CN112281180A - Method for preparing chlorine by electrolyzing concentrated seawater through bipolar membrane - Google Patents

Method for preparing chlorine by electrolyzing concentrated seawater through bipolar membrane Download PDF

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Publication number
CN112281180A
CN112281180A CN202011060341.XA CN202011060341A CN112281180A CN 112281180 A CN112281180 A CN 112281180A CN 202011060341 A CN202011060341 A CN 202011060341A CN 112281180 A CN112281180 A CN 112281180A
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chamber
bipolar membrane
concentrated seawater
cathode
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阮慧敏
吴思梵
沈江南
伍其辉
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Zhejiang University of Technology ZJUT
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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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Abstract

本发明公开了一种双极膜电解浓海水制氯的方法，包括如下步骤：(1)对浓海水进行预处理，使其中的钙镁离子浓度降至10ppm以下；(2)取一种以双极膜为隔膜的电解装置，所述电解装置的阳极室通入经步骤(1)预处理后的浓海水，阴极室通入NaOH溶液，开启直流电源进行电解，在直流电场的作用下，水在双极膜上分裂为氢离子和氢氧根离子，产生的氢氧根离子和氢离子分别进入阳极室和阴极室发生反应，最终在阳极室中生成有效氯，在阴极室中得到氢气和氢氧化钠溶液。本发明无需设置氯气分离装置，使氯气直接在阳极室溶液中反应生成有效氯，装置相对更为简易。The invention discloses a method for producing chlorine by bipolar membrane electrolysis of concentrated seawater, comprising the following steps: (1) pretreating the concentrated seawater to reduce the concentration of calcium and magnesium ions in it to less than 10 ppm; The bipolar membrane is an electrolysis device with a diaphragm, the anode chamber of the electrolysis device is fed with the concentrated seawater pretreated in step (1), the NaOH solution is fed into the cathode chamber, and the DC power supply is turned on for electrolysis. Under the action of the DC electric field, Water splits into hydrogen ions and hydroxide ions on the bipolar membrane, and the generated hydroxide ions and hydrogen ions enter the anode chamber and the cathode chamber respectively to react, and finally generate effective chlorine in the anode chamber, and obtain hydrogen in the cathode chamber. and sodium hydroxide solution. The invention does not need to set up a chlorine gas separation device, so that the chlorine gas directly reacts in the anode chamber solution to generate effective chlorine, and the device is relatively simpler.

