CN115634693A - Preparation method of nano composite material with hollow tube structure and application of nano composite material in catalysis of ammonia borane alcoholysis for hydrogen production - Google Patents

Preparation method of nano composite material with hollow tube structure and application of nano composite material in catalysis of ammonia borane alcoholysis for hydrogen production Download PDF

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CN115634693A
CN115634693A CN202211214002.1A CN202211214002A CN115634693A CN 115634693 A CN115634693 A CN 115634693A CN 202211214002 A CN202211214002 A CN 202211214002A CN 115634693 A CN115634693 A CN 115634693A
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stirring
hollow tube
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CN115634693B (en
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廖锦云
张静
宋春霞
唐瑾婷
曾威
李源钟
冯裕发
王慧泽
陈晓东
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Huizhou University
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Abstract

The application discloses a preparation method of a nano composite material with a hollow tube structure, relating to the technical field of nano catalytic materials; the method comprises the following steps: s1, dissolving soluble divalent copper salt and divalent nickel salt in water to prepare a mixed salt solution A; s2, adding 2-20 mmol of oxalate into water, stirring and dissolving to form a solution B; s3, slowly dripping the solution B into the solution A through a separating funnel under the condition of high-speed stirring to form a solution C, and stirring for 5-15 min; s4, transferring the solution C to a reaction kettle, reacting for 2-10 h at 120-200 ℃, filtering, washing, taking the solid at the bottom of the reaction kettle, and reacting for 1-5 h in a muffle furnace at 250-350 ℃; the application also provides an application of the nano composite material prepared by the preparation method as a catalyst in catalyzing alcoholysis of ammonia borane to produce hydrogen; the preparation process provided by the application is simple to operate, low in cost and easy for industrial production, and has an excellent effect on catalyzing ammonia borane to produce hydrogen.

