CN213112663U - Device for preparing defluorinating agent by bipolar membrane acid production - Google Patents
Device for preparing defluorinating agent by bipolar membrane acid production Download PDFInfo
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Abstract
The utility model discloses a device for preparing defluorinating agent by bipolar membrane acid production. A bipolar membrane for subjecting a solution containing an inorganic salt to electrolytic treatment; the acid liquor tank is connected with the acid generating chamber of the bipolar membrane; the first reaction tank is connected to the acid liquor tank; the first iron powder feeding port and the first oxidant feeding port are respectively connected to the acid liquor tank; the second reaction tank is connected to the acid liquor tank; the aluminum powder feeding port is connected with the acid liquid tank; the third reaction tank is connected with the acid liquor tank; the second iron powder feeding port, the calcium aluminate feeding port and the second oxidant feeding port are respectively connected to the acid liquor tank; the mixing tank is connected with the first reaction tank, the second reaction tank and the third reaction tank; and the mixing tank is also connected with a polyethylene polyamine storage tank. The utility model discloses a hydrochloric acid that bipolar membrane produced has prepared ferric chloride, aluminium chloride and polyaluminium ferric chloride solution, mixes it and adds diethylenetriamine pentaacetate and has obtained high-efficient defluorinating agent.
Description
Technical Field
The utility model relates to a device for preparing defluorinating agent by bipolar membrane acid production, which belongs to the technical field of water treatment agent.
Background
With the rapid development of industrial technologies, environmental problems become more severe, and in order to respond to the call of government ecological environment civilized construction, many chemical enterprises begin to perform zero-emission treatment on wastewater so as to achieve the purposes of emission reduction and resource utilization. The bipolar membrane is a core technology in a zero discharge system, is assembled into electrodialysis equipment together with homogeneous anion and cation exchange membranes, and can be directly used for salt-containing wastewaterThe corresponding acid and alkali are directly prepared from the salt by the treatment of (1), and the recovery and the cyclic utilization of the waste salt are realized. The utilization range of the generated alkali is wider, but the acid recycling approach needs to be further developed. In addition, scrap of aluminum and iron produced in the metal manufacturing industry is often discarded, resulting in waste of resources. The problem of fluorine pollution is also attracting more and more attention, and the fluorine removal technology mainly takes the chemical agent as the current technology, and the existing fluorine removal chemical agent is difficult to reduce fluorine to a lower level. E.g. using calcium salts to form CaF2Precipitation, the fluorine content in the produced water is basically about 10mg/L, and the calcium ions in the high-altitude water can be greatly increased.
In addition, in many production processes, it is necessary to treat wastewater containing salt by using a bipolar membrane, and obtain an alkali solution and an acid solution by means of electrolysis, for example, after a purification process of a lithium chloride solution, lithium hydroxide and acid can be obtained by performing electrolysis treatment on the lithium chloride solution by using the bipolar membrane, and lithium hydroxide is taken as a product, and a large amount of acid is by-produced in the above process, for example, reference CN106946275A relates to a method for directly preparing battery-grade lithium hydroxide monohydrate from lithium-rich brine in a salt lake, wherein the main process steps are as follows: (1) processing the lithium-rich brine in the salt lake to obtain deeply impurity-removed lithium-rich brine; (2) the method comprises the steps of sequentially passing the lithium-rich brine subjected to deep impurity removal through special-effect boron adsorption resin and chelating resin to obtain purified lithium-rich brine; (3) carrying out water splitting on the purified lithium-rich brine by using bipolar membrane electrodialysis equipment to obtain alkali liquor and acid liquor; (4) evaporating and crystallizing the alkali liquor to obtain a lithium hydroxide crude product; (5) and dissolving the lithium hydroxide crude product with water, evaporating and concentrating, washing the precipitated crystals with water, and drying to obtain the battery-grade lithium hydroxide monohydrate.
In addition, in many metal processing processes, solid wastes such as iron powder and aluminum powder are generated, which often causes certain difficulty in recycling, and the utilization rate of the wastes is low.
SUMMERY OF THE UTILITY MODEL
The utility model provides a method for preparing defluorinating agent by acid production of bipolar membrane, which produces a high-efficiency defluorinating agent by acid production of bipolar membrane and aluminum and iron waste materials through a certain chemical reaction, realizes recycling of acid and waste materials, and ensures that the fluorine content of effluent of fluorine-containing wastewater is lower than 1 mg/L.