Description

Method for preparing chlorine by electrolyzing concentrated seawater through bipolar membrane
Technical Field
The invention belongs to the technical field of water treatment and chlorine preparation, and particularly relates to a method for preparing effective chlorine by electrolysis in an electrolytic cell with a bipolar membrane as a diaphragm.
Background
The seawater desalination is one of important methods for solving global water resource shortage, and the concentrated seawater is a byproduct of the seawater desalination, is concentrated water formed by reverse osmosis of seawater, contains a large amount of chloride ions, has the concentration of about 3 percent, and is a natural bittern resource. Because the salt content is high, direct discharge can cause certain influence on the environment, so the method can be recycled by a series of process methods, such as concentration salt preparation, bipolar membrane electrodialysis acid and alkali preparation, lithium extraction, bromine extraction and the like, and the electrolytic preparation of available chlorine is an important process.
The available chlorine is chlorine gas, hypochlorous acid, hypochlorite and other oxidizing chlorine, and is commonly used as disinfectant, bactericide and bleaching agent.
The methods for producing chlorine by electrolysis in industry include mainly a non-diaphragm method, a diaphragm method and an ion membrane method. The diaphragm-free method mainly has the problems of low effective chlorine concentration, high energy consumption, more side reactions, easy scaling of electrodes and the like. The ion membrane method gradually replaces other two technologies due to the advantages of high yield of available chlorine, low energy consumption, high current efficiency and the like, and becomes the dominant process for preparing chlorine by electrolysis. The bipolar membrane is one kind of ionic membrane, has the characteristic of decomposing water into hydrogen ions and hydroxyl ions, and is mainly applied to the fields of electrodialysis and the like. In recent years, attention has been paid to the application of bipolar membranes to electrolysis.
Disclosure of Invention
The invention aims to provide a method for preparing chlorine by electrolyzing concentrated seawater by using an electrolysis device with a bipolar membrane as a diaphragm, wherein effective chlorine is directly obtained in an anode chamber, and alkali liquor obtained in a cathode chamber can be recycled.
A method for preparing chlorine by electrolyzing concentrated seawater through a bipolar membrane comprises the following steps:
(1) pretreating the concentrated seawater to reduce the concentration of calcium and magnesium ions in the seawater to below 10 ppm;
(2) taking an electrolysis device with a bipolar membrane as a diaphragm, introducing concentrated seawater pretreated in the step (1) into an anode chamber of the electrolysis device, introducing a NaOH solution into a cathode chamber, starting a direct-current power supply to carry out electrolysis, splitting water into hydrogen ions and hydroxide ions on the bipolar membrane under the action of a direct-current electric field, respectively introducing the generated hydroxide ions and hydrogen ions into the anode chamber and the cathode chamber to react, finally generating effective chlorine in the anode chamber, and obtaining hydrogen and a sodium hydroxide solution in the cathode chamber.
The reaction in the anode chamber is as follows:
2Cl-→Cl2+2e-；Cl2+H2O→HClO+HCl；NaOH+Cl2→NaClO+HCl；
the reaction in the cathode chamber is: h++2e-→H2。
The effective chlorine obtained in the anode chamber can be directly applied to disinfection and can also be further reacted with sodium hydroxide to generate sodium hypochlorite which can exist stably.
Preferably, the pretreatment method of the concentrated seawater comprises the following steps:
firstly, adding sodium hydroxide and sodium carbonate into concentrated seawater by a double-alkali chemical precipitation method to obtain calcium carbonate and magnesium hydroxide precipitates, removing most calcium and magnesium ions in the concentrated seawater, and simultaneously adjusting the pH to 6-7, so that the scaling problem can be effectively avoided;
and then, the calcium and magnesium ions and high-valence metal ions in the concentrated seawater are removed through adsorption of ion exchange resin, and the calcium and magnesium ions in the concentrated seawater are reduced to below 10ppm, so that the water quality requirement of the electrolyzed inlet water of the ion membrane is met.
In the invention, the adding amount of the sodium hydroxide and the sodium carbonate is excessive, namely more than the theoretical amount of the sodium hydroxide and the sodium carbonate required by calculation according to the content of calcium and magnesium ions in the concentrated seawater, so as to remove the calcium and magnesium ions in the concentrated seawater as far as possible.
In the present invention, the ion exchange resin is used for removing calcium and magnesium ions and high-valence metal ions, so that any ion exchange resin satisfying the above requirements is suitable, for example, 732 cation exchange resin, CH-93 chelate ion exchange resin, etc. The adsorption conditions can be determined according to the use requirements of the ion exchange resin and the concentration requirements of the final calcium and magnesium ions.
The invention provides an electrolysis device with a bipolar membrane as a diaphragm, which comprises: the device comprises an electrolytic cell, a bipolar membrane, an anode plate, a cathode plate, a direct current power supply, a circulating chamber and a metering pump; the electrolytic bath is divided into an anode chamber and a cathode chamber by the bipolar membrane, and the upper end and the lower end of the anode chamber and the lower end of the cathode chamber are respectively provided with a water outlet and a water inlet which are connected with the anode circulating chamber and the cathode circulating chamber by pipelines; the cathode chamber is provided with an exhaust port for discharging hydrogen, and the anode chamber is closed to enable chlorine to react in the solution to generate effective chlorine.
Preferably, the anode plate material is a mesh metal DSA, and the cathode plate material is a mesh titanium electrode plate.
