A multi-stage back-mixing, dissociation, and regeneration device and method for fluoride-containing sludge in the semiconductor industry

Abstract

This application provides a multi-stage back-mixing, dissociation, and regeneration device and method for fluorinated sludge in the semiconductor industry, comprising: a first reaction structure, a second reaction structure, and a gas treatment structure. The first reaction structure includes a first mixing component for driving the mixing of fluorinated sludge powder and mixed acid. The feed end of the second reaction structure is connected to the discharge end of the first reaction structure, and the second reaction structure includes a second mixing component for secondary mixing of the fluorinated sludge powder and mixed acid after the first reaction. The gas treatment structure's inlet end is connected to the outlet ends of both the first and second reaction structures. In this application, the first mixing component mixes the fluorinated sludge powder and mixed acid to improve the primary reaction effect, and the second mixing component performs secondary mixing of the fluorinated sludge powder and mixed acid to improve the secondary reaction effect. The hydrogen fluoride gas generated from the two reactions enters the gas treatment structure and is treated to obtain anhydrous hydrogen fluoride product.

Description

Technical Field

[0001] This application relates to the field of sludge treatment technology in the semiconductor industry, and in particular to a multi-stage back-mixing, dissociation and regeneration device and method for fluoride-containing sludge in the semiconductor industry. Background Technology

[0002] Downstream manufacturing processes in the semiconductor and fluorochemical industry chain (such as electronic semiconductors, photovoltaic cells, and high-purity hydrofluoric acid production) generate large quantities of complex fluorine-containing solid waste sludge. This type of sludge is mainly composed of multiphase substances such as calcium fluoride (CaF2), silicon dioxide (SiO2), calcium carbonate (CaCO3), calcium hydroxide (Ca(OH)2), and soluble fluoride salts, and is characterized by mixed components and a wide particle size distribution.

[0003] Currently, the main treatment technology for the resource utilization of fluorine-containing sludge is the acid leaching-precipitation method to prepare fluorite powder. However, in actual industrial production, the physical morphology of the raw fluorine-containing sludge deteriorates drastically after acid treatment. The sludge particles become significantly finer, and the specific surface area increases, making them prone to agglomeration. On the one hand, this agglomerates unreacted fluorides and acid reagents, leading to incomplete reactions and reducing the leaching and recovery efficiency of fluorine resources. On the other hand, the agglomerated sludge clumps exacerbate the problems of material jamming and accumulation during transportation, resulting in poor compatibility with subsequent feeding systems. This leads to low fluorine resource recovery rates and insufficient product purity, making it difficult to meet the production requirements of anhydrous hydrogen fluoride.

[0004] In addition, traditional anhydrous hydrogen fluoride production processes often use single-section long-distance augers to transport materials, but long augers are prone to blockage due to material adhesion, which further affects the mixing effect of acid and fluoride-containing sludge. Summary of the Invention

[0005] This application provides a multi-stage remixing and dissociation regeneration device and method for fluorine-containing sludge in the semiconductor industry, which improves the mixing uniformity of fluorine-containing sludge powder and mixed acid, and increases the fluorine conversion rate.

[0006] To achieve the above-mentioned objectives, this application adopts the following approach:

[0007] In a first aspect, this application provides a multi-stage remixing and dissociation regeneration device for fluoride-containing sludge in the semiconductor industry, comprising:

[0008] A first reaction structure, the first reaction structure includes a first mixing component, the first mixing component is used to drive the fluorine-containing sludge powder to mix with mixed acid, and the first reaction structure is used to allow the mixed fluorine-containing sludge powder and mixed acid to undergo a primary reaction.

[0009] The second reaction structure has its feed end connected to the discharge end of the first reaction structure. The second reaction structure includes a second mixing component, which is used to perform a secondary mixing of the fluorine-containing sludge powder and mixed acid after the first reaction. The second reaction structure is used to provide the fluorine-containing sludge powder and mixed acid after the secondary mixing for a secondary reaction.

[0010] A gas processing structure, wherein the gas inlet of the gas processing structure is connected to the gas outlet of the first reaction structure and the second reaction structure, respectively.

[0011] In one possible implementation, the first reaction structure includes:

[0012] The first reaction chamber has a first feed inlet and a second feed inlet at its top. The first feed inlet is used to feed fluorine-containing sludge powder, and the second feed inlet is used to feed mixed acid. A heating jacket is fitted on the circumferential outer wall of the first reaction chamber.

[0013] A drive assembly is disposed at one end of the first reaction chamber, the drive assembly is located on the side of the first feed inlet away from the second feed inlet, and the other end of the first reaction chamber is the discharge end;

[0014] The buffer chamber has its inlet connected to the outlet of the first reaction chamber and its outlet connected to the inlet of the second reaction structure. The diameter of the buffer chamber is larger than that of the first reaction chamber, and the outlet of the buffer chamber is connected to the inlet of the gas treatment structure.

[0015] The first mixing component is disposed in the first reaction chamber, and the driving component is located below the first feed inlet and the second feed inlet to mix the fluoride-containing sludge powder and mixed acid entering the first reaction chamber.

[0016] In one possible implementation, the first hybrid component includes:

[0017] A rotating shaft is disposed within the first reaction chamber;

[0018] A continuous spiral ribbon is disposed on the rotating shaft and located below the first feed inlet;

[0019] Multiple blades are spaced apart on the rotating shaft and located below the second feed inlet;

[0020] Multiple cleaning pins are spaced apart on the circumferential inner wall of the first reaction chamber, and the multiple cleaning pins are arranged alternately with the multiple blades.

[0021] At least two elastic baffles are disposed on the circumferential inner wall of the first reaction chamber, the at least two elastic baffles are located between the continuous spiral ribbon and the plurality of blades, and the rotating shaft is located between the at least two elastic baffles;

[0022] One end of the rotating shaft is connected to the output end of the drive assembly, and the other end of the rotating shaft extends to the discharge end.

[0023] In one possible implementation, the driving component includes:

[0024] A housing is disposed at one end of the first reaction chamber, and one end of the rotating shaft extends into the housing;

[0025] A pushing component is disposed at the end of the housing away from the first reaction chamber, and the output end of the pushing component extends into the housing and is hinged to the rotating shaft.

[0026] A first power component is disposed at the power input end of the push component;

[0027] The housing has a spiral guide groove on its circumferential inner wall, and the rotating shaft has a guide block that matches the spiral guide groove.

[0028] In one possible implementation, the pushing component includes:

[0029] A transmission box is disposed at the end of the housing away from the first reaction chamber;

[0030] The mounting shaft is rotatably mounted inside the transmission box and is connected to the output end of the first power assembly;

[0031] An eccentric wheel is disposed on the mounting shaft;

[0032] A connecting rod, one end of which is hinged to the eccentric wheel;

[0033] A push rod, one end of which is hinged to the other end of the connecting rod, and the other end of which extends into the housing and is hinged to the rotating shaft.

[0034] In one possible implementation, the second reaction structure includes:

[0035] The second reaction chamber has a feeding device at one end and a discharging device at the other end. The feeding end of the feeding device is connected to the discharging end of the first reaction structure. A heating sleeve is fitted on the circumferential outer wall of the feeding device.

[0036] The second power assembly is used to drive the second reaction chamber to rotate.

[0037] The second mixing component is disposed in the second reaction chamber to mix the fluoride-containing sludge powder and mixed acid entering the second reaction chamber.

[0038] In one possible implementation, the second hybrid component includes:

[0039] A cage agitator is disposed in the second reaction chamber and connected to the power output end of the feeding device or the discharging device. The feeding device or the discharging device is used to drive the cage agitator to rotate.

[0040] Multiple scrapers are spaced apart along the axial direction of the second reaction chamber on the circumferential inner wall of the second reaction chamber. There is an angle between the multiple scrapers and the radial direction of the second reaction chamber, and there is a gap between the multiple scrapers and the cage agitator.

