CN208234963U - A kind of equipment of arsenic lead mixed vapour fractional condensaion - Google Patents

A kind of equipment of arsenic lead mixed vapour fractional condensaion Download PDF

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Publication number
CN208234963U
CN208234963U CN201820336446.5U CN201820336446U CN208234963U CN 208234963 U CN208234963 U CN 208234963U CN 201820336446 U CN201820336446 U CN 201820336446U CN 208234963 U CN208234963 U CN 208234963U
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quartz ampoule
equipment
arsenic
heating zone
temperature measuring
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李夫
李一夫
蒲正浩
杨斌
徐宝强
刘大春
田阳
蒋文龙
熊能
张环
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The utility model relates to a kind of equipment of arsenic lead mixed vapour fractional condensaion, belong to alloy separation equipment technical field.The device includes vacuum evacuation device, flange, temperature measuring equipment, classification vacuum furnace body, quartz ampoule, charging ram, control cabinet, heating zone and recycling foil, and the quartz length of tube is 1.2 ~ 2m;Heating zone length is 0.15 ~ 0.25m;A temperature measuring equipment is arranged every 2 ~ 3cm in quartz ampoule.This equipment forms certain temperature gradient in quartz ampoule, condenses material within the scope of corresponding temperature, realizes the purpose efficiently separated;This application method and process is simple.

Description

A kind of equipment of arsenic lead mixed vapour fractional condensaion
Technical field
The utility model relates to a kind of equipment of arsenic lead mixed vapour fractional condensaion, belong to alloy separation equipment technology neck Domain.
Background technique
Arsenic, lead are non-ferrous metal metallurgies, cause the most important element of environmental pollution in removal process, handle such material Conventional method is that high-temperature fusion is segregated or is electrolysed, but such methods energy consumption is high and easily causes damages to environment.Vacuum distillation is A kind of green, environmental protection smelting process, can be used for metallurgical production process.But traditional vacuum distillation equipment is difficult to realize to temperature Control, cause volatile matter condensation together, be unfavorable for recycling.
Patent CN201210040524.4 discloses a kind of tin smelting aluminium slag environment-friendly treatment method, and the tin smelts aluminium slag For environment-friendly treatment method i.e. by aluminium slag by reduction shaft furnace melting, harmful element arsenic, antimony and tin therein generate tin arsenic antimony alloy, tin Arsenic antimony alloy obtains the earth of positive pole of scolding tin and rich antimony arsenic silver through being electrolysed, to achieve the purpose that tin is separated with arsenic antimony.But this method walks It is rapid complex, and a large amount of waste water can be generated by electrolysis, it is unfavorable for environmental requirement.
Patent CN200910095112.9 discloses a kind of method for separating multi-element alloy of lead, bismuth, gold, silver and copper, the separation lead The method of bismuth gold, silver and bronze multicomponent alloy is that multicomponent alloy is handled using the method for vacuum distillation, and vapo(u)rizing temperature is 1050 ~ 1100 DEG C, Distillation time is 60 ~ 80min, and vacuum degree is 5 ~ 15Pa in furnace, can be by feed separation at volatile matter (lead, bismuth alloy) and residual Object (gold, silver, copper alloy).But volatile substance collected by this method is still alloy, need to further separate, it is wide to constrain vacuum drying oven General application and development.
Therefore, it is necessary to develop a kind of method for efficiently separating arsenic lead materials recycling elemental arsenic, lead, simplification of flowsheet, peace Entirely, efficiently, it is pollution-free, reduce element loss.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, it is cold that the utility model provides a kind of arsenic lead mixed vapour classification Solidifying equipment.This equipment forms certain temperature gradient in quartz ampoule, condenses material within the scope of corresponding temperature, realizes The purpose efficiently separated;This application method and process is simple.The utility model is achieved through the following technical solutions.
A kind of equipment of arsenic lead mixed vapour fractional condensaion, including vacuum evacuation device, flange, temperature measuring equipment, classification vacuum Furnace body, quartz ampoule, charging ram, control cabinet, heating zone and recycling foil, quartz ampoule one end pass through flanged joint vacuum evacuation device, stone English pipe other end inner sealing is equipped with can be equipped with recycling layers of foil, quartz ampoule inside the charging ram of quartzy in-pipe, quartz ampoule Middle position region is equipped with heating zone, constitutes outside quartz ampoule equipped with furnace shell and is classified vacuum furnace body, equal at the top of classification vacuum furnace body Several temperature measuring equipments of even insertion and each temperature measuring equipment with contacted at the top of quartz ampoule, classification vacuum furnace body bottom is equipped with control Cabinet, controller in control cabinet respectively with the heating device of heating zone, several temperature measuring equipments and vacuum evacuation device mechanical pump electricity Connection;
The quartz length of tube is 1.2 ~ 2m;Heating zone length is 0.15 ~ 0.25m;Quartz ampoule is arranged one every 2 ~ 3cm Temperature measuring equipment.
