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Macroporous molecular sieve, preparation method and application in pyridylmethyl amine preparation

A technology of macroporous molecular sieve and picolylamine, applied in molecular sieve compounds, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of large pollution, long reaction time, high cost, etc., and achieve high conversion rate of raw materials and short reaction time , The effect of low product cost

Inactive Publication Date: 2011-09-07
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method takes a long time to react, the price of the reducing agent is high and cannot be recycled, so a large amount of solid waste and waste water are generated, and a large amount of volatile toxic solvent of chloroform is used in the purification process, the cost is high and the pollution is large

Method used

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  • Macroporous molecular sieve, preparation method and application in pyridylmethyl amine preparation
  • Macroporous molecular sieve, preparation method and application in pyridylmethyl amine preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 (example of optimal reaction conditions): Dissolve 2.1840g CTAB in 50ml of water, stir for 10min to make it clear, add NaOH (0.3435g) and 10ml of water, control the pH of the solution to 9, and obtain a colorless homogeneous solution . Then slowly add 14.42gTEOS to obtain a milky white turbid liquid. After stirring and reacting at room temperature for 8h, the solution is placed in a reaction kettle and heated at 100 0 C reacted for 3 days. Suction filtration, washed twice with ethanol and water respectively to obtain a white solid, the white solid 550 0 C, burn in the muffle furnace for 6h, 750 0 Calcined in C for 11 hours to obtain macroporous molecular sieve (MMCM), 11.6 g, yield 78%. Infrared spectral data (IR, cm -1 ): 1089, 800, 432. BET: 21.54m 2 g ?1 ; pore size is 100 nm (see attached figure 1 )

Embodiment 2

[0027] Example 2: Dissolve 2.1840g of CTAB in 50ml of water, stir for 10min to make it clear, and then add NaOH (0.3435g).

[0028] and 10ml of water to control the pH of the solution to 8 to obtain a colorless homogeneous solution. Then slowly add 14.42gTEOS to obtain a milky white turbid liquid. After stirring and reacting at room temperature for 8h, the solution is placed in a reaction kettle and heated at 100 0 C reacted for 3 days. Suction filtration, washed twice with ethanol and water to obtain a white solid, the white solid 650 0 C, burn in the muffle furnace for 6h, 900 0 Calcined in C for 11 hours to obtain macroporous molecular sieve (MMCM), 8.6 g, yield 58%. Infrared spectral data (IR, cm -1 ): 1089, 800, 432.

Embodiment 3

[0029]Example 3: Dissolve 2.1840g of CTAB in 50ml of water, stir for 10min to make it clear, add NaOH (0.3435g) and 10ml of water, control the pH of the solution to 10, and obtain a colorless homogeneous solution. Then slowly add 14.42gTEOS to obtain a milky white turbid liquid. After stirring and reacting at room temperature for 8h, the solution is placed in a reaction kettle and heated at 100 0 C reacted for 3 days. Suction filtration, washed twice with ethanol and water respectively to obtain a white solid, the white solid 550 0 C, burn in the muffle furnace for 6h, 800 0 C burned for 11 hours to obtain macroporous molecular sieve (MMCM), 7.8 grams, yield 53%. Infrared spectral data (IR, cm -1 ): 1089, 800, 432.

[0030] Preparation of 2-picolylamine

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Abstract

The invention relates to a novel macroporous molecular sieve, a preparation method and application in pyridylmethyl amine preparation, and belongs to the technical field of solid-phase catalysts. The novel macroporous molecular sieve with low adsorbability is prepared by hydrothermal reaction and multi-step thermal condensation from tetramethylsilane which is used as a raw material and cetyl trimethyl ammonium bromide (CTAB) which is used as a template agent. The application of the macroporous molecular sieve provided by the invention is as follows: the molecular sieve is used as a solid-phase catalyst in the gas-solid method for synthesizing 2-pyridylmethyl amine and di(2-pyridylmethyl) amine from pyridylmethyl chloride and ammonia water, which are used as raw materials. The method is characterized in that: the novel silicon-based macroporous molecular sieve is used as the catalyst and solid-phase solvent, other organic reagents are not needed, the product is easy to be separated from the catalyst, the macroporous molecular sieve is recycled, the conversion of raw materials is increased, the product cost is reduced, and the reaction time is shortened. The method is a zero-emission and energy-saving one for preparing 2-pyridylmethyl amine and di(2-pyridylmethyl) amine.

Description

technical field [0001] The invention relates to a new macroporous molecular sieve, a preparation method and its application in the preparation of picolylamine compounds, and belongs to the technical field of solid-phase catalyst preparation. Background technique [0002] As an important chemical intermediate, picolylamine is widely used in the preparation of biomimetic catalysts (S. V. Kryatov, S. Taktak, I. V. Korendovych, E. V. Rybak-Akimova, J. Kaizer, S. Torelli, X. Shan, S. Mandal, V. L. MacMurdo, A. M. Payeras, L. Q. Jr., Inorg. Chem. 2005, 44, 85-99.). Tripyridylamine iron complexes can mimic the function of toluene monooxygenase, and are used in the oxidative degradation of aromatic rings and the preparation of epoxidized products of ethylenic compounds (1.M. M. Cheng, Z. Y. Sun, W. H. Ma, C. C. Chen , J. C. Zhao, Z. P. Wang, Science in China Series B: Chem. 2006, 49(5), 407. 2. R. Mas-Balleste, M. Fujita, C. Hemmila, L. Q. Jr. J. Mol. Cat. A : Chem. 2006, 251, 49....

Claims

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Application Information

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IPC IPC(8): C01B37/00B01J29/03C07D213/38C07D213/36
Inventor 陈秋云
Owner JIANGSU UNIV
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