CN112850965B - High-concentration fluorine-containing wastewater recycling treatment process and device produced in silicon solar cell production - Google Patents
High-concentration fluorine-containing wastewater recycling treatment process and device produced in silicon solar cell production Download PDFInfo
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Abstract
The invention relates to a process and a device for recycling high-concentration fluorine-containing wastewater generated in the production of a silicon solar cell. The device of the process adopts a rotational flow medicine mixing device, a self-cleaning filter, a self-cleaning sand filter and the like; meanwhile, in the treatment process of the process, various medicaments are screened and compounded to obtain the granular medicament, the granular medicament is fully contacted with fluorine ions in the fluorine-containing wastewater under the centrifugal action and reacts to generate fluoride, the reacted fluoride is carried away by water, and the unreacted granular medicament is left to continue to react with the fluorine-containing wastewater. The invention can recycle reverse osmosis concentrated water, reduce the dosage and the slag yield of the medicament, has low hardness of the treated water quality, and can be directly reused as the production water of the silicon solar cell.
Description
Technical Field
The invention belongs to the technical field of industrial wastewater treatment, and particularly relates to a process and a device for recycling high-concentration fluorine-containing wastewater generated in silicon solar cell production.
Background
The photovoltaic is a power generation system which directly converts solar radiation energy into electric energy by utilizing a photovoltaic effect, and belongs to renewable green energy. Aiming at the increasingly prominent environmental and global climate warming problems, the main countries in the world are prompted to make legislation or take measures, the use of the conventional stone energy coal, petroleum and natural gas is reduced, the novel renewable energy capable of reducing the emission of carbon dioxide and other greenhouse gases is promoted to be adopted, and the photovoltaic industry is rapidly increased. A series of industrial policies are formulated in future energy development planning in China, and renewable energy sources are subsidized to gradually replace conventional energy sources. Solar power generation will account for more than 60% at the end of the century, and the photovoltaic industry has great development prospects in the energy field.
Photovoltaic power generation is performed by means of output power of a solar cell photoelectric conversion system composed of solar cell chips with semiconductor characteristics. The solar cell is divided into various types such as crystalline silicon, thin film, perovskite, organic and the like, and the crystalline silicon type accounts for most of market shares, is a current mainstream product and is also called as a silicon solar cell. In the production of the silicon solar cell, a large amount of hydrofluoric acid is used in the process stages of cleaning, texturing, etching and the like, further fluorine-containing wastewater with extremely high concentration is generated, the highest concentration of fluorine ions in water reaches 40000mg/L, the average concentration of fluorine ions is 2000-3000 mg/L, and the limit value of a discharge standard is far exceeded. With the increasing importance of our country on environmental protection, the management and control of production water and discharge are more and more strict. The national standard GB 30484 plus 2013 discharge Standard of pollutants for the Battery industry stipulates that the fluorine ion limit of water pollutants of the solar battery in the existing enterprises is 10mg/L, the newly-built enterprises are executed according to the special discharge limit of 2mg/L, the discharge requirement is difficult to reach by the existing wastewater treatment technology, and the large-scale development of the photovoltaic industry is severely restricted.
The prior art for treating fluorine-containing wastewater generated in the production of silicon solar cells mainly comprises a double calcium method, an adsorption method and an ion exchange method. The principle of the double-calcium method is that solid calcium oxide (CaO) is firstly added with water to become mature lime (Ca (OH)2) The lime milk is added into the fluorine-containing wastewater according to a certain proportion, calcium ions react with fluoride ions to generate calcium fluoride, a flocculating agent and a coagulant aid are subsequently added to precipitate calcium fluoride so as to achieve the purpose of removing fluoride in water, and the reaction formula is as follows:
CaO+H2O＝Ca(OH)2＝Ca2++2OH-，Ca2++2F-＝CaF2
in order to discharge fluoride reaching the standard, a sufficient amount of calcium ions exist in fluoride-containing water, and when the concentration of calcium hydroxide is lower than 15mg/L, the solubility of the calcium hydroxide cannot provide sufficient calcium ions, and soluble calcium salt calcium chloride needs to be added. The calcium fluoride needs a certain time for sedimentation, and flocculating agents of polyaluminium chloride (PAC) and Polyacrylamide (PAM) are added. To achieve the discharge of 5mg/L of fluoride ion, the redundancy of calcium ion concentration is at least 50mg/L, the ratio of the two is about 10 times, and the discharge standard of 2mg/L is difficult to achieve. The dual-calcium method has the defects of large dosage and large slag output, excessive calcium salt and flocculating agent are added to ensure that the hardness and the organic matter content in water are too high, and the treated water can only be discharged and cannot be recycled; the adsorption method has limited adsorption capacity and is only suitable for removing fluorine from light fluorine-containing water with fluorine content of less than 20mg/L and underground water; the regeneration of the ion exchange method exchanger generates secondary pollution, and is not suitable for the treatment of high fluorine-containing industrial wastewater.
No. CN102126798B entitled "a method for recycling wastewater containing fluorine and ammonia nitrogen in electronic industry", which is a defluorination process for light fluorine-containing water with fluorine ion content less than 100mg/L by adopting a mode of combining chemical reaction precipitation and coagulating precipitation separation, and calcium oxide, calcium hydroxide or soluble calcium salt is added into the wastewater to form calcium fluoride precipitate, namely a dual-calcium method defluorination process, which is not suitable for treating high-fluorine-containing wastewater, and the treated wastewater has too high hardness and cannot be recycled;
application No. 201710830427.8, namely a system and a method for treating fluorine-containing wastewater in photovoltaic industry, mainly relates to a method for removing fluorine from fluorine-containing water with high nitrate content and fluorine ion concentration of 100-300 mg/L, wherein the method comprises the processes of removing fluorine by a double calcium precipitation method, chemically softening sodium carbonate, reducing hardness by ion exchange resin, performing reverse osmosis interception and the like. The concentration of calcium and magnesium ions is increased by the double-calcium method, secondary pollution is generated by the regeneration of an exchanger by the ion exchange method, the treatment effect is unstable, and the stable operation of a reverse osmosis treatment device cannot be ensured;
no. CN103373774B Special high-power recovery system for fluorine-containing wastewater in photovoltaic industry by membrane method, adjusting pH value of the fluorine-containing wastewater by acid-base neutralization, filtering properly, and removing fluorine by a two-stage reverse osmosis device directly. After acid and alkali treatment, fluoride ions exist in water in the form of hydrogen fluoride, and because the molecular radius of the hydrogen fluoride is close to that of water molecules, reverse osmosis is difficult to intercept the fluoride ions, and an ideal defluorination effect is difficult to achieve.
