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A kind of preparation method of epoxy microcapsule with phenolic resin as wall material

A technology of phenolic resin and microcapsules, which is applied in the field of preparation of epoxy microcapsules, can solve problems such as the difficulty of epoxy microcapsules, and achieve the effect of good shape, low price and high coating rate

Inactive Publication Date: 2015-10-21
SHENZHEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first-stage Resole resin is very sensitive to the pH value during acid adjustment and curing, and the unsuitable pH value often cannot form the phenolic capsule wall; when heating promotes its curing reaction, a large number of methylol groups in the first-stage Resole resin are easy to combine with epoxy The epoxy end group of the resin undergoes an addition reaction to cure the epoxy. Therefore, it is difficult to prepare epoxy microcapsules with phenolic resin as the wall material using the first-stage Resole resin as the precursor.

Method used

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  • A kind of preparation method of epoxy microcapsule with phenolic resin as wall material
  • A kind of preparation method of epoxy microcapsule with phenolic resin as wall material

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preparation example Construction

[0014] The technical solution adopted by the present invention to solve the above-mentioned technical problems is to provide a kind of preparation method of epoxy microcapsules with phenolic resin as wall material, comprising the following steps:

[0015] S1: Mix epoxy resin, emulsifier, and water, and stir to make emulsion;

[0016] S2: adding phenol, aldehyde and pH regulator I to the emulsion, adjusting the pH to 7-9, and stirring;

[0017] S3: Add polyhydric phenol, curing accelerator, and pH adjuster II to the solution obtained in step S2, adjust the pH to 2-4, react for 2-3 hours, cool, stand, filter, and dry to obtain the phenolic resin Epoxy microcapsules for wall materials.

[0018] Wherein, the emulsifier in step S1 is a polyhydroxy compound, at least one selected from polyvinyl alcohol, polypropylene alcohol, polysaccharides, and alkyl glycosides. Further, the mass ratio of epoxy resin, emulsifier, and water in step S1 is 1:0.05-0.2:10-30; in order to fully emulsi...

Embodiment 1

[0023] In a 250ml three-neck flask, add 10ml of 5wt% polyvinyl alcohol (PVA-1788) aqueous solution, 100ml of deionized water, stir well, then slowly add 2.1g (0.022mol) of phenol, and after it dissolves, use ammonia water (NH 3 ·H 2 O) Adjust the pH value of the solution to 7, then slowly add 6.5g of epoxy resin, stir and emulsify at high speed for 60min, and the rotation speed is greater than 1000rpm, to obtain a uniform and stable oil-in-water epoxy emulsion.

[0024] Adjust the rotation speed to 400rpm, and slowly add 3.35g (0.041mol) formaldehyde (CH 2 O) aqueous solution, and at the same time slowly raise the temperature to 65°C, and keep it warm for 3 hours to form a water-soluble Resole phenolic resin. Then adjust the pH value to 4 with 3.7% hydrochloric acid solution, add 0.5g resorcinol, react for 30min, then add 0.5g NH 4 Cl, continue to react for 2.5h to form epoxy microcapsules with phenolic resin as the wall material.

[0025] After the reaction solution is coo...

Embodiment 2

[0027] The process of embodiment 2 is basically the same as that of embodiment 1, except that the pH is adjusted to 8 at the stage of resole phenolic resin formation, and the pH is adjusted to 3 at the stage of crosslinking and curing. Specific steps are as follows:

[0028] In a 250ml three-neck flask, add 10ml of 5wt% polyvinyl alcohol (PVA) aqueous solution, 100ml of deionized water, stir well, then slowly add 2.1g (0.022mol) of phenol, and after it dissolves, use ammonia water (NH 3 ·H 2 O) Adjust the pH value of the solution to 8, then slowly add 6.5g of epoxy resin, stir and emulsify at high speed for 60min, and the rotation speed is greater than 1000rpm to obtain a uniform and stable oil-in-water epoxy emulsion.

[0029] Adjust the rotation speed to 400rpm, and slowly add 3.35g (0.041mol) formaldehyde (CH 2 O) aqueous solution, and at the same time slowly raise the temperature to 65°C, and keep it warm for 3 hours to form a water-soluble Resole phenolic resin. Then a...

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Abstract

A method for preparing an epoxy microcapsule by using phenolic resin as a wall material comprises the following steps: mixing epoxy resin, an emulsifier and water, and stirring to prepare an emulsion; adding phenol, aldehyde and a pH regulator I into the emulsion, adjusting a pH value to 7 to 9, and stirring; and then, adding polyphenol, a curing accelerator and a pH regulator II to the obtained solution, adjusting the pH value to 2 to 4, reacting for 2 to 3 hours, cooling, standing, filtering and drying to obtain an epoxy microcapsule using the phenolic resin as a wall material. By means of the preparation method, a curing reaction between the wall material and a core material is avoided, and the epoxy microcapsule using the phenolic resin as the wall material, which have a good form and a high coating rate, is successfully synthesized.

Description

technical field [0001] The invention relates to the field of self-repairing materials, in particular to the field of self-repairing concrete, in particular to a method for preparing epoxy microcapsules using phenolic resin as a wall material. Background technique [0002] Self-healing material is a kind of intelligent material, which can repair its own defects such as voids and cracks. Technically, one of the main methods to realize the self-healing function of materials is to pre-embed the repairing agent in the matrix material. When the matrix material has cracks or cavities due to some physical or chemical factors, the repairing agent will be released automatically. Self-fix bugs. There are a large number of microcracks in concrete members, and these microcracks are difficult to be detected and repaired manually. For example, in a humid atmospheric environment, especially in a coastal environment, their existence will accelerate the corrosion of steel bars, reduce the d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/14
CPCB01J13/14
Inventor 朱光明周玉明汤皎宁董必钦王险峰韩宁旭邢峰
Owner SHENZHEN UNIV
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