CN106006573A - Preparation method of arsenic selenide - Google Patents
Preparation method of arsenic selenide Download PDFInfo
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- CN106006573A CN106006573A CN201610083120.1A CN201610083120A CN106006573A CN 106006573 A CN106006573 A CN 106006573A CN 201610083120 A CN201610083120 A CN 201610083120A CN 106006573 A CN106006573 A CN 106006573A
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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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Abstract
The invention provides a preparation method of arsenic selenide. The method comprises the steps of: subjecting selenium powder and arsenic powder to heating reaction under an inert gas condition to obtain arsenic selenide; wherein the heating includes the gradient temperature rise conditions of: conducting heating to 200-300DEG C at a rate of 1-3DEG C per minute, and performing thermal insulation for 1-3h; then conducting heating to 400-500DEG C at a rate of 1-3DEG C per minute, and performing thermal insulation for 1-3h. The preparation method of arsenic selenide provided by the invention takes selenium powder and arsenic powder as the raw materials, employs a specific heating procedure for low temperature synthesis of arsenic selenide, and avoids volatilization of selenium and arsenic. Therefore, vacuum tight reaction vessel is not needed, a tube furnace can realize the preparation process, and the reaction vessel can be reused. Also the prepared arsenic selenide has high yield. The result shows that the yield of the arsenic selenide prepared by the method provided by the invention is more than 99.5%.
Description
Technical field
The invention belongs to arsenic selenide technical field, be specifically related to the preparation method of a kind of arsenic selenide.
Background technology
Arsenic selenide (Arsenic Selenide), is a kind of black crystals or dark brown solid, chemical formula
As2Se3.Being mainly used in infrared optics field, the method being typically prepared is by elemental selenium block and elemental arsenic block
Mixed melting and obtain.The fusing point of selenium is 221 DEG C, and boiling point is 684.9 DEG C, and between the two temperature, selenium has
The biggest vapour pressure；Elemental arsenic fusing point 817 DEG C (28 atmospheric pressure), is heated to 613 DEG C, just can be without liquid
State, directly distils, and becomes steam.Therefore, prior art is when preparing arsenic selenide, and preparation temperature is higher,
In order to avoid elemental selenium and the volatilization loss of elemental arsenic, elemental selenium block and elemental arsenic block are placed in a vacuum
Airtight quartz ampoule in react, reaction terminate after need to crush quartz ampoule, reaction vessel cannot
Recycling, causes waste greatly；And the method temperature of mixed melting is higher in prior art,
Ask equipment and technique the most more complicated.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide the preparation method of a kind of arsenic selenide,
The preparation method that the present invention provides is simple, uses low temperature synthesis, and reaction vessel can reuse.
The invention provides the preparation method of a kind of arsenic selenide, comprise the following steps:
Selenium powder and arsenic powder are carried out reacting by heating under inert gas conditions, obtains arsenic selenide；
The gradient increased temperature condition of described heating is: per minute be heated to 200～300 DEG C with 1～3 DEG C, is incubated 1～3
Hour；Per minute it is heated to 400～500 DEG C with 1～3 DEG C again, is incubated 1～3 hour.
Preferably, the granularity of described selenium powder is-100 mesh～+200 mesh.
Preferably, the granularity of described arsenic powder is-100 mesh～+200 mesh.
Preferably, the mol ratio of described selenium powder and arsenic powder is 3:2.
Preferably, described noble gas is selected from nitrogen or helium.
Preferably, described selenium powder and arsenic powder are placed in tube furnace and react.
Preferably, the gradient increased temperature condition of described heating is: per minute be heated to 250 DEG C with 1 DEG C, insulation
1.5 hour；Per minute it is heated to 400 DEG C with 2 DEG C again, is incubated 1.5 hours.
Preferably, the gradient increased temperature condition of described heating is: per minute be heated to 300 DEG C with 1.5 DEG C, protects
Temperature 2 hours；Per minute it is heated to 420 DEG C with 1 DEG C again, is incubated 1 hour.
Preferably, the gradient increased temperature condition of described heating is: per minute be heated to 300 DEG C with 2 DEG C, insulation
1 hour；Per minute it is heated to 380 DEG C with 1.5 DEG C again, is incubated 2 hours.
