CN110373679B - Method for preparing anion-controlled multi-hydroxide - Google Patents

Method for preparing anion-controlled multi-hydroxide Download PDF

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CN110373679B
CN110373679B CN201910828203.2A CN201910828203A CN110373679B CN 110373679 B CN110373679 B CN 110373679B CN 201910828203 A CN201910828203 A CN 201910828203A CN 110373679 B CN110373679 B CN 110373679B
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hydroxide
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雷鸣
黄凯
许煜阳
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Beijing University of Posts and Telecommunications
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    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
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    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract

The invention relates to a method for preparing anion regulating and controlling multi-component oxyhydrogenThe method of chemical compound belongs to the field of material science, engineering technology and chemistry. The hydroxide used in the process of the present invention comprises Fe (OH)3、Co(OH)2、Ni(OH)2And complexes of three hydroxides, the anions for modulating hydroxide performance including F‑、Cl‑、Br‑、I‑And the like. By preparing electrolytes with metal ions in different proportions, a large amount of hydroxide ions are generated in the solution by an electrochemical method, and are combined with the metal ions in the solution to deposit on the surface of an electrode, and meanwhile, the regulating ions in the electrolytes are combined with hydroxide to obtain anion-regulated multi-hydroxide. The invention has the advantages of simple preparation process, high speed, high efficiency, wide application range and the like.

