CN204255077U - A kind of antimony reduction furnace - Google Patents

A kind of antimony reduction furnace Download PDF

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Publication number
CN204255077U
CN204255077U CN201420640907.XU CN201420640907U CN204255077U CN 204255077 U CN204255077 U CN 204255077U CN 201420640907 U CN201420640907 U CN 201420640907U CN 204255077 U CN204255077 U CN 204255077U
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furnace
reduction
pipe
quartz ampoule
reduction furnace
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种娜
詹科
曹昌威
向明川
李强
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EMEI SEMICONDUCTOR MATERIAL INSTITUTE
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EMEI SEMICONDUCTOR MATERIAL INSTITUTE
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Abstract

The utility model discloses a kind of antimony reduction furnace, comprise the reduction furnace furnace shell of quartz ampoule, resistance furnace and band peep hole, resistance furnace is placed in reduction furnace furnace shell, quartz ampoule is horizontally through the axis of reduction furnace furnace shell, and is positioned in resistance furnace, and described quartz ampoule comprises pipe, tail gas discharging pipe and discharge nozzle in reduction tube, in reduction tube, pipe is obliquely installed in quartz ampoule, its feed end is higher than discharge end, and in reduction tube, the feed end of pipe is provided with feed pipe and air inlet pipe, and discharge end is uncovered structure; The feed end of quartz ampoule is all located at by tail gas discharging pipe and discharge nozzle, and the end of tail gas discharging pipe connects exhaust gas processing device, and the bottom surface of quartz ampoule is located at by discharge nozzle; Resistance furnace is provided with resistance wire, and resistance wire connects electrical control gear.This antimony reduction furnace adopts self-emptying, avoids personnel to spatter wound by high-temperature metal drop in discharging process, and safety coefficient improves, and equipment operating is simple, easily manufactured, production and reduction efficiency high, production and application cost is low.