Compared with prior art, the invention provides the preparation method of a kind of arsenic selenide, comprise the following steps:
Selenium powder and arsenic powder are carried out reacting by heating under inert gas conditions, obtains arsenic selenide；The ladder of described heating
Degree Elevated Temperature Conditions is: per minute is heated to 200～300 DEG C with 1～3 DEG C, is incubated 1～3 hour；Again with 1～3
DEG C per minute it is heated to 400～500 DEG C, is incubated 1～3 hour.The preparation method of the arsenic selenide that the present invention provides
With selenium powder and arsenic powder as raw material, specific heating schedule low temperature is used to synthesize arsenic selenide, it is to avoid selenium and arsenic
Volatilization, therefore without using vacuum-tight reaction vessel, use tube furnace can realize preparation process,
Reaction vessel can reuse.And the productivity of the arsenic selenide prepared is higher.
Result shows, the yield of the arsenic selenide that the present invention provides is more than 99.5%.
Accompanying drawing explanation
The schematic diagram of the equipment preparing arsenic selenide that Fig. 1 provides for the present invention.
Detailed description of the invention
The invention provides the preparation method of a kind of arsenic selenide, comprise the following steps:
Selenium powder and arsenic powder are carried out reacting by heating under inert gas conditions, obtains arsenic selenide；
The gradient increased temperature condition of described heating is: per minute be heated to 200～300 DEG C with 1～3 DEG C, is incubated 1～3
Hour；Per minute it is heated to 400～500 DEG C with 1～3 DEG C again, is incubated 1～3 hour.
First the present invention by selenium powder and arsenic powder mix homogeneously, obtains mixed-powder.
Wherein, the present invention prepares arsenic selenide with selenium powder and arsenic powder for raw material.Wherein, the granularity of described selenium powder
Being preferably-100 mesh～+200 mesh, the granularity of described arsenic powder is preferably-100 mesh～+200 mesh.That is, the present invention
Selecting particle diameter is the selenium powder that can not be passed through 200 eye mesh screens by 100 mesh, and particle diameter is for passing through
100 mesh and can not be by the arsenic powder of 200 eye mesh screens.It is furthermore preferred that the granularity of described selenium powder is preferably-120
Mesh～+180 mesh, the granularity of described arsenic powder is preferably-120 mesh～+180 mesh.
In the present invention, described selenium powder is preferably 3:2 with the mol ratio of arsenic powder.
The mixed-powder of selenium powder and arsenic powder is carried out reacting by heating under inert gas conditions.The present invention is by institute
Stating mixed-powder to be placed in the reaction vessel preparing arsenic selenide, then one end is passed through noble gas, the other end
Carry out tail gas absorption, afterwards, start heater and mixed-powder is heated.The present invention is to described selenium
The reaction vessel changing arsenic does not has particular restriction, it is preferred to use tube furnace.
Schematic diagram referring specifically to the equipment preparing arsenic selenide that Fig. 1, Fig. 1 provide for the present invention.In Fig. 1,
1 is diamond heating device, and 2 is tube furnace quartz ampoule, and 3 is quartz boat, and 4 is the mixed of selenium powder and arsenic powder
Close powder.In FIG, noble gas enters from one end of tube furnace, and the synthesis for arsenic selenide provides one
Individual inert environments, then noble gas passes through tube furnace, the other end of tube furnace discharge, carry out tail gas
Absorb.
The present invention carries out the preparation of arsenic selenide with tube furnace, it is not necessary to seal reaction vessel, therefore,
Also being removed by product after being no need for being destroyed by consersion unit after the completion of reaction, reaction vessel can repeat profit
With, cost-effective.
In the present invention, described noble gas is preferably nitrogen or helium, more preferably nitrogen.
After being passed through noble gas, the heater of tube furnace starts, and the gradient increased temperature condition of described heating is:
Per minute it is heated to 200～300 DEG C with 1～3 DEG C, is incubated 1～3 hour；Per minute it is heated to 1～3 DEG C again
400～500 DEG C, it is incubated 1～3 hour.
