KR20120082530A - A recycling and treatment method of waste liquid in cutting mono silicon - Google Patents

Abstract

PURPOSE: A method for collecting cutting waste liquid of mono silicon is provided to have high recovery ratio and to contribute to environmental protection. CONSTITUTION: A method for collecting cutting waste liquid of mono silicon is as follows. The cutting waste liquid of mono silicon removing petroleum is put in a spraying stirrer(49), and hydrochloric acid is injected to obtain mixture. The mixture is discharged to a spraying mixer. The cutting waste liquid of mono silicon is mixed for 10 to 30 minutes at the temperature of 30°C-50°C again to obtain secondary mixture. The secondary mixture is put into a solid-liquid separator and is heated by an electric heating plate of which heating temperature is 50°C-80°C. Carbonized silicon and rough crystallized solid mixture of the silicon are discharged at the bottom of the solid-liquid separator. The solid mixture is put in a first spraying cleaner and implements a cleaning work for 10 to 30 minutes so that a first cleaning solid mixture removing residues can be obtained. The first cleaning solid mixture is put into a second spraying cleaner and is repetitively cleaned to obtain secondary cleaning solid mixture. The secondary cleaning solid mixture puts into a reactor and implements a stirring reaction for 10 to 30 minutes. The carbonized silicon and acid solution are cleaned and dried with alkaline solution after filtering, thereby collecting the carbonized silicon.

Description

Monocrystalline silicon cutting waste liquid treatment recovery method {A RECYCLING AND TREATMENT METHOD OF WASTE LIQUID IN CUTTING MONO SILICON}

The present invention relates to a single crystal silicon cutting waste liquid treatment recovery method.

As tensions and pollution increase over the years, the important visual attitudes of the use of clean energy sources have drawn attention. Globally, it is causing the trend of development of solar cell. In recent years, research and production of solar cell have been developed very fast in recent years, and the wide application to solar cell has already produced the production of single crystal silicon, the main raw material of solar cell. It's also very fast, so it's developing quickly and quickly. Monocrystalline silicon chips used in solar cells are made by cutting single-crystal silicon sticks, and during the cutting of single-crystal silicon sticks, cutting fluids that induce lubricative cooling must be used. As a result, a large amount of cutting waste fluid is produced during the cutting process. Conventionally, cutting fluids commonly employed in Korea include one of a mixture of polyethylene glycol, silicon carbide, triacetamide, saponification liquid, paraffin, and the like. As a result, the COD value of the cutting waste fluid is greatly exceeding the wastewater discharge standard, and wastewater discharge is prohibited based on the requirements of environmental protection and environmental safety. However, in the past, it was also impossible to produce a suitable waste liquid collection and recovery method, which is why the domestic mass production plant merely accumulates a large amount of waste liquid and leaves it unattended. The accumulated waste liquid accumulated over the mountain is also wrapped up like a mountain, and the companies are already forced to leave the waste liquid continuously produced. Therefore, there is an urgent search for a method for treating and recovering a single, simple and effective single crystal silicon cutting waste solution. Accordingly, among the cutting liquids, polyethylene glycol, silicon carbide, and silicon are mainly recovered. The recovery and recovery of the waste solution not only solves the environmental problems, but also has very large economic benefits.

The present invention provides a single crystal silicon cutting waste liquid treatment recovery method.

The single crystal silicon cutting waste liquid recovery method of the present invention includes the following steps.

1.Place petroleum-free single crystal silicon cutting waste solution in a spray stirrer and inject dilute hydrochloric acid.The concentration of hydrochloric acid is then 0.0001-0.4mol, and 100-500ml of hydrochloric acid solution is injected for every 1 kg of waste liquid. Mixing for 10 to 30 minutes via spraying gives the first stage of mixing material, which is then discharged and placed in the spray mixer, then mixed for 10 to 30 minutes with circulating spraying, the temperature is between 30 ° C and 50 ° C. Ascending, the second stage of mixed material is obtained and discharged.

In the production plant, the waste liquid already in the round barrel is inclined several times, and the waste is filtered out. Thus, the oil is basically removed from the waste liquid to be treated.

The single crystal silicon cutting waste liquid is a very strong and solid powder form, and has a high viscosity concentration, which makes it difficult to transport fluidly and process in the process. The waste liquid in the method of the present invention is treated with dilute hydrochloric acid, and hydrochloric acid is generated through neutralization to remove triacetamide and saponified liquid, which are alkaline substances contained in the waste liquid, and at the same time to ensure the viscosity of the waste liquid. Weakening and, through the circulating spray agitation mixing in the spray stirrer and spray mixer, can be easily made into a homogeneous mixed material to allow the waste liquor to be flowable in one flow, thereby benefiting processing in the process.

The spray stirrer mixes and reacts the injected acid solution with the highly viscous waste liquid as evenly as possible. The mixed material is ejected through the first spray passage in the spray stirrer, forms circulating mixing in one large range, and also creates negative pressure in the nozzle chamber, so that the mixed material is a liquid flow hole. Entering the spray chamber through, again, a small range of mixing is formed, whereby such a method can greatly increase the effect of stirring mixing and reaction.

The structural characteristics of the spray mixer are that the spray passage and the guide plate are installed in the spray apparatus, and an alternating current tube is installed in the spray passage, and the Reynolds number Re of the liquid flow (Reynolds ratio of the inertia and internal frictional force when the liquid flows) More than 3000, which causes the liquid flow to exhibit rapid rapid flow, causing the mixed material to collide and friction between molecules in the alternating tube, to mix the mixed material and to further granulate the granules. Again, due to the installation of the guide plate, the mixed material forms a small range of flows, which makes the effect of mixing and reaction even more desirable.

2. The secondary mixed material discharged from the spray mixer enters the solid liquid separator, and the mixed material is vaporized together with water vapor and polyethylene glycol through heating of an electric heating plate having a heating temperature of about 50 ° C to 80 ° C. By cooling through a 1st cooler, the liquid mixture of water and polyethylene glycol is obtained. After being put into the spray dehydrator for 15 minutes to 40 minutes of circulation spray dehydration, the temperature rises to 40 ° C. to 80 ° C., and the polyethylene glycol can be recovered immediately after the water is discharged from the spray dehydrator. . At the bottom of the solid liquid separator, a solid mixture of silicon carbide and coarse crystals of silicon is released.

The principle of operation of the spray dehydrator is that the liquid flow of water and polyethylene glycol causes alternating flow in the alternating passage, and collisions and friction between molecules occur in the alternating tube, which causes molecular granules of water and polyethylene glycol. In this more finely divided and circulating spray mixing process, as the temperature gradually rises, water molecules having a low boiling point are evaporated and discharged, thereby reaching the purpose of polyethylene glycol dehydration.

