CN107881351A - The device for deoxidizing and method of high purity arsenic - Google Patents
The device for deoxidizing and method of high purity arsenic Download PDFInfo
- Publication number
- CN107881351A CN107881351A CN201711241192.5A CN201711241192A CN107881351A CN 107881351 A CN107881351 A CN 107881351A CN 201711241192 A CN201711241192 A CN 201711241192A CN 107881351 A CN107881351 A CN 107881351A
- Authority
- CN
- China
- Prior art keywords
- deoxidation
- high purity
- purity arsenic
- furnace body
- stove
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
Abstract
The present invention proposes a kind of device for deoxidizing of high purity arsenic, the device for deoxidizing includes a deoxidation stove, the device for deoxidizing also includes the glove box that a hatch door is shared with deoxidation stove, the vavuum pump being connected with deoxidation stove by an airflow line and the exhaust gas processing device being connected with vavuum pump by airflow line, a deduster is provided between the deoxidation stove and vavuum pump, the deoxidation stove includes body of heater, the heating mantle and an air inlet pipe being coated on outside body of heater, the body of heater both sides include switchable the first hatch door and the second hatch door, first hatch door is deoxidation stove, glove box shares, the deduster is directly connected to by another airflow line with exhaust gas processing device.Using the device for deoxidizing and method of high purity arsenic of the present invention, the analysis result of preparation-obtained high purity arsenic shows that product oxygen content is less than 1ppm after deoxidation, reaches product requirement, high purity arsenic completes packaging in glove box after preparation-obtained deoxidation, and glittering metallic luster is presented in color.
Description
Technical field
The present invention relates to the device for deoxidizing and method of the preparation field of high purity arsenic, more particularly to a kind of high purity arsenic.
Background technology
High purity arsenic is the primary raw material for synthesizing gallium arsenide compound, indium arsenide compound, selenizing arsenic compound etc..Extensively should
For fields such as integrated circuit, photovoltaic solar generation technology, Hall elements.Recently as the development of new high-tech industry,
The application field of high purity arsenic is increasingly extensive.
According to the difference of purity, high purity arsenic can be divided into 6N, 7N, 7N+ product, and with the continuous improvement of purity, performance is also got over
It is better to come, but high purity arsenic has a general character --- it is very easy to be oxidized, and purity is higher, is more oxidized easily.This makes
The producing, crush of high purity arsenic, preserves during the risk being oxidized be present.Once high purity arsenic product is oxidized, its table
Face dimmed will black, and so as to influence the performance of product, it is necessary to re-work increase cost, even result in product rejection.
Therefore, it is necessary to the device for deoxidizing and method of a kind of high purity arsenic are designed, it is high-purity by what is be oxidized with relatively low cost
Arsenic deoxidation.
The content of the invention
It is an object of the invention to overcome above-mentioned technical problem, using the low boiling of arsenic oxide, with reference to the effect of vacuum
And the reduction of hydrogen, there is provided a kind of device for deoxidizing and method of oxidized high purity arsenic.
To realize object defined above, the present invention adopts the following technical scheme that:A kind of device for deoxidizing of high purity arsenic, the deoxidation dress
Put including a deoxidation stove, the device for deoxidizing also includes sharing a glove box of a hatch door with deoxidation stove, passes through one with deoxidation stove
One vavuum pump of airflow line connection and the exhaust gas processing device being connected with vavuum pump by airflow line, the deoxidation stove
A deduster is provided between vavuum pump, the deoxidation stove includes body of heater, the heating mantle being coated on outside body of heater and an air inlet
Pipe, the body of heater both sides include switchable the first hatch door and the second hatch door, and first hatch door is deoxidation stove, glove box is common
With the deduster is directly connected to by another airflow line with exhaust gas processing device.
As a further improvement on the present invention, the body of heater is prepared using quartz.