[0041] The first return assembly is disposed on the inner wall of the second reaction chamber near the feeding device.

[0042] The second return assembly is disposed on the inner wall of the second reaction chamber near the discharge device.

[0043] The rotation direction of the cage stirrer is opposite to that of the second reaction chamber;

[0044] The first return material component and the second return material component are located inside the cage agitator, and the conveying speed of the first return material component is greater than the conveying speed of the second return material component.

[0045] In one possible implementation, both the first return assembly and the second return assembly include:

[0046] A drive assembly is disposed on the inner wall of the second reaction chamber;

[0047] A helical conveyor rod, which is connected to the power output end of the drive assembly;

[0048] The drive assembly is used to drive the helical conveyor rod to reciprocate in a helical motion.

[0049] In one possible implementation, the gas processing structure includes:

[0050] A first gas processing component, wherein the inlet end of the first gas processing component is connected to the outlet end of the first reaction structure;

[0051] The second gas processing component has its inlet end connected to the outlet end of the first gas processing component and the outlet end of the second reaction structure, respectively.

[0052] In one possible implementation, the first gas processing assembly includes:

[0053] A rinsing device, wherein the air inlet of the rinsing device is connected to the air outlet of the first reaction structure;

[0054] A distillation apparatus, wherein the feed end of the distillation apparatus is connected to the discharge end of the scrubbing device, and one discharge end of the distillation apparatus is connected to the liquid inlet end of the scrubbing device;

[0055] The second gas processing assembly includes:

[0056] A crude distillation column, wherein the gas inlet of the crude distillation column is connected to the gas outlet of the scrubber and the gas outlet of the second reaction structure, respectively;

[0057] A collection tank is provided at the discharge end of the crude distillation column.

[0058] Secondly, this application provides a multi-stage back-mixing and dissociation regeneration method for fluoride-containing sludge in the semiconductor industry, applied to the multi-stage back-mixing and dissociation regeneration device for fluoride-containing sludge in the semiconductor industry described in any of the above claims, the method comprising:

[0059] Preparation of fluoride-containing sludge powder;

[0060] Fluorine-containing sludge powder and mixed acid are respectively put into the first reaction chamber, and the fluorine-containing sludge powder and mixed acid are mixed using the first mixing component. The mixed fluorine-containing sludge powder and mixed acid undergo a reaction once in the first reaction chamber.

[0061] The fluorinated sludge formed after the first reaction is transported to the second reaction chamber, and the hydrogen fluoride gas produced by the first reaction is transported to the first gas treatment component for treatment.

[0062] The fluoride-containing sludge is mixed a second time using a second mixing component, and the fluoride-containing sludge after the second mixing is then subjected to a second reaction in the second reaction chamber.

[0063] The hydrogen fluoride gas produced by the secondary reaction, along with the hydrogen fluoride gas processed by the first gas processing unit, is transported to the second gas processing unit for further processing.

[0064] In one possible implementation, the preparation of fluoride-containing sludge powder includes:

[0065] The fluoride-containing sludge is ground using a ball mill, and the ground powder is mixed with hydrofluoric acid solution to remove impurities.

[0066] The reacted material is dehydrated to obtain a molded body, and the molded body is dried to obtain dry sludge powder.

[0067] The dry sludge powder is sieved to remove mechanical impurities. The sieved dry sludge powder is then ground a second time to grind the sludge powder particles to the target particle size, thus obtaining fluoride-containing sludge powder.

[0068] In one possible implementation, the step of separately adding the fluorinated sludge powder and the mixed acid into the first reaction chamber and mixing the fluorinated sludge powder and the mixed acid using a first mixing component includes:

[0069] Fluorine-containing sludge powder is fed into the first reaction chamber through the first inlet, and mixed acid is fed into the first reaction chamber through the second inlet.

[0070] The propulsion component drives the continuous spiral ribbon and blades to reciprocate in the first reaction chamber, which fully mixes the fluorinated sludge powder and mixed acid for reaction.

[0071] In one possible implementation, the step of conveying the hydrogen fluoride gas produced in the primary reaction to a first gas processing assembly for processing includes:

[0072] The hydrogen fluoride gas is sprayed using a scrubber, and the purified hydrogen fluoride gas is demisted and then transported to the second gas treatment unit.

[0073] The mixture generated by spraying is distilled using a distillation apparatus. The resulting mixed acid is then transported to a scrubbing device, and the distilled hydrofluoric acid is used to prepare fluorinated sludge powder.

[0074] In one possible implementation, the secondary mixing of the mixture after the primary reaction using a second mixing component includes:

[0075] The second reaction chamber and the cage agitator are rotated in opposite directions, and the scraper and the cage agitator break up the fluoride-containing sludge.

[0076] The first and second return components are used to push the fluorinated sludge back into the second reaction chamber.

[0077] This application discloses a multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry. Fluorinated sludge powder and mixed acid are sequentially added to a first reaction structure. A first mixing component thoroughly mixes the fluorinated sludge powder and mixed acid, allowing them to undergo a primary reaction within the first reaction structure. The resulting fluorinated sludge is then transported to a second reaction structure, and the hydrogen fluoride gas generated in the primary reaction is transported to a gas treatment structure. A second mixing component performs a secondary mixing of the fluorinated sludge, and the resulting fluorinated sludge undergoes a secondary reaction within the second reaction structure. This thorough mixing of the fluorinated sludge and mixed acid by the first and second mixing components breaks down the agglomeration of the fluorinated sludge due to its small particle size after acidification, improves the uniformity of the mixing of the fluorinated sludge powder and mixed acid, and ensures a complete reaction, thereby increasing the fluorination reaction rate and fluorine conversion rate. The hydrogen fluoride gas produced in the two reactions is transported to a gas treatment structure, where it is processed to improve gas purity, reduce hydrofluoric acid loss, and increase raw material utilization. Attached Figure Description

[0078] The accompanying drawings, which are incorporated in and form part of this specification, illustrate embodiments consistent with this application and, together with the description, serve to explain the principles of this application. It is obvious that the drawings described below are merely some embodiments of this disclosure, and those skilled in the art can obtain other drawings based on these drawings without any inventive effort.

[0079] Figure 1 This is a schematic diagram of a multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry, as described in one embodiment of this application.

[0080] Figure 2 This is a schematic diagram of the structure of the first hybrid component in one embodiment of this application;

[0081] Figure 3 This is a schematic diagram of the structure of the driving component in one embodiment of this application;

[0082] Figure 4 This is a flowchart of a multi-stage remixing, dissociation, and regeneration method for fluoride-containing sludge in the semiconductor industry, as described in one embodiment of this application.

[0083] Figure 5 This is a flowchart of step S101 in one embodiment of this application;

[0084] Figure 6 This is a flowchart of step S102 in one embodiment of this application;

[0085] Figure 7 This is a flowchart of step S103 in one embodiment of this application;

[0086] Figure 8 This is a flowchart of step S104 in one embodiment of this application.

[0087] Explanation of reference numerals in the attached figures:

[0088] 100. First reaction structure; 101. First mixing assembly; 1011. Rotating shaft; 1012. Continuous helical ribbon; 1013. Paddle; 1014. Cleaning pin; 1015. Elastic baffle; 102. First reaction chamber; 103. First feed inlet; 104. Second feed inlet; 105. Drive assembly; 1051. Housing; 1052. Push assembly; 1053. First power assembly; 1054. Spiral guide groove; 1055. Transmission box; 1056. Mounting shaft; 1057. Eccentric wheel; 1058. Connecting rod; 1059. 106. Push rod; 107. Buffer chamber; 108. Material feeding device; 209. Second reaction structure; 200. Second mixing component; 201. Second reaction chamber; 202. Feeding device; 203. Discharge device; 204. Cage agitator; 205. Scraper; 206. First return component; 207. Second return component; 208. Gas treatment structure; 301. First gas treatment component; 302. Second gas treatment component; 303. Washer; 304. Distillation device; 305. Crude distillation column; 306. Collection tank; 400. Heating jacket. Detailed Implementation

[0089] Exemplary embodiments will now be described in detail, examples of which are illustrated in the accompanying drawings. When the following description relates to the drawings, unless otherwise indicated, the same numbers in different drawings denote the same or similar elements. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with this application. Rather, they are merely examples of apparatuses and methods consistent with some aspects of this application as detailed in the appended claims.

