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A kind of tricarboxylic amphoteric surfactant and preparation method thereof

A technology of surfactants and tricarboxylic groups, which is applied in the field of tricarboxylic amphoteric surfactants and its preparation, can solve the problems of high prices of surfactants, and achieve the effect of low cost and simple steps

Active Publication Date: 2021-11-12
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the price of this type of surfactant is more expensive, and its practical application range is smaller than that of other types of surfactants.

Method used

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  • A kind of tricarboxylic amphoteric surfactant and preparation method thereof
  • A kind of tricarboxylic amphoteric surfactant and preparation method thereof
  • A kind of tricarboxylic amphoteric surfactant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Add dodecylamine (18.5g, 0.1mol) and cyclobut-3-ene dicarboxylic anhydride (24.8g, 0.2mol) dropwise successively in a 250mL three-necked flask equipped with a reflux condenser, nitrogen gas 3 times, Then heated to 180° C. for 3 h, and TLC (Thin Layer Chromatography, thin layer chromatography) monitored the completion of the reaction. After the reaction was completed, it was cooled to room temperature, 50 mL of distilled water was added, extracted three times with 80 mL of ethyl acetate, dried over anhydrous magnesium sulfate, filtered, concentrated under reduced pressure to obtain a crude product, and finally separated by a column to obtain a colorless oily imide.

[0033] (2) Add 80 mL of tetrahydrofuran dried with sodium metal into a 250 mL three-neck flask, cool to 0°C in an ice-salt bath, and slowly add 3.8 g of LiAlH 4 After stirring for 3 minutes, the imide dissolved in tetrahydrofuran was slowly added dropwise into the three-necked flask, and after the additi...

Embodiment 2

[0037] (1) Add dodecylamine (18.5g, 0.1mol) and cyclobut-3-ene dicarboxylic anhydride (24.8g, 0.2mol) dropwise successively in a 250mL three-necked flask equipped with a reflux condenser, nitrogen gas 3 times, Then heated to 150° C. for 2 h, and TLC (Thin Layer Chromatography, thin layer chromatography) monitored the completion of the reaction. After the reaction was completed, it was cooled to room temperature, 50 mL of distilled water was added, extracted three times with 80 mL of ethyl acetate, dried over anhydrous magnesium sulfate, filtered, concentrated under reduced pressure to obtain a crude product, and finally separated by a column to obtain a colorless oily imide.

[0038] (2) Add 90 mL of tetrahydrofuran dried with sodium metal into a 250 mL three-neck flask, cool to 0°C in an ice-salt bath, and slowly add 4.18 g of LiAlH in batches 4 After stirring for 3 minutes, the imide dissolved in tetrahydrofuran was slowly added dropwise into the three-necked flask, and afte...

Embodiment 3

[0042] (1) Add dodecylamine (18.5g, 0.1mol) and cyclobut-3-ene dicarboxylic anhydride (24.8g, 0.2mol) dropwise successively in a 250mL three-necked flask equipped with a reflux condenser, nitrogen gas 3 times, Then heated to 200° C. for 5 h, and TLC (Thin Layer Chromatography, thin layer chromatography) monitored the completion of the reaction. After the reaction was completed, it was cooled to room temperature, 50 mL of distilled water was added, extracted three times with 80 mL of ethyl acetate, dried over anhydrous magnesium sulfate, filtered, concentrated under reduced pressure to obtain a crude product, and finally separated by a column to obtain a colorless oily imide.

[0043] (2) Add 100 mL of tetrahydrofuran dried with sodium metal into a 250 mL three-neck flask, cool to 0°C in an ice-salt bath, and slowly add 3.99 g of LiAlH 4 After stirring for 3 minutes, the imide dissolved in tetrahydrofuran was slowly added dropwise into the three-necked flask, and after the addi...

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Abstract

The invention discloses a tricarboxylic amphoteric surfactant and a preparation method thereof. The method comprises: 1) adding dodecylamine and cyclobut-3-enedicarboxylic anhydride into a three-necked flask, passing nitrogen gas, and performing nucleophilic addition-elimination reaction to generate imide; followed by LiAlH 4 Reducing the carbonyl group as a reducing agent; adding sodium chloroacetate for quaternization reaction. 2) Dilute the above reaction solution, slowly add potassium permanganate at 0°C, heat up to carry out oxidation reaction to generate carboxyl groups; add sodium sulfite after the reaction to remove excess potassium permanganate, filter with diatomaceous earth and extract with ethyl acetate Impurities, collect the water phase, adjust the pH to 2-4 to precipitate the product, filter and dry to constant weight to obtain the final product. The surfactant can be used in daily chemical industry, metal corrosion inhibition, petroleum exploration, textile, printing and dyeing and other fields.

Description

technical field [0001] The invention belongs to the field of surfactants, in particular to a tricarboxylic amphoteric surfactant and a preparation method. Background technique [0002] Surfactants refer to amphiphilic compounds containing non-polar lipophilic groups and polar hydrophilic groups in the molecular structure, which can form directional arrangements at the gas-liquid and solid-liquid interfaces, and adding a small amount to the solution can significantly reduce the concentration of the solution. Surface tension can effectively change the physical and chemical properties of the interface. Therefore, it is widely used in daily life, industry and agriculture, high-tech and other fields, and has become one of the important industries of chemical technology in various countries. Amphoteric surfactants are surfactants that contain both anionic and cationic hydrophilic groups in the same molecule. The biggest feature is that it can both give protons and accept protons...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01F17/18B01F17/32B01F17/28C07D207/16C09K23/18C09K23/28C09K23/32
CPCC07D207/16C09K23/00
Inventor 王晨邱冠钧王海花杨晓武李刚辉张康
Owner SHAANXI UNIV OF SCI & TECH
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