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Preparation method of acid-base bifunctional c3n4 catalyst and cyclic carbonate

An acid-base bifunctional, C3N4 technology, applied in the field of preparation of acid-base bifunctional C3N4 catalysts, can solve the problems of complex preparation process, low catalytic ring reaction activity, small specific surface area and the like

Active Publication Date: 2018-06-19
HUNAN KAIMEITE GASES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the above report C 3 N 4 The preparation process is complicated and the yield is low
Using melamine as the precursor to prepare C 3 N 4 The yield is the highest, and the raw material is cheap, but the C prepared by the precursor 3 N 4 Due to its large block shape and small specific surface area, the activity of catalytic cycloaddition reaction is low, so it has not been reported.

Method used

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  • Preparation method of acid-base bifunctional c3n4 catalyst and cyclic carbonate
  • Preparation method of acid-base bifunctional c3n4 catalyst and cyclic carbonate
  • Preparation method of acid-base bifunctional c3n4 catalyst and cyclic carbonate

Examples

Experimental program
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Effect test

Embodiment example 1

[0015] At room temperature, 10mmol of melamine and 0.25mmol of hexafluorocyclotriphosphazene were fully ground, placed in a muffle furnace, heated to 180℃ at a heating rate of 2℃ / min, kept for 2h, and then heated to at a heating rate of 5℃ / min Keep at 450℃ for 3h, cool to room temperature and grind to obtain light yellow powder. Add the powder to 5wt% hydrochloric acid solution, stir for 6h, wash with deionized water to neutrality, and place in 60℃ oven to dry for 24h to obtain light yellow powder. Yellow powder is recorded as PC 3 N 4 -40 (180, 450).

Embodiment example 2

[0017] At room temperature, 10mmol of melamine and 5mmol of hexachlorocyclotriphosphazene were fully ground, placed in a muffle furnace, heated to 120°C at a heating rate of 2°C / min, maintained for 2h, and then heated to 530 at a heating rate of 5°C / min Keep it at ℃ for 3h, cool to room temperature and grind to obtain light yellow powder. Add the powder to 5wt% hydrochloric acid solution, stir for 6h, wash with deionized water to neutrality, place in 60℃ oven and dry for 24h to obtain light yellow Powder is recorded as PC 3 N 4 -2 (120, 530).

Embodiment example 3

[0019] At room temperature, 10mmol of melamine and 2.5mmol of hexahydroxycyclotriphosphazene were fully ground, placed in a muffle furnace, heated to 250℃ at a heating rate of 2℃ / min, kept for 2h, and then heated to at a heating rate of 5℃ / min Keep at 580°C for 3h, cool to room temperature and grind to obtain a light yellow powder. Add the powder to a 5wt% hydrochloric acid solution, stir for 6h, wash with deionized water to neutrality, and place in an oven at 60°C to dry for 24h to obtain a light yellow powder. Yellow powder is recorded as PC 3 N 4 -4 (250, 580).

[0020] figure 1 P-C shown 3 N 4 -2 (120, 530) XRD spectra, can prove that the prepared catalyst is C 3 N 4 material; figure 2 P-C shown 3 N 4 -2 (120, 530) XPS spectrum, it can prove that P was successfully introduced into C 3 N 4 Structure; from image 3 P-C shown 3 N 4 -2(120,530) TG chart, it can be seen that C after doping P 3 N 4 Have good thermal stability.

[0021] Epoxide and CO 2 Cycloaddition reaction to pre...

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Abstract

The preparation method of an acid-alkali bi-functionalized C3N4 catalyst comprises the following steps: fully grinding solid melamine and solid cyclotriphosphazene according to a mole ratio of (2-40):1 at a room temperature, placing the mixture in a muffle furnace, raising the temperature to 120-250 DEG C in a speed of 2 DEG C / min, maintaining the temperature for 2 hours, then raising the temperature to 450 to 580 DEG C in a speed of 5 DEG C / min, maintaining the temperature for 3 hours, cooling to the temperature, grinding to obtain light yellow powder, adding the powder into a hydrochloric acid solution (5 wt%), stirring the hydrochloric acid solution for 6 hours, washing the powder by deionized water until the powder turn neutral, and drying the powder in a baking oven with a temperature of 60 DEG C for 24 hours to obtain the acid-alkali bi-functionalized C3N4 catalyst. The prepared acid-alkali bi-functionalized C3N4 catalyst can high efficiently and high selectively catalyze the cyclo-addition reactions between epoxide and CO2 to prepare cyclic carbonic ester without any solvent under mild conditions, and the activity is barely changed after several times of circulation.

Description

【Technical Field】 [0001] The invention relates to an acid-base bifunctional C for catalyzing the cycloaddition reaction of epoxide and carbon dioxide to prepare cyclic carbonate 3 N 4 Catalyst preparation method. 【Background technique】 [0002] With the progress of science and technology and the development of industrialization, a large amount of fossil fuels are consumed, and CO in the atmosphere 2 The sharp increase in concentration has led to global warming, melting of glaciers, rising sea levels and other greenhouse effects, which seriously threaten human survival and development. But it’s worth noting that at the same time CO 2 It is also a rich and cheap C1 resource, which is expected to replace toxic CO, phosgene and other raw materials to synthesize high value-added chemical products. Although about CO 2 There have been many researches on resource utilization, but through CO 2 Cycloaddition reaction with epoxides to synthesize cyclic carbonates is one of the few CO that h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24C07D317/36
CPCB01J27/24C07D317/36
Inventor 尹双凤兰东辉祝恩福李文盛张晓辉郭静楠杨泛明陈浪
Owner HUNAN KAIMEITE GASES