CN117286513A - Microgram-grade alkali preparation process based on industrial wastewater electrolysis - Google Patents
Microgram-grade alkali preparation process based on industrial wastewater electrolysis Download PDFInfo
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- 239000010842 industrial wastewater Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 239000003513 alkali Substances 0.000 title claims abstract description 40
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 40
- 239000003792 electrolyte Substances 0.000 claims abstract description 49
- 238000001035 drying Methods 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 23
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000004065 wastewater treatment Methods 0.000 claims abstract description 14
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001948 sodium oxide Inorganic materials 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 285
- 239000012535 impurity Substances 0.000 claims description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 29
- 238000005406 washing Methods 0.000 claims description 25
- 239000011347 resin Substances 0.000 claims description 23
- 229920005989 resin Polymers 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 22
- 239000003957 anion exchange resin Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 21
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 19
- 150000002500 ions Chemical class 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000010926 purge Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- 238000004364 calculation method Methods 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 239000013557 residual solvent Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 6
- 230000007423 decrease Effects 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000011328 necessary treatment Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 238000006479 redox reaction Methods 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 239000003344 environmental pollutant Substances 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 239000008188 pellet Substances 0.000 claims description 3
- 231100000719 pollutant Toxicity 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 88
- 239000002351 wastewater Substances 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 7
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000012670 alkaline solution Substances 0.000 description 4
- 239000012267 brine Substances 0.000 description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- -1 chlorine ions Chemical class 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/34—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis
- C25B1/46—Simultaneous production of alkali metal hydroxides and chlorine, oxyacids or salts of chlorine, e.g. by chlor-alkali electrolysis in diaphragm cells
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/04—Combinations of filters with settling tanks
- B01D36/045—Combination of filters with centrifugal separation devices
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/28—Purification; Separation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/28—Purification; Separation
- C01D1/30—Purification; Separation by crystallisation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/28—Purification; Separation
- C01D1/32—Purification; Separation by absorption or precipitation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/44—Preparation in the form of granules, pieces, or other shaped products
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/50—Processes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B15/00—Operating or servicing cells
- C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
- C25B15/085—Removing impurities
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses a preparation process of microgram-grade alkali based on industrial wastewater electrolysis, which comprises the steps of preparing raw materials, preparing ion exchange resins, treating industrial wastewater, preparing electrolyte, preparing electrolysis, drying and purifying, drying and mixing to dissolve, wherein the raw materials are prepared for preparing an electrolytic tank and electrolyzing and alkali-preparing articles, the ion exchange resins are used for improving the purity of sodium oxide, the industrial wastewater treatment and the electrolyte preparation are matched for preparing the electrolyte to save water resources, the drying and purifying are used for saving the time of a process flow, and the purifying, drying and mixing and dissolving are matched for improving the quality of microgram-grade alkali.
Description
Technical Field
The invention relates to the technical field of microgram-scale alkali preparation processes, in particular to an industrial wastewater electrolysis-based microgram-scale alkali preparation process.
Background
The preparation process of the microgram-grade alkali is characterized in that industrial wastewater is used as electrolyte, sodium hydroxide with certain purity is used as solvent to prepare microgram-grade alkaline solution, a large amount of water is needed to be used as electrolyte for the alkaline solution, and the preparation process of the microgram-grade alkali based on industrial wastewater electrolysis can save water resources by using the treated industrial wastewater as electrolyte.
The existing microgram-scale alkali preparation process has the following defects:
1. in JP2000064074a, an electrolytic alkali production process and an electrolytic cell are disclosed, mainly considering how to avoid occurrence of a pressure difference between an upper portion and a lower portion of a gas diffusion electrode mounted on a vertical electrolytic cell, and to avoid problems of liquid leakage from a cathode chamber to a gas chamber of the lower portion and gas leakage from the upper portion to an electrolyte side, and not considering how to use industrial wastewater as an electrolyte, a problem of water resource waste;
2. in patent document SU01411353A1, an alkali production method is disclosed, mainly considering how to eliminate the problem of using a scarce material so as to reduce the cost of the process, and not considering how to increase the concentration of sodium hydroxide produced;
3. in patent document CN107022770B, a process system and a method for preparing alkali by using a high-nitrate brine full-halogen ion membrane are disclosed, mainly considering how to refine and denitrate the high-nitrate brine, directly obtaining refined brine, and being used for preparing alkali by using an ion membrane, but not considering how to improve the drying speed and save the preparation time;
4. patent document CN102851684B discloses a full brine mechanical vapor recompression process for preparing alkali, mainly considering how to realize the problems of low cost, low energy consumption and long service life of equipment, but not how to improve quality of preparing alkali in microgram scale.
