CN113355535B - Method and device for purifying tannin germanium slag by combining ultrasonic wave with air floatation method - Google Patents
Method and device for purifying tannin germanium slag by combining ultrasonic wave with air floatation method Download PDFInfo
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Abstract
The invention relates to a method and a device for purifying tannin germanium slag by combining ultrasonic waves with an air floatation method, and belongs to the technical field of nonferrous metallurgy. In the invention, the tannin germanium slag is added into water to obtain a system to be reacted, and the pH value of the system is controlled to be 7-9 by adopting NaOH solution; charging air into the system to be reacted to ensure that the diameter of bubbles is 30-60 mu m, and carrying out neutralization-air floatation impurity removal purification reaction for 10-30 min under the ultrasonic condition; removing floating slag on the water surface, and performing solid-liquid separation to obtain the purified tannin germanium slag. The method utilizes the cavitation effect of ultrasonic in the solution to open the tannin germanium slag inclusion, promotes the impurity elements Fe and As to be effectively dissolved out of the tannin germanium slag, and promotes the iron in the system to be hydrolyzed to generate a large amount of Fe (OH) by adjusting the PH of the solution to be 7-9 3 The colloid adsorbs arsenic-containing anions in the solution to cause the arsenic-containing anions to be coprecipitated, the precipitate is adhered to bubbles generated by the air floatation method, floats to the water surface along with the bubbles, is separated to a slag collecting tray by a slag removing mechanism to be removed, and the purpose of purifying the tannin germanium slag is realized.
Description
Technical Field
The invention relates to a method and a device for purifying tannin germanium slag by combining ultrasonic waves with an air floatation method, and belongs to the technical field of nonferrous metallurgy.
Background
The tannin germanium precipitation method is the method which is most widely applied to industrial germanium enrichment, and germanium ingots can be prepared from the germanium-containing tannin residues obtained by the method through burning, chlorination distillation, rectification, hydrolysis, reduction and zone melting in sequence. However, in the actual production process, the tannin germanium residue obtained by filtering the germanium precipitation solution often contains a large amount of impurities, such as tannin molecules, (Zn, mg, fe) SO 4 、Fe 2 (SO 4 ) 3 、H 3 AsO4、H 2 AsO 4 - Etc., in addition to part of Fe in the pre-leaching solution 3+ Will precipitate Fe (OH) by hydrolysis 3 In the form of slag.
The impurity elements cannot be removed in time, so that the consumption of hydrochloric acid in the subsequent chlorination distillation process is increased, more distillation residues are generated, and a large amount of resource waste and environmental pollution are caused.
In the prior art, a water washing purification impurity removal mode is adopted for the tannin germanium slag, so that part of impurity components can be removed. However, this method has little effect on the removal of impurity elements Fe and As. In order to improve the purification effect of tannin germanium residue and further reduce the hydrochloric acid consumption and residue amount in the chlorination distillation process, and realize the full utilization of resources and environmental protection, a more effective purification and impurity removal method needs to be found urgently.
Disclosure of Invention
The invention provides a method and a device for purifying tannin germanium slag by an ultrasonic enhanced gas floating method, aiming at the problems of low germanium concentrate grade, high hydrochloric acid consumption in the chlorination distillation process, more generated distillation residues and the like caused by incomplete purification and impurity removal of tannin germanium slag, and providing the method and the device for purifying the tannin germanium slag by the ultrasonic enhanced gas floating method, namely, opening tannin germanium slag inclusion by the cavitation effect of ultrasonic in a solution, promoting the effective dissolution of impurity elements Fe and As from the tannin germanium slag, and promoting the iron in the system to be hydrolyzed to generate a large amount of Fe (OH) by adjusting the pH of the solution to be 7-9 3 The colloid adsorbs arsenic-containing anions in the solution to cause the arsenic-containing anions to be coprecipitated, the precipitate is adhered to bubbles generated by the air floatation method, floats to the water surface along with the bubbles, is separated to a slag collecting tray by a slag removing mechanism to be removed, and the purpose of purifying the tannin germanium slag is realized.