A kind of method of deoxidation of high purity arsenic is also proposed, using the device for deoxidizing of above-mentioned high purity arsenic, method of deoxidation is included such as
Lower step:
S1, oxidized high-purity arsenic raw material installed with quartz boat or Packaging Bottle, then quartz boat or Packaging Bottle are transferred to deoxidation
In stove;
S2, the Absolute truth reciprocal of duty cycle of deoxidation furnace body is extracted into less than 20Pa with vavuum pump and maintains 10 ~ 90min;
Started to warm up in S3, deoxidation furnace body, be warming up to 250 ~ 450 DEG C of simultaneously constant temperature 1 ~ 15 hours;
S4, from the arsenic oxide of high purity arsenic surface separation with air-flow, a part is deposited on the other end of deoxidation furnace body, another
The gas dust remover that part is installed on airflow line is collected;
After S5, reaction terminate, stop heating, treat that deoxidation furnace body temperature is reduced to room temperature, stop vacuumizing, protected in inert gas
Under shield, blow-on discharging packaging.
As a further improvement on the present invention, S3 also includes S31 before heating:Vavuum pump is closed, into deoxidation furnace body
Hydrogen is passed through with certain flow.
As a further improvement on the present invention, hydrogen flowing quantity is 100 ~ 5000L/h in S31.
As a further improvement on the present invention, the Packaging Bottle is prepared using Pyrex.
A kind of method of deoxidation of high purity arsenic is separately proposed, using the device for deoxidizing of above-mentioned high purity arsenic, method of deoxidation includes as follows
Step:
T1, oxidized high-purity arsenic raw material installed with quartz boat or Pyrex product package bottle, then by quartz boat or packaging
Bottle is transferred in deoxidation stove;
T2, the Absolute truth reciprocal of duty cycle of deoxidation furnace body is extracted into less than 20pa with vavuum pump and maintains 10 ~ 90min;
T3, deoxidation furnace body start to warm up, and are warming up to 250 ~ 450 DEG C of simultaneously constant temperature 1 ~ 15 hours, while vavuum pump ensures body of heater
Vacuum;
T4, from the arsenic oxide of high purity arsenic surface separation with air-flow, a part is deposited on the other end of deoxidation furnace body, another
The deduster that part is installed on airflow line is collected;
T5, stop heating, deoxidation furnace body temperature is down to room temperature;
T6, the Absolute truth reciprocal of duty cycle of deoxidation furnace body is extracted into less than 20pa with vavuum pump and maintains 10 ~ 90min;Close vavuum pump,
Hydrogen is passed through with certain flow into deoxidation furnace body, deoxidation furnace body starts to warm up, and is warming up to 250 ~ 450 DEG C and constant temperature 1 ~ 15
Hour;
T7, from the arsenic oxide of high purity arsenic surface separation with air-flow, a part is deposited on the other end of deoxidation furnace body, another
The gas dust remover that part is installed on airflow line is collected;
T8, stop heating, treat that deoxidation furnace temperature is down to room temperature;Stopping vacuumizes, under inert gas shielding, blow-on spout bag
Dress.
As a further improvement on the present invention, hydrogen flowing quantity is 100 ~ 5000L/h in T6.
As a further improvement on the present invention, the Packaging Bottle is prepared using Pyrex.
Using the device for deoxidizing and method of high purity arsenic of the present invention, the analysis result of preparation-obtained high purity arsenic is shown, is taken off
Product oxygen content is less than 1ppm after oxygen, reaches product requirement, and high purity arsenic completes bag in glove box after preparation-obtained deoxidation
Glittering metallic luster is presented in dress, color.
Brief description of the drawings
Fig. 1 is the overall structure diagram of the embodiment of the device for deoxidizing of high purity arsenic of the present invention.
