CN112708901A - Method for comprehensively utilizing salt lake brine with high added value - Google Patents
Method for comprehensively utilizing salt lake brine with high added value Download PDFInfo
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- CN112708901A CN112708901A CN202110108119.0A CN202110108119A CN112708901A CN 112708901 A CN112708901 A CN 112708901A CN 202110108119 A CN202110108119 A CN 202110108119A CN 112708901 A CN112708901 A CN 112708901A
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- 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
- C25B1/18—Alkaline earth metal compounds or magnesium compounds
- C25B1/20—Hydroxides
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- 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
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- 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
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- 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
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
A method for comprehensively utilizing salt lake brine with high added value comprises the following steps: (1) preparing a brine solution with a certain concentration; (2) assembling a direct current electrolysis device; (3) a diaphragm device is arranged in the cathode chamber; (4) adding an organic solution into the cathode chamber, and then electrifying direct current to electrolyze; (5) ultrasonically dispersed anode and cathode (excluding products facing the anode portion) products; (6) standing and layering to obtain an anode product A, a cathode product C and a cathode precipitate product B; (7) and drying to obtain graphene products A and C and a magnesium hydroxide/graphene composite product B which adsorb different ions. The method for comprehensively utilizing the salt lake brine with high added value provided by the invention solves the problem of comprehensive utilization of the salt lake brine. The method can directly use salt lake brine as a raw material, can simultaneously produce magnesium hydroxide/graphene compound, graphene for adsorbing cations, graphene for adsorbing anions, hydrogen and chlorine in the same device, can comprehensively utilize valuable elements in the brine, can obtain various products with high added values, and is simple in process, easy to process by the device and suitable for industrial large-scale production.
Description
Technical Field
The invention belongs to the technical field of salt chemical engineering, and particularly relates to a method for comprehensively utilizing salt lake brine with high added value.
Background
The main components of the salt lake brine are salifying elements such as alkali metal, alkaline earth metal, halogen and the like. The salt lake brine in China contains more than 60 chemical components, and mainly comprises main chemical elements such as sodium, potassium, magnesium, lithium, chlorine, sulfate, borate and the like and acid radicals. For a long time, because of the problems of technical economy and the like, magnesium resources cannot be put into large-scale industrial production, a large amount of brine discharged in the process of potassium recovery still cannot be commercially developed and utilized in a large scale, and even salt lake components are changed to cause disasters. Taking the Qinghai salt lake as an example, the salt lake produces about 50 ten thousand tons of potassium chloride every year, and each 1 ton of potassium chloride produces 10-12 tons of magnesium chloride as a byproduct, wherein various valuable elements are added, and the valuable elements are not reasonably utilized. Therefore, the comprehensive utilization of various resources must be considered in the development of brine mine, and the problems of low economic benefit, serious resource waste, tailing (old brine) treatment, resource and environment protection and the like caused by single product are very urgent to solve.
Based on the problems, the invention provides a method for comprehensively utilizing salt lake brine with high added value. The method can directly use salt lake brine as a raw material, can simultaneously produce magnesium hydroxide/graphene compound, graphene for adsorbing cations, graphene for adsorbing anions, hydrogen and chlorine in the same device, can comprehensively utilize valuable elements in the brine, can obtain various products with high added values, and is simple in process, easy to process by the device and suitable for industrial large-scale production.
Disclosure of Invention
A method for comprehensively utilizing salt lake brine with high added value is characterized by comprising the following steps:
(1) preparing a brine solution with a certain concentration: dissolving solid or liquid salt lake brine by using a certain amount of deionized water, removing insoluble solid substances by filtering, and preparing filtrate into a solution with the concentration of 1-30%;
(2) assembling a direct current electrolysis device: graphite is used as an anode, and graphite is used as a cathode; the two electrode plates are respectively connected with the positive electrode and the negative electrode of the direct current power supply through leads; a diaphragm is arranged between the anode plate and the cathode plate and divides the electrolytic cell into an anode chamber and a cathode chamber;
(3) a diaphragm device is arranged in the cathode chamber: a diaphragm is arranged under a cathode electrode of the cathode chamber, and divides the cathode into a part facing to the anode and a part back to the anode;
(4) and D, electrifying direct current for electrolysis: adding the prepared brine solution into an electrolytic cell, simultaneously adding a certain mass of organic solution into a cathode chamber, switching on a direct current power supply, controlling the current density between two polar plates to be 0.1-4A/cm 2 to carry out constant voltage electrolysis, obtaining chlorine at an anode, and obtaining hydrogen at a cathode;
(5) ultrasonic dispersion: performing ultrasonic dispersion on products obtained by an anode and a cathode (excluding products facing the anode), wherein the ultrasonic power is 10-100 kHz, and the dispersion time is 5-60 min;
(6) standing and layering: standing the ultrasonically dispersed anode product A, the cathode product B facing the anode part and the product C facing away from the cathode part for 1-120 min respectively, and performing vacuum filtration to obtain a precipitate A, a precipitate B and a precipitate C respectively;
(7) and (3) drying: drying the precipitate A and the precipitate C for 60-360 min from-40-120 ℃ by a freeze dryer through programmed heating, wherein the programmed heating rate is 1-10 ℃/min, and obtaining graphene products A and C which adsorb different ions; and drying the precipitate B for 60-360 min at a constant temperature of 80-120 ℃ through an oven to obtain a magnesium hydroxide/graphene composite product B.
