CN210261925U

CN210261925U - Small intermittent reduction distillation device

Info

Publication number: CN210261925U
Application number: CN201721680878.XU
Authority: CN
Inventors: 张波; 刘浪; 李春晓; 肖波
Original assignee: Hunan University of Technology
Current assignee: Hunan University of Technology
Priority date: 2017-12-06
Filing date: 2017-12-06
Publication date: 2020-04-07
Anticipated expiration: 2027-12-06

Abstract

The utility model relates to a small-sized reduction distillation device, which is mainly used for laboratory research or preparation of small-batch volatile metals and oxides, and comprises a reduction distillation furnace, wherein the top opening of the reduction distillation furnace is provided with a furnace cover which is matched with the opening part, the furnace cover is provided with a gas outlet, the reduction distillation furnace is arranged in layers, and specifically comprises a reduction reaction layer at the lower part, a sedimentation layer between the reduction reaction layer and the gas outlet and a material containing layer between the reduction reaction layer and the sedimentation layer, the device also comprises a condensation chamber, the reduction distillation furnace is communicated with the condensation chamber through the gas outlet on the furnace cover, the utility model discloses a sedimentation partition board separates gas, so that gaseous substances in products are fully condensed, meanwhile, the products which are not fully condensed in the sedimentation layer are cooled again in the condensation chamber, and the dust is collected through a cloth bag at the outlet of the condensation chamber, thereby preventing the products from, the utility model discloses reduction distillation plant result yield is high, installs simple structure moreover, and it is easy to make, install and maintain.

Description

Small intermittent reduction distillation device

Technical Field

The utility model belongs to the metallurgical equipment field, more specifically relates to a small-size reduction distillation plant, mainly used laboratory research, or the preparation of the volatile metal of small batch and oxide.

Background

The reduction distillation is a reduction smelting method in which volatilization and condensation of reduced substances (metals) are simultaneously performed in a metallurgical facility. The whole process comprises the steps of reduction of metal oxide and volatilization and condensation of reduced metal. The reduction distillation is a unique metallurgical method, and is based on the premise that the reduced metal can be volatilized in a large amount at high temperature. Solid or liquid metals have a certain vapor pressure at a certain temperature, and the vapor pressure of the metal increases with increasing temperature. The metal vapor is obtained by reducing the metal oxide to a metal state at a high temperature. The metal vapor is volatilized from the metallurgical reactor, separated from high boiling point impurities in the charge such as gangue, and condensed to obtain the metal. The reduced metal from such metallurgical processes is volatilized in a gaseous state, so that there is generally no need to produce molten slag, and the resulting solid residue is discharged from the retort.

However, gases such as carbon monoxide or carbon dioxide are generated in the reduction reaction process, and when the main product is gaseous, the gases are difficult to separate after being mixed with the gases such as carbon monoxide or carbon dioxide, and the gases cannot be prepared by adopting the conventional vacuum distillation equipment.

SUMMERY OF THE UTILITY MODEL

The utility model aims to solve the technical problem that overcome not enough and the defect mentioned in the above background art, provide a simple structure, the high small-size intermittent type formula reduction distillation plant of result yield.

In order to achieve the above purpose, the utility model discloses technical scheme as follows:

the utility model provides a small-size intermittent type formula reduction distillation device, includes reduction distillation stove, reduction distillation stove open-top, the opening part is equipped with the bell of looks adaptation, is equipped with the gas outlet on the bell, reduction distillation stove includes:

the reduction reaction layer is arranged at the lower part of the reaction chamber, the reduction reaction layer is provided with a reaction chamber for reacting materials, the reaction chamber is provided with an outlet, and the inner wall of the reaction chamber is provided with a heating component;

a sedimentation layer between the reduction reaction layer and the gas outlet, wherein the sedimentation layer comprises a plurality of sedimentation partition plates, and each sedimentation partition plate is provided with an opening;

the material containing layer is arranged between the reduction reaction layer and the sedimentation layer, and a feed inlet of the material containing layer is opposite to an opening of the sedimentation partition plate at the bottommost layer of the sedimentation layer;

wherein the openings of the sedimentation partition plates at the bottommost layer of the sedimentation layer are staggered with the outlet of the reaction chamber.