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 only part of the embodiment of the present invention, rather than whole embodiments.It is common based on the embodiment in the present invention, this area
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
Referring to Fig. 1, the present invention proposes a kind of device for deoxidizing 100 of high purity arsenic, it includes a deoxidation stove 110 and deoxidation
Stove 110 shares a glove box 120, a vavuum pump 130, the tail being connected with deoxidation stove 110 by airflow line 160 of a hatch door
Flash Gas Compression Skid System 140, is provided with a deduster 150 between deoxidation stove 110 and vavuum pump 130, deoxidation stove 110 includes body of heater 111, bag
Heating mantle 112, the air inlet pipe 113 overlayed on outside body of heater 111, the both sides of body of heater 111 include the first switchable hatch door 114 and second
Hatch door 115, the first hatch door 114 is deoxidation stove 110, glove box 120 shares, and deduster 150 passes through another airflow line 160 and tail
Flash Gas Compression Skid System 140 is directly connected to.
Air inlet pipe 113 plays a part of air inlet as hydrogen and the entrance of inert gas.
As a modification of the present invention, the free of contamination material of the material selection of body of heater 111 --- quartz.
In order to ensure that the high purity arsenic after deoxidation is not oxidized again, blow-on spout bag is mounted under inert gas shielding and completed,
The design of deoxidation stove 110 is connected as a single entity with glove box 120, is separated by the first hatch door 114, during charging, the second hatch door 115 of opening,
Oxidized high-purity arsenic raw material is loaded in deoxidation stove 110;When coming out of the stove, the first hatch door 114 is opened directly by Product transport to having
In the glove box 120 of inert gas shielding, product completes packaging in glove box 120 after deoxidation.
The present invention proposes a kind of method of deoxidation of high purity arsenic simultaneously, using the device for deoxidizing of above-mentioned high purity arsenic, deoxidation side
Method comprises the following steps:
S1, oxidized high-purity arsenic raw material installed with quartz boat or Packaging Bottle, then quartz boat or Packaging Bottle are transferred to deoxidation
In stove;
S2, the Absolute truth reciprocal of duty cycle of deoxidation furnace body is extracted into less than 20Pa with vavuum pump and maintains 10 ~ 90min;
Started to warm up in S3, deoxidation furnace body, be warming up to 250 ~ 450 DEG C of simultaneously constant temperature 1 ~ 15 hours;Preferably, it is warming up to 300 ~
400 DEG C and constant temperature 4 ~ 12 hours;It is highly preferred that it is warming up to 320 ~ 380 DEG C of simultaneously constant temperature 5 ~ 10 hours;
S4, from the arsenic oxide of high purity arsenic surface separation with air-flow, a part is deposited on the other end of deoxidation furnace body, another
The gas dust remover that part is installed on airflow line is collected;
After S5, reaction terminate, stop heating, treat that deoxidation furnace body temperature is reduced to room temperature;Stopping vacuumizes, and is protected in inert gas
Under shield, blow-on discharging packaging.
By S3, the oxide and free oxygen of arsenic, due to vacuum and the effect of heating, progressively separated from the surface of arsenic.
In certain embodiments of the present invention, Packaging Bottle is prepared using Pyrex.Packaging Bottle uses Pyrex
Preparation can avoid Packaging Bottle from polluting raw material.
In certain embodiments of the present invention, S3 also includes S31 before heating:Vavuum pump is closed, into deoxidation furnace body
Hydrogen is passed through with certain flow.It is passed through oxide of the hydrogen as reducing agent reduction arsenic.If not including S31, the present invention is
Using the mode of heating in vacuum, using the low boiling of arsenic oxide, to realize vacuum deaeration.And if including S31, then it is to utilize
The reproducibility of hydrogen realizes deoxidation.
In certain embodiments of the present invention, hydrogen flowing quantity is 100 ~ 5000L/h in S31.Preferably, hydrogen stream in S31
Measure as 200 ~ 4000L/h.It is highly preferred that hydrogen flowing quantity is 500 ~ 1000L/h in S31.
Another embodiment then realizes deoxidation using the low boiling of arsenic oxide and the reproducibility of hydrogen simultaneously, reaches more preferable
Treatment effect.