[0090] The technical solution of this application and how the technical solution of this application solves the above-mentioned technical problems are described in detail below with specific embodiments. These specific embodiments can be combined with each other, and the same or similar concepts or processes may not be described again in some embodiments. The following will be combined with... Figures 1-8 The embodiments of this application will be described below.

[0091] This application provides a multi-stage back-mixing, dissociation, and regeneration device for fluoride-containing sludge in the semiconductor industry. (See also...) Figure 1The multi-stage back-mixing and dissociation regeneration device for fluorinated sludge in the semiconductor industry includes: a first reaction structure 100, a second reaction structure 200, and a gas treatment structure 300. The first reaction structure 100 includes a first mixing component 101, which is used to drive the mixing of fluorinated sludge powder and mixed acid. The first reaction structure 100 is used to supply the mixed fluorinated sludge powder and mixed acid for a primary reaction. The feed end of the second reaction structure 200 is connected to the discharge end of the first reaction structure 100. The second reaction structure 200 includes a second mixing component 201, which is used to perform a secondary mixing of the fluorinated sludge powder and mixed acid after the primary reaction. The second reaction structure 200 is used to supply the secondary-mixed fluorinated sludge powder and mixed acid for a secondary reaction. The gas treatment structure 300 is connected to the gas outlets of the first reaction structure 100 and the second reaction structure 200, respectively.

[0092] In this embodiment, the discharge end of the first reaction structure 100 is connected to the feed end of the second reaction structure 200, and the air inlet of the gas treatment structure 300 is connected to the air outlet of the first reaction structure 100 and the second reaction structure 200 respectively. The first reaction structure 100 includes a first mixing component 101, and the second reaction structure 200 includes a second mixing component 201. The first mixing component 101 is used to drive the fluorinated sludge powder and mixed acid to mix, and the second mixing component 201 is used to perform secondary mixing of the fluorinated sludge powder and mixed acid after the first reaction.

[0093] If the fluorinated sludge powder and mixed acid to be reacted are sequentially added into the first reaction structure 100, the fluorinated sludge powder and mixed acid are mixed once by the first mixing component 101, so that the mixed fluorinated sludge powder and mixed acid react once in the first reaction structure 100 to generate hydrogen fluoride gas. The fluorinated sludge formed after the first reaction is transported to the second reaction structure 200, where the fluorinated sludge is mixed a second time by the second mixing component 201. The fluorinated sludge after the second mixing reacts a second time in the second reaction structure 200 to generate hydrogen fluoride gas. The hydrogen fluoride gas generated from the two reactions is then processed in the gas treatment structure to generate hydrogen fluoride product.

[0094] In some embodiments, the mixed acid may include 98% concentrated sulfuric acid, 105% fuming sulfuric acid, and washing acid.

[0095] In some embodiments, see Figure 1 and Figure 2The first reaction structure 100 includes: a first reaction chamber 102, a drive assembly 105, and a buffer chamber 106. The top of the first reaction chamber 102 is provided with a first inlet 103 and a second inlet 104. The first inlet 103 is used to feed fluoride-containing sludge powder, and the second inlet 104 is used to feed mixed acid. The drive assembly 105 is located at one end of the first reaction chamber 102, on the side of the first inlet 103 away from the second inlet 104. The other end of the first reaction chamber 102 is the discharge end. The buffer chamber 106... The feed end of the buffer chamber 106 is connected to the discharge end of the first reaction chamber 102, and the discharge end of the buffer chamber 106 is connected to the feed end of the second reaction structure 200. The diameter of the buffer chamber 106 is larger than the diameter of the first reaction chamber 102. The gas outlet of the buffer chamber 106 is connected to the gas inlet of the gas treatment structure 300. The first mixing component 101 is disposed inside the first reaction chamber 102, and the driving component 105 is located below the first feed inlet 103 and the second feed inlet 104 to mix the fluorinated sludge powder and mixed acid entering the first reaction chamber 102. In this way, the fluorinated sludge powder and mixed acid can be fully mixed, and the fluorinated sludge powder and mixed acid can be fully reacted.

[0096] In one possible implementation, both the first reaction chamber 102 and the buffer chamber 106 can be horizontally arranged. The top of the buffer chamber 106 is provided with an exhaust pipe, and the buffer chamber 106 is connected to the air inlet of the gas processing structure 300 through the exhaust pipe.

[0097] It should be noted that the bottom inner wall of the buffer chamber 106 is located below the bottom inner wall of the first reaction chamber 102, meaning there is a height difference between the bottom inner wall of the first reaction chamber 102 and the bottom inner wall of the buffer chamber 106. This prevents the backflow of mixed acid when the fluorinated sludge powder reacts with the mixed acid in the first reaction and is transported to the buffer chamber 106. The fluorinated sludge falls onto the bottom inner wall of the buffer chamber 106 due to the height difference, naturally pulverizing during the fall and reducing sludge agglomeration. Simultaneously, the increased space of the buffer chamber 106 slows the airflow, allowing dust carried by the hydrogen fluoride gas generated in the first reaction chamber 102 to settle, reducing the dust load in the subsequent gas path and minimizing the risk of fine powder adhesion.

[0098] In one possible implementation, a heating jacket 400 is fitted onto the circumferential outer wall of the first reaction chamber 102, and the heating jacket 400 is used to heat the first reaction chamber 102. In this way, heat can be provided for the reaction of fluorinated sludge powder and mixed acid, a suitable reaction temperature can be maintained, the viscosity of the mixture of fluorinated sludge powder and mixed acid can be reduced, and the fluidity of the mixture can be improved.

[0099] Optionally, the heating mantle 400 is electrically connected to a temperature control device.

[0100] In one example, the heating temperature of the heating jacket 400 can be 100~140°C. This maintains a suitable temperature for the reaction between the fluorinated sludge powder and the mixed acid, reducing the viscosity of the mixture and improving its fluidity.

[0101] Preferably, the heating temperature of the heating jacket 400 is 120°C.

[0102] In one possible implementation, the first reaction chamber 102 may include an outer shell and an inner shell fitted inside the outer shell, and the heating jacket 400 may be disposed between the outer shell and the inner shell.

[0103] In one possible implementation, there can be multiple second feed ports 104, which are spaced apart at the top of the first reaction chamber 102.

[0104] In one possible implementation, a plurality of material-dredging devices 107 may be provided at the top of the first reaction chamber 102, the material-dredging devices 107 being used to clear the fluoride-containing sludge in the first reaction chamber 102.

[0105] Optionally, the second feed inlet 104 can be provided on the feeding device 107.

[0106] In some embodiments, see Figure 1 and Figure 2 The first mixing assembly 101 includes: a rotating shaft 1011, a continuous spiral ribbon 1012, multiple blades 1013, multiple cleaning pins 1014, and at least two elastic baffles 1015. The rotating shaft 1011 is disposed within the first reaction chamber 102. The continuous spiral ribbon 1012 is disposed on the rotating shaft 1011 and is located below the first feed inlet 103. The multiple blades 1013 are spaced apart on the rotating shaft 1011 and are located below the second feed inlet 104. The multiple cleaning pins 1014... A plurality of cleaning pins 1014 and a plurality of paddles 1013 are staggered on the circumferential inner wall of the first reaction chamber 102. At least two elastic baffles 1015 are disposed on the circumferential inner wall of the first reaction chamber 102, located between the continuous screw ribbon 1012 and the plurality of paddles 1013. A rotating shaft 1011 is located between the at least two elastic baffles 1015, with one end of the rotating shaft 1011 connected to the output end of the drive assembly 105 and the other end of the rotating shaft 1011 extending to the discharge end. In this way, the fluorinated sludge powder and the mixed acid can be thoroughly mixed, achieving a complete reaction between the fluorinated sludge powder and the mixed acid.