The technical scheme is as follows:
a method for preparing a fluorine removal agent by bipolar membrane acid production comprises the following steps:
step 1, carrying out electrolytic treatment on a solution containing lithium chloride by adopting a bipolar membrane to obtain lithium hydroxide and a hydrochloric acid solution;
step 3, taking the hydrochloric acid solution obtained in the step 1, adding aluminum powder to dissolve the aluminum powder, and using the aluminum powder as AlCl3A solution;
step 4, adding iron powder into the hydrochloric acid solution obtained in the step 1 to dissolve the iron powder, and then adding an oxidant to enable Fe2+Oxidation to Fe3+Then adding calcium aluminate powder for reaction, and adding a stabilizer to obtain a polyaluminum ferric chloride solution;
step 5, FeCl is added3Solution, AlCl3Mixing the solution with polyaluminum ferric chloride solution, and adding polyethylene polyamine to obtain the defluorinating agent.
In one embodiment, the hydrochloric acid solution has a concentration of 1 to 4 mol/L.
In one embodiment, the oxidant is sodium hypochlorite or hydrogen peroxide.
In one embodiment, the stabilizer is sodium phosphate.
In one embodiment, the polyethylene polyamine is diethyl triamine pentaacetate.
In one embodiment, the calcium aluminate is added in an amount 2 to 4 times the amount of the iron powder in the 4 th step.
In one embodiment, in said step 5, FeCl3Solution, AlCl3The volume ratio of the solution to the polyaluminum ferric chloride solution is 0.1-0.5: 2-5: 0.6 to 2; the weight of the polyethylene polyamine is 5-15% of the weight of the ferric chloride solution.
The defluorinating agent directly obtained by the preparation method.
The application of the fluorine removal agent in fluorine removal of fluorine-containing wastewater.
In one embodiment, the application comprises the following steps: taking a certain volume of fluorine-containing wastewater, adding the defluorination medicament, adjusting the pH value, adding a certain volume of coagulant aid, slowly stirring, standing, filtering produced water, and filtering out flocculating constituents.
In one embodiment, the amount of fluorine removal agent added to the wastewater is in accordance with AlCl3The mass ratio of the/F is 35-40.
In one embodiment, adjusting the pH is adjusting to between 6.5 and 7.5.
In one embodiment, the filtration process is cross-flow filtration using a tubular ceramic membrane filter 9.
In one embodiment, the cross-flow filtration has a membrane face flow rate of 1 to 5 m/s.
In one embodiment, the two ends of the tubular ceramic membrane filter are end sockets, the two ends of the end sockets are respectively provided with a raw material liquid inlet and a raw material liquid outlet, a ceramic membrane element is arranged in the tubular ceramic membrane filter, a penetrating liquid outlet is also formed in the tubular ceramic membrane filter, and the penetrating liquid outlet is communicated with the penetrating side of the ceramic membrane element; the ceramic membrane element is provided with a raw material liquid inlet, the ceramic membrane element is provided with an inner channel opening, the inner channel opening is arranged at the position, facing the raw material liquid inlet, of the ceramic membrane element, the conical joint is arranged at the position, facing the raw material liquid inlet, of the side, with the larger radius, of the conical joint, and an inner swirl groove is further arranged inside the conical joint and used for generating swirl for the raw material liquid flowing into the ceramic membrane element.
In one embodiment, the distance between adjacent groove bodies is 0.5-2mm, the height of the groove bodies is 1-3mm, and the helix angle is 10-50 degrees.
Advantageous effects
The method for preparing the defluorinating agent by acid production through the bipolar membrane has the following advantages: 1. provides a new utilization way of acid production by the bipolar membrane, further promotes the engineering application of the bipolar membrane, and the mature process for preparing ferric chloride, aluminum chloride and polyaluminum ferric chloride by hydrochloric acid. 2. The raw materials are the wastes of metal processing factories, the sources are wide, the price is low, the reutilization of waste resources is realized, and the requirements of green production are met. 3. The fluorine content of the effluent of the fluorine-containing wastewater can be reduced to 1mg/L by adopting the fluorine removing agent prepared by bipolar membrane acid production, the aluminum content of the raw water is less than 0.5mg/L, and the total iron content is almost zero.
