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Method for preparing enhanced epoxy resin/curing agent double-wall microcapsule

A technology of epoxy resin and epoxy resin emulsion, which is applied in the fields of organic composite materials and national defense, can solve the problems that the mechanical properties are difficult to meet the use requirements, the utilization rate of the capsule wall is not high, and the microcapsules take a long time. Excellent performance, improved repair effect, rich variety of effects

Inactive Publication Date: 2011-10-05
UNIV OF SCI & TECH BEIJING +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of enhanced epoxy resin / curing agent double-walled microcapsules, which solves the problem of long time-consuming preparation of microcapsules with urea-formaldehyde resin, complicated process, low utilization rate of capsule wall, and single-ring repair agent. Oxygen resin, the mechanical properties after repair are difficult to meet the use requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Step 1, prepare epoxy resin emulsion

[0017] Mix Tween 20 and Span 60 at a mass ratio of 3:7 to form a compound emulsifier; mix 9g of epoxy resin with 1g of compound emulsifier, heat and stir in a water bath at 50°C, and the stirring speed is 3000rpm, slowly 30 ml of deionized water was added dropwise to the mixture, and an epoxy resin emulsion was formed after a certain period of time.

[0018] Step 2, preparation of capsule wall prepolymer

[0019] Mix the three raw materials of melamine, formaldehyde and deionized water according to the mass ratio of 7:11:12, stir in a water bath at 80°C at a constant temperature, and the stirring speed is generally 1000rpm. When it becomes a colorless and transparent solution, use 1mol / L NaOH solution to adjust the pH between 8-9, and obtain a colorless and transparent capsule wall prepolymer in about 50 minutes.

[0020] Step 3, the preparation of single-wall microcapsules

[0021] Mix 40g of epoxy resin emulsion and 20g of pre...

Embodiment 2

[0029] Step 1, prepare epoxy resin emulsion

[0030] Mix Tween 20 and Span 60 uniformly at a mass ratio of 3:7 to form a compound emulsifier; mix 8.8g of epoxy resin with 1.2g of compound emulsifier, heat and stir in a water bath at 60°C, and the stirring speed is 2000rpm , slowly add 30ml of deionized water dropwise to the mixture, and form an epoxy resin emulsion after 30min.

[0031] Step 2, preparation of capsule wall prepolymer

[0032] Mix the three raw materials of melamine, formaldehyde and deionized water according to the mass ratio of 7:11:12, stir in a water bath at 80°C at a constant temperature, and the stirring speed is generally 1000rpm. When it becomes a colorless and transparent solution, use 1mol / L NaOH solution to adjust the pH between 8-9, and obtain a colorless and transparent capsule wall prepolymer in about 50 minutes.

[0033] Step 3, the preparation of single-wall microcapsules

[0034] Mix 40g of epoxy resin-carbon nanotube emulsion and 20g of prep...

Embodiment 3

[0042] Step 1, acidification of carbon nanotubes

[0043] Pure sulfuric acid and pure nitric acid were prepared into 240ml mixed strong acid at a volume ratio of 3:1, and 1g of carbon nanotubes were added to the mixed strong acid, dispersed in an ultrasonic (150W) water bath (65°C) for 6 hours, and left to stand for 5 hours. Extract the acidified carbon nanotubes, add deionized water to centrifuge and precipitate repeatedly, remove the acid remaining in the solution until the solution is basically neutral, and dry to remove water.

[0044] Step 2, preparation of epoxy resin-carbon nanotube emulsion

[0045] Mix Tween 20 and Span 60 at a mass ratio of 3:7 to form a compound emulsifier; mix 9g of epoxy resin with 1g of compound emulsifier, heat and stir in a water bath at 50°C, and the stirring speed is 3000rpm, slowly Add 30ml of deionized water dropwise to the mixture to form an epoxy resin emulsion after a certain period of time; add 0.001g of carbon nanotubes to the epoxy r...

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Abstract

The invention provides a method for preparing a double-wall self-repairing microcapsule by compounding an epoxy resin or a mixture of epoxy resins and carbon nanotubes as an inner capsule core repairing agent and using a curing agent as an outer capsule core. The invention belongs to the field of organic compound materials. The method comprises the following steps: intensely stirring and ultrasonically dispersing the epoxy resin or the mixture of epoxy resins and carbon nanotubes under the action of an emulsifier, so as to form an epoxy resin emulsion or an epoxy resin carbon nanotube emulsion; after preparing a melamine formaldehyde pre-polymer solution, preparing a single-wall microcapsule by using the melamine formaldehyde pre-polymer solution together with the epoxy resin emulsion or the epoxy resin carbon nanotube emulsion under an acid condition; after preparing a curing agent emulsion, stirring the curing agent emulsion and the single-wall microcapsule under an acid environment, thereby leading the curing agent grains to be uniformly attached on the periphery of the single-wall microcapsule; and then generating a second capsule wall layer by adding the melamine formaldehydepre-polymer solution. The prepared microcapsule contains the enhancing repairing agent and the curing agent, which can further enhance the repairing effect of the microcapsule and increase the mechanical property.

Description

technical field [0001] The invention belongs to the field of organic composite materials, and in particular relates to a preparation method of enhanced double-wall self-repairing microcapsules, which are applied in the fields of national defense such as aviation and aerospace. Background technique [0002] During the use of composite materials, affected by environmental factors such as heat and force, microcracks will inevitably occur, which will degrade the performance of the material. Repairing cracks can effectively prolong the service life of materials. The microcapsules coated with repairing agent are embedded in the matrix material, and when cracks are formed, the repairing agent can be broken in time and flow out for repairing. It can be seen that the restoration agent has a great influence on the restoration effect. Currently, DCPD is the most widely used restorative agent. Low molecular weight polyamide, epoxy resin, silicone resin, styrene monomer and high molecu...

Claims

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Application Information

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IPC IPC(8): B01J13/14B01J13/20C08L63/00C08K7/00C08K3/04C08G12/32
Inventor 郑裕东田茹周章铭付小丽梁馨凌英谭珏吴健马衍轩
Owner UNIV OF SCI & TECH BEIJING
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