The temperature measuring equipment is K-type or Pt-Rh type thermocouple.
The heating zone heating device is resistance heating.
The recycling foil is graphite foil or metal foil, with a thickness of 0.2 ~ 0.4mm.
A kind of application method of the equipment of arsenic lead mixed vapour fractional condensaion, the specific steps of which are as follows:
Arsenic lead materials are placed in quartz ampoule and with charging ram against arsenic lead materials by step 1, then will be equipped with charging ram One side seal of quartz ampoule, controller controls vacuum evacuation device and quartzy intraductal pressure is evacuated to 0.1 ~ 50Pa, control heating The heating temperature of the heating device in area is 800 ~ 1100 DEG C, and arsenic lead materials are then pushed into heating zone by charging ram, heat preservation 60 ~ 120min is evaporated in vacuo to obtain arsenic steam and lead steam;
Step 2, the quartz ampoule regional temperature close to heating zone are high, and the regional temperature of quartz ampoule two sides is low, through step 1 vacuum Obtained lead steam is distilled close to heating zone and recycling foil region that temperature is 480 ~ 700 DEG C condenses, and is evaporated in vacuo through step 1 Obtained arsenic steam recycles foil region in the low temperature that temperature is 110 ~ 300 DEG C and condenses.
Arsenic content is 1 ~ 50wt% in the arsenic lead materials.
The beneficial effects of the utility model are:
1, the utility model, can be in quartz by the control to heating temperature and soaking time during distillation Certain temperature gradient is formed in pipe.It condenses material within the scope of corresponding temperature, realizes the purpose efficiently separated.
2, the temperature that the utility model can be fed back according to thermocouple adjusts Heating Zone Temperature, controls temperature gradient, to realize The accurate recycling of material.
3, the utility model can be not only used for processing arsenic lead materials, can be also used for different a variety of of processing condensation property Metal alloy such as lead antimony, lead arsenic antimony alloy etc..Use process is safe and pollution-free.At the same time, using utility model device Fundamental research is carried out to alloy purification technique.
Detailed description of the invention
Fig. 1 is the utility model structure diagram;
Fig. 2 is the utility model classification vacuum furnace body schematic cross-sectional view.
In figure: 1- vacuum evacuation device, 2- flange, 3- temperature measuring equipment, 4- classification vacuum furnace body, 5- quartz ampoule, 6- charging ram, 7- control cabinet, the heating zone 8-.
Specific embodiment
With reference to the accompanying drawings and detailed description, the utility model is described in further detail.
Embodiment 1
As illustrated in fig. 1 and 2, the equipment of the arsenic lead mixed vapour fractional condensaion, including vacuum evacuation device 1, flange 2, thermometric Device 3, classification vacuum furnace body 4, quartz ampoule 5, charging ram 6, control cabinet 7, heating zone 8 and recycling foil, 5 one end of quartz ampoule passes through method Orchid 2 connects vacuum evacuation device 1, and 5 other end inner sealing of quartz ampoule is equipped with the charging ram 6 that can be moved in quartz ampoule 5, quartz ampoule 5 inside are equipped with recycling layers of foil, and 5 middle position region of quartz ampoule is equipped with heating zone 8, is equipped with furnace shell outside quartz ampoule 5 and constitutes classification Vacuum furnace body 4, several temperature measuring equipments 3 are uniformly inserted at 4 top of classification vacuum furnace body and each temperature measuring equipment 3 is pushed up with quartz ampoule 5 Portion's contact, classification 4 bottom of vacuum furnace body are equipped with control cabinet 7, the controller in control cabinet 7 respectively with the heating device of heating zone 8, Several temperature measuring equipments 3 and the electrical connection of 1 mechanical pump of vacuum evacuation device;
Wherein 5 length of quartz ampoule is 1.2m;8 length of heating zone is 0.15m;Quartz ampoule 5 is arranged a thermometric every 2cm and fills Set 3;Temperature measuring equipment 3 is K-type thermocouple;8 heating device of heating zone is resistance heating;Recycling foil is graphite foil, with a thickness of 0.2mm。
