CN115636415A - Polycrystalline silicon acid pickling impurity removal equipment and impurity removal method - Google Patents
Polycrystalline silicon acid pickling impurity removal equipment and impurity removal method Download PDFInfo
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- CN115636415A CN115636415A CN202211327763.8A CN202211327763A CN115636415A CN 115636415 A CN115636415 A CN 115636415A CN 202211327763 A CN202211327763 A CN 202211327763A CN 115636415 A CN115636415 A CN 115636415A
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Abstract
The invention provides a polycrystalline silicon acid cleaning impurity removing device and an impurity removing method, which solve the problems of polycrystalline silicon acid impurity residue and the like. The invention has the advantages of good impurity removal effect, stable structure and the like.
Description
Technical Field
The invention belongs to the technical field of polycrystalline silicon recovery, and particularly relates to polycrystalline silicon acid-washing impurity-removing equipment.
Background
Polycrystalline silicon is a form of elemental silicon, and when molten elemental silicon is solidified under a supercooling condition, silicon atoms are arranged in a diamond lattice form into a plurality of crystal nuclei, and if the crystal nuclei grow into crystal grains with different crystal plane orientations, the crystal grains are combined to crystallize into polycrystalline silicon. The polycrystalline silicon wafer has obvious polycrystal characteristics compared with the monocrystalline silicon wafer. The existing polysilicon recovery usually needs to remove quartz, metal ions and the like on the surface of a silicon material, firstly uses alkali liquor to remove quartz and the like, then uses acid mixed liquor to carry out acid pickling, is soaked to be neutral by deionized water washing liquor, and finally is dried and stored in a classified manner. However, in the actual treatment process, the temperature control effect of the existing pickling impurity removal equipment in the pickling process is poor, and the metal impurities cannot be fully reacted and dissolved. In addition, in the actual pickling impurity removal process, when equipment is continuously fed, the internal acidity cannot be adjusted, so that the reaction of metal impurities is uneven, and silicon material particles at the bottom of the equipment still have more impurities.
In order to solve the defects of the prior art, people have long searched for and put forward various solutions. For example, chinese patent literature discloses an acid cleaning impurity removal method, an acid cleaning impurity removal apparatus, and a polysilicon purification method and system [200910177449.4], which includes the steps of: and slowing down the cooling process of the metallurgical silicon discharged from the furnace, and after the cooled metallurgical silicon is crushed into silicon powder with certain granularity, selecting various acids to carry out acid washing operation on the silicon powder according to a certain sequence.
The problem that the temperature control effect in the equipment is poor in the pickling process is solved to a certain extent by the aid of the scheme, but the scheme still has many defects, such as excessive silicon material impurities at the bottom of the equipment and the like.
Disclosure of Invention
Aiming at the problems, the invention provides the polycrystalline silicon acid-washing impurity-removing equipment which is reasonable in design and can effectively reduce the residual silicon material impurities at the bottom.
The invention also aims to solve the problems and provide a polycrystalline silicon acid-washing impurity-removing method with good impurity-removing effect.
In order to achieve the purpose, the invention adopts the following technical scheme: the utility model provides a polycrystalline silicon pickling edulcoration equipment, includes crushing unit, and crushing unit is connected with the pickling box, and the built-in heating element of pickling box, the inside a plurality of independent pickling chambeies that have of pickling box, the pickling intracavity install respectively centrifugal screen material subassembly and with set up the fluidization subassembly in the pickling intracavity, the pickling box is equipped with automatic acid supplementation subassembly and warm-pressing balance subassembly. Silicon material particles are conducted into the pickling cavity after the polycrystalline silicon fragments are crushed, the fluidization assembly drives the particles to flow and fully react with acid liquor, uneven reaction caused by sedimentation of the silicon material is avoided, the temperature and pressure balance assembly maintains the constant temperature and pressure in the pickling cavity, and the reaction rate of metal impurities is guaranteed.
In foretell polycrystalline silicon pickling edulcoration equipment, crushing unit is provided with one-way feeding subassembly including smashing the barrel, smashing barrel entrance, and it carries the material subassembly to smash barrel exit, smashes inside cutting assembly and the grinding unit of setting up of barrel. The crushing assembly is used for further crushing the chip-shaped polycrystalline silicon to obtain the particle diameter meeting the fluidization reaction.
In the above polycrystalline silicon acid cleaning impurity removing equipment, the cutting assembly comprises a cutting motor, and the cutting motor is in transmission connection with a cutting blade through a synchronous transmission assembly; the synchronous transmission assembly comprises a transmission gear and a transmission gear ring which are concentrically arranged, a plurality of driven gears which are symmetrically arranged relative to the center of the transmission gear are in meshing transmission between the transmission gear and the transmission gear ring, the driven gears are connected with the cutting blade, the transmission gear is connected with a plurality of reversing gears in meshing transmission, and the reversing gears and the transmission gear ring are connected with the cutting motor through driving gears; cutting blade is discoid and the upper end is provided with relative central symmetry and is the cutting arch of triangle-shaped, and cutting blade is provided with the sawtooth along circumference, smashes the inside toper boss that is used for rotating installation cutting blade that is provided with of barrel, and the cutting blade bottom is provided with the conical surface that covers in the toper boss outside. A plurality of cutting blades rotate synchronously, and the hard polycrystalline silicon wafer is crushed, so that subsequent grinding is facilitated.