Application No. 201811615422.4 fluorine-containing wastewater treatment system and method provides a fluorine-containing wastewater treatment system and method, which is characterized in that aluminum salt is added into fluorine-containing water as a conversion agent, and then calcium hydroxide, calcium chloride and other double-calcium fluorine removal agents are added to form calcium fluoroaluminate precipitates, so that the fluorine removal function is realized, the conversion agent is added first, and then the double-calcium fluorine removal agent is added, so that the fluorine removal efficiency is reduced. The defluorination concentration of the method is lower than 100mg/L, and the method is not suitable for treating wastewater with high fluorine content.
The defluorination method provided by application number 202010149123.7 fluorine-containing wastewater treatment device and process of liquid crystal panel production plant comprises the steps of adjusting the pH value of fluorine-containing wastewater, softening resin and performing reverse osmosis defluorination, and also has the problems that secondary pollution is generated by reverse osmosis defluorination and exchange resin regeneration without adding a defluorination agent, the treatment effect is unstable, the fluorine concentration of the fluorine-containing wastewater is less than 200mg/L, and the defluorination method is not suitable for treating high-concentration fluorine-containing wastewater.
Disclosure of Invention
The invention aims to solve the defects of large dosing amount, large slag output, poor treatment effect on high-fluorine water and high hardness of treated water and incapability of recycling in the prior art, and provides a process and a device for recycling high-concentration fluorine-containing wastewater generated in the production of silicon solar cells. The device of the process adopts a rotational flow medicine mixing device, a self-cleaning filter, a self-cleaning sand filter and the like; meanwhile, in the treatment process of the process, various medicaments are screened and compounded to obtain the granular medicament, the granular medicament is fully contacted with fluorine ions in the fluorine-containing wastewater under the centrifugal action and reacts to generate fluoride, the reacted fluoride is carried away by water, and the unreacted granular medicament is left to continue to react with the fluorine-containing wastewater. The invention can recycle reverse osmosis concentrated water, reduce the dosage and the slag yield of the medicament, has low hardness of the treated water quality, and can be directly reused as the production water of the silicon solar cell.
In order to achieve the above object, the present invention adopts the following technical solutions:
a high-concentration fluorine-containing wastewater recycling treatment process generated in silicon solar cell production comprises the following steps:
(1) pumping the fluorine-containing wastewater stored in the homogeneous fluorine-containing water tank and the reverse osmosis concentrated water stored in the reverse osmosis concentrated water tank into a pipeline mixer through a fluorine water pump and a concentrated water pump respectively for mixing, and feeding the obtained mixed water into a rotational flow medicine mixing device;
wherein the fluorine ion content of the fluorine-containing wastewater is 1000-2000 mg/L; the hardness of the reverse osmosis concentrated water is 1000-2000 mg/L; the flow ratio of the fluorine-containing wastewater to the reverse osmosis concentrated water is 1: 5-5: 1, the water inflow of mixed water of the rotational flow medicine mixing device is 5-50 t/h, the diameter of a cylinder of the rotational flow medicine mixing device is 500-1500 mm, and the height of the cylinder is 1500-2500 mm;
(2) the mixed water of the fluorine water and the concentrated water is mixed with the granular medicament in a rotational flow mode along the inner wall of the rotational flow medicament mixing device through a water inlet of the rotational flow medicament mixing device, the water mixed with the medicament is concentrated at the central part of the rotational flow medicament mixing device and flows out along a water outlet pipe through a water inlet end of a water outlet pipe of the rotational flow medicament mixing device; the granular medicament returns to the bottom of the rotational flow medicament mixing device along the inner wall of the rotational flow medicament mixing device under the action of centrifugal force and gravity;
wherein, the granular medicament in the solid medicament groove enters the rotational flow medicament mixing device through the spiral feeder through the medicament feeding port of the rotational flow medicament mixing device; the initial adding amount of the solid medicament is 10-30% of the volume of the rotational flow medicament mixing device, and the medicament adding amount during operation is supplemented in an equivalent manner according to the reaction consumption amount;
the granular medicament comprises 0.5-5% of sepiolite, 0.5-5% of diatomite, 35-75% of calcium bicarbonate and 20-45% of tricalcium phosphate; the particle size of the granular medicament is 50-100 meshes.