Drawings
FIG. 1 is a flow chart of the present invention for preparing a fluorine removing agent;
FIG. 2 is a diagram of an apparatus for preparing a fluorine removing agent according to the present invention;
FIG. 3 is a structural diagram of a tubular ceramic membrane used in a defluorination process using the defluorinating agent of the present invention;
FIG. 4 shows the comparison of the pore diameter distribution of the ceramic membrane filtering flocculating constituent before and after the operation of the defluorinating agent of the utility model applied to the defluorination process of the biochemical produced water of coking wastewater.
Wherein, 1, a bipolar membrane; 2. an acid liquor tank; 31. 32, 33 are respectively a first reaction tank, a second reaction tank and a third reaction tank; 41. 42, 43 are the first, second, third filters, respectively; 51. 52, 53 are a first, a second and a third tank, respectively; 6. a mixing tank; 7. a polyethylene polyamine storage tank; 81. a first iron powder charging port; 82. a first oxidant addition port; 83. An aluminum powder inlet; 84. a second iron powder charging port; 85. a calcium aluminate inlet; 86. a second oxidant addition port; 9. a tubular ceramic membrane filter; 10. sealing the end; 11. a feed solution inlet; 12. a raw material liquid outlet; 13. a permeate outlet; 14. a ceramic membrane element; 15. a tapered joint; 16. an inner swirl groove.
Detailed Description
The utility model provides a method for preparing defluorinating agent by bipolar membrane acid production, the preparation process is shown in figure 1.
The utility model mainly utilizes two industrial wastes, one is the acid of the bipolar membrane by-product in the process of electrolyzing the salt solution, and the other is the waste iron and aluminum powder.
The method comprises the steps of respectively preparing aluminum chloride, ferric chloride and polyaluminum ferric chloride by using hydrochloric acid produced by a bipolar membrane, mixing the two materials according to a certain proportion, and simultaneously adding an auxiliary agent DTPA to finally obtain the defluorinating agent product.
Preparation of ferric chloride: and adding scrap iron according to the concentration of hydrochloric acid produced by the bipolar membrane, adding one of sodium hypochlorite or hydrogen peroxide as an oxidant after the scrap iron is dissolved, and filtering and purifying to obtain a ferric chloride solution. In this step, hydrochloric acid can dissolve iron filings to generate Fe2+By adding oxidizing agent and then adding Fe2+Oxidation to Fe3+As FeCl3And (3) solution.
Preparation of aluminum chloride: and adding aluminum scraps according to the concentration of hydrochloric acid produced by the bipolar membrane, dissolving the aluminum scraps, and filtering and purifying to obtain an aluminum chloride solution. In the step, the aluminum scraps can be dissolved by hydrochloric acid to generate AlCl3And (3) solution.
Preparation of polyaluminum ferric chloride: adding scrap iron according to the concentration of hydrochloric acid produced by the bipolar membrane, heating for dissolving reaction, adding one of sodium hypochlorite or hydrogen peroxide as an oxidant, adding calcium aluminate, stirring for reaction, filtering while hot, and adding a proper amount of stabilizer to obtain the final polyaluminum ferric chloride solution. The calcium aluminate powder contains monocalcium aluminate (Ca. A1) as main mineral component2O3) Monocalcium dialuminate (Ca 2A 1)2O), main reaction of calcium aluminate powder and hydrochloric acid to generate mAl2（OH）nCl6-n→［Al2（OH）nCl6N ] m, basic aluminum chloride is generated in the reaction process, and basic ferric chloride is accompanied. When the pH value is increased to a certain value, two adjacent hydroxyl groups generate bridging polymerization and self-polymerization until a certain polymerization degree is reached.
Finally, mixing ferric chloride, aluminum chloride and polyaluminum ferric chloride according to a certain volume ratio, adding Diethyl Triamine Pentaacetate (DTPA), and compounding to prepare the defluorinating agent. The components are mixed according to the following volume ratio: 60-80% of aluminum chloride solution, 20-30% of polyaluminum ferric chloride solution, 5-10% of ferric chloride solution and 0.5-2% of diethylenetriamine pentaacetate by mass concentration.