A kind of method of deoxidation of high purity arsenic, it comprises the following steps:
T1, oxidized high-purity arsenic raw material installed with quartz boat or Pyrex product package bottle, then by quartz boat or packaging
Bottle is transferred in deoxidation stove;
T2, the Absolute truth reciprocal of duty cycle of deoxidation furnace body is extracted into less than 20pa with vavuum pump and maintains 10 ~ 90min;
T3, deoxidation furnace body start to warm up, and are warming up to 250 ~ 450 DEG C of simultaneously constant temperature 1 ~ 15 hours, while vavuum pump ensures body of heater
Vacuum;Preferably, 300 ~ 400 DEG C of simultaneously constant temperature 4 ~ 12 hours are warming up to;It is highly preferred that be warming up to 320 ~ 380 DEG C and constant temperature 5 ~
10 hours;
T4, from the arsenic oxide of high purity arsenic surface separation with air-flow, a part is deposited on the other end of deoxidation furnace body, another
The deduster that part is installed on airflow line is collected;
T5, stop heating, deoxidation furnace body temperature is down to room temperature;
T6, the Absolute truth reciprocal of duty cycle of deoxidation furnace body is extracted into less than 20pa with vavuum pump and maintains 10 ~ 90min;Close vavuum pump,
Hydrogen is passed through with certain flow into deoxidation furnace body, deoxidation furnace body starts to warm up, and is warming up to 250 ~ 450 DEG C and constant temperature 1 ~ 15
Hour;Preferably, 300 ~ 400 DEG C of simultaneously constant temperature 4 ~ 12 hours are warming up to;It is highly preferred that it is warming up to 320 ~ 380 DEG C and constant temperature 5 ~ 10
Hour;
T7, from the arsenic oxide of high purity arsenic surface separation with air-flow, a part is deposited on the other end of deoxidation furnace body, another
The deduster that part is installed on airflow line is collected;
T8, stop heating, treat that deoxidation furnace temperature is down to room temperature, stop vacuumizing, under inert gas shielding, blow-on spout bag
Dress.
To prevent from polluting, deoxidation furnace body is from free of contamination Material texture --- quartz is prepared.
In certain embodiments of the present invention, the Packaging Bottle is prepared using Pyrex.
In certain embodiments of the present invention, hydrogen flowing quantity is 100 ~ 5000L/h in T6.Preferably, hydrogen flowing quantity in S31
For 200 ~ 4000L/h.It is highly preferred that hydrogen flowing quantity is 500 ~ 1000L/h in S31.
By the above method, arsenic oxide is separated and is deposited on the other end of deoxidation furnace body or is received by deduster
Collection, or arsenic is reduced to, realize deoxidation.
Using the device for deoxidizing and method of high purity arsenic of the present invention, the analysis result of preparation-obtained high purity arsenic is shown, is taken off
Product oxygen content is less than 1ppm after oxygen, reaches product requirement.High purity arsenic is completed in glove box 120 after preparation-obtained deoxidation
Glittering metallic luster is presented in packaging, color.
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 realize in the case of scope and spirit of the present invention disclosed in not departing from by appended claims, various to change
It is possible for entering, increasing and substituting.
Claims (9)
1. a kind of device for deoxidizing of high purity arsenic, the device for deoxidizing includes a deoxidation stove, it is characterised in that:The device for deoxidizing is also
Including the glove box that a hatch door is shared with deoxidation stove, the vavuum pump that is connected with deoxidation stove by an airflow line and with it is true
The exhaust gas processing device that empty pump is connected by airflow line, a deduster is provided between the deoxidation stove and vavuum pump, it is described
Deoxidation stove includes body of heater, the heating mantle and an air inlet pipe that are coated on outside body of heater, and the body of heater both sides include switchable the
One hatch door and the second hatch door, first hatch door are that deoxidation stove, glove box share, the deduster by another airflow line with
Exhaust gas processing device is directly connected to.
2. the device for deoxidizing of the high purity arsenic according to claim 1, it is characterised in that:The body of heater prepared using quartz and
Into.
