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A preparation method for a novel dendritic oligomeric quaternary ammonium surfactant

A surfactant and dendritic technology, applied in the field of oligomeric surfactant synthesis, can solve the problems of single and single morphological structure, and achieve the effect of high surface activity, wide application prospect and low critical micelle concentration

Inactive Publication Date: 2013-09-11
山东大学(威海)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the research on the synthesis of oligomeric surfactants by quaternization modified PAMAM is still in its infancy, and many problems remain to be solved. For example, the reaction nucleus of the initiator for the synthesis of PAMAM is relatively single, and most of the synthetic surfactants are tetrameric surfactants. , single shape structure, etc.

Method used

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  • A preparation method for a novel dendritic oligomeric quaternary ammonium surfactant
  • A preparation method for a novel dendritic oligomeric quaternary ammonium surfactant
  • A preparation method for a novel dendritic oligomeric quaternary ammonium surfactant

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1, the preparation of a kind of quaternized polyamide-amine dendritic surfactant

[0030] (1) Preparation of compound (I)

[0031] Place a 50mL three-necked flask in an ice-water bath, first pass nitrogen gas for 3 to 5 minutes, then add 5mL of methanol, measure 2.05g (20mmol) N, N-dimethyl-1,3-propanediamine, and add it to the three-necked flask while stirring , continue to stir for 20min, then measure 6.89g (80mmol) of methyl acrylate, and drop it into the flask at a rate of drop / 3s. 2 The stirring reaction was continued for 1 day under protection. After the reaction, add methanol repeatedly for vacuum rotary evaporation to remove excess methyl acrylate, and finally remove the solvent methanol by rotary evaporation. The vacuum rotary evaporation temperature is controlled at 30-40°C. During vacuum rotary evaporation, the pressure should be increased a little to prevent the sample from bumping. . Finally, 5.35 g of slightly viscous transparent liquid was o...

Embodiment 2

[0036] Embodiment 2, the preparation of a kind of quaternized polyamide-amine dendritic surfactant

[0037] (1) Preparation of compound (I)

[0038] As described in Example 1, the difference is that the quality of N,N-dimethyl-1,3-propylenediamine is changed to 1.04g (10mmol), and the quality of methyl acrylate is changed to 5.18g (60mmol) , the quality of the obtained compound (I) was 2.67g, and the yield was 95.7%.

[0039] (2) Preparation of compound (II)

[0040]As described in Example 1, the difference is that the quality of N,N-dimethyl-1,3-propanediamine is changed to 5.09g (50mmol), and the quality of compound (I) is changed to 1.40g (5mmol) ), as a result, compound (I) has not reacted completely for 6 days.

[0041] (3) Preparation of compound (III)

[0042] As described in Example 1, the difference is that the quality of compound (II) is changed to 1.24g (3mmol), and the quality of bromododecane is changed to 4.48g (18mmol), and the quality of gained compound (II...

Embodiment 3

[0043] Embodiment 3, the preparation of a kind of quaternized polyamide-amine dendritic surfactant

[0044] (1) As described in Example 1, the difference is that the quality of N,N-dimethyl-1,3-propylenediamine is changed to 20.6g (202mmol), and the quality of methyl acrylate is changed to 70.7g (822mmol), the quality of the obtained compound (I) was 54.0g, and the yield was 97.6%.

[0045] (2) As described in Example 1, the difference is that the reaction temperature is raised to 40° C., and the reaction time is 3 to 4 days, but it can be seen from the hydrogen spectrum that there are miscellaneous peaks and the product is impure.

[0046] (3) As described in Example 1, the difference is that the quality of compound (II) is changed to 1.66g (4mmol), the volume dissolved in solvent is 6mL, and the quality of bromododecane is changed to 7.97g ( 32mmol), the volume dissolved in the solvent was 6mL, the quality of the obtained compound (III) was 3.71g, and the yield was 79.8%. ...

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Abstract

The present invention provides a preparation method for a novel dendritic oligomeric quaternary ammonium surfactant. The method comprises the following steps: (1) N, N-dimethyl-1,3 - propanediamine and an excess amount of methyl acrylate are subjected to a Michael addition reaction to generate a compound (I); (2) the compound (I) and an excess amount of N, N-dimethyl-1 ,3 - propanediamine are subjected to an amidation reaction to obtain a compound (II); and (3) the compound (II) and bromododecane are subjected to a quaternization reaction to obtain the final product of a compound (III). The surfactant prepared by using the method of the invention has excellent performances, and can be widely used in fields such as daily chemicals, water treatment, paper making and oilfield development.

Description

technical field [0001] The invention relates to a preparation method of a quaternary ammonium salt surfactant, in particular to a preparation method of a polyamide-amine (PAMAM) dendritic quaternary ammonium salt surfactant, and belongs to the technical field of oligomeric surfactant synthesis. Background technique [0002] Dendritic oligomeric surfactant is a new type of surfactant with a special structure, which is composed of two or more amphiphilic groups connected by a linking group, and its relative molecular weight is usually between the traditional surface Between the active agent and the polymer surfactant, it fills the gap between the two. Compared with traditional surfactants, oligomeric surfactants have lower critical micelle concentration, higher surface activity and unique rheological properties. Based on its superiority in various aspects, oligomeric surfactants have good application prospects in the synthesis of new substances, emulsion polymerization, corro...

Claims

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Application Information

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IPC IPC(8): C07C237/10C07C231/12B01F17/18B01F17/22C09K23/18C09K23/22
Inventor 车玉菊孟凡君房美灵马庆林
Owner 山东大学(威海)
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