In foretell polycrystalline silicon pickling edulcoration equipment, grinding assembly is including setting up the grinding room in cutting assembly below, and grinding room internal rotation installs the abrasive disc that a plurality of superpositions were arranged, and evenly distributed has the small opening on the abrasive disc, and the relative one side of adjacent abrasive disc distributes and has the grinding grained layer, installs the shower nozzle that is used for spouting grinding aid in the grinding room. And continuously spraying the grinding aid in the grinding process to realize wet grinding, wherein silicon material particles after grinding are adhered to each other, and the silicon material particles are prevented from floating in the transmission process.
In the polycrystalline silicon acid washing impurity removing equipment, the one-way feeding assembly comprises a feeding hole formed in the upper end of a crushing barrel, a feeding box body is arranged at the upper end of the crushing barrel, the feeding box body is internally divided into a plurality of independent feeding cavities by obliquely arranged baffles, an opening and closing opening opposite to the internal feeding cavities is formed in one side of each feeding cavity, the opening and closing opening is closed by a plurality of opening and closing plates in sliding connection, and a step-by-step discharging assembly is arranged between one end of the feeding box body and the feeding hole; the progressive discharging assembly comprises discharging guide rails arranged on two sides of the feeding port, discharging slide blocks are respectively mounted on the discharging guide rails in a sliding mode, the discharging guide rails extend to the upper portion of the crushing barrel body, the discharging slide blocks are rotatably connected with the feeding box body, a stop strip for stopping the opening and closing plate from falling into the crushing barrel body is arranged at the edge of the feeding port, a discharging motor is mounted at the upper end of the crushing barrel body, a discharging gear is fixed at the output end of the discharging motor, and a discharging rack in meshing transmission with the discharging gear is arranged on the outer side of the feeding box body; the material lifting assembly comprises a material lifting cylinder which is obliquely arranged, a material lifting screw rod is arranged in the material lifting cylinder, and the material lifting screw rod is in transmission connection with a material lifting motor through a coupler. The unidirectional feeding component is used for controlling the feeding amount and is matched with the centrifugal screening component to obtain the best screening effect.
In the polycrystalline silicon acid cleaning impurity removing equipment, the acid cleaning box body comprises a main box body and a box cover for sealing the upper end of the main box body, acid cleaning cavities are arranged in the main box body at equal intervals, acid-resistant surface layers cover the inner sides of the acid cleaning cavities, and the acid cleaning cavities are mutually separated through sealing components; the sealing assembly comprises a sealing inserting plate arranged on the inner side of the box cover, the sealing inserting plate is arranged between the pickling cavities, heat insulating layers are respectively arranged inside the sealing inserting plate and inside the pickling box body, sealing grooves which are oppositely arranged are formed between the main box body and the side opening of the box cover, alkaline liquid is injected into the sealing grooves, and the main box body and the box cover are pressed and fixed through lock catches. The pickling box body has good sealing performance and heat preservation effect, acid liquor leakage and heat loss are effectively avoided, materials can be taken by opening the box cover, and the requirement of pickling large batches of polycrystalline silicon is met.
In the polycrystalline silicon pickling impurity removal equipment, the centrifugal screening component comprises a screening cylinder, screens are uniformly distributed on the screening cylinder, the screening cylinder is in transmission connection with the centrifugal driving component, a material blocking cylinder is arranged around the screening cylinder, and a material guide component is arranged in the screening cylinder; the material guide assembly comprises material guide plates which are spirally and uniformly arranged on the inner side of the screening material cylinder, and the material guide plates are provided with base plates which are mutually overlapped and are opposite to the center of the screening material cylinder; the centrifugal driving assembly comprises a driving rod connected with the center of the screening cylinder, and the driving rod is in transmission connection with the servo motor; the material blocking barrel is in a cone shape, and the diameter of the upper end of the material blocking barrel is smaller than that of the lower end of the material blocking barrel. After the granular silicon material is conducted into the centrifugal sieve material component, the granular silicon material is uniformly distributed into the pickling cavity under the centrifugal action, and the residual large-particle silicon material is subjected to secondary grinding.
In the polycrystalline silicon acid cleaning impurity removing equipment, the fluidization assembly comprises a fluidization pipe which is coiled at the bottom of the acid cleaning cavity, the surface of the fluidization pipe is provided with an upward fluidization nozzle, a one-way valve is arranged between the fluidization nozzle and the fluidization pipe, and a dispersion pipe is reserved in the fluidization nozzle; the dispersion pipe comprises a main pipe connected with the fluidization nozzle and branch pipes which incline downwards, and the branch pipes are arranged in a central symmetry way relative to the main pipe; the automatic acid supplementing assembly comprises an acid supplementing pipe communicated with the fluidization pipe, the acid supplementing pipe is externally connected with an evaporating tank and an acid supplementing pump, an electric heating coil is installed on the inner wall of the evaporating tank in a fitting manner, a pressure regulating valve is installed on the acid supplementing pipe, and pH sensors are respectively arranged in the acid supplementing pipe and the acid pickling cavity. The fluidization assembly is arranged at the bottom of the pickling cavity, silicon material deposition is avoided, and meanwhile, the fluidization assembly is matched with the automatic acid supplementing assembly to continuously supply acid to the pickling cavity so as to ensure impurity removal rate.
