Preparation method of carboxyl-contained polyacrylic ester with low molecular weight
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A technology of polyacrylate and acrylate, which is applied in the direction of coating, etc., and can solve problems such as hindering the application range
Inactive Publication Date: 2011-02-09
BEIJING UNIV OF CHEM TECH
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Embodiment 1
[0030] The first step is to add acrylic acid (AA), methyl acrylate (MA) and ethyl acrylate (BA) with a molar ratio of 1:1:1 in a reactor equipped with a condenser, a stirrer, and a heating device. Initiator AIBN with 1 mol% of the total amount of monomers is the chain transfer agent n-dodecanethiol [S] with 0.5 mol% of the total amount of monomers, add the solvent toluene, stir and heat to 50°C to dissolve all the reactants, and then heat to 73°C, after one hour of reaction, start to measure the infrared spectrum, wait until 1650cm -1 and 810cm -1 The absorption peak of the acrylate double bond disappears, that is, the reaction is complete.
[0031] The molecular weight (Mn) and molecular weight distribution (PDI) of the product were measured, and the results are shown in Table 1.
[0032] In the second step, the product is dried and dissolved in acetone, and the acid value is measured with KOH ethanol solution as the titrant and phenolphthalein as the indicator. Then, acco...
Embodiment 2～ example 3
[0035] Embodiment 2~Example 3, with embodiment 1, only the consumption of chain transfer agent changes, changes into 2%, 4% respectively.
Embodiment 4
[0037] The first step is to add acrylic acid (AA) and ethyl acrylate (EA) with a molar ratio of 1:2 in a reactor equipped with a condenser, an agitator, and a heating device, and the addition is 0.25mol% of the total amount of monomers Agent AIBN is the chain transfer agent n-dodecanethiol [S] with 3.0mol% of the total amount of monomers. Add the solvent toluene, stir and heat to 50°C and all the reactants are completely dissolved, then heat to 73°C, and react for one hour. Start to measure the infrared spectrum, wait for 1650cm -1 and 810cm -1 The absorption peak of the acrylate double bond disappears, that is, the reaction is complete.
[0038] The molecular weight (Mn) and molecular weight distribution (PDI) of the product were measured, and the results are shown in Table 1.
[0039] In the second step, the product is dried and dissolved in acetone, and the acid value is measured with KOH ethanol solution as the titrant and phenolphthalein as the indicator. Then, accordi...
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Abstract
The invention relates to a preparation method of carboxyl-contained polyacrylic ester with low molecular weight, belonging to the field of light-curing low polymers. The low polymer side chain contains carboxyls, has low molecular weight and high reaction speed and conversion rate as well as obviously enhanced absorption capability to a substrate by the carboxyl content in the structure. The preparation method of the low polymer comprises the following steps of: copolymerizing solution free radicals of one or more of (methyl) acrylic acid and (methyl) acrylic alkyl acrylate to obtain a main chain including pure C-C bonds; and then, introducing the side chain with light reaction activity through a condensation reaction of functional groups, wherein monomers participating in the condensation reaction include glycidyl methacrylate, heahydroxy-ethyl acrylate, and the like. The invention controls the molecular weight and the molecular weight distribution of the low polymer by selecting the monomers and controlling the content of acrylic acid and the dosages of an initiator and a chain transfer agent and controls the content of carboxyl groups by controlling the esterification rate to prepare the polyacrylic ester low polymer with excellent performance. The process has the advantages of simple and convenient operation and easy industrial production.
Description
Technical field: [0001] The present invention relates to UV photocurable acrylate resin. It belongs to the field of photocurable oligomers. Background technique [0002] UV curing technology has "5E" advantages, namely: Efficient (high efficiency), Enabling (wide adaptability), Economical (economical), Energy Saving (energy saving) and Environmental Friendly (environmental friendly), widely used in coatings, inks, adhesives , printing plate making, stereolithography and precision machining and other fields. The UV curing system is mainly composed of oligomers, reactive diluents, photoinitiators and other additives, among which oligomers account for 50-80% of the entire formula, which determines the main physical and chemical properties of the cured film and is the most important made of. [0003] Polyacrylate acrylic resin is an oligomer with less research, but it is an important type of photocurable prepolymer, which has the following main advantages: 1. There is no benz...
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