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Preparation method of composite shell coated liquid isocyanate self-repairing microcapsule

A technology for self-repairing microcapsules and isocyanates, applied in microcapsule preparations, microsphere preparation and other directions, can solve the problems of fragility, poor microcapsule strength, high active core liquid outflow, etc., and achieves good particle size controllability and cost. Inexpensive, smooth-looking results

Inactive Publication Date: 2017-07-14
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This not only leads to the increase of production cost, but also makes it difficult to separate and wash the subsequent microcapsules.
In addition, the microcapsules of the single-layer shell have poor strength and are easily broken during the mixing process with the resin substrate, resulting in the outflow and inactivation of the highly active core fluid.

Method used

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  • Preparation method of composite shell coated liquid isocyanate self-repairing microcapsule
  • Preparation method of composite shell coated liquid isocyanate self-repairing microcapsule
  • Preparation method of composite shell coated liquid isocyanate self-repairing microcapsule

Examples

Experimental program
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Effect test

Embodiment 1

[0028] At room temperature, add polyvinyl alcohol with a degree of alcoholysis of 95% and a molecular weight of 70000-80000 g / mol into deionized water and stir for 30 minutes, then heat to 80 °C and stir for 3 hours. Finally cooling to obtain 5wt% polyvinyl alcohol aqueous solution. Take 60ml of the prepared polyvinyl alcohol aqueous solution and stir at 1600rpm, then mix 12g of isophorone diisocyanate and 4 g of polyphenyl polymethylene polyisocyanate into a homogeneous oil phase and slowly pour it into the polyvinyl alcohol aqueous solution for emulsification for 4min Forms a stable oil-in-water emulsion. 0.025 g, 0.050 g, 0.100 g, 0.200 g, 0.400 g, and 0.800 g of diethylenetriamine were respectively dissolved in 10 ml of deionized water to prepare 6 equal parts of diethylenetriamine solutions. Six parts of diethylenetriamine solutions were added dropwise from low concentration to high concentration into the stable oil-in-water emulsion, and each part of diethylenetriamine ...

Embodiment 2

[0030] At room temperature, add polyvinyl alcohol with a degree of alcoholysis of 98% and a molecular weight of 170,000-180,000 g / mol into deionized water and stir for 30 minutes, then heat to 95°C and stir for 1.5 hours. Finally cooled to obtain 2wt% polyvinyl alcohol aqueous solution. Get 60ml of the prepared polyvinyl alcohol aqueous solution and stir at 600rpm, then mix 12 g of isophorone diisocyanate and 4 g of polyphenyl polymethylene polyisocyanate into a homogeneous oil phase and slowly pour it into the polyvinyl alcohol aqueous solution for emulsification 4 min to form a stable oil-in-water emulsion. 0.030 g, 0.060 g, 0.120 g, 0.240 g, 0.480 g, and 0.960 g of diethylenetriamine were respectively dissolved in 10 ml of deionized water to prepare 6 equal parts of diethylenetriamine solutions. After emulsification, 6 parts of diethylenetriamine solution were added dropwise to the emulsion successively, and each part of diethylenetriamine solution was added at an interval...

Embodiment 3

[0032]At room temperature, add polyvinyl alcohol with 85% alcoholysis degree and molecular weight of 20000-30000g / mol into deionized water and stir for 30min, then heat to 70°C and stir for 5h. Finally cooled to obtain 12wt% polyvinyl alcohol aqueous solution. Get 60 ml of prepared polyvinyl alcohol aqueous solution and stir at 400rpm, then 12g isophorone diisocyanate and 4g polyphenyl polymethylene polyisocyanate are mixed into a homogeneous oil phase and slowly poured into the polyvinyl alcohol aqueous solution for emulsification 4 min to form a stable oil-in-water emulsion. Dissolve 0.015g, 0.030g, 0.060g, 0.120g, 0.240g, and 0.480g of diethylenetriamine in 10 ml of deionized water respectively to prepare 6 equal parts of diethylenetriamine solutions. After emulsification, 6 parts of diethylenetriamine solution were added dropwise to the emulsion successively, and each part of diethylenetriamine solution was added at an interval of 10 min. After the dropwise addition was ...

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Abstract

A preparation method of a composite shell coated liquid isocyanate self-repairing microcapsule comprises the following steps: adding a polyisocyanate shell material and a low-activity liquid isocyanate core material into a polyvinyl alcohol-water solution to form a core material and shell material mixed oil phase, emulsifying the oil phase to form a stable oil-in-water emulsion, dividing an amine cross-linking agent into six parts, respectively adding the six parts of the amine cross-linking agent into deionized water to prepare six amine solutions with the same volume, sequentially dropwise adding the six solutions into the emulsion from low concentration to high concentration, carrying out a heating reaction, cooling the obtained emulsion to room temperature, washing the cooled emulsion, carrying out decantation to obtain a microcapsule, and drying the separated microcapsule at room temperature to obtain the self-repairing microcapsule. The preparation method has the advantages of simple synthesis steps, low cost, high cladding rate, controllable dimension and high composite shell strength.

Description

[0001] Field [0002] The invention belongs to the field of preparation of self-repairing microcapsules, in particular to a method for preparing self-repairing microcapsules in which a compound shell is coated with liquid isocyanate. Background technique [0003] Self-healing microcapsule technology is a method of encapsulating self-healing agents in tiny, airtight capsules. Self-healing microcapsules are widely used in the repair of microcrack defects in coatings and structural polymers. Among all self-healing microcapsules, since isocyanate can easily react with moisture in the surrounding environment, microcapsules coated with liquid isocyanate become a self-healing system that can initiate a self-healing reaction quickly and efficiently without a catalyst . [0004] In the prior art CN201210218226.X, when coating isocyanate, a large amount of toxic solvents such as capsule core diluent and co-solvent are used. This will lead to a significant reduction in the coverage ra...

Claims

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Application Information

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IPC IPC(8): B01J13/02C08G18/32
CPCB01J13/02C08G18/3228
Inventor 王军威龙李其峰贺正龙亢茂青
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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