3. A silicon mixture of coarse crystals of silicon carbide and silicon is sent to the first spray washer, adding 10% to 20% water by weight of the solid mixture of coarse crystals, and performing a circulating spray cleaning for 10-30 minutes. The temperature is then raised to 40 ° C.-80 ° C., after washing, the mixture is placed on a first rocking table and the light weight “remaining residues of the outer shell” are separated off. To obtain a first wash solid mixture of silicon carbide and silicon. And then sent back to the second spray washer, after which the solid mixture was again duplicated in the same form as before, after the first circulating spray wash, the mixture was placed in the second separator and again the "remaining residue of the outer shell". By separating off, a second wash solid mixture of silicon carbide and silicon is obtained.

Sodium and other impurities contained in a solid mixture of silicon carbide and coarse crystals, produced by neutralization, are very difficult to remove from the outer surface of silicon carbide powder and silicon powder because they are tightly wrapped in the form of an "outer shell". . Secondly, the spray washing machine is used for washing with water, and by repeated circulation stirring, the molecules of the material material and the water molecules in the mixture are broken and the granules of the material material are subdivided during the collision and friction process. As the outer shell breaks up and comes off, it acts as a cleaning action, again separated through the separator, and due to the difference in specific gravity, the silicon carbide and silicon are separated from the "remaining residue of the outer shell" and the "outer" After recovering the remaining residues of the shell ", it can also be used for fertilizers.

4. A second wash solid mixture of silicon carbide and silicon is sent to the reactor to recover the reaction in which silicon produces fluorosilicic acid and to separate and recover the silicon carbide and silicon in the solid mixture. A mixed acid solution composed of HNO ₃ with a concentration of about 5% and HF with a concentration of about 30% is added. The volume ratio is HNO _₃ : HF = 1: 5, and every 1 kg of silicon carbide and silicon solid 1-1.5 kg of mixed acid solution is added to the mixture, which is subjected to a circulating spray stirring reaction for about 10 to 30 minutes and the temperature is raised to the reflux temperature, so that the fluorinated silicone acid solution is evaporated and cooled through the second cooler. As a result, a colorless transparent fluorinated silicone acid solution can be obtained. In order to operate a silicon fluoride solution according to a conventional method, after drying it, it is a method of recovering silicon after processing into single crystal silicon. The excess silicon carbide and acid solution in the reactor can be washed with an alkaline solution of 5-10 wt% after filtration and dried until the pH reaches 7-7.5 to recover the silicon carbide. The alkaline solution may be selected by mixing NaOH and KOH or Na ₃ CO₃.

Apparatus used in the single crystal silicon cutting waste liquid treatment recovery method to be realized in the present invention, the spray stirrer 49, the spray mixer 50, the solid liquid separator 30, the spray dehydrator 51, the first spray washing machine, the reactor (52).

The structure of the spray stirrer 49 should refer to FIGS. 2 and 3, and the spray stirrer 49 includes a first mixing tank 65, a first material supply tank 63, and a first spray passage 66. And a first diaphragm pump 61, a first T-pipe valve 62, and a first material discharge pipe 64. A first material addition tube 69 under the first material supply tank 63 is mounted in a cover on the first mixing tank 65 and is also placed in the first mixing tank 65. The first spray passage 66 includes a nozzle 70, a nozzle chamber 72 and a first nozzle outlet 73, which are in turn communicating with each other, one on each side of the wall of the nozzle chamber 72 The liquid flow hole 71 is provided, and the diameter of the nozzle is about 3 mm-4 mm. The first diaphragm pump 61 is located on a first connecting pipe 68 that is identical to the first T-pipe valve 62 and the first material outlet 67 at the bottom of the first mixing tank 65. The first material discharge pipe 64 is interconnected with the first T-way valve 62.

The first material discharge pipe 64 of the spray stirrer 49 is interconnected with the spray mixer 50, the structure of the spray mixer 50 (the equipment has already applied for a utility model patent, the patent number (200620039272.3) refers to the drawings of FIGS. 4 to 6, wherein the mixing tank 3, the material supply tank 6, the spraying device 5, the diaphragm pump 1, and the heat resistance temperature measurement The head 2, the T-pipe valve 7 and the material discharge pipe (4). The material addition pipe 9 below the material supply tank 6 is mounted on the cover of the mixing tank 3 and is also put into the mixing tank 3. The spray device 5 comprises a spray passage 19 and a guide plate 15. The spray passage 19 includes a nozzle inlet 10, an alternating tube 11, a mixing chamber 12, and a nozzle outlet 13 which in turn communicate with each other. The nozzle inlet 10 has a funnel shape, the diameter of the AC tube 11 is 1.2 mm-3 mm, and one liquid flow inlet 14 is provided on each side of the wall of the mixing chamber 12. Is installed. The guide plate 15 is installed vertically on the spray passage 19, and is located between the liquid flow guide port 14 and the nozzle outlet 13, and the small holes 16 on the guide plate 15. ) Is distributed, the hole diameter of the small hole 16 is about 1mm-3mm, the porosity of the guide plate 15 is about 60%-80%. The diaphragm pump is located on the connecting pipe 8 between the T-pipe valve 7 and the material outlet 18 at the bottom of the mixing tank 3, and the material discharge pipe 4 interacts with the T-pipe valve 7. It is connected. The heat resistance temperature measuring head 2 is fixedly installed in the mixing tank 3, and the upper cover of the mixing tank 3 penetrating through the lead wire is interconnected with the temperature indicator 17.

The structure of the solid liquid separator 30 refers to FIGS. 7 and 8, and the solid liquid separator 30 includes a sprinkler head 31, a gas outlet pipe 33, a conical plate 42, and a funnel. A type plate 41, a solid outlet 37, and the like, and the material discharge pipe 4 of the spray mixer interacts with the sprinkler head 31 installed at the center of the top cover of the solid liquid separator 30. In the solid liquid separator 30, two units of electric heating plates are installed on the outer wall 36 and fixed up and down symmetrically. The structure of the electric heating plates of each unit is as follows. That is, the upper direction is one conical plate 42, the lower direction is one funnel plate 41 and the hole 40, and the diameter of the funnel plate 41 is the conical plate It is larger than the diameter of 42. The conical plate 42 is fixed on three position fixing nails 32 which are arranged at 120 ° C., and the three fixing nails 32 are fixed on the outer wall 36. The funnel-shaped plate 41 is fixed on the tray 35, and the tray 35 is fixed on the outer wall 36 with fixing screws 34. A gas outlet pipe 33 is provided on the top cover, a solid outlet 37 is provided at the bottom, and a baffle plate 39 is provided around four locations of the solid outlet 37. In addition, one liquid outlet 38 is provided.