A method for purifying tannin germanium slag by combining ultrasonic waves with an air floatation method comprises the following specific steps:
(1) The tannin germanium slag is flocculent precipitate in appearance, contains ferric hydroxide colloid and a large amount of tannin-metal complex molecules, and is obtained by performing solid-liquid separation on a mixed solution obtained after tannin germanium precipitation; adding the tannin germanium slag into water to obtain a system to be reacted, controlling the pH value of the system to be 7-9 by adopting NaOH solution, converting impurity element iron into ferric hydroxide colloid, and adsorbing arsenate ions in the system for coprecipitation;
(2) Charging air into the system to be reacted to make the diameter of the bubbles be 30-60 μm, and carrying out neutralization-air floatation impurity removal purification reaction for 10-30 min under the condition of ultrasonic wave; the ultrasonic waves can effectively open flocculent inclusions of the tannin germanium slag, promote the dissolution of impurity components, simultaneously refine the grain size of reaction particles, increase the contact area of the reaction and further greatly strengthen the mass transfer process of the solid-liquid reaction; the microbubbles and the coprecipitation colloid which is adhered to the microbubbles and contains elements Fe and As float to the water surface together, so that the impurity components and the solution system are layered;
(3) Removing floating slag on the water surface, and carrying out solid-liquid separation to obtain purified tannin germanium slag.
The moisture content of the tannin germanium slag in the step (1) is 20-70%, and the mass ratio of water to the tannin germanium slag is (5).
The aeration quantity of the air in the step (2) is 60-360L/h.
The ultrasonic frequency of the step (2) is 25KHz, and the ultrasonic intensity is 2.4-8.4W/cm 2 。
The device for purifying tannin germanium slag by the ultrasonic wave combined air floatation method comprises a box body 6, wherein the bottom of the box body 6 is horizontally provided with a material placing disc 8, the surface of the material placing disc 8 is uniformly provided with a plurality of air holes 9, the bottom end of the box body 6 is provided with an ultrasonic generator 10, an ultrasonic probe of the ultrasonic generator 10 is vertically upward, the ultrasonic generator 10 is oppositely arranged at two sides of the material placing disc 8, an internal cavity of the material placing disc 8 is externally connected with an air supply device through an air inlet pipe, and the top end of the box body 6 is provided with a NaOH solution spray head;
the top end of the box body 6 is provided with a slag scraper 11, the top end of the side wall of the box body 1 is provided with a slag collecting disc 18, and the slag collecting disc 18 is positioned below the side of the slag scraper 11;
the gas supply device comprises an air compressor 1 and a pressure vessel 2, the air compressor 1 is communicated with a gas inlet of the pressure vessel 2, a gas outlet at the bottom of the pressure vessel 2 is communicated with an inner cavity of the material placing disc 8 through a gas inlet pipe, and the gas inlet pipe is provided with a gas inlet valve 3;
a water inlet 4 is formed in the top of the side wall of the box body 6, and a water outlet 5 is formed in the bottom end of the box body 6;
the box 6 is fixedly arranged on the base 7.
The invention has the beneficial effects that:
(1) The method has the advantages that the tannin germanium slag is purified by combining the ultrasonic wave with the air floatation method, so that the soluble impurities in the tannin germanium slag can be removed, and the effect of obviously removing metal impurity elements Fe and As is achieved; the purified tannin germanium slag is beneficial to reducing the consumption of hydrochloric acid and distillation residues in the subsequent chlorination distillation process, saving resources and protecting the environment;
(2) The method has remarkable energy-saving effect of purifying the tannin germanium slag by combining the ultrasonic wave with the air floatation method, and the power consumption for treating each ton of tannin germanium slag is 0.1-0.3kw;
(3) The tannin germanium slag is purified by combining the ultrasonic wave with the air floatation method, so that elements Fe and As which are difficult to remove in the tannin germanium slag can float to the water surface in a scum form and are separated, and the scum removal rate can reach more than 93%;
(4) The invention adopts the cooperation of the air supply device and the material placing disc, can continuously and stably release tiny bubbles with the diameter of 30-60 mu m, and has good scum separation effect.
Drawings
FIG. 1 is a schematic view of an apparatus for purifying tannin germanium slag by ultrasonic wave combined with air floatation;
in the figure: 1-an air compressor, 2-a pressure tank, 3-an air inlet valve, 4-a water inlet, 5-a water outlet, 6-a box body, 7-a base, 8-a material placing disc, 9-an air hole, 10-an ultrasonic generator, 11-a slag scraper and 12-a slag collecting disc.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
The invention relates to a device for purifying tannin germanium slag by an ultrasonic wave combined air floatation method (see figure 1), which comprises a box body 6, wherein the bottom of the box body 6 is horizontally provided with a material placing disc 8, the surface of the material placing disc 8 is uniformly provided with a plurality of air holes 9, the bottom end of the box body 6 is provided with an ultrasonic generator 10, an ultrasonic probe of the ultrasonic generator 10 is vertically upward, the ultrasonic generator 10 is oppositely arranged at two sides of the material placing disc 8, an internal cavity of the material placing disc 8 is externally connected with an air supply device through an air inlet pipe, and the top end of the box body 6 is provided with a NaOH solution spray head;
the top end of the box body 6 is provided with a slag scraper 11, the top end of the side wall of the box body 1 is provided with a slag collecting disc 18, and the slag collecting disc 18 is positioned below the side of the slag scraper 11;
the gas supply device comprises an air compressor 1 and a pressure vessel 2, the air compressor 1 is communicated with a gas inlet of the pressure vessel 2, a gas outlet at the bottom of the pressure vessel 2 is communicated with an inner cavity of the material placing disc 8 through a gas inlet pipe, and the gas inlet pipe is provided with a gas inlet valve 3;
a water inlet 4 is formed in the top of the side wall of the box body 6, and a water outlet 5 is formed in the bottom end of the box body 6;
the box 6 is fixedly arranged on the base 7.