A kind of 3. method of deoxidation of high purity arsenic, it is characterised in that:Using the device for deoxidizing of the high purity arsenic described in claim 1, take off
Oxygen method comprises the following steps:
S1, oxidized high-purity arsenic raw material installed with quartz boat or Packaging Bottle, then quartz boat or Packaging Bottle are transferred to deoxidation
In stove;
S2, the Absolute truth reciprocal of duty cycle of deoxidation furnace body is extracted into less than 20Pa with vavuum pump and maintains 10 ~ 90min;
Started to warm up in S3, deoxidation furnace body, be warming up to 250 ~ 450 DEG C of simultaneously constant temperature 1 ~ 15 hours;
S4, from the arsenic oxide of high purity arsenic surface separation with air-flow, a part is deposited on the other end of deoxidation furnace body, another
The gas dust remover that part is installed on airflow line is collected;
After S5, reaction terminate, stop heating, treat that deoxidation furnace body temperature is reduced to room temperature, stop vacuumizing, protected in inert gas
Under shield, blow-on discharging packaging.
4. the method for deoxidation of the high purity arsenic according to claim 3, it is characterised in that:S3 also includes S31 before heating:Close
Vavuum pump is closed, hydrogen is passed through with certain flow into deoxidation furnace body.
5. the method for deoxidation of the high purity arsenic according to claim 4, it is characterised in that:In S31 hydrogen flowing quantity be 100 ~
5000L/h。
6. the method for deoxidation of the high purity arsenic according to claim 3, it is characterised in that:The Packaging Bottle uses Pyrex
It is prepared.
A kind of 7. method of deoxidation of high purity arsenic, it is characterised in that:Using the device for deoxidizing of the high purity arsenic described in claim 1, take off
Oxygen method comprises the following steps:
T1, oxidized high-purity arsenic raw material installed with quartz boat or Pyrex product package bottle, then by quartz boat or packaging
Bottle is transferred in deoxidation stove;
T2, the Absolute truth reciprocal of duty cycle of deoxidation furnace body is extracted into less than 20pa with vavuum pump and maintains 10 ~ 90min;
T3, deoxidation furnace body start to warm up, and are warming up to 250 ~ 450 DEG C of simultaneously constant temperature 1 ~ 15 hours, while vavuum pump ensures body of heater
Vacuum;
T4, from the arsenic oxide of high purity arsenic surface separation with air-flow, a part is deposited on the other end of deoxidation furnace body, another
The deduster that part is installed on airflow line is collected;
T5, stop heating, deoxidation furnace body temperature is down to room temperature;
T6, the Absolute truth reciprocal of duty cycle of deoxidation furnace body is extracted into less than 20pa with vavuum pump and maintains 10 ~ 90min;Close vavuum pump,
Hydrogen is passed through with certain flow into deoxidation furnace body, deoxidation furnace body starts to warm up, and is warming up to 250 ~ 450 DEG C and constant temperature 1 ~ 15
Hour;
T7, from the arsenic oxide of high purity arsenic surface separation with air-flow, a part is deposited on the other end of deoxidation furnace body, another
The gas dust remover that part is installed on airflow line is collected;
T8, stop heating, treat that deoxidation furnace temperature is down to room temperature;Stopping vacuumizes, under inert gas shielding, blow-on spout bag
Dress.
8. the method for deoxidation of the high purity arsenic according to claim 7, it is characterised in that:In T6 hydrogen flowing quantity be 100 ~
5000L/h。
9. the method for deoxidation of the high purity arsenic according to claim 7, it is characterised in that:The Packaging Bottle uses Pyrex
It is prepared.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110923457A (en) * | 2019-12-27 | 2020-03-27 | 中国科学院电工研究所 | Preparation method of high-purity arsenic crystal |
CN115418719A (en) * | 2022-08-22 | 2022-12-02 | 峨眉山嘉美高纯材料有限公司 | Preparation method of low-oxygen compact ultra-high-purity arsenic rod |
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CN115418719B (en) * | 2022-08-22 | 2023-08-29 | 峨眉山嘉美高纯材料有限公司 | Preparation method of low-oxygen compact ultra-high purity arsenic rod |
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Application publication date: 20180406 |