Description

Method for preparing anion-controlled multi-hydroxide
Technical Field
The invention relates to a method for regulating and controlling multi-hydroxide by anions, belonging to the field of material science, engineering technology and chemistry.
Background
The layered multi-element metal hydroxide shows outstanding performances in structural characteristics, micro-morphology, surface properties and the like, and becomes one of novel multifunctional materials with potential and development value at present. By utilizing the isomorphous substitution of the metal ions of the laminate, multi-element transition metals (such as Ni, Co, Fe and the like) can be introduced, and a series of hydrotalcite materials with electrochemical characteristics can be prepared and synthesized. The multi-element metal hydroxide has stable electrochemical properties, the preparation method is simple and easy to obtain, the surface structure and the electronic energy band of the multi-element metal hydroxide are changed after anion regulation, and the multi-element metal hydroxide has excellent physical and chemical properties.
Meanwhile, the energy problem is paid more and more attention, hydrogen production through water electrolysis is a carbon-free environment-friendly energy utilization mode, and the hydrodynamic process of electrolysis is closely related to the binding capacity between hydrogen atoms regulated and controlled by electrochemical potential and the surface of a catalyst, so that the hydrogen production is accelerated by utilizing noble metal catalysts such as Pt and Ir, and the large-scale popularization of the renewable hydrogen energy production mode is limited to a great extent.
The multi-metal hydroxides undergo rearrangement of metal-metal bonds and electron transfer between metal and non-metal atoms during formation, resulting in a contraction of the d-band of the metal and further enhanced density of states (DOS) near the fermi level. F-、Cl-The regulation and control effect of plasma anions can cause the change of lattice constant and enhanced d electron density, and the more excellent catalytic activity is shown.
Therefore, the anion-regulated multi-element transition metal hydroxide can play a strong role in the electrochemical field and the promotion of the development of clean energy, and has a wide application prospect.
At present, among the preparation methods of the multi-element metal hydroxide, the electrodeposition method is one of the methods with highest efficiency and best product quality, the application technology is mature, but the subsequent complex steps are needed by adding anion regulation. The method of the invention controls F on the basis of electrodeposition technology-、Cl-The content of the anions is regulated and controlled, so that the deposition and regulation and control of the hydroxide can be completed in the same procedure, the process flow is greatly shortened, and the production efficiency is improved. The product obtained by the method has uniform size, convenient collection and flexible control of product components, and is beneficial to further application of the anion-regulated multi-element metal hydroxide in electrochemistry and other fields.
In conclusion, the preparation method of the anion-regulated multi-element metal hydroxide provided by the invention has the advantages of short process flow, high production efficiency, stable product quality, high raw material utilization rate, flexible component control and the like, and can effectively promote the production and application of the anion-regulated multi-element metal hydroxide.
Disclosure of Invention
1. Objects of the invention
The invention aims to provide a method for preparing anion-controlled multi-hydroxide, which is uniform in thickness and doped with different anions. The regulation and control of different anions on the lamellar hydroxide are realized through a simpler process flow, and more excellent catalytic performance is shown.
2. The invention of the technology
The key points of the invention are as follows:
(1) 250g/m2～300g/m2The foam nickel material with the thickness of 0.2 mm-1 mm is cut into about 6cm2The rectangle is sequentially washed in acetone and ethanol by ultrasound for 30min and then placed in a blast drying oven, and the temperature is set to 40 ℃ for drying, and the rectangle is used as an electrodeposition carrier for standby.
(2) Mixing Fe (NO)3)3、Co(NO3)2、Ni(NO3)20.5 mol/L-1 mol/L electrolyte is prepared according to different molar ratios of 1: 1, 1: 2: 1 and the like (the ratio is adjusted according to the needed hydroxide), meanwhile, salt which is combined with regulating ions, such as KCl, NaF, KI, NaBr and the like, is added into the electrolyte to the concentration of 0.01 mol/L-0.2 mol/L, and the electrolyte is used as soon as possible in order to avoid the long-term deterioration of the electrolyte.
(3) The electrode clamp fixes and washes foam nickel as a cathode, a carbon rod or a Pt electrode as an anode, the two electrodes are immersed in electrolyte, and the current density is adjusted to about 1mA/cm according to the area of the foam nickel of the cathode2～5mA/cm2The electrolysis time is 20 min-40 min, and at the moment, a large amount of hydroxide radicals are gathered by the cathode to be rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel.
(4) And (3) washing the electrodeposited foamed nickel with ethanol, and drying to obtain the lamellar anion-regulated multi-hydroxide.
The method for regulating and controlling the multi-hydroxide by the anion has the advantages that: the method can complete the preparation of the multi-hydroxide and the regulation and control of anions in one step, can obtain various different multi-hydroxides by regulating the concentration of each component in the electrolyte, realizes the regulation and control of various anions, has simple process flow and low preparation cost, and can be used for large-scale preparation.
Drawings
FIG. 1 shows F prepared by the process of the present invention-SEM image of doped Fe, Co, Ni ternary hydroxide.
As can be seen from FIG. 1, the anion-controlled multi-hydroxide obtained by the invention has uniform thickness and obvious lamellar structure, and is beneficial to application of the anion-controlled multi-hydroxide in aspects of electrocatalysis and the like.
FIG. 2 shows F prepared by the method of the present invention-And (3) an electrocatalytic performance diagram of the doped Fe, Co and Ni ternary hydroxide.
As shown in FIG. 2, the anion-regulated multi-hydroxide obtained by the invention has excellent OER and HER catalytic performances, particularly in the aspect of OER performance, F-The regulation and control function of the method obviously improves the performance of the multi-hydroxide, and is particularly suitable for the fields of hydrogen production by water electrolysis and energy storage.
(6) Examples of the invention
The following describes embodiments of the method of the invention:
example 1
F-Regulated Co (OH)2Preparation of
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and mixing with Co (NO)3)2Dissolving in ultrapure water to prepare 0.5-1 mol/L electrolyte, and adding NaF to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. And (3) washing the electrodeposited foamed nickel with ethanol, and drying to obtain the lamellar metal hydroxide regulated by anions.
Example 2
F-Preparation of regulated Co and Ni binary hydroxide
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and mixing with Co (NO)3)2、Ni(NO3)2Dissolving the mixture in ultrapure water according to a molar ratio of 1: 1 to prepare 0.5-1 mol/L electrolyte, and adding NaF to a concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. Washing the electrodeposited foam nickel with ethanol, and drying to obtain lamellar F-A controlled dibasic hydroxide.
Example 3
F-Preparation of regulated Co, Ni and Fe ternary hydroxide
Cutting the foamed nickel material to about 6cm2In a rectangular shape, sequentially immersingSoaking in acetone and ethanol, ultrasonic washing, oven drying, and adding Fe (NO)3)3、Co(NO3)2、Ni(NO3)2Dissolving the mixture in ultrapure water according to the molar ratio of 1: 2: 1 to prepare 0.5-1 mol/L electrolyte, and adding NaF to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. Washing the electrodeposited foam nickel with ethanol, and drying to obtain lamellar F-A regulated ternary hydroxide.
Example 4
I-Regulated Co (OH)2Preparation of
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and mixing with Co (NO)3)2Dissolving in ultrapure water to prepare 0.5-1 mol/L electrolyte, and adding KI to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. And (3) washing the electrodeposited foamed nickel with ethanol, and drying to obtain the lamellar metal hydroxide regulated by anions.
Example 5
I-Preparation of regulated Co and Ni binary hydroxide
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and mixing with Co (NO)3)2、Ni(NO3)2Dissolving the mixture in ultrapure water according to the molar ratio of 1: 1 to prepare 0.5-1 mol/L electrolyte, and adding KI or NaI to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the electric currentDensity of about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. Washing the electrodeposited foam nickel with ethanol, and drying to obtain lamellar I-A controlled dibasic hydroxide.
Example 6
I-Preparation of regulated Co, Ni and Fe ternary hydroxide
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and adding Fe (NO)3)3、Co(NO3)2、Ni(NO3)2Dissolving the mixture in ultrapure water according to the molar ratio of 1: 2: 1 to prepare 0.5-1 mol/L electrolyte, and adding KI to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. Washing the electrodeposited foam nickel with ethanol, and drying to obtain lamellar I-A regulated ternary hydroxide.
Example 7
F-、I-Preparation of Co-regulated Co and Ni binary hydroxide
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and mixing with Co (NO)3)2、Ni(NO3)2Dissolving in ultrapure water according to the molar ratio of 1: 1 or 2: 1 to prepare 0.5-1 mol/L electrolyte, and adding NaF and NaI to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. The foam nickel after electrodeposition is dried after being washed by ethanol,obtaining the lamellar F-、I-A co-regulated binary hydroxide.
Example 8
F-、I-Preparation of Co-regulated Co and Fe binary hydroxide
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and mixing with Co (NO)3)2、Fe(NO3)3Dissolving in ultrapure water according to the molar ratio of 1: 1 or 2: 1 to prepare 0.5-1 mol/L electrolyte, and adding NaF and NaI to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. Washing the electrodeposited foam nickel with ethanol, and drying to obtain lamellar F-、I-A co-regulated binary hydroxide.
Example 9
F-、I-Preparation of co-regulated Fe and Ni binary hydroxide
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and adding Fe (NO)3)3、Ni(NO3)2Dissolving in ultrapure water according to the molar ratio of 1: 1 or 1: 2 to prepare 0.5-1 mol/L electrolyte, and adding NaF and NaI to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. Washing the electrodeposited foam nickel with ethanol, and drying to obtain lamellar F-、I-A co-regulated binary hydroxide.
Example 10
Cl-Regulated ternary of Co, Ni and FePreparation of hydroxides
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and adding Fe (NO)3)3、Co(NO3)2、Ni(NO3)2Dissolving the mixture in ultrapure water according to the molar ratio of 1: 2: 1 to prepare 0.5-1 mol/L electrolyte, and adding KCl to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. Washing the electrodeposited foam nickel with ethanol, and drying to obtain lamellar Cl-A regulated ternary hydroxide.
Example 11
Br-Regulated Co (OH)2Preparation of
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and mixing with Co (NO)3)2Dissolving in ultrapure water to prepare 0.5-1 mol/L electrolyte, and adding NaBr to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. And (3) washing the electrodeposited foamed nickel with ethanol, and drying to obtain the lamellar metal hydroxide regulated by anions.
Example 12
Br-Preparation of regulated Co and Ni binary hydroxide
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and mixing with Co (NO)3)2、Ni(NO3)2Dissolving in ultrapure water according to the molar ratio of 1: 1 to prepare 0.5-1 mol/L electrolyte, and adding NaBr to concentrateThe degree is 0.01 mol/L-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. Washing the electrodeposited foam nickel with ethanol and drying to obtain lamellar Br-A controlled dibasic hydroxide.
Example 13
Br-Preparation of regulated Co, Ni and Fe ternary hydroxide
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and adding Fe (NO)3)3、Co(NO3)2、Ni(NO3)2Dissolving in ultrapure water according to the molar ratio of 1: 2: 1 to prepare 0.5-1 mol/L electrolyte, and adding NaBr to the concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2The electrolysis time is 20 min-40 min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. Washing the electrodeposited foam nickel with ethanol and drying to obtain lamellar Br-A regulated ternary hydroxide.
Example 14
F-、I-Preparation of Co-regulated Co, Fe and Ni ternary hydroxide
Cutting the foamed nickel material to about 6cm2Soaking in acetone and ethanol in sequence, ultrasonic washing, oven drying, and adding Fe (NO)3)3、Ni(NO3)2、Co(NO3)2According to the ratio of 1: 1 or 1; dissolving in ultrapure water in a molar ratio of 1: 2 to prepare 0.5-1 mol/L electrolyte, and adding NaF and NaI to a concentration of 0.01-0.2 mol/L. The electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode is regarded as the positive pole, regulate the current density about 1mA/cm2～5mA/cm2At the time of electrolysisThe time is 20min to 40min, so that a large amount of hydroxide radicals accumulated by the cathode are rapidly combined with various ions in the electrolyte and attached to the surface of the foamed nickel. Washing the electrodeposited foam nickel with ethanol, and drying to obtain lamellar F-、I-A co-regulated ternary hydroxide.
From the practical example results, the invention can quickly and efficiently prepare various anion-controlled multi-hydroxide. The multi-element hydroxide prepared by the method has high quality and good uniformity, and has wide and excellent application in the fields of catalysis and the like.