(3) Allowing the reaction liquid flowing out of the water outlet of the rotational flow medicine mixing device to pass through a medicine filter tank, and allowing the reaction liquid to enter a sedimentation tank for standing for 20-40 minutes; meanwhile, the fluorine ion chelating agent solution in the liquid medicine tank is pumped from the sedimentation tank through a circulating medicine adding pump and is injected into the sedimentation tank through a jet medicine adding device, so that the pH value of the solution in the sedimentation tank is 5-8;
the fluorine ion chelating agent is one or a plurality of compounds of 60-100% of calcium hydroxy phosphate, 10-100% of chitosan and 20-100% of calcium bicarbonate, and the concentration of the fluorine ion chelating agent is 30-80 mg/L;
(4) discharging sediment in a sedimentation tank into a mud tank, pumping mud in the mud tank into a water collecting tank of a self-cleaning filter through a mud pump, rotating a ceramic filter disc of the self-cleaning filter, absorbing the mud in the water collecting tank to the surface of the filter disc by negative pressure inside the ceramic filter disc, discharging dry filter residue from the filter residue collecting tank into a mud tank through a residue scraping plate, returning filter water from the negative pressure filtering of the filter to the water inlet end of the sedimentation tank, wherein the filtering aperture of the ceramic filter disc is 0.5-10 mu m;
meanwhile, the upper clear water of the sedimentation tank is pumped into the bottom of the filter sand through a self-cleaning sand filter by a water pump through a middle pipeline, the water after sand filtration enters a fluorine removal water production tank through a top clear water outlet, the bottom dirty sand is lifted to a sand washer on the upper part of the sand filter by compressed air through a middle sand lifting pipe, the cleaned filter sand returns to the upper layer of the filter sand in the sand filter, the sand washing sewage is discharged into a mud slurry tank through a sand washing water outlet, and the diameter of the filter sand is 0.5-2.0 mm;
(5) after water in the defluorination water production pool is defluorinated and purified, the water is pumped into an ionic membrane desalination device through a water pump to be subjected to hardness removal softening treatment, and two streams of water are produced, one is produced water, and the other is concentrated water; the product water of demineralizer gets into the reuse water pond, and the concentrated water of demineralizer gets into homogeneity fluorine-containing water pond and continues to mix reaction with high enriched fluorine-containing water, reduces the use of defluorinating medicament, and the demineralizer desalination rate is 50 ~ 80%, product water quality: the fluorine ion concentration is 1-5 mg/L, the hardness is 100-500 mg/L, and the recycling requirement of reverse osmosis process water is met.
A high-concentration fluorine-containing wastewater recycling treatment device for silicon solar cell production comprises a homogeneous fluorine-containing water tank, a reverse osmosis concentrated water tank, a sedimentation tank, a slurry tank, a fluorine-removing water-producing tank, a reuse water tank, a solid medicine tank, a medicine filtering tank, a liquid medicine tank, a sludge tank, a pipeline mixer, a screw feeder, a rotational flow medicine mixing device, a self-cleaning filter, a jet medicine adding device, a self-cleaning sand filter, an ionic membrane desalting device, a fluorine water pump, a concentrated water pump, a circulating medicine adding pump, a mud pump, an intermediate water pump 1, an intermediate water pump 2, a proportion regulator and a pH controller;
the connection relationship is as follows: the homogeneous fluorine-containing water tank and the reverse osmosis concentrated water tank are respectively connected to a rotational flow pesticide mixing device through a fluorine water pump and a concentrated water pump through a pipeline mixer, the rotational flow pesticide mixing device is also connected with one end of a pesticide filter tank, and the pesticide filter tank is communicated with a sedimentation tank after being converged with a pipeline of the self-cleaning filter; the sedimentation tank is also connected with a self-cleaning sand filter through an intermediate water pump 1, the self-cleaning sand filter is connected with a fluorine removal water production tank, and the fluorine removal water production tank is also connected with an ionic membrane desalination device through an intermediate water pump 2; the ionic membrane desalination device is also respectively connected with the reuse water pool and the homogeneous fluorine-containing water pool; the self-cleaning sand filter is also connected with a mud tank, and the mud tank is connected with the self-cleaning filter through a mud pump; the self-cleaning filter is also respectively connected with the sedimentation tank and the sludge tank; the liquid medicine tank is connected with the sedimentation tank through the jet flow medicine feeder, a sensor probe of the pH controller is arranged in the sedimentation tank, and the transmission output of the pH controller is connected with the circulating medicine feeding pump.
The proportion regulator is connected with the concentrated water pump and the fluorine water pump through signal lines, and the concentrated water pump is a variable frequency water pump; the control of the amount of the liquid medicament added is realized by the pH controller inserted into the sedimentation tank.
The invention has the beneficial effects that:
compared with the prior art, the method has the following characteristics:
1, high-hardness concentrated water generated in the process of preparing pure water by reverse osmosis for solar cell production is completely utilized and reacts with high-fluorine-containing wastewater to generate fluoride, so that the utilization rate of the production water is improved, the discharge is reduced, and the use amount and the slag discharge amount of a fluorine removal agent are reduced.
2, the defluorinating agent is difficult to dissolve particles, and the stirring and solid-liquid separation are completed at one time by mixing the defluorinating agent through rotational flow, so that the power consumption of stirring equipment is reduced, and the dosage of the agent can be effectively reduced.
3 the process of self-cleaning sand filtration and sand washing is continuously finished, and the sand washing water is recycled after deslagging and filtering by the self-cleaning filter.
4, the produced water after defluorination is desalted by an ion membrane without adding chemical agents and ion exchange resin regenerants, and secondary pollution is avoided.
5 the invention has excellent effect of removing fluorinion. The existing double-calcium method aims to achieve F-It is very difficult to be less than or equal to 10mg/L, and the national standard F-The concentration limit value of 2mg/L is a very high standard, which greatly limits the operation of the existing enterprises, while the invention F-Less than or equal to 1mg/L, thus fundamentally solving the problem of environmental protection.