Disclosure of Invention
The invention aims to provide a microgram-grade alkali preparation process based on industrial wastewater electrolysis, which aims to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: the preparation process comprises the steps of preparing raw materials, preparing ion exchange resins, treating industrial wastewater, preparing electrolyte, preparing electrolysis, drying, purifying, drying and mixing for dissolving, wherein the raw materials are prepared for preparing electrolytic tanks and electrolysis and alkali preparation articles, the ion exchange resins are used for improving the purity of sodium oxide, the industrial wastewater treatment and the electrolyte preparation are matched for preparing electrolyte to save water resources, the drying and purifying are used for saving the time of a process flow, and the purification, drying and the mixing for dissolving are matched for improving the quality of the microgram-grade alkali;
the industrial wastewater treatment needs to adopt the following necessary treatment methods:
(1) Precipitating;
(2) Filtering;
(3) Centrifuging;
electrolyte preparation is needed after the industrial wastewater treatment is completed, the treated industrial wastewater is needed to be added into an electrolytic tank during the electrolyte preparation, and then NaOH solids are slowly added into the treated industrial wastewater to form a solution to be used as electrolyte;
the preparation process of the microgram-scale alkali preparation based on industrial wastewater electrolysis comprises the following steps:
step S1, raw material preparation: preparing and treating industrial wastewater, and preparing NaOH solids as raw materials;
step S2, preparing ion exchange resin: selecting anion exchange resin, and pre-treating the anion exchange resin;
step S3, industrial wastewater treatment: collecting industrial wastewater and carrying out necessary treatment;
step S4, preparing electrolyte: slowly adding NaOH solid into a solution formed in the treated industrial wastewater, uniformly stirring, and heating the solution to improve the reaction rate and the solubility of NaOH;
step S5, electrolytic preparation: flowing electrolyte through an electrolytic cell, and applying a voltage;
step S6, drying and purifying: firstly separating a precipitate generated by electrolysis in electrolyte from a solution by a membrane separation method, concentrating the separated solution, and finally blowing and drying a concentrated product by using nitrogen with a concentration of 300 sccm;
step S7, purifying and drying: (1) dissolving, (2) filtering, (3) cooling crystallization, (4) filtering and washing, and (5) drying;
step S8, mixing and dissolving: grinding the purified and dried NaOH into powder, and gradually adding the powder into water to be stirred and dissolved.
Preferably, in the step S2, the method further includes the following steps:
step S21, washing and activating before pretreatment of anion exchange resin;
washing: washing out impurities remained on the resin by using a washing liquid, so as to ensure that all ion impurities adsorbed on the resin are removed;
activating: the ion exchange resin was sufficiently immersed in an HCl solution having a concentration of 1M (mol/l) for 2 hours to remove impurities and ions adsorbed on the resin.
Preferably, in the step S3, the method further includes the following steps:
step S31, (1) precipitation: precipitating suspended matters in the industrial wastewater to the bottom through the action of gravity;
(2) And (3) filtering: the suspension is trapped by using a filter medium of a combination of filter paper and activated carbon;
(3) And (3) centrifuging: the suspension is separated off by centrifugal force.