The structure of the spray dehydrator 51 (see FIG. 9, the spray device 5 'in FIG. 9 refers to FIGS. 5 and 6) is basically the same as the spray mixer 50, and the spray The improvement in the structure of the dehydrator 51 is that one drain pipe 21 is provided on the top cover, in which the solid liquid separator 30 passes through the first cooler and is interconnected with the spray dehydrator 51. do.

The structure of the spray dehydrator 51 is mainly composed of a mixing tank 3 ', a material supply tank 6', a spray device 5 ', a diaphragm pump 1', a heat resistance thermometry head 2 '. And a T-pipe valve 7 ', a material discharge pipe 4' and a drain pipe 21 are included. A material addition tube 9 'below the material supply tank 6' is mounted on the top cover of the mixing tank 3 ', and is also contained in the mixing tank 3'. In addition, one drain pipe 21 is provided on the upper cover of the mixing tank 3 '. The spray device 5 'includes a spray passage 19' and a guide plate 15 '. The spray passage 19 'includes a nozzle inlet 10', an alternating tube 11 ', a mixing chamber 12', and a nozzle outlet 13 'which communicate with each other in turn. The nozzle inlet 10 'has a funnel shape, and the diameter of the AC tube 11' is about 1.2 mm-3 mm, and the liquid flow guide holes are formed at both sides of the wall surface of the mixing chamber 12 ', respectively. 14 ') is installed. The guide plate 15 'is installed on the spray passage 19' with a vertical direction, and is located between the liquid flow guide 14 'and the nozzle outlet 13', and the guide plate ( 15 '), small pores 16' are distributed, the diameter of the small holes 16 'is about 1mm-3mm, and the porosity on the guide plate 15' is about 60%-80%. The diaphragm pump 1 ′ is located on a connecting pipe 8 ′ between the T-shape valve 7 ′ and the bottom material outlet 18 ′ of the mixing tank 3 ′. ') And the T-pipe valve 7' are interconnected. The thermal resistance temperature measuring head 2 'is fixedly installed in the mixing tank 3', and an upper cover through the mixing tank 3 'through a lead wire is interconnected with the temperature indicator 17'. do.

A first spray washer (not shown) is interconnected with the solid outlet 37 of the solid liquid separator 30. The structure of the first spray washer is the same as that of the spray mixer 50. The first spray washer is in turn interconnected with the first separator, the second spray washer, and the second separator, the structure of the second spray washer is the same as the structure of the first spray washer, and the second spray The washer is again interconnected with the reactor 52.

The reactor 52 (as shown in FIG. 10, see FIG. 3 for an enlarged view of the spray passage 66 in FIG. 10) is essentially the same as the spray stirrer 49, and in the structure The improvement is that one vapor liquid tube 22 is provided on the top cover, and the steam liquid tube 22 is connected to the second cooler in the apparatus.

The structure of the reactor 52 is mainly composed of a second mixing tank 65 ', a second material supply tank 63', a second spray passage 66 ', a second diaphragm pump 61', a second A T-tube valve 62 ', a second material discharge pipe 64' and a vapor liquid pipe 22. A second material addition tube 69 'below the second material supply tank 63' is mounted on the top cover of the second mixing tank 65 ', and also within the second mixing tank 65'. Expand it. In addition, the one vapor liquid pipe 22 is provided on the upper cover of the second mixing tank 65 '. The second spray passage 66 'includes a second nozzle 70', a second nozzle chamber 72 'and a second nozzle outlet 73' which in turn communicate with each other. One liquid flow hole 71 'is provided at both sides of the wall surface of the nozzle chamber 72', and the diameter of the second nozzle is approximately 3mm-4mm. The second diaphragm pump 61 ′ is a second connecting pipe 68 ′ between the second T-pipe valve 62 ′ and the bottom second material outlet 67 ′ of the second mixing tank 65 ′. And the second material discharge pipe 64 'is interconnected with the second T-pipe valve 62'.

In the present invention, the treatment recovery method of the single crystal silicon cutting waste liquid has a simple method, a simple facility, an easy operation in control, a low cost, and a high treatment recovery ratio. The total recovery calculated on the basis of the total amount of cutting waste is 26%-46%, of which polyethylene glycol accounts for 20%-30%, and silicon carbide accounts for 5%-15%. Accounts for 1%-2%. In addition, the quality of the products made from recovered products can all reach or approach the standards of standard products, and this technology can be applied directly to the production of solar energy batteries or in other industrial areas. For this reason, the method of the present invention not only has enormous economic benefits, but can also make a great contribution to environmental protection, and the present invention is a method for recovering single crystal silicon cutting waste liquid, which is likely to be developed.

1 is a processing process diagram of a method for recovering a single crystal cutting waste liquid according to the present invention;
2 is a structural diagram of a spray stirrer of the apparatus of the method to realize the present invention.
3 is an enlarged view of a portion A in FIG. 2.
4 is a structural diagram of a spray mixer of the apparatus of the method to realize the present invention.
FIG. 5 is a longitudinal sectional view of the spray apparatus in FIG.
6 is a left side of the guide plate in FIG.
7 is a structural diagram of a solid liquid separator of the apparatus of the method to implement the present invention.
8 is a bird's eye view of the A-A direction in FIG.
9 is a structural diagram of a spray dehydrator of the apparatus of the method to realize the present invention.
10 is a structural diagram of a reactor in an apparatus of a method to implement the present invention.

Example  One

Reference is made to FIGS. 1 to 6 of the drawings. 50 kg of petroleum-free single crystal silicon cutting waste and 10 liters of dilute hydrochloric acid having a concentration of 0.01 mol are added to the first mixing tank of the spray stirrer 49 through the first material supply tank 63 and the first material addition tube 69. It is injected into (65). The first T-pipe valve 62 opens the passage with the first spray passage 66, closes the passage with the first material discharge pipe 64, and operates the first diaphragm pump 61 (starting diaphragm pump). The product serial of QBY-40, was produced by Shanghai Changchun Pump Manufacturing Co., Ltd.). The air pressure is 3 kg / cm 2, and the mixed material flows out of the first material outlet 67 at the bottom of the first mixing tank 65 so that the first diaphragm pump 61, the first connecting pipe 68, and the first material are discharged. Via the 1 T tube valve 62, the nozzle 70 enters the nozzle 70 having a nozzle diameter of 3 mm, and the mixed material passes through the nozzle chamber 72 at a high speed. Ejected at the nozzle outlet 73 to form one large range of circulating mixing. In addition, a negative pressure is formed in the nozzle chamber 72, and a pressure difference is made inside and outside the wall of the nozzle chamber 72, and the mixed material outside the wall is transferred through the liquid flow hole 71. Entering the nozzle chamber 72, again, a small range of cyclic mixing is formed, whereby the mixing and reaction effects are more desirable. This configuration allows a mixed material to pass through the first material outlet 67 at the bottom of the first mixing tank 65, wherein the first diaphragm pump 61 is connected to the first spray passage 66 and one circulation circuit. The repeated circulation as described above is performed for about 25 minutes of stirring and mixing with respect to the nozzle 70. The first T-pipe valve 62 closes the passage with the first spray passage 66, and opens the passage with the first material discharge tube 64, so that the first stage mixed material obtained in the starting stage is collected from the first stage. The material is discharged from the discharge pipe 64, and then reenters the spray mixer 50 again to proceed with mixing. The first stage mixed material obtained in the starting stage is mixed through the spray stirrer, and the viscosity of the mixed material is relatively low to some extent, but there are phenomena in which the concentration of the liquid and the solid powder is thick and do not mix uniformly.

