CN109680165A - Hydro-reduction device - Google Patents
Hydro-reduction device Download PDFInfo
- Publication number
- CN109680165A CN109680165A CN201710979046.6A CN201710979046A CN109680165A CN 109680165 A CN109680165 A CN 109680165A CN 201710979046 A CN201710979046 A CN 201710979046A CN 109680165 A CN109680165 A CN 109680165A
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- Prior art keywords
- heating
- hydro
- reduction device
- branch pipe
- heating zone
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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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The present invention relates to a kind of hydro-reduction devices, it includes a horizontal positioned reaction quartz ampoule, a heating mantle for being heated to reaction quartz ampoule, one evaporating kettle, one air inlet pipe, the reaction quartz ampoule includes a conversion zone and a deposition section, the conversion zone includes a loading area and a buffer area, the buffer area and deposition section are adjacent, the heating mantle includes one first heating zone, one second heating zone and a third heating zone, first heating zone, second heating zone, third heating zone, which respectively corresponds, is coated on loading area, buffer area, deposit section, a reduction tube is fixed in the loading area, in one end insertion reduction tube of the air inlet pipe, the other end bifurcated of the air inlet pipe is the first branch pipe and the second branch pipe, first branch pipe is connected to evaporating kettle, second branch pipe is connected to a hydrogen inlet and a nitrogen inlet.This hydro-reduction device list furnace production capacity is big, and reaction conversion ratio is high, operates easier.
Description
Technical field
The present invention relates to high purity arsenic preparation field more particularly to a kind of the hydrogenation of high purity arsenic is prepared also using arsenic trichloride
Original device.
Background technique
High purity arsenic is the primary raw material for synthesizing the semiconducting compounds such as GaAs, indium arsenide, arsenic selenide.These semiconductor transformations
It closes object and is widely used in the fields such as integrated circuit, photovoltaic solar power generation, Hall element.Recently as new high-tech industry
Development, the application field of high purity arsenic is increasingly extensive, and demand is increasing.There are many preparation methods for high purity arsenic, wherein hydrogenation is also
Former method is to produce the common method of high purity arsenic, please refers to one kind of Chinese patent application CN201510425035.4 proposition for height
The hydro-reduction device and high purity arsenic preparation method of pure arsenic production, but the hydro-reduction device that the technical solution uses still has
Separate unit low output, the production cycle is long, restores the not high technical problem of conversion ratio.
Thus, it is necessary to design the new hydro-reduction device of one kind to solve the above technical problems.
Summary of the invention
High, with short production cycle, reduction high conversion rate hydrogenation that the object of the present invention is to provide a kind of separate unit yield is also
Original device.
To realize foregoing purpose, the present invention adopts the following technical scheme: a kind of hydro-reduction device comprising horizontal positioned
A reaction quartz ampoule, the heating mantle for being heated to reaction quartz ampoule, an evaporating kettle, an air inlet pipe, the reaction is quartzy
Pipe includes a conversion zone and a deposition section, and the conversion zone includes a loading area and a buffer area, the buffer area and deposition section
Adjacent, the heating mantle includes one first heating zone, one second heating zone and a third heating zone, first heating zone, the
Two heating zones, third heating zone, which respectively correspond, is coated on loading area, buffer area, deposition section, fixes a reduction in the loading area
One end of pipe, the air inlet pipe is inserted into reduction tube, and the other end bifurcated of the air inlet pipe is the first branch pipe and the second branch pipe, institute
It states the first branch pipe to be connected to evaporating kettle, second branch pipe is connected to a hydrogen inlet and a nitrogen inlet.
As a further improvement of the present invention, the deposition section includes a side surface of rotary table side wall shape and for sealing
A bottom surface, the side surface is gradually increased along far from the direction cross-sectional area of buffer area, and the rotary table of the side surface is female
The angle that the extended line of both line and rotary table axis is formed is between 0-45 °.
As a further improvement of the present invention, the rotary table bus and the extended line of both rotary table axis of the side surface are formed
Angle be 15 °.
As a further improvement of the present invention, the deposition section further includes an extension, the extension both ends respectively with
Side surface is connected with bottom surface, and the cross-sectional area of the extension remains unchanged.
As a further improvement of the present invention, the hydro-reduction device further includes an exhaust gas processing device, the tail gas
Processing unit includes being sequentially communicated for being passed through one first offgas duct of tail gas, the process tank for handling tail gas and being used for
One second offgas duct of tail gas is discharged, is connected to form a tail with deposition section through bottom surface before and after the front end of first offgas duct
Gas outlet.
As a further improvement of the present invention, a heating plate is additionally provided in the extension, the heating plate includes one perpendicular
Straight portion and a horizontal part, the horizontal part are vertically fixed on bottom surface, and the vertical portion is embedded in a heater strip, the heating
The heating temperature of silk is 600-900 DEG C, and the front that the vertical portion is located at offgas outlet forms barrier.
