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Preparation method for non-ionic reactive water-borne epoxy resin emulsion

A water-based epoxy resin, non-ionic technology, applied in the direction of epoxy resin coating, coating, etc., can solve the problems of high reaction temperature, large emulsion particle size, poor emulsion stability, etc., to achieve simple operation method, emulsion particle size Small, good stability effect

Inactive Publication Date: 2015-04-29
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The document "Journal of Liaoning Petrochemical University" [2008,28(1):8-14] prepared epoxy-acrylic acid self-emulsifying water-based anticorrosion emulsion by graft copolymerization of acrylic epoxy resin, but the disadvantage of grafting reaction is that The randomness of the branch point, the competition between the grafting reaction and the self-polymerization of the modifier is difficult to control, and the quality of batch products is not stable
The literature "Polymer Materials Science and Engineering" [2006,22(4):40-45] carries out alcoholysis reaction with maleic anhydride and the secondary hydroxyl group on the main chain of bisphenol A epoxy resin, and in the main chain of epoxy resin Hydrophilic carboxyl groups are introduced into the water-based epoxy resin, but the disadvantage of the esterification method is that the ester bond of the esterification product will be hydrolyzed with time, resulting in an unstable system
The document "Coating Industry" [2010,40(9)] catalyzed by epoxy resin E-51 and polyethylene glycol in triphenylphosphine, at a reaction temperature of 150°C, reacted for 4 hours to synthesize waterborne epoxy Resin, add 10% emulsifier of epoxy resin E-51 mass to emulsify epoxy resin, add distilled water dropwise, stir vigorously, make water-based epoxy resin emulsion, but this method is because the molecular weight of epoxy resin used is low, makes synthesis The molecular chain segment of the emulsifier is short, it is difficult to fully cover the epoxy resin, and the particle size of the obtained emulsion is large, and the reaction temperature of this method is too high, the reaction is easy to cross-link, which affects the number of effective emulsifier molecules, thereby affecting emulsification effect, making the emulsion less stable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a 250ml four-neck flask equipped with a stirrer, a reflux condenser, a dropping funnel, and a thermometer, preheat the bisphenol A epoxy resin E-20 at 70°C under a nitrogen atmosphere to melt it, and then add non- Ionic hydrophilic segment polyethylene glycol PEG2000, the molar ratio of epoxy resin to polyethylene glycol is, n(E-20): n(PEG2000)=1:1, after fully stirring and mixing, remove heat treatment; Add the boron trifluoride diethyl ether catalyst diluted with propylene glycol methyl ether to the above epoxy resin mixture, the amount of catalyst is 0.5% of the total mass of the reactants, the time for dropping the catalyst is not less than 30min, and then stably stir for 30min; The mixture was reacted stably for 6h at 90°C under the condition of a stirring speed of 600r / min to obtain a modified epoxy resin; the above-mentioned modified epoxy resin was prepared at a temperature of 60°C and a stirring speed of 800r / min. The phase inversion experiment was carried o...

Embodiment 2

[0040] In a 250ml four-neck flask equipped with a stirrer, a reflux condenser, a dropping funnel, and a thermometer, preheat the bisphenol A epoxy resin E-44 at 60°C under a nitrogen atmosphere to melt it, and then add non- Ionic hydrophilic segment polyethylene glycol PEG4000, the molar ratio of epoxy resin to polyethylene glycol is, n(E-44): n(PEG4000)=1:1.2, after fully stirring and mixing, remove heat treatment; In above-mentioned epoxy resin mixture, add potassium persulfate catalyst, catalyst consumption is 1% of reactant gross mass, the time of dripping catalyst is not less than 30min, then stable stirring 30min; Above-mentioned mixture is at 90 DEG C, stirring speed is Stable reaction 6h under 700r / min, obtains modified epoxy resin; With the modified epoxy resin of above-mentioned preparation, temperature is 50 ℃, and the speed of high-speed stirring is carried out phase inversion experiment under the condition of 900r / min, high-speed stirring and Slowly and evenly dro...

Embodiment 3

[0051] In a 250ml four-neck flask equipped with a stirrer, a reflux condenser, a dropping funnel, and a thermometer, preheat the bisphenol A epoxy resin E-20 at 50°C under a nitrogen atmosphere to melt it, and then add non- Ionic hydrophilic segment polyethylene glycol PEG6000, the molar ratio of epoxy resin to polyethylene glycol is, n(E-51): n(PEG6000)=1.1:1, after fully stirring and mixing, remove heat treatment; Add the triphenylphosphine catalyst diluted with propylene glycol methyl ether to the above epoxy resin mixture, the amount of the catalyst is 0.6% of the total mass of the reactants, the time for adding the catalyst dropwise is not less than 30min, and then stably stir for 30min; the above mixture At 90°C, a stirring speed of 500r / min was used to react stably for 6h to obtain a modified epoxy resin; the modified epoxy resin prepared above was at a temperature of 70°C, and the speed of high-speed stirring was 1000r / min. Perform a phase inversion experiment, stir at...

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Abstract

The invention provides a preparation method for non-ionic reactive water-borne epoxy resin emulsion. A preparation process for the non-ionic reactive water-borne epoxy resin emulsion comprises the following steps: simultaneously adding a certain amount of non-ionic hydrophilic segment polyethylene glycol and boron trifluoride diethyl etherate serving as a catalyst into epoxy resin, performing stable reaction for 3-8 hours to obtain non-ionic reactive epoxy resin, then strongly stirring at the temperature of 50 DEG C, and uniformly and dropwise adding distilled water to form water-dispersed epoxy resin emulsion by a phase inversion technology. The preparation method has the benefits that the particle size of the dispersion phase of the prepared non-ionic reactive water-borne epoxy resin emulsion is dozens to hundreds of nanometer; both under high-speed centrifugation and long-time storage, the non-ionic reactive water-borne epoxy resin emulsion is high in stability; furthermore, the emulsion is higher in dilutability, salt resistance, alkali resistance, high temperature resistance, and freeze-thaw stability. The raw materials used in the method are simple, efficient, environment-friendly, safe and non-toxic and can be widely applied to the fields of coatings, composite materials and the like.

Description

technical field [0001] The invention relates to the field of water-based coatings, in particular to a preparation method of a non-ionic reactive water-based epoxy resin emulsion. Background technique [0002] Epoxy resin is widely used in various industries such as composite materials, coatings, and adhesives due to its high strength, excellent heat resistance, chemical corrosion resistance, good bonding performance, and good insulation. Epoxy resin is insoluble in water and only soluble in organic solvents, which are not only expensive, but also volatile and easily pollute the environment. With the increasingly stringent requirements for environmental protection, waterborne epoxy resin systems have become a research hotspot for new environmentally friendly materials. [0003] Waterborne epoxy resin usually refers to a stable dispersion system prepared by dispersing in the form of particles or droplets in a dispersion medium with water as the continuous phase. Water-base...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/20C08G59/62C08J3/03C09D163/00
Inventor 李鹏李晋杨小平
Owner BEIJING UNIV OF CHEM TECH
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