Synthesis method of 3, 5-dimethyl piperidine onium salt template agent and molecular sieve

A technology of dimethylpiperidinium and synthesis method, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., to achieve the effects of solving difficulties in anion treatment, low price and economical preparation process

Active Publication Date: 2021-12-28
南京华洲新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of synthetic method of novel molecular sieve template agent, adopt step-by-step method to synthesize template agent, overcome the aftertreatment difficulty that other quaternization reagents cause and the impact of cis-trans isomer ratio on synthetic molecular sieve, The quaternization reagent used is relatively cheap and easy to realize industrial production

Method used

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  • Synthesis method of 3, 5-dimethyl piperidine onium salt template agent and molecular sieve
  • Synthesis method of 3, 5-dimethyl piperidine onium salt template agent and molecular sieve
  • Synthesis method of 3, 5-dimethyl piperidine onium salt template agent and molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043]Add 107g of 3,5-lutidine, 90g of ethanol, and 10g of water into a four-necked flask, start stirring, raise the temperature to 70-80°C, and slowly inject methyl chloride gas into the solution until the total amount of methyl chloride is equal to 3,5 -The molar ratio of lutidine is 1.1:1, the generated pyridinium quaternary ammonium salt is precipitated in the ethanol solution, the crystals are filtered out, washed with ethanol repeatedly three times, and the crystals are dried in a vacuum oven at 60°C to obtain 132.6g1,3 , 5-trimethylpyridinium quaternary ammonium salt; the filtrate and washing liquid were combined for the next application.

Embodiment 2

[0045] Prepare 1,3,5-collidine quaternary ammonium salt according to Example 1, put 300g 1,3,5-collidine quaternary ammonium salt into the autoclave, add 200g methanol and 2% ruthenium carbon catalyst (2 The amount of ruthenium carbon catalyst is 2% of the mass of 1,3,5-trimethylpyridinium quaternary ammonium salt), cover the autoclave lid and tighten it, fill the air in the kettle body with nitrogen for 15min, and then replace it twice with hydrogen , close the outlet valve and inlet valve, pressurize with hydrogen to 4MPa, start to heat up, when the temperature rises to 170°C, continue to fill in hydrogen to a pressure of 5.5MPa, heat preservation and pressure until the pressure change in the kettle is less than 0.1MPa within 0.5h , keep warm for 2 hours, cool down to room temperature and take out the sample, filter out the catalyst, and remove the methanol by rotary evaporation of the filtrate to obtain 290.4g 1,3,5-trimethylpiperidine (trans isomer 21.6%, cis isomer 77.6%,...

Embodiment 3

[0049] Seed crystal: ammonia-type ultra-stable molecular sieve, specifically ammonium-type Y molecular sieve, the appearance is white to off-white Si / Al=10-14, unit cell parameters: 24.42-24.49; SiO 2 Content: 73.0~80.0%, Al 2 o 3 Content: 9.2~11.3%, Na 2 O content: <0.15%.

[0050] Silicon source: 30% silica sol.

[0051] Template agent: the template agent prepared in Example 2.

[0052] First mix 16g of seed crystals with 150g of deionized water, stir with a stirrer for 1h, then add 50g of the template agent prepared in Example 1 and 175g of silicon source successively, raise the temperature to 50°C, and stir for 3h; then pour the materials into the autoclave During the process, cover and tighten the autoclave lid, raise the temperature to 160°C, conduct a hydrothermal reaction for 48 hours, take out the material, let it stand, filter, wash the filter cake with deionized water until it is neutral, remove the water and dry the material, and then place it in a In a Furnac...

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Abstract

The invention discloses a synthesis method of a 3, 5-dimethyl piperidine onium salt template agent. The method comprises the following steps: synthesizing 1, 3, 5-trimethyl pyridine quaternary ammonium salt from chloromethane and 3, 5-dimethyl pyridine; under the action of a catalyst, carrying out hydrogenation reaction on the 1, 3, 5-trimethylpyridine quaternary ammonium salt to generate 1, 3, 5-trimethylpiperidine; reacting 1, 3, 5-trimethylpiperidine with dimethyl carbonate in a nitrogen atmosphere to generate a 3, 5-dimethyl piperidine onium salt with methyl carbonate radicals; and dissolving the 3, 5-dimethyl piperidine onium salt with methyl carbonate radicals in water, standing for layering, removing an organic phase in the raw material, taking a water phase, distilling, adding calcium hydroxide, reacting to obtain a 3, 5-dimethyl piperidine onium salt with hydroxide radicals asanions, and concentrating until the mass fraction of the 3, 5-dimethyl piperidine onium salt is 24-32% and the mass fraction of the hydroxide radicals is 3-4%. The invention also discloses a method for preparing a molecular sieve by adopting the 3, 5-dimethyl piperidine onium salt template agent.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and relates to a synthesis method of a novel molecular sieve template agent, in particular to a synthesis method of a 3,5-dimethylpiperidinium salt template agent, the template agent has a certain proportion of cis-trans iso The structure can effectively prepare molecular sieves with high crystallinity, high purity and good catalytic performance. Background technique [0002] Molecular sieves are widely used in the fields of industry, agriculture, and medicine. Molecular sieves are in the most important position in the technical field of MTO (methanol to olefins technology). At present, environmental problems are becoming more and more serious, and people's awareness of environmental protection is increasing day by day. [0003] At present, air pollution mainly comes from industrial flue gas emissions and vehicle exhaust emissions. In order to reduce pollutant emissions, countries are activ...

Claims

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Application Information

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IPC IPC(8): C01B39/04C01B39/48
CPCC01B39/04C01B39/48C01P2002/72C01P2004/03C01P2006/80C01P2004/62C01P2004/61
Inventor 邢华忠陶远贤邢语恬张华张迎春
Owner 南京华洲新材料有限公司
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