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A kind of branched polyquaternium salt and its synthetic method
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A technology of polyquaternium and quaternary ammonium salt, which is applied in the field of branched polyquaternium salt and its synthesis, and can solve the problems of low reaction efficiency and the like
Active Publication Date: 2017-06-27
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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[0004] In the method for preparing polyquaternium salt in the prior art, directly react with halogenated compound and polyethyleneimine, and reaction efficiency is low, needs a large amount of halogenated compound to obtain polyquaternium salt with higher degree of quaternization
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Embodiment 1
[0104] (1) Dissolve 1 mole of branched polyethyleneimine in water, add 10 moles of formic acid and 5 moles of formaldehyde, and perform amine methylation reaction at 70°C for 1 day to obtain methylated branched polyethyleneimine. Ethyleneimine;
[0105] The 1H NMR spectrum of methylated branched polyethyleneimine is as follows figure 2 shown.
[0106] (2) Dissolve the product of step (1) in N,N-dimethylformamide, then add 1.5 molar parts of dodecylbromoacetate, and carry out the reaction at 50°C for 1 day, the solvent N, N-dimethylformamide is removed, then precipitated and dried to obtain branched polyquaternium salts.
[0107] Adopt conventional NMR technique to detect, the 1H nuclear magnetic resonance spectrum of gained branched polyquaternium salt is as follows figure 1 As shown, 0.89(t,3H,CH 3 ),1.24~1.37(m,(CH 2 ) n ),1.58(m,2H,CH 2 ),1.68(m,2H,CH 2 ),3.65(s,3H,(CH 3 ) 2 N + ),3.82(t,2H,CH 2 ),4.20(t,2H,O-CH 2 ),4.83(s,2H,CH 2 -CO).
[0112] (2) Dissolve 1 mole part of the product of step (1) in N,N-dimethylacetamide, then add 5 mole parts of tetradecyl chloroacetate, and react at 90°C for 5 days. Solvent N,N-dimethylacetamide is removed, then precipitated and dried to obtain branched polyquaternium salt.
Embodiment 3
[0114] (1) Dissolve 1 mole of branched polyethyleneimine in ether, add 15 moles of formic acid and 10 moles of formaldehyde, and react at 90°C for 2 days to obtain methylated branched polyethyleneimine ;
[0115] (2) Dissolve 1 mole part of the product of step (1) in methanol, then add 2 mole parts of benzyl bromide, react at 80°C for 2 days, remove the solventmethanol, then precipitate and dry to obtain branched poly quaternary ammonium salt.
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Abstract
The present invention provides a branched poly quaternaryammonium salt (PQAS). The present invention further provides a method for synthesizing the PQAS, wherein branched polyethyleneimine is subjected to an aminomethylation reaction to obtain methylated branched polyethyleneimine, and the methylated branched polyethyleneimine reacts with a halogenated compound to obtain the PQAS. According to the present invention, the method has characteristics of rapidness, efficiency, low cost, simple process and high yield; and the PQAS has the contact type bactericidal capacity, the internal branched structure can embed the guest molecules such as antibiotics, dyes and the like to form the slow release type bactericidal capacity, and the compatibility between the PQAS and the water or resin can be adjusted with different halogenated compounds, such that the PQAS can be used in the fields of antibacterial lotion and material formula, dyeing formulas of plastics, coating materials or films, and the like.
Description
technical field [0001] The invention relates to the field of chemical engineering, in particular to a branched polyquaternary ammonium salt and a synthesis method thereof. Background technique [0002] Microbial contamination has a huge impact and hazards on food and water safety, medical and drug safety, biological materials, etc., and is closely related to our lives. The current antibacterial materials are mainly divided into contact type and release type. Typical contact antibacterial materials are materials containing functional groups of quaternaryammonium radicals and cationic polymers on the surface, which can play an antibacterial effect by destroying the cell structure of bacteria, but have the disadvantage of being insensitive to Gram-negative bacteria and specific resistant bacteria. The release antibacterial material mainly achieves long-term antibacterial effect by coating some toxic substances such as antibiotics, algaecides, preservatives, and nanosilver in ...
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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/00A01N33/12A01P3/00
Inventor 韩金姜道义周鑫乌学东
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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