In some embodiments of the invention, the gradient increased temperature condition of described heating is: per minute add with 1 DEG C
Heat, to 250 DEG C, is incubated 1.5 hours；Per minute it is heated to 400 DEG C with 2 DEG C again, is incubated 1.5 hours.
In other embodiments of the present invention, the gradient increased temperature condition of described heating is: with 1.5 DEG C every point
Clock is heated to 300 DEG C, is incubated 2 hours；Per minute it is heated to 420 DEG C with 1 DEG C again, is incubated 1 hour.
In other embodiments of the present invention, the gradient increased temperature condition of described heating is: per minute with 2 DEG C
It is heated to 300 DEG C, is incubated 1 hour；Per minute it is heated to 380 DEG C with 1.5 DEG C again, is incubated 2 hours.
The preparation method of the arsenic selenide that the present invention provides, with selenium powder and arsenic powder as raw material, uses specific intensification
Program low temperature synthesis arsenic selenide, it is to avoid the volatilization of selenium and arsenic, therefore without using vacuum-tight reaction
Container, uses tube furnace can realize preparation process, and reaction vessel can reuse.And it is prepared into
The productivity of the arsenic selenide arrived is higher.
Result shows, the yield of the arsenic selenide that the present invention provides is more than 99.5%.
In order to be further appreciated by the present invention, below in conjunction with the embodiment preparation to the arsenic selenide that the present invention provides
Method illustrates, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
1. 6mol granularity is-100 mesh～the selenium powder of+170 mesh and 4mol granularity is-140 mesh～+200 mesh
Mesh arsenic powder mix homogeneously；
2. the material mixed is put in quartz boat, put in tube furnace；
3. in tube furnace, it is continually fed into nitrogen, opens heating；
4. heat gradient is: per minute is heated to 250 DEG C with 1 DEG C, is incubated 1.5 hours；Again with 2 DEG C every point
Clock is heated to 400 DEG C, is incubated 1.5 hours；
5. stop heating, treat that temperature drops to room temperature, close nitrogen, take out material and obtain arsenic selenide.Measure
Its yield is 99.73%.
Embodiment 2
1. 9mol granularity is-140 mesh～the selenium powder of+170 mesh and 6mol granularity is-100 mesh～+170 mesh
Arsenic powder mix homogeneously
2. the material mixed is put in quartz boat, put in tube furnace
3. in tube furnace, it is continually fed into nitrogen, opens heating
4. heat gradient is: per minute is heated to 300 DEG C with 1.5 DEG C, is incubated 2 hours；Again with 1 DEG C every point
Clock is heated to 420 DEG C, is incubated 1 hour.
5. stopping heating, slow-witted temperature drops to room temperature, closes nitrogen, takes out material and obtains arsenic selenide.Measure
Its yield is 99.85%.
Embodiment 3
1. 3mol granularity is-140 mesh～the selenium powder of+170 mesh and 2mol granularity is-100 mesh～+200 mesh
Arsenic powder mix homogeneously
2. the material mixed is put in quartz boat, put in tube furnace
3. in tube furnace, it is continually fed into nitrogen, opens heating
4. heat gradient is: per minute is heated to 300 DEG C with 2 DEG C, is incubated 1 hour；Again with 1.5 DEG C every point
Clock is heated to 380 DEG C, is incubated 2 hours.
5. stopping heating, slow-witted temperature drops to room temperature, closes nitrogen, takes out material and obtains arsenic selenide.Measure
Its yield is 99.69%.
The above is only the preferred embodiment of the present invention, it is noted that general for the art
For logical technical staff, under the premise without departing from the principles of the invention, it is also possible to make some improvement and profit
Decorations, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
1. the preparation method of an arsenic selenide, it is characterised in that comprise the following steps:
Selenium powder and arsenic powder are carried out reacting by heating under inert gas conditions, obtains arsenic selenide；
The gradient increased temperature condition of described heating is: per minute be heated to 200～300 DEG C with 1～3 DEG C, is incubated 1～3
Hour；Per minute it is heated to 400～500 DEG C with 1～3 DEG C again, is incubated 1～3 hour.