Example 1: a method for purifying tannin germanium slag by combining ultrasonic wave with air floatation process comprises the following steps:
(1) The tannin germanium slag is flocculent precipitate in appearance, contains ferric hydroxide colloid and a large amount of tannin-metal complex molecules, and is obtained by performing solid-liquid separation on a mixed solution obtained after tannin germanium precipitation; adding tannin germanium slag on a material placing disc, then adding water through a water inlet to obtain a system to be reacted, spraying NaOH solution by using a NaOH solution spray head to control the pH value of the system to be 7.0, converting impurity element iron into ferric hydroxide colloid, and adsorbing arsenate ions in the system for coprecipitation; wherein the moisture content of the tannin germanium slag is 20%, and the mass ratio of water to the tannin germanium slag is 5;
(2) Air is filled into a system to be reacted through an air compressor and a pressure-containing tank of an air supply device to ensure that the diameter of bubbles is 30-60 mu m, and neutralization-air floatation impurity removal purification reaction is carried out for 15min under the ultrasonic condition; the ultrasonic wave can effectively open flocculent inclusions of the tannin germanium slag, promote the dissolution of impurity components, simultaneously refine the grain size of reaction particles, increase the contact area of the reaction, and further greatly strengthen the mass transfer process of the solid-liquid reaction; the microbubbles and the coprecipitation colloid which is adhered to the microbubbles and contains elements Fe and As float to the water surface together, so that the impurity components and the solution system are layered; wherein the air charging amount is 120L/h, the ultrasonic frequency is 25KHz, and the power intensity is 2.4W/cm 2 ；
(3) Removing floating slag on the water surface, and performing solid-liquid separation to obtain purified tannin germanium slag;
the removal rate of impurity elements in the tannin germanium slag in the embodiment is as follows: fe 86.12% and As 88.25%.
Example 2: a method for purifying tannin germanium slag by combining ultrasonic waves with an air floatation method comprises the following specific steps:
(1) The tannin germanium slag is flocculent precipitate in appearance, contains ferric hydroxide colloid and a large amount of tannin-metal complex molecules, and is obtained by performing solid-liquid separation on a mixed solution obtained after tannin germanium precipitation; adding tannin germanium slag onto a material placing disc, then adding water through a water inlet to obtain a system to be reacted, spraying NaOH solution from a NaOH solution spray head to control the pH value of the system to be 8.0, converting impurity element iron into ferric hydroxide colloid, adsorbing arsenate ions in the system, and performing coprecipitation; wherein the moisture content of the tannin germanium slag is 50%, and the mass ratio of water to the tannin germanium slag is 6;
(2) Air is filled into a system to be reacted through an air compressor and a pressure vessel of an air supply device to ensure that the diameter of bubbles is 30-60 mu m, and neutralization-air flotation impurity removal purification reaction is carried out for 25min under the ultrasonic condition; the ultrasonic waves can effectively open flocculent inclusions of the tannin germanium slag, promote the dissolution of impurity components, simultaneously refine the grain size of reaction particles, increase the contact area of the reaction and further greatly strengthen the mass transfer process of the solid-liquid reaction; the microbubbles and the coprecipitation colloid which is adhered to the microbubbles and contains elements Fe and As float to the water surface together, so that the impurity components and the solution system are layered; wherein the air inflation amount is 300L/h, the ultrasonic frequency is 25KHz, and the power intensity is 5.8W/cm 2 ；
(3) Removing floating slag on the water surface, and performing solid-liquid separation to obtain purified tannin germanium slag;
the removal rate of impurity elements in the tannin germanium slag in the embodiment is as follows: fe 93.45% and As 91.68%.
