Efficient copper extraction device for organic silicon slurry residues
Through the combined structure of the oxidation kettle, displacement kettle and filter, efficient separation and recovery of copper element in silicone slurry is achieved, solving the problems of low recovery rate and low purity of copper element in existing devices, improving the recovery rate and purity of copper, and providing a flocculant for sewage treatment.
Patent Information
- Application Number
- CN202423143788.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-19
- Publication Date
- 2025-10-14
- Estimated Expiration
- 2034-12-19
AI Technical Summary
In the existing organosilicon slurry copper extraction device, the recovery rate of copper element is low, the purity is not high, and the separation effect is not ideal.
The combined structure of oxidation kettle and displacement kettle is adopted. The filter residue and sulfuric acid solution are fully reacted through the stirring component. The solid-liquid separation is carried out by the first-level filter. The displacement kettle uses iron powder to replace the copper element. The second-level filter is used for further separation to form ferrous sulfate solution and high-purity copper element.
The recovery rate and purity of copper element are improved, and efficient copper separation is achieved. The ferrous sulfate solution can be used as a flocculant for sewage treatment. The structure design is reasonable and easy to promote.
Smart Images
Figure CN223433518U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of organic silicon production and processing, and particularly relates to an organic silicon slurry residue high-efficiency copper extraction device. Background Art
[0002] Silicone slurry refers to a dark oily solid-liquid mixture with a high boiling point, complex composition, and a small amount of silicon powder and copper catalyst produced during the synthesis of chlorosilane monomers. Its total emission accounts for about 1.5-2% of the mass of the mixed monomers. The slurry is flammable and has a strong pungent odor. It will burn and form strong acid mist when exposed to the air. Direct emission will cause serious environmental pollution and fire accidents. Currently, there are two main methods for treating waste slurry: cracking and hydrolysis. The cracking method is mainly based on high-temperature cracking and catalytic cracking. The high-temperature cracking method is to heat the slurry at a temperature of 300-900℃. The high-boiling substances in the pulp residue are cracked to obtain silane monomers, but the temperature of this method is too high and carbon deposition is easy to occur. The catalytic cracking method uses a catalyst to crack the high-boiling substances in the pulp residue at a specific temperature and pressure, but this method cannot crack all components and the cost is relatively high. At present, the main means of treating the pulp residue is the hydrolysis method. The hydrolysis method is to directly add hydrochloric acid to the pulp residue for hydrolysis, and then filter the hydrolyzate. The filtrate after filtration is used to recover high-boiling substances. The filter residue contains copper components, and directly entering the incinerator for incineration will cause waste of copper elements. In the existing technology, the filter residue obtained by hydrolysis and pressure filtration is subjected to copper extraction treatment and then incinerated. The existing organosilicon slurry copper extraction device uses a crushing mechanism to crush the filter residue again, and then adds sulfuric acid to the crushed filter residue for reaction. After the reaction, the components in the filter residue react with the sulfuric acid and are filtered through a filter mesh. The remaining components in the filter residue are discharged with the sulfuric acid, and the copper element remains in the filter mesh, thereby achieving copper separation in the filter residue. In the above-mentioned purification device, the copper in the filter residue cannot be completely separated, and the recovery rate of the copper element is low. At the same time, the separated copper impurity content is high, the iron content in the separated copper is high, and the copper purity is low, resulting in unsatisfactory copper extraction effect. Therefore, it is objectively necessary to develop an organosilicon slurry copper extraction device with a reasonable structural design, high copper element recovery rate, and high copper element purity. Summary of the Invention
[0003] The purpose of the utility model is to provide an organosilicon slurry residue efficient copper extraction device with reasonable structural design, high copper element recovery rate and high copper element purity.
[0004] The purpose of the utility model is achieved in this way, including an oxidation kettle and a displacement kettle, the upper part of the oxidation kettle is provided with a feed port and an acid addition port, the interior of the oxidation kettle is provided with a stirring assembly, the bottom outlet of the oxidation kettle is connected to a primary filter through a first connecting pipe, the slag outlet of the primary filter is connected to a tailings tank, the liquid outlet of the primary filter is connected to the upper part of the displacement kettle through a second connecting pipe, the top of the displacement kettle is provided with an iron powder inlet, the interior of the displacement kettle is provided with an agitator, the bottom outlet of the displacement kettle is connected to a secondary filter through a third connecting pipe, the bottom outlets of the oxidation kettle and the displacement kettle are both provided with control valves, the liquid outlet of the secondary filter is connected to a recovery tank through a drain pipe, and the slag outlet of the secondary filter is connected to a copper storage tank.