Preferably, in the step S4, the method further includes the following steps:
s41, adding the treated industrial wastewater into an electrolytic tank, slowly adding NaOH solids into the treated industrial wastewater to form a solution, uniformly stirring the solution, and simultaneously heating the solution to improve the reaction rate and the solubility, so that acidic or alkaline substances in the NaOH are subjected to neutralization reaction, and the pH value is between 6.5 and 7.5, and using the solution as an electrolyte;
step S42, reaction of NaOH dissolution in water:
NaOH+H2O→Na++OH-。
preferably, in the step S5, the method further includes the following steps:
step S51, the electrolyte flows through an electrolytic tank, and voltage is applied to enable Cl & lt- & gt in the electrolyte to undergo oxidation-reduction reaction with water molecules, wherein a specific reaction equation is as follows:
2Cl-+2H2O->Cl2+H2+2OH-
generating Cl2 and NaOH to form a solution containing NaOH and ionic impurities;
the following molar mass calculation formula is used:
M＝g÷mol
calculating the molar mass and the molar quantity of each chemical substance;
step S52, inserting the prepared anion exchange resin into an electrolytic bath, and enabling the solution to be in contact with the resin for 2 hours;
the time for the solution to contact the resin was calculated from the following equation:
r＝Δ[c]/Δt；
assuming that the concentration of reactant A in the chemical reaction decreases from 0.1mol/L to 0.05mol/L and this change occurs within 5 minutes, you can calculate the reaction rate as follows:
Δ[c]＝0.05mol/L-0.1mol/L＝-0.05mol/L
Δt=5 minutes=5/60 hours=1/12 hours
These values are then substituted into the formula:
r=Δ [ c ]/Δt= (-0.05 mol/L)/(1/12 hours) = -0.6 mol/(l·h)
Therefore, the reaction rate was-0.6 mol/(L.h).
Preferably, in the step S6, the method further includes the following steps:
step S61, carrying out precipitation separation after an electrolysis preparation process, standing electrolyte to precipitate part of pollutants in the electrolysis preparation process, separating the precipitate from a solution by using membrane separation, concentrating and agglomerating, heating the separated solution to evaporate a solvent, and concentrating to obtain NaOH particles;
step S62, drying the concentrated NaOH by using a nitrogen purging method of 300sccm to remove the residual solvent.
Preferably, in the step S7, the method further includes the following steps:
step S71, purifying and drying: (1) dissolution: mixing and dissolving NaOH particles in water;
(2) And (3) filtering: separating the solution and the impurities by using filter paper and activated carbon, and removing insoluble impurities to obtain a solution containing NaOH and a small amount of impurities;
(3) Cooling and crystallizing: slowly cooling the solution to a temperature 3 ℃ below room temperature, and re-agglomerating NaOH from the solution along with the temperature decrease to form new NaOH particle blocks;
(4) Filtration and washing: separating the NaOH particle blocks from the residual solution by centrifugal filtration, and then washing the NaOH particle blocks with 96% ethanol;
(5) And (3) drying: the washed NaOH pellet was again dried using a 300 seem nitrogen purge.
Preferably, in the step S8, the method further includes the following steps:
step S81, mixing and dissolving: grinding the purified and dried NaOH into powder, gradually adding the powder into water at normal temperature, and stirring to ensure that the NaOH is fully dissolved, so as to prepare a solution with the NaOH content of 255 mug/L;
step S82, determining how to prepare a solution of a desired concentration by mixing a solution of a concentration with a proper volume of solvent when mixing and dissolving, is calculated using the following formula:
it is derived how much initial solution and how much solvent is needed to prepare the desired solution.
Preferably, in the step S51, the method further includes the steps of:
step S53, the following calculation is performed assuming that 1 gram of hydrogen is calculated in terms of the molar quantity using the formula:
mol＝g÷g/mol
hydrogen has a molar mass of about 1g/mol for each of the two hydrogen atoms and a molar mass of about 2g/mol for hydrogen (H2);
mol＝1g/2g/mol＝0.5mol
therefore, there is 1 gram of hydrogen, then it contains about 0.5 mole of hydrogen molecules.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention collects industrial wastewater during raw material preparation, precipitates suspended matters at the bottom of the collected industrial wastewater through the action of gravity, filters the industrial wastewater by utilizing filter paper and active carbon, traps the precipitated suspended matters to clear the wastewater, separates residual suspended matters in the filtered industrial wastewater by utilizing centrifugal force, further treats and removes suspended matters, color, peculiar smell and most of impurities in the industrial wastewater, then adds the treated industrial wastewater into an electrolytic tank, slowly adds NaOH solid into the wastewater to form a solution, uniformly stirs the solution, and heats the solution to neutralize acidic or alkaline matters in the wastewater to react so that the PH value of the wastewater is between 6.5 and 7.5 for being used as electrolyte, thereby realizing reutilization of the industrial wastewater and saving water resources.