Description

A kind of antimony reduction furnace
Technical field
The utility model relates to a kind of antimony reduction furnace, particularly relates to a kind of assembly of reduction furnace of high pure metal antimony, belongs to high pure metal purifying plant technical field.
Background technology
High purity antimony refers to the high pure metal antimony of more than 5N, and mainly for the preparation of semi-conducting material, it can form the compound semiconductors such as aluminium antimonide, gallium antimonide, indium antimonide; As the adulterant of the monocrystalline such as semiconductor Germanium, silicon, it is made to form N-type semiconductor; In addition, other high pure metal alloys of preparation can also be used as.In some photoelectric fields, as infrared acquisition, piezoelectricity, the electronic original part such as pressure-sensitive, property material based on it, General Requirements metal purity is at 5-7N.The preparation of high purity antimony is mainly through process implementations such as chlorination, rectifying, reduction, distillations.
Because traditional high purity antimony reduction apparatus is vertical heater, quartz ampoule and reduction furnace are placed vertically, and raw material and hydrogen are entered by upper end feed pipe, carry out reacting after gas-liquid distributed contact, be deposited on below quartz ampoule through quartz filler ring; Below quartz ampoule, siphon pipe is set; During discharging, product material is flowed out in splicing boat by siphon.There is following weak point in this device:
Body of heater
1. be plumbness, in discharging process, product easily spatters and hurts sb.'s feelings;
2., due to no liquid in quartz ampoule, when liquid flows downward along packing layer, have the phenomenon of deflection tube wall flowing, distributor easily produces wall stream, and then causes gas-liquid skewness in packing layer, and mass-transfer efficiency is declined, and reduction reaction efficiency reduces;
3. the inlet amount of reduction reaction is limited, causes production efficiency low;
4. reduction furnace is without liquid level peep hole, cannot determine liquid level in quartz ampoule, when liquid level exceedes pipe height in quartz ampoule, easily security incident occurs;
5. during the tail gas recycle produced in production process, need connect tracheae separately, owing to containing hydrogen in tail gas, misoperation easily sets off an explosion, and there is certain potential safety hazard.
Utility model content
The purpose of this utility model is: provide a kind of antimony reduction furnace, overcomes the shortcoming that traditional reduction furnace potential safety hazard is large, production cost is high, reduction efficiency is low, operation sequence is complicated, thus can effectively solve above-mentioned problems of the prior art.
The purpose of this utility model is realized by following technical proposals: a kind of antimony reduction furnace, comprise the reduction furnace furnace shell of quartz ampoule, resistance furnace and band peep hole, resistance furnace is placed in reduction furnace furnace shell, quartz ampoule is horizontally through the axis of reduction furnace furnace shell, and be positioned in resistance furnace, described quartz ampoule comprises pipe, tail gas discharging pipe and discharge nozzle in reduction tube, in reduction tube, pipe is obliquely installed in quartz ampoule, its feed end is higher than discharge end, in reduction tube, the feed end of pipe is provided with feed pipe and air inlet pipe, and discharge end is uncovered structure; The feed end of quartz ampoule is all located at by tail gas discharging pipe and discharge nozzle, and the end of tail gas discharging pipe connects exhaust gas processing device, and the bottom surface of quartz ampoule is located at by discharge nozzle; Resistance furnace is provided with resistance wire, and resistance wire connects electrical control gear.
As preferred embodiment, in described reduction tube, the center line of pipe becomes 20 ° of overturning angles with the center line of quartz ampoule.
As further preferred embodiment, thermocouple is three right, is located at the leading portion of reduction furnace furnace shell, stage casing and back segment respectively; Resistance wire is divided into three sections, is located at the leading portion of resistance furnace stove cylinder, stage casing and back segment respectively.
As further preferred embodiment, between resistance wire and reduction furnace furnace shell, be provided with spun-glass insulation cotton; Spun-glass insulation end that is cotton and reduction furnace furnace shell is provided with shrouding.
As preferred embodiment, described electrical control gear comprises total power switch and TIC thermoindicating controller, and reduction furnace furnace shell is provided with thermocouple, and thermocouple and resistance wire are by total power switch access TIC thermoindicating controller.
As preferred embodiment, also comprise servicing unit, described servicing unit comprises suspension ring and lifting motor, and described suspension ring are fixed on reduction furnace furnace shell, and one end of lifting motor and suspension ring mount.
As preferred embodiment, also comprise bracing or strutting arrangement, described bracing or strutting arrangement is the bearing supporting reduction furnace furnace shell.
In the utility model, the effect of part is as follows:
Quartz ampoule: as the capital equipment of antimony reduction furnace, for material reaction provides contact area and time of contact, and the storage of product, by the thermal release of absorption out for reaction provides required heat energy;
Spun-glass insulation is cotton: as the infrastructure device of antimony reduction furnace, plays insulation and certain supporting role, avoid the thermal losses of resistance wire, economize energy to stove cylinder;
Stove cylinder: as the capital equipment of antimony reduction furnace, is exotic material, can bears higher temperature, passes to quartz ampoule by the heat directly contacted resistance wire produces;
Thermocouple: as the infrastructure device of antimony reduction furnace, is measured the temperature of resistance wire, temperature signal is converted to electromotive force and current signal, and shown by Displaying Meter and control;
Reduction furnace furnace shell: as the auxiliary equipment of antimony reduction furnace, is fixed on spun-glass insulation cotton between stove cylinder, shields to quartz ampoule, has certain effect of heat insulation, reduces heat leakage, connects other auxiliary equipment.
Compared with prior art, the beneficial effects of the utility model:
1, this reduction furnace adopts self-emptying, overcomes the shortcoming of traditional siphon discharging, avoids personnel to spatter wound by high-temperature product in discharging process, and equipment operating is simple, and security is high;
2, reduction furnace and horizontal direction tilt, and product discharge is convenient; Reduction tube inner space is fully utilized, and is convenient to increase inventory, improves production capacity;
3, adopt three sections of temperature controls, be conducive to reaction zone temperature and control, improve reduction efficiency high, reduce production cost;
4, increase exhaust gas processing device, exhaust pipe directly accesses exhaust gas processing device, avoids the hydrogen in tail gas to meet high temperature, naked light and blasts; Exhaust treatment system can reduce environmental pollution simultaneously, and recycling becomes spent acid, and recycles, for suitability for industrialized production lays the foundation;