[0107] In one possible implementation, at least two resilient baffles 1015 may be located between the first feed port 103 and the second feed port 104.

[0108] In one possible implementation, a blade 1013 is located between two adjacent cleaning pins 1014, with a gap between the blade 1013 and both cleaning pins 1014.

[0109] In one possible implementation, at least two elastic baffles 1015 abut against each other on their sidewalls, at least two elastic baffles 1015 abut against the outer wall of the rotating shaft 1011, and at least two elastic baffles 1015 are adapted to the surface shape of the continuous screw ribbon 1012.

[0110] It should be noted that the elastic baffle 1015 is used to isolate the fluorinated sludge powder from the mixed acid. The elastic baffle 1015 and the rotating shaft 1011 form a dynamic seal to prevent the mixed acid from flowing back and generating hydrogen fluoride gas. At the same time, it avoids local material accumulation at the first feed inlet 103, so that the contact section between the fluorinated sludge powder and the mixed acid is always unobstructed, reducing the initial agglomeration of the fluorinated sludge.

[0111] In some embodiments, see Figure 1 , Figure 2 and Figure 3 The drive assembly 105 includes a housing 1051, a push assembly 1052, and a first power assembly 1053. The housing 1051 is located at one end of the first reaction chamber 102, and one end of the rotating shaft 1011 extends into the housing 1051. The push assembly 1052 is located at the end of the housing 1051 away from the first reaction chamber 102, and its output end extends into the housing 1051 and is hinged to the rotating shaft 1011. The first power assembly 1053 is located at the power input end of the push assembly 1052. A spiral guide groove 1054 is provided on the circumferential inner wall of the housing 1051, and a guide block adapted to the spiral guide groove 1054 is provided on the rotating shaft 1011. In this way, the continuous spiral ribbon 1012 and the blade 1013 can be driven to reciprocate spirally in the first reaction chamber 102, achieving thorough mixing of the fluorinated sludge powder and the mixed acid.

[0112] In some embodiments, see Figure 3The driving assembly 1052 includes a transmission box 1055, an eccentric wheel 1057, a connecting rod 1058, and a push rod 1059. The transmission box 1055 is located at the end of the housing 1051 away from the first reaction chamber 102. A mounting shaft 1056 is rotatably mounted inside the transmission box 1055 and connected to the output end of the first power assembly 1053. The eccentric wheel 1057 is mounted on the mounting shaft 1056. One end of the connecting rod 1058 is hinged to the eccentric wheel 1057, and one end of the push rod 1059 is hinged to the other end of the connecting rod 1058. The other end of the push rod 1059 extends into the housing 1051 and is hinged to the rotating shaft 1011. In this way, the continuous screw ribbon 1012 and the blade 1013 can be driven to reciprocate in a spiral motion in the first reaction chamber 102 through eccentric motion, achieving thorough mixing of the fluorinated sludge powder and the mixed acid.

[0113] In one possible implementation, the transmission box 1055 is connected to the housing 1051, and the push rod 1059 can move at the connection between the transmission box 1055 and the housing 1051.

[0114] In one possible implementation, the rotational speed of the eccentric wheel 1057 can be 10~30 r / min.

[0115] Preferably, the rotational speed of the eccentric wheel 1057 is 15 r / min.

[0116] In some embodiments, the first power assembly 1053 may include a first motor, a reducer, and a coupling connected in sequence, with the output end of the coupling connected to the power input end of the mounting shaft 1056.

[0117] In one possible implementation, the power input end of the mounting shaft 1056 is provided with a gear transmission structure, and the output end of the coupling is connected to the gear transmission structure.

[0118] In one possible implementation, the speed of the output shaft of the first motor can be 500 to 900 r / min, and the speed ratio of the reducer can be 20:1 to 30:1.

[0119] In the above embodiment, after the fluorinated sludge powder and mixed acid are sequentially added into the first reaction structure 100, the first motor drives the eccentric wheel 1057 to rotate. The eccentric wheel 1057 drives the push rod 1059 and the rotating shaft 1011 to reciprocate within the housing 1051, causing the guide block to reciprocate within the spiral guide groove 1054. This causes the rotating shaft 1011 to rotate intermittently in both directions within the housing 1051, resulting in the rotating shaft 1011 reciprocating spirally within the housing 1051 and the first reaction chamber 102. This, in turn, causes the continuous spiral ribbon 1012 and the blade 1013 to reciprocate spirally within the first reaction chamber 102. The continuous spiral ribbon 1012 rotates and moves forward, pushing the fluorinated sludge powder forward. At least two elastic baffles 1015 separate the fluorinated sludge powder, which then enters the mixed acid storage area within the first reaction chamber 102. This allows the fluorinated sludge powder to mix with the mixed acid. The paddle 1013 propels the fluorinated sludge powder and mixed acid to fully mix and react. The movement of the paddle 1013 continuously agitates the mixture, producing a periodic kneading and dispersing effect. This continuously breaks up the fluorinated sludge clumps, allowing the acid solution to contact the surface of new fluorinated sludge powder particles, improving the reaction effect between the fluorinated sludge powder and mixed acid, and increasing the fluorine leaching rate. Furthermore, the propulsion of the paddle 1013 reduces the local residence time of the fluorinated sludge, preventing excessive adhesion and caking caused by prolonged residence, thus ensuring the continuous and stable forward transport of the fluorinated sludge.

[0120] Multiple blades 1013 reciprocate in a spiral motion within the first reaction chamber 102. The multiple blades 1013 scrape against the adjacent cleaning pins 1014, which remove the fluorinated sludge adhering to the surface of the blades 1013, keeping the surface of the blades 1013 clean, preventing scale accumulation, ensuring smooth transport of the fluorinated sludge, and preventing material jamming or blockage in the first reaction chamber 102.

[0121] In some embodiments, see Figure 1 The second reaction structure 200 includes a second reaction chamber 202 and a second power assembly. A feeding device 203 is provided at one end of the second reaction chamber 202, and a discharging device 204 is provided at the other end. The feeding end of the feeding device 203 is connected to the discharging end of the first reaction structure 100. The second power assembly drives the second reaction chamber 202 to rotate. A second mixing assembly 201 is disposed inside the second reaction chamber 202 to mix the fluorinated sludge powder and mixed acid entering the second reaction chamber 202. In this way, the fluorinated sludge formed after the first reaction can be transported to the second reaction chamber 202, achieving secondary mixing of the fluorinated sludge and ensuring a complete reaction between the fluorinated sludge powder and the mixed acid.

[0122] It is understandable that the second reaction chamber 202 is rotatably connected to the discharge end of the feeding device 203 and the feed end of the discharge device 204, respectively. This facilitates the input of fluoride-containing sludge into the second reaction chamber 202 during its rotation and the output of the material that has completed the reaction in the second reaction chamber 202.

[0123] In one possible implementation, the feeding device 203 can be a feeding auger, and the discharging device 204 can be a discharging auger.

[0124] It should be noted that the feed auger is located below the buffer chamber 106, and the top of the feed auger is connected to the bottom of the buffer chamber 106.

[0125] In one example, the bottom of the buffer chamber 106 can be a mesh structure, and the top of the feed auger is connected to the mesh structure.

[0126] In one possible implementation, the feeding speed of the feeding device 203 can be 0.5 to 1.2 m / min.

[0127] In one possible implementation, see Figure 2 A heating jacket 400 is fitted onto the circumferential outer wall of the feeding device 203 to heat the feeding device 203. This allows for temperature control of the fluorinated sludge before it enters the second reaction chamber 202, preheating the fluorinated sludge and preventing localized accumulation within the feeding device 203, thus ensuring a continuous and stable flow of the fluorinated sludge into the second reaction chamber 202.