[0005] Compared with the existing technology, the advantages of this device are: it optimizes the structure of the original oxidation separation kettle, and the oxidation kettle provided provides a reaction space for the filter residue and the sulfuric acid solution after the filter press. The filter residue and the sulfuric acid solution can fully react under the stirring action of the stirring component, so that the copper element in the filter residue is fully dissolved in the sulfuric acid solution to react to form a copper sulfate solution, and the copper in the filter residue is completely separated; the first-level filter provided can perform solid-liquid separation on the copper sulfate solution and the filter residue after the oxidation reaction, and completely separate the filter residue in the copper sulfate solution, thereby realizing the recovery of the copper sulfate solution, thereby improving The copper recovery rate is high; the replacement kettle set up can use iron powder to replace the copper element in the copper sulfate solution. After the replacement reaction, the copper sulfate solution and the iron powder undergo a replacement reaction to generate ferrous sulfate solution and copper element; the secondary filter set up can perform solid-liquid separation on the ferrous sulfate solution and copper element after the replacement reaction again, and the separated ferrous sulfate solution can be used as a flocculant for sewage treatment after recovery. The separated copper element has high purity and high quality; in summary, the device has the advantages of reasonable structural design, good copper extraction effect, and high copper element recovery rate, and is easy to promote and use. BRIEF DESCRIPTION OF THE DRAWINGS
[0006] Figure 1 It is a schematic diagram of the overall structure of the utility model;
[0007] Figure 2 This is a schematic structural diagram of the primary filter 4 in the present invention;
[0008] In the figure: 1-oxidation kettle, 101-feed port, 102-acid addition port, 103-stirring assembly, 104-grinding partition, 105-grinding chamber, 106-oxidation chamber, 107-sieve hole, 108-double-axis motor, 109-grinding roller, 110-turntable frame, 111-material guide cylinder, 112-material guide plate, 113-distribution pipe, 2-displacement kettle, 201-iron powder inlet, 202-stirrer, 3-first connecting Tube, 4-primary filter, 401-filter box, 402-rotating drum, 403-outer gear ring, 404-drive motor, 405-transmission shaft, 406-driving gear, 407-discharging shaft, 408-first gear, 409-second gear, 410-spiral blade, 5-tailings tank, 6-second connecting pipe, 7-third connecting pipe, 8-secondary filter, 9-drain pipe, 10-recovery tank, 11-copper storage tank. DETAILED DESCRIPTION
[0009] The present invention will be further described below in conjunction with the accompanying drawings, but the present invention is not limited in any way. Any changes or improvements made based on the teachings of the present invention shall fall within the scope of protection of the present invention.
[0010] like Figures 1-2 As shown, the utility model includes an oxidation kettle 1 and a displacement kettle 2, the upper part of the oxidation kettle 1 is provided with a feed port 101 and an acid addition port 102, the interior of the oxidation kettle 1 is provided with a stirring assembly 103, the bottom outlet of the oxidation kettle 1 is connected to a primary filter 4 through a first connecting pipe 3, the slag outlet of the primary filter 4 is connected to a tailings tank 5, the liquid outlet of the primary filter 4 is connected to the upper part of the displacement kettle 2 through a second connecting pipe 6, the top of the displacement kettle 2 is provided with an iron powder inlet 201, the interior of the displacement kettle 2 is provided with an agitator 202, the bottom outlet of the displacement kettle 2 is connected to a secondary filter 8 through a third connecting pipe 7, the bottom outlets of the oxidation kettle 1 and the displacement kettle 2 are both provided with control valves, the liquid outlet of the secondary filter 8 is connected to a recovery tank 10 through a drain pipe 9, and the slag outlet of the secondary filter 8 is connected to a copper storage tank 11.