Drawings
FIG. 1 is a schematic structural diagram of a high-concentration fluorine-containing wastewater recycling treatment device for silicon solar cell production;
FIG. 2 is a schematic structural view of a rotational flow mixing device;
FIG. 3 is a schematic view of a self-cleaning filter;
FIG. 4 is a schematic view of the jet applicator structure;
FIG. 5 is a schematic view of a self-cleaning sand filter construction;
wherein the content of the first and second substances,
11 homogenizing a fluorine-containing water tank;
12 a reverse osmosis concentrated water tank;
13, a sedimentation tank; 131 at the water inlet end of the sedimentation tank; 132 sediment outlet; 133 clear liquid outlet; 134 a pH controller socket;
14 a mud pit;
15 defluorination water generating pool;
16, a reuse water pool;
21 solid medicine groove;
22 medicine filter tank;
23 liquid medicine tank;
24, a sludge groove;
31 a pipeline mixer;
a 32-screw feeder;
33 a rotational flow medicine mixing device; 331 a water inlet; 332, a water outlet; 333 medicine adding port; 334 a cylinder body; 335 a water outlet pipe; 336 outlet pipe water inlet end
34 self-cleaning filter; 341 water collecting tank; 342 ceramic filter discs; 343 self-cleaning filter outlet end; 344 scraper bar;
35 jet dosers; 351, a water inlet of a jet medicine adding device; a 352 jet doser water outlet; 353, negative pressure medicine adding port;
36 self-cleaning sand filter; 361 cleaning the water inlet of the sand filter; 362 clear water outlet; 363 a sand washing water outlet; 364 compressed air inlet; 365 sand washer; 366 filtering sand; 367 a sand extraction pipe;
37 ion membrane desalination device; 371 ion membrane desalination device water inlet end; 372 the water production end of the ionic membrane desalination device; 373 at the concentrated water end of the ion membrane desalination device;
41 a fluorine water pump;
42 a concentrate pump;
43 circulation dosing pump;
44 a mud pump;
45, an intermediate water pump 1;
46 an intermediate water pump 2;
51 a proportional regulator;
a pH controller 52;
Detailed Description
The existing double-calcium method defluorination technology adopts: adding calcium oxide, calcium chloride → adding flocculant PAC → adding coagulant aid PAM → sedimentation tank sedimentation → filter pressing deslagging → treated water discharging and the like, and has the defects of large dosage, large slag output and incapability of recycling the treated wastewater (the treated wastewater cannot be used as reverse osmosis inlet water due to high hardness);
the process route of the invention is as follows: mixing the fluorine water and the concentrated water → mixing the solid medicament by rotational flow → adding the medicament in proportion to the liquid medicament → self-cleaning sand filtration → slag discharge of the precipitate → desalting by an ionic membrane → water quality meeting the requirement of reuse water, and has the advantages of small dosage, small slag discharge and capability of being reused as reverse osmosis inlet water.
The insoluble granular medicament in the fluorine-containing wastewater recycling treatment process is one of innovations of the invention, and the effect achieved by matching the combined device and the granular medicament in the process is completely different from that of the existing fluorine removal technology; through the binding effect of the sepiolite and the diatomite, the sepiolite and the diatomite are mixed and roasted with other chemicals to form slow-release particles, and calcium and magnesium elements in the components can react with fluoride ions to form fluoride.
The granular medicament comprises 0.5-5% of sepiolite, 0.5-5% of diatomite, 35-75% of calcium bicarbonate and 20-45% of tricalcium phosphate, and is prepared into the granular medicament with the particle size of 50-100 meshes through the processes of grinding, mixing, forming, roasting at the low temperature of 200-300 ℃ and the like.
The device for recycling and treating the high-concentration fluorine-containing wastewater generated in the production of the silicon solar cell has the following characteristics:
(1) the rotational flow medicine mixing device (33) in the fluorine-containing wastewater recycling treatment device uniformly mixes the fluorine-containing wastewater with the granular medicine which is not easy to dissolve through the centrifugal effect, fluorine ions are changed into fluoride after the reaction and are taken away by water, and the undissolved medicine is remained in the device to continuously act with the subsequent fluorine-containing water, so that the dosage can be saved compared with the medicine adding mode of the existing fluorine removing technology;
(2) the self-cleaning filter (34) part in the fluorine-containing wastewater recycling treatment device is filtered by plate-type ceramic plates under negative pressure, and has better filtering and deslagging effects compared with a plate-and-frame filter pressing mode of the existing fluorine removal technology;
(3) in the self-cleaning sand filter (36) part of the fluorine-containing wastewater reuse treatment device, the filter medium is continuously cleaned, so that the process flow is uninterrupted, and compared with the filtering mode of the existing fluorine removal technology, the water quality after being filtered and treated by hardness reduction can meet the requirement of reuse water;
example 1
The invention relates to a high-concentration fluorine-containing wastewater recycling treatment device produced in silicon solar cell production, which comprises a homogeneous fluorine-containing water tank (11), a reverse osmosis concentrated water tank (12), a sedimentation tank (13), a mud slurry tank (14), a fluorine removal water production tank (15), a reuse water tank (16), a solid medicine tank (21), a medicine filter tank (22), a liquid medicine tank (23), a mud residue tank (24), a pipeline mixer (31), a spiral feeder (32), a rotational flow medicine mixing device (33), a self-cleaning filter (34), a jet flow medicine feeder (35), a self-cleaning sand filter (36), an ionic membrane desalting device (37), a fluorine water pump (41), a concentrated water pump (42), a circulating medicine feeding pump (43), a mud pump (44), an intermediate water pump 1(45), an intermediate water pump 2(46), a proportion regulator (51) and a pH controller (52), wherein the homogeneous fluorine-containing water tank (12), the sedimentation tank (13), the mud slurry tank (14), the fluorine removal water production tank (15), the self-cleaning filter (34), the jet flow medicine feeding device (35) and the intermediate water pump (44);
the connection relationship is as follows: the homogeneous fluorine-containing water tank (11) and the reverse osmosis concentrated water tank (12) are respectively connected to a rotational flow pesticide mixing device (33) through a fluorine water pump (41) and a concentrated water pump (42) through a pipeline mixer (31), the rotational flow pesticide mixing device (33) is also connected with one end of a pesticide filtering tank (22), and the pesticide filtering tank (22) is communicated with the sedimentation tank (13) after being converged with a pipeline of a self-cleaning filter (34); the sedimentation tank (13) is also connected with a self-cleaning sand filter (36) through an intermediate water pump 1(45), the self-cleaning sand filter (36) is connected with a fluorine removal water production tank (15), and the fluorine removal water production tank (15) is also connected with an ionic membrane desalination device (37) through an intermediate water pump 2 (46); the ionic membrane desalination device (37) is also respectively connected with the reuse water pool (16) and the homogeneous fluorine-containing water pool (11); the self-cleaning sand filter (36) is also connected with a mud pool (14), and the mud pool (14) is connected with the self-cleaning filter (34) through a mud pump (44); the self-cleaning filter (34) is also respectively connected with the sedimentation tank (13) and the sludge tank (24); the liquid medicine tank (23) is connected with the sedimentation tank (13) through the jet flow medicine adding device (35), a sensor probe of the pH controller (52) is arranged in the sedimentation tank (13), and the transmitting output of the pH controller (52) is connected with the circulating medicine adding pump (43).