In the above fluorine-removing agent, Al3+、Fe3+Can be combined with F-Form stable complexes, and they hydrolyze in water to form flocculated hydroxide precipitates with strong adsorption capacity to adsorb F in large quantities from waste water-The auxiliary agent can be effectively added with diethylenetriamine pentaacetateGround improvement of F in defluorination flocculation-The adsorption and flocculation effects of (1).
Based on the above method, the device provided by the utility model is shown in fig. 2, comprising
A bipolar membrane 1 for subjecting a solution containing an inorganic salt to electrolytic treatment;
the acid liquor tank 2 is connected with the acid producing chamber of the bipolar membrane 1 and is used for storing acid liquor generated by electrolysis;
the first reaction tank 31 is connected to the acid liquor tank 2 and is used for carrying out the preparation reaction of ferric chloride;
a first iron powder feeding port 81 and a first oxidizing agent feeding port 82, which are respectively connected to the acid solution tank 2 and are respectively used for feeding iron powder and an oxidizing agent into the acid solution tank 2;
the second reaction tank 32 is connected to the acid liquor tank 2 and is used for carrying out the preparation reaction of aluminum chloride;
the aluminum powder adding port 83 is connected to the acid liquor tank 2 and is used for adding aluminum powder into the acid liquor tank 2;
the third reaction tank 33 is connected to the acid liquor tank 2 and is used for carrying out the preparation reaction of the polyaluminum ferric chloride;
the second iron powder feeding port 84, the calcium aluminate feeding port 85 and the second oxidant feeding port 86 are respectively connected to the acid liquor tank 2 and are respectively used for feeding powder, an oxidant and calcium aluminate into the acid liquor tank 2;
the mixing tank 6 is connected with the first reaction tank 31, the second reaction tank 32 and the third reaction tank 33 and is used for mixing the prepared products; and a polyethylene polyamine storage tank 7 is connected to the mixing tank 6.
Preferably, the first reaction tank 31 is connected to the mixing tank 6 sequentially through the first filter 41 and the first storage tank 51.
Preferably, the second reaction tank 32 is connected to the mixing tank 6 sequentially through the second filter 42 and the second storage tank 51.
Preferably, the third reaction tank 33 is connected to the mixing tank 6 sequentially through the third filter 43 and the third storage tank 51.
When the fluorine removing agent is used, the following method can be adopted: taking a certain volume of fluorine-containing wastewater according to AlCl3Quality of/< F >Adding the fluorine removal agent according to the weight ratio of 35-40, stirring for 10-15 min, adjusting the pH to be 6.5-7.5, adding a certain volume of coagulant aid, slowly stirring, standing for 10min, filtering produced water, and filtering to remove floccules to obtain filtrate with the fluorine content of less than 1 mg/L.
In the filtering process, a tubular or multi-channel ceramic membrane element can be adopted for filtering to remove the flocculating agent and improve the water quality of wastewater treatment. As shown in fig. 3, the tubular ceramic membrane filter 9 used herein may be configured such that two ends of the tubular ceramic membrane filter 9 are end sockets 10, two ends of the end sockets 10 are respectively provided with a raw material liquid inlet 11 and a raw material liquid outlet 12, a ceramic membrane element 14 is installed inside the tubular ceramic membrane filter 9, the tubular ceramic membrane filter 9 is further provided with a penetrating fluid outlet 13, and the penetrating fluid outlet 13 is communicated with a penetrating side of the ceramic membrane element 14; a taper joint 15 is further provided at the internal passage opening of the ceramic membrane element 14 at a position facing the raw material liquid inlet 11, the side of the taper joint 15 having a larger radius faces the raw material liquid inlet 11, and an internal swirling flow groove 16 is further provided inside the taper joint 15, the internal swirling flow groove 16 being for swirling the raw material liquid flowing into the ceramic membrane element 14.
During the filtering process of the flocculating constituent, a filter cake is formed in the internal channel of the ceramic membrane element 14, and the filter cake layer near the raw material liquid inlet 11 is usually thin (mainly because the flow is large and the scouring force is strong when entering the channel, so that the filter cake is not easy to form), while the filter cake layer near the raw material liquid outlet 12 is thick (mainly because after filtering, more penetrating liquid leaves the pipe, so that the flow in the pipe is reduced and the scouring force is weakened); this situation may cause more wear of the flocs on the inner wall of the passage near the raw material liquid inlet 11, and the inner swirl groove 16 makes the raw material liquid flowing at high speed generate swirl at the opening, so that the flocs can be collected more at the middle position of the liquid by the action of the swirl when entering the inlet of the ceramic membrane element 14, avoiding the contact with the wall surface, and reducing the problem of excessive wear caused by the thinner filter cake layer at the inlet of the ceramic membrane element 14.