The primary mixed material obtained in the starting stage is passed through the material supply tank 6 and the material addition tube 9 into the mixing tank 3 of the spray mixer 50, and the T-screw valve 7 is connected to the nozzle inlet. Opening the passage with (10) and closing the passage with the material discharge pipe (4) to start the diaphragm pump (1), wherein the mixed material flows out of the material outlet (18) at the bottom of the mixing tank (3) and the diaphragm It enters the nozzle inlet 10 of the spray device 5 via the pump 1 and the connecting pipe 8 and the T-pipe valve 7, and enters the AC pipe 11 (the corresponding pump flow rate is 3 M 3 / h, the diameter of the alternating current tube 11 is 2.4 mm, when the power viscosity of the mixed material is 33.2 Pa · S, Reynolds number = 8326), the mixed material exhibits an alternating current, thus mixing The material is the collision of the molecules and friction occurs in the alternating current tube 11, the mixed material is mixed with The granular material is further subdivided, the mixed material exits the flow tube 11 and is ejected towards the mixing chamber 12 as a uniformly small granule of mist-like liquid, which also penetrates rapidly at the nozzle outlet 13, The conventional mixing material penetrates through the pores 16 on the guide plate 15 in the opposite direction and enters the outside of the wall of the mixing chamber 12, whereby a pressure difference is generated inside and inside the wall of the mixing chamber 12. By being made, the mixed material passes through the liquid flow inlet 14 so that a small range of flow is formed, thereby further enhancing the effects of mixing and reaction. In this form, the mixed material passes through the material outlet 18 of the bottom of the mixing tank 3, and the diaphragm pump 1 and the spray device 5 constitute one circulation circuit. The repetitive circulation is spray mixed for about 20 minutes, the temperature is raised to 35 ° C. (measured through the thermal resistance thermometry head 2 and showing the condition of the temperature on the temperature indicator 17). The T-pipe valve 7 closes the passage with the nozzle inlet 10 and opens the passage with the material discharge pipe 4 to discharge the secondary mixed material from the material discharge pipe 4 and through spray mixing. By reliably lowering the viscosity of the subsequent secondary mixed material, a uniformly mixed mixed material which is already easy to flow is produced.

After mixing through the spray mixer, the secondary mixed material enters the solid liquid separator 30, the structure of which is shown in FIGS. 7 and 8, the sprinkler head 31, the gas outlet pipe 33 , Conical plate 42, funnel plate 41, solid outlet 37, and the like. Inside the solid liquid separator 30, two electric heating plates are provided which are fixed on the outer wall 36 in the vertically symmetrical manner. The mixed material is injected into the solid liquid separator 30 through the sprinkler head 31 in which the top cover center is installed, and the mixed material is outside the conical plate 42 in the upper direction of one electric heating plate unit located at the top. It falls on the layer and again falls on the inner layer of the funnel-shaped plate 41 in the downward direction along the four circumferences and proceeds with heating. It enters again on the lower one electric heating plate through the hole 40 in the bottom of the funnel-shaped plate 41, and heating proceeds in the same manner, and the temperature of the electric heating plate is maintained at 70 ° C. After the mixed material is heated, the water vapor and polyethylene glycol together evaporate out of the gas outlet tube 33 at high speed and are cooled through the first cooler, i.e., a mixture of water and polyethylene glycol can be obtained. Slightly cooled liquid droplets may appear on the inner wall of the solid liquid separator 30 and flow along the wall, ie outflow to the liquid outlet 38. The solid obtained by the heat separation is discharged to the solid outlet 37 installed at the bottom of the solid liquid separator 30, and the released material becomes a mixture of coarse crystals of silicon carbide and silicon, i.e., it contains the produced sodium and impurities One is a mixture of silicon carbide and silicon. In order to prevent the mixture of the silicon carbide and the coarse crystals of silicon from being blown toward the surrounding wall surface, the liquid droplets flowing from the inner wall surface are splashed into the solid outlet 37 while being discharged straight down toward the solid outlet 37. In order to prevent the flow, the baffle plate 39 is provided around the four places.

The mixed liquid of the obtained water and polyethylene glycol enters the spray dehydrator 51. Referring to FIG. 9, the structure of the spray dehydrator 51 is basically the same as that of the spray mixer 50, and the improved change in the structure of the spray dehydrator 51 is one drain pipe 21 on the top cover. Is installed. The mixed liquid of water and polyethylene glycol enters the mixing tank 3 'of the spray dehydrator 51 through the material supply tank 6' and the material addition tube 9 ', and the diaphragm pump 1' is operated. In addition, the circulation spray dehydration proceeds repeatedly, the operation process is the same as the spray mixer, the liquid flow is the alternating flow appears in the alternating pipe (11 '), the flow rate of the diaphragm pump (1') of the circulation is 2.5 ㎥ / h, the diameter of the flow tube is 2.0 mm, and the Reynolds number = 7319 when the power viscosity of the water and polyethylene glycol mixture is 19.2 Pa.S. The circulation spray dehydration time is about 20 minutes, the temperature rises to 70 ° C., and after the water is discharged to the drain pipe 21, the T-pipe valve 7 'closes the passage with the nozzle inlet 10'. , Opening the passage with the material discharge pipe 4 ', the polyethylene glycol is discharged and recovered from the material discharge pipe 4', 15kg of colorless transparent polyethylene glycol is obtained, the measured molecular weight is 205, PH = 6.5, moisture content <0.3 wt% (the molecular weight of the standard product of polyethylene glycol is 300, PH = 4-7, moisture content <= 0.5 wt%), polyethylene glycol calculated on the basis of 50 kg of cutting waste liquid Recovery reaches 30%.