The utility model discloses distillation plant mainly used is volatile metal or compound in the reduction in-process principal product, or produces the reaction of a large amount of gases, for example the preparation or the purification of product for metal or compound such as zinc, cadmium, arsenic oxide. The reaction chamber on this device reduction reaction layer produces gases such as carbon monoxide or carbon dioxide at reduction reaction in-process, and the main product mixes with gases such as carbon monoxide or carbon dioxide when gaseous state, gets into the settlement layer through the export, and the baffle separation is gaseous through the settlement of settling the layer, makes recoverable gaseous product fully condense in the product, subsides on the settlement baffle, falls into flourishing material layer through the opening on the settlement baffle finally and collects, and gases such as carbon monoxide or carbon dioxide discharge away.

Furthermore, the two ends of the sedimentation partition plates are inclined downwards towards the opening parts of the sedimentation partition plates, the sedimentation partition plates are inclined to enable the materials settled at the two ends to move towards the outlet, and then the materials enter the next layer of sedimentation partition plates and finally fall into the material containing layer through the openings of the sedimentation partition plates at the bottommost layer, and the collection of the materials is facilitated.

Furthermore, the staggered openings of the adjacent sedimentation partition plates are farther apart, and the longer the material moving speed is, the longer the material stays in the sedimentation layer, the higher the sedimentation efficiency is.

Furthermore, one of a cooling water jacket, a heating jacket or a heat preservation jacket is arranged on the outer wall of the sedimentation layer and the material containing layer of the reduction distillation furnace. The required temperature (temperature reduction, temperature rise or heat preservation) in the sedimentation layer and the material containing layer is determined according to different conditions, and the sedimentation temperature is controlled to enable the reduction product to generate liquid or solid.

Furthermore, the reduction reaction layer, the sedimentation layer and the material containing layer are respectively provided with a temperature thermocouple. And the temperature of each layer in the reduction distillation furnace is monitored in real time, so that the reduction distillation process is ensured to be carried out smoothly.

Furthermore, a heat insulation layer is arranged between the reduction reaction layer and the material containing layer, and a channel communicated with the sedimentation layer is arranged at the outlet of the heat insulation layer corresponding to the reaction chamber. The thermal insulation layer is arranged to avoid interference of high temperature of the reduction reaction layer on the sedimentation layer and the material containing layer.

The utility model discloses reduction distillation device still includes the condensation chamber, the condensation chamber communicates with each other with reduction distillation stove through the gas outlet on the bell. The gas outlet is connected with the condensing chamber, so that the product which is not fully condensed in the settling chamber is cooled again, and the product yield is improved.

Further, still include the draught fan, the draught fan passes through bleed pipe and condensation chamber intercommunication, sets up the removal that the draught fan is favorable to vapour, improves device condensation efficiency.

Furthermore, a filter bag is arranged at an inlet of the air guide pipe in the condensation chamber, so that condensed solid products are prevented from entering the induced draft fan.

Furthermore, a temperature thermocouple is arranged in the condensation chamber.

Compared with the prior art, the beneficial effects of the utility model reside in that:

(1) the utility model discloses reduction distillation stove is gaseous through the subside baffle separation of subside layer at first, makes the abundant condensation of gaseous object in the result, and the baffle of subsiding simultaneously can set up the polylith, also can set up the inclination, makes the abundant condensation of result retrieve, improves the result yield, and reduction distillation stove passes through the air duct connection condensation chamber simultaneously for not cooling down once more at the result of the abundant condensation of subside layer, and set up in condensation chamber exit and cross the filter bag, prevent that the result from getting into the draught fan.

(2) The utility model discloses a multiple spot temperature measurement and accuse temperature can effective control reaction temperature and settlement temperature, make the reduction product generate liquid or solid.