Preparation method the most according to claim 1, it is characterised in that the granularity of described selenium powder is-100
Mesh～+200 mesh.
Preparation method the most according to claim 1, it is characterised in that the granularity of described arsenic powder is-100
Mesh～+200 mesh.
Preparation method the most according to claim 1, it is characterised in that rubbing of described selenium powder and arsenic powder
That ratio is 3:2.
Preparation method the most according to claim 1, it is characterised in that described noble gas is selected from nitrogen
Gas or helium.
Preparation method the most according to claim 1, it is characterised in that described selenium powder and arsenic powder are placed in
Tube furnace reacts.
Preparation method the most according to claim 1, it is characterised in that the gradient increased temperature of described heating
Condition is: per minute is heated to 250 DEG C with 1 DEG C, is incubated 1.5 hours；Per minute it is heated to 2 DEG C again
400 DEG C, it is incubated 1.5 hours.
Preparation method the most according to claim 1, it is characterised in that the gradient increased temperature of described heating
Condition is: per minute is heated to 300 DEG C with 1.5 DEG C, is incubated 2 hours；Per minute it is heated to 1 DEG C again
420 DEG C, it is incubated 1 hour.
Preparation method the most according to claim 1, it is characterised in that the gradient increased temperature of described heating
Condition is: per minute is heated to 300 DEG C with 2 DEG C, is incubated 1 hour；Per minute it is heated to 1.5 DEG C again
380 DEG C, it is incubated 2 hours.
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| CN201610083120.1A CN106006573B (en) | 2016-02-05 | 2016-02-05 | A kind of preparation method of arsenic selenide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498909A (en) * | 2020-05-25 | 2020-08-07 | 先导薄膜材料（广东）有限公司 | Preparation method of manganese-arsenic compound |
| CN114590784A (en) * | 2022-03-11 | 2022-06-07 | 先导薄膜材料（广东）有限公司 | Preparation method of bismuth selenide |
| CN114590837A (en) * | 2022-03-15 | 2022-06-07 | 先导薄膜材料（广东）有限公司 | Preparation method and application of high-purity cadmium antimonide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2887359A (en) * | 1953-11-12 | 1959-05-19 | Francois F Gans | Method for preparing pentavalent arsenic selenides |
| CN102086030A (en) * | 2010-11-25 | 2011-06-08 | 广东先导稀有材料股份有限公司 | Method for preparing arsenic selenide granules |
-
2016
- 2016-02-05 CN CN201610083120.1A patent/CN106006573B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2887359A (en) * | 1953-11-12 | 1959-05-19 | Francois F Gans | Method for preparing pentavalent arsenic selenides |
| CN102086030A (en) * | 2010-11-25 | 2011-06-08 | 广东先导稀有材料股份有限公司 | Method for preparing arsenic selenide granules |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498909A (en) * | 2020-05-25 | 2020-08-07 | 先导薄膜材料（广东）有限公司 | Preparation method of manganese-arsenic compound |
| CN114590784A (en) * | 2022-03-11 | 2022-06-07 | 先导薄膜材料（广东）有限公司 | Preparation method of bismuth selenide |
| CN114590837A (en) * | 2022-03-15 | 2022-06-07 | 先导薄膜材料（广东）有限公司 | Preparation method and application of high-purity cadmium antimonide |
| CN114590837B (en) * | 2022-03-15 | 2023-09-01 | 先导薄膜材料（广东）有限公司 | Preparation method and application of high-purity cadmium antimonide |
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| CN106006573B (en) | 2018-06-26 |
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Effective date of registration: 20181122 Address after: 511500 Tellurium Chemical Workshop of Guangdong Pioneer Rare Materials Co., Ltd., Heyun Town, Qingxin District, Qingyuan City, Guangdong Province Patentee after: Guangdong Pioneer Precious Metals Material Co., Ltd. Address before: 511517 Guangdong Industrial Development Zone, Qingxian County, Qingyuan, Guangdong (beside the fish dam road) Guangdong pioneer thin material Limited by Share Ltd Patentee before: Guangdong Vital Rare Material Co., Ltd. |