Description

Preparation method of nano composite material with hollow tube structure and application of nano composite material in catalysis of ammonia borane alcoholysis for hydrogen production
Technical Field
The application relates to the technical field of nano catalytic materials, in particular to a preparation method of a nano composite material with a hollow tube structure and application of the nano composite material in catalyzing alcoholysis of ammonia borane to produce hydrogen.
Background
Hydrogen is considered to be the most desirable alternative to fossil energy as a clean energy source. The development of safe, efficient and stable hydrogen storage materials is one of the biggest challenges facing current research on hydrogen energy application. Ammonia borane (NH) 3 BH 3 AB) owing to its higher hydrogen storage density (146 g. L) -1 19.6 percent of mass fraction), safety, no toxicity, high chemical stability and the like, and becomes an important chemical solid hydrogen storage material. The ammonia borane hydrolysis hydrogen production reaction has mild conditions, but needs to be carried out in the presence of a suitable catalyst. The alcoholysis hydrogen production rate of ammonia borane can be obviously improved by adjusting the active components, the particle size, the dispersion degree of the active components, the electronic structure and the like of the catalyst.
Currently, ammonia borane decomposition hydrogen production has three modes: thermal decomposition, hydrolysis and alcoholysis. Because of the high AB thermal decomposition temperature and the associated polymer [ -B ] in the thermal decomposition hydrogen releasing process 3 N 3 H 6 -] n And gaseous by-product NH 3 、B 2 H 6 And B 3 N 3 H 6 And various byproducts are generated, so that the method is difficult to be practically applied. Compared with ammonia borane pyrolysis, the ammonia borane can release 3 equivalent hydrogen by hydrolysis or alcoholysis at room temperature by introducing a proper catalytic system.
Ammonia gas is released by ammonia borane hydrolysis in a concentrated solution, the ammonia gas can generate a toxic effect on a Pt-based fuel cell catalyst, and hydrolysis products of AB cannot be recovered due to strong B-O bonds. Compared with the former two decomposition hydrogen production modes, the AB alcoholysis hydrogen production method has the advantages of more stability under environmental conditions and generation of pure H 2 No ammonia is released, and decomposition by-products are easily converted into ammonia borane. Therefore, the research on a system for producing hydrogen by catalyzing the alcoholysis of ammonia borane has important practical significance.
Noble metals (such as Rh, pd, ru and Pt) are widely studied in ammonia borane catalyzed alcoholysis hydrogen production reaction; however, the precious metal cannot realize large-scale industrial application due to the problems of reserve content and cost of the precious metal, so that in the field of ammonia borane catalytic hydrogen production, the prepared catalyst is one of the preconditions for realizing large-scale industrial popularization of ammonia borane catalytic hydrogen production by using metal elements with high reserve content and low cost and a simple preparation method.
Disclosure of Invention
The application aims to provide a preparation method of a nano composite material with a hollow tube structure and application of the nano composite material in hydrogen production by catalyzing alcoholysis of ammonia borane.
In order to achieve the technical purpose, the application provides a preparation method of a nanocomposite material with a hollow tube structure and an application of the nanocomposite material in catalyzing alcoholysis of ammonia borane to produce hydrogen, and in a first aspect, the application provides a preparation method of a nanocomposite material with a hollow tube structure, which comprises the following steps:
s1, dissolving soluble divalent copper salt and divalent nickel salt in water to prepare a mixed salt solution A;
s2, adding 2-20 mmol of oxalate into 20-100 mL of water, and stirring for dissolving to form a solution B;
s3, slowly dripping the solution B into the solution A through a separating funnel under the condition of high-speed stirring to form a solution C, and stirring for 5-15 min;
and S4, transferring the solution C to a reaction kettle, reacting for 2-10 h at 120-200 ℃, filtering, washing, and reacting for 1-5 h at 250-350 ℃ in a muffle furnace.
Preferably, the oxalate salt is sodium oxalate.
Preferably, the step S1 is configured to contain Ni 2+ /Cu 2+ Mixed salt solution a in a molar ratio of 4:1.
Preferably, the soluble divalent copper salt is selected from one of copper chloride, copper sulfate, copper nitrate and copper acetate.
Among them, copper acetate is more preferable.
Preferably, the soluble divalent nickel salt is selected from one of nickel chloride, nickel sulfate, nickel nitrate and nickel acetate.
Among them, nickel acetate is more preferable.
Preferably, in step S4, the reaction kettle bottom solid is reacted in a muffle furnace at 350 ℃ for 4h.
Preferably, in step S2, cu 2+ ：Ni 2+ ：C 2 O 4 2- Is 1:4:10.
in a second aspect, the present application provides a use of the nanocomposite prepared by any of the above preparation methods as a catalyst for catalyzing alcoholysis of ammonia borane to produce hydrogen.
Compared with the prior art, the beneficial effect of this application lies in:
(1) The invention adopts a hydrothermal synthesis method, oxalate is skillfully selected as a precipitator to generate a precursor of nickel oxide-copper oxide precipitate, and a proper calcination temperature is selected to calcine and synthesize the composite hollow nanotube, so that the nickel-copper ratio in the raw materials is effectively set in the process, the whole preparation process is simple to operate, environment-friendly, very good in experimental reproducibility, low in cost, easy for industrial production, and capable of producing the nickel oxide-copper oxide nano hollow tube in a large scale;