[0128] Optionally, the heating mantle 400 is electrically connected to a temperature control device.

[0129] In one example, the heating temperature of the heating jacket 400 can be 110–130°C.

[0130] In one possible implementation, the second reaction chamber 202 can be a reactor body, the temperature of the second reaction chamber 202 can be 400-550℃, and the rotation speed of the second reaction chamber 202 can be 0.5-1.5 r / min.

[0131] In some embodiments, see Figure 1The second mixing component 201 includes: a cage agitator 205, multiple scrapers 206, a first return component 207, and a second return component 208. The cage agitator 205 is disposed inside the second reaction chamber 202 and is connected to the power output end of the feeding device 203 or the discharging device 204. The feeding device 203 or the discharging device 204 drives the cage agitator 205 to rotate. The multiple scrapers 206 are axially spaced on the circumferential inner wall of the second reaction chamber 202, and the multiple scrapers 206 are radially spaced from the second reaction chamber 202. There is an angle between the multiple scrapers 206 and the cage agitator 205. The first return material assembly 207 is located on the inner wall of the second reaction chamber 202 near the feeding device 203, and the second return material assembly 208 is located on the inner wall of the second reaction chamber 202 near the discharging device 204. The rotation direction of the cage agitator 205 is opposite to that of the second reaction chamber 202. The first return material assembly 207 and the second return material assembly 208 are located inside the cage agitator 205, and the conveying speed of the first return material assembly 207 is greater than that of the second return material assembly 208. In this way, the fluorinated sludge entering the second reaction chamber 202 can be fully mixed, the residence time of the fluorinated sludge in the second reaction chamber 202 can be extended, the material can be fully reacted, and the fluorine conversion rate can be improved.

[0132] In one possible implementation, the cage stirrer 205 is coaxially arranged with the second reaction chamber 202, and the rotation speed of the cage stirrer 205 can be 1.0 to 2.5 r / min.

[0133] It should be noted that the cage agitator 205 is a cylindrical cage frame structure. The outer diameter of the cage agitator 205 can be 0.72 to 0.75 times the inner diameter of the second reaction chamber 202, and the length of the cage agitator 205 can be 0.70 to 0.90 times the length of the second reaction chamber 202. The number of circumferential ring beams arranged axially in the cage agitator 205 can be 15-20 rings, and the distance between the outer wall of the cage agitator 205 and the inner wall of the second reaction chamber 202 can be 30-80 mm. In this way, through the counter-rotation of the cage agitator 205 and the second reaction chamber 202, the fluorinated sludge is thoroughly scraped and dispersed, avoiding material jamming between the cage agitator 205 and the inner wall of the second reaction chamber 202, thus achieving thorough crushing and dispersion of the fluorinated sludge and realizing secondary mixing of the fluorinated sludge.

[0134] Preferably, the length of the cage agitator 205 can be 0.80 to 0.85 times the length of the second reaction chamber 202.

[0135] In one possible implementation, the cage agitator 205 can be fixedly mounted on the outer wall of the feeding device 203 or the discharging device 204. In this way, the cage agitator 205 rotates relative to the second reaction chamber 202.

[0136] In one possible implementation, the scraper 206 is tilted toward the discharge device 204.

[0137] It should be noted that the radial angle between the scraper 206 and the second reaction chamber 202 can be 18° to 22°, the axial distance between two adjacent scrapers 206 can be 500 to 800 mm, the height of the scraper 206 can be 150 to 200 mm, the width of the scraper 206 can be 400 to 600 mm, and the distance between the scraper 206 and the outer wall of the cage agitator 205 can be 20 to 30 mm. In this way, the scraper 206 rotates with the second reaction chamber 202, lifting the material and facilitating its crushing.

[0138] In one possible implementation, the transmission speed of the first return material assembly 207 can be 8 to 12 r / min, and the transmission speed of the second return material assembly 208 can be 4 to 8 r / min.

[0139] In the above embodiment, after the fluorinated sludge is conveyed into the second reaction chamber 202 by the feeding device 203, the second reaction chamber 202 drives the material to rotate. The inclined scraper 206 continuously turns over the material in the second reaction chamber 202 and continuously throws and disperses the material into the second reaction chamber 202, so as to achieve uniform and sufficient distribution and contact mixing of the material in the second reaction chamber 202. The second reaction chamber 202 and the scraper 206 rotate in the same direction, while the second reaction chamber 202 and the cage agitator 205 rotate in opposite directions. The relative linear velocities of the two are superimposed to form a strong shearing and crushing zone. The clumps of material are carried to a certain height by the second reaction chamber 202 and the scraper 206 and then broken up and fall after contact with the cage agitator 205. This makes the surface of the material constantly renewed, breaks up the adhesion and agglomeration of the fluorinated sludge, avoids the encapsulation of unreacted fluorides, and achieves continuous reaction of the material.

[0140] The first return material component 207 and the second return material component 208 push the fluorinated sludge into the second reaction chamber 202, forcibly returning the material that has been pushed into the middle and later sections of the second reaction chamber 202 to the front section, thus extending the residence time of the material in the second reaction chamber 202 and avoiding the short-circuit phenomenon of "discharge before complete reaction". In addition, the conveying speed of the first return material component 207 is greater than that of the second return material component 208, so that the material can be discharged while maintaining the return ratio, achieving full reaction of the material and improving the fluorine conversion rate.

[0141] In some embodiments, both the first return assembly 207 and the second return assembly 208 include a drive assembly 105 and a spiral conveying rod. The drive assembly 105 is disposed on the inner wall of the second reaction chamber 202, and the spiral conveying rod is connected to the power output end of the drive assembly 105. The drive assembly 105 is used to drive the spiral conveying rod to reciprocate in a spiral motion. This improves the agitation effect of the first return assembly 207 and the second return assembly 208.

[0142] It should be noted that a transmission box 1055 is provided on the inner wall of the second reaction chamber 202. A housing 1051 is provided at the end of the transmission box 1055 away from the inner wall of the second reaction chamber 202, and the housing 1051 is connected to the transmission box 1055. A spiral guide groove 1054 is provided on the circumferential inner wall of the housing 1051. One end of the spiral conveying rod extends into the housing 1051, and a guide block adapted to the spiral guide groove 1054 is provided on the spiral conveying rod. A first power assembly 1053 is provided inside the transmission box 1055. The output end of the first power assembly 1053 is provided with a mounting shaft 1056. The mounting shaft 1056 is rotatably mounted inside the transmission box 1055. An eccentric wheel 1057 is provided on the mounting shaft 1056. One end of the connecting rod 1058 is hinged to the eccentric wheel 1057, and the other end of the connecting rod 1058 is hinged to one end of the push rod 1059. The other end of the push rod 1059 extends into the housing and is hinged to the screw conveyor rod.

[0143] Optionally, an elastic sealing plate is provided on the outer wall of one end of the screw conveyor rod that extends into the housing 1051, and the elastic sealing plate can move with the screw conveyor rod. Optionally, the elastic sealing plate is located on the side of the screw guide groove 1054 away from the transmission box 1055.

[0144] In some embodiments, the discharge end of the discharge device 204 is connected to the feed end of the slag cooler, and the discharge end of the slag cooler is connected to the slag bin.

[0145] It should be noted that the reacted material is transported to a slag cooler for cooling, and the heat generated is transported to the second reaction chamber 202 to provide heat for the secondary reaction of the fluorinated sludge powder and mixed acid. The cooled residue is then transported to a slag silo for storage.

[0146] In some embodiments, see Figure 1 The gas processing structure 300 includes a first gas processing component 301 and a second gas processing component 302. The inlet of the first gas processing component 301 is connected to the outlet of the first reaction structure 200, and the inlet of the second gas processing component 302 is connected to both the outlet of the first gas processing component 301 and the outlet of the second reaction structure 200. This allows for the processing of hydrogen fluoride gas generated from the two reactions, producing qualified hydrogen fluoride products, ensuring gas purity, reducing hydrofluoric acid loss, and improving resource utilization.