In the above polycrystalline silicon acid cleaning impurity removing equipment, the heating assembly comprises a heating pipe communicated with the inside of the acid cleaning cavity, the heating pipe is externally connected with a heating box, and an electric heating pipe and a circulating fan are arranged in the heating box; the temperature and pressure balance assembly comprises a pressure relief pipe communicated with the pickling cavity, the pressure relief pipe is externally connected with a pressure relief pump and a neutralization pond, and a temperature sensor and a pressure sensor are arranged inside the pickling cavity. The internal temperature of the pickling tank body rises, the reaction rate of the acidic substance rises along with the temperature rise, and the temperature and pressure balance assembly discharges pressure in time to maintain the internal pressure within a specified range.
A polycrystalline silicon acid cleaning impurity removing method comprises the following steps:
s1: crushing and grinding the polysilicon fragments by using a crushing assembly;
s2: inputting the crushed polycrystalline silicon powder into a pickling box body, and uniformly dispersing the polycrystalline silicon powder into each pickling cavity through a centrifugal screening assembly;
s3: the fluidization component introduces acidic steam into the pickling cavity towards the pickling cavity to carry out fluidization reaction;
s4: the heating assembly and the temperature-pressure balancing assembly feed back and adjust the temperature and the pressure inside the pickling cavity;
s5: the temperature and pressure balance assembly is used for pumping pressure in the pickling cavity and guiding out redundant acidic substances;
s6: and drying and leading out the pickled polycrystalline silicon powder by the heating assembly and the fluidizing assembly. Compared with a conventional impurity removal method, the method combines fluidization reaction and acid impurity removal, ensures that the silicon material at the bottom fully reacts with acid liquor, further reduces the residue of metal impurities, and improves the recovery effect of the polysilicon silicon material.
Compared with the prior art, the invention has the advantages that: continuously supplementing acid in the process of the fluidization reaction, so that the silicon material impurities inside the pickling cavity maintain a higher reaction rate, and the impurity removal effect is improved; the temperature and pressure balancing component maintains the internal temperature and pressure of the pickling tank body to be constant, so that the internal pickling substance is ensured to be in a mist state and to be in full contact reaction with impurities; the polysilicon fragments are crushed before reaction, so that the subsequent transmission and processing are facilitated.
Drawings
FIG. 1 is a schematic view of the shredder assembly of the present invention;
FIG. 2 is a structural cross-sectional view of the size reduction assembly of the present invention;
FIG. 3 is a partial cross-sectional view of the cutting assembly of the present invention;
FIG. 4 is a partial cross-sectional view of the one-way feed assembly of the present invention;
FIG. 5 is a schematic view of the material lifting assembly of the present invention;
FIG. 6 is a structural cross-sectional view of a pickling tank of the invention;
FIG. 7 is a partial cross-sectional view of the centrifugal screen assembly of the present invention;
FIG. 8 is a partial cross-sectional view of the fluidization assembly of the present invention;
FIG. 9 is a partial cross-sectional view of the pickling tank of the invention;
in the figure, the position of the upper end of the main shaft, the crushing assembly 1, the crushing cylinder 11, the unidirectional feeding assembly 12, the feeding hole 121, the feeding box 122, the baffle 123, the feeding cavity 124, the opening and closing port 125, the opening and closing plate 126, the lifting assembly 13, the cutting assembly 14, the cutting motor 141, the cutting blade 142, the transmission gear 143, the transmission gear ring 144, the driven gear 145, the reversing gear 146, the driving gear 147, the cutting protrusion 148, the conical boss 149, the grinding assembly 15, the grinding chamber 151, the grinding disc 152, the leakage hole 153, the ground particle layer 154, the progressive discharging assembly 16, the discharging guide rail 161, the discharging slider 162, the baffle 163, the discharging motor 164, the discharging gear 165, the discharging rack 166, the lifting cylinder 167, the lifting screw 168, the discharging screw rod the device comprises a material lifting motor 169, an acid pickling box body 2, a main box body 21, a box cover 22, a sealing inserting plate 23, a sealing groove 24, a lock catch 25, a heating assembly 3, a heating pipe 31, a heating box 32, an electric heating pipe 33, a circulating fan 34, an acid pickling cavity 4, a centrifugal material sieving assembly 5, a material sieving cylinder 51, a screen 52, a material stopping cylinder 53, a material guide plate 54, a base plate 55, a driving rod 56, a servo motor 57, a fluidizing assembly 6, a fluidizing pipe 61, a fluidizing nozzle 62, a dispersing pipe 63, a main pipe 64, a branch pipe 65, an acid supplementing pipe 66, an evaporation tank 67, an acid supplementing pump 68, an electric heating coil pipe 69, a pressure regulating valve 691, an automatic acid supplementing assembly 7, a temperature and pressure balancing assembly 8, a pressure relief pipe 81, a pressure relief pump 82 and a neutralization tank 83.
Detailed Description
The invention is described in further detail below with reference to the drawings and the detailed description.