Claims (1)

1. A method for preparing an anion-modulating polyhydroxide, characterized in that the method comprises the steps of:
(1) taking 250g/m2～300g/m2Cutting the foamed nickel with the thickness of 0.2 mm-1 mm into 6cm2The sheet is sequentially ultrasonically washed in acetone and ethanol and dried to be used as an electro-deposition carrier;
(2) mixing Fe (NO)3)3、Co(NO3)2、Ni(NO3)2Preparing 0.5-1 mol/L electrolyte according to different molar proportions, and simultaneously adding salt containing regulating ions, wherein the salt containing the regulating ions is KCl, NaF, KI or NaBr, the concentration of the salt is controlled to be 0.01-0.2 mol/L, and the salt is used as soon as possible in order to prevent the electrolyte from being deteriorated after being placed for a long time;
(3) the electrode clamp fixes and washes the foam nickel as the negative pole, the carbon rod or Pt electrode as the positive pole, soak in the electrolyte, regulate the current density to be 1mA/cm2～5mA/cm2The electrolysis time is 20min to 40 min;
(4) and washing the electrodeposited foamed nickel with ethanol, and drying to obtain the lamellar anion-regulated multi-hydroxide.
CN201910828203.2A 2019-09-03 2019-09-03 Method for preparing anion-controlled multi-hydroxide Active CN110373679B (en)

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