2. The method comprises the steps of preparing anion exchange resin to remove chloride Cl < - > as anions when raw materials are prepared, firstly washing the prepared anion exchange resin by using a washing liquid to wash away impurities remained on the anion exchange resin, ensuring that all the ion impurities adsorbed on the resin are removed, then fully soaking the ion exchange resin in hydrochloric acid (HCl) solution with the concentration of 1M (mol/L) for 2 hours to remove the impurities and ions adsorbed on the resin, then inserting the ion exchange resin into an electrolytic tank after the electrolytic process, and contacting the solution with the resin for 2 hours to ensure that the resin adsorbs the ion impurities without adsorbing NaOH, thereby improving the purity of NaOH solution prepared after the electrolytic process.
3. According to the invention, ion exchange resin is inserted into an electrolytic tank to adsorb ion impurities, and a 300sccm nitrogen purging method is used for drying concentrated NaOH particle blocks to remove residual solvent, and then the dissolved, filtered, cooled, crystallized and filtered and washed NaOH particle blocks are purged again by using 300sccm nitrogen, so that the NaOH particle blocks are accelerated to be dried, the drying speed is improved, and the time of a drying process is saved.
4. The invention inserts ion exchange resin into an electrolytic tank to adsorb ion impurities, and dries the concentrated NaOH particle blocks by using a 300sccm nitrogen purging method to remove residual solvent, then dissolves the NaOH particle blocks in water, separates undissolved impurities or sediment from the solution in the dissolving process, slowly cools the solution generated by dissolving to a temperature lower than 3 ℃ of room temperature to enable NaOH to agglomerate again from the solution to form new NaOH particle blocks, finally grinds the formed new NaOH particle blocks into powder, gradually adds the powder into water and stirs the powder to ensure full dissolution, and prepares an alkaline solution with the content of 255 mug/L, thereby enabling the quality of the prepared microgram-grade alkali and the solution to be higher.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a flow chart of an industrial wastewater treatment process of the present invention;
FIG. 3 is a flow chart of ion exchange resin preparation according to the present invention;
FIG. 4 is a flow chart of the electrolytic preparation and purification drying process of the present invention;
FIG. 5 is a table of chemical formulas of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment one:
referring to fig. 1, 2 and 3, a process for preparing microgram-scale alkali based on industrial wastewater electrolysis comprises preparing raw materials, preparing ion exchange resin, treating industrial wastewater, preparing electrolyte, preparing electrolysis, drying, purifying, drying and mixing for dissolving, wherein the raw materials are prepared for preparing an electrolytic tank and electrolysis and alkali-preparing articles, the ion exchange resin is used for improving the purity of sodium oxide, the industrial wastewater treatment and the electrolyte preparation are matched for preparing electrolyte to save water resources, the drying and purifying are used for saving process flow time, and the purification, drying and mixing for dissolving are matched for improving the quality of microgram-scale alkali;
the industrial wastewater treatment needs to adopt the following necessary treatment methods:
(1) Precipitating;
(2) Filtering;
(3) Centrifuging;
further, electrolyte preparation is needed after the industrial wastewater treatment is completed, the treated industrial wastewater is needed to be added into an electrolytic tank during the electrolyte preparation, and then NaOH solids are slowly added into the treated industrial wastewater to form a solution to be used as electrolyte;
embodiment two:
referring to fig. 1, 2 and 3, a process for preparing microgram-scale alkali based on industrial wastewater electrolysis,
the preparation process of the microgram-scale alkali preparation based on industrial wastewater electrolysis comprises the following steps:
step S1, raw material preparation: preparing and treating industrial wastewater, and preparing NaOH solids as raw materials;
step S2, preparing ion exchange resin: selecting anion exchange resin, and pre-treating the anion exchange resin;
step S3, industrial wastewater treatment: collecting industrial wastewater and carrying out necessary treatment;
the step S3 further includes the following steps:
step S31, (1) precipitation: precipitating suspended matters in the industrial wastewater to the bottom through the action of gravity;
(2) And (3) filtering: the suspension is trapped by using a filter medium of a combination of filter paper and activated carbon;
(3) And (3) centrifuging: the suspension is separated off by centrifugal force.
