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Si-C novel organosilicon quaternary ammonium salt surfactant and preparation method thereof

A technology of organosilicon quaternary ammonium salt and surfactant, which is applied in the field of preparation of quaternary ammonium salt surfactant to achieve the effect of easy separation and purification, simple post-treatment and mild conditions

Active Publication Date: 2022-07-29
CHUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention: solve the above-mentioned problems existing in the synthesis process of the existing organic silicon surfactant

Method used

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  • Si-C novel organosilicon quaternary ammonium salt surfactant and preparation method thereof
  • Si-C novel organosilicon quaternary ammonium salt surfactant and preparation method thereof
  • Si-C novel organosilicon quaternary ammonium salt surfactant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: prepare organosilicon quaternary ammonium salt surfactant as follows:

[0031] Preparation of chloroplatinic acid catalyst: prepared by dissolving 0.9711 g of chloroplatinic acid in 10 ml of THF treated with distilled water, and stored in a refrigerator before use. Transfer 1.0 mL of this solution to a 100 mL volumetric flask, dilute it to the mark with dry THF, and store at low temperature in the dark after mixing, which can be used for hydrosilation reaction.

[0032] The first step: dimethyl dodecyl allyl ammonium bromide (BC 12 ) preparation:

[0033] A three-necked flask equipped with a thermometer and a reflux condenser was placed in a water bath controlled by a magnetic stirrer, and 40 mL of anhydrous tetrahydrofuran, 8.62 g (0.1 mol) of N,N-dimethylpropenylamine, 24.92 g (0.11 mol) of N-dimethylpropenylamine were added. 1-Bromododecane and 0.33g (0.005mol) zinc powder were reacted at 65°C for 12h, and the reaction was completed. At 45°C, tetrahy...

Embodiment 2

[0036] Embodiment 2: prepare organosilicon quaternary ammonium salt surfactant as follows:

[0037] The first step: dimethyl dodecyl allyl ammonium bromide (BC 16 ) preparation:

[0038] A three-necked flask equipped with a thermometer and a reflux condenser was placed in a water bath controlled by a magnetic stirrer, and 40 mL of anhydrous tetrahydrofuran, 12.92 g (0.15 mol) of N,N-dimethylpropenylamine, 50.38 g (0.165 mol) of N-dimethylpropenylamine were added. 1-Bromohexadecane and 0.49g (0.0075mol) zinc powder were reacted at 65°C for 10h, and the reaction was completed. The tetrahydrofuran was rotary evaporated at 45°C, washed with 30 mL of anhydrous ether for 5 times, and vacuum-dried at 45°C for 5 h to obtain the product.

[0039] The second step: Dimethylhexadecyltriisopropylsilylpropylammonium bromide (TPBC 16 ) preparation:

[0040] Add dimethylhexadecylallylammonium bromide (0.01mol) and 2 mL of chloroplatinic acid catalyst into a three-necked flask equipped wit...

Embodiment 3

[0041]Embodiment 3: prepare organosilicon quaternary ammonium salt surfactant as follows:

[0042] The first step: Dimethyl octadecyl allyl ammonium bromide (BC 18 ) preparation:

[0043] A three-necked flask equipped with a thermometer and a reflux condenser was placed in a water bath controlled by a magnetic stirrer, and 40 mL of anhydrous tetrahydrofuran, 8.62 g (0.1 mol) of N,N-dimethylpropenylamine, 24.92 g (0.11 mol) of N-dimethylpropenylamine were added. 1-Bromooctadecane and 0.33g (0.005mol) zinc powder were reacted at 50°C for 18h, and the reaction was completed. At 45°C, tetrahydrofuran was rotary evaporated, washed with 30 mL of anhydrous ether for 5 times, and vacuum-dried at 45°C for 5 hours to obtain the product.

[0044] The second step: dimethyl octadecyl trihexyl propyl ammonium bromide (TPBC 18 ) preparation:

[0045] Add dimethyl octadecyl allyl ammonium bromide (0.01 mol) and 6 mL of chloroplatinic acid catalyst into a three-necked flask equipped with a...

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Abstract

The invention discloses a novel Si-C organosilicon quaternary ammonium salt surfactant and a preparation method thereof. The preparation method comprises the following steps: 1) preparation of a cationic intermediate: carrying out a reaction on dimethylallylamine and brominated long-chain alkane to prepare the cationic intermediate; and 2) by taking anhydrous tetrahydrofuran as a solvent, chloroplatinic acid as a catalyst and alkyl silane as a raw material, reacting the cationic intermediate prepared in the step 1 with trialkyl silane according to a molar ratio of 1: (1.1-1.3), heating under the protection of nitrogen, stirring at 70-90 DEG C for 5-8 hours, and after the reaction is finished, treating the obtained reaction liquid to obtain the Si-C novel organosilicon quaternary ammonium salt surfactant. The novel Si-C organosilicon quaternary ammonium salt surfactant has the advantages of excellent surface activity, certain bactericidal activity and wide application space. The method is simple to operate, mild in reaction condition and high in product purity. Good reaction characteristics are shown.

Description

technical field [0001] The invention relates to the technical field of preparation of quaternary ammonium salt surfactants, in particular to a new Si-C organosilicon quaternary ammonium salt surfactant and a preparation method. Background technique [0002] Silicone surfactant is a new type of surfactant developed with new silicone materials. Its hydrophobic groups (Si-O-Si, etc.) are more hydrophobic than traditional carbon chains, and have excellent surface tension reduction. It is a kind of efficient surfactant, so it has also become one of the research hotspots in the field of surfactants. [0003] Silicone surfactant is composed of polysiloxane and hydrophilic group, and its general structural formula is shown in the following formula. Among them, when R is a polyoxyethylene ether nonionic group, it is a non-ionic silicone surfactant; R is a polar group such as a sulfonic acid group, a carboxyl group and a phosphoric acid group, and it is an anionic surfactant; R conta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K23/54C07F7/10
CPCC07F7/0829C07F7/081
Inventor 刘学立满晓磊魏春晖耿庆保
Owner CHUZHOU UNIV
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