(3) The utility model discloses equipment structure is simple, and it is easy to make, install and maintain.

Drawings

FIG. 1 is a structural diagram of the reduction distillation apparatus of the present invention.

Wherein, 1, the furnace body; 2-refractory materials; 3, a heating element; 4-graphite crucible; 5, a crucible partition plate; 6-heat insulating layer; 7, a material containing basin; 8-a settling partition; 9-cooling water jacket; 10-gas-guide tube; 11-a condensation chamber; 12-a bleed air duct; 13-a filter bag; 14-temperature thermocouple; 15-furnace cover.

Detailed Description

To facilitate understanding of the present invention, the present invention will be described more fully and specifically with reference to the accompanying drawings and preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.

Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.

Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by an existing method.

Example 1

The embodiment provides a small-size intermittent type formula reduction distillation device, including

reduction distillation stove

1, 1 open-top of reduction distillation stove, the opening part is equipped with the bell 15 of looks adaptation, is equipped with the gas outlet on the bell 15, and reduction distillation stove 1 is the layered structure, specifically includes:

a reduction reaction layer at the lower part of the reaction chamber, wherein the reduction reaction layer is provided with a reaction chamber for reacting materials, the reaction chamber is provided with an outlet, and the inner wall of the reaction chamber is provided with a heating element 3; in the embodiment, the reaction chamber is a graphite crucible 4 which can be taken out, the outlet of the graphite crucible 4 is the outlet of the reaction chamber, a crucible partition plate 5 is covered on the outlet, and a refractory material 2 is filled between the heating element 3 and the shell of the reduction distillation furnace body;

a sedimentation layer between the reduction reaction layer and the gas outlet, wherein the sedimentation layer comprises a plurality of sedimentation partition plates 8, each sedimentation partition plate 8 is provided with an opening, and two ends of each sedimentation partition plate 8 are inclined downwards (for example, conical) towards the opening (the inclined state is not explicitly shown in figure 1, and does not represent that the sedimentation partition plate cannot be inclined); in the embodiment, the number of the settling partition plates 8 is 4, the openings of the adjacent settling partition plates 8 are staggered, and the opening of the settling partition plate 8 at the bottommost layer of the settling layer is staggered with the outlet of the graphite crucible 4;

a material containing layer is arranged between the reduction reaction layer and the sedimentation layer, and a feed inlet of the material containing layer is opposite to an opening of the sedimentation partition plate 4 at the bottommost layer of the sedimentation layer; the material containing layer is a material containing basin 7 in the embodiment;

wherein a heat insulating layer 6 (namely a heat insulating layer) is arranged between the reduction reaction layer and the material containing layer, and the material of the heat insulating layer 6 is determined according to the temperature requirement; the crucible partition 5, the heat insulating layer 6 and the material containing basin 7 are provided with openings corresponding to the outlet of the reaction chamber, and the openings form a steam channel for communicating the reduction reaction layer with the sedimentation layer.

The utility model discloses in, according to subside layer and the required temperature in flourishing material layer, reduction distillation furnace 1 is equipped with one of cooling jacket, heating jacket or insulation cover in subside layer and flourishing material layer outer wall department alternative. The required temperature (temperature reduction, temperature rise or heat preservation) in the sedimentation layer and the material containing layer is determined according to different conditions, the sedimentation temperature is controlled, and the reduction product is made into liquid or solid, and a cooling water jacket 9 is adopted in the embodiment.

The reduction distillation apparatus of this embodiment further comprises a condensation chamber 11, and the condensation chamber 11 is communicated with the reduction distillation furnace 1 through an air outlet on a furnace cover 15. The gas outlet of the reduction distilling furnace 1 is connected with a condensing chamber 11 through a gas-guide tube 10, so that the product which is not fully condensed in the sedimentation layer is cooled again, and the product yield is improved. The condensing chamber 11 is provided with an outlet which is connected with an induced draft fan through an induced draft tube 12, and a filter bag 13 is arranged at the inlet of the induced draft tube 12 in the condensing chamber 11.