[0147] In some embodiments, see Figure 1 The first gas treatment assembly 301 includes a scrubber 303 and a distillation device 304. The inlet of the scrubber 303 is connected to the outlet of the first reaction structure 100, the inlet of the distillation device 304 is connected to the outlet of the scrubber 303, and one outlet of the distillation device 304 is connected to the liquid inlet of the scrubber 303. This allows for the treatment of hydrogen fluoride gas generated in a single reaction.

[0148] In one possible implementation, the shower head 303 is provided with atomizing nozzles and multi-layer spray plates, a storage tank is provided at the bottom of the shower head 303, and multi-layer air distribution plates are provided inside the shower head 303.

[0149] Optionally, a demisting unit is provided at the top inside the shower 303.

[0150] In one possible implementation, the temperature inside the shower 303 can be 20-30°C.

[0151] It should be noted that the hydrogen fluoride gas generated in the first reaction chamber 102 enters the lower end of the scrubber 303 through the buffer chamber 106. It is evenly dispersed by the gas distribution plate, allowing the gas to rise uniformly within the scrubber 303 and fully contact the downward-spraying liquid. Solid dust entrained in the gas settles into the storage tank due to gravity caused by the deceleration of the airflow and initial droplet collisions. The purified hydrogen fluoride gas then passes through a demister unit to remove entrained droplets before further processing. The material settled in the storage tank enters the distillation device 304. The mixed acid obtained through distillation in the distillation device 304 is recycled back to the scrubber 303, and the resulting hydrofluoric acid is used to prepare fluorinated sludge powder. The temperature inside the scrubber 303 is lower than that of the hydrogen fluoride gas, reducing the kinetic energy of the dust entrained in the hydrogen fluoride gas, enhancing the dust settling effect, and simultaneously avoiding concentration fluctuations in the spray liquid caused by high-temperature evaporation.

[0152] In one possible implementation, the spray solution comprises a mixture of acid and hydrofluoric acid.

[0153] It should be noted that the spray solution is made by mixing recycled mixed acid and hydrofluoric acid in a certain proportion. It is sprayed from top to bottom in an atomized manner, forming a countercurrent and efficient contact with the rising hydrogen fluoride gas.

[0154] In one possible implementation, see [link to relevant documentation]. Figure 1The second gas processing component 302 includes a crude distillation column 305 and a collection tank 306. The inlet of the crude distillation column 305 is connected to the outlet of the scrubber 303 and the outlet of the second reaction structure 200, respectively. The collection tank 306 is located at the outlet of the crude distillation column 305. In this way, the hydrogen fluoride gas treated by the first gas processing component 301 and the hydrogen fluoride gas generated in the crude distillation column 305 can be processed to produce qualified hydrogen fluoride products.

[0155] Optionally, the collection tank 306 may be located at the bottom of the crude distillation column 305.

[0156] Furthermore, this application also provides a multi-stage back-mixing and dissociation regeneration method for fluoride-containing sludge in the semiconductor industry, see [link to relevant documentation]. Figure 4 The method, applied to the multi-stage back-mixing and dissociation regeneration device for fluoride-containing sludge in the semiconductor industry in any of the above embodiments, includes:

[0157] Step S101: Prepare fluoride-containing sludge powder.

[0158] Step S102: Fluorine-containing sludge powder and mixed acid are respectively put into the first reaction chamber 102, and the fluorine-containing sludge powder and mixed acid are mixed using the first mixing component 101. The mixed fluorine-containing sludge powder and mixed acid undergo a reaction once in the first reaction chamber 102.

[0159] Step S103: The fluorine-containing sludge formed after the first reaction is transported to the second reaction chamber 202, and the hydrogen fluoride gas generated in the first reaction is transported to the first gas treatment component 301 for treatment.

[0160] Step S104: The fluoride-containing sludge is mixed a second time using the second mixing component 201, and the fluoride-containing sludge after the second mixing undergoes a second reaction in the second reaction chamber 202.

[0161] Step S105: The hydrogen fluoride gas generated by the secondary reaction and the hydrogen fluoride gas treated by the first gas treatment component 301 are transported to the second gas treatment component 302 for further processing.

[0162] In this embodiment, fluorinated sludge from various sources in the semiconductor industry is prepared into qualified fluorinated sludge powder. The fluorinated sludge powder is conveyed to the first inlet 103 via a Schenker scale and a screw conveyor and then fed into the first reaction chamber 102. Mixed acid is fed into the first reaction chamber 102 through the second inlet 104. The first mixing component 101 pushes the fluorinated sludge powder forward, allowing it to be fully mixed with the mixed acid and react fully. The hydrogen fluoride gas generated by the reaction of the fluorinated sludge powder and the mixed acid enters the first gas treatment component 301 for treatment. The first mixing component 101 pushes the fluorinated sludge formed by mixing the fluorinated sludge powder and the mixed acid to the second reaction structure 200. Fluorine-containing sludge is conveyed to the second reaction chamber 202 by the feeding device 203. The material is continuously scattered and dispersed by the second reaction chamber 202 and the second mixing component 201, so that the material is evenly and fully distributed and mixed in the second reaction chamber 202, realizing continuous reaction of the material. The hydrogen fluoride gas generated by the secondary reaction of fluorine-containing sludge powder and mixed acid enters the second gas treatment component 302 for treatment. At the same time, the second gas treatment component 302 further treats the hydrogen fluoride gas treated by the first gas treatment component 301 to generate qualified hydrogen fluoride product, thereby reducing hydrofluoric acid loss and improving resource utilization.

[0163] In some embodiments, see Figure 5 Step S101, preparing fluoride-containing sludge powder includes:

[0164] Step S1011: Grind the fluoride-containing sludge using a ball mill, and mix the ground powder with hydrofluoric acid solution to remove impurities.

[0165] Step S1012: Dehydrate the reacted material to obtain a molded body, and dry the molded body to obtain dry sludge powder.

[0166] Step S1013: Screen the dry sludge powder to remove mechanical impurities, and then grind the screened dry sludge powder a second time to grind the sludge powder particles to the target particle size to obtain fluoride-containing sludge powder.

[0167] In this embodiment, fluorinated sludge from various sources in the semiconductor industry is finely dispersed using a ball mill, then fed into an acidification reactor. Hydrofluoric acid solution (5%-6%) is added to remove impurities such as SiO2, CaCO3, and Ca(OH)2. The reacted material is then transported to a mixing tank for uniform mixing, and dewatered using a plate and frame filter press or centrifuge until the moisture content is ≤60% to form a sludge cake. The sludge cake is dried in a rotary kiln or fluidized bed dryer to obtain dry sludge powder. After sieving to remove mechanical impurities, the powder is ground to the target particle size to obtain fluorinated sludge powder, which is then sent to a silo for storage via a bucket elevator.

[0168] In some embodiments, see Figure 6Step S102: Fluorine-containing sludge powder and mixed acid are respectively added into the first reaction chamber 102, and the fluorine-containing sludge powder and mixed acid are mixed using the first mixing component 101, including:

[0169] Step S1021: Fluorine-containing sludge powder is fed into the first reaction chamber 102 through the first feed port 103, and mixed acid is fed into the first reaction chamber 102 through the second feed port 104.

[0170] Step S1022: Using the pushing component 1052 to drive the continuous screw ribbon 1012 and the blade 1013 to reciprocate in the first reaction chamber 102, the fluorinated sludge powder and mixed acid are fully mixed and reacted.

