Composite ball containing self-assembly microcapsule and preparation method thereof

A technology of microcapsules and self-assembly, which is applied in the direction of microsphere preparation and microcapsule preparation, etc. It can solve the problems of complex preparation process, self-polymer impurities, low capsule purity, etc., and achieve high encapsulation efficiency, little influence on pH value, well-formed effect

Active Publication Date: 2016-09-28
天津优米优科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When using this method to prepare capsules, due to the influence of pH value, some emulsifiers will undergo polycondensation, crosslinking and solidification under the action of heat and catalyst acid, and the prepolymer will also self-assemble into small balls, which will affect the encapsulation efficiency. It brings great difficulties to the suction filtration and washing of the capsule suspension, which seriously limits its industrialization to a certain extent and affects its product quality.
[0004] In patent CN1513938A (a microcapsule-coated phase-change material and its preparation method), Wang Lixin, Ren Li, etc., use the phase-change material as the capsule core, and divide the aqueous solution of melamine-formaldehyde prepolymer into two equal parts. Add it dropwise to the emulsion with pH=4~5 for a few times, and raise the temperature to obtain microcapsules with double-layer capsule walls. If too much acid is added to the emulsion or too fast, the emulsifier will be solidified and cross-linked; and the water-soluble Melamine-formaldehyde resin will dissolve in the water phase, resulting in low capsule purity, self-polymer impurities, and complicated preparation process

Method used

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  • Composite ball containing self-assembly microcapsule and preparation method thereof
  • Composite ball containing self-assembly microcapsule and preparation method thereof
  • Composite ball containing self-assembly microcapsule and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Stir 10g of n-dodecyl alcohol and 10g of n-butyl etherified amino resin evenly to obtain an oil phase solution; add this oil phase solution to 150g of SMA aqueous solution with a concentration of 2wt%, and then emulsify at a high speed at 5000rpm for 5min to obtain Stable oil-in-water emulsion; 75g of 5wt% sodium alginate is added as a matrix and stirred to increase the dispersion of the emulsion, using an electrospinning nozzle (coaxial composite nozzle (inner diameter 0.6mm outer diameter 1.5mm) ) is sprayed into a low-concentration calcium chloride solution, the Ca in the calcium chloride solution 2+ It will complex with carboxylate ions in sodium alginate to form a gel of calcium alginate; in this process, use 20wt% citric acid solution to adjust the pH value to 1-2; mix the above-mentioned calcium chloride with the spherical product Transfer to a three-necked flask, heat up to 90°C while stirring at a speed of 400rpm, adjust the pH value to about 7 with 20wt% sodiu...

Embodiment 2

[0031] Stir 1kg of coconut essence and 500g of methyl etherified amino resin evenly to obtain an oil phase solution; add this oil phase solution to 2kg of emulsifier OP-10 aqueous solution with a concentration of 5wt%, and then emulsify at a high speed of 5,000rpm for 20 minutes , to produce a stable oil-in-water emulsion. Add 1kg of 5% polymaleic anhydride as a matrix and fully stir it, and spray it into the manganese chloride solution at low concentration under different jets, airflows, concentrations, and thrusts by using an electrospinning nozzle; the composite ball Pour the mixed liquid with polymaleic anhydride into the three-port burnt product, and heat up to 90°C while stirring at a speed of 400rpm. During this process, use 20% citric acid solution to adjust the pH value to about 2. After reacting for 3 hours, filter and wash , drying to get amino resin composite balls. Observing the sample with a scanning electron microscope, the microcapsule particle size distributi...

Embodiment 3

[0034]Mix 2kg of mosquito repellent incense oil, 1kg of n-octyl etherified amino resin and 100g of acetone to obtain an oil phase solution; add this oil phase solution to the emulsifier aqueous solution prepared by dissolving 1kg of polyvinylpyrrolidone in 10kg of water , high-speed emulsification at 2000rpm for 30 minutes to obtain an oil-in-water emulsion with an average particle size of 20 μm; 10kg of 5% polyvinyl alcohol was added as a matrix and fully stirred. Spray it into a calcium nitrate solution at a low concentration under low concentration, concentration, and thrust, add citric acid dropwise to adjust the pH value to 3, then raise the temperature to 85°C, and react for 2 hours to obtain an amino resin composite ball of mosquito repellent fragrance. The morphology and structure of the samples were observed with a scanning electron microscope, and most of the particle sizes of the microcapsules inside the spherical capsules were distributed in the range of 5-100 μm. ...

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Abstract

The invention provides an in-situ preparation method for capsules with amino resin as wall forming monomer. The method comprises the following steps that firstly, the alkanol etherified amino resin with different carbon chain lengths and an oil soluble substance are mixed and stirred fully to be dissolved, and a uniform oil phase is obtained; secondly, the prepared uniform oil phase is added into a water solution containing an emulsifier, the mixture is stirred fully, sheared and emulsified, and emulsion droplets with the particle size ranging from 1 micron to 100 microns are obtained; thirdly, a water-soluble polymer solution and the emulsion are mixed and jetted, and a composite ball containing uniform dispersion emulsion is prepared; fourthly, the mixed solution of the composite ball and a salt solution is slowly heated, the pH value is adjusted, the emulsion droplets of the etherified amino resin inside the composite ball are subjected to a polymerization curing reaction, and a capsule wall of a microcapsule for wrapping the oil phase is formed; fifthly, after filtering and washing, the composite ball containing the self-assembly microcapsule is obtained, and the particle size of composite balls is uniform. The synthetic process is simple, energy consumption is low, the requirements for equipment is low, reaction conditions and the particle size are easy to control, and the method has a prospect of mass production. The simple encapsulation method has very wide application prospects in the fields of pesticide, cosmetics and intelligent heat accumulation thermoregulation products.

Description

technical field [0001] The invention relates to a method for preparing a composite ball containing self-assembled microcapsules, in particular to a method for preparing a composite ball with an alkanol etherified amino resin as the wall of the microcapsule. Background technique [0002] Capsule technology is a technology in which film-forming materials wrap solids, liquids or gases to form tiny particles, which can protect the capsule core, control release, and achieve permanent solidification, which greatly facilitates the application range of the capsule core material. According to The particle size can be divided into: nanocapsules with a particle size of less than 1 μm, microcapsules with a particle size of 1-1000 μm, and macrocapsules with a particle size greater than 1 mm. Their application areas cover medicine, food, coatings, pesticides, adhesives, inks, and textile dyeing and finishing. [0003] At present, amino resin capsules often use amino resin prepolymers. By...

Claims

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Application Information

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IPC IPC(8): B01J13/02
CPCB01J13/02
Inventor 李伟黄睿霍晓楠宗记文张泓
Owner 天津优米优科技有限公司
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