A solid mixture of silicon carbide and coarse crystals of silicon discharged from the solid outlet 37 of the solid liquid separator 30 is sent into the first spray washer, the structure of the first spray washer (not shown) of the spray mixer 50 The same as the structure, the solid mixture of silicon carbide and the coarse crystals of silicon enters the mixing tank 3 through the material supply tank and the material addition tube in the same form, and again 15% for the weight of the solid mixture of coarse crystals. Add a little water. The diaphragm pump is operated, and the cyclic spray mixing washing is repeatedly performed, and the operation process is the same as that of the spray mixer 50. The mixture exhibits an alternating flow in an alternating tube, and the flow rate of the circulating diaphragm pump is 2.1 m 3 / h. The diameter of the AC tube is 2.6 mm, and the Reynolds number is 3979 when the power viscosity of the mixed material of the solid mixture and the water is 13.5 Pa · S. The cycle mixing wash time is about 30 minutes, the temperature is raised to 70 ° C, and after washing, the mixture is placed in the first separator (provided by Shanghai Huayan Equipment Co., Ltd., product number HWY-211), so that the specific gravity The remaining debris of the shell "is removed and the water is discharged to a tank installed on the separator, to obtain a first washing solid mixture of silicon carbide and silicon, which is then sent to a second spray washer, the structure of which is first It is the same as the spray washer, and the solid mixture is repeatedly subjected to the first circulation spray mixing washing, the flow rate of the circulating diaphragm pump is 3㎥ / h, the diameter of the alternating tube is 2.1mm, and the mixed material When the power viscosity is 16.8 Pa? S, the Reynolds number = 8670, and the rest of the operation is the same. After washing, the mixture is placed in a second separator (provided by Shanghai Huayan Equipment Co., Ltd., product number 350R), and the "remaining residue of the outer shell" and water are separated and removed, and a second washing solid mixture of silicon carbide and silicon is removed. Obtained. After recovering the separated "remaining residue of the outer shell", it can be used for fertilizers.

The obtained second carbide solid mixture of silicon carbide and silicon is sent to the reactor 52. Referring to FIG. 10, the structure of the reactor 52 is basically the same as that of the spray stirrer 49, and the improvement in structure The change is that one vapor liquid conduit 22 is installed on the top. A secondary wash solid mixture of silicon carbide and silicon enters into the second mixing tank 65 'of the reactor 52 through the second material supply tank 63' and the second material addition tube 69 '. In addition, the same amount of mixed acid solution (volume HNO ₃ : HF = 1: 5) as the solid mixture composed of HNO ₃ having a concentration of about 5% and HF having a concentration of about 30% is added. The pump 61 'is operated and the circulation spray agitation reaction is repeatedly performed for about 10 minutes, the diameter of the second nozzle is 3.5 mm, the temperature reaches the reflux temperature, and the silicon fluoride solution is a vapor liquid tube. It is evaporated and discharge | released to 22, and it cools through a 2nd cooler, and a colorless transparent fluoric-acid fluoric acid solution can be collect | recovered. The concentration of the silicon fluoride solution is 30wt%, the silicon fluoride solution is operated in a conventional manner, and after drying, it is put into a single crystallization furnace and processed into single crystal silicon. When the vacuum in the single crystal furnace is reduced, hydrogen is added as a protective gas, it is melted through electric heating, and the temperature is controlled again by using cooling water, so that the crystal starts when the furnace temperature is maintained at about 1420 ° C. 0.6 kg of silicon was obtained by extracting the single crystal silicon stick by using one small single crystal as a factor to draw out a single crystal, and the recovery rate calculated based on 50 kg of cutting waste weight was 1.2%. Fermi energy levels were measured for the recovered silicon: the Fermi energy level was represented by C ^B = 10 ¹⁵ cm ^-3 , corresponding to p = 5.0 ohmcm, and the position of the Fermi energy level was It is about 0.31 electron volts higher than the center of the (energy band) interval, about 0.24 electron volts lower than the conduction band, and about 0.86 electron volts higher than the valence band. In the above measurement, the index indicates that the index belongs to polycrystalline silicon in proximity to monocrystalline silicon. Excess silicon carbide and acid solution in the reactor 52 is discharged to the second material discharge pipe (64 '), filtered, washed with a 5wt% NaOH solution, washed with water until the pH is 7.5 and dried, It is a light grayish, fine powdery product that can recover 7.5kg of silicon carbide. According to the analysis, the purity reaches 94%, Mohs hardness is 9.5, and the result of the electron microscopic examination shows that the crystal form is α-SiC hexagonal crystal system (the purity of the standard product of silicon carbide is 94 It becomes -99%, Mohs hardness is 9.2-9.6, and it is (alpha) -SiC hexagonal crystal system), and the recovery calculated based on 50 kg of cutting waste liquid weight is 15%.

Example  2

50 kg of petroleum-free single crystal silicon cutting waste liquid and 15 L of dilute hydrochloric acid having a concentration of 0.001 mol are injected into the first mixing tank 65 of the spray stirrer 49, and the cyclic spray stirring and reaction are repeatedly performed for about 20 minutes. Let's do it. By entering the primary mixed material obtained in the starting step into the spray mixer 50 and repeatedly carrying out the circulation spray mixing and reaction for about 20 minutes, the temperature rises to 50 ° C., and the mixed material enters the AC tube 11 The alternating current state appears, wherein the flow rate of the pump is 3 m 3 / h, the diameter of the AC tube is 1.5 mm, and the Reynolds number = 9845 when the power viscosity of the mixed material is 40.6 Pa · S. The secondary mixed material after mixing through the spray mixer enters the solid liquid separator 30 and is heated with two units of electric heating plates maintaining a temperature of 60 ° C., where water vapor and polyethylene glycol are evaporated and released together. After cooling, a mixture of water and polyethylene glycol can be obtained. At the solid outlet 37 at the bottom of the solid liquid separator 30, a solid mixture of silicon carbide and coarse crystals of silicon is released. The obtained water and polyethylene glycol mixture enters the spray dehydrator 51, and if the circulation spray dehydration is repeatedly performed for about 15 minutes, the temperature rises to 40 ° C, and the liquid flow flows in the alternating current in the alternating tube 11. When the flow rate of the circulation is 2.5㎥ / h, the diameter of the AC tube is 2.5mm, when the power viscosity of the mixture of water and polystyrene glycol is 14 Pa? S, the Reynolds number = 5139 do. After dehydration, 11.9 kg of colorless transparent polyethylene glycol can be obtained with a recovery of 23.8% based on the cutting waste weight. The solid mixture of coarse crystals of silicon carbide and silicon is sent to a first spray washer, which is then infused with water having a weight of 10% by weight of the solid mixture of coarse crystals. It appears as an alternating flow in the tube, the flow rate of the circulation is 2.1㎥ / h, the diameter of the alternating tube is 2.5mm, and when the power viscosity of the solid and water mixture is 10.2 Pa? S, Reynolds Number = 5925. When the cycle mixing wash time is about 10 minutes, the temperature rises to 80 ° C. After washing, the mixture is placed in a first separator and separated, and the first washed solid mixture is sent to a second spray washer, and the solid mixture is repeatedly subjected to a circulating spray mixing washing process in the same form, and the circulation flow rate is 3 M3 / h, the diameter of the alternating tube is 1.8 mm, and the Reynolds number = 11229 when the power viscosity of the mixture is 20.6 Pa · S. After washing, it can be placed in a second separator and separated, i.e. a second wash solid mixture of silicon carbide and silicon can be obtained. The obtained secondary carbide solid compound of silicon carbide and silicon is sent to the reactor 52, and then 1.2 times of the mixed acid solution of HNO ₃ and HF of the solid mixture is injected, and the process of cyclic spray stirring reaction is repeatedly performed for about 10 minutes. In progress, 0.8 kg of silicon can be recovered from the obtained silicon fluoride solution, and the recovery rate calculated based on the cutting waste liquid is 1.6%. The excess in the reactor is washed with 5wt% KOH solution through filtration, and washed with water until the pH reaches 7.2, to obtain 5.1 kg of fine powdery silicon carbide in pale gray green color, The recovery rate calculated based on the weight of the cutting waste liquid of 50 kg is 10.2%, and the remaining operation method of this embodiment is the same as that of the first embodiment.

