is -40~-60 DEG C, the pressure in condenser is 5-10 atmospheric pressure.
5. the preparation method of hydrogen selenide according to claim 1, it is characterised in that：Vulcanize in the first selenizing hydrogen production
The content of hydrogen is higher than the second selenizing hydrogen production, the 3rd selenizing hydrogen production.
6. the preparation method of the hydrogen selenide according to claim 1, it is characterised in that：Sulphur in the second selenizing hydrogen production
The content for changing hydrogen is higher than the 3rd selenizing hydrogen production.
7. the preparation method of the hydrogen selenide according to claim 1, it is characterised in that：Also include selenizing between the S6-S8
The multiple of hydrogen fills collection.
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| CN201710244129.0A CN106904581A (en) | 2017-04-14 | 2017-04-14 | The preparation method of hydrogen selenide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108726492A (en) * | 2018-05-28 | 2018-11-02 | 太和气体（荆州）有限公司 | High-purity hydrogen selenide production equipment and high-purity hydrogen selenide production technology based on it |
| CN113874547A (en) * | 2019-11-12 | 2021-12-31 | 昭和电工株式会社 | Method for removing deposit and method for forming film |
| CN114887567A (en) * | 2022-05-16 | 2022-08-12 | 苏州金宏气体股份有限公司 | Hydrogen selenide continuous synthesis equipment and method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167422A (en) * | 2011-01-21 | 2011-08-31 | 南京工业大学 | Recovery process of industrial waste acid |
| CN102674268A (en) * | 2011-03-11 | 2012-09-19 | 大连立方化学技术有限公司 | Hydrogen selenide preparation device and method |
-
2017
- 2017-04-14 CN CN201710244129.0A patent/CN106904581A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167422A (en) * | 2011-01-21 | 2011-08-31 | 南京工业大学 | Recovery process of industrial waste acid |
| CN102674268A (en) * | 2011-03-11 | 2012-09-19 | 大连立方化学技术有限公司 | Hydrogen selenide preparation device and method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108726492A (en) * | 2018-05-28 | 2018-11-02 | 太和气体（荆州）有限公司 | High-purity hydrogen selenide production equipment and high-purity hydrogen selenide production technology based on it |
| CN113874547A (en) * | 2019-11-12 | 2021-12-31 | 昭和电工株式会社 | Method for removing deposit and method for forming film |
| CN114887567A (en) * | 2022-05-16 | 2022-08-12 | 苏州金宏气体股份有限公司 | Hydrogen selenide continuous synthesis equipment and method |
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Application publication date: 20170630 |