Preparation method of organic silicon modified normal-temperature multiple self-crosslinked 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 consuming epoxy groups, affecting application performance, and prone to gelation, etc., and achieves improved corrosion resistance and wear resistance , fast drying speed, and the effect of increasing the crosslinking density

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

[0004] 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 water-based epoxy resin 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, but the performance is better than the former. It has been greatly improved, and this technology does not involve silicone modification. In terms of mechanical properties, especially in terms of impact resistance and flexibility, it needs to be further improved, which seriously affects its application performance.

Method used

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  • Preparation method of organic silicon modified normal-temperature multiple self-crosslinked epoxy resin emulsion
  • Preparation method of organic silicon modified normal-temperature multiple self-crosslinked epoxy resin emulsion
  • Preparation method of organic silicon modified normal-temperature multiple self-crosslinked 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-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, 2g tetra 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, 3g vinyltriethoxysilane (A‐151) and 1g dibenzoyl peroxide (BPO) mixed solution, constant temperature reaction 4h, Cool to 50°C, add 10g of triethylamine (TEA) dropwise to form a salt, add 250g of deionized water, and stir rapidly at 1000r / min for 30min to obtain a water-based epoxy emulsion. Adj...

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, 2g of vinyl continuously dropwise within 1h A mixed solution of trimethoxysilane (A‐171) and 5g of azobisisobutylcyanide, reacted at constant temperature for 4h, cooled to 50°C, added 10gTEA dropwise to form a salt, added 250g of deionized water, and stirred rapidly at 1000r / min for 30min to obtain Waterborne epoxy emulsion. Adjust the pH to 7, then add 2g of ADH aqueous solution...

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 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 AA, 20g of MMA, 10g of St, 40g of BA, 3g of DAAM, 1g of vinyl triisopropoxide dropwise within 1h A mixed solution of base silane (A-1706) and 3g di-tert-butyl peroxide, react at constant temperature for 4h, cool to 50°C, add 10gTEA dropwise to form a salt, add 250g deionized water, stir rapidly at 1000r / min for 30min to obtain water-based epoxy emulsion. Adjust the pH to 9, then add 2g of ADH aqueous solution, and stir for 20 minutes to o...

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Abstract

The invention discloses a preparation method of organic silicon modified normal-temperature multiple self-crosslinked epoxy resin emulsion. The preparation method comprises the following steps: opening a ring of epoxy resin by using lauric acid; consuming away epoxy groups; performing grafting polymerization by using double-bond organo-siloxane, diacetone-acrylamide and an acrylic acid type monomer; and neutralizing the emulsion and adding hexane diacid dihydrazide to obtain the organic silicon modified normal-temperature multiple self-crosslinked epoxy resin emulsion. After the emulsion is formed into a film, ketone carbonyl and hydrazine have dehydration reaction under an acidic condition to generate a hydrazine compound; silanol and an active group of a polymer are condensed to form a three-dimensional network structure in order to realize normal-temperature multiple self-crosslinking. The solid content of the emulsion prepared by the method disclosed by the invention is 45% to 55%; the adhesive force reaches 0-1 grade after the film is formed by room temperature curing; 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 a 3% NaCl solution is 100h to 180h. The emulsion disclosed by the invention can be widely applied to various water-based paints as base resin.

Description

technical field [0001] The invention relates to an epoxy resin emulsion, in particular to a method for preparing an organosilicon-modified room temperature multiple self-crosslinking epoxy resin emulsion. Water-based architectural coatings and the like have a wide range of applications and belong to the field of functional polymer materials. Background technique [0002] Epoxy resins are widely used in the fields of coatings, adhesives and composite materials because of their good mechanical properties, adhesive properties, curing shrinkage and process properties. However, most epoxy resins are insoluble in water and easily soluble in organic solvents, which are flammable, explosive, and pollute the environment, which brings a lot of inconvenience to storage, transportation and construction. 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 en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/10C08F230/08C08F220/58C08F220/18C08F220/06C08F220/14C08F212/08C08G59/16C08J3/24C09D151/08C09D5/08
Inventor 袁腾涂伟萍周显宏王锋胡剑青
Owner SOUTH CHINA UNIV OF TECH
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