CN115093139A - Carbonizable magnesium oxide cementing material produced by electrolyzing seawater and preparation method thereof - Google Patents

Carbonizable magnesium oxide cementing material produced by electrolyzing seawater and preparation method thereof Download PDF

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Publication number
CN115093139A
CN115093139A CN202210882040.8A CN202210882040A CN115093139A CN 115093139 A CN115093139 A CN 115093139A CN 202210882040 A CN202210882040 A CN 202210882040A CN 115093139 A CN115093139 A CN 115093139A
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China
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seawater
magnesium oxide
carbonizable
cathode
material produced
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蒋正武
高文斌
李晨
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Tongji University
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Tongji University
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B9/00—Magnesium cements or similar cements
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/02—Magnesia
    • C01F5/06—Magnesia by thermal decomposition of magnesium compounds
    • C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
    • 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
    • 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
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
    • C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Electrolytic Production Of Metals (AREA)

Abstract

The invention relates to a carbonizable magnesium oxide cementing material produced by electrolyzing seawater and a preparation method thereof, and the specific process flow is as follows: (1) constructing an electrolytic cell provided with a cathode and an anode, and arranging an ion exchange membrane between the cathode and the anode in the electrolytic cell; (2) introducing seawater into the electrolytic cell, electrifying for electrolysis to ionize the seawater to generate ions, and enriching Mg in the cathode region by the filtration of the ion exchange membrane 2+ (ii) a (3) The pH of the cathode region is controlled so that Mg 2+ Completely precipitating to form magnesium hydroxide; (4) after calcining the obtained magnesium hydroxide, namelyObtaining the target product of the magnesium oxide gel material capable of being carbonized. Compared with the prior art, the main raw material seawater used by the cementing material has wide source and low cost, and the obtained cementing material has high purity and high carbonization activity, can form a high-strength product by absorbing carbon dioxide, and has great significance for carbon neutralization in the building material industry of China.

