Porphyrin structure derivative, preparation method thereof and dyeing-flame-retardant-anti-dripping integrated polyester
A technology of derivatives, pyrrole derivatives, used in the field of porphyrin structure derivatives and their preparation, dyeing-flame-retardant-anti-droplet integrated polyester field, can solve accelerated decomposition, melt viscosity and strength decrease, environmental and human health hazards, etc.
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[0041] The present invention also provides a preparation method for the porphyrin structure derivative described in the above scheme, comprising the following steps:
[0042] Protocatechualdehyde and pyrrole derivatives are mixed for condensation reaction to obtain a porphyrin structural intermediate; the structure of the pyrrole derivative is shown in formula II; the structural formula of the porphyrin structural intermediate is shown in formula III:
[0043]
[0044] In Formula II~Formula III: R 1 The kind is consistent with formula I;
[0045] The porphyrin structure intermediate and phosphorus oxychloride are mixed for esterification to obtain the phosphorus-containing porphyrin structure intermediate; the structural formula of the phosphorus-containing porphyrin structure intermediate is shown in formula IV:
[0046]
[0047] In Formula IV, R 1 and R 2 The kind is consistent with formula I;
[0048] The phosphorous-containing porphyrin structure intermediate and...
Embodiment 1
[0073] The preparation of the porphyrin structure derivative of structure shown in formula I, in formula I: M is Cu 2+ , R 1 for H, R 2 for Concrete preparation steps are as follows:
[0074] (1) Preparation of porphyrin structural intermediate: Add 50 g of protocatechuic aldehyde and 500 mL of propionic acid into the reactor, start stirring and heating, control the reaction temperature to 130 ° C, then dilute 27 g of pyrrole in 50 mL of propionic acid, pass Add the pyrrole solution drop by drop to the reaction system with a constant pressure dropping funnel. After the addition, maintain the reaction temperature and continue the reaction for 1 hour. After the reaction, add 500 mL of methanol to the reaction system, refrigerate and stand for 12 hours in the refrigerator, and filter under reduced pressure. , the filter cake is washed with ethanol, and the porphyrin structure intermediate is obtained after drying; the infrared spectrum of the gained porphyrin structure interm...
Embodiment 2
[0081] The preparation of the porphyrin structure derivative of structure shown in formula I, in formula I: M is Fe 2+ , R 1 for R 2 for Concrete preparation steps are as follows:
[0082] (1) Preparation of porphyrin structural intermediate: Add 50g of protocatechuic aldehyde and 600mL of propionic acid into the reactor, start stirring and heating, control the reaction temperature to 135°C, then add 40g of 3-propenylpyrrole in 50mL of propionic acid Add 3-propenylpyrrole solution drop by drop to the reaction system through a constant pressure dropping funnel, maintain the reaction temperature after the addition, and continue the reaction for 1.5h; after the reaction, add 600mL of methanol to the reaction system Put it aside in cold storage for 12 hours, filter under reduced pressure, wash the filter cake with ethanol, and dry to obtain the porphyrin structure intermediate; the infrared spectrum identification shows that this step successfully synthesized the porphyrin s...
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Abstract
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