The brine is selected from seawater liquid brine, seawater solid brine, salt lake liquid brine or salt lake solid brine.
The graphite anode and cathode materials are highly oriented pyrolytic graphite, graphite foil, crystalline flake graphite or porous graphite electrodes.
The diaphragm material is selected from a polypropylene membrane, a cation exchange membrane or a polytetrafluoroethylene membrane.
The diaphragm material is organic glass diaphragm, conductive glass diaphragm or cation exchange membrane.
The added organic solution is selected from propylene carbonate, dimethyl sulfoxide, tetrahydrofuran or a mixture thereof.
And the anode chamber is internally provided with a cathode chamber, the cathode chamber is internally provided with a cathode chamber, the anode chamber is internally provided with an anode and a cathode chamber, the cathode chamber is internally provided with a cathode chamber, the anode chamber is internally provided with a cathode chamber, the cathode chamber is internally provided.
The graphene product for adsorbing anions in the anode chamber comprises sulfate ions, borate ions, chloride ions and the like, and the graphene product for adsorbing cations in the cathode chamber comprises potassium ions, lithium ions, sodium ions, magnesium ions and the like.
The electrolysis time is 1-12 hours after electrification or the anode plate or the cathode plate finishes the electrolysis after reaction.
The direct current electrolysis temperature is room temperature electrolysis.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention.
The invention has the advantages of
The method for comprehensively utilizing the salt lake brine with high added value provided by the invention solves the problem of comprehensive utilization of the salt lake brine. According to the method, salt lake brine can be directly used as a raw material, and a magnesium hydroxide/graphene compound, graphene for adsorbing cations, graphene for adsorbing anions, hydrogen and chlorine can be simultaneously produced in the same device. The magnesium hydroxide/graphene compound in the generated product is a flame retardant with performance superior to that of magnesium hydroxide; graphene adsorbing cations is a good electrode material; graphene adsorbing anions is a good capacitor material; hydrogen and chlorine are important chemical raw materials. The method can comprehensively utilize valuable elements in the brine, can obtain various products with high added values, has simple process and easy processing of devices, and is suitable for industrial large-scale production.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting. The upper and lower line values and intervals of the process parameters listed in the technical scheme of the invention can realize the products required by the invention.
Example 1
(1) Preparing a brine solution with a certain concentration: dissolving solid or liquid salt lake brine by using a certain amount of deionized water, removing insoluble solid substances by filtering, and preparing filtrate into a solution with the concentration of 10%;
(2) assembling a direct current electrolysis device: taking a graphite foil as an anode and a porous graphite rod as a cathode; the two electrode plates are respectively connected with the positive electrode and the negative electrode of the direct current power supply through leads; a cation exchange diaphragm is arranged between the anode plate and the cathode plate and divides the electrolytic cell into an anode chamber and a cathode chamber;
(3) a diaphragm device is arranged in the cathode chamber: an organic glass diaphragm is arranged under a cathode electrode of the cathode chamber, and the diaphragm divides the cathode into a part facing the anode and a part back to the anode;
(4) and D, electrifying direct current for electrolysis: adding the prepared brine solution into an electrolytic cell, simultaneously adding a certain mass of dimethyl sulfoxide organic solution into a cathode chamber, switching on a direct current power supply, controlling the current density between two polar plates to be 1A/cm2 to carry out constant voltage electrolysis, obtaining chlorine at an anode and hydrogen at a cathode;
(5) ultrasonic dispersion: performing ultrasonic dispersion on products obtained by an anode and a cathode (excluding products facing the anode part), wherein the ultrasonic power is 100kHz, and the dispersion time is 60 min;
(6) standing and layering: standing the ultrasonically dispersed anode product A, the cathode product B facing the anode part and the product C facing away from the cathode part for 60min respectively, and obtaining a precipitate A, a precipitate B and a precipitate C through vacuum filtration respectively;
(7) and (3) drying: drying the precipitate A and the precipitate C for 120min from-40 to 110 ℃ by a freeze dryer through programmed heating, wherein the programmed heating rate is 10 ℃/min, and obtaining graphene products A and C adsorbing different ions; and drying the precipitate B for 120min at constant temperature of 100 ℃ by using an oven to obtain a magnesium hydroxide/graphene composite product B.