As shown in figures 1 and 6, the polycrystalline silicon acid cleaning impurity removing equipment comprises a crushing assembly 1, wherein the crushing assembly 1 is arranged on an automatic production line, and polycrystalline silicon fragments are guided into the crushing assembly for crushing treatment in an automatic transmission or manual transmission mode. The crushing assembly 1 is connected with an acid washing box body 2 for carrying out closed acid washing treatment on the polysilicon particles. The heating assembly 3 is arranged in the pickling tank body 2 to heat the inside of the pickling tank body, so that the reaction rate of metal impurities and acid liquor is increased, the evaporation of the acid liquor is increased after pickling, and the acid liquor residue on the surface of a silicon material is reduced. The inside of the pickling tank body 2 is provided with a plurality of independent pickling cavities 4 which can work synchronously or asynchronously, and the polysilicon particles are transmitted to each pickling cavity 4 for independent pickling. The inside of the pickling chamber 4 is respectively provided with a centrifugal screen material component 5 and a fluidizing component 6 arranged in the pickling chamber 4, the polycrystalline silicon particles in the pickling chamber 4 are in a suspension motion state in the fluidizing component 6, and the particles cannot be lost due to the closed structure of the pickling chamber 4. The pickling tank 2 is provided with an automatic acid supplementing assembly 7 and a temperature and pressure balancing assembly 8. The commonly used acid liquid comprises hydrofluoric acid, nitric acid and acetic acid, the proportion of the acid liquid is selected according to different metal impurity contents, when the pH value in the pickling cavity 4 is higher than a preset value, the automatic acid supplementing assembly 7 automatically supplements acid to reduce the pH value, and the temperature and pressure balancing assembly 8 feed back and adjust the temperature and pressure in the pickling cavity 4.
As shown in FIG. 2, unlike the conventional crushing apparatus, the present crushing assembly 1 includes a closed crushing drum 11, and a one-way feeding assembly 12 is provided at an inlet of the crushing drum 11 to prevent the fragments from being ejected during the crushing process. The outlet of the crushing cylinder 11 is provided with a material lifting component 13 to realize the lifting transmission of the polysilicon particles, and the processed polysilicon particles are directly transmitted into the pickling box body 2. The cutting assembly 14 and the grinding assembly 15 are arranged inside the crushing cylinder 11 to carry out double crushing treatment on the flaky polycrystalline silicon until the particle diameter meets the fluidization reaction requirement.
As can be seen from fig. 3, the cutting assembly 14 includes a cutting motor 141, the cutting motor 141 is in transmission connection with the cutting blade 142 through a synchronous transmission assembly, and the synchronous transmission assembly provides a larger circumferential rotation speed for the cutting blade 142; the synchronous transmission assembly comprises a transmission gear 143 and a transmission gear ring 144 which are concentrically arranged, a plurality of driven gears 145 which are symmetrically arranged relative to the center of the transmission gear 143 and the transmission gear ring 144 are in meshing transmission, the driven gears 145 are connected with the cutting blade 142, the transmission gear 143 is connected with a plurality of reversing gears 146 in meshing transmission, and the reversing gears 146 and the transmission gear ring 144 are connected with the cutting motor 141 through driving gears 147; the reversing gear 146 does not change the transmission ratio of the driven gear 145, and the reversing gear 146, the transmission gear ring 144 and the driving gear 147 are synchronously meshed for transmission, so that the driven gears 145 and the cutting blades 142 connected with the driven gears 145 have better rotation stability; the cutting blade 142 is disc-shaped, the upper end of the cutting blade is provided with cutting protrusions 148 which are symmetrical relative to the center of the cutting blade and are triangular, sawteeth are arranged on the cutting blade 142 along the circumferential direction, and the cutting blade 142 rotates at a high speed to crush the polycrystalline silicon wafer into fine fragments. The crushing cylinder 11 is provided with a tapered boss 149 for rotatably mounting the cutting blade 142 therein, and the bottom of the cutting blade 142 is provided with a tapered surface covering the outside of the tapered boss 149. Tapered bosses 149 overlap each other to prevent debris from intruding into the rotational connection of cutting blade 142 and tapered bosses 149.
Further, the crushed polysilicon fragments can be directly subjected to acid washing or further ground to increase the contact area with acid liquor. The grinding assembly 15 comprises a grinding chamber 151 which is arranged below the cutting assembly 14 and is independent relative to the cutting assembly 14, a plurality of grinding discs 152 which are arranged in an overlapped mode are rotatably arranged in the grinding chamber 151, the grinding discs 152 are in transmission connection with the cutting motor 141, and a reversing gear set is arranged between every two adjacent grinding discs 152 to achieve synchronous rotation and opposite rotation directions. The grinding disc 152 is uniformly distributed with the leakage holes 153, and the polysilicon fragments fall into the leakage holes 153 and are crushed along with the rotation of the grinding disc 152. A grinding particle layer 154 is distributed on one side opposite to the adjacent grinding disc 152 for improving the friction coefficient, and a spray head for spraying grinding aid is arranged in the grinding chamber 151. The grinding aid is injected into the grinding chamber 151, so that the adhesion degree of polycrystalline silicon particles can be improved and the loss of fine particles is avoided besides the auxiliary grinding of polycrystalline silicon fragments.
As can be seen from FIG. 4, since the pulverizing assembly 1 continuously feeds and pulverizes, the unidirectional feeding assembly 12 is used to control the single feeding amount, thereby avoiding uneven pulverization caused by excessive silicon material inside the pulverizing barrel 11. The unidirectional feeding component 12 comprises a feeding port 121 arranged at the upper end of the crushing cylinder 11, a feeding box 122 is arranged at the upper end of the crushing cylinder 11, and the feeding box 122 indirectly supplies the crushing cylinder 11. The interior of the feeding box 122 is divided into a plurality of independent feeding cavities 124 by inclined baffles 123, one side of the feeding cavity 124 is provided with an opening and closing port 125 opposite to the inner feeding cavity 124, and the opening and closing port 125 is closed by a plurality of opening and closing plates 126 which are connected in a sliding manner. The polysilicon fragments are placed in the feed box 122, and then the opening 125 is completely closed by the opening and closing plate 126.