[0011] The working process of this device is as follows: after the organic silicon slurry residue after hydrolysis is filter-filtered, the filter residue obtained by the filter press enters the oxidation kettle 1 through the feed port 101, and then sulfuric acid solution is added to the oxidation kettle 1 through the acid addition port 102 according to the requirement of the addition ratio. The filter residue and the sulfuric acid solution can fully react under the stirring action of the stirring component 103, so that the copper element in the filter residue is fully dissolved in the sulfuric acid solution to react to form a copper sulfate solution, so that the copper in the filter residue is completely separated. After the oxidation reaction is completed, the copper sulfate solution and the filter residue enter the primary filter 4 through the first connecting pipe 3. The primary filter 4 can perform solid-liquid separation on the copper sulfate solution and the filter residue after the oxidation reaction, and completely separate the filter residue in the copper sulfate solution, thereby realizing the recovery of the copper sulfate solution and improving the recovery rate of copper. The filter residue filtered out by the primary filter 4 is collected by the tailings tank 5 and then incinerated in the furnace. The copper sulfate solution filtered out by the primary filter 4 enters the displacement kettle 2 through the secondary connecting pipe 6. After the copper sulfate solution enters the displacement kettle 2, a certain amount of iron powder is added to the displacement kettle 2 through the iron powder inlet 201. The added iron powder and copper sulfate solution undergo a replacement reaction in the displacement kettle 2, and the copper element in the copper sulfate solution is replaced by the iron powder. After the replacement reaction, the copper sulfate solution and the iron powder undergo a replacement reaction to generate ferrous sulfate solution and copper element. After the replacement reaction, the ferrous sulfate solution and the copper element enter the secondary filter 8 through the third connecting pipe 7. After filtering and separation by the secondary filter 8, the ferrous sulfate solution and the copper element after the replacement reaction can be separated into solid and liquid again. The separated ferrous sulfate solution enters the recovery tank 10 through the drain pipe 9 for recovery. The recovered ferrous sulfate solution can be used as a flocculant for sewage treatment. The separated copper element has high purity and high quality. The separated elemental copper enters the copper storage tank 11 for recovery. The device has the advantages of reasonable structural design, good copper extraction effect, and high copper element recovery rate.
[0012] Furthermore, in order to achieve complete and thorough separation of the copper element, a grinding partition 104 is horizontally provided at the upper part of the oxidation kettle 1, and the grinding partition 104 divides the inner cavity of the oxidation kettle 1 into a grinding chamber 105 and an oxidation chamber 106. The feed port 101 is provided at the upper part of the grinding chamber 105, and a grinding mechanism is provided in the grinding chamber 105. A plurality of sieve holes 107 are provided on the grinding partition 104, and the acid addition port 102 is provided at the upper part of the oxidation chamber 106. The stirring assembly 103 is provided inside the oxidation chamber 106. When the filter residue enters the oxidation chamber 1 06, it needs to enter the grinding chamber 105 first. The grinding mechanism set in the grinding chamber 105 can grind the filter residue so that the copper element wrapped in the filter residue can be separated by grinding. The filter residue after grinding has a uniform particle size and passes through the sieve hole 107 to enter the oxidation chamber 106 to fully react with the sulfuric acid solution for oxidation, which is conducive to improving the separation effect of the copper element. The grinding mechanism includes a dual-axis motor 108 and a grinding roller 109. The dual-axis motor 108 is a structure used in the prior art and can be directly purchased according to the power used. The product is provided with a housing at the center of the top surface of the grinding partition 104, the dual-axis motor 108 is installed in the housing, the bottom transmission shaft of the dual-axis motor 108 passes through the grinding partition 104 and is connected to the stirring assembly 103, the top transmission shaft of the dual-axis motor 108 passes through the housing and is installed with a turntable frame 110, a guide cylinder 111 connected to the grinding partition 104 is provided on the inner wall of the grinding chamber 105, the grinding rollers 109 are 3 to 4, and the grinding rollers 109 are evenly distributed in the space between the guide cylinder 111 and the housing, and the bottom surface of the grinding roller 109 is connected to the grinding partition 104. The top surface of the grinding partition 104 is in sliding contact, and the top surface of the grinding roller 109 is connected to the turntable frame 110 through a connecting rod. The sieve hole 107 is set on the grinding partition 104 between the guide barrel 111 and the housing. When in use, the dual-axis motor 108 drives the turntable frame 110 to rotate, which can rotate the grinding roller 109 through the connecting rod. During the rotation of the grinding roller 109, the filter residue can be ground. At the same time, the dual-axis motor 108 drives the grinding roller 109 to rotate, which can also drive the stirring assembly 103 to rotate, thus achieving the purpose of energy saving. Preferably, in order to prevent the filter residue from clogging the sieve hole 107 during grinding, bristles are provided on the bottom surface of the grinding roller 109. During the rotation of the grinding roller 109, the bristles can clean the sieve hole 107 to prevent the sieve hole 107 from clogging.