(2) The nickel oxide-copper oxide nano material prepared by the invention has better performance in the aspect of catalyzing alcoholysis of ammonia borane to produce hydrogen, and is expected to realize industrial preparation of catalysts for catalyzing hydrogen production.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is an XRD spectrum of a sample obtained in example 3;
FIG. 2 is a SEM photograph of a sample obtained in example 3;
FIG. 3 is a SEM photograph of a sample obtained in example 4;
FIG. 4 is a SEM photograph of a sample obtained in example 5;
FIG. 5 is a SEM photograph of a sample obtained in example 6.
Detailed Description
The present invention will now be described in detail with reference to the following examples, in order to make the objects, features and advantages of the present invention more comprehensible. Several embodiments of the invention are given below. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete:
example 1
S1, dissolving 4mmol of nickel acetate and 1mmol of copper acetate in 40mL of water, and stirring for 3 minutes to form a mixed solution A;
s2, adding 10mmol of sodium oxalate into 40mL of water, and stirring for dissolving; stirring the solution B at a high speed;
s3, slowly dropwise adding the solution B to the solution A through a separating funnel, mixing to form a solution C, and continuously stirring for 5min;
s4, transferring the solution C into a 100mL reaction kettle to react for 6 hours at 170 ℃; and (3) filtering and washing the solid at the bottom of the reaction kettle, and reacting for 4 hours at 250 ℃ in a muffle furnace to obtain composite powder, namely a target product.
About 5mL of hydrogen gas can be generated in 1 minute by taking 10mg of the powder of the complex prepared by the above method and putting the powder into a methanol solution containing 5mmol of sodium hydroxide and 3mmol of ammonia borane as a catalyst.
Example 2
S1, dissolving 4mmol of nickel acetate and 1mmol of copper acetate in 40mL of water, and stirring for 3 minutes to form a mixed solution A;
s2, adding 10mmol of sodium oxalate into 40mL of water, and stirring for dissolving; stirring the solution B at a high speed;
s3, slowly dropwise adding the solution B to the solution A through a separating funnel, mixing to form a solution C, and continuously stirring for 5min;
s4, transferring the solution C into a 100mL reaction kettle to react for 6h at 170 ℃; and (3) filtering and washing the solid at the bottom of the reaction kettle, and reacting for 4 hours in a muffle furnace at 300 ℃ to obtain composite powder, namely the target product.
About 10mL of hydrogen gas can be generated in 1 minute by taking 10mg of the powder of the compound prepared by the above method and putting the powder into a methanol solution containing 5mmol of sodium hydroxide and 3mmol of ammonia borane as a catalyst.
Example 3
S1, dissolving 4mmol of nickel acetate and 1mmol of copper acetate in 40mL of water, and stirring for 3 minutes to form a mixed solution A;
s2, adding 10mmol of sodium oxalate into 40mL of water, and stirring for dissolving; stirring the solution B at a high speed;
s3, slowly dropwise adding the solution B to the solution A through a separating funnel, mixing to form a solution C, and continuously stirring for 5min;
s4, transferring the solution C into a 100mL reaction kettle to react for 6h at 170 ℃; and (3) filtering and washing the solid at the bottom of the reaction kettle, and reacting for 4 hours in a muffle furnace at 350 ℃ to obtain composite powder, namely the target product.
About 20mL of hydrogen gas can be generated in 1 minute by taking 10mg of the powder of the compound prepared by the above method and putting the powder into a methanol solution containing 5mmol of sodium hydroxide and 3mmol of ammonia borane as a catalyst.
Further referring to fig. 1 and 2, it can be seen from fig. 1 that the crystallization effect of the target product is better, and it can be seen from fig. 2 that the target product is in a hollow tube structure and has a good forming effect.
Example 4
S1, dissolving 4mmol of nickel acetate and 1mmol of copper acetate in 40mL of water, and stirring for 3 minutes to form a mixed solution A;
s2, adding 10mmol of sodium oxalate into 40mL of water, and stirring for dissolving; stirring the solution B at a high speed;
s3, slowly dropwise adding the solution B to the solution A through a separating funnel, mixing to form a solution C, and continuously stirring for 5min;
s4, transferring the solution C into a 100mL reaction kettle to react for 6h at 170 ℃; and (3) filtering and washing the solid at the bottom of the reaction kettle, and reacting for 4 hours in a muffle furnace at 400 ℃ to obtain composite powder, namely the target product.
About 7mL of hydrogen gas can be generated in 1 minute by taking 10mg of the powder of the complex prepared by the above method and putting the powder into a methanol solution containing 5mmol of sodium hydroxide and 3mmol of ammonia borane as a catalyst.
Referring further to fig. 3, it can be seen from fig. 3 that no nanotube tube is formed in the final target product, resulting in nanorod agglomerates with a diameter of 300-400 nm.
Example 5
S1, dissolving 4mmol of nickel acetate and 1mmol of copper acetate in 40mL of water, and stirring for 3 minutes to form a mixed solution A;
s2, adding 10mmol of hexamethylenetetramine into 40mL of water, and stirring for dissolving; stirring the solution B at a high speed;
s3, slowly dropwise adding the solution B to the solution A through a separating funnel, mixing to form a solution C, and continuously stirring for 5min;