Example 3: a method for purifying tannin germanium slag by combining ultrasonic wave with air floatation process comprises the following steps:
(1) The tannin germanium slag is flocculent precipitate in appearance, contains ferric hydroxide colloid and a large amount of tannin-metal complex molecules, and is obtained by performing solid-liquid separation on a mixed solution obtained after tannin germanium precipitation; adding tannin germanium slag on a material placing disc, then adding water through a water inlet to obtain a system to be reacted, spraying NaOH solution by using a NaOH solution spray head to control the pH value of the system to be 8.0, converting impurity element iron into ferric hydroxide colloid, and adsorbing arsenate ions in the system for coprecipitation; wherein the moisture content of the tannin germanium slag is 70%, and the mass ratio of water to the tannin germanium slag is 8;
(2) Air is filled into the system to be reacted by an air compressor and a pressure-containing tank of the air supply device to make the airThe bubble diameter is 30-60 μm, and neutralization-air floatation impurity removal purification reaction is carried out for 30min under the ultrasonic condition; the ultrasonic wave can effectively open flocculent inclusions of the tannin germanium slag, promote the dissolution of impurity components, simultaneously refine the grain size of reaction particles, increase the contact area of the reaction, and further greatly strengthen the mass transfer process of the solid-liquid reaction; the microbubbles and the coprecipitation colloid which is adhered to the microbubbles and contains elements Fe and As float to the water surface together, so that the impurity components and the solution system are layered; wherein the air inflation amount is 100L/h, the ultrasonic frequency is 25KHz, and the power intensity is 8.0W/cm 2 ；
(3) Removing floating slag on the water surface, and performing solid-liquid separation to obtain purified tannin germanium slag;
the removal rate of impurity elements in the tannin germanium slag in the embodiment is as follows: fe 90.12% and As 89.87%.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (9)
1. A method for purifying tannin germanium slag by combining ultrasonic wave with air floatation is characterized by comprising the following specific steps:
(1) Adding tannin germanium slag into water to obtain a system to be reacted, controlling the pH value of the system to be 7-8 by adopting NaOH solution to convert impurity element iron into ferric hydroxide colloid, and adsorbing arsenate ions in the system for coprecipitation;
(2) Charging air into the system to be reacted to ensure that the diameter of the air bubble is 30 to 60 mu m, and carrying out neutralization-air floatation impurity removal purification reaction under the condition of ultrasonic waves for 10 to 30min;
(3) Removing floating slag on the water surface, and carrying out solid-liquid separation to obtain purified tannin germanium slag.
2. The method for purifying tannin germanium slag by the ultrasonic wave combined air floatation method according to claim 1, is characterized in that: in the step (1), the moisture content of the tannin germanium slag is 20-70%, and the mass ratio of water to the tannin germanium slag is 5.
3. The method for purifying tannin germanium slag by combining ultrasonic waves with an air floatation method according to claim 1, is characterized by comprising the following steps of: the aeration quantity of the air in the step (2) is 60-360L/h.
4. The method for purifying tannin germanium slag by combining ultrasonic waves with an air floatation method according to claim 1, is characterized by comprising the following steps of: the ultrasonic frequency of the step (2) is 25KHz, and the ultrasonic intensity is 2.4-8.4W/cm 2 。
5. The apparatus of the method of claims 1-4, wherein: the device comprises a box body (6), wherein a material placing disc (8) is horizontally arranged at the bottom of the box body (6), a plurality of air holes (9) are uniformly formed in the surface of the material placing disc (8), an ultrasonic generator (10) is arranged at the bottom end of the box body (6), an ultrasonic probe of the ultrasonic generator (10) is vertically upward, the ultrasonic generator (10) is arranged on two sides of the material placing disc (8), an internal cavity of the material placing disc (8) is externally connected with an air supply device through an air inlet pipe, a NaOH solution spray head is arranged at the top end of the box body (6), and the air supply device and the material placing disc (8) are cooperated to continuously and stably release tiny bubbles with the diameter of 30-60 mu m.
6. The apparatus of claim 5, wherein: the top end of the box body (6) is provided with a slag scraper (11), the top end of the side wall of the box body (6) is provided with a slag collecting disc (12), and the slag collecting disc (12) is positioned below the side of the slag scraper (11).
7. The apparatus of claim 5, wherein: the gas supply device comprises an air compressor (1) and a pressure containing tank (2), the air compressor (1) is communicated with a gas inlet of the pressure containing tank (2), a gas outlet at the bottom of the pressure containing tank (2) is communicated with an inner cavity of the material placing disc (8) through a gas inlet pipe, and the gas inlet pipe is provided with a gas inlet valve (3).
8. The apparatus of claim 5, wherein: a water inlet (4) is formed in the top of the side wall of the box body (6), and a water outlet (5) is formed in the bottom end of the box body (6).
9. The apparatus of claim 5, wherein: the box body (6) is fixedly arranged on the base (7).
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| CN115537584B (en) * | 2022-11-29 | 2023-03-10 | 昆明理工大学 | Method for reinforcing tannin germanium precipitation through ultrasonic and tannic acid modification |
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