Example  3

50 kg of petroleum-free single crystal silicon cutting waste and 25 L of dilute hydrochloric acid having a concentration of 0.0001 mol are injected into the first mixing tank 65 of the spray stirrer 49, and the cyclic spray stirring and reaction are repeatedly performed for about 30 minutes. Let's do it. By entering the primary mixed material obtained in the starting step into the spray mixer 50 and repeatedly carrying out the circulation spray mixing and reaction for about 10 minutes, the temperature rises to 40 ° C, and the mixed material enters the alternating current tube 11 When the alternating current is shown, the flow rate of the pump is 3 m 3 / h, the diameter of the AC tube is 2.5 mm, the Reynolds number = 3040 when the power viscosity of the mixed material is 28.4 Pa · S. The secondary mixed material after mixing through the spray mixer enters the solid liquid separator 30 and is heated with two units of electric heating plates maintaining a temperature of 80 ° C., where water vapor and polyethylene glycol are evaporated and released together. After cooling, a mixture of water and polyethylene glycol can be obtained. At the solid outlet 37 at the bottom of the solid liquid separator 30, a solid mixture of silicon carbide and coarse crystals of silicon is released. The obtained water and polyethylene glycol mixed liquid enters the spray dehydrator 51, and if the circulation spray dehydration is repeatedly performed for about 40 minutes, the temperature rises to 80 ° C., and the liquid flow is in the form of alternating current in the alternating tube 11 '. When the flow appears, the flow rate of the circulation is 2.5 m 3 / h, the diameter of the alternating tube is 1,8 mm, and the Reynolds number = when the power viscosity of the mixture of water and polystyrene glycol is 21.4 Pa? S 9007. After dehydration, 10.2 kg of colorless transparent polyethylene glycol can be obtained, and the recovery based on the cutting waste weight reaches 20.4%. A solid mixture of coarse crystals of silicon carbide and silicon is sent to the first spray washer, and again water is injected into the coarse crystal solids weight of about 15%, repeating the cyclic spray mixing wash, and the liquid flow is alternating It appears as an alternating flow in the tube, the flow rate of the circulation is 2.1㎥ / h, the diameter of the alternating tube is 3.0mm, and when the power viscosity of the solid mixture and the mixed material of water is 9.6 Pa? S, Reynolds Number = 3643. When the cycle mixing wash time is about 30 minutes, the temperature rises to 70 ° C. After washing, the mixture is placed in a first separator and separated, and then the first washing solid mixture is sent to a second spray washing machine, and the solid mixture is repeatedly subjected to the first circulation spray mixing washing process in the same form, and the corresponding circulation flow rate. Is 3 m 3 / h, the diameter of the AC tube is 2.4 mm, and the Reynolds number = 6970 when the power viscosity of the mixture is 14.0 Pa · S. After washing, it can be placed in a second separator and separated, i.e. a second wash solid mixture of silicon carbide and silicon can be obtained. The obtained second carbide solid mixture of silicon carbide and silicon is sent to the reactor 52, and then 1.5 times of the amount of the mixed acid solution of HNO ₃ and HF of the solid mixture is injected, and the process of cyclic spray stirring and reaction is repeated for 20 minutes. Advancing to the extent, 1 kg of silicon can be recovered from the obtained silicon fluoride acid solution, and the recovery rate calculated based on the cutting waste liquid is 2%. The excess in reactor 52) is washed with 10wt% NaOH solution through filtration and washed with water until pH reaches 7.3 to obtain 2.9kg of fine powdery silicon carbide with pale grey-green color. The recovery rate calculated based on the weight of the cutting waste liquid 50 kg is 5.8%, and the remaining operation method of this embodiment is the same as in Example 1.

