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Microwave synthetic method of dodecyl methyl biethoxyl ammonium bromide

A technology of dodecyl bromide and methyldiethanolamine, applied in the field of chemistry, can solve the problems of slow reaction speed, reduced yield, longer reaction time, etc., and achieves the advantages of improving yield, being beneficial to absorption, and suppressing side reactions. Effect

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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

If the temperature is too high, a large number of by-products will be produced, which will reduce the yield; if the temperature is too low, the reaction rate will be slow, the required reaction time will be longer, and the yield will be reduced or even no reaction will occur.

Method used

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  • Microwave synthetic method of dodecyl methyl biethoxyl ammonium bromide
  • Microwave synthetic method of dodecyl methyl biethoxyl ammonium bromide
  • Microwave synthetic method of dodecyl methyl biethoxyl ammonium bromide

Examples

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Effect test

example 1

[0042] 1. Preparation: Dissolve 1.19g of N-methyldiethanolamine and 2.49g of dodecyl bromide in 7ml of n-butanol, boil and reflux in a microwave with a power of 636W for 23 minutes, and finally add the reaction product to the reaction solution The product was crystallized with 6 times the volume of anhydrous ether to obtain a white solid, the product. Using bromophenol blue-ethanol as an indicator, the conversion rate of the target product was measured to be 92% by hydrochloric acid-ethanol titration.

[0043] 2. The resulting white solid is identified by the following method:

[0044] (1) Identification of quaternary ammonium salt (potassium ferricyanide test)

[0045] Dissolve 0.1 g of the resulting white solid in 50 mL of water, and add potassium ferricyanide solution (3 g / L) to 10 mL of the solution to generate a yellow precipitate. Show the existence of quaternary ammonium salt, reaction formula is:

[0046]

[0047] (2) Infrared spectral analysis

[0048] Take a s...

example 2～21

[0064] N-methyldiethanolamine and dodecyl bromide are mixed and dissolved in n-butanol, boiled and refluxed in the microwave for reaction, and finally anhydrous ether which is 6 times the volume of the reaction product is added to the reaction solution to crystallize the product to obtain white solid. Each parameter and reaction result in the reaction are as shown in table 3, wherein a, b, A, B, C, D and R represent respectively the amount of N-methyldiethanolamine, the amount of lauryl bromide, the amount of n-butanol amount, microwave power, yield and conversion of the desired product (i.e. the resulting white solid).

[0065] table 3

[0066]

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Abstract

The invention provides a method for synthesizing dodecyl methyl dihydroxyethyl ammonium bromide by microwave. The method comprises the following steps: dissolving N-methyl diethano lamine and dodecyl bromide in normal butanol with the volume times of between 1.5 and 3; refluxing the mixed solution for 17 to 23 minutes in microwave with the power of between 500 and 700W; and adding absolute ether in the reaction solution after the reaction is completed to cause the product to be crystallized, thereby obtaining white solid. In the process of refluxing reaction, continuous action of the microwave and boiling of the reaction solution are maintained all along. By the prior method, the rate of conversion of the target product of the method is equivalent to that of the prior method, or even improved, but the reaction time required by the method is only about 5 percent of that of the prior method.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a microwave synthesis method for quaternary ammonium salts. Background technique [0002] N-Methyldiethanolamine (MDEA) is an excellent solvent, pharmaceutical intermediate and high-efficiency desulfurization and decarburization agent, which can remove H from natural gas, Claus sulfur tail gas and other gases 2 S, can remove CO in synthetic ammonia with the participation of activators 2 . In addition, MDEA can also be used as insecticide, emulsifier, semi-finished product of fabric auxiliaries, intermediate of antineoplastic drug nitrogen mustard hydrochloride, catalyst of urethane coating, fiber auxiliaries, etc. However, the production of N-methyldiethanolamine (MDEA) in our country is too abundant, and further research and development are needed to expand new application channels. Zheng Qing from Zhejiang University proposed a new surfactant, dodecylmethyldihydroxyethyl, synthesize...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/40C07C213/00
Inventor 郑成毛桃嫣张新强
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