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Synthetic method of biquaternary ammonium salt

A synthesis method and a technology for diquaternary ammonium salts are applied in the field of preparation of diquaternary ammonium salts, which can solve the problems of slow reaction speed, increase the difficulty of recycling, and use a large amount of solvent, so as to accelerate the reaction speed, reduce the preparation time, prevent the The effect of agglomeration trends

Active Publication Date: 2012-05-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the reaction temperature and reaction concentration are high, the reaction is more violent, and the product is easy to form a solid large block, which is not conducive to removing the product from the reactor, nor is it conducive to the subsequent steps of washing, filtering and recrystallization
Therefore, the synthesis of the above-mentioned diquaternary ammonium salts is generally carried out at low temperature and lower reaction concentration at present. At this time, although smaller granular products can be generated, which is beneficial to subsequent washing, filtration, and recrystallization steps, due to the reaction The speed is relatively slow, the reaction time can reach 3-10 days, the yield of the product is low, and a large amount of solvent is needed, which increases the difficulty of recycling

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Mix 40mL, 30mL, and 70.5mL of N-methylpyrrolidine, 1,5-dibromopentane, and acetone in a three-necked flask with a reflux device, then place the three-necked flask in a 50kHz ultrasonic dispersion water bath, and start the ultrasonic wave Disperser, the mixture was vigorously stirred at 35°C for 8 hours until a suspension containing a large number of small particles was formed. The suspension was frozen at -10°C, a large amount of powder solids were precipitated, and then the solids were separated by filtration. Put the solid matter into ether at 25°C, stir continuously and add ether according to the degree of dissolution until the solid matter is completely dissolved in ether. Afterwards, the above solution was frozen at -10°C, a large amount of powdery solids were precipitated, and then the solids were separated by filtration. The above steps of washing, recrystallization and separation were repeated 3 times to finally obtain a beige solid powder, which was confirmed ...

Embodiment 2

[0019] Mix 60mL, 27.7mL, and 55mL of N-methylpyrrolidine, 1,5-dibromopentane, and acetone in a three-necked flask with reflux, and then place the three-necked flask in a 70kHz ultrasonic dispersion water bath to start ultrasonic dispersion The mixture was stirred vigorously at 40°C for 3 hours until a suspension containing a large number of small particles was formed. The suspension was frozen at -10°C, a large amount of powder solids were precipitated, and then the solids were separated by filtration. Put the solid matter into ether at 25°C, stir continuously and add ether according to the solubility until the solid matter is completely dissolved in ether. Afterwards, the above solution was frozen at -10°C, and a large amount of powder solids were precipitated, and then the solids were separated by filtration. The above steps of washing, recrystallization and separation were repeated 3 times to finally obtain a beige solid powder, which was confirmed to be the diquaternary a...

Embodiment 3

[0021] Mix 40mL, 24mL, and 35.5mL of N-methylpyrrolidine, 1,5-dibromopentane, and ethanol in a three-necked flask with reflux, then place the three-necked flask in a 100kHz ultrasonic dispersion water bath, and start ultrasonic dispersion The mixture was stirred vigorously at 50°C for 2 hours until a suspension containing a large number of small particles was formed. The suspension was frozen at -5°C, a large amount of powder solids were precipitated, and then the solids were separated by filtration. Put the solid matter into acetone at 25°C, stir continuously and supplement acetone according to the solubility until the solid matter is completely dissolved in acetone. Afterwards, the above solution was frozen at -5°C, and a large amount of powder solids were precipitated, and then the solids were separated by filtration. The above steps of washing, recrystallization and separation were repeated 3 times to finally obtain a beige solid powder, which was confirmed to be the diqu...

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Abstract

The invention discloses a synthetic method of biquaternary ammonium salt. In the method, ultrasonic waves are introduced into a reaction system in a dispersing manner, and a biquaternary ammonium pentane-1,5 (methylpyrrolidinium) dibromide can be synthesized under the high temperature and high concentration. In the method, the quantity of the used solvent is fewer, the particles of the biquaternary ammonium salt which is generated by the reaction are smaller, so that the following washing, filtering, recrystallization and other operations are very facilitated.

Description

technical field [0001] The invention belongs to the field of fine organic synthesis, and specifically relates to a preparation method of a double quaternary ammonium salt, Background technique [0002] Microporous molecular sieve materials are widely used in adsorption, separation, chemical industry, catalysis and other fields due to their regular channels and large specific surface area. Most of the preparation of microporous molecular sieves needs to be synthesized by using structure-directing agents as templates for channel formation, and the utilization of novel templates is the key to the preparation of molecular sieves with new structures. [0003] In recent years, diquaternary ammonium salt templates have shown their unique guiding properties in the design of new pore structures, especially in the synthesis of new molecular sieves with staggered channels. Journal of Catalysis 215 (2003) 151-170, US 5989410, US 5968475, US 6136290 and CN1234012A, CN11406120C all repor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/037
Inventor 杨卫亚凌凤香王少军沈智奇王丽华季洪海郭长友孙万付
Owner CHINA PETROLEUM & CHEM CORP
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