In addition, a progressive material discharging assembly 16 is arranged between one end of the feeding box body 122 and the feeding hole 121; the progressive discharging assembly 16 comprises discharging guide rails 161 symmetrically arranged at two sides of the feeding port 121, discharging sliders 162 are respectively installed on the discharging guide rails 161 in a sliding mode, and sliding tracks of the discharging sliders 162 are limited by the discharging guide rails 161. The discharging guide rail 161 extends to the upper part of the crushing cylinder 11, the discharging slider 162 is rotatably connected with the feeding box body 122, and the feeding box body 122 can rotate from a horizontal state to a vertical state and is then slidably inserted into the feeding port 121.
The edge of the inlet 121 is provided with a barrier 163 for preventing the opening/closing plate 126 from falling into the pulverizing cylinder 11, and when the inlet 121 is vertically lowered, the opening/closing plate 126 is restricted by the barrier 163 to store one by one and open the opening/closing port 125. The upper end of the crushing cylinder 11 is provided with a discharging motor 164 to drive the feeding box 122 to turn and vertically lift, the output end of the discharging motor 164 is fixed with a discharging gear 165, and the outer side of the feeding box 122 is provided with a discharging rack 166 which is in meshing transmission with the discharging gear 165. When the discharging gear 165 is driven by the discharging motor 164 to rotate, the feeding box 122 is slidably inserted into the feeding hole 121. As shown in fig. 5, the lifting assembly 13 includes a lifting cylinder 167 disposed obliquely, a lifting screw 168 is installed inside the lifting cylinder 167, and the lifting screw 168 is in transmission connection with a lifting motor 169 through a coupling. The lower end of the lifting cylinder 167 is in communication with the bottom of the crushing cylinder 11 and conducts the slurry mixed with grinding aid and polysilicon to the next processing station.
In addition, different from the conventional pickling mode, the acid liquor utilization rate is improved by adopting the closed pickling tank body 2. The pickling tank 2 includes a main tank 21 and a tank cover 22 that closes an upper end of the main tank 21, and the main tank 21 and the tank cover 22 are normally opened and closed by being lifted or turned over. The pickling chambers 4 are arranged in the main tank body 21 at equal intervals, and the inner side of the pickling chambers is covered with an acid-resistant surface layer to prevent the pickling tank body 2 from being corroded. The pickling chambers 4 are mutually separated through the sealing assemblies, so that the reaction effect of metal impurities in each pickling chamber 4 can be conveniently detected, and the acid injection amount and the temperature can be timely adjusted; the sealing assembly comprises a sealing inserting plate 23 arranged on the inner side of the box cover 22, the sealing inserting plate 23 further improves the sealing effect of the box cover 22 and the main box body 21, the sealing inserting plate 23 is arranged between the pickling cavities 4, heat insulation layers are respectively arranged inside the sealing inserting plate 23 and inside the pickling box body 2, a sealing groove 24 which is oppositely arranged is formed between the side openings of the main box body 21 and the box cover 22, alkaline liquid is injected into the sealing groove 24 to prevent acidic steam from being dissipated to cause pollution to the outside, and the main box body 21 and the box cover 22 are pressed and fixed through a lock catch 25 to enable the main box body 21 to bear larger internal pressure.
In fig. 6, the centrifugal screen assembly 5 is integrally installed inside the box cover 22, the centrifugal screen assembly 5 includes a screen cylinder 51, the screen 52 is uniformly distributed on the screen cylinder 51 to disperse silicon particles into the pickling chamber 4 at a uniform speed, and the screen cylinder 51 is in transmission connection with the centrifugal driving assembly to provide a centrifugal driving moment for the screen cylinder 51. A material blocking cylinder 53 is arranged around the screen cylinder 51 to limit the scattered particles, and the scattered particles are collected in the pickling chamber 4. A material guide assembly is arranged inside the sieving cylinder 51; the material guiding component comprises a material guiding plate 54 which is spirally and uniformly arranged on the inner side of the screening cylinder 51, and the polycrystalline silicon particles are blocked by the material guiding plate 54 in the falling process in the screening cylinder 51 so as to be uniformly guided out from the surface of the screen 52. The guide plate 54 has base plates 55 overlapped with each other and opposite to the center of the screen cylinder 51, the base plates 55 being opposite to the inlet at the top of the screen cylinder 51; the centrifugal driving assembly comprises a driving rod 56 in transmission connection with the center of the screening drum 51, and the driving rod 56 is in transmission connection with a servo motor 57; the material blocking barrel 53 is in a cone shape, and the diameter of the upper end of the material blocking barrel 53 is smaller than that of the lower end. The servo motor 57 drives the driving rod 56 to rotate, and the upper end of the screening cylinder 51 is provided with a toothed ring which is meshed with the driving rod 56 for transmission, so that the normal feeding of the center of the upper end of the screening cylinder 51 is not influenced.
As can be seen, the fluidizing assembly 6, as shown in fig. 8, includes a fluidizing pipe 61 coiled at the bottom of the pickling chamber 4, the fluidizing pipe 61 is externally connected with an air injection line, and acid steam is injected through the fluidizing pipe 61, so that the reaction rate is higher than that of conventional acid solutions. Upward fluidization nozzles 62 are arranged on the surface of the fluidization pipe 61, the fluidization nozzles 62 are arranged at the bottom of the pickling chamber 4 in a matrix form, and a one-way valve is arranged between the fluidization nozzles 62 and the fluidization pipe 61 to ensure that the fluidization nozzles 62 jet air in one way. The fluidization nozzles 62 leave dispersion pipes 63; the dispersion pipe 63 comprises a main pipe 64 connected with the fluidization nozzle 62 and a branch pipe 65 which is obliquely downward, wherein the branch pipe 65 is arranged in central symmetry relative to the main pipe 64 and is used for guiding steam to be transmitted to the bottom of the pickling chamber 4, and the phenomenon that part of polycrystalline silicon particles are deposited at the bottom of the pickling chamber 4 and react unevenly is avoided.