s4, transferring the solution C into a 100mL reaction kettle to react for 6h at 170 ℃; and (3) filtering and washing the solid at the bottom of the reaction kettle, and reacting for 4 hours in a muffle furnace at 350 ℃ to obtain composite powder, namely the target product.
About 8mL of hydrogen gas can be generated in 1 minute by taking 10mg of the powder of the complex prepared by the above method and putting the powder into a methanol solution containing 5mmol of sodium hydroxide and 3mmol of ammonia borane as a catalyst.
With further reference to fig. 4, it can be seen from fig. 4 that the target product is not formed by nano hollow tubes at all, and the nano sheets are obtained.
Example 6
S1, dissolving 4mmol of nickel acetate and 1mmol of copper acetate in 40mL of water, and stirring for 3 minutes to form a mixed solution A;
s2, adding 10mmol of sodium hydroxide into 40mL of water, and stirring for dissolving; stirring the solution B at a high speed;
s3, slowly dropwise adding the solution B to the solution A through a separating funnel, mixing to form a solution C, and continuously stirring for 5min;
s4, transferring the solution C into a 100mL reaction kettle to react for 6h at 170 ℃; and (3) filtering and washing the solid at the bottom of the reaction kettle, and reacting for 4 hours in a muffle furnace at 350 ℃ to obtain composite powder, namely the target product.
About 8mL of hydrogen gas can be generated in 1 minute by taking 10mg of the powder of the complex prepared by the above method and putting the powder into a methanol solution containing 5mmol of sodium hydroxide and 3mmol of ammonia borane as a catalyst.
With further reference to fig. 5, it can be seen from fig. 5 that the target product is not finally formed with the nano hollow tubes, resulting in nano particles.
Example 7
S1, dissolving 4mmol of nickel acetate and 1mmol of copper acetate in 40mL of water, and stirring for 3 minutes to form a mixed solution A;
s2, adding 2mmol of sodium oxalate into 40mL of water, and stirring for dissolving; stirring the solution B at a high speed;
s3, slowly dropwise adding the solution B to the solution A through a separating funnel, mixing to form a solution C, and continuously stirring for 5min;
s4, transferring the solution C into a 100mL reaction kettle to react for 6h at 170 ℃; and (3) filtering and washing the solid at the bottom of the reaction kettle, and reacting for 4 hours in a muffle furnace at 350 ℃ to obtain composite powder, namely the target product.
About 9mL of hydrogen gas can be generated in 1 minute by taking 10mg of the powder of the compound prepared by the above method and putting the powder into a methanol solution containing 5mmol of sodium hydroxide and 3mmol of ammonia borane as a catalyst.
Example 8
S1, dissolving 4mmol of nickel acetate and 1mmol of copper acetate in 40mL of water, and stirring for 3 minutes to form a mixed solution A;
s2, adding 5mmol of sodium oxalate into 40mL of water, and stirring for dissolving; stirring the solution B at a high speed;
s3, slowly dropwise adding the solution B to the solution A through a separating funnel, mixing to form a solution C, and continuously stirring for 5min;
s4, transferring the solution C into a 100mL reaction kettle to react for 6h at 170 ℃; and (3) filtering and washing the solid at the bottom of the reaction kettle, and reacting for 4 hours in a muffle furnace at 350 ℃ to obtain composite powder, namely a target product.
About 14mL of hydrogen gas can be generated in 1 minute by taking 10mg of the powder of the complex prepared by the above method and putting the powder into a methanol solution containing 5mmol of sodium hydroxide and 3mmol of ammonia borane as a catalyst.
Example 9
S1, dissolving 4mmol of nickel acetate and 1mmol of copper acetate in 40mL of water, and stirring for 3 minutes to form a mixed solution A;
s2, adding 15mmol of sodium oxalate into 40mL of water, and stirring for dissolving; stirring the solution B at a high speed;
s3, slowly adding the solution B into the solution A through a separating funnel, mixing to form a solution C, and continuously stirring for 5min;
s4, transferring the solution C into a 100mL reaction kettle to react for 6h at 170 ℃; and (3) filtering and washing the solid at the bottom of the reaction kettle, and reacting for 4 hours in a muffle furnace at 350 ℃ to obtain composite powder, namely the target product.
About 16mL of hydrogen gas can be generated in 1 minute by taking 10mg of the powder of the complex prepared by the above method and putting the powder into a methanol solution containing 5mmol of sodium hydroxide and 3mmol of ammonia borane as a catalyst.
Example 10
S1, dissolving 4mmol of nickel acetate and 1mmol of copper acetate in 40mL of water, and stirring for 3 minutes to form a mixed solution A;
s2, adding 20mmol of sodium oxalate into 40mL of water, and stirring for dissolving; stirring the solution B at a high speed;
s3, slowly dropwise adding the solution B to the solution A through a separating funnel, mixing to form a solution C, and continuously stirring for 5min;
s4, transferring the solution C into a 100mL reaction kettle to react for 6h at 170 ℃; and (3) filtering and washing the solid at the bottom of the reaction kettle, and reacting for 4 hours in a muffle furnace at 350 ℃ to obtain composite powder, namely the target product.
About 12mL of hydrogen gas can be generated in 1 minute by taking 10mg of the powder of the compound prepared by the above method and putting the powder into a methanol solution containing 5mmol of sodium hydroxide and 3mmol of ammonia borane as a catalyst.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The above description is only for the preferred embodiment of the present application and should not be taken as limiting the present application in any way, and all simple modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present application are intended to be included within the scope of the present application.

