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Dendritic tetrameric quaternary ammonium salt surfactant preparation method

A surfactant and polyquaternary ammonium salt technology, which is applied in the preparation of polyamide-amine dendritic quaternary ammonium salt surfactants, and the field of preparation of quaternary ammonium salt surfactants, can solve the problem of single morphological structure and single reaction core, etc. problems, to achieve the effect of easy availability of raw materials, high surface activity, and simple synthesis

Inactive Publication Date: 2016-04-27
SHANDONG UNIV
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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 through quaternization modified PAMAM is still in its infancy, and many problems still need to be solved. Tetrameric surfactants with single morphological structure, etc.

Method used

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  • Dendritic tetrameric quaternary ammonium salt surfactant preparation method
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  • Dendritic tetrameric quaternary ammonium salt surfactant preparation method

Examples

Experimental program
Comparison scheme
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 3~5min, weigh 0.9g (10mmol) of 2-hydroxy-1,3-propanediamine, dissolve it in 10ml of methanol, add it to the three-necked flask, and continue stirring for 20min , then measure 17.2g (200mmol) methyl acrylate, drop it into the flask at a rate of drop / 3s, after the dropwise addition, wait for the temperature to rise to room temperature naturally, then heat up to 30°C, N 2 Under protection, the stirring reaction was continued for 36h. 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 30~35°C. During vacuum rotary evaporation, the pressure should be increased a little to preven...

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 methyl acrylate is changed to 5.16g (60mmol), the quality of the obtained compound (I) is 4.23g, and the yield is 97.74%. The analysis of the hydrogen spectrum shows that the obtained non-target product , not connected with four chains, suspected to be a mixture of three chains and two chains.

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

[0040]As described in Example 1, the difference is that the mass of N,N-dimethyl-1,3-propanediamine is changed to 4.22g (41.4mmol), and after reaction 5, the compound (I) is still not completely reacted .

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

[0042] As described in Example 1, the difference is that the mass of compound (II) is changed to 0.77g (1.08mmol), the volume dissolved in the solvent is 6mL, and the mass of bromododeca...

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 mass of 2-hydroxy-1,3-propylenediamine is changed to 0.18g (2mmol), and the mass of methyl acrylate is changed to 2.06g (24mmol), The mass of the obtained compound (I) was 0.41 g, and the yield was 96%. According to the analysis of the hydrogen spectrum, as the proportion of methyl acrylate increased, the product was suspected to be part of the target product and part of the three-chain product.

[0045] (2) As described in Example 1, the difference is that the reaction temperature is increased to 40°C, and the reaction time is 4-5 days, but there are miscellaneous peaks in the hydrogen spectrum, and the product is impure.

[0046] (3) As described in Example 1, the difference is that the mass of compound (II) is changed to 0.79g (1.1mmol), the volume dissolved in the solvent is 6mL, and the mass of bromododecane ...

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Abstract

The invention provides a novel dendritic tetrameric quaternary ammonium salt surfactant preparation method. The method comprises the following steps: (1) 2-hydroxy-1,3-propanediamine is subjected to a Michael addition reaction with excessive methyl acrylate, such that a compound (I) is obtained; (2) the compound (I) is subjected to an amidation reaction with excessive N,N-dimethyl-1,3-propanediamine, such that a compound (II) is obtained; and (3) the compound (II) is subjected to a quaternization reaction with bromododecane, such that a final product compound (III) is obtained. With the method provided by the invention, the prepared surfactant has excellent properties, and has good application prospects in the fields of daily chemicals, water treatment, papermaking, oil field development and the like.

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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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/10C07C231/12B01F17/22C09K23/22
Inventor 车玉菊孟凡君房美灵陈思齐
Owner SHANDONG UNIV
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