Example 1
Preparation of ferric chloride: taking 1.5L of bipolar membrane to produce hydrochloric acid (the acid concentration is 2 mol/L), adding 100g of scrap iron, stirring for reaction and dissolution, adding excessive sodium hypochlorite to oxidize ferrous iron into ferric iron, and filtering to obtain a ferric chloride clear solution.
Preparation of aluminum chloride: taking 4L of bipolar membrane produced hydrochloric acid (the acid concentration is 2 mol/L), adding 190g of aluminum scraps, stirring, reacting, dissolving, and filtering to obtain an aluminum chloride clear solution.
Preparation of polyaluminum ferric chloride: taking 2.5L of bipolar membrane hydrochloric acid (acid concentration is 2 mol/L), adding 35g of scrap iron, stirring for reaction and dissolution, adding excessive sodium hypochlorite to oxidize ferrous iron into ferric iron, adding 110g of calcium aluminate, stirring for reaction, filtering while hot, adding sodium phosphate as a stabilizer, and stirring for reaction to obtain polyaluminum ferric chloride.
0.4L of ferric chloride solution, 4.0L of aluminum chloride solution, 1.5L of polyaluminum ferric chloride solution and 30g of diethyl triamine pentaacetate are respectively mixed to obtain the defluorinating agent.
Example 2
Preparation of ferric chloride: taking 1L of bipolar membrane to produce hydrochloric acid (the acid concentration is 2 mol/L), adding 80g of scrap iron, stirring, reacting and dissolving, adding excessive sodium hypochlorite to oxidize ferrous iron into ferric iron, and filtering to obtain a ferric chloride clear solution.
Preparation of aluminum chloride: taking 5L of bipolar membrane produced hydrochloric acid (the acid concentration is 2 mol/L), adding 200g of aluminum scraps, stirring, reacting, dissolving, and filtering to obtain an aluminum chloride clear solution.
Preparation of polyaluminum ferric chloride: taking 2L of bipolar membrane hydrochloric acid (acid concentration is 2 mol/L), adding 30g of scrap iron, stirring for reaction and dissolution, adding excessive sodium hypochlorite to oxidize ferrous iron into ferric iron, adding 100g of calcium aluminate, stirring for reaction, filtering while hot, adding sodium phosphate as a stabilizer, and stirring for reaction to obtain polyaluminum ferric chloride.
0.3L of ferric chloride solution, 3.5L of aluminum chloride solution, 1.2L of polyaluminum ferric chloride solution and 25 g of diethyl triamine pentaacetate are respectively mixed to obtain the defluorinating agent.
Example 3
Preparation of ferric chloride: taking 0.8L of bipolar membrane to produce hydrochloric acid (the acid concentration is 2 mol/L), adding 80g of scrap iron, stirring for reaction and dissolution, adding excessive sodium hypochlorite to oxidize ferrous iron into ferric iron, and filtering to obtain a ferric chloride clear solution.
Preparation of aluminum chloride: taking 4.5L of bipolar membrane produced hydrochloric acid (acid concentration is 2 mol/L), adding 200g of aluminum scraps, stirring, reacting, dissolving and filtering to obtain an aluminum chloride clear solution.
Preparation of polyaluminum ferric chloride: taking 1.8L of bipolar membrane hydrochloric acid (acid concentration is 2 mol/L), adding 30g of scrap iron, stirring for reaction and dissolution, adding excessive sodium hypochlorite to oxidize ferrous iron into ferric iron, adding 90g of calcium aluminate, stirring for reaction, filtering while hot, adding sodium phosphate as a stabilizer, and stirring for reaction to obtain polyaluminum ferric chloride.
0.5L of ferric chloride solution, 4.5L of aluminum chloride solution, 1.8L of polyaluminum ferric chloride solution and 30g of diethyl triamine pentaacetate are respectively mixed to obtain the defluorinating agent.