Claims (8)

1. A preparation method of a nano composite material with a hollow tube structure is characterized by comprising the following steps: the method comprises the following steps:
s1, dissolving soluble divalent copper salt and divalent nickel salt in water to prepare a mixed salt solution A;
s2, adding 2-20 mmol of oxalate into water, stirring and dissolving to form a solution B;
s3, slowly dripping the solution B into the solution A through a separating funnel under the condition of high-speed stirring to form a solution C, and stirring for 5-15 min;
and S4, transferring the solution C to a reaction kettle, reacting for 2-10 h at 120-200 ℃, filtering, washing, taking the solid at the bottom of the reaction kettle, and reacting for 1-5 h at 250-350 ℃ in a muffle furnace.
2. The method for producing a hollow-tube structured nanocomposite material according to claim 1, wherein: the oxalate is sodium oxalate.
3. The method for preparing a hollow tube structured nanocomposite material according to claim 1, characterized in that: is configured to contain Ni in step S1 2+ /Cu 2+ Mixed salt solution a at a molar ratio of 4:1.
4. The hollow tube structure of claim 1, wherein: the soluble cupric salt is selected from one of cupric chloride, cupric sulfate, cupric nitrate and cupric acetate.
5. The method for preparing a hollow tube structured nanocomposite material according to claim 1, characterized in that: the soluble divalent nickel salt is selected from one of nickel chloride, nickel sulfate, nickel nitrate and nickel acetate.
6. The method for preparing a hollow tube structured nanocomposite material according to claim 1, characterized in that: in step S4, the reaction kettle bottom solid is reacted in a muffle furnace at 350 ℃ for 4h.
7. The method for preparing a hollow tube structured nanocomposite material according to claim 1, characterized in that: in step S2, cu 2+ ：Ni 2+ ：C 2 O 4 2- Is 1:4:10.
8. use of the nanocomposite prepared by the preparation method according to any one of claims 1 to 7 as a catalyst for catalyzing alcoholysis of ammonia borane to produce hydrogen.
CN202211214002.1A 2022-09-30 2022-09-30 Preparation method of nanocomposite with hollow tube structure and application of nanocomposite in catalyzing aminoborane alcoholysis to produce hydrogen Active CN115634693B (en)

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CN108996557A (en) * 2018-06-22 2018-12-14 安徽师范大学 A kind of hollow ball structure nickel oxide/copper oxide composite nano materials and preparation method thereof
CN109225284A (en) * 2017-07-11 2019-01-18 中国科学院理化技术研究所 Hydrogen storage material decomposition and desorption system
CN109663595A (en) * 2018-12-11 2019-04-23 中科廊坊过程工程研究院 A kind of copper based composite metal oxidate hollow microsphere, preparation method and the usage

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN105381800A (en) * 2014-09-09 2016-03-09 中国科学院大连化学物理研究所 Non-noble metal oxide combustion catalyst, and preparation method and use thereof
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