The application method of the equipment of the arsenic lead mixed vapour fractional condensaion, the specific steps of which are as follows:
20g arsenic lead materials (arsenic content is 3.34wt% in arsenic lead materials, remaining as lead) are placed on quartz ampoule 5 by step 1 It is interior and with charging ram 6 abut arsenic lead materials, then will be equipped with charging ram 65 one side seal of quartz ampoule, controller control vacuumize Pressure in quartz ampoule 5 is evacuated to 1 ~ 10Pa by device 1, and the heating temperature for controlling the heating device of heating zone 8 is 850 DEG C, so Arsenic lead materials are pushed into heating zone 8 by charging ram 6 afterwards, heat preservation 100min is evaporated in vacuo to obtain arsenic steam and lead steam;
Step 2,5 regional temperature of quartz ampoule close to heating zone 8 are high, and the regional temperature of 5 two sides of quartz ampoule is low, through step 1 Obtained lead steam is evaporated in vacuo close to heating zone 8 and recycling foil region that temperature is 510 ~ 700 DEG C condenses, it is true through step 1 The arsenic steam that sky distillation obtains recycles foil region in the low temperature that temperature is 120 ~ 300 DEG C and condenses, and condensation obtains purity and is The lead bullion of 99.82wt% and the crude arsenic of 99.91wt%.
Embodiment 2
As illustrated in fig. 1 and 2, the equipment of the arsenic lead mixed vapour fractional condensaion, including vacuum evacuation device 1, flange 2, thermometric Device 3, classification vacuum furnace body 4, quartz ampoule 5, charging ram 6, control cabinet 7, heating zone 8 and recycling foil, 5 one end of quartz ampoule passes through method Orchid 2 connects vacuum evacuation device 1, and 5 other end inner sealing of quartz ampoule is equipped with the charging ram 6 that can be moved in quartz ampoule 5, quartz ampoule 5 inside are equipped with recycling layers of foil, and 5 middle position region of quartz ampoule is equipped with heating zone 8, is equipped with furnace shell outside quartz ampoule 5 and constitutes classification Vacuum furnace body 4, several temperature measuring equipments 3 are uniformly inserted at 4 top of classification vacuum furnace body and each temperature measuring equipment 3 is pushed up with quartz ampoule 5 Portion's contact, classification 4 bottom of vacuum furnace body are equipped with control cabinet 7, the controller in control cabinet 7 respectively with the heating device of heating zone 8, Several temperature measuring equipments 3 and the electrical connection of 1 mechanical pump of vacuum evacuation device;
Wherein 5 length of quartz ampoule is 1.2m;8 length of heating zone is 0.15m;Quartz ampoule 5 is arranged a thermometric every 2cm and fills Set 3;Temperature measuring equipment 3 is K-type thermocouple;8 heating device of heating zone is resistance heating;Recycling foil is graphite foil, with a thickness of 0.2mm。
The application method of the equipment of the arsenic lead mixed vapour fractional condensaion, the specific steps of which are as follows:
Step 1, by 30g arsenic lead materials, (arsenic lead materials are tin-lead arsenic alloy, and Theil indices 30wt%, arsenic contain in tin-lead arsenic alloy Amount is 5wt%, remaining as lead) it is placed in quartz ampoule 5 and with charging ram 6 against arsenic lead materials, it then will be equipped with charging ram 6 5 one side seal of quartz ampoule, controller control vacuum evacuation device 1 and pressure in quartz ampoule 5 are evacuated to 1 ~ 10Pa, control heating zone The heating temperature of 8 heating device is 900 DEG C, arsenic lead materials is then pushed into heating zone 8 by charging ram 6, heat preservation 60min is carried out Vacuum distillation obtains the tin in arsenic steam and lead steam and remaining crucible;
Step 2,5 regional temperature of quartz ampoule close to heating zone 8 are high, and the regional temperature of 5 two sides of quartz ampoule is low, through step 1 Obtained lead steam is evaporated in vacuo close to heating zone 8 and recycling foil region that temperature is 480 ~ 680 DEG C condenses, it is true through step 1 The arsenic steam that sky distillation obtains recycles foil region in the low temperature that temperature is 110 ~ 280 DEG C and condenses, and condensation obtains purity and is The thick tin that the lead bullion of 99.91wt% and the crude arsenic of 99.87wt% and crucible moderate purity are 99.32wt %.