Step S4, preparing electrolyte: slowly adding NaOH solid into a solution formed in the treated industrial wastewater, uniformly stirring, and heating the solution to improve the reaction rate and the solubility of NaOH;
preferably, in the step S4, the method further includes the following steps:
s41, adding the treated industrial wastewater into an electrolytic tank, slowly adding NaOH solids into the treated industrial wastewater to form a solution, uniformly stirring the solution, and simultaneously heating the solution to improve the reaction rate and the solubility, so that acidic or alkaline substances in the NaOH are subjected to neutralization reaction, and the pH value is between 6.5 and 7.5, and using the solution as an electrolyte;
step S42, reaction of NaOH dissolution in water:
NaOH+H2O→Na++OH-。
step S5, electrolytic preparation: flowing electrolyte through an electrolytic cell, and applying a voltage;
step S6, drying and purifying: firstly separating a precipitate generated by electrolysis in electrolyte from a solution by a membrane separation method, concentrating the separated solution, and finally blowing and drying a concentrated product by using nitrogen with a concentration of 300 sccm;
step S7, purifying and drying: (1) dissolving, (2) filtering, (3) cooling crystallization, (4) filtering and washing, and (5) drying;
step S8, mixing and dissolving: grinding the purified and dried NaOH into powder, and gradually adding the powder into water to be stirred and dissolved.
Further, collecting industrial wastewater during raw material preparation, precipitating suspended matters in the industrial wastewater to the bottom, filtering the industrial wastewater by using filter paper and activated carbon, intercepting the precipitated suspended matters, separating residual suspended matters by using centrifugal force, further treating and removing suspended matters, colors, peculiar smell and most of impurities in the industrial wastewater, adding the treated industrial wastewater into an electrolytic tank, slowly adding NaOH solid into the wastewater, stirring uniformly to form a solution, and heating the solution to neutralize acidic or alkaline matters in the wastewater to react so that the PH value of the wastewater is between 6.5 and 7.5 for being used as electrolyte, thereby realizing reutilization of the industrial wastewater and saving water resources.
Embodiment III:
referring to fig. 1 and 2, a process for preparing a microgram-scale alkali based on electrolysis of industrial wastewater, in the step S2, further includes the following steps:
step S21, washing and activating before pretreatment of anion exchange resin;
washing: washing out impurities remained on the resin by using a washing liquid, so as to ensure that all ion impurities adsorbed on the resin are removed;
activating: fully soaking the ion exchange resin in HCl solution with the concentration of 1M (mol/L) for 2 hours to remove impurities and ions adsorbed on the resin;
concentration calculation formula:
wherein C represents concentration, typically expressed in units of mol/L, represents the molar amount of solute in the solution per liter of solution, n represents the molar amount, expressed in units of mol, represents the molar amount of solute in the solution, V represents volume, expressed in units of L, represents the total volume of the solution;
this formula is used to calculate the concentration of the solution, i.e., the molar concentration of the solute in the solution, and the concentration C can be obtained by dividing the molar quantity n of the solute by the total volume V of the solution;
then the washed and activated anion exchange resin is inserted into an electrolytic tank, so that the solution is contacted with the anion exchange resin, and the anion exchange resin adsorbs ion impurities;
step S52, inserting the prepared anion exchange resin into an electrolytic bath, and enabling the solution to be in contact with the resin for 2 hours;
the time for the solution to contact the resin was calculated from the following equation:
r＝Δ[c]/Δt；
assuming that the concentration of reactant A in the chemical reaction decreases from 0.1mol/L to 0.05mol/L and this change occurs within 5 minutes, you can calculate the reaction rate as follows:
Δ[c]＝0.05mol/L-0.1mol/L＝-0.05mol/L
Δt=5 minutes=5/60 hours=1/12 hours
These values are then substituted into the formula:
r=Δ [ c ]/Δt= (-0.05 mol/L)/(1/12 hours) = -0.6 mol/(l·h)
Therefore, the reaction rate was-0.6 mol/(L.h).
Further, when preparing raw materials, preparing anion exchange resin to remove chloride ion Cl < - >, firstly, washing the prepared anion exchange resin by using a washing liquid to wash away impurities remained on the anion exchange resin, ensuring that all the ion impurities adsorbed on the resin are removed, then fully soaking the ion exchange resin in hydrochloric acid (HCl) solution with the concentration of 1M (mol/L) for 2 hours to remove the impurities and ions adsorbed on the resin, then inserting the ion exchange resin into an electrolytic tank after the electrolytic process is carried out, enabling the solution to contact the resin for 2 hours, enabling the resin to adsorb the ion impurities without adsorbing NaOH, and further improving the purity of NaOH solution prepared after the electrolytic process.