Example 2
(1) Preparing a brine solution with a certain concentration: dissolving solid or liquid salt lake brine by using a certain amount of deionized water, removing insoluble solid substances by filtering, and preparing filtrate into a solution with the concentration of 20%;
(2) assembling a direct current electrolysis device: taking a porous graphite rod as an anode and highly-oriented pyrolytic graphite as a cathode; the two electrode plates are respectively connected with the positive electrode and the negative electrode of the direct current power supply through leads; a polytetrafluoroethylene diaphragm is arranged between the anode plate and the cathode plate and divides the electrolytic cell into an anode chamber and a cathode chamber;
(3) a diaphragm device is arranged in the cathode chamber: a cation exchange membrane is arranged under a cathode electrode of the cathode chamber, and the cathode is divided into an anode facing part and an anode back facing part by the cation exchange membrane;
(4) and D, electrifying direct current for electrolysis: adding the prepared brine solution into an electrolytic cell, simultaneously adding a certain mass of propylene carbonate organic solution into a cathode chamber, switching on a direct current power supply, controlling the current density between two polar plates to be 2A/cm2 to carry out constant voltage electrolysis, obtaining chlorine at an anode and hydrogen at a cathode;
(5) ultrasonic dispersion: performing ultrasonic dispersion on products obtained by an anode and a cathode (excluding products facing the anode part), wherein the ultrasonic power is 50kHz, and the dispersion time is 60 min;
(6) standing and layering: standing the ultrasonically dispersed anode product A, the cathode product B facing the anode part and the product C facing away from the cathode part for 100min respectively, and obtaining a precipitate A, a precipitate B and a precipitate C through vacuum filtration respectively;
(7) and (3) drying: drying the precipitate A and the precipitate C for 360min from-40 to 120 ℃ by a freeze dryer through programmed heating, wherein the programmed heating rate is 5 ℃/min, and obtaining graphene products A and C adsorbing different ions; and drying the precipitate B for 120min at constant temperature of 120 ℃ by using an oven to obtain a magnesium hydroxide/graphene composite product B.
Example 3
(1) Preparing a brine solution with a certain concentration: dissolving solid or liquid salt lake brine by using a certain amount of deionized water, removing insoluble solid substances by filtering, and preparing filtrate into a solution with the concentration of 30%;
(2) assembling a direct current electrolysis device: taking highly oriented pyrolytic graphite as an anode and a porous graphite rod as a cathode; the two electrode plates are respectively connected with the positive electrode and the negative electrode of the direct current power supply through leads; a cation exchange diaphragm is arranged between the anode plate and the cathode plate and divides the electrolytic cell into an anode chamber and a cathode chamber;
(3) a diaphragm device is arranged in the cathode chamber: a conductive glass diaphragm is arranged under a cathode electrode of the cathode chamber, and the diaphragm divides the cathode into a part facing the anode and a part back to the anode;
(4) and D, electrifying direct current for electrolysis: adding the prepared brine solution into an electrolytic cell, simultaneously adding a certain mass of propylene carbonate organic solution into a cathode chamber, switching on a direct current power supply, controlling the current density between two polar plates to be 1A/cm2 to carry out constant voltage electrolysis, obtaining chlorine at an anode and hydrogen at a cathode;
(5) ultrasonic dispersion: performing ultrasonic dispersion on products obtained by an anode and a cathode (excluding products facing the anode part), wherein the ultrasonic power is 40kHz, and the dispersion time is 60 min;
(6) standing and layering: standing the ultrasonically dispersed anode product A, the cathode product B facing the anode part and the product C facing away from the cathode part for 60min respectively, and obtaining a precipitate A, a precipitate B and a precipitate C through vacuum filtration respectively;
(7) and (3) drying: drying the precipitate A and the precipitate C for 240min from minus 20 ℃ to 100 ℃ by a freeze dryer through programmed heating, wherein the programmed heating rate is 10 ℃/min, and obtaining graphene products A and C which adsorb different ions; and drying the precipitate B for 120min at constant temperature of 120 ℃ by using an oven to obtain a magnesium hydroxide/graphene composite product B.
