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Method for synthesizing tetraphenylporphyrin by using return pipe type reactor

A technology of tubular reactor and tetraphenylporphyrin, applied in the direction of organic chemistry, can solve the problems of increasing the three wastes and regional reaction selectivity, using a large amount of catalyst, sticky acidic filtrate, etc., so as to avoid contact with toxic and harmful substances , Avoid raw material recovery process, avoid the effect of tar

Active Publication Date: 2021-02-05
CHEMVON BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] There are some problems when conventional laboratory equipment and reactors are put into the reaction, such as: the amount of catalyst used in the reaction process is large, resulting in waste; the increase in the three wastes and the poor selectivity of the regional reaction, more dihydroaryl porphyrin impurities are generated; the reaction In the process, because pyrrole is easy to polymerize, the color of the system is dark red, and the acidic filtrate is sticky, the composition is complex, and the waste liquid cannot be treated, etc., the overall reaction yield is also low
[0005] Therefore, for the process scale-up of this product, there are still many difficulties, and it is still necessary to find reaction conditions suitable for industrial scale-up

Method used

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  • Method for synthesizing tetraphenylporphyrin by using return pipe type reactor
  • Method for synthesizing tetraphenylporphyrin by using return pipe type reactor

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Effect test

Embodiment 1

[0033] 1) After the two reaction modules A1 and A2 are connected in parallel, they are connected in series with the two reaction modules B and C in sequence, and the microchannel reactor is replaced with a protonic acid; 106g (1mol) of benzaldehyde and 67g (1mol) of pyrrole are weighed and mixed into a homogeneous solution Put it into storage tank V-01, with a volume of about 170mL; weigh 680g of propionic acid and put it into storage tank V-02, with a volume of about 681mL;

[0034] 2) Control the volume flow rate of the mixed solution of benzaldehyde and pyrrole to 2.0mL / min, enter the first reaction module A1 by pump P-01 to preheat at 110°C; control the volume flow rate of propionic acid to 7.8mL / min by pump P- 02 Enter the second reaction module A2 to preheat 120°C; then enter the third reaction module B for mixing; when the mixed material enters the fourth reaction module C, 184.5g of nitrobenzene in the pre-storage tank V-03 Pump in; through the tube reactor delay pipel...

Embodiment 2

[0039] 1) After the two reaction modules A1 and A2 are connected in parallel, they are connected in series with the two reaction modules B and C in sequence, and the microchannel reactor is replaced with a protonic acid; 106g (1mol) of benzaldehyde and 67g (1mol) of pyrrole are weighed and mixed into a homogeneous solution Put it into storage tank V-01, with a volume of about 170mL; weigh 727g of acetic acid and put it into storage tank V-02, with a volume of about 693mL;

[0040] 2) Control the volume flow rate of the mixed solution of benzaldehyde and pyrrole to 2.0mL / min, enter the first reaction module A1 by pump P-01 to preheat 120°C; control the volume flow rate of acetic acid to 8.2mL / min by pump P-02 Enter the second reaction module A2 to preheat 115°C; then enter the third reaction module B for mixing; when the mixed material enters the fourth reaction module C, the compressed air is fed at 80cm3 / min; through the tube reaction The delay pipeline of the device is compl...

Embodiment 3

[0045] 1) After the two reaction modules A1 and A2 are connected in parallel, they are connected in series with the two reaction modules B and C in sequence, and the microchannel reactor is replaced with a protonic acid; 106g (1mol) of benzaldehyde and 67g (1mol) of pyrrole are weighed and mixed into a homogeneous solution Put it into storage tank V-01, with a volume of about 170mL; weigh 788g of acetic anhydride and put it into storage tank V-02, with a volume of about 730mL;

[0046] 2) Control the volume flow rate of the mixed solution of benzaldehyde and pyrrole to 2.0mL / min and enter the first reaction module A1 to preheat at 120°C through the pump P-01; control the volume flow rate of acetic anhydride to 9.2mL / min from the pump P- 02 Enter the second reaction module A2 to preheat at 115°C; then enter the third reaction module B for mixing; when the mixed material enters the fourth reaction module C, the compressed air is fed at 30cm3 / min; through the tube Reactor delay p...

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Abstract

The invention discloses a method for synthesizing tetraphenylporphyrin by using a return pipe type reactor, wherein the method comprises the steps: carrying out condensation reaction on benzaldehyde and pyrrole in an equal molar ratio in the presence of acid or anhydride deprotons and an oxidant by using the return pipe type reactor and controlling the temperature to 110-140 DEG C and the pressureto 0-0.2 MPa under a fluidity condition to synthesize the tetraphenylporphyrin. According to the process, the materials are uniformly mixed, the equivalent ratio of the materials in the reaction process is reduced, the use amount of a catalyst in the reaction process is reduced, the raw material conversion rate and the product selectivity are improved, side reactions and polymerization reactionsare reduced, the product separation and purification difficulty is reduced, and the reaction yield is remarkably improved.

Description

technical field [0001] The invention relates to the application of a reflux tube reactor in organic synthesis, in particular to a method for using a reflux tube reactor to react tetraphenylporphyrin, and belongs to the field of organic synthesis. Background technique [0002] Tetraphenylporphyrine, English name: meso-tetraphenylporphyrine, referred to as TPP, CAS: 917-23-7, molecular formula C 40 h 33 N 4 , is one of the most important compounds in porphyrin derivatives. It is an important luminescent material, sensitive material, semiconductor material, and its metal complexes are widely used in gas sensors, smart materials and sensor technology. [0003] The first porphyrin compounds obtained by people were extracted from living organisms. Since Hans Fisher synthesized iron protoporphyrin IX in 1929 and won the Nobel Prize, a major breakthrough has been made in the research of porphyrin synthesis. However, the synthetic method still starts with natural porphyrin compoun...

Claims

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Application Information

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IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 薛峰刘洪强
Owner CHEMVON BIOTECH CO LTD
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