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Preparation method and application of water-soluble porphyrin-stabilized metal nanoparticle catalyst

A water-soluble, porphyrin technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as agglomeration and catalytic performance degradation

Active Publication Date: 2021-11-05
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The high surface energy of ultra-small nanoparticles may agglomerate due to thermodynamic instability, thereby reducing their catalytic performance

Method used

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  • Preparation method and application of water-soluble porphyrin-stabilized metal nanoparticle catalyst
  • Preparation method and application of water-soluble porphyrin-stabilized metal nanoparticle catalyst
  • Preparation method and application of water-soluble porphyrin-stabilized metal nanoparticle catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] First, polyethylene glycol monomethyl ether 350 (17.5g, 50mmol, n in polyethylene glycol monomethyl ether represents the number of units, and the value is 8-9) and p-benzenesulfonamide chloride (10g, 50mmol) Dissolve in 150mL dichloromethane, add 10mL triethylamine, react overnight to obtain compound 1, and then react the above compound 1 (16.7g, 33mmol) with p-hydroxybenzaldehyde (3.66g, 30mmol) for two hours to obtain compound 2. Finally, compound 2 (2.976g, 6mmol) and pyrrole (414uL, 6mmol) were dissolved in 600mL dichloromethane and stirred for 15min, and boron trifluoride ether (75μL, 0.6mmol), triethyl orthoacetate (1.09mL , 0.6mmol), chloranil (1.11g, 4.5mmol) were reacted in the dark for 20h under a nitrogen atmosphere. The product is rotary evaporated, separated and purified to obtain the final product TPP-PEG 350 , the specific structural formula is as follows:

[0041] n represents the number in the unit, and the value is 8-9.

[0042] figure 1 and fi...

Embodiment 2

[0044] The preparation scheme that the present invention adopts comprises the following steps

[0045] Step 1: Put 5×10 -3 mmolTPP-PEG 350 (prepared in Example 1) was dissolved in deionized water (8 mL) and stirred in a round bottom flask.

[0046] Step 2: Put the 5×10 -3 One mmol of rhodium nitrate solution was dissolved in deionized water (1 mL), added dropwise to the aqueous solution obtained in step 1, and stirred until uniform in an ice-bath environment.

[0047] Step 3: Divide the 5×10 -2 One mmol of sodium borohydride was dissolved in 1 mL of deionized water, and added dropwise at a rate of 3 min / mL to the ice-bath mixed solution obtained in step 2, and reacted for 2 hours. Water-soluble porphyrin-stabilized rhodium nanoparticles (RhNP / TPP-PEG 350 )catalyst.

[0048]The rhodium nitrate solution was replaced by ruthenium trichloride and potassium tetrachloropalladate respectively, and the above operations were repeated to obtain water-soluble porphyrin-stabilized p...

Embodiment 3

[0050] Rhodium metal nanoparticles (RhNP / TPP-PEG) prepared according to embodiment 2 350 ) catalyst in the catalytic ammonia (NH 3 BH 3 ) The concrete steps of borane hydrolysis hydrogen production are as follows:

[0051] NH 3 BH 3 +4H 2 O→NH 4 B(OH) 4 +3H 2 (g)

[0052] Step 1: Dissolving an appropriate amount of ammonia borane in deionized water to form a 0.5mmol / L solution;

[0053] Step 2: Put the 4×10 -3 mmol RhNP / TPP-PEG 350 Dissolved in deionized water (4mL), then the solution was placed in the reactor, and the reactor was sealed and stirred;

[0054] Step 3: Take 1 mL of the ammonia borane solution in Step 1 with a syringe, and quickly inject it into the reactor in Step 2, and start timing at the same time;

[0055] Step 4: Record the hydrogen volume at the corresponding time.

[0056] RhNP / TPP-PEG in the above step 2 350 Respectively replaced by RuNP / TPP-PEG 350 and PdNP / TPP-PEG 350 , the relationship between the reaction time of the ruthenium nanopar...

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Abstract

The invention provides a preparation method of a novel water-soluble porphyrin-stabilized metal nanoparticle catalyst and application of the novel water-soluble porphyrin-stabilized metal nanoparticle catalyst in catalysis of ammonia borane hydrolysis for hydrogen production. A metal salt is used as a raw material, water-soluble porphyrin (TPP-PEG350) is used as a stabilizer, the metal salt and the water-soluble porphyrin (TPP-PEG350) are fully stirred and mixed in deionized water, and then under the action of a reducing agent sodium borohydride, the metal ions are reduced to atoms. Metal atoms are combined with oxygen on a PEG chain on water-soluble porphyrin (TPP-PEG350) and nitrogen atoms on a large ring, so that metal nanoparticles are stabilized on porphyrin molecules, and ammonia borane is catalyzed to be hydrolyzed to produce hydrogen. By comparing the hydrogen production efficiency of ammonia borane under the conditions of different metal catalysts, different substance amounts of catalysts, different stabilizer contents, different ammonia borane concentrations and the like, the catalyst is found to have good ammonia borane hydrogen production catalysis performance, and cyclic experiments are carried out to show that the catalyst has good stability and cyclicity.

Description

technical field [0001] The invention belongs to the field of functional materials, and relates to a preparation method and application of a novel water-soluble porphyrin-stabilized nanoparticle catalyst. Background technique [0002] Hydrogen is considered as an environmentally friendly fuel due to its harmless by-products and renewability, and is expected to become a clean energy source to solve the shortage of fossil materials. Ammonia borane and formic acid have been widely used in research. Ammoniaborane is considered to be one of the most promising chemical hydride candidates due to its very high capacity and excellent stability under ambient conditions. [0003] So far, there have been many reports on the preparation and optimization of metal nanoparticle catalysts. It was found that the catalytic activity of metal nanoparticle catalysts largely depends on the metal nanoparticles and support and the interaction between them. The high surface energy of ultra-small nan...

Claims

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Application Information

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IPC IPC(8): C07D487/22B01J31/02B01J31/06B01J37/16C01B3/06
CPCC07D487/22B01J31/0254B01J31/069B01J37/16C01B3/065C01B2203/1041B01J35/23Y02E60/36
Inventor 晏佳莹周宇航刘湘张诺诺刘根江
Owner CHINA THREE GORGES UNIV
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