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Prolinol rapid desulfurizer and preparation method thereof

A technology of desulfurization agent and prolinol, which is applied in the field of prolinol fast desulfurization agent and its preparation, can solve the problem that it is difficult to meet the needs of various catalytic reaction sites at the same time, the easy recombination of photogenerated electrons and holes, and the utilization rate of visible light Low-level problems, to achieve the effect of easy operation, easy access to raw materials, and simple preparation methods

Active Publication Date: 2020-11-17
XIAN TECHNOLOGICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention provides a prolinol fast desulfurizer and its preparation method to overcome the low utilization rate of visible light existing in the prior art and it is difficult to simultaneously satisfy the The site requirements of various catalytic reactions, and the problems of easy recombination of photogenerated electron-hole pairs and low quantum efficiency

Method used

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  • Prolinol rapid desulfurizer and preparation method thereof
  • Prolinol rapid desulfurizer and preparation method thereof
  • Prolinol rapid desulfurizer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: a kind of prolinol fast desulfurizer, prepared by the following steps:

[0026] Weigh 0.54g of 1-(4-methylphenyl)pyrrole-2-carbaldehyde (2.5mmol), and weigh (2.5mmol) 0.37g of 2-3-dihydroxyamine-2-3-dimethyl with the same molar ratio Butane and 20ml chromatographic methanol were put into a one-necked flask and heated to reflux for 24 hours. The methanol solvent was removed by rotary evaporation, and the remaining substance was dissolved in 20 ml of dichloromethane, placed in an ice-water bath, and stirred. Add sodium nitrite (103 mg, 1.5 mmol) and stir at reflux for 1 h. The dichloromethane was removed under reduced pressure to obtain a deep red solution, which was dried under reduced pressure. The crude product was analyzed and purified by gradient elution column chromatography on a silica gel column to obtain 0.56 g of a light yellow viscous product radical with a yield of 68%. R f =0.58(CH 2 Cl 2 / CH 3 OH,15:1).EI-MS(m / z)330.2181[M] + .IR(KBr)340...

Embodiment 2

[0027] Embodiment 2: a kind of prolinol fast desulfurizer, prepared by the following steps:

[0028] Weigh 0.62g of 1-(4-nitrophenyl)pyrrole-2-carbaldehyde (2.5mmol), and weigh (2.5mmol) 0.37g of 2-3-dihydroxyamine-2-3-dimethyl with the same molar ratio Butane and 20ml chromatographic methanol were put into a one-necked flask and heated to reflux for 24 hours. The methanol solvent was removed by rotary evaporation, and the remaining substance was dissolved in 20 ml of dichloromethane, placed in an ice-water bath, and stirred. Add sodium nitrite (103 mg, 1.5 mmol) and stir at reflux for 1 h. The dichloromethane was removed under reduced pressure to obtain a deep red solution, which was dried under reduced pressure. The crude product was analyzed and purified by gradient elution column chromatography on a silica gel column to obtain 0.54 g of a light yellow viscous product radical with a yield of 60%. R f =0.49(CH 2 Cl 2 / CH 3 OH,15:1).EI-MS(m / z)360.1562[M] + .IR(KBr)3359...

Embodiment 3

[0029] Embodiment 3: a kind of prolinol fast desulfurizer, prepared by the following steps:

[0030] Weigh 0.55g of 1-(3-fluorophenyl)pyrrole-2-carbaldehyde (2.5mmol), and weigh (2.5mmol) 0.37g of 2-3-dihydroxyamine-2-3-dimethyl with the same molar ratio Butane and 20ml chromatographic methanol were put into a one-necked flask and heated to reflux for 24 hours. The methanol solvent was removed by rotary evaporation, and the remaining substance was dissolved in 20 ml of dichloromethane, placed in an ice-water bath, and stirred. Add sodium nitrite (103 mg, 1.5 mmol) and stir under reflux for 1 h. The dichloromethane was removed under reduced pressure to obtain a dark red solution, which was dried under reduced pressure. The crude product was analyzed and purified by gradient elution column chromatography on a silica gel column to obtain 0.45 g of a light yellow viscous product free radical with a yield of 54%. R f =0.61 (CH 2 Cl 2 / CH 3 OH,15:1), EI-MS (m / z) 334.1924[M] +...

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Abstract

The invention relates to the technical field of environmental protection, in particular to a prolinol rapid desulfurizer and a preparation method thereof. The problems that in the prior art, the visible light utilization rate is very low, point location requirements of various catalytic reactions are difficult to meet at the same time, meanwhile, photo-generated electron hole pairs are easy to compound, and the quantum efficiency is low are solved. The invention provides the prolinol rapid desulfurizer, the general formula of the desulfurizer is shown in the specification, wherein R1 to R5 areH, OCH3, NO2, X (F, Cl, Br), COOH and CF3. The desulfurizer is formed by condensation of R1 to R5 substituted phenylacetaldehyde and 2,3-dimethyl-2,3-dihydroxylamino butane, and R1 to R5 are respectively and independently selected from H, OCH3, NO2, halogen, COOH and CF3. The preparation method is simple, raw materials are easy to obtain, operation is easy, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of environmental protection, in particular to a prolinol fast desulfurizer and a preparation method thereof. Background technique [0002] Petroleum remains by far the main fossil fuel-based energy source consumed by countries around the world. There are many kinds of sulfur in petroleum, including mercaptans, thioethers, disulfides and sulfides, etc. Sulfuric acid (SOX) produced by fuel combustion is the main source of air pollution and acid rain, which has a serious impact on the environment. . With the rise of the automobile industry, automobiles have an increasing demand for fuel oil, and at the same time, more serious automobile exhaust emission problems are brought. As the world's largest automobile manufacturing and automobile demand country, China has implemented the "National V" standard since 2017, requiring the upper limit of the sulfur content of gasoline to be 10mg / kg, and the stricter "Nation...

Claims

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Application Information

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IPC IPC(8): C07D403/04B01J31/02C10G27/04
CPCC07D403/04B01J31/0271B01J31/0247C10G27/04C10G2300/202
Inventor 田敏郭玉书张改高敏
Owner XIAN TECHNOLOGICAL UNIV
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