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Method for catalyzing propylene epoxidation in micro-channel by utilizing metalloporphyrin loaded titanium silicate molecular sieve

A titanium-silicon molecular sieve and metalloporphyrin technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of increasing the input cost of propylene oxide production, restricting the industrialization process, and high explosion-proof requirements, and achieves Screening and optimization of process conditions, high reaction selectivity and safety, and good operability

Inactive Publication Date: 2019-06-14
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This shortcoming correspondingly increases the production input cost of propylene oxide, and in addition, peracetic acid must be prepared in the production process, which has poor safety and high explosion-proof requirements, so the industrialization process of this method is limited.

Method used

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  • Method for catalyzing propylene epoxidation in micro-channel by utilizing metalloporphyrin loaded titanium silicate molecular sieve
  • Method for catalyzing propylene epoxidation in micro-channel by utilizing metalloporphyrin loaded titanium silicate molecular sieve
  • Method for catalyzing propylene epoxidation in micro-channel by utilizing metalloporphyrin loaded titanium silicate molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Weigh 1.2g TS-1, add 100mL 0.1mol / L chloroform solution of 3-aminopropyltrimethoxysilane and mix, N 2 Stir mechanically at room temperature for 12 hours during protection, filter, and wash with chloroform and dichloromethane several times until the washing liquid has no characteristic UV-visible absorption peak of porphyrin, and dry to obtain modified TS-1*; weigh 1.3g TS-1*, add dry 10mL pyridine, 40mg DMAP, 2mL triethylamine, 6g succinic anhydride, mechanically stir at room temperature for 20h, filter, wash with pyridine, dichloromethane and diethyl ether successively, and dry to obtain the new catalyst Ⅰ, which structure is like figure 1 shown.

[0042] Measure 100mL of propionic acid into a flask, heat and control the temperature of the oil bath to about 140°C, make the propionic acid slightly boil, add 1.17g of p-hydroxybenzaldehyde (9.57mmol), 2.67mL of benzaldehyde (26.3mmol) in sequence, and stir to make it Dissolve, and drop 2.43mL double-distilled pyrrole (3...

Embodiment 2

[0046] Weigh 1.2g TS-1, add 100mL 0.1mol / L chloroform solution of 3-aminopropyltrimethoxysilane and mix, N 2 Stir mechanically at room temperature for 12 hours during protection, filter, and wash with chloroform and dichloromethane several times until the washing liquid has no characteristic UV-visible absorption peak of porphyrin, and dry to obtain modified TS-1*; weigh 1.3g TS-1*, add dry 10mL pyridine, 40mg DMAP, 2mL triethylamine, 6g succinic anhydride, mechanically stir at room temperature for 20h, filter, wash with pyridine, dichloromethane and diethyl ether successively, and dry to obtain the new catalyst Ⅰ.

[0047] Measure 100mL of propionic acid into a flask, heat and control the temperature of the oil bath to about 140°C, make the propionic acid slightly boil, add 1.17g of p-hydroxybenzaldehyde (9.57mmol), 2.67mL of benzaldehyde (26.3mmol) in sequence, and stir to make it Dissolve, and drop 3.02mL double-distilled pyrrole (45mmol) in 5 minutes in the way of constant...

Embodiment 3

[0051] Weigh 1.2g TS-1, add 100mL 0.1mol / L chloroform solution of 3-aminopropyltrimethoxysilane and mix, N 2 Stir mechanically at room temperature for 12 hours during protection, filter, and wash with chloroform and dichloromethane several times until the washing liquid has no characteristic UV-visible absorption peak of porphyrin, and dry to obtain modified TS-1*; weigh 1.3g TS-1*, add dry 10mL pyridine, 40mg DMAP, 2mL triethylamine, 6g succinic anhydride, mechanically stir at room temperature for 20h, filter, wash with pyridine, dichloromethane and diethyl ether successively, and dry to obtain the new catalyst Ⅰ.

[0052] Measure 100mL of propionic acid into a flask, heat and control the temperature of the oil bath to about 140°C, make the propionic acid slightly boil, add 1.17g of p-hydroxybenzaldehyde (9.57mmol), 2.67mL of benzaldehyde (26.3mmol) in sequence, and stir to make it Dissolve, and drop 2.43mL double-distilled pyrrole (35mmol) in 5 minutes in the way of constant...

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Abstract

The invention discloses a method for catalyzing propylene epoxidation in a micro-channel by utilizing a metalloporphyrin loaded titanium silicate molecular sieve. According to the method, metalloporphyrin with catalytic activity on epoxidation reaction is grafted to a modified titanium silicate molecular sieve through a grafting method to prepare a novel catalyst with higher activity, and furthermore, the propylene epoxidation is catalyzed in a micro-reactor; a micro-channel reactor has micron-grade dispersion scales and continuous flowing of two phases, and fluid can obtain an extremely largespecific surface area, so that the fluid is subjected to efficient heat exchange with a wall surface and more deal mass transfer and heat exchange efficiency is obtained; compared with a traditionalreactor, accurate temperature, pressure and reaction time in the micro-reactor are controlled; and obtained propylene oxide has good selectivity, high yield and great safety and meets the industrial requirements better.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for catalyzing the epoxidation of propylene in a microchannel by using a titanium-silicon molecular sieve supported by a novel metalloporphyrin. Background technique [0002] Propylene oxide (PO) is an important basic organic chemical raw material and the third largest organic chemical product in the production of propylene derivatives after polypropylene and acrylonitrile. It is mainly used in the production of polyether, propylene glycol, polyurethane, etc., and is also the main raw material of the fourth-generation detergent nonionic surfactant, oil field demulsifier, pesticide emulsifier, etc., and has broad development prospects. At present, the industrial production of propylene oxide is mainly based on the chlorohydrin method and the co-oxidation method (also known as the cogeneration method or the Haakon method), and these two methods account for mor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89C07D303/04C07D301/12B01J8/00B01J19/00
Inventor 郭凯陈琳李昕齐豪刘壮苗珊珊
Owner NANJING UNIV OF TECH
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