Description

Carbonizable magnesium oxide cementing material produced by electrolyzing seawater and preparation method thereof
Technical Field
The invention belongs to the technical field of seawater resource utilization and low-carbon cementing material development, and relates to a carbonizable magnesium oxide cementing material produced by seawater electrolysis and a preparation method thereof.
Background
In recent years, researchers have found that magnesium oxide can form a product with higher strength through a carbonization reaction, and carbon dioxide can be permanently solidified in the product, so that the magnesium oxide has great carbon reduction potential. Magnesium oxide can be derived from forsterite and magnesite, which, although widely distributed, cannot be efficiently converted to MgO by the prior art. Magnesite can obtain magnesium oxide through calcination, but the production energy consumption and carbon emission are higher than OPC. Therefore, the problem of the source of magnesium oxide remains to be solved.
The seawater is rich in a large amount of magnesium ions, and the magnesium is extracted by an electrodeposition mode and converted into magnesium oxide, so that the problem of insufficient magnesium oxide resources can be solved. Therefore, the development of the magnesium oxide cementing material which is suitable for seawater electrolysis and can be carbonized has very important significance for realizing the double-carbon target in China.
Disclosure of Invention
The invention aims to provide a carbonizable magnesium oxide cementing material produced by electrolyzing seawater and a preparation method thereof, and opens up a new way for ocean resource utilization and low-carbon cementing material preparation.
The purpose of the invention can be realized by the following technical scheme:
one of the technical schemes of the invention provides a preparation method of a carbonizable magnesium oxide cementing material produced by electrolyzing seawater, which comprises the following steps:
(1) constructing an electrolytic cell provided with a cathode and an anode, and arranging an ion exchange membrane between the cathode and the anode in the electrolytic cell;
(2) introducing seawater into the electrolytic cell, electrifying for electrolysis to ionize the seawater to generate ions, and enriching Mg in the cathode region by the filtration of the ion exchange membrane 2+ ；
(3) The pH of the cathode region is controlled so that Mg 2+ Completely precipitating to form magnesium hydroxide;
(4) and calcining the obtained magnesium hydroxide to obtain the target product of the magnesium oxide cementing material capable of being carbonized.
Furthermore, the cathode and the anode can be zinc rods.
Further, the ion exchange membrane is a mixed fiber microporous filter membrane, a polypropylene filter membrane or a polyether sulfone filter membrane, and specifically, the aperture range of the selected filter membrane is 0.4-0.6 nm.
Furthermore, the power supply current in the electrolysis process is 3.5-6.5A.
Further, the pH value of the cathode region is 9.4-12.4.
Furthermore, the calcining temperature is 350-450 ℃, and the calcining time is 1-3 h.
Further, the atmosphere of calcination is N 2 Or O 2 An atmosphere.
Further, the equipment used for calcination is a muffle furnace or a sintering furnace with controllable atmosphere.
Furthermore, the content of magnesium ions in the seawater used in the step (2) is not less than 3.69 wt%.
Further, the seawater in the step (2) is natural seawater, laboratory simulated seawater or concentrated seawater.
The second technical scheme of the invention provides a carbonizable magnesium oxide cementing material produced by electrolyzing seawater, which is prepared by the preparation method.
Introducing seawater with magnesium ion content not less than 3.69 wt% into an electrolytic cell, connecting a cathode and an anode with an external power supply, controlling the external power supply to enable current to be 3.5-6.5A, and electrolyzing the solution in the electrolytic cell to generate Cl - 、OH - 、Na + 、Mg 2+ 、Ca 2+ Plasma, cations in the solution need to obtain electrons to reach charge balance, so the cations can migrate to a cathode, and in the migration process, an ion exchange membrane (a mixed fiber microporous filter membrane, a polypropylene filter membrane or a polyether sulfone filter membrane) can block other cations to ensure that only Mg is contained 2+ Reaches the cathode region through the ion exchange membrane, and then ensures the pH value of the cathode region to be within the range of 9.4-12.4 under the regulation of a pH regulation system according to Mg (OH) 2 The solubility product constant of (1), Mg at pH 9.4-12.4 2+ Can be reacted with OH - Reacting to form precipitate, filtering the precipitate, taking out, and adding N at 350-450 DEG C 2 Or O 2 Calcining in muffle furnace or sintering furnace for 1-3h while using Mg (O)H) 2 MgO is generated by decomposition. The reactions that mainly occur are as follows:
2H 2 O+2e - →2OH - +H 2 (g)
O 2 +2H 2 O+4e - →4OH -
2OH - +Mg 2+ →Mg(OH) 2 (s)
Mg(OH) 2 →MgO+H 2 O
the MgO obtained by the invention has high carbonization activity mainly because magnesium hydroxide generated by seawater electrodeposition has crystal defects, and the generated magnesium oxide is in a metastable state (the more the crystal defects are, the more unstable the magnesium oxide is, the more the magnesium oxide is, the carbonization reaction is easier to form stable magnesium carbide. Generally, the magnesia cement of the present invention is more susceptible to carbonization than conventional magnesia, and therefore, has a better carbon sequestration effect. The reaction of MgO carbonization is as follows:
MgO+CO 2 →MgCO 3
MgO+CO 2 +3H 2 O→MgCO 3 ·3H 2 O
compared with the prior art, the invention has the following advantages:
1. the method extracts magnesium resources from seawater and prepares the magnesium resources into the magnesium oxide cementing material capable of being carbonized, so that the seawater resources are reasonably utilized, the exploitation of ore raw materials in the magnesium oxide production process is reduced, the problem of insufficient resources of the traditional magnesium oxide is solved, and the method has very important economic and environmental protection significance.
2. The invention recovers magnesium ions in seawater by using the electrolysis principle of the electrolytic cell, and designs the ion exchange membrane in the electrolytic cell, thereby improving the enrichment efficiency of magnesium ions at the cathode and ensuring the stable growth of cathode products.
3. The magnesium oxide cementing material can generate carbonization reaction, on one hand, the magnesium oxide carbonization process can absorb carbon dioxide to realize carbon paving; on the other hand, the magnesium oxide cementing material of the invention is carbonized to form a hard carbonized product, thereby realizing carbon sequestration.
Detailed Description
The present invention will be described in detail with reference to specific examples. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following examples, unless otherwise specified, all the starting materials and processing techniques used are those conventionally available in the art.
The preparation method of the carbonizable magnesium oxide cementing material produced by electrolyzing seawater comprises the following steps:
(1) constructing an electrolytic cell provided with a cathode and an anode, and arranging an ion exchange membrane between the cathode and the anode in the electrolytic cell;
(2) introducing seawater into the electrolytic cell, electrifying for electrolysis to ionize the seawater to generate ions, and enriching Mg in the cathode region by the filtration of the ion exchange membrane 2+ ；
(3) The pH of the cathode region is controlled so that Mg 2+ Completely precipitating to form magnesium hydroxide;
(4) and calcining the obtained magnesium hydroxide to obtain the target product of the carbonized magnesium oxide gel material.
The following preparation experiments of the magnesium oxide gel material capable of being carbonized are carried out by combining the preparation process flows, and the preparation experiments respectively comprise the following steps:
example 1
Selecting a yellow sea water solution as an electrolyte, wherein the magnesium ion content of the electrolyte is 5.42%; the power supply current in the electrolytic cell is 5A; the cathode and anode are made of zinc bars; the ion exchange membrane is a mixed cellulose ester microporous filter membrane which can allow magnesium ions to pass through and can selectively block other cations, and is purchased from a Square filtration equipment plant in the Hainin market; by controlling the pH of the cathode region to be 11.2 and keeping the pH basically unchanged; the equipment used for calcination is a muffle furnace; the calcining temperature in the calcining process is 370 ℃, and the calcining time is 1.5 h. The purity of the obtained magnesium oxide gel material capable of being carbonized is 85 percent, the strength after 2 hours of carbonization is 40MPa, and the solid carbon content is 0.81kg of CO 2 In kg, i.e. 1kg carbonizable magnesia gel Material curable 0.8kg CO 2 。
Example 2
Selecting a seawater solution simulated in a laboratory as an electrolyte, wherein the magnesium ion content of the seawater solution is 5.48%; the power supply current of the electrolytic cell is 5.2A; the cathode and anode are made of zinc bars; the ion exchange membrane is a polyether sulfone filter membrane and is purchased from Yonghao filtration equipment limited company of Hainin. Controlling the pH value of the cathode region to be 11.5 by a pH control system and keeping the pH value basically unchanged; the equipment used for calcination is a muffle furnace; the calcining temperature in the calcining process is 410 ℃, and the calcining time is 1.2 h. The purity of the obtained carbonized magnesia gel material is 87 percent, the strength after 2h carbonization is 42MPa, and the solid carbon content is 0.93kg CO 2 /kg。
Example 3
Selecting an east sea water solution as an electrolyte, wherein the magnesium ion content of the east sea water solution is 6.23%; the supply current of the electrolytic cell is 6.2A; the cathode and anode are made of zinc bars; the cation exchange membrane is a polypropylene filter membrane and is purchased from Hangzhou Kanjie membrane separation technology GmbH; the anion exchange membrane is a mixed fiber microporous filter membrane; controlling the pH value of the cathode region to be 13.2 by a pH control system and keeping the pH value basically unchanged; the equipment used for calcination is a sintering furnace; the calcining temperature in the calcining process is 470 ℃, and the calcining time is 1 h. The purity of the obtained carbonized magnesia gel material is 95 percent, the strength after 2 hours of carbonization is 48MPa, and the solid carbon content is 1.02 percent.
Example 4:
compared with example 1, most of them are the same except that the supply current is adjusted to 3.5A. The purity of the obtained magnesium oxide gel material capable of being carbonized is 82 percent, the strength after 2 hours of carbonization is 30MPa, and the solid carbon content is 0.75kg CO 2 /kg
Example 5:
compared to example 1, most of them were the same except that the pH was adjusted to 9.8. The purity of the obtained magnesium oxide gel material capable of being carbonized is 80 percent, the strength after 2 hours of carbonization is 40MPa, and the solid carbon content is 0.86kg of CO 2 /kg。
Example 6:
most of them were the same as in example 1 except that the calcination temperature was adjusted to 380 ℃. The purity of the obtained carbonized magnesia gel material is 95 percent, the strength after 2h carbonization is 45MPa, and the solid carbon content is 0.92kg CO 2 /kg。