The proportion regulator (51) is connected with the concentrated water pump (42) and the proportion regulator (51) is connected with the fluorine water pump (41) through signal lines, and the concentrated water pump (42) is a variable frequency water pump; the control of the amount of the liquid medicament is realized by a pH controller (52) inserted into the sedimentation tank (13).
The rotational flow medicine mixing device (33) comprises a water inlet (331), a water outlet (332), a medicine adding port (333), a cylinder body (334), a water outlet pipe (335) and a water inlet end (336) of the water outlet pipe; the water inlet (331) is located at the middle-lower part of the barrel (334), the water outlet (332) is located at the bottom of the barrel (334), the medicine adding port (333) is located at the top of the barrel, the water outlet pipe (335) is arranged at the longitudinal circle center part of the barrel (334), the water inlet end (336) of the water outlet pipe at the top is funnel-shaped, and the conical surface of the water inlet end can guide the solid medicine into the swirling water body and does not discharge along with water flow; the water pipe of the water inlet (331) adopts stainless steel with the caliber of DN32 and the material of SUS 304, is provided with a flange interface and is welded at the middle lower part of the body; the water pipe of the water outlet (332) is made of SUS 304 stainless steel with the caliber of DN50 and is provided with a flange interface and welded at the bottom of the body; the dosing port (333) is square, the outer side of the dosing port is inclined towards the body and is welded on the upper part of the circular rotational flow dosing device, and the cylinder body (334) is made of SUS 304 stainless steel or Q235 structural steel, the diameter of the cylinder body is 1000mm, and the height of the cylinder body is 1700 mm; the water outlet pipe (335) is made of SUS 304 stainless steel with the caliber of DN50, penetrates through the cylinder body (334) and is welded with the flange, a water outlet of a water inlet end (336) of the water outlet pipe is welded and matched with the water outlet pipe (335), and the taper is 30 degrees; the part of the lower part of the body is hollow conical, and the conical surface can guide the solid medicament into the swirling water body and does not discharge with water flow; the water flow is guided into the lower water inlet (331) along the inner wall, and the water flow rotates at a high speed along the inner wall by taking the axis as the center under the action of the high-pressure water pump to form vortex-shaped water flow, so that the granular medicament can return to the bottom of the cylinder for repeated reaction;
the self-cleaning filter (34) is a known device and comprises a water collecting tank (341), a ceramic filter disc (342), a self-cleaning filter water outlet end (343) and a slag scraping plate (344); wherein, the water collecting tank (341) is a rectangular tank body with an open upper end, the size is 2000mm 1500mm 1000mm, the material is carbon steel, and an epoxy anticorrosive coating is attached inside; the ceramic filter disc (342) has the diameter of 1500mm and the shape of a hollow disc structure, and porous ceramics with the pore diameter of 1 mu m are uniformly distributed on the two axial surfaces; the water pipe at the water outlet end (343) of the self-cleaning filter adopts DN32 with caliber, a connecting port is a thread, and is made of SUS 304 stainless steel and is positioned in the center of the disc; the slag scraping plate (344) is in a rectangular sheet shape with the thickness of 750mm x 50mm, is made of hard polyurethane and has certain elasticity and strength;
the jet medicine feeder (35) is made of SUS 304 stainless steel and is a commercially available jet medicine feeder with the flow rate of 10L/h, and comprises a jet medicine feeder water inlet (351), a jet medicine feeder water outlet (352) and a negative pressure medicine feeding port (353);
the self-cleaning sand filter (36) is a known device and comprises a self-cleaning sand filter water inlet (361), a clean water outlet (362), a sand washing water outlet (363), a compressed air inlet (364), a sand washer (365), sand filter (366) and a sand lifting pipe (367); wherein, the water pipes of the water inlet (361), the clear water outlet (362) and the sand washing water outlet (363) of the self-cleaning sand filter adopt DN32 caliber and SUS 304 stainless steel, are provided with flange interfaces and are welded on the sand filtering layer of the body; the sand extracting pipe (367) is a stainless steel pipe with the diameter of phi 10mm, the upper end of the sand extracting pipe is connected with the sand washer (365), and the lower end of the sand extracting pipe is covered to the bottom of the sand filter; the sand washer (365) is of a cylindrical double-layer structure, the inner layer is of a corrugated pipe shape, and the material is SUS 304 stainless steel; the compressed air inlet (364) water pipe is made of stainless steel SUS 304 with the caliber of DN20 and a flange as a connecting port and is positioned at the bottom of the body; the filter sand (366) is white quartz sand with the grain diameter of 1mm, and the filling position of the filter sand is two thirds of the height in the body and below; the lower part of the body is in a hollow conical shape;
the granular medicament comprises 5 percent of sepiolite, 5 percent of diatomite, 55 percent of calcium bicarbonate and 35 percent of tricalcium phosphate, is prepared by wet grinding with a ball mill and water, wherein the ball-feed ratio is 2:1, grinding to 100 meshes, stirring and mixing in a kneading mixer for 0.7 hour, drying by hot air, and roasting at the low temperature of 250 ℃ for 1.5 hours to prepare the granular medicament with the particle size of 80 meshes.