Embodiment 3
As illustrated in fig. 1 and 2, the equipment of the arsenic lead mixed vapour fractional condensaion, including vacuum evacuation device 1, flange 2, thermometric Device 3, classification vacuum furnace body 4, quartz ampoule 5, charging ram 6, control cabinet 7, heating zone 8 and recycling foil, 5 one end of quartz ampoule passes through method Orchid 2 connects vacuum evacuation device 1, and 5 other end inner sealing of quartz ampoule is equipped with the charging ram 6 that can be moved in quartz ampoule 5, quartz ampoule 5 inside are equipped with recycling layers of foil, and 5 middle position region of quartz ampoule is equipped with heating zone 8, is equipped with furnace shell outside quartz ampoule 5 and constitutes classification Vacuum furnace body 4, several temperature measuring equipments 3 are uniformly inserted at 4 top of classification vacuum furnace body and each temperature measuring equipment 3 is pushed up with quartz ampoule 5 Portion's contact, classification 4 bottom of vacuum furnace body are equipped with control cabinet 7, the controller in control cabinet 7 respectively with the heating device of heating zone 8, Several temperature measuring equipments 3 and the electrical connection of 1 mechanical pump of vacuum evacuation device;
Wherein 5 length of quartz ampoule is 2m;8 length of heating zone is 0.25m;A temperature measuring equipment is arranged every 3cm in quartz ampoule 5 3;Temperature measuring equipment 3 is K-type thermocouple;8 heating device of heating zone is resistance heating;Recycling foil is graphite foil, with a thickness of 0.4mm.
The application method of the equipment of the arsenic lead mixed vapour fractional condensaion, the specific steps of which are as follows:
Step 1,20g arsenic lead materials (arsenic content is 1wt% in arsenic lead materials, remaining as lead) are placed in quartz ampoule 5 and Arsenic lead materials are abutted with charging ram 6, then will be equipped with 5 one side seal of quartz ampoule of charging ram 6, controller controls vacuum evacuation device Pressure in quartz ampoule 5 is evacuated to 0.1 ~ 5Pa by 1, and the heating temperature for controlling the heating device of heating zone 8 is 800 DEG C, then will Arsenic lead materials are pushed into heating zone 8 by charging ram 6, and heat preservation 120min is evaporated in vacuo to obtain arsenic steam and lead steam;
Step 2,5 regional temperature of quartz ampoule close to heating zone 8 are high, and the regional temperature of 5 two sides of quartz ampoule is low, through step 1 Obtained lead steam is evaporated in vacuo close to heating zone 8 and recycling foil region that temperature is 500 ~ 660 DEG C condenses, it is true through step 1 The arsenic steam that sky distillation obtains recycles foil region in the low temperature that temperature is 110 ~ 220 DEG C and condenses.
Embodiment 4
As illustrated in fig. 1 and 2, the equipment of the arsenic lead mixed vapour fractional condensaion, including vacuum evacuation device 1, flange 2, thermometric Device 3, classification vacuum furnace body 4, quartz ampoule 5, charging ram 6, control cabinet 7, heating zone 8 and recycling foil, 5 one end of quartz ampoule passes through method Orchid 2 connects vacuum evacuation device 1, and 5 other end inner sealing of quartz ampoule is equipped with the charging ram 6 that can be moved in quartz ampoule 5, quartz ampoule 5 inside are equipped with recycling layers of foil, and 5 middle position region of quartz ampoule is equipped with heating zone 8, is equipped with furnace shell outside quartz ampoule 5 and constitutes classification Vacuum furnace body 4, several temperature measuring equipments 3 are uniformly inserted at 4 top of classification vacuum furnace body and each temperature measuring equipment 3 is pushed up with quartz ampoule 5 Portion's contact, classification 4 bottom of vacuum furnace body are equipped with control cabinet 7, the controller in control cabinet 7 respectively with the heating device of heating zone 8, Several temperature measuring equipments 3 and the electrical connection of 1 mechanical pump of vacuum evacuation device;
Wherein 5 length of quartz ampoule is 1.8m;8 length of heating zone is 0.20m;Quartz ampoule 5 is arranged a thermometric every 3cm and fills Set 3;Temperature measuring equipment 3 is K-type thermocouple;8 heating device of heating zone is resistance heating;Recycling foil is graphite foil, with a thickness of 0.3mm。