5, set up peep hole, liquid level and Product Status in quartz ampoule can be observed in time, determine charging when discharging time, improve safety coefficient;
6, equipment carries lifting motor and suspension ring, is convenient to charging and discharging, realizes automatically controlling, and reduces person works's amount.
Accompanying drawing explanation
Fig. 1 is the structural representation of the utility model antimony reduction furnace;
Fig. 2 is the structural representation of quartz ampoule in Fig. 1.
In figure: 1-quartz ampoule, 2-shrouding, 3-spun-glass insulation is cotton, 4-resistance wire, 5-stove cylinder, 6-thermocouple, 7-reduction furnace furnace shell, 8-suspension ring, 9-lifting motor, 10-bearing, 11-ground, 12-exhaust gas processing device, 13-discharging opening, 14-tail gas discharging pipe, 15-feed pipe, pipe in 16-reduction tube.
Detailed description of the invention
Below in conjunction with specific embodiment, the utility model is further described.
All features disclosed in this description, or the step in disclosed all methods or process, except the speciality mutually repelled and/or step, all can combine by any way, unless specifically stated otherwise, all can be replaced by other equivalences or the alternative features with similar object, namely, unless specifically stated otherwise, an embodiment in a series of equivalence of each feature or similar characteristics.
As shown in Figure 1, 2:
The utility model antimony reduction furnace comprises quartz ampoule 1, electrical control gear, resistance furnace, the reduction furnace furnace shell 7 of band peep hole, servicing unit and bracing or strutting arrangement.
Quartz ampoule 1 is horizontally through the axis of reduction furnace furnace shell 7, and is placed in resistance furnace.Quartz ampoule 1 comprises pipe 16 in reduction tube, tail gas discharging pipe 14 and discharge nozzle 13, and the end of tail gas discharging pipe 14 connects exhaust gas processing device 12.In reduction tube, pipe 16 is obliquely installed in quartz ampoule 1, in reduction tube, the feed end of pipe 16 is provided with feed pipe and air inlet pipe 15, discharge end is uncovered structure, the feed end of quartz ampoule 1 is all located at by tail gas discharging pipe 14 and discharge nozzle 13, the end of tail gas discharging pipe 14 connects exhaust gas processing device 12, and the bottom surface of quartz ampoule 1 is located at by discharge nozzle 13.In the present embodiment, in described reduction tube, the center line of pipe 16 becomes 20 ° of overturning angles with the center line of quartz ampoule 1; And its feed end is higher than discharge end.If angle of inclination is excessive, product discharge difficulty, if it is too small to dump angle, reduction tube capacity cannot be played, and inventory of once reducing is less, and production cost is high, therefore, the utility model adopts reduction furnace and horizontal direction to be 20 ° of angles, and whole reduction furnace is arranged on bearing 10, to reach best discharging effect.
For the ease of regulating its angle of inclination, be also provided with servicing unit, described servicing unit comprises suspension ring 8 and lifting motor 9, and described suspension ring 8 are fixed on reduction furnace furnace shell 7, and one end and the suspension ring 8 of lifting motor 9 mount.Bracing or strutting arrangement is the bearing 10 supporting reduction furnace furnace shell 7, and bearing 10 is located on ground 11.
The operation principle of this antimony reduction furnace is: before whole reduction furnace runs, and first connect feed pipe 15 and tail gas discharging pipe 14, feed pipe 15 connects feed arrangement, and tail gas discharging pipe 14 is communicated with exhaust gas processing device 12, seals discharging opening with plastic tube simultaneously; In quartz ampoule 1, pass into gas, adopt gradient heating, after furnace temperature is heated to design temperature, opens feed pipe 15 and pass into trichloride antimony and heat, make trichloride antimony and hydrogen generation reduction reaction.Observe the height of liquid level and the molten condition of product by the peep hole on reduction furnace furnace shell, thus determine the charge ratio of hydrogen and raw material.Trichloride antimony and hydrogen in reduction tube in pipe 16 after completion of the reaction, metallic antimony flows out from interior pipe, outer tube deposition, reaction terminate after, stop charging, close intake valve.Got ready by charging basket, take off out dipleg, to be tilted body of heater by suspension ring 8, antimony stream goes out shrend and becomes little antimony regulus, till having gone out.After completing, again open lifting motor 9, place body of heater aft mount 10.Course of reaction generates gas by tail gas discharging pipe 14, enters in exhaust gas processing device 12, regularly from sewer pipe discharge waste liquid.
Described resistance furnace comprises resistance furnace stove cylinder 5 and is wrapped in the resistance wire 4 of stove cylinder 5 outside, and resistance wire 4 connects electrical control gear.Described electrical control gear comprises total power switch and TIC thermoindicating controller, and reduction furnace furnace shell is provided with thermocouple 6, and thermocouple 6, resistance wire 4 are by total power switch access TIC thermoindicating controller; TIC controller connects power supply, resistance wire and thermocouple, is controlled to adjust, realize setting and the control of furnace temperature by the temperature data of reduction furnace sidewall thermocouple feedback to resistance wire electric current.The temperature of furnace shell two points is just surveyed in existing temperature survey, and the utility model adds a monitoring temperature measurement point, and this control point also can regulate temperature simultaneously.Thermocouple is used for thermometric, and temperature can directly be reflected in TIC thermoindicating controller, then regulates temperature by regulating power, that is to say, if temperature ratio requires low, with regard to increasing power, allows electric furnace heating wire heat up, reaches set point of temperature.Temperature due to reduction furnace controls to be three sections of temperature controls, therefore, can reach the temperature accurately controlling reduction furnace head, middle part, afterbody.
In addition, glass fibre moisturizing cotton 3 is provided with between resistance wire 4 and reduction furnace furnace shell 7; The end of spun-glass insulation cotton 3 and reduction furnace furnace shell 7 is provided with shrouding 2.
The reduction efficiency of antimony calculates according to the trichloride antimony dropped into and the last antimony gauge generated, trichloride antimony and hydrogen reaction generate antimony, this equipment adopts three sections of temperature controls, object increases the high-temperature area of reduction reaction, make reaction more abundant, reduction efficiency brings up to 80% by original 55%, improves yield rate.
The foregoing is only preferred embodiment of the present utility model; not in order to limit the utility model; all do within spirit of the present utility model and principle any amendment, equivalent to replace and improvement etc., all should be included within protection domain of the present utility model.