As a further improvement of the present invention, on first branch pipe, the second branch pipe, hydrogen inlet and nitrogen inlet
It is equipped with a control valve, is also connected with a relief valve on second branch pipe.
As a further improvement of the present invention, the heater for heating to evaporating kettle is set below the evaporating kettle.
As a further improvement of the present invention, the first branch pipe cladding is provided with the warmer for heat preservation.
As a further improvement of the present invention, the heating temperature of first heating zone is 800-900 DEG C；Described second adds
The heating temperature of hot-zone is 600-800 DEG C；The heating temperature of the third heating zone is 300-400 DEG C.
This hydro-reduction device list furnace production capacity is big, reduces heating energy consumption；Gas-gas reaction improves reaction efficiency；Pass through
Increase heating plate, reaction conversion ratio is high；Arsenic is directly collected in deposition section, is operated easier.
Detailed description of the invention
Fig. 1 is the overall structure diagram of the embodiment of hydro-reduction device of the present invention.
Specific embodiment
Technical solution 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 the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Referring to Fig. 1, the present invention proposes a kind of hydro-reduction device 100, which includes horizontal positioned
One reaction quartz ampoule 110, for reaction quartz ampoule 110 heat a heating mantle 120, an evaporating kettle 130, an air inlet pipe
140, reaction quartz ampoule 110 includes a conversion zone 111 and a deposition section 112, and conversion zone 111 is slow including a loading area 111a and one
Area 111b is rushed, buffer area 111b and deposition section 112 are adjacent, and heating mantle 120 includes one first heating zone 121, one second heating zone
122 and a third heating zone 123, the first heating zone 121, the second heating zone 122, third heating zone 123 respectively correspond and are coated on
Loading area 111a, buffer area 111b, section 112 is deposited, a reduction tube 111c is fixed in loading area 111a, reduction tube 111c is to occur
The main place of reduction reaction, in one end insertion reduction tube 111c of air inlet pipe 140, the other end bifurcated of air inlet pipe 140 is the
One branch pipe 141 and the second branch pipe 142, the first branch pipe 141 are connected to evaporating kettle 130, and the second branch pipe 142 is connected to a hydrogen inlet
150 and a nitrogen inlet 160.
In certain embodiments of the present invention, deposition section 112 includes a side surface 112a of rotary table side wall shape and is used for
One bottom surface 112c of sealing, side surface 112a are gradually increased along the direction cross-sectional area far from buffer area 111b, side surface
The angle that the rotary table bus of 112a and the extended line of both rotary table axis are formed is between 0-45 °, in the present embodiment, the angle
Preferably 15 °, the purpose that the angle is arranged is convenient for arsenic deposition and subsequent discharging in deposition section 112.
In certain embodiments of the present invention, deposition section 112 further includes an extension 112b, the both ends extension 112b difference
It is connect with side surface 112a and bottom surface 112c, the cross-sectional area of extension 112b remains unchanged.
In certain embodiments of the present invention, hydro-reduction device 100 further includes an exhaust gas processing device 180, at tail gas
Reason device 180 includes one first offgas duct 181 for being passed through tail gas being sequentially communicated, the process tank for handling tail gas
182 and one second offgas duct 183 for tail gas to be discharged, through bottom surface 112c and heavy before and after the front end of the first offgas duct 181
The product connection of section 112 forms an offgas outlet.The tail gas of the present apparatus includes hydrogen chloride gas, unreacted arsenic trichloride, hydrogen, nitrogen
Gas, stores pure water in process tank 182, the first pure water seal of offgas duct 181, then hydrogen chloride gas, unreacted tri-chlorination
Arsenic is by absorbing pure water, and hydrogen and nitrogen then pass through the discharge of the second offgas duct 183.First offgas duct 181 can also with pure water seal
It enough prevents from the oxygen in air from entering reaction quartz ampoule to mix and explode with hydrogen.
In certain embodiments of the present invention, a heating plate 170 is additionally provided in extension 112b, heating plate 170 includes one
Vertical portion 171 and a horizontal part 172, horizontal part 172 are vertically fixed on bottom surface 112c, and vertical portion 171 is embedded in a heating
Silk 173, the heating temperature of heater strip 173 are 600-900 DEG C, and the front that vertical portion 171 is located at offgas outlet forms barrier.Prolonging
The purpose of setting heating plate 170 is in long portion 112b: the unreacted arsenic trichloride that mixes in air-flow, hydrogen are here again
Reduction reaction occurs, the front formation barrier that vertical portion 171 is located at offgas outlet is also able to extend air-flow and enters tail gas recycle dress
It sets for 180 time, increases the time of contact of arsenic trichloride, hydrogen, promote reactivity and conversion ratio.
