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Preparation method of asymmetric Gemini fluorocarbon surfactant

A fluorocarbon surface and active agent technology, which is applied in the field of preparation of asymmetric Gemini fluorocarbon surfactants, can solve the problems of structural asymmetry, difficulty in preparation, and difficulty in separation, so as to avoid operational difficulties, easy biodegradation, The effect of low reaction temperature

Inactive Publication Date: 2020-08-11
SHAANXI YUTENG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the asymmetry of the existing structure, the synthesis is relatively complicated, and the separation and preparation are difficult.

Method used

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  • Preparation method of asymmetric Gemini fluorocarbon surfactant
  • Preparation method of asymmetric Gemini fluorocarbon surfactant
  • Preparation method of asymmetric Gemini fluorocarbon surfactant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Synthesis of asymmetric Gemini fluorocarbon surfactant FCDA-1:

[0058] Step 1: At room temperature, put succinoyl chloride (1eq, 0.05mol, 7.75g) and ethyl acetate 40g in a 150mL three-neck round bottom flask, stir for 5min at a stirrer speed of 200r / min, and heat to 40°C;

[0059] Step 2: Mix triethylamine (1.2eq, 0.06mol, 6.06g) and 1H, 1H-perfluorohexylamine (1eq, 0.05mol, 14.95g) in a 100mL beaker, transfer to a 100mL constant pressure funnel, drop by drop Add the mixed solution dropwise, the dropping time is 10min, and react for 1h after the dropping is completed;

[0060] Step 3: Use a 100mL beaker to mix triethylamine (1.2eq, 0.06mol, 6.06g) and n-hexylamine (1eq, 0.05mol, 5.05g) evenly, transfer to a 100mL constant pressure funnel, add the mixed solution drop by drop, drop The addition time is 10min, and the reaction is 1h after the dropwise addition is completed;

[0061] Step 4: Continue to add 15 g of ethanol dropwise to the round bottom flask, and cool to ...

Embodiment 2

[0067] Synthesis of asymmetric Gemini fluorocarbon surfactant FCDA-2:

[0068] Step 1: At room temperature, put succinoyl chloride (1eq, 0.05mol, 7.75g) and 40g of ethyl acetate in a 150mL three-neck round bottom flask, stir for 10min at a stirrer speed of 300r / min, and heat to 50°C;

[0069] Step 2: Use a 100mL beaker to mix triethylamine (1.2eq, 0.06mol, 6.06g) and 1H,1H-perfluorohexylamine (1eq, 0.05mol, 14.95g) evenly, transfer to a 100mL constant pressure funnel, drop by drop Add the mixed solution dropwise, the dropping time is 20min, and react for 2h after the dropping is completed;

[0070] Step 3: Use a 100mL beaker to mix triethylamine (1.2eq, 0.06mol, 6.06g) and n-octylamine (1eq, 0.05mol, 5.75g) evenly, transfer to a 100mL constant pressure funnel, add the mixed solution drop by drop, drop The addition time is 20min, and the reaction is 2h after the dropwise addition is completed;

[0071] Step 4: Continue to add 10 g of ethanol dropwise to the round bottom flask...

Embodiment 3

[0077] Synthesis of asymmetric Gemini fluorocarbon surfactant FCDA-3:

[0078]Step 1: At room temperature, put succinoyl chloride (1eq, 0.05mol, 7.75g) and 40g of ethyl acetate in a 150mL three-neck round bottom flask, stir for 7min at a stirrer speed of 250r / min, and heat to 45°C;

[0079] Step 2: Use a 100mL beaker to mix triethylamine (1.2eq, 0.06mol, 6.06g) and 1H,1H-perfluorohexylamine (1eq, 0.05mol, 14.95g) evenly, transfer to a 100mL constant pressure funnel, drop by drop Add the mixed solution dropwise, the dropping time is 15min, and react for 1.5h after the dropping is completed;

[0080] Step 3: Use a 100mL beaker to mix triethylamine (1.2eq, 0.06mol, 6.06g) and n-octylamine (1eq, 0.05mol, 5.75g) evenly, transfer to a 100mL constant pressure funnel, add the mixed solution drop by drop, drop The addition time is 15 minutes, and the reaction is 1.5 hours after the dropwise addition is completed;

[0081] Step 4: Add 20 g of ethanol dropwise to the round-bottomed fla...

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Abstract

The invention discloses a preparation method of an asymmetric Gemini fluorocarbon surfactant. The preparation method comprises the following steps: step 1, mixing succinyl chloride and a solvent; step2, mixing triethylamine and 1H, 1H-perfluorohexylamine, and drwowise adding the mixed solution at a constant speed to conduct a reaction; step 3, mixing triethylamine and hydrocarbon long-chain primary amine, dropwise adding the mixed solution at a constant speed, and carrying out a reaction; and step 4, continuously dropwise adding 10-20 g of ethanol into a three-neck round-bottom flask, and cooling to room temperature after dropwise adding is completed. The asymmetric Gemini fluorocarbon surfactant is superior to or equivalent to a conventional fluorocarbon surfactant on the market in surface tension reducing capacity and efficiency; meanwhile, the synthesized fluorocarbon surfactant molecule contains a hydrocarbon long chain with a certain length, and has a remarkable effect of reducing the interfacial tension of oil and water.

Description

technical field [0001] The invention belongs to the field of surfactants, and in particular relates to a preparation method of an asymmetric Gemini fluorocarbon surfactant. Background technique [0002] Chemically, the property of reducing the surface tension of a solvent is called surface activity. Substances with surface activity are called surface active substances. Substances that can reduce the surface tension of the solvent, change the interface state of the system, and produce properties such as wetting, emulsification, and foaming are called surfactants. Fluorocarbon surfactants are widely used in various industries due to their unique properties of "three highs and two phobias". [0003] Traditional fluorocarbon surfactants all use C8 fluorocarbon surfactants as raw materials, which react with other chemical raw materials to form corresponding products. In recent years, studies have found that C8 fluorocarbon surfactants, including perfluorooctanoic acid and perfl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01F17/22C07C231/02C07C233/13C09K23/22
CPCC07C231/02C09K23/00
Inventor 陈力群韩跃旺李秀林
Owner SHAANXI YUTENG IND
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