Claims (10)
1. A method for comprehensively utilizing salt lake brine with high added value is characterized by comprising the following steps:
(1) preparing a brine solution with a certain concentration: dissolving solid or liquid salt lake brine by using a certain amount of deionized water, removing insoluble solid substances by filtering, and preparing filtrate into a solution with the concentration of 1-30%;
(2) assembling a direct current electrolysis device: graphite is used as an anode, and graphite is used as a cathode; the two electrode plates are respectively connected with the positive electrode and the negative electrode of the direct current power supply through leads; a diaphragm is arranged between the anode plate and the cathode plate and divides the electrolytic cell into an anode chamber and a cathode chamber;
(3) a diaphragm device is arranged in the cathode chamber: a diaphragm is arranged under a cathode electrode of the cathode chamber, and divides the cathode into a part facing to the anode and a part back to the anode;
(4) and D, electrifying direct current for electrolysis: adding the prepared brine solution into an electrolytic cell, simultaneously adding a certain mass of organic solution into a cathode chamber, switching on a direct current power supply, and controlling the current density between two polar plates to be 0.1-4A/cm2Performing constant voltage electrolysis to obtain chlorine at the anode and hydrogen at the cathode;
(5) ultrasonic dispersion: performing ultrasonic dispersion on products obtained by an anode and a cathode (excluding products facing the anode), wherein the ultrasonic power is 10-100 kHz, and the dispersion time is 5-60 min;
(6) standing and layering: standing the ultrasonically dispersed anode product A, the cathode product B facing the anode part and the product C facing away from the cathode part for 1-120 min respectively, and performing vacuum filtration to obtain a precipitate A, a precipitate B and a precipitate C respectively;
(7) and (3) drying: drying the precipitate A and the precipitate C for 60-360 min from-40-120 ℃ by a freeze dryer through programmed heating, wherein the programmed heating rate is 1-10 ℃/min, and obtaining graphene products A and C which adsorb different ions; and drying the precipitate B for 60-360 min at a constant temperature of 80-120 ℃ through an oven to obtain a magnesium hydroxide/graphene composite product B.
2. The method for high value-added comprehensive utilization of salt lake brine according to claim 1, wherein in the step (1), the brine is selected from seawater liquid brine, seawater solid brine, salt lake liquid brine or salt lake solid brine.
3. The method for high value-added comprehensive utilization of salt lake brine according to claim 1, wherein in the step (2), the graphite anode and cathode materials are highly oriented pyrolytic graphite, graphite foil, flake graphite or porous graphite electrodes.
4. The method for comprehensively utilizing salt lake brine with high added value according to claim 1, wherein in the step (2), the diaphragm is made of polypropylene membrane, cation exchange membrane or polytetrafluoroethylene membrane.
5. The method for high value-added comprehensive utilization of salt lake brine according to claim 1, wherein in the step (3), the material of the diaphragm is an organic glass diaphragm, a conductive glass diaphragm or a cation exchange membrane.
6. The method for high value-added comprehensive utilization of salt lake brine according to claim 1, wherein in the step (4), the added organic solution is selected from propylene carbonate, dimethyl sulfoxide, tetrahydrofuran or a mixture thereof.
7. The method for high value-added comprehensive utilization of salt lake brine according to claim 1, wherein in step (4), electrochemical intercalation is performed in the anode chamber to prepare anion-adsorbed graphene product, electrochemical deposition is performed in the cathode chamber facing to the anode side to prepare magnesium hydroxide/graphene composite product, and electrochemical intercalation is performed in the cathode chamber facing away from the anode side to prepare cation-adsorbed graphene product.
8. The method for high value-added comprehensive utilization of salt lake brine according to claim 1, wherein in the step (4), the graphene products adsorbing anions in the anode chamber comprise sulfate ions, borate ions, chloride ions and the like, and the graphene products adsorbing cations in the cathode chamber comprise potassium ions, lithium ions, sodium ions, magnesium ions and the like.
9. The method for comprehensively utilizing the salt lake brine with high added value according to claim 1, wherein in the step (4), the electrolysis is finished after the power is applied for 1-12 hours or the anode plate or the cathode plate is reacted.
10. The method for high value-added comprehensive utilization of salt lake brine according to claim 1, wherein in the step (4), the direct current electrolysis temperature is room temperature electrolysis.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114672820A (en) * | 2022-05-03 | 2022-06-28 | 营口理工学院 | Safe and environment-friendly utilization method for high added value of low-grade magnesite |
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2021
- 2021-01-27 CN CN202110108119.0A patent/CN112708901A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114672820A (en) * | 2022-05-03 | 2022-06-28 | 营口理工学院 | Safe and environment-friendly utilization method for high added value of low-grade magnesite |
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