In this embodiment, the temperature of the furnace body can be automatically controlled by the heating element 3, and temperature thermocouples are arranged at specific positions of the device, such as a reduction reaction layer, a sedimentation layer, a material containing layer and a condensation chamber, so as to monitor the temperature of each layer in the reduction distillation furnace in real time and ensure the smooth operation of the reduction distillation process.

The reduction distillation apparatus provided in this embodiment is a small batch type, and is mainly used for laboratory research, or preparation of small batches of volatile metals and oxides, or reaction for generating a large amount of gas. For example, the product is the preparation or purification of metals or compounds such as zinc, cadmium, arsenic oxide and the like. The operation steps are as follows:

s1, putting uniformly mixed materials into a graphite crucible 4;

s2, covering a crucible partition plate 5 of the graphite crucible 4;

s3, putting a heat insulation layer material 6, wherein the heat insulation layer material is determined according to the temperature requirement;

s4, placing a material containing basin 7, and filling gaps between the material containing basin and the periphery of the furnace body with refractory materials;

s5, adding a sedimentation partition plate 8 according to the requirement, wherein the openings on each layer of sedimentation partition plate are staggered;

s6, covering a furnace cover 15 and installing an air duct 10;

s7, connecting the gas guide pipe 10 with the condensing chamber 11 by adopting a stainless steel corrugated pipe;

s8, a filter bag 13 is arranged at the lower end of a pipeline 12 caused at an outlet of the condensing chamber 11, and the upper end of the pipeline 12 caused at the outlet is connected with an induced draft fan;

s9, heating of the furnace body is controlled by a heating element 3 (which can be automatically controlled), and temperature is measured at specific parts (such as a sedimentation layer, a reaction chamber and a condensation chamber) of the furnace body by a temperature thermocouple 14;

and S10, opening the induced draft fan after the furnace body begins to be heated.

S11, controlling the water inlet speed of the cooling water jacket 9, controlling the temperature in the sedimentation layer, and collecting the condensation products in the material containing layer and the condensation chamber.

Claims

1. The utility model provides a small-size intermittent type formula reduction distillation device, its characterized in that, includes reduction distillation stove, reduction distillation stove open-top, the opening part is equipped with the bell of looks adaptation, is equipped with the gas outlet on the bell, the layering arranges in the reduction distillation stove furnace body specifically includes:

a sedimentation layer between the reduction reaction layer and the gas outlet, wherein the sedimentation layer comprises a plurality of sedimentation partition plates which are sequentially transversely arranged in the furnace from top to bottom, each sedimentation partition plate is provided with an opening, the opening of the sedimentation partition plate at the bottommost layer of the sedimentation layer is staggered with the outlet of the reaction chamber, and two ends of each sedimentation partition plate are inclined downwards towards the opening;

one of a cooling water jacket, a heating jacket or a heat-insulating jacket is arranged on the outer wall of the sedimentation layer and the material containing layer of the reduction distillation furnace; and a heat insulation layer is arranged between the reduction reaction layer and the material containing layer, and a channel communicated with the sedimentation layer is arranged at the outlet of the heat insulation layer corresponding to the reaction chamber.

2. The reductive distillation apparatus of claim 1, wherein the openings of adjacent settling partitions are staggered.

3. The reductive distillation apparatus according to claim 1, wherein the reduction reaction layer, the sedimentation layer and the material containing layer are each provided with a temperature thermocouple.

4. A reductive distillation apparatus as claimed in any one of claims 1 to 3, further comprising a condensation chamber, said condensation chamber being in communication with the reductive distillation furnace through an air outlet port formed in the furnace cover.

5. The reductive distillation apparatus according to claim 4 further comprising an induced draft fan, said induced draft fan communicating with the condensation chamber via an air draft tube.

6. The reductive distillation apparatus according to claim 5, wherein a filter bag is installed at an inlet of the air-entraining duct in the condensation chamber.

7. A reductive distillation apparatus according to claim 4, wherein a temperature thermocouple is provided within the condensation chamber.