Embodiment four:
referring to fig. 1 and 2, in the step S5, a process for preparing a microgram-scale alkali based on electrolysis of industrial wastewater further includes the following steps:
step S51, the electrolyte flows through an electrolytic tank, and voltage is applied to enable Cl & lt- & gt in the electrolyte to undergo oxidation-reduction reaction with water molecules, wherein a specific reaction equation is as follows:
2Cl-+2H2O->Cl2+H2+2OH-
chlorine ions (Cl-) in the wastewater generate oxidation-reduction reaction with water molecules to generate chlorine (Cl 2) and sodium hydroxide (NaOH)
Further: generating Cl2 and NaOH to form a solution containing NaOH and ionic impurities;
the following molar mass calculation formula is used:
M＝g÷mol
the molar mass and the molar quantity of each chemical were calculated.
Fifth embodiment:
referring to fig. 1 and 2, a process for preparing a microgram-scale alkali based on electrolysis of industrial wastewater, in the step S6, further includes the following steps:
step S61, carrying out precipitation separation after an electrolysis preparation process, standing electrolyte to precipitate part of pollutants in the electrolysis preparation process, separating the precipitate from a solution by using membrane separation, concentrating and agglomerating, heating the separated solution to evaporate a solvent, and concentrating to obtain NaOH particles;
step S62, drying the concentrated NaOH by using a nitrogen purging method of 300sccm to take out residual solvent;
the step S7 further includes the following steps:
step S71, purifying and drying: (1) dissolution: mixing and dissolving NaOH particles in water;
(2) And (3) filtering: separating the solution and the impurities by using filter paper and activated carbon, and removing insoluble impurities to obtain a solution containing NaOH and a small amount of impurities;
(3) Cooling and crystallizing: slowly cooling the solution to a temperature 3 ℃ below room temperature, and re-agglomerating NaOH from the solution along with the temperature decrease to form new NaOH particle blocks;
(4) Filtration and washing: separating the NaOH particle blocks from the residual solution by centrifugal filtration, and then washing the NaOH particle blocks with 96% ethanol;
(5) And (3) drying: the washed NaOH pellet was again dried using a 300 seem nitrogen purge.
And further, the ion exchange resin is inserted into an electrolytic tank to adsorb ion impurities, the concentrated NaOH particle blocks are dried by a 300sccm nitrogen purging method to remove residual solvent, and then the dissolved, filtered, cooled, crystallized and filtered and washed NaOH particle blocks are purged again by the 300sccm nitrogen, so that the NaOH particle blocks are accelerated to be dried, the drying speed is improved, and the time of a drying process is saved.
The step S8 further includes the following steps:
step S81, mixing and dissolving: grinding the purified and dried NaOH into powder, gradually adding the powder into water at normal temperature, and stirring to ensure that the NaOH is fully dissolved, so as to prepare a solution with the NaOH content of 255 mug/L;
step S82, determining how to prepare a solution of a desired concentration by mixing a solution of a concentration with a proper volume of solvent when mixing and dissolving, is calculated using the following formula:
c1 represents the concentration of the initial solution, i.e. the concentration of the solution you already have;
v1 represents the volume of the initial solution, i.e. the volume of solution you already have;
c2 represents the final desired solution concentration, i.e. the target concentration you want to prepare;
v2 represents the final required volume of solution, i.e. the total volume of solution you intend to prepare;
assume that: with an initial concentration of C1, a volume of V2 of the solution of target concentration of C2 is prepared, and can be usedEquations to calculate how much initial solution and how much solvent is needed to prepare the desired solution;
it is derived how much initial solution and how much solvent is needed to prepare the desired solution.
Further, ion exchange resin is inserted into an electrolytic tank to absorb ion impurities, the concentrated NaOH particle blocks are dried by a nitrogen purging method of 300sccm to remove residual solvent, then the NaOH particle blocks are dissolved in water, insoluble impurities or precipitates in the dissolving process are separated from the solution, the solution generated by dissolving is slowly cooled to a temperature lower than room temperature by 3 ℃ to enable NaOH to be agglomerated again from the solution to form new NaOH particle blocks, finally the formed new NaOH particle blocks are ground into powder, the powder is gradually added into water and stirred to ensure full dissolution, and an alkaline solution with the content of 255 mug/L is prepared, so that the quality of the prepared microgram-grade alkali and solution can be higher.
