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Preparation method of epoxy quaternary ammonium salt

A technology of epoxy quaternary ammonium salt and epichlorohydrin, applied in the field of antibacterial materials, can solve the problems of intensified ring opening, difficult post-processing, sudden rise in system temperature, etc., and achieves moderate reaction rate, saving energy consumption and solvent consumption. less effect

Pending Publication Date: 2019-12-31
QILU UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

If the feeding rate is not controlled during the reaction, the heat of reaction generated will cause the temperature of the system to rise sharply, resulting in aggravated ring opening
And the solvent used in this method is isopropanol, because the higher boiling point causes post-processing difficulties

Method used

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  • Preparation method of epoxy quaternary ammonium salt
  • Preparation method of epoxy quaternary ammonium salt
  • Preparation method of epoxy quaternary ammonium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0039] A kind of preparation method of epoxy quaternary ammonium salt, comprises steps as follows:

[0040] (1) When equipped with N 2 14.73g of N,N-dimethyltetradecylamine and 5ml of solvent methanol were added to the three-neck flask with protection device, thermometer, reflux condenser and magnet, and the temperature was slowly raised to 38°C.

[0041] (2) After the temperature of the system reaches 38°C, slowly add a mixture of 7.25g of epichlorohydrin and 5ml of methanol dropwise. After the dropwise addition, keep the reaction at 38°C for 6 hours, stop the reaction, and cool down to room temperature.

[0042] (3) The reaction mixture was rotary evaporated for 2 hours to remove the solvent methanol, eluted with anhydrous petroleum ether for 6-8 times, and vacuum-dried at 40° C. for 24 hours to obtain a white product.

[0043] The epoxy quaternary ammonium salt 1HNMR spectrum that present embodiment obtains is as figure 1 As shown, FT-IR as figure 2 shown.

Embodiment 2

[0045] A kind of preparation method of epoxy quaternary ammonium salt, comprises steps as follows:

[0046] (1) When equipped with N 2 A certain amount of N,N-dimethylhexadecylamine (15.51 g) and solvent methanol (5 ml) were added to a three-necked flask with a protective device, a thermometer, and a reflux condenser, and the temperature was slowly raised to 38°C.

[0047] (2) After the system temperature reaches 38°C, slowly add a certain amount of epichlorohydrin (8.06g) and methanol (5ml) mixture dropwise. After the dropwise addition, keep the reaction at 38°C for 6 hours, stop the reaction, and cool down to room temperature.

[0048](3) The reaction mixture was rotatably evaporated to remove solvent methanol, eluted with anhydrous petroleum ether for 6-8 times to remove impurities, and finally vacuum-dried for 24 hours to obtain a white product of 18.83 g.

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Abstract

The invention relates to a preparation method of an epoxy quaternary ammonium salt. The method includes: taking epichlorohydrin as a quaternization reagent for reaction with alkyl dimethyl tertiary amine in an organic solvent at 30DEG C-45DEG C for 2-8h. The epoxy quaternary ammonium salt prepared by the method has good quaternization rate and epoxy value, the product purity is greater than or equal to 90%, and the epoxy group content can reach up to about 27%, thus being more beneficial to subsequent modification combination with gelatin. According to the method disclosed by the invention, the conversion rate can reach 80-90% within 4-6h at a low reaction temperature, and the reaction rate is moderate.

Description

technical field [0001] The invention relates to a preparation method of epoxy quaternary ammonium salt, in particular to a preparation method of epoxy quaternary ammonium salt with high epoxy value and excellent antibacterial performance, belonging to the technical field of antibacterial materials. Background technique [0002] The epoxy quaternary ammonium salt is based on the structure of the conventional quaternary ammonium salt, and an epoxy group is introduced, thereby improving its own reactivity. The corresponding cationic products can be obtained through the reaction of the epoxy group in the epoxy quaternary ammonium salt with the hydroxyl group, amino group and other active groups in the natural polymer. Therefore, epoxy quaternary ammonium salt is not only a cationic surfactant, but also a good functional cationic monomer modifier, and has broad application value. [0003] The current synthesis method basically uses epichlorohydrin and tertiary amine hydrochlorid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/00C07D303/36C07D301/32
CPCC07D301/00C07D303/36C07D301/32
Inventor 李俊英马烽于宁朱志飞吴启铭
Owner QILU UNIV OF TECH
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