Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of synthesis method of tetrazine hypercrosslinked porous photocatalyst

A technology of photocatalyst and synthesis method, applied in chemical instruments and methods, physical/chemical process catalysts, catalytic reactions, etc., can solve the problems of homogeneous catalysts that are difficult, difficult to recycle, expensive, etc., and achieve large specific surface area and density Effect of small and wide visible light absorption range

Active Publication Date: 2021-05-28
HENAN AGRICULTURAL UNIVERSITY
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it should be pointed out that these homogeneous catalysts are difficult to separate from the product, difficult to recycle, and some are very expensive

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of synthesis method of tetrazine hypercrosslinked porous photocatalyst
  • A kind of synthesis method of tetrazine hypercrosslinked porous photocatalyst
  • A kind of synthesis method of tetrazine hypercrosslinked porous photocatalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Place the methoxy-substituted bispyridine tetrazine monomer (165mg, 0.37mmol) and ferric chloride (2.4g, 14mmol) in a dry two-necked flask, vacuum 3-5 times under nitrogen protection, and then pass the needle Add 7.4mL of 1,2-dichloroethane into the flask, stir at room temperature for 0.5h, then add 1.33mL of dimethoxymethane into the flask, stir at 45°C for 5h, then raise the temperature to 90°C and continue the reaction for 19h. Then add 20mL of methanol to the flask, stir at 90°C for 0.5h, vacuum filter, wash with N,N-dimethylformamide and methanol, transfer the solid to the flask, add 20mL of concentrated hydrochloric acid, stir at room temperature for 2h, vacuum Suction filtration, after washing with N,N-dimethylformamide, methanol, and dichloromethane in sequence, the residue was subjected to Soxhlet extraction for 48 hours (methanol:dichloromethane=1:1), and dried in an oven to obtain the tetrazine Super-crosslinked porous photocatalyst TZ-HCP1 (brown black solid...

Embodiment 2

[0044] Place methoxy-substituted bispyridine tetrazine monomer (179mg, 0.4mmol) and iron trichloride (520mg, 3.2mmol) in a dry two-necked flask, vacuum 3-5 times under the protection of nitrogen, and then pour into the flask Add 1.6mL of 1,2-dichloroethane and 0.11mL of benzene, stir at room temperature for 0.5h, then add 0.29mL of dimethoxymethane into the flask, stir at 45°C for 5h, then raise the temperature to 90°C to continue the reaction for 19h. The reaction system was vacuum-filtered, washed successively with petroleum ether and acetone, the solid was transferred to a dry flask, 20 mL of hydrochloric acid (6M) was added, and stirred at room temperature for 2 h. Vacuum filtration, after washing with N,N-dimethylformamide, methanol and dichloromethane in sequence, Soxhlet extraction of the crude product with acetone as solvent for 48 hours, and drying in an oven at 80°C to obtain tetrazine supernatants Cross-linked porous photocatalyst TZ-HCP2@A (black solid powder) 241m...

Embodiment 3

[0046] Place methoxy-substituted bispyridine tetrazine monomer (103mg, 0.23mmol) and ferric trichloride (464mg, 2.86mmol) in a dry two-necked flask, evacuate 3-5 times under nitrogen protection, and then pour into the flask Add 1.43mL of 1,2-dichloroethane and 0.11mL of benzene, stir at room temperature for 0.5h, then add 0.26mL of dimethoxymethane into the flask, stir at 45°C for 5h, then raise the temperature to 90°C to continue the reaction for 19h. The reaction system was vacuum-filtered, washed successively with petroleum ether and acetone, the solid was transferred to a dry flask, 20 mL of hydrochloric acid (6M) was added, and stirred at room temperature for 2 h. Vacuum filtration, after washing with N,N-dimethylformamide, methanol and dichloromethane in sequence, Soxhlet extraction of the crude product with acetone as solvent for 48 hours, and drying in an oven at 80°C to obtain tetrazine supernatants Cross-linked porous photocatalyst TZ-HCP2@B (brown solid powder) 214m...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
specific surface areaaaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for synthesizing a tetrazine hypercrosslinked porous photocatalyst, which comprises the following steps: placing a precursor methoxy-substituted bispyridine tetrazine monomer, an aromatic block, and a catalyst, iron trichloride, in In a dry two-necked flask, add the solvent 1,2-dichloroethane and the cross-linking agent dimethoxymethane under the protection of nitrogen, stir at 45°C for 5-24 hours, then raise the temperature to 90°C and continue the reaction for 19-48 hours After the reaction, the tetrazine hypercrosslinked porous photocatalyst TZ‑HCPs can be prepared by treating with methanol and concentrated hydrochloric acid, vacuum filtration, Soxhlet extraction and drying. The TZ-HCPs catalyst obtained by this method has a small density, a large specific surface area and a wide range of visible light absorption, and can efficiently catalyze electrophilic compounds such as o-phenylenediamine and p-chlorobenzaldehyde under room temperature, air atmosphere and visible light irradiation. Coupling reaction between reagents, and has good reusability.

Description

technical field [0001] The invention relates to the technical field of organic synthesis and functional materials, in particular to the synthesis of a tetrazine hypercrosslinked porous photocatalyst and its application in the field of photocatalysis. Background technique [0002] Facing the challenges of the current energy and environmental crisis, photocatalysis has attracted more and more attention due to its mild and efficient reaction rate and green reaction. Since the 1970s, scientists have developed various inorganic semiconductor materials (photosensitizers or photocatalysts) based on elements such as titanium, gallium, cadmium, zinc, and tungsten. However, due to the limitation of the structure of inorganic substances, such substances have high toxicity, narrow absorption range of visible light, wide band gap, low utilization efficiency of sunlight, and poor selectivity when catalyzing the synthesis of organic substances. . The difference is that there are many kin...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06B01J35/10C07D235/18
CPCB01J31/06C07D235/18B01J2231/4283B01J35/60B01J35/39B01J35/647
Inventor 安万凯张慧星尚甜甜郑仕佳潘振良金秋杨湛昆
Owner HENAN AGRICULTURAL UNIVERSITY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com