[0171] In this embodiment, fluoride-containing sludge powder in the silo is conveyed to the first inlet 103 and fed into the first reaction chamber 102 via a Schenker scale and a screw conveyor. Mixed acid is fed into the first reaction chamber 102 via the second inlet 104. The first motor drives the eccentric wheel 1057 to rotate. The eccentric wheel 1057 drives the push rod 1059 and the rotating shaft 1011 to reciprocate within the housing 1051, causing the guide block to reciprocate within the spiral guide groove 1054. This causes the rotating shaft 1011 to reciprocate spirally within the housing 1051 and the first reaction chamber 102, driving the continuous screw ribbon 1012 and the blade 1013 in the first reaction chamber 102. The reciprocating spiral rotation within reaction chamber 102, along with the continuous spiral ribbon 1012 rotating and moving forward, propels the fluorinated sludge powder forward, causing the elastic baffle 1015 to separate. The fluorinated sludge powder then enters the mixed acid storage area within the first reaction chamber 102, allowing the fluorinated sludge powder to mix with the mixed acid. The paddle 1013 propels the fluorinated sludge powder and mixed acid to fully mix and react. The movement of the paddle 1013 continuously agitates the mixture of fluorinated sludge powder and mixed acid, producing a periodic kneading and dispersing effect, continuously breaking up fluorinated sludge clumps, and enabling the acid solution to contact the surface of new fluorinated sludge powder particles, thereby improving the reaction efficiency between the fluorinated sludge powder and the mixed acid.

[0172] In some embodiments, see Figure 7 Step S103: The hydrogen fluoride gas produced in the primary reaction is transported to the first gas processing assembly 301 for processing, including:

[0173] Step S1031: Use the scrubber 303 to spray the hydrogen fluoride gas, and after the purified hydrogen fluoride gas is demisted, it is transported to the second gas treatment component 302.

[0174] Step S1032: Distill the mixture generated by spraying using distillation apparatus 304, and transport the distilled mixed acid to scrubber 303. Use the distilled hydrofluoric acid to prepare fluorine-containing sludge powder.

[0175] In this embodiment, the hydrogen fluoride gas generated in the first reaction chamber 102 enters the lower end of the scrubber 303 through the buffer chamber 106. It is evenly dispersed by the gas distribution plate, so that the gas rises evenly in the scrubber 303 and comes into full contact with the downward sprayed liquid. The solid dust entrained in the gas settles into the storage tank by gravity under the deceleration of the airflow and the collision of the initial droplets. After the purified hydrogen fluoride gas passes through the demisting unit to remove the entrained droplets, it undergoes subsequent processing. The material that settles in the storage tank enters the distillation device 304. The mixed acid obtained by distillation in the distillation device 304 is recycled back to the scrubber 303, and the hydrofluoric acid obtained is recycled back to the acidification reactor to prepare fluorinated sludge powder.

[0176] In some embodiments, see Figure 8 Step S104: The mixture after the first reaction is mixed a second time using the second mixing component 201, including:

[0177] Step S1041: Rotate the second reaction chamber 202 and the cage agitator 205 in opposite directions, and use the scraper 206 and the cage agitator 205 to break up the fluoride-containing sludge.

[0178] Step S1042: Use the first return component 207 and the second return component 208 to push the fluorinated sludge back into the second reaction chamber 202.

[0179] In this embodiment, after the fluorinated sludge is conveyed into the second reaction chamber 202 by the feeding device 203, the second reaction chamber 202 drives the material to rotate. The inclined scraper 206 continuously turns over the material in the second reaction chamber 202 and continuously throws and disperses the material into the second reaction chamber 202. The second reaction chamber 202 and the scraper 206 rotate in the same direction, while the second reaction chamber 202 and the cage agitator 205 rotate in opposite directions. The relative linear velocities of the two are superimposed, forming a strong shearing and crushing zone. The clumped material is crushed by the second reaction chamber. The material is moved to a certain height by scraper 202 and scraper 206 and then breaks up and falls after contact with cage agitator 205. The first return component 207 and the second return component 208 push the fluorinated sludge into the second reaction chamber 202, forcibly returning the material in the middle and rear sections of the second reaction chamber 202 to the front section, extending the residence time of the material in the second reaction chamber 202, so that the surface of the material is constantly renewed, breaking the adhesion and agglomeration of fluorinated sludge, preventing unreacted fluorides from being encapsulated, realizing the continuous reaction of the material, and improving the fluorine conversion rate.

[0180] It should be noted that the terms "one embodiment," "embodiment," "exemplary embodiment," "some embodiments," etc., mentioned in the specification indicate that the described embodiment may include a specific feature, structure, or characteristic, but not every embodiment necessarily includes that specific feature, structure, or characteristic. Furthermore, such phrases do not necessarily refer to the same embodiment. Moreover, when a specific feature, structure, or characteristic is described in connection with an embodiment, implementing such a feature, structure, or characteristic in conjunction with other embodiments, whether explicitly described or not, is within the knowledge scope of those skilled in the art.

[0181] Finally, it should be noted that other embodiments of the invention will readily occur to those skilled in the art upon consideration of the specification and practice of the invention disclosed herein. This invention is intended to cover any variations, uses, or adaptations of the invention that follow the general principles of the invention and include common knowledge or customary techniques in the art not disclosed herein, and is not limited to the precise structures described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope. The scope of the invention is limited only by the appended claims.

Claims

1. A multi-stage backmixing dissociation regeneration device for fluorine-containing sludge in the semiconductor industry, characterized by, include: The first reaction structure (100) includes a first mixing component (101), which is used to drive the fluorine-containing sludge powder to mix with the mixed acid, and the first reaction structure (100) is used to allow the mixed fluorine-containing sludge powder and the mixed acid to undergo a single reaction. The second reaction structure (200) has its feed end connected to the discharge end of the first reaction structure (100). The second reaction structure (200) includes a second mixing component (201), which is used to perform secondary mixing of the fluorine-containing sludge powder and mixed acid after the first reaction. The second reaction structure (200) is used to provide the fluorine-containing sludge powder and mixed acid after secondary mixing for secondary reaction. A gas processing structure (300) has its inlet end connected to the outlet ends of the first reaction structure (100) and the second reaction structure (200), respectively.

2. The multi-stage backmixing dissociation regeneration device for fluorine-containing sludge in the general semiconductor industry according to claim 1, characterized in that, The first reaction structure (100) includes: The first reaction chamber (102) is provided with a first feed inlet (103) and a second feed inlet (104) at the top. The first feed inlet (103) is used to feed fluorine-containing sludge powder, and the second feed inlet (104) is used to feed mixed acid. A heating sleeve (400) is fitted on the circumferential outer wall of the first reaction chamber (102). A drive assembly (105) is disposed at one end of the first reaction chamber (102). The drive assembly (105) is located on the side of the first feed inlet (103) away from the second feed inlet (104). The other end of the first reaction chamber (102) is the discharge end. A buffer chamber (106) is provided, the feed end of which is connected to the discharge end of the first reaction chamber (102), the discharge end of which is connected to the feed end of the second reaction structure (200), the diameter of the buffer chamber (106) is larger than the diameter of the first reaction chamber (102), and the gas outlet end of the buffer chamber (106) is connected to the gas inlet end of the gas treatment structure (300). The first mixing component (101) is disposed in the first reaction chamber (102), and the driving component (105) is located below the first feed inlet (103) and the second feed inlet (104) to mix the fluorinated sludge powder and mixed acid entering the first reaction chamber (102).

3. The multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry according to claim 2, characterized in that, The first hybrid component (101) includes: A rotating shaft (1011) is disposed inside the first reaction chamber (102); A continuous spiral ribbon (1012) is disposed on the rotating shaft (1011) and is located below the first feed inlet (103); Multiple blades (1013) are spaced apart on the rotating shaft (1011) and are located below the second feed inlet (104); Multiple cleaning pins (1014) are spaced apart on the circumferential inner wall of the first reaction chamber (102), and the multiple cleaning pins (1014) are arranged alternately with the multiple blades (1013); At least two elastic baffles (1015) are disposed on the circumferential inner wall of the first reaction chamber (102), the at least two elastic baffles (1015) are located between the continuous spiral ribbon (1012) and the plurality of blades (1013), and the rotating shaft (1011) is located between the at least two elastic baffles (1015); One end of the rotating shaft (1011) is connected to the output end of the drive assembly (105), and the other end of the rotating shaft (1011) extends to the discharge end.