In certain embodiments of the present invention, the first branch pipe 141, the second branch pipe 142, hydrogen inlet 150 and nitrogen into
It is equipped with a control valve 145 on port 160, a relief valve 143 is also connected on the second branch pipe 142.The purpose of relief valve 143 is set
It is to prevent the blocking of the second branch pipe 142 from causing stress excessively high, once the second branch pipe 142 blocks, relief valve 143 can be passed through
Pressure release.The purpose that control valve 145 is arranged is to control the gas flow of each pipeline.
In certain embodiments of the present invention, the heater for heating to evaporating kettle 130 is set below evaporating kettle 130
131, because being placed with the arsenic trichloride of liquid in evaporating kettle, heater 131 is vaporizated into the arsenic trichloride of liquid for heat supply
Gaseous arsenic trichloride.
In certain embodiments of the present invention, the first branch pipe 141 cladding is provided with the warmer 144 for heat preservation, protects
The effect of warm device 144 is to keep the temperature the arsenic trichloride for preventing gaseous arsenic trichloride from liquefying in the first branch pipe for liquid.
In certain embodiments of the present invention, the heating temperature of the first heating zone 121 is 800-900 DEG C；Second heating zone
122 heating temperature is 600-800 DEG C；The heating temperature of third heating zone 123 is 300-400 DEG C.The subregion of heating mantle 120 adds
The arsenic trichloride and hydrogen that heat is convenient in air-flow occur reduction reaction in loading area 111a and generate arsenic and hydrogen chloride, and with air-flow
By buffer area 111b and deposition section 112, arsenic is deposited in deposition section.
The operational process of this hydro-reduction device 100 are as follows: the liquid under the heat effect of heater 131, in evaporating kettle 130
The vaporization of state arsenic trichloride becomes gaseous arsenic trichloride, enters air inlet pipe 140, reduction tube 111c by the first branch pipe 141, with this
Meanwhile hydrogen and nitrogen also enter air inlet pipe 140, reduction tube 111c by the second branch pipe 142, arsenic trichloride and hydrogen occur
Gas-gas reduction reaction generates arsenic and hydrogen chloride, then includes arsenic, hydrogen chloride, hydrogen, nitrogen and unreacted three in mixed airflow
Arsenic chloride, mixed airflow is by buffer area 111b and deposition section 112, and because deposition 112 temperature of section is lower, arsenic is deposited on deposition section
In 112, when mixed airflow passes through heating plate 170, unreacted arsenic trichloride, the hydrogen mixed in air-flow occurs also here
Original reaction, increases reactivity, then tail gas enters exhaust gas processing device 180.
The single furnace production capacity of this hydro-reduction device 100 is big, reduces heating energy consumption；Gas-gas reaction improves reaction efficiency；It is logical
Increase heating plate 170 is crossed, reaction conversion ratio is high；Arsenic is directly collected in deposition section 112, is operated easier.
Although for illustrative purposes, the preferred embodiment of the present invention is had been disclosed, but the ordinary skill people of this field
Member will realize without departing from the scope and spirit of the invention as disclosed by the appended claims, various to change
Into, increase and replace be possible.
Claims (10)
1. a kind of hydro-reduction device, it is characterised in that: it includes a horizontal positioned reaction quartz ampoule, for giving reaction quartz
One heating mantle of pipe heating, an evaporating kettle, an air inlet pipe, the reaction quartz ampoule includes a conversion zone and one deposits section, described
Conversion zone includes a loading area and a buffer area, and the buffer area and deposition section are adjacent, and the heating mantle includes one first heating
Area, one second heating zone and a third heating zone, first heating zone, the second heating zone, third heating zone respectively correspond packet
It is overlying on loading area, buffer area, deposition section, a reduction tube is fixed in the loading area, reduction tube is inserted into one end of the air inlet pipe
Interior, the other end bifurcated of the air inlet pipe is the first branch pipe and the second branch pipe, and first branch pipe is connected to evaporating kettle, described the
Two branch pipes are connected to a hydrogen inlet and a nitrogen inlet.
2. the hydro-reduction device according to claim 1, it is characterised in that: the deposition section includes rotary table side wall shape
One side surface and a bottom surface for sealing, the side surface gradually increase along the direction cross-sectional area far from buffer area
Greatly, the angle that the extended line of the rotary table bus and both rotary table axis of the side surface is formed is between 0-45 °.
3. the hydro-reduction device according to claim 2, it is characterised in that: the rotary table bus and rotary table of the side surface
The angle that the extended line of both axis is formed is 15 °.
4. according to any hydro-reduction device of Claims 2 or 3, it is characterised in that: the deposition section further includes prolonging
Long portion, the extension both ends are connect with side surface and bottom surface respectively, and the cross-sectional area of the extension remains unchanged.