Example  4

50 kg of petroleum-free single crystal silicon cutting waste liquid and 7.5 L of dilute hydrochloric acid having a concentration of 0.2 mol are injected into the first mixing tank 65 of the spray stirrer 49, and the cyclic spray stirring and reaction are repeatedly performed for about 15 minutes. Let's do it. By entering the primary mixed material obtained in the starting step into the spray mixer 50 and repeatedly carrying out the circulating spray mixing and reaction for about 20 minutes, the temperature rises to 30 ° C., and the mixed material enters the AC tube 11 The alternating current state appears, wherein the flow rate of the pump is 3 m 3 / h, the diameter of the AC tube is 2.0 mm, and the Reynolds number = 4736 when the power viscosity of the mixed material is 35.6 Pa · S. The secondary mixed material after mixing through the spray mixer enters the solid liquid separator 30 and is heated with two units of electric heating plates maintaining a temperature of 50 ° C., where water vapor and polyethylene glycol are evaporated and released together. After cooling, a mixture of water and polyethylene glycol can be obtained. At the solid outlet 37 at the bottom of the solid liquid separator 30, a solid mixture of silicon carbide and coarse crystals of silicon is released. The obtained water and polyethylene glycol mixture enters the spray dehydrator 51, and if the circulation spray dehydration is repeatedly performed for about 15 minutes, the temperature rises to 50 ° C, and the liquid flow is in the form of alternating current in the alternating tube 11 '. When the flow appears, the flow rate of the circulation is 2.5 m 3 / h, the diameter of the AC tube is 3.0 mm, and the Reynolds number = 3620 when the power viscosity of the mixed liquid of water and polystyrene glycol is 11.5 Pa? S. Becomes After dehydration, 13.7 kg of colorless transparent polyethylene glycol can be obtained, and the recovery based on the cutting waste weight reaches 27.4%. The solid mixture of coarse crystals of silicon carbide and silicon is sent to the first spray washer, which is then infused with water having a weight of about 20% by weight of the solid mixture of coarse crystals, followed by a cyclic spray mixing wash, the liquid flow being alternating It appears as an alternating flow in the tube, the flow rate of the circulation is 2.1㎥ / h, the diameter of the alternating tube is 2.7mm, and Reynolds when the power viscosity of the mixed material of solid mixture and water is 11.2 Pa? S Number = 4283. When the cycle mixing wash time is about 20 minutes, the temperature rises to 50 ° C. After washing, the mixture is placed in a first separator and separated, and the first washed solid mixture is sent to a second spray washer, and the solid mixture is repeatedly subjected to a circulating spray mixing washing process in the same form, and the circulation flow rate is 3 M3 / h, the diameter of the alternating current tube is 3.0 mm, and the Reynolds number = 4626 when the power viscosity of the mixture is 16.8 Pa · S. After washing, it can be placed in a second separator and separated, ie a second wash solid mixture of silicon carbide and silicon. The obtained second carbide solid mixture of silicon carbide and silicon was sent to the reactor 52, and then a mixed acid solution of HNO ₃ and HF was added in an amount of 1.1 times that of the solid mixture, and the process of circulating spray stirring was repeated for about 30 minutes. In progress, 0.5 kg of silicon can be recovered from the obtained silicon fluoride solution, and the recovery rate calculated based on the cutting waste liquid is 1%. The excess in the reactor is washed with 7wt% KOH solution through filtration and washed with water until the pH reaches 7 to obtain 6.3kg of fine powdery silicon carbide with a light gray green color. The recovery calculated on the basis of 50 kg of the cutting waste liquid is 12.6%, and the remaining operating method of the present embodiment is the same as that of the first embodiment.

Diaphragm Pump (1) Heat Resistance Temperature Measuring Head (2) Mixing Tank (3)
Material discharge pipe (4) Spraying device (5) Material supply tank (6)
T-pipe valve (7) Connecting pipe (8) Material addition pipe (9)
Nozzle Inlet (10) AC Tube (11) Mixing Chamber (12)
Nozzle outlet (13) Liquid oil tool (14)
Guide Plate (15) Small Hole (16)
Temperature indicator (17) Material outlet (18) Spray passage (19)
Drain pipe (21) Steam liquid pipe (22)
Solid Liquid Separator (30) Spray Head (31) Retention Lock (32)
Gas outlet pipe (33) Fixing screw (34) Tray (35)
Outer wall (36) Solid outlet (37) Liquid outlet (38)
Baffle Plate (39) Holes (40)
Funnel Plate (41) Conical Plate (42) Spray Agitator (49)
Spray Mixer (50) Spray Dehydrator (51) Reactor (52)
First Diaphragm Pump 61 First T-Screw Valve 62
First Material Supply Tank (63) First Material Discharge Tube (64) First Mixing Tank (65)
First spray passage (66) Material outlet (67)
First connecting pipe 68 First material adding pipe 69 Nozzle 70
Liquid hole (71) Nozzle chamber (72) First nozzle outlet (73)
Diaphragm pump (1 ') Mixing tank (3') Material discharge pipe (4 ')
Sprayer (5 ') Material supply tank (6') T-pipe valve (7 ')
Connecting pipe (8 ') Material addition pipe (9') Nozzle inlet (10 ')
AC tube 11 'Mixing chamber 12' Nozzle outlet 13 '
Liquid flow tool (14 ') Guide plate (15') Small hole (16 ')
Temperature indicator (17 ') Material outlet (18') Spray passage (19 ')
Second Diaphragm Pump 61 'Second T-Screw Valve 62'
Second material supply tank 63 'Second material discharge pipe 64' Second mixing tank 65 '
Second spray passage (66 ') material outlet (67')
Second Connection Pipe 68 'Second Material Additive Tube 69' Nozzle 70 '
Liquid flow hole 71 'Second nozzle chamber 72' Second nozzle outlet 73 '

Claims (5)