Claims (7)

1. an antimony reduction furnace, comprise quartz ampoule (1), the reduction furnace furnace shell (7) of resistance furnace and band peep hole, resistance furnace is placed in reduction furnace furnace shell (7), quartz ampoule (1) is horizontally through the axis of reduction furnace furnace shell (7), and be positioned in resistance furnace, it is characterized in that: described quartz ampoule (1) comprises pipe (16) in reduction tube, tail gas discharging pipe (14) and discharge nozzle (13), in reduction tube, pipe (16) is obliquely installed in quartz ampoule (1), its feed end is higher than discharge end, in reduction tube, the feed end of pipe (16) is provided with feed pipe and air inlet pipe (15), discharge end is uncovered structure, the feed end of quartz ampoule (1) is all located at by tail gas discharging pipe (14) and discharge nozzle (13), and the end of tail gas discharging pipe (14) connects exhaust gas processing device (12), and the bottom surface of quartz ampoule (1) is located at by discharge nozzle (13), resistance furnace is provided with resistance wire (4), and resistance wire (4) connects electrical control gear.
2. antimony reduction furnace as claimed in claim 1, is characterized in that: in described reduction tube, the center line of pipe (16) becomes 20 ° of overturning angles with the center line of quartz ampoule (1).
3. antimony reduction furnace as claimed in claim 2, is characterized in that: thermocouple (6) is three right, is located at the leading portion of reduction furnace furnace shell (7), stage casing and back segment respectively; Resistance wire (4) is divided into three sections, is located at the leading portion of resistance furnace stove cylinder (5), stage casing and back segment respectively.
4. antimony reduction furnace as claimed in claim 3, is characterized in that: be provided with spun-glass insulation cotton (3) between resistance wire (4) and reduction furnace furnace shell (7); The end of spun-glass insulation cotton (3) and reduction furnace furnace shell (7) is provided with shrouding (2).
5. antimony reduction furnace as claimed in claim 1, it is characterized in that: described electrical control gear comprises total power switch and TIC thermoindicating controller, reduction furnace furnace shell is provided with thermocouple (6), and thermocouple (6) and resistance wire (4) are by total power switch access TIC thermoindicating controller.
6. antimony reduction furnace as claimed in claim 1, it is characterized in that: also comprise servicing unit, described servicing unit comprises suspension ring (8) and lifting motor (9), and described suspension ring (8) are fixed on reduction furnace furnace shell (7), and one end and the suspension ring (8) of lifting motor (9) mount.
7. antimony reduction furnace as claimed in claim 1, is characterized in that: also comprise bracing or strutting arrangement, and described bracing or strutting arrangement is the bearing (10) supporting reduction furnace furnace shell (7).
CN201420640907.XU 2014-10-31 2014-10-31 A kind of antimony reduction furnace Active CN204255077U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105333733A (en) * 2015-11-25 2016-02-17 江西德义半导体科技有限公司 Vertical reduction furnace for high-purity antimony production
CN106802083A (en) * 2015-11-25 2017-06-06 衡阳恒荣高纯半导体材料有限公司 A kind of antimony reduction furnace
CN108411125A (en) * 2017-12-26 2018-08-17 中国恩菲工程技术有限公司 The extraction system of antimony metal
CN117248114A (en) * 2023-11-14 2023-12-19 昆明冶金研究院有限公司 Short-flow system for preparing metallic antimony and method for preparing metallic antimony

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105333733A (en) * 2015-11-25 2016-02-17 江西德义半导体科技有限公司 Vertical reduction furnace for high-purity antimony production
CN106802083A (en) * 2015-11-25 2017-06-06 衡阳恒荣高纯半导体材料有限公司 A kind of antimony reduction furnace
CN108411125A (en) * 2017-12-26 2018-08-17 中国恩菲工程技术有限公司 The extraction system of antimony metal
CN117248114A (en) * 2023-11-14 2023-12-19 昆明冶金研究院有限公司 Short-flow system for preparing metallic antimony and method for preparing metallic antimony
CN117248114B (en) * 2023-11-14 2024-02-02 昆明冶金研究院有限公司 Short-flow system for preparing metallic antimony and method for preparing metallic antimony

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