5. the hydro-reduction device according to claim 4, it is characterised in that: the hydro-reduction device further includes a tail
Flash Gas Compression Skid System, the exhaust gas processing device include being sequentially communicated for being passed through one first offgas duct of tail gas, for handling
One process tank of tail gas and one second offgas duct for tail gas to be discharged run through bottom surface before and after the front end of first offgas duct
It is connected to form an offgas outlet with deposition section.
6. the hydro-reduction device according to claim 5, it is characterised in that: a heating plate is additionally provided in the extension,
The heating plate includes a vertical portion and a horizontal part, and the horizontal part is vertically fixed on bottom surface, and the vertical portion is embedded
Enter a heater strip, the heating temperature of the heater strip is 600-900 DEG C, and the front that the vertical portion is located at offgas outlet forms screen
Barrier.
7. the hydro-reduction device according to claim 6, it is characterised in that: first branch pipe, the second branch pipe, hydrogen
It is equipped with a control valve on air inlet and nitrogen inlet, is also connected with a relief valve on second branch pipe.
8. the hydro-reduction device according to claim 1, it is characterised in that: setting is steamed for giving below the evaporating kettle
Send out a heater of kettle heating.
9. the hydro-reduction device according to claim 1, it is characterised in that: the first branch pipe cladding, which is provided with, to be used for
One warmer of heat preservation.
10. the hydro-reduction device according to claim 1, it is characterised in that: the heating temperature of first heating zone is
800-900℃；The heating temperature of second heating zone is 600-800 DEG C；The heating temperature of the third heating zone is 300-
400℃。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710979046.6A CN109680165B (en) | 2017-10-19 | 2017-10-19 | Hydrogenation reduction device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710979046.6A CN109680165B (en) | 2017-10-19 | 2017-10-19 | Hydrogenation reduction device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109680165A true CN109680165A (en) | 2019-04-26 |
| CN109680165B CN109680165B (en) | 2020-10-27 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710979046.6A Active CN109680165B (en) | 2017-10-19 | 2017-10-19 | Hydrogenation reduction device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109680165B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114538756A (en) * | 2022-03-15 | 2022-05-27 | 广东先导微电子科技有限公司 | Charging mold for high-purity arsenic and repairing method thereof |
| CN114717429A (en) * | 2022-04-18 | 2022-07-08 | 广东先导微电子科技有限公司 | Arsenic trichloride reduction device and arsenic trichloride reduction method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB875898A (en) * | 1959-04-13 | 1961-08-23 | Ass Elect Ind | Improved process for the purification of arsenic |
| CN101935767A (en) * | 2010-09-26 | 2011-01-05 | 山西龙港高纯材料有限公司 | Method for preparing high-purity arsenic |
| CN104975191A (en) * | 2015-07-17 | 2015-10-14 | 广东先导稀材股份有限公司 | Hydrogenation reduction device for high-purity arsenic production and high-purity arsenic preparing method |
-
2017
- 2017-10-19 CN CN201710979046.6A patent/CN109680165B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB875898A (en) * | 1959-04-13 | 1961-08-23 | Ass Elect Ind | Improved process for the purification of arsenic |
| CN101935767A (en) * | 2010-09-26 | 2011-01-05 | 山西龙港高纯材料有限公司 | Method for preparing high-purity arsenic |
| CN104975191A (en) * | 2015-07-17 | 2015-10-14 | 广东先导稀材股份有限公司 | Hydrogenation reduction device for high-purity arsenic production and high-purity arsenic preparing method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114538756A (en) * | 2022-03-15 | 2022-05-27 | 广东先导微电子科技有限公司 | Charging mold for high-purity arsenic and repairing method thereof |
| CN114538756B (en) * | 2022-03-15 | 2023-12-26 | 广东先导微电子科技有限公司 | Charging mould for high-purity arsenic and repairing method thereof |
| CN114717429A (en) * | 2022-04-18 | 2022-07-08 | 广东先导微电子科技有限公司 | Arsenic trichloride reduction device and arsenic trichloride reduction method |
| CN114717429B (en) * | 2022-04-18 | 2023-12-26 | 广东先导微电子科技有限公司 | Arsenic trichloride reduction device and arsenic trichloride reduction method |
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| Publication number | Publication date |
|---|---|
| CN109680165B (en) | 2020-10-27 |
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Application publication date: 20190426 Assignee: Guangdong lead Microelectronics Technology Co.,Ltd. Assignor: FIRST SEMICONDUCTOR MATERIALS Co.,Ltd. Contract record no.: X2023990000449 Denomination of invention: Hydrogenation reduction device Granted publication date: 20201027 License type: Common License Record date: 20230505 |