Preferably, the bipolar membrane is one of a BP-1 type bipolar membrane (ASTOM Co, Japan) or an FBM type bipolar membrane (Fuma-Tech Co, Germany).
Preferably, when the direct current power supply carries out electrolysis, the distance between the electrode plates is 1-10cm, and the current density is 100--2The flow rate of each chamber is 20-50L/h, and the electrolysis temperature is controlled to be 15-35 ℃.
Preferably, the NaOH solution is introduced into the cathode chamber at an initial concentration of 0.05-2 mol/L.
Compared with the traditional ionic membrane electrolysis method, the method has the beneficial effects that: the invention does not need to arrange a chlorine gas separation device, so that the chlorine gas directly reacts in the anode chamber solution to generate the effective chlorine, and the device is relatively simple.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a schematic view of an electrolysis apparatus according to the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1
The pretreatment method of concentrated seawater (wherein the concentration of calcium ions is 552.38ppm, the concentration of magnesium ions is 1615.12ppm, and the concentration of NaCl is about 1.5%) is shown in figure 1. firstly, by a double-alkali chemical precipitation method, sodium hydroxide and sodium carbonate reagents are added into the concentrated seawater, 5.5g of sodium hydroxide and 1.5g of sodium carbonate are added into each liter of concentrated seawater, so that most of calcium and magnesium ions and polyvalent metal ions in the concentrated seawater are precipitated, and calcium carbonate and magnesium hydroxide are generated. Then, suspended matters in the sediment and the concentrated seawater are removed through suction filtration, and meanwhile, the pH value is adjusted to 6-7, so that the scaling problem can be effectively avoided. Further, the high-valence metal ions such as calcium, magnesium and the like in the concentrated seawater are further reduced in concentration by adsorbing through CH-93 ion exchange resin at the room temperature of 25 ℃ and controlling the flow rate to be 10BV/h, so that the water inlet requirement of electrolysis is met.
The concentration of NaCl in the pretreated concentrated seawater is about 3 percent; the calcium ion concentration is 2.58ppm, and the removal rate is 99.53 percent; the concentration of magnesium ions in the pretreated concentrated seawater is 2.26ppm, and the removal rate is 99.86%.
FIG. 2 shows an ionic membrane electrolysis apparatus, which is different from other ionic membrane electrolysis apparatuses, and in the present invention, a BP-1 type bipolar membrane (ASTOM Co, Japan) is used as an electrolysis diaphragm instead of a common perfluorosulfonic acid cation exchange membrane. The electrolysis device consists of a direct current power supply 6, a cathode plate 2, an anode plate 3, a bipolar membrane 1, a cathode chamber 4, an anode chamber 5, a cathode circulating chamber 7, an anode circulating chamber 8 and metering pumps 9 and 10. Wherein the bipolar membrane 1 separates the anode chamber 5 from the cathode chamber 4, and the upper end and the lower end of the anode chamber 5 and the lower end of the cathode chamber 4 are respectively provided with a water outlet and a water inlet which are connected with the anode circulating chamber 8 and the cathode circulating chamber 7 through pipelines. The cathode chamber is provided with an exhaust port for discharging hydrogen. The anode plate material is a net-shaped metal DSA, and the cathode plate material is a net-shaped titanium electrode plate.
Specifically, the cathode plate is connected with the cathode of the direct current power supply, and the anode plate is connected with the anode of the direct current power supply. Introducing the pretreated concentrated seawater (the NaCl concentration is about 30g/L) into an anode circulation chamber, and feeding the pretreated concentrated seawater into an anode chamber through a metering pump for electrolysis. 0.5M sodium hydroxide solution was added to the cathode recycle chamber and fed into the cathode chamber through a metering pump for electrolysis. The volume ratio of the electrolyte in the cathode chamber to the electrolyte in the anode chamber is 1: 1. The flow rates of the cathode chamber and the anode chamber are both 30L/h.
The pretreated concentrated seawater enters the anode chamber through the anode circulating chamber to be electrolyzed, and chloride ions in the concentrated seawater are reduced into effective chlorine. And (3) adding a dilute sodium hydroxide solution into the cathode circulating chamber, reacting in the cathode chamber to generate hydrogen and an alkali solution with higher concentration, wherein the hydrogen can be directly discharged from an exhaust port, and the alkali solution can be recycled.
Condensed water reflux is arranged in the anode circulating chamber and the cathode circulating chamber, and the electrolysis temperature is controlled to be about 25 ℃ at room temperature. Control electricityThe source is a steady current, and the current density is 100--2The distance between the electrode plates is 5cm, and the electrolysis time is 120 min.
The final effective chlorine concentration in the anode chamber can reach 1.152%, and the energy consumption is 59.58 kwh.kg-1An available chlorine.
Example 2
Instead of the commonly used cation-exchange membrane of perfluorosulfonic acid, a bipolar membrane of the FBM type (Fuma-Tech co, Germany) was used as the electrolytic membrane. The rest is the same as example 1.
The concentration of the available chlorine finally obtained in the anode chamber can reach 1.032%, and the energy consumption is 60.34 kwh.kg < -1 > of the available chlorine.
The bipolar membrane is adopted as the electrolytic diaphragm, and the characteristics of water decomposition on the bipolar membrane are utilized to generate hydroxyl ions, so that the generation of sodium hypochlorite is facilitated. Compared with the traditional ionic membrane electrolysis, the device does not need to be provided with a chlorine separation device, is simpler and easier, is favorable for realizing the resource utilization of concentrated seawater and realizes sustainable production.