The automatic acid supplementing assembly 7 and the fluidizing pipe 61 share the fluidizing nozzle 62, the automatic acid supplementing assembly 7 comprises an acid supplementing pipe 66 communicated with the fluidizing pipe 61, the fluidizing pipe 61 is not only filled with high-temperature steam to improve the reaction rate of metal impurities, but also filled with hydrofluoric acid and nitric acid to integrally adjust the internal pH value, and the acid liquor ratio is adjusted according to different metal impurities. The acid supplementing pipe 66 is externally connected with an evaporating pot 67 and an acid supplementing pump 68, an electric heating coil 69 is installed on the inner wall of the evaporating pot 67 in a fitting mode, acid liquor is injected into the evaporating pot 67, and acid gas is generated under the heating effect of the electric heating coil 69. The acid supplementing pipe 66 is provided with a pressure regulating valve 691, and pH sensors are respectively arranged in the acid supplementing pipe 66 and the acid washing cavity 4. The pressure regulating valve 691 maintains the internal pressure of the acid replenishing pipe 66 constant, and the PH sensor feedback-regulates the PH value inside the acid washing chamber 4.
As is apparent from fig. 9, the heating assembly 3 includes a heating pipe 31 communicating with the inside of the pickling chamber 4, and an insulating layer and a heat conductive layer are disposed between the heating pipe 31 and the pickling chamber 4 to indirectly heat the inside of the pickling chamber 4. The heating pipe 31 is externally connected with a heating box 32, and an electric heating pipe 33 and a circulating fan 34 are arranged in the heating box 32; the warm-pressing balancing component 8 comprises a pressure relief pipe 81 communicated with the pickling cavity 4, the pressure relief pipe 81 is externally connected with a pressure relief pump 82 and a neutralization pond 83, and a temperature sensor and a pressure sensor are arranged inside the pickling cavity 4. The pressure relief pipe 81 leads out excess gas inside, and the neutralization tank 83 contains a high-concentration alkaline solution for neutralizing acidic substances.
A method for removing impurities from polysilicon by acid washing comprises the following steps:
s1: crushing and grinding the polysilicon fragments by using the crushing assembly 1;
s2: the crushed polysilicon powder is input into an acid washing box body 2 and is uniformly dispersed into each acid washing cavity 4 by a centrifugal screening component 5;
s3: the fluidizing component 6 introduces acidic steam into the pickling chamber 4 for fluidizing reaction;
s4: the heating component 3 and the temperature-pressure balancing component 8 feed back and adjust the temperature and the pressure in the pickling cavity 4;
s5: the warm-pressure balance component 8 is used for pumping pressure inside the pickling cavity 4 and guiding out redundant acidic substances;
s6: the polysilicon powder after the completion of the acid cleaning is dried and discharged by the heating unit 3 and the fluidizing unit 6.
Example one
The crushing component 1 crushes and grinds the polysilicon fragments, then polysilicon particles are led into the pickling tank body 2, the fluidizing component 6 is introduced with acid steam, the polysilicon particles float under the fluidizing effect, and metal impurities on the surface of the polysilicon particles react with acid substances.
Then high-temperature steam is introduced into the fluidization assembly 6 to remove acid and wash the surface of the polycrystalline silicon, redundant solution is led out through the temperature and pressure balance assembly 8, the pickling tank 2 is opened after acid substances in the pickling tank 2 are completely led out, and polycrystalline silicon particles after impurity removal are led out.
Example two
The structure, the principle and the implementation steps of the embodiment are similar to those of the embodiment, and the difference is that the centrifugal sieving assembly 5 in the embodiment centrifugally separates the polysilicon particles introduced into the pickling tank 2, larger polysilicon fragments are suspended in the pickling chamber 4 by the centrifugal sieving assembly 5, and when acid gas is introduced into the pickling chamber 4, the centrifugal sieving assembly 5 drives the polysilicon fragments to rotate at a high speed, so that the polysilicon fragments and metal impurities on the surface of the polysilicon fragments jump and react with acid liquor in a contact manner.
EXAMPLE III
The structure, the principle and the implementation steps of this embodiment are similar to those of the embodiment, and the difference lies in that the fluidization assembly 6 and the automatic acid supplementation assembly 7 in this embodiment cooperate and continuously inject acidic steam towards the pickling chamber 4, the polycrystalline silicon particle surface is washed by the temperature and pressure balance assembly 8 after the reaction is completed, then the heating assembly 3 heats the inside of the pickling tank body 2, and meanwhile, the fluidization assembly 6 continuously injects high-temperature air to keep the inside polycrystalline silicon particles in a boiling state, so that the internal moisture is fully evaporated, and the relatively dry polycrystalline silicon particles are obtained.
