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Preparation method of biquaternary ammonium salt compound

A salt compound and diquaternary ammonium technology, applied in the field of chemistry, can solve the problems of high cost of synthetic raw materials, complicated post-processing, etc., and achieve the effects of simple and economic post-processing and high-efficiency reaction

Inactive Publication Date: 2021-06-22
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] Aiming at the problems of relatively high cost of synthetic raw materials and complicated post-treatment in the current technology, the present invention proposes a method for preparing bis-quaternary ammonium salt compounds, that is, dibromoalkane and trimethylamine aqueous solution are used as reactants, and ethanol is used as a solvent in The homogeneous reaction is carried out under heating conditions, which has the characteristics of fast conversion, high yield, convenient post-treatment and low cost

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  • Preparation method of biquaternary ammonium salt compound
  • Preparation method of biquaternary ammonium salt compound
  • Preparation method of biquaternary ammonium salt compound

Examples

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Effect test

Embodiment 1

[0021] Embodiment 1: Reaction under different temperatures

[0022] Take 1,6-dibromohexane (24.4g, 100mmol) and place it in a reaction kettle, add 50mL of ethanol, and mix well. Then trimethylamine aqueous solution (30%wt, 39.3g, 200mmol) was added, and the reaction was stirred at different temperatures for several hours. After the reaction, the solvent was evaporated under reduced pressure to obtain a white solid crude product. Add a small amount of ethyl acetate to the crude product, wash and filter with suction to obtain the product. The yields at different temperatures are shown in Table 1.

[0023] Table 1

[0024]

[0025]

[0026] It can be seen from Table 1 that within the same time period of 6 hours, the reaction yield at 25° C. is low, and a yield of 91.4% can be obtained by extending the reaction time to 12 hours. Heating the reaction solution to above 60°C can significantly increase the reaction yield. Increasing the reaction temperature from 60°C to 80°...

Embodiment 2

[0027] Embodiment 2: different molar ratio reaction

[0028] Take 1,6-dibromohexane (24.4g, 100mmol) and place it in a reaction kettle, add ethanol, and mix well. Then trimethylamine aqueous solution (30%wt) in different molar ratios was added, and the mixture was stirred and reacted at 60°C for 6 hours. After the reaction, the solvent was evaporated under reduced pressure to obtain a white solid crude product. Add a small amount of ethyl acetate to the crude product, wash and filter with suction to obtain the product. The reaction results of different molar ratios are shown in Table 2.

[0029] Table 2

[0030] serial number n(1,6-dibromohexane): n(trimethylamine) Yield (%) 1 1:2 95.5 2 1:2.2 96.9 3 1:2.4 96.5

[0031] It can be seen from Table 2 that, under the same other reaction conditions, increasing the trimethylamine to 2.2 equivalents can slightly increase the reaction yield, but continuing to increase the amount of trimethylamin...

Embodiment 3

[0032] Embodiment 3: washing with different washing solvents

[0033] Take 1,6-dibromohexane (24.4g, 100mmol) and place it in a reaction kettle, add 50mL of ethanol, and mix well. Then trimethylamine aqueous solution (30%wt, 39.3g, 200mmol) was added, and the reaction was stirred at 60°C for 6 hours. After the reaction, the solvent was evaporated under reduced pressure to obtain a white solid crude product. Add a small amount of organic solvent to the crude product, wash and filter with suction to obtain the product. The yields after washing and suction filtration with different organic solvents are shown in Table 3.

[0034] table 3

[0035] serial number solvent Yield (%) 1 ethyl acetate 95.5 2 petroleum ether 96.3 3 Dichloromethane 96.0 4 ethanol 92.8

[0036] As can be seen from Table 3, different washing solvents lead to significant differences in yields, which are mainly related to the different solubility of bis-quaterna...

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Abstract

The invention belongs to the field of chemistry, and provides a preparation method of a biquaternary ammonium salt compound. The preparation method comprises the following steps: by taking dibromoalkane and a trimethylamine aqueous solution as raw materials and ethanol as a solvent, reacting in a homogeneous system at 25-80 DEG C for 4-48 hours, and after the reaction is finished, distilling and washing to obtain a pure product. The reaction is simple and efficient, the cost is low, and the use of trimethylamine gas and other high-safety-risk raw materials and trimethylamine methanol solution and other high-economic-cost raw materials can be avoided in the preparation process; the defects of heterogeneous reaction and low conversion rate caused by independently using a trimethylamine aqueous solution and dibromoalkane as reaction raw materials are overcome; high-risk organic solvents such as diethyl ether are not used in the post-treatment process, and all the used organic solvents can be recycled.

Description

technical field [0001] The invention belongs to the field of chemistry, and relates to a preparation method of a bisquaternary ammonium compound, in particular to a preparation method of a bisquaternary ammonium compound. Background technique [0002] Hexamethylammonium bromide and other bis-quaternary ammonium salt compounds are commonly used in the manufacture of molecular sieves as a structure-directing agent, and are important raw materials for preparing molecular sieves such as ITQ-13 and EU-1. A simple, economical and industrially produced method for preparing diquaternary ammonium salt compounds can promote the rapid development of the related molecular sieve manufacturing industry. The method for synthesizing diquaternary ammonium salts such as hexamethyl ammonium bromide generally has two kinds of methods, namely 1) aliphatic diamine and methylating reagent reaction, and 2) dibromoalkane and trimethylamine reaction. In the prior art of the above two reactions, ther...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/12C07C209/86C07C211/63
CPCC07C209/12C07C209/86C07C211/63
Inventor 梁长海刘亚军尹俊泽
Owner DALIAN UNIV OF TECH
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