Comparative example 1:
compared to example 1, most of them are the same except that the ion exchange membrane arrangement is omitted from the electrolytic cell. The purity of the obtained magnesium oxide gel material capable of being carbonized is 75 percent, the strength after 2 hours of carbonization is 38MPa, and the carbon content is 0.79kg CO 2 Per kg, i.e. 1kg carbonizable magnesia gel material curable 0.79kg CO 2 。
Comparative example 2:
compared to example 1, most of them were the same except that conventional commercially available MgO, which was obtained from Guangxi magnesia refractory Co., Ltd, was directly used for carbon sequestration. The strength after 2h of carbonization is 25MPa, and the carbon content is 0.45kg CO 2 Per kg, i.e. 1kg carbonizable magnesia gel material curable 0.45kg CO 2 。
Comparative example 3:
compared with example 1, the power supply current is mostly the same except that the power supply current is adjusted to 2A. The purity of the obtained magnesium oxide cementing material capable of being carbonized is 81 percent, the strength after 2 hours of carbonization is 37MPa, and the solid carbon content is 0.76kg of CO 2 Per kg, i.e. 1kg carbonizable magnesia cement curable 0.76kg CO 2 。
Comparative example 4:
compared to example 1, the same is mostly true, except that the pH is adjusted to 8.5. The purity of the obtained magnesium oxide gel material capable of being carbonized is 69 percent, the strength after 2 hours of carbonization is 35MPa, and the carbon content is 0.72kg CO 2 Per kg, i.e. 1kg carbonizable magnesia cement curable 0.72kg CO 2 。
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. The preparation method of the carbonizable magnesium oxide cementing material produced by electrolyzing seawater is characterized by comprising the following steps:
(1) constructing an electrolytic cell provided with a cathode and an anode, and arranging an ion exchange membrane between the cathode and the anode in the electrolytic cell;
(2) introducing seawater into the electrolytic cell, electrifying for electrolysis to ionize the seawater to generate ions, and enriching Mg in the cathode region by the filtration of the ion exchange membrane 2+ ；
(3) The pH of the cathode region is controlled so that Mg 2+ Completely precipitating to form magnesium hydroxide;
(4) and calcining the obtained magnesium hydroxide to obtain the target product of the magnesium oxide cementing material capable of being carbonized.
2. The method for preparing the carbonizable magnesium oxide cementing material produced by electrolyzing seawater as claimed in claim 1, wherein the cathode and the anode are both zinc rods.
3. The method for preparing the carbonized magnesia gel material produced by electrolyzing seawater according to claim 1, wherein the ion exchange membrane is a mixed fiber microporous filter membrane, a polypropylene filter membrane or a polyether sulfone filter membrane.
4. The preparation method of the carbonizable magnesium oxide cementing material produced by electrolyzing seawater according to claim 1, wherein the power supply current in the electrolysis process is 3.5-6.5A.
5. The method for preparing the carbonized magnesia gel material produced by electrolyzing seawater as recited in claim 1, wherein the pH value of the cathode region is 9.4-12.4.
6. The method for preparing the magnesium oxide cementing material capable of being carbonized and produced by electrolyzing seawater as claimed in claim 1, wherein the calcining temperature is 350-450 ℃ and the calcining time is 1-3 h.
7. The method for preparing the carbonizable magnesium oxide gel material produced by electrolyzing seawater as claimed in claim 1, wherein the calcining atmosphere is N 2 Or O 2 An atmosphere.
8. The method for preparing the carbonized magnesia gel material produced by electrolyzing seawater according to claim 1, wherein the calcining apparatus is a muffle furnace or a sintering furnace with controllable atmosphere.
9. The method for preparing a carbonizable magnesium oxide gel material by electrolyzing seawater according to claim 1, wherein the seawater used in step (2) is natural seawater, laboratory simulated seawater or concentrated seawater, and the magnesium ion content is not less than 3.69 wt%.
10. A carbonizable magnesium oxide gelled material produced by electrolyzing seawater, which is prepared by the preparation method as claimed in any one of claims 1 to 9.
CN202210882040.8A 2022-07-26 2022-07-26 Carbonizable magnesium oxide cementing material produced by electrolyzing seawater and preparation method thereof Pending CN115093139A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020179435A1 (en) * 2001-06-04 2002-12-05 Maddan Orville Lee Apparatus and method for producing magnesium from seawater
US20050011770A1 (en) * 2003-07-18 2005-01-20 Tatenuma Katsuyoshi Reduction method of atmospheric carbon dioxide, recovery and removal method of carbonate contained in seawater, and disposal method of the recovered carbonate
JP2009234829A (en) * 2008-03-26 2009-10-15 Bio Coke Lab Co Ltd Method and apparatus for recycling magnesium hydroxide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020179435A1 (en) * 2001-06-04 2002-12-05 Maddan Orville Lee Apparatus and method for producing magnesium from seawater
US20050011770A1 (en) * 2003-07-18 2005-01-20 Tatenuma Katsuyoshi Reduction method of atmospheric carbon dioxide, recovery and removal method of carbonate contained in seawater, and disposal method of the recovered carbonate
JP2009234829A (en) * 2008-03-26 2009-10-15 Bio Coke Lab Co Ltd Method and apparatus for recycling magnesium hydroxide

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
刘松玉等: "压实度对MgO碳化土加固效果的影响及其机理研究", 《中国公路学报》, vol. 31, no. 08, 15 August 2018 (2018-08-15), pages 30 - 38 *
张联盟等: "《实用耐火原料手册》", vol. 1, 武汉理工大学出版社, pages: 530 *
王成彦等, 冶金工业出版社 *

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