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Method of continuously synthesizing quaternary ammonium salt by using microreaction device

A technology of micro-reaction device and reaction device, which is applied in the direction of cyanide reaction preparation, chemical instruments and methods, botany equipment and methods, etc., can solve the problems of unavoidable side reactions, inaccurate control of reaction temperature, cumbersome reaction steps, etc. To shorten the reaction time, simplify the process and improve the reaction efficiency

Inactive Publication Date: 2017-12-08
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved in the present invention is to provide a method for continuously synthesizing quaternary ammonium salts using a micro-reaction device, so as to solve the problems in the prior art that the reaction steps are cumbersome, the reaction temperature cannot be accurately controlled, and side reactions are inevitable.

Method used

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  • Method of continuously synthesizing quaternary ammonium salt by using microreaction device
  • Method of continuously synthesizing quaternary ammonium salt by using microreaction device
  • Method of continuously synthesizing quaternary ammonium salt by using microreaction device

Examples

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Embodiment 1

[0034] Take 50g / 100mL of methyl iodide in toluene, 20wt% sodium hydroxide aqueous solution and 40g / 100mL of phenylalanine methyl in toluene, suck them into syringes A, B, and C respectively, and fix them on the syringe pump. Mix the toluene solution of phenylalanine methyl ester and sodium hydroxide aqueous solution through a Y-type mixer with a syringe pump, preheat the resulting mixture to 80°C, and then mix it with the toluene solution of methyl iodide through a bayer mixer , pumped into the microreactor for reaction. The specification of the polytetrafluoroethylene coil as the microreactor is 1mm / 20mL. The molar ratio of phenylalanine methyl ester, sodium hydroxide, and methyl iodide is 1:2:3.3, and the flow rate ratio is 1:0.73:2.1. The specific flow rate is 0.5mL / min for phenylalanine methyl ester, and 0.365 mL / min for sodium hydroxide mL / min, methyl iodide 1.05mL / min. The microreactor was placed in an oil bath to control the temperature, the reaction temperature was k...

Embodiment 2

[0036]Take 50g / 100mL methyl iodide in toluene, 20wt% sodium hydroxide aqueous solution and 40g / 100mL ethyl phenylalanine in toluene, suck them into syringes A, B and C respectively, and fix them on the syringe pump. Mix the toluene solution of ethyl phenylalanine and sodium hydroxide solution through a Y-type mixer with a syringe pump, preheat the resulting mixture to 80°C, and then mix it with the toluene solution of methyl iodide through a bayer mixer , pumped into the microreactor for reaction. The specification of the polytetrafluoroethylene coil as the microreactor is 1mm / 20mL. The molar ratio of ethyl phenylalanine, sodium hydroxide, and methyl iodide is 1:2:3.3, and the flow rate ratio is 1:0.68:1.98. The specific flow rate is ethyl phenylalanine 0.5mL / min, sodium hydroxide 0.34 mL / min, methyl iodide 0.99mL / min. The microreactor was placed in an oil bath to control the temperature, the reaction temperature was kept at 90°C, and the reaction retention time was 11 minut...

Embodiment 3

[0038] Take 50g / 100mL methyl iodide in toluene solution, 20wt% sodium hydroxide aqueous solution and 40g / 100mL phenylalanine propyl ester in toluene solution, draw them into syringes A, B and C respectively, and fix them on the syringe pump. First mix the toluene solution of propyl phenylalanine and sodium hydroxide solution through a Y-type mixer through a syringe pump, and the resulting mixture is preheated to 80°C, and then mixed with the toluene solution of methyl iodide through a bayer mixer , pumped into the microreactor for reaction. The specification of the polytetrafluoroethylene coil as the microreactor is 1mm / 20mL. The molar ratio of propyl phenylalanine, sodium hydroxide, and methyl iodide is 1:2:3.3, and the flow rate ratio is 1:0.63:1.82. The specific flow rate is 0.5 mL / min for propyl phenylalanine, and 0.315 mL / min for sodium hydroxide. mL / min, methyl iodide 0.91mL / min. The microreactor was placed in an oil bath to control the temperature, the reaction temper...

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Abstract

The invention discloses a method of continuously synthesizing quaternary ammonium salt by using a microreaction device. An amino acid derivative and halohydrocarbon as reactants, and sodium hydroxide as an acid-binding agent for a reaction are pumped into a microreactor for the reaction in a thrice feeding manner. An obtained product is a quaternary ammonium salt compound derived from amino acid. Compared with the prior art, the method is high in automation degree; a material ratio and a reaction temperature of the reactants are controlled accurately; the reaction time is short; the equipment and energy loss is low; the method is easy and simple to operate; and the required manpower and material resources are greatly reduced. At the same time, when the method is used for the reaction, a catalyst, various complicated instruments and a dangerous reagent are not required to be used; reaction conditions can be met only by heating; in addition, the problem of local heat release in a reaction process is solved; the uniform and stable temperature is achieved; and the high-quality product can be obtained efficiently.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for continuously synthesizing quaternary ammonium salts using a micro-reaction device. Background technique [0002] Organic quaternary ammonium salt is a compound with a wide range of uses, and its status in industry, agriculture, and medicine cannot be underestimated. Take the phase transfer catalyst as an example. In the phase transfer catalytic reaction, the quaternary ammonium salt can form an ion pair with the nucleophile in the water phase and enter the organic phase, thereby speeding up the reaction rate, reducing side reactions and increasing the yield. In industry, organic quaternary ammonium salts, as cationic surfactants, are valued by various industrial sectors due to its excellent adsorption, emulsification and thickening properties, such as sodium cetylbenzenesulfonate. Acryloyloxyalkyl quaternary ammonium cationic monomers and acrylamide alk...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/18C07C229/36A01N37/44A01P3/00A01P1/00
CPCA01N37/44C07C227/18C07C229/36
Inventor 郭凯杨宇航方正孙芹朱宁李昕万力欧阳平凯
Owner NANJING UNIV OF TECH
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