The particle medicament after roasting has certain strength and slow-release water solubility. The solubility is related to the composition proportion, the roasting temperature and the roasting time of each component of the composite medicament; the higher the firing temperature, the longer the firing time, and the higher the strength.
The water inlets of the fluorine water pump (41) and the concentrated water pump (42) are respectively connected with one end of a homogeneous fluorine-containing water tank (11) and one end of a reverse osmosis concentrated water tank (12), the water outlets of the two water pumps are respectively connected through DN100UPVC water pipes and converged into a three-way water inlet end of the pipeline mixer (31), the water outlet of the pipeline mixer (31) is connected to a water inlet (331) of a rotational flow medicine mixing device (33) through a D50UPVC water pipe through a flange, the rotational flow medicine mixing device (33) is made of SUS 304 stainless steel, on one hand, the feed end of a spiral feeder (32) with the length of 2 meters is arranged at the bottommost part of a PVC solid medicine groove (21) with the inclined surface at the bottom, the other end of the spiral feeder (32) is arranged on a hopper of a medicine adding port (333) at the upper part of the rotational flow medicine mixing device (33) in a lap joint mode, the transmission of the spiral feeder (32) is controlled by a program timer, and solid particle medicines can be added or supplemented according to a set time sequence. The water outlet (332) of the rotational flow medicine mixing device is connected to the water inlet at the upper part of the PVC medicine filtering tank (22) through a DN100UPVC water pipe, and the water outlet of the medicine filtering tank (22) is connected to the water collecting weir at the upper part of the per structure sedimentation tank (13) through the DN100UPVC water pipe. The water inlet of circulation dosing pump (43) passes through DN50UPVC water pipe and inserts sedimentation tank (13) middle part, its export adopts the water inlet of DN20UPVC water pipe and efflux doser (35) to be connected, the export of efflux doser (35) adopts DN20UPVC water piping connection to sedimentation tank (13) upper portion to intake water collecting weir, efflux doser (35) are advanced the medicine mouth and are passed through DN15UPVC water pipe and are connected with PVC liquid medicine groove (23), efflux doser (35) body material is SUS 304 stainless steel. The sediment water outlet (132) of the sedimentation tank is connected with the mud tank (14) through a DN200UPVC water pipe at the bottom, and a blow-down valve is arranged on the pipe. The water inlet of a mud pump (44) is connected with a mud pit (14) through a DN100UPVC (unplasticized polyvinyl chloride) water pipe, the water outlet is connected with a carbon steel water collecting tank (341) of a self-cleaning filter (34) through a DN50UPVC water pipe, the water outlet end (343) of the self-cleaning filter is connected with a water collecting weir of a water inlet end (131) at the upper part of a sedimentation tank through the DN50UPVC water pipe, a residue scraping plate (344) of the self-cleaning filter is made of hard polyurethane and has certain elasticity and strength, and the falling residues of the residue scraping plate (344) fall into a carbon steel residue tank (24) along with the diversion. The sensor probe of the on-line pH controller (52) is protected by a protective sleeve and is arranged in a pH controller socket (134) of the sedimentation tank (13), and the transmission output of the pH controller (52) is connected with a variable frequency controller of the circulating dosing pump (43). The water inlet of the middle water pump 1(45) is connected with a clear liquid water outlet (133) of the sedimentation tank through a DN100UPVC water pipe, the water outlet of the water pump is connected with a water inlet (361) of the self-cleaning sand filter through a DN50UPVC water pipe, a clear water outlet (362) of the self-cleaning sand filter is connected to a fluorine removal water production tank (15) through the DN50UPVC water pipe, the fluorine removal water production tank (15) is used for coating an epoxy corrosion prevention all-in-one structure on the inner wall, the sand cleaning water outlet (363) of the self-cleaning sand filter is connected to a mud slurry tank (14) through the DN50UPVC water pipe, a compressed air inlet (364) of the self-cleaning sand filter is connected with a self-provided air compressor or a compressed air pipeline through a pressure hose, white quartz sand with the grain diameter of 1mm is filled in the self-cleaning sand filter (36), and the self-cleaning sand filter (36) is made of SUS 304 stainless steel. The water inlet of the middle water pump 2(46) is connected to the middle of the defluorination water production pool (15) through a DN50UPVC water pipe, the water outlet is connected to the water inlet end (371) of the ionic membrane desalination device through a DN25UPVC water pipe, the water production end (372) of the ionic membrane desalination device is connected to the reuse water pool (16) through a DN25UPVC water pipe, the concentrated water end (373) of the ionic membrane desalination device is connected to one end of the homogeneous fluorine-containing water pool through a DN25UPVC water pipe, the ionic membrane desalination device (37) is a combined device, the main material is SUS 304 stainless steel, and the reuse water pool (16) is of an epoxy anticorrosion integrated structure with an inner wall painting.
The pump heads of the fluorine water pump (41) and the concentrated water pump (42) are made of corrosion-resistant fluoroplastic and have the flow rate of 30m3H, the lift is 10 m;
the circulating dosing pump is a variable frequency water pump;
the control of the amount of the liquid agent to be added is realized by a pH controller (52) inserted into the sedimentation tank (13).
