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
View PDF4 Cites 0 Cited by
  • 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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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

Example Embodiment

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

Example Embodiment

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

[0028] And 10ml of water, control the pH of the solution to 8, to obtain a colorless homogeneous solution. Then 14.42g TEOS was slowly added to obtain a milky white turbid liquid. After stirring and reacting at room temperature for 8 hours, the solution was placed in the reactor at 100 0 C reacts for 3 days. Suction filtration, washing with ethanol and water twice to obtain a white solid, the white solid 650 0 C, fired in the muffle furnace for 6h, 900 0 C burned for 11h to obtain a macroporous molecular sieve (MMCM), 8.6 g, and the yield was 58%. Infrared spectrum data (IR, cm -1 ): 1089, 800, 432.

Example Embodiment

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

[0030] Preparation of 2-picolylamine

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C01B37/00B01J29/03C07D213/38C07D213/36
Inventor 陈秋云
Owner JIANGSU UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products