(1) The petroleum-free single crystal silicon cutting waste solution is placed in a spray stirrer and hydrochloric acid is injected for treatment. At this time, the concentration of hydrochloric acid is 0.0001-0.4 mol, and 100-500 ml of hydrochloric acid solution is injected per 1 kg of waste liquid. Stirring for 10-30 minutes through to obtain a mixture of the first stage and discharged to the spray mixer, and mixing again for 10-30 minutes at a temperature rise of 30 ℃-50 ℃ with a circulating spray to obtain a secondary mixture to discharge it;
(2) The secondary mixture discharged from the spray mixer was placed in a solid liquid separator and heated by an electric heating plate having a heating temperature of 50 ° C.-80 ° C. to evaporate water vapor and polyethylene glycol together, and cooled by the first cooler. After obtaining a mixed solution of water and polyethylene glycol, it is put back into the spray dehydrator, and after 15-40 minutes of circulation spray dehydration at 40 ° C.-80 ° C., polyether glycol can be recovered immediately after the water is discharged from the spray dehydrator. Releasing a solid mixture of silicon carbide and coarse crystals of silicon at the bottom of the liquid separator;
(3) The solid mixture of the silicon carbide and the coarse crystals of silicon was placed in the first spray washer and 10-20% of the water weight of the solid mixture of the coarse crystal was added. After rising to 40 ° C.-80 ° C., the washed mixture is placed in a first separator to separate out remaining residues of the outer shell, to obtain a first washed solid mixture of silicon carbide and silicon, and the solid mixture is placed in a second spray washer. After repeated cyclic spray washing, the mixture is placed in a second separator to separate and remove the remaining residues of the outer shell, thereby obtaining a second washed solid mixture of silicon carbide and silicon;
(4) A secondary washing solid mixture of silicon carbide and silicon is placed in a reactor, and a mixed acid solution composed of 5% HNO ₃ and 30% HF is injected, and the volume ratio of both is HNO ₃ : HF = 1: 5, 1-1.5 kg mixed acid solution is added to 1 kg of silicon carbide and silicon solid mixture, and the stirring reaction is performed for 10-30 minutes. The temperature of the silicon fluoride solution is evaporated by rising to reflux temperature. Cooled to give a colorless transparent silicone fluoride solution, reprocessed to recover the silicon, the excess silicon carbide and acid solution in the reactor is filtered and washed with an alkaline solution until the pH reaches 7-7.5 and dried Recovering the single carbide silicon cutting waste liquid treatment method comprising the step of recovering silicon carbide. The method of claim 1, wherein the spray stirrer includes a first mixing tank, a first material supply tank, a first spray passage, a first diaphragm pump, a first T-pipe valve, and a first material discharge pipe. A first material tube in the lower part of the tank is mounted to the cover on the first mixing tank and extends into the first mixing tank, and the first spray passage passes through the nozzles, the nozzle chambers and the first nozzle outlets which in turn communicate with each other. And a liquid flow hole is provided at both sides of the nozzle chamber wall, respectively, and the diameter of the nozzle is 3-4 mm, and the first diaphragm pump includes the first T-pipe valve and the first mixing tank bottom. Located on a first connection pipe that is the same as the first material outlet, the first material discharge pipe is interconnected with the first T-pipe valve,
The spray mixer is connected to the spray stirrer through the first material discharge pipe of the spray stirrer, the third mixing tank, the third material supply tank, the third spray device, the third diaphragm pump, the first heat resistance temperature measuring head, And a third T-tube valve and a third material discharge pipe, wherein the third material adding pipe below the third material supply tank is mounted on the cover of the third mixing tank and extends into the third mixing tank, The spraying device includes a third spray passage and a first guide plate, and the third spray passage includes a third nozzle inlet, a first alternating tube, a first mixing chamber, and a third nozzle outlet, which in turn communicate with each other. The third nozzle inlet has a funnel shape, the diameter of the first AC tube is 1.2-3 mm, and a first liquid flow first inlet is provided at both sides of the wall of the first mixing chamber, respectively. Guide plate is vertically Is installed on the third spray passage and located between the liquid flow first inlet port and the third nozzle outlet, small holes are distributed on the first guide plate, the third diaphragm pump is the third T-tube Located on a third connecting pipe between the valve and the third material outlet of the bottom of the third mixing tank, the third material discharge pipe is interconnected with the third T-tube valve, the first heat resistance temperature measurement The head is fixedly installed in the third mixing tank, and the upper cover of the third mixing tank penetrating through the lead wire is interconnected with the first temperature indicator,
The solid liquid separator includes a sprinkler head, a gas outlet pipe, a conical plate, a funnel plate and a solid outlet, and the third material discharge pipe of the spray mixer is installed at the center of the top cover of the solid liquid separator. Two units of electric heating plates interconnected with the head and fixed up and down symmetrically on the outer wall are installed in the solid liquid separator, and the structure of the electric heating plates of each unit is one conical plate in the upper direction. The lower direction is made of a funnel plate and a hole, the diameter of the funnel plate is larger than the diameter of the conical plate, the conical plate is arranged at 120 ° formed of three fixed nails Fixed to the top, the three positioning nails It is fixed on the outer wall, the funnel plate is fixed on the tray, the tray is fixed on the outer wall with a fixing screw, a gas outlet pipe is installed on the top cover, the bottom is a solid outlet A baffle plate is installed around four of the solid outlets, and a liquid outlet is provided at the bottom thereof.
The spray dehydrator is the same as the structure of the spray mixer except that one drain pipe is installed on the top cover, the solid liquid separator is interconnected with the spray dehydrator through a first cooler, the spray dehydrator A fourth mixing tank, a fourth material supply tank, a fourth spraying device, a fourth diaphragm pump, a second heat resistance temperature measuring head, a fourth T-tube valve, a fourth material discharge pipe and a drain pipe, and the fourth material supply The fourth material adding pipe at the bottom of the tank is mounted on the fourth mixing tank top cover and extends into the fourth mixing tank, and one drain pipe is installed on the fourth mixing tank top cover, and the fourth spray The apparatus includes a fourth spray passage and a second guide plate, wherein the fourth spray passage in turn communicates with the fourth nozzle inlet, the second alternating tube, the second mixing chamber, and the fourth. A fourth outlet port is included, and the fourth nozzle inlet has a funnel shape, and the diameter of the second AC tube is 1.2-3 mm, and both sides of the liquid flow second guide port are respectively provided on both sides of the wall of the second mixing chamber. Is installed, the second guide plate is installed on the fourth spray passage facing vertically and is located between the liquid flow second guide port and the fourth nozzle outlet, small holes are distributed in the second guide plate The fourth diaphragm pump is located on a fourth connecting pipe between the fourth T-pipe valve and the bottom fourth material outlet of the fourth mixing tank, and the fourth material discharge pipe and the fourth T-pipe valve are An upper cover which is interconnected and the second heat resistance temperature measuring head is fixedly installed in the fourth mixing tank and penetrates the fourth mixing tank through a lead wire. The indicator is interconnected with a second temperature,
The first spray washer is interconnected with the solid outlet of the solid liquid separator, the structure of the first spray washer is the same as the structure of the second spray mixer, and the first spray washer is in turn the first separator, A second spray washer and a second separator are interconnected, the structure of the second spray washer is the same as the structure of the first spray washer, the second spray was again interconnected with the reactor,
The reactor structure is the same as the structure of the spray stirrer except that one vapor liquid tube is installed on the top cover, the vapor liquid tube is connected to the second cooler, the reactor is a second mixing tank, And a second material supply tank, a second spray passage, a second diaphragm pump, a second T-pipe valve, a second material discharge pipe, and a vapor liquid pipe. 2 is installed on the mixing tank top cover and extends into the second mixing tank, the one vapor liquid pipe is installed on the second mixing tank top cover, and the second spray passages are in turn communicating with each other. 2 nozzles, a second nozzle chamber, and a second nozzle outlet, each of which has one liquid flow hole provided on both sides of the wall of the nozzle chamber, and the diameter of the second nozzle is 3-4 mm. The second diaphragm pump is installed on a second connection pipe between the second T-pipe valve and the second material outlet of the bottom of the second mixing tank, and the second material discharge pipe is connected to the second T-pipe valve. Apparatus of a single crystal silicon cutting wastewater treatment recovery method characterized in that the interconnection. The method of claim 1, wherein the alkaline solution wash in step (4) is selected and washed 5-10wt% alkaline solution prepared by combining NaOH, KOH or Na ₃ CO ₃ Recovery of single crystal silicon cutting waste liquid treatment Way. The monocrystalline silicon according to claim 2, wherein the pore diameter of the pores distributed on the first guide plate of the spray mixer is 1-3 mm, and the porosity of the first guide plate is 60-80%. Cutting waste treatment recovery method. The monocrystalline silicon according to claim 2, wherein the pore diameter of the pores distributed on the second guide plate of the spray mixer is 1-3mm, and the porosity of the second guide plate is 60-80%. Cutting waste treatment recovery method.

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