Example 2
The high-concentration fluorine-containing wastewater reuse treatment device for the production of the silicon solar cell, which is formed in the embodiment 1, is used for treating the high-concentration fluorine-containing wastewater produced by the production of certain solar cell enterprises, wherein the fluorine content of the wastewater is 2000mg/L and the fluorine-containing water content of the wastewater is 15 t/h. High-concentration fluorine-containing wastewater from a production workshop and reverse osmosis concentrated water with the hardness of 1200mg/L are respectively stored in a homogeneous fluorine-containing water tank (11) and a reverse osmosis concentrated water tank (12), and are mixed by a pipeline mixer (31) according to the proportion that the flow rate of the fluorine-containing water is 1.5 to 1 and the flow rate of the concentrated water is 1.5 to 1, the water inflow of mixed water of a rotational flow medicine mixing device (33) is 20t/h, the concentration of fluorine ions is reduced to 1750mg/L, and the hardness is reduced to 310 mg/L.
The method aims to fully mix high-hardness concentrated water generated in the process of preparing pure water by reverse osmosis for production with high-fluorine-containing wastewater, reduce the concentration of fluorine ions in the high-fluorine-containing water and the hardness of the concentrated water by utilizing the reaction of calcium and magnesium ions in the reverse osmosis concentrated water and the fluorine ions in the high-fluorine-containing water in the mixing process, reduce the dosage of a medicament, and simultaneously fully recycle the concentrated water generated by the reverse osmosis.
Granular fluorine removal agent prepared by sepiolite, diatomite, calcium bicarbonate and tricalcium phosphate is added into a chemical adding port (333) of the rotational flow chemical mixing device, the initial adding amount is 100kg, the feeding amount control screw feeder (32) is intermittent for 1 hour every 3 minutes, the feeding amount is 40kg/h, and mixed water and the granular chemical react in the rotational flow chemical mixing device (33) and then enter a chemical filtering tank (22).
The granular defluorinating agent which is not easy to dissolve in the solid medicine tank (21) is fed into the cyclone medicine mixing device (33) from a medicine feeding port (333) above the cyclone medicine mixing device along the inner wall through a screw feeder (32), the medicine and the liquid are rapidly rotated and mixed to react, under the action of centrifugal force, the granular medicine moves along the direction of the semi-radial inner wall of the cyclone, water spirally rises to a water outlet pipe (335) in the middle part and then flows out, the unreacted granular medicine returns to the bottom of the medicine mixing device to be reused, the liquid medicine separation effect after the reaction is achieved, the granular medicine is compounded by sepiolite, diatomite, calcium bicarbonate and tricalcium phosphate, the particle size is 50 meshes, and the granular medicine can be excessively fed; the effluent of the rotational flow medicine mixing device (33) enters a medicine filter tank (22) filled with the same particle fluorine removal agent and is changed into a static flow state (which is a static reaction of wastewater and a medicament) because the water entering the sedimentation tank (13) keeps advection as much as possible, so that the impact on sediments in the water of the sedimentation tank (13) is reduced, and a good sedimentation effect is achieved. The rotational flow mixed medicine plays the roles of uniform stirring and solid-liquid separation, the fluoride after reaction is taken away in water, the medicament is intercepted, and the dosage is further reduced.
The effluent of the drug filter tank (22) enters a sedimentation tank (13), the content of fluorine ions in the inlet water of the sedimentation tank (13) is reduced to 4.77mg/L, a prepared fluorine ion chelating agent prepared by 70% of calcium hydroxy phosphate, 10% of chitosan and 20% of calcium bicarbonate is arranged in the liquid drug tank (23), the drug adding amount is controlled to be 30mg/L through a circulating drug adding pump (43) (namely the drug adding amount of each liter of solution in the sedimentation tank is 30 mg), and after the drugs are added, the content of the fluorine ions in the outlet water of the sedimentation tank (13) is reduced to 3.42 mg/L.
The circulating dosing pump (43) is a variable frequency water pump, and the dosage of the liquid medicament is controlled by a pH controller (52) inserted into the sedimentation tank (13), wherein the pH control range is 7. For local point type dosing, a circulating water pump is matched with a pipeline jet flow dosing device (35) to enable dosing to be more uniform.
And after passing through a self-cleaning sand filter (36), the fluorine ion content of the effluent is further reduced to 1.53mg/L, thereby achieving the fluorine removal requirement. After the drug adding treatment link, the water hardness of the defluorination water generating tank (15) is increased to 860mg/L, and then the water passes through the ionic membrane desalination device (37), and the water quality in the reuse water tank (16) has the fluorine ion content of 1.27mg/L and the hardness of 307 mg/L. The requirement of reverse osmosis process water inlet quality is met.
The above embodiments have been described in detail with reference to the accompanying drawings, and the shapes, sizes, materials, connection manners, and the types, amounts and manners of the drug to be applied are only used for illustrating the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the claims of the present invention. All equivalent changes or modifications made according to the spirit of the present invention are covered in the protection scope of the present invention.
The invention is not the best known technology.