[0013] Furthermore, in order to achieve uniform mixing of the filter residue and the sulfuric acid solution, a guide plate 112 is obliquely installed in the oxidation chamber 106 below the grinding partition 104, and a guide port is provided at the lower end of the guide plate 112. A distribution pipe 113 is provided above the higher end of the guide plate 112, and both ends of the distribution pipe 113 are closed. The acid addition port 102 is connected to the distribution pipe 113, and a plurality of nozzles are provided on the distribution pipe 113. The outlet of the nozzle is directed toward the lower end of the guide plate 112. The filter residue after grinding is not The filter residue flows out from the sieve hole 107 and falls onto the guide plate 112. When the filter residue falls onto the guide plate 112, it can enter the reaction chamber 106 through the guide port at a speed at which the guide plate 112 slides obliquely downward. When the filter residue falls onto the guide plate 112, the sulfuric acid solution is transported to the distribution pipe 113 through the acid inlet 102. After the sulfuric acid solution enters the distribution pipe 113, it will be sprayed out through the nozzle to contact the filter residue. At the same time, the fluidity of the sulfuric acid solution can be used to flush the filter residue falling on the guide plate 113 into the oxidation chamber 106.
[0014] In order to achieve a better filtering and separation effect, the structure of the primary filter 4 is the same as that of the secondary filter 8. The structure and use principle of the primary filter 4 and the secondary filter 8 are the same. The method of using the secondary filter 8 refers to the method of using the primary filter 4. Preferably, the primary filter 4 includes a filter box 401 and a drum 402 rotatably installed in the filter box 401. The drum 402 is arranged obliquely in the filter box 401. The outlet of the first connecting pipe 3 is located in the higher end of the drum 402. The lower end of the drum 402 passes through the filter box 401. The tailings trough 5 is located below the lower end of the drum 402. A plurality of filter holes are evenly distributed on the drum 402 located in the filter box 401. An outer gear ring 403 is installed on the outer wall of the lower end of the drum 402. A base is installed on the outer side of the drum 402. A drive motor 404 is installed on the base. The driving motor 404 is a device used in the prior art. The finished product is directly purchased according to the power used. A transmission shaft 405 is installed on the output shaft of the driving motor 404. A driving gear 406 is installed on the transmission shaft 405. The driving gear 406 and the outer ring gear 403 are meshed with each other. A spiral discharging mechanism connected to the transmission shaft 405 is coaxially installed in the rotating drum 402. When in use, the driving motor 404 drives the transmission shaft 405 to rotate. During the rotation of the transmission shaft 405, it can drive the driving gear 406 to rotate. During the rotation of the driving gear 406, it can drive the outer ring gear 403 and the rotating drum 402. The drum 402 rotates, and filtering and separation can be achieved during the rotation process. The tailings after filtering and separation are discharged from the slag outlet of the drum 402 into the tailings tank 5, and the copper sulfate solution after filtering and separation flows out from the filter holes of the drum 402 into the bottom of the filter box 401. In order to avoid the tailings from accumulating in the drum 402, the tailings are discharged from the drum 402 in time. The spiral discharging mechanism includes a discharging shaft 407, a first gear 408 and a second gear 409. The higher end of the discharging shaft 407 is rotatably connected to the inner wall of the filter box 401, and the lower end of the discharging shaft 407 passes through the filter box 401 and extends to On the outside of the drum 402, a spiral blade 410 is installed on the discharge shaft 407, the first gear 408 is installed on the transmission shaft 405, and the second gear 409 is installed on the lower end of the discharge shaft 407. The second gear 409 and the first gear 408 are engaged with each other. When the drum 402 is filtering and separating, the transmission shaft 405 drives the first gear 408 to rotate, and the first gear 408 drives the second gear 409 to rotate. During the rotation, the second gear 409 drives the discharge shaft 407 and the spiral blade 410 to rotate. During the rotation, the spiral blade 410 can discharge the tailings in the drum 402 in time.
[0015] In order to prevent the copper sulfate solution from gathering in the filter box 401, the bottom surface of the filter box 401 is set to an inclined surface structure, and the liquid outlet is set at the lower end of the inclined surface of the filter box 401, so that the copper sulfate solution can be discharged from the filter box 401 in a timely manner.
Claims
1. An efficient copper extraction device for silicone slurry, characterized by: The invention comprises an oxidation kettle (1) and a displacement kettle (2), wherein the upper portion of the oxidation kettle (1) is provided with a feed port (101) and an acid addition port (102), the interior of the oxidation kettle (1) is provided with a stirring assembly (103), the bottom outlet of the oxidation kettle (1) is connected to a primary filter (4) via a first connecting pipe (3), the slag outlet of the primary filter (4) is connected to a tailings tank (5), and the liquid outlet of the primary filter (4) is connected to the upper portion of the displacement kettle (2) via a second connecting pipe (6). The top of the displacement kettle (2) is provided with an iron powder inlet (201), the interior of the displacement kettle (2) is provided with an agitator (202), the bottom outlet of the displacement kettle (2) is connected to a secondary filter (8) via a third connecting pipe (7), the bottom outlets of the oxidation kettle (1) and the displacement kettle (2) are both provided with control valves, the liquid outlet of the secondary filter (8) is connected to a recovery tank (10) via a drain pipe (9), and the slag outlet of the secondary filter (8) is connected to a copper storage tank (11).