Comparative example 1
The difference from example 3 is that: no diethyl triamine pentaacetate is added in the preparation process of the fluorine removal agent.
Application example
The coking wastewater obtained from a coking plant is subjected to biochemical treatment by an A-O-O (reduction oxidation-oxidation) method,
the water quality of the wastewater after biochemical treatment is as follows:
adding 6L of the defluorinating agent into 500L of effluent of the sedimentation tank, continuously adding 20ppm of coagulant aid cationic polyacrylamide to perform flocculation reaction, performing 3m/s cross-flow filtration on the reaction effluent through a 500nm tubular ceramic membrane, and then obtaining water after defluorination treatment.
The water quality of the wastewater treated in each example is as follows:
as can be seen from the above table, the defluorinating agent adopted by the utility model has better defluorinating effect when defluorinating the produced water of the coking wastewater after biochemical treatment, and can realize the removal rate of more than 95 percent of the fluorine content in the wastewater; successfully realizes the joint preparation of the defluorinating agent by the electrolysis waste liquid of the bipolar membrane and the industrial solid waste; when the coagulant aid is used together, the COD, nitrogen and chroma in the secondary produced water can be reduced.
The pipe-type ceramic membrane channel used has the internal channel diameter of 8mm, the conical joint is processed and installed at the raw material liquid inlet, the joint height is 20cm, the diameter of the conical bottom surface is 15mm, the inside of the conical joint is provided with a swirl groove, the distance between adjacent groove bodies is 1mm, the height of the groove bodies is 1.5mm, and the helix lift angle is 30 degrees. The characterization result of the surface pore size distribution of the ceramic membrane after 8 batches of coking biochemical produced water (500L per batch) is shown in FIG. 4. It can be seen from the figure that after continuous operation, the generation of macropores in the membrane tube can be effectively avoided by using the conical joint, compared with the joint without the swirl groove, and the figure can show that after the conventional tubular ceramic membrane is operated for many times, macropores appear at about 1000nm, and the support layer is exposed due to the abrasion of the surface of the membrane; it is explained that the large pores generated by abrasion of the membrane surface can be avoided by adopting the above structure.
Claims (4)
1. A device for preparing a fluorine removal agent by bipolar membrane acid production is characterized by comprising:
a bipolar membrane (1) for subjecting a solution containing an inorganic salt to electrolytic treatment;
the acid liquor tank (2) is connected with the acid generating chamber of the bipolar membrane (1) and is used for storing acid liquor generated by electrolysis;
the first reaction tank (31) is connected to the acid liquor tank (2) and is used for carrying out the preparation reaction of ferric chloride;
the first iron powder adding port (81) and the first oxidant adding port (82) are respectively connected to the acid liquor tank (2) and are respectively used for adding iron powder and an oxidant into the acid liquor tank (2);
the second reaction tank (32) is connected to the acid liquor tank (2) and is used for carrying out the preparation reaction of the aluminum chloride;
the aluminum powder adding port (83) is connected with the acid liquor tank (2) and is used for adding aluminum powder into the acid liquor tank (2);
the third reaction tank (33) is connected with the acid liquor tank (2) and is used for carrying out the preparation reaction of the polyaluminum ferric chloride;
the second iron powder feeding port (84), the calcium aluminate feeding port (85) and the second oxidant feeding port (86) are respectively connected to the acid liquor tank (2) and are respectively used for feeding powder, an oxidant and calcium aluminate into the acid liquor tank (2);
the mixing tank (6) is connected with the first reaction tank (31), the second reaction tank (32) and the third reaction tank (33) and is used for mixing the prepared products; and a polyethylene polyamine storage tank (7) is connected to the mixing tank (6).
2. The device for preparing the defluorinating agent by bipolar membrane acidogenesis according to claim 1, wherein the first reaction tank (31) is connected to the mixing tank (6) through the first filter (41) and the first storage tank (51) in sequence.
3. The device for preparing the fluorine removal agent by bipolar membrane acidogenic method according to claim 1, wherein the second reaction tank (32) is connected to the mixing tank (6) through the second filter (42) and the second storage tank (52) in sequence.
4. The device for preparing the defluorinating agent by bipolar membrane acidogenesis according to claim 1, wherein the third reaction tank (33) is connected to the mixing tank (6) through a third filter (43) and a third storage tank (53) in sequence.
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