Claims (2)
1. A high-concentration fluorine-containing wastewater recycling treatment process generated in silicon solar cell production is characterized by comprising the following steps:
(1) pumping the fluorine-containing wastewater stored in the homogeneous fluorine-containing water tank and the reverse osmosis concentrated water stored in the reverse osmosis concentrated water tank into a pipeline mixer through a fluorine water pump and a concentrated water pump respectively for mixing, and feeding the obtained mixed water into a rotational flow medicine mixing device;
wherein the fluorine ion content of the fluorine-containing wastewater is 1000-2000 mg/L; the hardness of the reverse osmosis concentrated water is 1000-2000 mg/L; the flow ratio of the fluorine-containing wastewater to the reverse osmosis concentrated water is 1: 5-5: 1, the water inflow of mixed water of the rotational flow medicine mixing device is 5-50 t/h, the diameter of a cylinder of the rotational flow medicine mixing device is 500-1500 mm, and the height of the cylinder is 1500-2500 mm;
(2) the mixed water of the fluorine water and the concentrated water is mixed with the granular medicament in a rotational flow mode along the inner wall of the rotational flow medicament mixing device through a water inlet of the rotational flow medicament mixing device, the water mixed with the medicament is concentrated at the central part of the rotational flow medicament mixing device and flows out along a water outlet pipe through a water inlet end of a water outlet pipe of the rotational flow medicament mixing device; the granular medicament returns to the bottom of the rotational flow medicament mixing device along the inner wall of the rotational flow medicament mixing device under the action of centrifugal force and gravity;
wherein, the granular medicament in the solid medicament groove enters the rotational flow medicament mixing device through the spiral feeder through the medicament feeding port of the rotational flow medicament mixing device; the initial adding amount of the solid medicament is 10-30% of the volume of the rotational flow medicament mixing device, and the medicament adding amount during operation is supplemented in an equivalent manner according to the reaction consumption amount;
the granular medicament comprises 0.5-5% of sepiolite, 0.5-5% of diatomite, 35-75% of calcium bicarbonate and 20-45% of tricalcium phosphate;
(3) after passing through the drug filter tank, the feed liquid flowing out of the water outlet of the rotational flow drug mixing device enters a sedimentation tank and stands for 20-40 minutes; meanwhile, the fluorine ion chelating agent solution in the liquid medicine tank is pumped from the sedimentation tank through a circulating medicine adding pump and is injected into the sedimentation tank through a jet medicine adding device, so that the pH value of the solution in the sedimentation tank is 5-8;
the fluorine ion chelating agent is one or a plurality of compounds of 60-100% of calcium hydroxy phosphate, 10-100% of chitosan and 20-100% of calcium bicarbonate, and the concentration of the fluorine ion chelating agent is 30-80 mg/L;
(4) discharging sediment in a sedimentation tank into a mud tank, pumping mud in the mud tank into a water collecting tank of a self-cleaning filter through a mud pump, rotating a ceramic filter disc of the self-cleaning filter, absorbing the mud in the water collecting tank to the surface of the filter disc by negative pressure inside the ceramic filter disc, discharging dry filter residue from the filter residue collecting tank into a mud tank through a residue scraping plate, returning filter water from the negative pressure filtering of the filter to the water inlet end of the sedimentation tank, wherein the filtering aperture of the ceramic filter disc is 0.5-10 mu m;
meanwhile, the upper clear water of the sedimentation tank is pumped into the bottom of the filter sand through a self-cleaning sand filter by a water pump through a middle pipeline, the water after sand filtration enters a fluorine removal water production tank through a top clear water outlet, the bottom dirty sand is lifted to a sand washer on the upper part of the sand filter by compressed air through a middle sand lifting pipe, the cleaned filter sand returns to the upper layer of the filter sand in the sand filter, the sand washing sewage is discharged into a mud slurry tank through a sand washing water outlet, and the diameter of the filter sand is 0.5-2.0 mm;
(5) after water in the defluorination water production pool is defluorinated and purified, the water is pumped into an ionic membrane desalination device through a water pump to be subjected to hardness removal softening treatment, and two streams of water are produced, one is produced water, and the other is concentrated water; the product water of demineralizer gets into the reuse water pond, and the concentrated water of demineralizer gets into homogeneity fluorine-containing water pond and continues to mix reaction with high enriched fluorine-containing water, reduces the use of defluorinating medicament, and the demineralizer desalination rate is 50 ~ 80%, product water quality: the fluorine ion concentration is 1-5 mg/L, the hardness is 100-500 mg/L, and the recycling requirement of reverse osmosis process water is met;
the particle size of the granular medicament is 50-100 meshes;
the device comprises a homogeneous fluorine-containing water tank, a reverse osmosis concentrated water tank, a sedimentation tank, a slurry tank, a fluorine-removing water-producing tank, a reuse water tank, a solid medicine tank, a medicine filtering tank, a liquid medicine tank, a sludge tank, a pipeline mixer, a screw feeder, a rotational flow medicine mixing device, a self-cleaning filter, a jet medicine adding device, a self-cleaning sand filter, an ionic membrane desalting device, a fluorine water pump, a concentrated water pump, a circulating medicine adding pump, a mud pump, an intermediate water pump 1, an intermediate water pump 2, a proportion regulator and a pH controller;
the connection relationship is as follows: the homogeneous fluorine-containing water tank and the reverse osmosis concentrated water tank are respectively connected to a rotational flow pesticide mixing device through a fluorine water pump and a concentrated water pump through a pipeline mixer, the rotational flow pesticide mixing device is also connected with one end of a pesticide filter tank, and the pesticide filter tank is communicated with a sedimentation tank after being converged with a pipeline of the self-cleaning filter; the sedimentation tank is also connected with a self-cleaning sand filter through an intermediate water pump 1, the self-cleaning sand filter is connected with a fluorine removal water production tank, and the fluorine removal water production tank is also connected with an ionic membrane desalination device through an intermediate water pump 2; the ionic membrane desalination device is also respectively connected with the reuse water pool and the homogeneous fluorine-containing water pool; the self-cleaning sand filter is also connected with a mud tank, and the mud tank is connected with the self-cleaning filter through a mud pump; the self-cleaning filter is also respectively connected with the sedimentation tank and the sludge tank; the liquid medicine tank is connected with the sedimentation tank through the jet flow medicine mixer, a sensor probe of the pH controller is placed in the sedimentation tank, and the transmission output of the pH controller is connected with the circulating medicine feeding pump.
2. The process of claim 1, wherein the process is used in a device for recycling and treating high-concentration fluorine-containing wastewater generated in the production of silicon solar cells, the ratio regulator is connected with a concentrated water pump, and the ratio regulator is connected with a fluorine water pump through signal lines, and the concentrated water pump is a variable frequency water pump; the control of the amount of the liquid medicament added is realized by the pH controller inserted into the sedimentation tank.
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| JP2001225082A (en) * | 2000-02-16 | 2001-08-21 | Nec Environment Eng Ltd | Fluorine-containing wastewater treatment method |
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