Example six:
referring to fig. 1 and 2, in the step S51, a process for preparing a microgram-scale alkali based on electrolysis of industrial wastewater further includes the following steps:
step S53, the following calculation is performed assuming that 1 gram of hydrogen is calculated in terms of the molar quantity using the formula:
mol＝g÷g/mol
hydrogen has a molar mass of about 1g/mol for each of the two hydrogen atoms and a molar mass of about 2g/mol for hydrogen (H2);
mol＝1g/2g/mol＝0.5mol
therefore, there is 1 gram of hydrogen, then it contains about 0.5 mole of hydrogen molecules.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. The preparation process of the microgram-scale alkali preparation based on the electrolysis of industrial wastewater is characterized by comprising the following steps of: the method comprises the steps of preparing raw materials, preparing ion exchange resin, treating industrial wastewater, preparing electrolyte, preparing electrolysis, drying, purifying, drying and mixing for dissolving, wherein the raw materials are prepared for preparing an electrolytic tank and electrolysis and alkali-making articles, the ion exchange resin is used for improving the purity of sodium oxide, the industrial wastewater treatment and the electrolyte preparation are matched for preparing the electrolyte to save water resources, the drying and purifying are used for saving process flow time, and the purification, drying, mixing and dissolving are matched for improving the quality of microgram-grade alkali;
the industrial wastewater treatment needs to adopt the following necessary treatment methods:
(1) Precipitating;
(2) Filtering;
(3) Centrifuging;
electrolyte preparation is needed after the industrial wastewater treatment is completed, the treated industrial wastewater is needed to be added into an electrolytic tank during the electrolyte preparation, and then NaOH solids are slowly added into the treated industrial wastewater to form a solution to be used as electrolyte;
the preparation process of the microgram-scale alkali preparation based on industrial wastewater electrolysis comprises the following steps:
step S1, raw material preparation: preparing and treating industrial wastewater, and preparing NaOH solids as raw materials;
step S2, preparing ion exchange resin: selecting anion exchange resin, and pre-treating the anion exchange resin;
step S3, industrial wastewater treatment: collecting industrial wastewater and carrying out necessary treatment;
step S4, preparing electrolyte: slowly adding NaOH solid into a solution formed in the treated industrial wastewater, uniformly stirring, and heating the solution to improve the reaction rate and the solubility of NaOH;
step S5, electrolytic preparation: flowing electrolyte through an electrolytic cell, and applying a voltage;
step S6, drying and purifying: firstly separating a precipitate generated by electrolysis in electrolyte from a solution by a membrane separation method, concentrating the separated solution, and finally blowing and drying a concentrated product by using nitrogen with a concentration of 300 sccm;
step S7, purifying and drying: (1) dissolving, (2) filtering, (3) cooling crystallization, (4) filtering and washing, and (5) drying;
step S8, mixing and dissolving: grinding the purified and dried NaOH into powder, and gradually adding the powder into water to be stirred and dissolved.
2. The process for preparing the microgram-scale alkali based on the electrolysis of industrial wastewater according to claim 1, which is characterized in that: the step S2 further includes the following steps:
step S21, washing and activating before pretreatment of anion exchange resin;
washing: washing out impurities remained on the resin by using a washing liquid, so as to ensure that all ion impurities adsorbed on the resin are removed;
activating: the ion exchange resin was sufficiently immersed in an HCl solution having a concentration of 1M (mol/l) for 2 hours to remove impurities and ions adsorbed on the resin.
3. The process for preparing the microgram-scale alkali based on the electrolysis of industrial wastewater according to claim 1, which is characterized in that: the step S3 further includes the following steps:
step S31, (1) precipitation: precipitating suspended matters in the industrial wastewater to the bottom through the action of gravity;
(2) And (3) filtering: the suspension is trapped by using a filter medium of a combination of filter paper and activated carbon;
(3) And (3) centrifuging: the suspension is separated off by centrifugal force.