4. The multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry according to claim 3, characterized in that, The driving component (105) includes: A housing (1051) is disposed at one end of the first reaction chamber (102), and one end of the rotating shaft (1011) extends into the housing (1051); A pushing assembly (1052) is disposed at one end of the housing (1051) away from the first reaction chamber (102), and the output end of the pushing assembly (1052) extends into the housing (1051) and is hinged to the rotating shaft (1011); A first power assembly (1053) is disposed at the power input end of the push assembly (1052); The housing (1051) has a spiral guide groove (1054) on its circumferential inner wall, and the rotating shaft (1011) has a guide block that is adapted to the spiral guide groove (1054).

5. The multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry according to claim 4, characterized in that, The actuation component (1052) includes: A transmission box (1055) is disposed at one end of the housing (1051) away from the first reaction chamber (102); Mounting shaft (1056) is rotatably mounted inside the transmission box (1055) and is connected to the output end of the first power assembly (1053). An eccentric wheel (1057) is disposed on the mounting shaft (1056); A connecting rod (1058), one end of which is hinged to the eccentric wheel (1057); A push rod (1059) is provided, one end of which is hinged to the other end of the connecting rod (1058), and the other end of which extends into the housing (1051) and is hinged to the rotating shaft (1011).

6. The multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry according to claim 2, characterized in that, The second reaction structure (200) includes: The second reaction chamber (202) is provided with a feeding device (203) at one end and a discharging device (204) at the other end. The feeding end of the feeding device (203) is connected to the discharging end of the first reaction structure (100). A heating sleeve (400) is fitted on the circumferential outer wall of the feeding device (203). The second power assembly is used to drive the second reaction chamber (202) to rotate; The second mixing component (201) is disposed in the second reaction chamber (202) to mix the fluoride-containing sludge powder and mixed acid that enter the second reaction chamber (202).

7. The multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry according to claim 6, characterized in that, The second hybrid component (201) includes: A cage agitator (205) is disposed in the second reaction chamber (202). The cage agitator (205) is connected to the power output end of the feeding device (203) or the discharging device (204). The feeding device (203) or the discharging device (204) is used to drive the cage agitator (205) to rotate. Multiple scrapers (206) are spaced apart along the axial direction of the second reaction chamber (202) on the circumferential inner wall of the second reaction chamber (202). There is an angle between the multiple scrapers (206) and the radial direction of the second reaction chamber (202). There is a gap between the multiple scrapers (206) and the cage agitator (205). The first return material assembly (207) is disposed on the inner wall of the second reaction chamber (202) near the feeding device (203); The second return assembly (208) is disposed on the inner wall of the second reaction chamber (202) near the discharge device (204); The rotation direction of the cage stirrer (205) is opposite to that of the second reaction chamber (202); The first return component (207) and the second return component (208) are located inside the cage agitator (205), and the conveying speed of the first return component (207) is greater than the conveying speed of the second return component (208).

8. The multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry according to claim 7, characterized in that, Both the first return material assembly (207) and the second return material assembly (208) include a drive assembly (105), which is disposed on the inner wall of the second reaction chamber (202); A helical conveyor rod, which is connected to the power output end of the drive assembly (105); The drive assembly (105) is used to drive the spiral conveyor rod to reciprocate in a spiral motion.

9. The multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry according to claim 1, characterized in that, The gas handling structure (300) includes: The first gas processing component (301) has its inlet end connected to the outlet end of the first reaction structure (100). The second gas processing component (302) has its inlet end connected to the outlet end of the first gas processing component (301) and the outlet end of the second reaction structure (200), respectively.

10. The multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry according to claim 9, characterized in that, The first gas processing assembly (301) includes: A rinsing device (303) has its air inlet connected to the air outlet of the first reaction structure (100). A distillation apparatus (304) is provided, wherein the feed end of the distillation apparatus (304) is connected to the discharge end of the scrubber (303), and one discharge end of the distillation apparatus (304) is connected to the liquid inlet end of the scrubber (303). The second gas processing assembly (302) includes: The crude distillation column (305) has its inlet end connected to the outlet end of the scrubber (303) and the outlet end of the second reaction structure (200), respectively. A collection tank (306) is provided at the discharge end of the crude distillation column (305).

11. A multi-stage back-mixing and dissociation regeneration method for fluoride-containing sludge in the semiconductor industry, characterized in that, The method applied to the multi-stage back-mixing, dissociation, and regeneration device for fluorinated sludge in the semiconductor industry as described in any one of claims 1-10 includes: Preparation of fluoride-containing sludge powder; Fluorine-containing sludge powder and mixed acid are respectively put into the first reaction chamber (102), and the fluorine-containing sludge powder and mixed acid are mixed using the first mixing component (101). The mixed fluorine-containing sludge powder and mixed acid undergo a reaction once in the first reaction chamber (102). The fluorinated sludge formed after the first reaction is transported to the second reaction chamber (202), and the hydrogen fluoride gas generated in the first reaction is transported to the first gas treatment component (301) for treatment. The fluorine-containing sludge is mixed a second time using the second mixing component (201), and the fluorine-containing sludge after the second mixing is subjected to a second reaction in the second reaction chamber (202); The hydrogen fluoride gas produced by the secondary reaction and the hydrogen fluoride gas after being processed by the first gas processing unit (301) are transported to the second gas processing unit (302) for further processing.

12. The multi-stage back-mixing and dissociation regeneration method for fluoride-containing sludge in the semiconductor industry according to claim 11, characterized in that, The preparation of fluoride-containing sludge powder includes: The fluoride-containing sludge is ground using a ball mill, and the ground powder is mixed with hydrofluoric acid solution to remove impurities. The reacted material is dehydrated to obtain a molded body, and the molded body is dried to obtain dry sludge powder. The dry sludge powder is sieved to remove mechanical impurities. The sieved dry sludge powder is then ground a second time to grind the sludge powder particles to the target particle size, thus obtaining fluoride-containing sludge powder.

13. The multi-stage back-mixing and dissociation regeneration method for fluoride-containing sludge in the semiconductor industry according to claim 11, characterized in that, The step of separately adding fluoride-containing sludge powder and mixed acid into the first reaction chamber (102) and mixing the fluoride-containing sludge powder and mixed acid using the first mixing component (101) includes: Fluorine-containing sludge powder is fed into the first reaction chamber (102) through the first feed port (103), and mixed acid is fed into the first reaction chamber (102) through the second feed port (104); The continuous spiral ribbon (1012) and the blade (1013) are driven by the push component (1052) to reciprocate in the first reaction chamber (102) to fully mix the fluorinated sludge powder and mixed acid for reaction.

14. The multi-stage back-mixing and dissociation regeneration method for fluoride-containing sludge in the semiconductor industry according to claim 11, characterized in that, The step of conveying the hydrogen fluoride gas generated in the primary reaction to the first gas processing assembly (301) for processing includes: Hydrogen fluoride gas is sprayed using a scrubber (303), and the purified hydrogen fluoride gas is demisted and then transported to the second gas treatment unit (302). The mixture generated by spraying is distilled using a distillation apparatus (304), and the distilled mixed acid is transported to a scrubber (303). The distilled hydrofluoric acid is used to prepare fluorine-containing sludge powder.

15. The multi-stage back-mixing and dissociation regeneration method for fluoride-containing sludge in the semiconductor industry according to claim 11, characterized in that, The secondary mixing of the mixture after the first reaction using the second mixing component (201) includes: The second reaction chamber (202) and the cage agitator (205) are rotated in opposite directions, and the scraper (206) and the cage agitator (205) are used to break up the fluoride-containing sludge. The first return component (207) and the second return component (208) are used to push the fluorinated sludge back into the second reaction chamber (202).

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