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Sulfamate gemini surfactant and preparation method thereof

A technology of sulfamate and gemini surface, applied in the fields of sulfonate preparation, chemical instruments and methods, organic chemistry, etc., to achieve the effect of mild reaction conditions, easy separation and simple operation

Inactive Publication Date: 2012-08-22
YANGTZE UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But existing surfactant also has many shortcomings
For example: the performance of some surfactants cannot meet the engineering requirements, it is difficult to achieve ultra-low interfacial tension, the performance of temperature resistance and salt resistance is low, and it is easy to be adsorbed by the surface of clay minerals in the formation, especially it cannot have low oil-water interfacial tension and good oil-water interfacial tension at the same time. Foam, foam stabilization effect

Method used

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  • Sulfamate gemini surfactant and preparation method thereof
  • Sulfamate gemini surfactant and preparation method thereof
  • Sulfamate gemini surfactant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of sodium N,N'-bisoctylethylenediamine diethanesulfonate (EM-10):

[0035] 1. Synthesis of the intermediate product N,N'-sodium diethylsulfonate ethylenediamine

[0036] Add 19.82 g (0.33 mol) of ethylenediamine and 26.39 g (0.66 mol) of 50% sodium hydroxide in a 500 mL three-necked flask equipped with a stirrer and a reflux condenser (93.5 mL), and slowly add 2-chloro Sodium ethylsulfonate 109.51 g (0.66 mol) aqueous solution (120 mL), reacted at 80 °C for 8 hours, the pH was maintained at 9-10, after the reaction, cooled to below 10 °C, a large amount of solids precipitated, and the precipitated solids were dried Finally, 102.3 g of a white solid was obtained, with a yield of 70.7%.

[0037] 2. Synthesis of EM-10

[0038] Add 6.08 g (0.019 mol) of the intermediate and 1.49 g (0.037 mol) of sodium hydroxide into a 100 mL three-necked flask equipped with a stirrer and a reflux condenser, then add 20 mL of ethanol, and add 1-bromo Decane 8.29 g (0.037...

Embodiment 2

[0040] Preparation of sodium N,N'-dilauryl ethylenediamine diethanesulfonate (EM-12):

[0041] 1. The intermediate product synthesized by the method of Example 1.

[0042] 2. Synthesis of EM-12

[0043] Add 12 g (0.037 mol) of the intermediate and 2.99 g (0.074 mol) of sodium hydroxide into a 100 mL three-necked flask equipped with a stirrer and a reflux condenser, then add 40 mL of ethanol, and add 1-bromo 18.68 g (0.036 mol) of laurane, keep the pH greater than 8, react at 80°C for 8 hours, cool down to below 10°C, a large amount of solids precipitate out, filter with suction to obtain a white solid, recrystallize with ethanol, and dry to obtain surfactant EM- 12, weighed 13.45 g, and the yield was 54.6%.

Embodiment 3

[0045] Preparation of sodium N,N'-ditetradecylethylenediamine diethanesulfonate (EM-14):

[0046] 1. The intermediate product synthesized by the method of Example 1.

[0047] 2. Synthesis of EM-14

[0048] Add 10 g (0.031 mol) of the intermediate and 2.49 g (0.062 mol) of sodium hydroxide into a 100 mL three-necked flask equipped with a stirrer and a reflux condenser, then add 40 mL of ethanol, and add 1-bromo Tetradecane 17.31 g (0.062 mol), keep the pH greater than 8, react at 80 °C for 7 hours, cool below 10 °C, a large amount of solids precipitate, filter with suction to obtain a white solid, recrystallize with ethanol, and dry to obtain surfactant EM-14 , weighed 11.89 g, and the yield was 49.51%.

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Abstract

The invention discloses a preparation method for a sulfamate gemini surfactant. The sulfamate gemini surfactant is N,N'-dialkyl ethylenediamine diethyl sodium sulfonate. A synthetic method for the sulfamate gemini surfactant comprises the following steps of: 1, adding ethylenediamine and aqueous solution of sodium hydroxide into a reactor, adding the aqueous solution of 2-sodium chloroethanesulfonate into the mixture, stirring the mixture, reacting the mixture at the temperature of 80 DEG C for 6 to 8 hours, keeping the pH to be between 9 and 10, cooling the reaction product until a white solid is separated out, and drying the white solid to obtain N,N'-diethyl sodium sulfonate ethanediamine; and 2, adding the reaction product obtained in the step 1 into the reactor, adding ethanol, adding sodium hydroxide and CH3(CH2)nBr under stirring, wherein n is 7, 9, 11, 13, 15 and 17 respectively, reacting the mixture at the temperature of 80 DEG C for 6 to 8 hours, cooling the reaction product to room temperature until a solid is separated out, filtering the solution, performing recrystallization by using absolute ethyl alcohol, and drying the product to obtain the surfactant. The surfactant is relatively high in surface activity, excellent in cooperativity, simple in synthetic method, mild in reaction conditions, simple in operation, few in by-products, high in yield and easy to separate.

Description

1. Technical field [0001] The invention relates to a synthesis method of a sulfamate gemini surfactant. 2. Background technology [0002] Gemini surfactants usually contain 2 hydrophilic groups and 2 hydrophobic groups. The patent for surfactants with this structure appeared as early as 1935 (Kreimeier, US2106180, 1935.), but about its large-scale Research began in the 1970s. In 1971, Bunton et al. synthesized a series of cationic gemini surfactants in order to explore phase transfer catalysts for nucleophilic substitution reactions, and studied their surface properties and critical micelle concentration (CMC). Properties of water, hydrophobic, flexible and rigid gemini surfactants (Bunton C. A., Robinson L., Catalysis of nucleophilic substitutions by micelles of dicationic detergent[J]. J. Org. Chem, 1971, 36(3): 2346- 2352.). In 1974, Deinega et al. synthesized a double quaternary ammonium salt phase transfer catalyst with the structural characteristics of the surfact...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01F17/16C07C309/14C07C303/32C09K23/16
Inventor 唐善法田磊欧阳向南方飞飞
Owner YANGTZE UNIVERSITY