4. The process for preparing the microgram-scale alkali based on the electrolysis of industrial wastewater according to claim 1, which is characterized in that: the step S4 further includes the following steps:
s41, adding the treated industrial wastewater into an electrolytic tank, slowly adding NaOH solids into the treated industrial wastewater to form a solution, uniformly stirring the solution, and simultaneously heating the solution to improve the reaction rate and the solubility, so that acidic or alkaline substances in the NaOH are subjected to neutralization reaction, and the pH value is between 6.5 and 7.5, and using the solution as an electrolyte;
step S42, reaction of NaOH dissolution in water:
NaOH+H2O→Na++OH-。
5. the process for preparing the microgram-scale alkali based on the electrolysis of industrial wastewater according to claim 1, which is characterized in that: the step S5 further includes the following steps:
step S51, the electrolyte flows through an electrolytic tank, and voltage is applied to enable Cl & lt- & gt in the electrolyte to undergo oxidation-reduction reaction with water molecules, wherein a specific reaction equation is as follows:
2Cl-+2H2O->Cl2+H2+2OH-
generating Cl2 and NaOH to form a solution containing NaOH and ionic impurities;
the following molar mass calculation formula is used:
M＝g÷mol
calculating the molar mass and the molar quantity of each chemical substance;
step S52, inserting the prepared anion exchange resin into an electrolytic bath, and enabling the solution to be in contact with the resin for 2 hours;
the time for the solution to contact the resin was calculated from the following equation:
r＝Δ[c]/Δt；
assuming that the concentration of reactant A in the chemical reaction decreases from 0.1mol/L to 0.05mol/L and this change occurs within 5 minutes, you can calculate the reaction rate as follows:
Δ[c]＝0.05mol/L-0.1mol/L＝-0.05mol/L
Δt=5 minutes=5/60 hours=1/12 hours
These values are then substituted into the formula:
r=Δc/Δt= (-0.05 mol/L)/(1/12 hours) = -0.6 mol/(l·h) so the reaction rate is-0.6 mol/(l·h).
6. The process for preparing the microgram-scale alkali based on the electrolysis of industrial wastewater according to claim 1, which is characterized in that: the step S6 further includes the following steps:
step S61, carrying out precipitation separation after an electrolysis preparation process, standing electrolyte to precipitate part of pollutants in the electrolysis preparation process, separating the precipitate from a solution by using membrane separation, concentrating and agglomerating, heating the separated solution to evaporate a solvent, and concentrating to obtain NaOH particles;
step S62, drying the concentrated NaOH by using a nitrogen purging method of 300sccm to remove the residual solvent.
7. The process for preparing the microgram-scale alkali based on the electrolysis of industrial wastewater as claimed in claim 6, which is characterized in that: the step S7 further includes the following steps:
step S71, purifying and drying: (1) dissolution: mixing and dissolving NaOH particles in water;
(2) And (3) filtering: separating the solution and the impurities by using filter paper and activated carbon, and removing insoluble impurities to obtain a solution containing NaOH and a small amount of impurities;
(3) Cooling and crystallizing: slowly cooling the solution to a temperature 3 ℃ below room temperature, and re-agglomerating NaOH from the solution along with the temperature decrease to form new NaOH particle blocks;
(4) Filtration and washing: separating the NaOH particle blocks from the residual solution by centrifugal filtration, and then washing the NaOH particle blocks with 96% ethanol;
(5) And (3) drying: the washed NaOH pellet was again dried using a 300 seem nitrogen purge.
8. The process for preparing the microgram-scale alkali based on the electrolysis of industrial wastewater as claimed in claim 7, which is characterized in that: the step S8 further includes the following steps:
step S81, mixing and dissolving: grinding the purified and dried NaOH into powder, gradually adding the powder into water at normal temperature, and stirring to ensure that the NaOH is fully dissolved, so as to prepare a solution with the NaOH content of 255 mug/L;
step S82, determining how to prepare a solution of a desired concentration by mixing a solution of a concentration with a proper volume of solvent when mixing and dissolving, is calculated using the following formula:
it is derived how much initial solution and how much solvent is needed to prepare the desired solution.
9. The process for preparing the microgram-scale alkali based on the electrolysis of the industrial wastewater, which is disclosed in claim 5, is characterized in that: in the step S51, the method further includes the steps of:
step S53, the following calculation is performed assuming that 1 gram of hydrogen is calculated in terms of the molar quantity using the formula:
mol＝g÷g/mol
hydrogen has a molar mass of about 1g/mol for each of the two hydrogen atoms and a molar mass of about 2g/mol for hydrogen (H2);
mol＝1g/2g/mol＝0.5mol
therefore, there is 1 gram of hydrogen, then it contains about 0.5 mole of hydrogen molecules.
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