In summary, the principle of the present embodiment is: the crushing assembly 1 further crushes the polysilicon fragments and guides the crushed polysilicon fragments into the pickling chamber 4, the fluidization assembly 6 keeps the polysilicon particles in a suspension state, the automatic acid supplementing assembly 7 introduces acid steam to react with metal impurities on the surfaces of the polysilicon particles, and the temperature and pressure balancing assembly 8 keeps the internal temperature and pressure constant, so that the metal impurities and the acid substances have higher reaction rate.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Although the pulverization assembly 1, the pulverization barrel 11, the unidirectional feed assembly 12, the feed inlet 121, the feed box 122, the baffle 123, the feed cavity 124, the opening and closing port 125, the opening and closing plate 126, the lifting assembly 13, the cutting assembly 14, the cutting motor 141, the cutting blade 142, the transmission gear 143, the transmission gear ring 144, the driven gear 145, the reversing gear 146, the driving gear 147, the cutting protrusion 148, the tapered boss 149, the grinding assembly 15, the grinding chamber 151, the grinding disc 152, the orifice 153, the ground particle layer 154, the step-by-step discharging assembly 16, the discharging guide rail 161, the discharging slider 162, the baffle 163, the discharging motor 164, the discharging gear 165, the discharging rack 166, the lifting barrel 167, the lifting screw 168, the lifting motor 169, the pickling box 2, the main box 21, the box cover 22, the sealing insertion plate 23, the lock 24, the lock 25, the heating assembly 3, the heating pipe 31, the heating box 32, the electric heating pipe 33, the circulating fan 34, the pickling cavity 4, the centrifugal sieve assembly 5, the pressing barrel 51, the screen 52, the baffle 53, the baffle 54, the base plate 55, the base plate 56, the servo feed assembly 57, the fluidization nozzle assembly 66, the fluidization pump assembly 66, the fluidization nozzle assembly 83, the fluidization pump 66, the fluidization tank 66, the fluidization distribution tank 66, the automatic fluidization distribution valve assembly, the fluidization distribution tank 66, the fluidization distribution pump 65, the fluidization distribution tank 66, the fluidization pump 65, and the fluidization distribution tank 65. These terms are used merely to more conveniently describe and explain the nature of the present invention; they are to be construed as being without limitation to the spirit of the present invention.
Claims (10)
1. The utility model provides a polycrystalline silicon pickling edulcoration equipment, includes crushing unit (1), crushing unit (1) be connected with pickling box (2), pickling box (2) built-in heating element (3), its characterized in that, pickling box (2) inside a plurality of independent pickling chamber (4) have, pickling chamber (4) in install respectively centrifugal sieve material subassembly (5) and with fluidization subassembly (6) of setting in pickling chamber (4), pickling box (2) be equipped with automatic acid supplementation subassembly (7) and warm-pressing balance subassembly (8).
2. The polycrystalline silicon acid cleaning impurity removing device according to claim 1, wherein the crushing assembly (1) comprises a crushing cylinder (11), a one-way feeding assembly (12) is arranged at an inlet of the crushing cylinder (11), a material lifting assembly (13) is arranged at an outlet of the crushing cylinder (11), and a cutting assembly (14) and a grinding assembly (15) are arranged inside the crushing cylinder (11).
3. The polycrystalline silicon acid cleaning impurity removing device according to claim 2, wherein the cutting assembly (14) comprises a cutting motor (141), and the cutting motor (141) is in transmission connection with a cutting blade (142) through a synchronous transmission assembly; the synchronous transmission assembly comprises a transmission gear (143) and a transmission toothed ring (144) which are concentrically arranged, a plurality of driven gears (145) which are symmetrically arranged relative to the center of the transmission gear (143) and the transmission toothed ring (144) are in meshing transmission between the transmission gear (143) and the transmission toothed ring (144), the driven gears (145) are connected with the cutting blade (142), the transmission gear (143) is connected with a plurality of reversing gears (146) in meshing transmission, and the reversing gears (146) and the transmission toothed ring (144) are connected with the cutting motor (141) through a driving gear (147); cutting blade (142) be discoid and the upper end be provided with relative central symmetry and be triangle-shaped cutting arch (148), cutting blade (142) be provided with the sawtooth along circumference, crushing barrel (11) inside be provided with and be used for rotating cone boss (149) of installation cutting blade (142), cutting blade (142) bottom be provided with the conical surface that covers in cone boss (149) outside.
4. The polycrystalline silicon acid washing impurity removing equipment according to claim 3, wherein the grinding assembly (15) comprises a grinding chamber (151) arranged below the cutting assembly (14), a plurality of grinding discs (152) which are arranged in a stacked mode are rotatably arranged in the grinding chamber (151), leak holes (153) are uniformly distributed in the grinding discs (152), grinding particle layers (154) are distributed on one side, opposite to the adjacent grinding discs (152), of each grinding disc, and a spray head used for spraying grinding aid is arranged in the grinding chamber (151).
