A kind of preparation method and application of polymerizable monomer
A technology for polymerizing monomers and monomers, which is applied in the field of preparation of polymerizable monomers, can solve the problems of difficult reaction control, low yield and purity of polymerizable monomers, and high production costs, and achieves low production costs and excellent heat resistance. Performance and salt resistance, the effect of less by-products
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preparation example Construction
[0017] The invention provides a kind of preparation method of polymerizable monomer, this method comprises the following steps:
[0018] (1) Under condensation reaction conditions, the general formula is NH 2 -(CH 2 ) n -NH 2 Diamines with the general formula HOOC-(CH 2 ) m The dibasic fatty acid of -COOH is contacted, obtains the intermediate M shown in formula (I);
[0019]
[0020] (2) Under amidation reaction conditions, the intermediate M is contacted with acrylic acid to obtain a polymerizable monomer represented by formula (II);
[0021]
[0022] Wherein, n is an integer of 1-6, m is an integer of 1-8; preferably, n is an integer of 2-6, and m is an integer of 4-8.
[0023] It should be noted that, for the sake of distinction, the present invention refers to the reaction of dibasic fatty acid and amine to obtain amide by removing a molecule of water as condensation reaction, and the reaction of acrylic acid and amine to obtain amide by removing a molecule of...
preparation example 1
[0052] This preparation example is used to illustrate the preparation method of the polymerizable monomer provided by the present invention.
[0053] (1) Preparation of intermediates
[0054] In the there-necked flask, first add 0.1 mol of ethylenediamine, then add 0.1 mol of sebacic acid, start stirring to mix the two evenly, heat to 110°C, and react for 6 hours to obtain the compound containing the structure shown in formula (Ⅲ) The product of intermediate M1.
[0055]
[0056] (2) Preparation of polymerizable monomers
[0057] Under stirring, first dissolve the product containing intermediate M1 obtained in step (1) in 150 ml of dichloromethane, after the dissolution is complete, heat to 70°C, start to add 0.1 mol of acrylic acid dropwise, react for 3 hours, and distill off the solvent And dry it with calcium oxide at 70°C, and recrystallize the product more than three times with acetone solvent to obtain a polymerizable functional monomer D1. The calculated and tested...
preparation example 2
[0061] This preparation example is used to illustrate the preparation method of the polymerizable monomer provided by the present invention.
[0062] (1) Preparation of intermediates
[0063] In the there-necked flask, first add 0.1 mol of hexamethylenediamine, then add 0.1 mol of sebacic acid, start stirring to mix the two evenly, heat to 160°C, and react for 2 hours to obtain the compound containing the structure shown in formula (IV). Product of intermediate M2.
[0064]
[0065] (2) Preparation of polymerizable monomers
[0066] Under stirring, first dissolve the product containing intermediate M2 obtained in step (1) in 150 ml of dichloromethane, after the dissolution is complete, heat to 60°C, start to add 0.1 mol of acrylic acid dropwise, react for 4 hours, and distill off the solvent And dry it with calcium oxide at 70°C, and recrystallize the product more than three times with acetone solvent to obtain a polymerizable functional monomer D2. The calculated and tes...
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