The application method of the equipment of the arsenic lead mixed vapour fractional condensaion, the specific steps of which are as follows:
20g arsenic lead materials (arsenic content is 50wt% in arsenic lead materials, remaining as lead) are placed in quartz ampoule 5 by step 1 And arsenic lead materials are abutted with charging ram 6, it then will be equipped with 5 one side seal of quartz ampoule of charging ram 6, controller controls vacuum means It sets 1 and pressure in quartz ampoule 5 is evacuated to 40 ~ 50Pa, the heating temperature for controlling the heating device of heating zone 8 is 1100 DEG C, so Arsenic lead materials are pushed into heating zone 8 by charging ram 6 afterwards, heat preservation 60min is evaporated in vacuo to obtain arsenic steam and lead steam;
Step 2,5 regional temperature of quartz ampoule close to heating zone 8 are high, and the regional temperature of 5 two sides of quartz ampoule is low, through step 1 Obtained lead steam is evaporated in vacuo close to heating zone 8 and recycling foil region that temperature is 520 ~ 700 DEG C condenses, it is true through step 1 The arsenic steam that sky distillation obtains recycles foil region in the low temperature that temperature is 180 ~ 300 DEG C and condenses.
In conjunction with attached drawing, the specific embodiments of the present invention are described in detail above, but the utility model is not Be limited to above embodiment, within the knowledge of a person skilled in the art, can also do not depart from it is practical Various changes can be made under the premise of novel objective.

Claims (4)

1. a kind of equipment of arsenic lead mixed vapour fractional condensaion, it is characterised in that: including vacuum evacuation device (1), flange (2), survey Warm device (3), classification vacuum furnace body (4), quartz ampoule (5), charging ram (6), control cabinet (7), heating zone (8) and recycling foil, stone By flange (2) connection vacuum evacuation device (1), quartz ampoule (5) other end inner sealing is equipped with can be in quartz ampoule for English pipe (5) one end (5) charging ram (6) moved in, quartz ampoule (5) is internal to be equipped with recycling layers of foil, and quartz ampoule (5) middle position region is equipped with heating Area (8) is equipped with furnace shell outside quartz ampoule (5) and constitutes classification vacuum furnace body (4), and classification vacuum furnace body (4) is if top uniformly insertion Dry temperature measuring equipment (3) and each temperature measuring equipment (3) with contact at the top of quartz ampoule (5), classification vacuum furnace body (4) bottom, which is equipped with, to be controlled Cabinet (7) processed, controller in control cabinet (7) respectively with the heating device of heating zone (8), several temperature measuring equipments (3) and take out true Empty device (1) mechanical pump electrical connection;
Quartz ampoule (5) length is 1.2 ~ 2m;Heating zone (8) length is 0.15 ~ 0.25m;Quartz ampoule (5) is set every 2 ~ 3cm Set a temperature measuring equipment (3).
2. the equipment of arsenic lead mixed vapour fractional condensaion according to claim 1, it is characterised in that: the temperature measuring equipment It (3) is K-type or Pt-Rh type thermocouple.
3. the equipment of arsenic lead mixed vapour fractional condensaion according to claim 1, it is characterised in that: the heating zone (8) Heating device is resistance heating.
4. the equipment of arsenic lead mixed vapour fractional condensaion according to claim 1, it is characterised in that: the recycling foil is stone Black foil or metal foil, with a thickness of 0.2 ~ 0.4mm.
CN201820336446.5U 2018-03-13 2018-03-13 A kind of equipment of arsenic lead mixed vapour fractional condensaion Active CN208234963U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108285983A (en) * 2018-03-13 2018-07-17 昆明理工大学 A kind of equipment and its application process of arsenic lead mixed vapour fractional condensaion
CN111960389A (en) * 2020-08-24 2020-11-20 昆明理工大学 Method for recycling metal tellurium from tellurium-containing waste through vacuum fractional condensation

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108285983A (en) * 2018-03-13 2018-07-17 昆明理工大学 A kind of equipment and its application process of arsenic lead mixed vapour fractional condensaion
CN111960389A (en) * 2020-08-24 2020-11-20 昆明理工大学 Method for recycling metal tellurium from tellurium-containing waste through vacuum fractional condensation

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