Claims (8)

1.一种双极膜电解浓海水制氯的方法，包括如下步骤：1. a method for producing chlorine by bipolar membrane electrolysis of concentrated seawater, comprising the steps: (1)对浓海水进行预处理，使其中的钙镁离子浓度降至10ppm以下；(1) Pretreatment is carried out to the concentrated seawater, so that the calcium and magnesium ion concentration in it is reduced to below 10ppm; (2)取一种以双极膜为隔膜的电解装置，所述电解装置的阳极室通入经步骤(1)预处理后的浓海水，阴极室通入NaOH溶液，开启直流电源进行电解，在直流电场的作用下，水在双极膜上分裂为氢离子和氢氧根离子，产生的氢氧根离子和氢离子分别进入阳极室和阴极室发生反应，最终在阳极室中生成有效氯，在阴极室中得到氢气和氢氧化钠溶液。(2) get a kind of electrolysis device with bipolar membrane as diaphragm, the anode chamber of described electrolysis device is passed into the concentrated seawater after step (1) pretreatment, and the cathode chamber is passed into NaOH solution, and the direct current power supply is turned on to carry out electrolysis, Under the action of the DC electric field, the water splits into hydrogen ions and hydroxide ions on the bipolar membrane, and the generated hydroxide ions and hydrogen ions enter the anode chamber and the cathode chamber respectively to react, and finally generate effective chlorine in the anode chamber. , hydrogen and sodium hydroxide solution are obtained in the cathode compartment. 2.如权利要求1所述的方法，其特征在于：所述浓海水的预处理方法为：2. method as claimed in claim 1 is characterized in that: the pretreatment method of described concentrated seawater is: 首先通过双碱化学沉淀法，往浓海水中加入氢氧化钠和碳酸钠，得到碳酸钙和氢氧化镁沉淀，除去浓海水中大部分的钙镁离子，同时将pH调至6-7；First, by double-alkali chemical precipitation method, add sodium hydroxide and sodium carbonate to the concentrated seawater to obtain calcium carbonate and magnesium hydroxide precipitation, remove most of the calcium and magnesium ions in the concentrated seawater, and adjust the pH to 6-7 at the same time; 然后通过离子交换树脂进行吸附，除去浓海水中的钙镁离子和高价金属离子，将浓海水中钙镁离子降至10ppm以下。Then, it is adsorbed by ion exchange resin to remove calcium and magnesium ions and high-valent metal ions in the concentrated seawater, and reduce the calcium and magnesium ions in the concentrated seawater to less than 10ppm. 3.如权利要求2所述的方法，其特征在于：所述的离子交换树脂为732阳离子交换树脂或CH-93螯合离子交换树脂。3. The method of claim 2, wherein the ion exchange resin is 732 cation exchange resin or CH-93 chelating ion exchange resin. 4.如权利要求1-3之一所述的方法，其特征在于：所述以双极膜为隔膜的电解装置，包括：电解槽，双极膜，阳极板，阴极板，直流电源，循环室，计量泵；其中双极膜将电解槽分隔为阳极室和阴极室，阳极室和阴极室的上端和下端分别设有出水口和进水口，通过管道与阳极循环室和阴极循环室相连；所述阴极室设有排气口供排放氢气，阳极室密闭使氯气在溶液中反应生成有效氯。4. The method according to any one of claims 1-3, wherein the electrolysis device using the bipolar membrane as a diaphragm comprises: an electrolytic cell, a bipolar membrane, an anode plate, a cathode plate, a DC power supply, a circulation The bipolar membrane divides the electrolytic cell into an anode chamber and a cathode chamber, and the upper and lower ends of the anode chamber and the cathode chamber are respectively provided with a water outlet and a water inlet, which are connected with the anode circulation chamber and the cathode circulation chamber through pipes; The cathode chamber is provided with an exhaust port for discharging hydrogen gas, and the anode chamber is sealed so that chlorine gas can react in the solution to generate effective chlorine. 5.如权利要求4所述的方法，其特征在于：阳极板材料为网状金属DSA，阴极板材料为网状钛电极板。5 . The method of claim 4 , wherein the anode plate material is mesh metal DSA, and the cathode plate material is mesh titanium electrode plate. 6 . 6.如权利要求1-3之一所述的方法，其特征在于：双极膜为BP-1型双极膜或FBM型双极膜。6 . The method according to claim 1 , wherein the bipolar membrane is a BP-1 type bipolar membrane or an FBM type bipolar membrane. 7 . 7.如权利要求1-3之一所述的方法，其特征在于：直流电源进行电解时，电极板间距为1-10cm，电流密度为100-2000A/m-2，各室流速均为20-50L/h，电解温度控制为15-35℃。7. The method according to one of claims 1-3, characterized in that: when the DC power source is electrolyzed, the electrode plate spacing is 1-10cm, the current density is 100-2000A/m -2 , and the flow rate of each chamber is 20 -50L/h, the electrolysis temperature is controlled to 15-35℃. 8.如权利要求1-3之一所述的方法，其特征在于：所述阴极室通入的NaOH溶液的起始浓度为0.05-2mol/L。8 . The method according to claim 1 , wherein the initial concentration of the NaOH solution introduced into the cathode chamber is 0.05-2 mol/L. 9 .
CN202011060341.XA 2020-09-30 2020-09-30 Method for preparing chlorine by electrolyzing concentrated seawater through bipolar membrane Pending CN112281180A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022119407A1 (en) * 2020-12-03 2022-06-09 한국에너지기술연구원 Seawater electrolysis apparatus and seawater electrolysis fuel cell link system comprising same
CN116812959A (en) * 2023-07-17 2023-09-29 天津大学 Electric energy driven seawater carbon fixing system
CN117222779A (en) * 2021-04-30 2023-12-12 迪诺拉永久电极股份有限公司 Sodium hypochlorite solution manufacturing method and manufacturing device

