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Preparation method and application of normal-temperature ketone and hydrazine self-crosslinked nanometer epoxy resin emulsion

A technology of epoxy resin emulsion and epoxy resin, which is applied in coatings, anti-corrosion coatings, etc., can solve the problems of affecting performance, complicated reaction steps, and difficult to disperse, and achieve simple use process, reduce energy consumption, and good cross-linking effect of effect

Inactive Publication Date: 2015-07-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the process of adding water to disperse, due to the hydrogen bond between the epoxy group and water, the viscosity is relatively high and it is not easy to disperse
[0006] The invention patent with the authorized notification number CN102432831B discloses a preparation method of a one-component normal temperature self-drying water-based epoxy resin modified by unsaturated fatty acid and its coating, although it can also realize normal temperature self-crosslinking and epoxy resin water-based It has good performance, but it does not first use lauric acid to open the ring of epoxy resin, consume epoxy groups, and then use acrylic monomers for grafting, so the reaction process is difficult to control, and gels are prone to occur. It is also difficult to increase the solid content of the obtained product
The publication number is CN103319665A. On the basis of the invention patent with the authorized announcement number CN102432831B, the cross-linking monomer glycidyl methacrylate and N-methylol acrylamide are added to realize multiple self-crosslinking. The reaction steps are complicated, and the performance is better than the former. It has been greatly improved, but it still needs to be improved in terms of impact resistance and flexibility, which seriously affects its performance

Method used

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  • Preparation method and application of normal-temperature ketone and hydrazine self-crosslinked nanometer epoxy resin emulsion
  • Preparation method and application of normal-temperature ketone and hydrazine self-crosslinked nanometer epoxy resin emulsion
  • Preparation method and application of normal-temperature ketone and hydrazine self-crosslinked nanometer epoxy resin emulsion

Examples

Experimental program
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Effect test

Embodiment 1

[0035]Put 20g of epoxy resin E-06 into a four-necked flask equipped with a stirrer, thermometer and condenser tube, heat it to 100°C to melt it completely, add the remaining 80g of epoxy resin, 75g of lauric acid, 3g of four-necked Ethylammonium bromide, stirred, and after 1h, the temperature was raised to 110°C to continue the reaction, and the reaction was stopped when the acid value reached 3mg / L. Add 10g of n-butanol and 20g of propylene glycol monobutyl ether mixed solvent to dissolve, under the protection of nitrogen, stir and heat to 115°C, add 10g of methacrylic acid (MAA) and 20g of methyl methacrylate (MMA) dropwise continuously within 1h , 10g styrene (St), 40g butyl acrylate (BA), 3gDAAM and 3g dibenzoyl peroxide (BPO) mixed solution, constant temperature reaction for 4h, cooled to 50 ° C, dropwise added 10g triethylamine (TEA) To form a salt, add 250g of deionized water, and stir rapidly at 1000r / min for 30min to obtain a water-based epoxy emulsion. Adjust the pH...

Embodiment 2

[0040] Put 20g of epoxy resin E‐12 into a four-necked flask equipped with a stirrer, thermometer and condenser, heat it to 100°C to melt it completely, add the remaining 80g of epoxy resin, 75g of lauric acid, 3g of Ethylamine, stirred, and after 1 hour, the temperature was raised to 110°C to continue the reaction, and the reaction was stopped when the acid value reached 3 mg / L. Add 10g of n-butanol and 20g of propylene glycol monobutyl ether mixed solvent to dissolve, under the protection of nitrogen, stir and heat to 115°C, add 15g of acrylic acid (AA), 20g of MMA, 10g of St, 40g of BA, 2g of DAAM and 5g of azo continuously dropwise within 1h The mixed solution of diisobutylcyanide was reacted at constant temperature for 4 hours, cooled to 50°C, 10g of TEA was added dropwise to form a salt, and 250g of deionized water was added, and stirred rapidly at 1000r / min for 30min to obtain a water-based epoxy emulsion. Adjust the pH to 7, then add 2g of ADH aqueous solution, and stir...

Embodiment 3

[0043] Put 20g of epoxy resin E‐20 into a four-neck flask equipped with a stirrer, thermometer and condenser, heat it to 100°C to melt it completely, add the remaining 80g of epoxy resin, 75g of lauric acid, 3g of Phenylphosphine was stirred, and after 1 hour, the temperature was raised to 110°C to continue the reaction, and the reaction was stopped when the acid value reached 3 mg / L. Add 10g of n-butanol and 20g of propylene glycol monobutyl ether mixed solvent to dissolve, under the protection of nitrogen, stir and heat to 115°C, add 10gMAA, 20gMMA, 10gSt, 40gBA, 3gDAAM and 3g di-tert-butyl peroxide dropwise within 1h The mixed solution of the compound was reacted at constant temperature for 4 hours, cooled to 50°C, 10g of TEA was added dropwise to form a salt, and 250g of deionized water was added, and stirred rapidly at 1000r / min for 30min to obtain a water-based epoxy emulsion. Adjust the pH to 7, then add 3g of ADH aqueous solution, and stir for 20 minutes to obtain a ro...

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Abstract

The invention discloses a preparation method and an application of normal-temperature ketone and hydrazine self-crosslinked nanometer epoxy resin emulsion. The preparation method comprises the following steps: firstly opening a ring of epoxy resin by using lauric acid; consuming away epoxy groups; performing grafting polymerization by using diacetone-acrylamide and an acrylic acid type monomer; neutralizing the emulsion and adding water for dispersion to obtain grafted epoxy emulsion; and adding hexane diacid dihydrazide to prepare normal-temperature self-crosslinked nanometer epoxy resin emulsion. The solid content of the emulsion disclosed by the invention is 45% to 55%; the particle size is 80nm to 100nm; the storage stability is above 6 months; the adhesive force reaches 0-1 grade after the emulsion becomes a film by room temperature curing; the hardness of a pencil is H to 2H; the impact resistance is 50kg.cm to 65kg.cm; the flexibility is 2mm to 3mm; the water resistance is 120h to 150h; and the resistance to 3% NaCl solution is 100h to 180h. The emulsion disclosed by the invention can be widely applied to the fields of water-based anticorrosive paints, water-based wood paints, water-based automobile paints, water-based building paints and the like as base resin.

Description

technical field [0001] The present invention relates to an epoxy resin emulsion, in particular to a preparation method of room temperature ketone hydrazine self-crosslinking nano-epoxy resin emulsion. Coatings and the like have a wide range of applications and belong to the field of functional polymer materials. Background technique [0002] At this stage, domestic epoxy resins still need to add a large amount of co-solvents during the water-based process, and the solid content is basically below 40%, which is not really environmentally friendly. Secondly, the water-based epoxy resin system is generally a two-component system. It is often necessary to add a curing agent before construction, so that the system has a contradiction between curing temperature, curing time and storage stability, and the self-crosslinking system at room temperature can solve this problem well. Contradictions, so the study of low VOC room temperature self-crosslinking epoxy resin emulsion has far-...

Claims

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Application Information

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IPC IPC(8): C08F283/10C08F220/14C08F220/18C08F212/08C08F220/06C09D151/08C09D5/08
Inventor 袁腾涂伟萍周显宏王锋胡剑青
Owner SOUTH CHINA UNIV OF TECH
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