2. The device for efficiently extracting copper from organosilicon slurry according to claim 1, characterized in that: A grinding partition (104) is horizontally arranged at the upper part of the oxidation kettle (1), and the grinding partition (104) divides the inner cavity of the oxidation kettle (1) into a grinding chamber (105) and an oxidation chamber (106). The feed port (101) is arranged at the upper part of the grinding chamber (105), and a grinding mechanism is arranged in the grinding chamber (105). A plurality of sieve holes (107) are arranged on the grinding partition (104). The acid addition port (102) is arranged at the upper part of the oxidation chamber (106), and the stirring component (103) is arranged inside the oxidation chamber (106).
3. The device for efficiently extracting copper from organosilicon slurry according to claim 2, characterized in that: The grinding mechanism comprises a dual-axis motor (108) and a grinding roller (109). A housing is installed at the center of the top surface of the grinding partition (104). The dual-axis motor (108) is installed in the housing. The bottom transmission shaft of the dual-axis motor (108) passes through the grinding partition (104) and is connected to the stirring component (103). The top transmission shaft of the dual-axis motor (108) passes through the housing and is installed with a turntable frame (110). The inner wall of the grinding chamber (105) is provided with a rotating disc frame (110). A material guide cylinder (111) is connected to a grinding partition (104), and there are 3 to 4 grinding rollers (109). The grinding rollers (109) are evenly distributed in the space between the material guide cylinder (111) and the housing. The bottom surface of the grinding roller (109) is in sliding contact with the top surface of the grinding partition (104). The top surface of the grinding roller (109) is connected to the turntable frame (110) through a connecting rod. The sieve hole (107) is set on the grinding partition (104) between the material guide cylinder (111) and the housing.
4. The device for efficiently extracting copper from organosilicon slurry according to claim 3, characterized in that: Brush bristles are provided on the bottom surface of the grinding roller (109).
5. The device for efficiently extracting copper from organosilicon slurry according to claim 2, characterized in that: A material guide plate (112) is obliquely installed in the oxidation chamber (106) below the grinding partition (104). A material guide port is provided at the lower end of the material guide plate (112). A distribution pipe (113) is provided above the higher end of the material guide plate (112). Both ends of the distribution pipe (113) are closed. The acid addition port (102) is connected to the distribution pipe (113). A plurality of nozzles are provided on the distribution pipe (113), and the outlets of the nozzles are directed toward the lower end of the material guide plate (112).
6. The device for efficiently extracting copper from organosilicon slurry according to claim 1, characterized in that: The structure of the primary filter (4) is the same as that of the secondary filter (8).
7. The device for efficiently extracting copper from organosilicon slurry according to claim 6, characterized in that: The primary filter (4) comprises a filter box (401) and a drum (402) rotatably mounted in the filter box (401), the drum (402) being arranged obliquely in the filter box (401), the outlet of the first connecting pipe (3) being located in the higher end of the drum (402), the lower end of the drum (402) penetrating the filter box (401), the tailings trough (5) being located below the lower end of the drum (402), and a plurality of flow paths being evenly distributed on the drum (402) located in the filter box (401). The filter hole is provided with an outer gear ring (403) on the outer wall of the lower end of the rotating drum (402), a base is provided on the outer side of the rotating drum (402), a driving motor (404) is provided on the base, a transmission shaft (405) is provided on the output shaft of the driving motor (404), a driving gear (406) is provided on the transmission shaft (405), the driving gear (406) and the outer gear ring (403) are meshed with each other, and a spiral discharging mechanism connected to the transmission shaft (405) is coaxially provided in the rotating drum (402).
8. The device for efficiently extracting copper from organosilicon slurry according to claim 7, characterized in that: The spiral discharging mechanism includes a discharging shaft (407), a first gear (408) and a second gear (409); the higher end of the discharging shaft (407) is rotatably connected to the inner wall of the filter box (401); the lower end of the discharging shaft (407) passes through the filter box (401) and extends to the outside of the rotating drum (402); a spiral blade (410) is installed on the discharging shaft (407); the first gear (408) is installed on the transmission shaft (405); the second gear (409) is installed on the lower end of the discharging shaft (407); and the second gear (409) and the first gear (408) are meshed with each other.
9. The device for efficiently extracting copper from organosilicon slurry according to claim 7, characterized in that: The bottom surface of the filter box (401) is configured as an inclined surface structure, and the liquid outlet is provided at the lower end of the inclined surface of the filter box (401).