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Publication number Priority date Publication date Assignee Title
KR101361651B1 (en) * 2012-09-27 2014-02-12 (주) 테크윈 A device using electrolyzer with a bipolar membrane and the method of producing hypochlorite solution and hydrogen gas thereby
JP2016168542A (en) * 2015-03-12 2016-09-23 株式会社東芝 Device and method for generating electrolytic water
CN110577229A (en) * 2018-06-08 2019-12-17 江苏久吾高科技股份有限公司 Method and device for reusing waste salt
CN210458375U (en) * 2019-05-21 2020-05-05 中国水利水电科学研究院 A device for electrolyzing seawater to produce sodium hypochlorite disinfectant

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
KR101361651B1 (en) * 2012-09-27 2014-02-12 (주) 테크윈 A device using electrolyzer with a bipolar membrane and the method of producing hypochlorite solution and hydrogen gas thereby
JP2016168542A (en) * 2015-03-12 2016-09-23 株式会社東芝 Device and method for generating electrolytic water
CN110577229A (en) * 2018-06-08 2019-12-17 江苏久吾高科技股份有限公司 Method and device for reusing waste salt
CN210458375U (en) * 2019-05-21 2020-05-05 中国水利水电科学研究院 A device for electrolyzing seawater to produce sodium hypochlorite disinfectant

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022119407A1 (en) * 2020-12-03 2022-06-09 한국에너지기술연구원 Seawater electrolysis apparatus and seawater electrolysis fuel cell link system comprising same
CN117222779A (en) * 2021-04-30 2023-12-12 迪诺拉永久电极股份有限公司 Sodium hypochlorite solution manufacturing method and manufacturing device
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CN116812959A (en) * 2023-07-17 2023-09-29 天津大学 Electric energy driven seawater carbon fixing system

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Application publication date: 20210129