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Preparation of catechol-derived porous polymer and photocatalytic application of catechol-derived porous polymer loaded with high-spin monatomic iron

A porous polymer, catechol technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, organic chemistry, etc., can solve the difficulty of styrene oxide selectivity At the same time reaching 80%, system pollution, high cost problems

Active Publication Date: 2021-02-05
DEEPCHEM TECH (BEIJING) CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these catalysts have a single structure and are mainly porphyrin iron, and most of these catalytic systems need to introduce sacrificial agents or oxidants, which will cause system pollution, and some of them need to be heated to react.
[0005] At present, in the research on the reaction of preparing styrene oxide from styrene (Ding Liqin, Zhang Juntao, Liang Shengrong, Wang Xiaoquan, Research Progress on Catalysts for the Preparation of Styrene Oxide by Styrene Epoxidation, Journal of Xi'an Shiyou University, 2011, 26, 71 -77; Bai Xiangxiang, Guan Xiuhua, Shen Jian, Research progress of styrene epoxidation, Chemical Science and Technology, 2010, 18, 78-84; Gao Xiaohong, Feng Huixia, Research progress of catalysts for styrene epoxidation to styrene oxide , Applied Chemical Industry, 43,1489-1492), the conversion rate of most of styrene is lower than 90% or the selectivity of styrene oxide is lower than 90% (as the Chinese patent of publication number CN103012323A discloses styrene epoxidation The reaction prepares styrene oxide, the catalyst is molybdenum Schiff base complex 2-acetylpyridine anthraniophenol molybdenum complex, the conversion rate of styrene is 69.35%, and the selectivity of styrene oxide is 80.19% The publication number is CN103204830A, which discloses a method for catalyzing the oxidation of styrene with a heteroatom molecular sieve catalyst modified by soluble zinc salt, and the conversion rate of styrene and the selectivity of styrene oxide are difficult to reach more than 80% simultaneously; the publication number For the patent of CN101972665A, Co2+ is used as the active component, and the amino-functionalized mesoporous molecular sieve SBA-15 ion adsorption method is used to adsorb Co2+ to prepare the styrene epoxidation catalyst, and the selectivity of styrene oxide is up to 63.4%), However, if both are higher than 90%, it is often necessary to introduce an oxidizing agent or the reaction conditions are relatively harsh, and the cost of industrial application is relatively high.

Method used

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  • Preparation of catechol-derived porous polymer and photocatalytic application of catechol-derived porous polymer loaded with high-spin monatomic iron
  • Preparation of catechol-derived porous polymer and photocatalytic application of catechol-derived porous polymer loaded with high-spin monatomic iron
  • Preparation of catechol-derived porous polymer and photocatalytic application of catechol-derived porous polymer loaded with high-spin monatomic iron

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] A kind of preparation of porous polymer, step is as follows:

[0075]In 1,3,5-tris(3,4-dimethoxybenzyl)benzene (0.4mmol), 9,9-dimethyl-2,7-fluorenedial (0.6mmol), acetic anhydride (20mmol) Add 100 mL of dichloromethane solvent into the mixed system with ferric chloride (0.08 mmol), and react with magnetic stirring at 25° C. for 48 h. Ferric chloride (72 mmol) was added to the system again, and the reaction was performed under magnetic stirring at 25°C for 12 h under an argon atmosphere. Then add methanol to the system to quench, filter under reduced pressure, and wash the solid residue with water and methanol to obtain the product (POG-OMe) shown in formula 2 with a yield of 91%. BET characterization of POG-OMe (see accompanying drawing figure 1 ), the results show that at lower relative pressure (P / P 0 2 g -1 . Afterwards, carry out infrared characterization and nuclear magnetic characterization to POG-OMe (see accompanying drawing figure 2 ), the infrared char...

Embodiment 2

[0078] A preparation of a catechol-derived porous polymer, the steps are as follows:

[0079] Weigh 100 mg of POG-OMe and add 200 mL of CH under argon 2 Cl 2 , the reaction system was placed at -20°C, boron tribromide (1 mL) was added, and the reaction system was transferred to an oil bath at 50°C, and stirred by magnetic force for 48 hours. Deionized water was added to quench the reaction, and the solid residue was washed with water and methanol to obtain the product (POG-OH) represented by formula 3 with a yield of 95%. Simultaneously, carry out infrared characterization and NMR characterization to POG-OH (see Figure 4 ), can see 3500cm by infrared test -1 The characteristic peak signal of -OH; at the same time, the C-OH signal peak appears at 150ppm. Then UV test was carried out on POG-OH, the result is shown in the attached picture image 3 shown.

[0080]

Embodiment 3

[0082] A kind of preparation that contains the porous polymer derived from azacyclic pyrocatechol, the steps are as follows:

[0083] In 1,3,5-tris(3,4-dimethoxybenzyl)benzene (0.4mmol), 9H-carbazole-2,7-dialdehyde (0.6mmol), acetic anhydride (20mmol) and trichloride 100 mL of dichloromethane solvent was added to the iron (0.08 mmol) mixed system, and the reaction was performed under magnetic stirring at 25° C. for 48 h. Ferric chloride (72 mmol) was added to the system again, and the reaction was performed under magnetic stirring at 25°C for 12 h under an argon atmosphere. Then add methanol to the system to quench, filter under reduced pressure, and wash the solid residue with water and methanol to obtain the product (as shown in formula 4). Through the BET test of the product, the BET surface area of ​​the product shown in formula 4 can be calculated as high as 893m 2 g -1 .

[0084]

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Abstract

The invention relates to a series of porous polymers with brand-new structures, a series of pyrocatechol-derived porous polymers with brand-new structures are prepared from the porous polymers, and then a pyrocatechol-derived porous polymer-loaded high-spin monatomic iron catalyst is finally prepared on the basis of the pyrocatechol-derived porous polymers. According to the preparation method of the catechol-derived porous polymer-loaded high-spin monatomic iron catalyst, a catechol-derived porous polymer is used as a catalyst skeleton and reacts with an iron source, and the high-spin monatomic iron catalyst is obtained. The invention also discloses an application of the high-spin monatomic iron catalyst in catalyzing styrene epoxidation under illumination to prepare styrene oxide. When the catalyst is used for catalyzing styrene epoxidation reaction, the reaction conversion rate can reach 100%, the selectivity is 94%, and the catalyst has the advantages of high reaction activity, goodselectivity and the like. The catalyst not only has high catalytic activity, high selectivity and high stability, but also is simple in preparation method and can be repeatedly used.

Description

technical field [0001] The invention relates to a preparation method of a catechol-derived porous polymer, and the preparation and catalytic application of the porous polymer as a skeleton loaded high-spin monoatomic iron catalyst. Background technique [0002] Styrene oxide is an important fine chemical, which is widely used in organic synthesis, pharmaceutical and perfume industries, etc. Therefore, it has broad application prospects. [0003] The synthetic method of relevant styrene oxide mainly contains following several at present: 1, halohydrin method (Liao Weilin, Chen Feibiao, a kind of method for preparing epoxide by halohydrin method, Chinese patent, CN106518811A): this method technique is simple, but in Chlorine gas will be used in the production process, and many by-products will be produced at the same time, the material consumption is high, and it does not meet the road of green and sustainable development; 2, the peroxide oxidation method (Tan Rong, Deng Jian...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/02B01J31/06C07D303/04C07D301/06
CPCC08G61/02B01J31/069C07D303/04C07D301/06C08G2261/314C08G2261/142B01J35/39Y02P20/584
Inventor 刘宇宙谷得发
Owner DEEPCHEM TECH (BEIJING) CO LTD
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