5. The polycrystalline silicon acid cleaning impurity removing equipment according to claim 2, characterized in that the one-way feeding component (12) comprises a feeding port (121) arranged at the upper end of the crushing cylinder body (11), a feeding box body (122) is arranged at the upper end of the crushing cylinder body (11), the feeding box body (122) is internally divided into a plurality of independent feeding cavities (124) by obliquely arranged baffle plates (123), an opening and closing port (125) opposite to the internal feeding cavity (124) is formed in one side of the feeding cavity (124), the opening and closing port (125) is closed by a plurality of opening and closing plates (126) which are in sliding connection, and a step-by-step discharging component (16) is arranged between one end of the feeding box body (122) and the feeding port (121); the progressive discharging assembly (16) comprises discharging guide rails (161) arranged on two sides of a feeding port (121), discharging sliding blocks (162) are respectively installed on the discharging guide rails (161) in a sliding mode, the discharging guide rails (161) extend to the upper side of the crushing barrel body (11), the discharging sliding blocks (162) are rotatably connected with a feeding box body (122), a barrier strip (163) for preventing an opening and closing plate (126) from falling into the crushing barrel body (11) is arranged at the edge opening of the feeding port (121), a discharging motor (164) is installed at the upper end of the crushing barrel body (11), a discharging gear (165) is fixed at the output end of the discharging motor (164), and a discharging rack (166) in meshing transmission with the discharging gear (165) is arranged on the outer side of the feeding box body (122); the material lifting assembly (13) comprises a material lifting barrel (167) which is obliquely arranged, a material lifting screw rod (168) is arranged in the material lifting barrel (167), and the material lifting screw rod (168) is in transmission connection with a material lifting motor (169) through a coupler.
6. The polycrystalline silicon acid cleaning impurity removing device according to claim 1, wherein the acid cleaning box body (2) comprises a main box body (21) and a box cover (22) for closing the upper end of the main box body (21), the acid cleaning cavities (4) are arranged in the main box body (21) at equal intervals, the inner sides of the acid cleaning cavities are covered with acid-proof surface layers, and the acid cleaning cavities (4) are mutually separated through a sealing assembly; seal assembly including setting up at inboard sealed picture peg (23) of case lid (22), sealed picture peg (23) arrange between pickling chamber (4), sealed picture peg (23) inside and pickling box (2) inside be provided with the insulating layer respectively, main tank body (21) and case lid (22) limit mouth between open seal groove (24) that have the relative arrangement, seal groove (24) in inject alkaline liquid, main tank body (21) and case lid (22) compress tightly fixedly through hasp (25).
7. The polycrystalline silicon acid washing impurity removing equipment according to claim 1, wherein the centrifugal screen material component (5) comprises a screen material cylinder (51), screen meshes (52) are uniformly distributed on the screen material cylinder (51), the screen material cylinder (51) is in transmission connection with a centrifugal driving component, a material blocking cylinder (53) is arranged around the screen material cylinder (51), and a material guiding component is arranged inside the screen material cylinder (51); the material guiding assembly comprises a material guiding plate (54) which is uniformly arranged on the inner side of the material screening cylinder (51) in a spiral shape, and the material guiding plate (54) is provided with base plates (55) which are mutually overlapped and are opposite to the center of the material screening cylinder (51); the centrifugal driving assembly comprises a driving rod (56) in transmission connection with the center of the screen material cylinder (51), and the driving rod (56) is in transmission connection with a servo motor (57); the material blocking cylinder (53) is in a cone cylinder shape, and the diameter of the upper end of the material blocking cylinder (53) is smaller than that of the lower end.
8. The polycrystalline silicon acid cleaning impurity removing device according to the claim 1, characterized in that the fluidizing component (6) comprises a fluidizing pipe (61) coiled at the bottom of the acid cleaning chamber (4), the surface of the fluidizing pipe (61) is provided with upward fluidizing nozzles (62), a one-way valve is arranged between the fluidizing nozzles (62) and the fluidizing pipe (61), and the fluidizing nozzles (62) are provided with a dispersion pipe (63); the dispersion pipe (63) comprises a main pipe (64) connected with the fluidization nozzle (62) and a branch pipe (65) which is inclined downwards, and the branch pipe (65) is arranged in a central symmetry way relative to the main pipe (64); automatic mend sour subassembly (7) include the benefit sour pipe (66) that communicate with fluidization pipe (61), benefit sour pipe (66) external evaporating pot (67) and benefit acid pump (68), evaporating pot (67) inner wall laminating install electric heating coil (69), benefit sour pipe (66) on install pressure regulating valve (691), benefit sour pipe (66) and pickling chamber (4) in be provided with the PH sensor respectively.
9. The polycrystalline silicon acid cleaning impurity removing device according to claim 1, wherein the heating assembly (3) comprises a heating pipe (31) communicated with the inside of the acid cleaning chamber (4), the heating pipe (31) is externally connected with a heating box (32), and an electric heating pipe (33) and a circulating fan (34) are arranged in the heating box (32); warm pressure balance subassembly (8) include pressure release pipe (81) with pickling chamber (4) intercommunication, pressure release pipe (81) external pressure release pump (82) and neutralization pond (83), pickling chamber (4) inside be provided with temperature sensor and pressure sensor.
10. A polycrystalline silicon acid cleaning impurity removal method adopts the polycrystalline silicon acid cleaning impurity removal device of any one of claims 1 to 9, and is characterized by comprising the following steps:
s1: crushing and grinding the polysilicon fragments by using a crushing assembly (1);
s2: the crushed polysilicon powder is input into an acid washing box body (2) and is uniformly dispersed into each acid washing cavity (4) by a centrifugal screening component (5);
s3: the fluidizing component (6) introduces acidic steam into the pickling chamber (4) to perform a fluidizing reaction;
s4: the heating component (3) and the temperature and pressure balancing component (8) feed back and regulate the temperature and pressure inside the pickling cavity (4);
s5: the temperature and pressure balance component (8) is used for pumping the interior of the pickling cavity (4) and leading out redundant acidic substances;
s6: the polysilicon powder after the acid cleaning is dried and discharged by the heating assembly (3) and the fluidizing assembly (6).
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