CN110128708A - A kind of suction wave-self-repairing microcapsule and preparation method thereof - Google Patents
A kind of suction wave-self-repairing microcapsule and preparation method thereof Download PDFInfo
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- CN110128708A CN110128708A CN201910456050.3A CN201910456050A CN110128708A CN 110128708 A CN110128708 A CN 110128708A CN 201910456050 A CN201910456050 A CN 201910456050A CN 110128708 A CN110128708 A CN 110128708A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/26—Cellulose ethers
- C08L1/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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Abstract
The invention discloses a kind of preparation methods of microcapsules for having both suction wave energy and self-repair function.The problem of caused absorbing material absorbing property declines when the present invention can be used for weakening incorporation self-repairing microcapsule.The present invention uses ultrasonic disperse-solvent evaporated method, and using ethyl cellulose as wall material, wave absorbing agent is functional modifier, and epoxy resin is that wave-self-repairing microcapsule is inhaled in core material preparation.Wave-self-repairing microcapsule absorbing property is excellent, particle characteristics are good, size distribution is suitable for suction of the invention, and has stable chemical structure, and material can be assigned by being mixed in common material preferably inhales wave energy and self-repair function；Absorbing material self-repair function can be assigned while not significantly reducing Absorbing Materials by being mixed in absorbing material.
Description
Technical field
The invention belongs to microcapsules technology fields, and in particular to a kind of suction wave-self-repairing microcapsule and preparation method thereof.
Background technique
Self-repairing microcapsule is that the chemical substances renovation agent such as epoxy resin is filled into the micro- glue formed in high molecular material
Capsule.Basis material is mixed, in matrix crack extension, the connection between microcapsules and matrix can be repaired with microcapsules rupture
Multiple agent is flowed out and is penetrated into around crack with crack, is reacted with the curing agent of preparatory incorporation matrix, is repaired to reach crack
Multiple effect.
Absorbing material be wave absorbing agent and basis material are carried out it is compound after obtained material, wherein wave absorbing agent is to electromagnetic wave
Decaying plays a major role, but the design of the structure of wave absorbing agent and basis material also has larger impact to the impedance matching property of material.
Electromagnetic wave absorbent material is for numerous areas such as defence and military, electronic communication, industry, scientific research and medical treatment, to inhibit radar special
Influence of the worsening electromagnetic pollution of reference number, abatement to equipment and people.
Currently, the preparation process of self-repairing microcapsule is increasingly mature, it is already possible to apply to the matrixes such as cement base, resin base
In, and after incorporation self-repairing microcapsule, basis material has good repairing effect.Self-repairing microcapsule itself is generally without electricity
Electro-magnetic wave absorption agent is too weak to electromagnetic wave attenuation ability, and incorporation self-repairing microcapsule (does not have suction wave energy or absorbing property is poor)
Absorbing material matrix, can there are problems that electromagnetic wave attenuation reduced capability.
In conclusion researching and developing a kind of intelligence and function for having both the microcapsules for inhaling wave energy and self-repair function for material
Energyization development has great importance.
Summary of the invention
For the technology for preparing self-repairing microcapsule using ultrasonic disperse-solvent evaporated method at present, the purpose of the present invention exists
In providing a kind of suction wave-self-repairing microcapsule for absorbing material matrix, preparation method is also disclosed.
The present invention is realized by following proposal:
A kind of suction wave-self-repairing microcapsule, using ethyl cellulose as wall material, wave absorbing agent is functional modifier, epoxy resin
For core material, in parts by mass, including 6~29 parts of ethyl cellulose, 4~30 parts of wave absorbing agent, 5~74 parts of epoxy resin, emulsifier 3
~35 parts, 87~236 parts of organic solvent, 542~749 parts of deionized water.
The wave absorbing agent is one or more of carbonyl iron, ferroso-ferric oxide, graphene, graphene oxide.
The epoxy resin is in bisphenol A type epoxy resin, bisphenol-s epoxy resin or bisphenol f type epoxy resin
It is one or more of.
The organic solvent is one or more of methylene chloride, benzene, toluene, ethyl alcohol, chloroform and methanol.
The emulsifier is one or more of gelatin, neopelex, lauryl sodium sulfate.It is preferred that
, the emulsifier is the composition of gelatin and neopelex/or lauryl sodium sulfate.
A kind of suction wave-self-repairing microcapsule preparation method, comprising the following steps:
(1) prepared by water phase: 3~35 parts of emulsifiers are dissolved in 542~749 parts of deionized waters as water phase；
(2) oil is mutually prepared: by 6~29 parts of ethyl celluloses, 4~30 parts of wave absorbing agents, 5~74 parts of epoxy resin and 87~
236 parts of organic solvent mixing, ultrasonic disperse dissolution；
(3) it emulsifies: oil being mutually poured slowly into water phase, 2~6h is stirred with certain temperature and certain speed, in shear action
It is lower to form spherical emulsion oil-in-water；The temperature range is 25~35 DEG C, and the range of speeds is in 100r/min~1500r/
min；
(4) solidify: temperature being risen to 40 DEG C~45 DEG C and continues to stir 1h~3h, so that organic solvent sufficiently volatilizees；
(5) filtration washing: suspension obtained after solidification is cooled to room temperature, and removal swims in the waste residue and mistake on upper layer
Filter, obtained sediment is washed with distilled water, and air-dries obtain inhaling wave-self-repairing microcapsule at room temperature.
Preferably, in step 1, the emulsifier includes gelatin, and the emulsifier is dissolved in deionized water, and heats
To 70 DEG C, stirring to dissolution, and it is cooled to 25 DEG C.
The invention has the benefit that
For the present invention using ethyl cellulose as wall material, wave absorbing agent is functional modifier, and epoxy resin is core material, using ultrasound point
Scattered-solvent evaporated method preparation can be used for assigning absorbing material self-repair function or assign common material self-repair function and inhale wave function
Suction wave-self-repairing microcapsule of energy.Suction wave-self-repairing microcapsule absorbing property provided by the invention is excellent, particle characteristics are good,
Size distribution is suitable for (30~700 μm), and has stable chemical structure, is mixed in basis material, basis material is to electricity
The reflection loss of magnetic wave is obviously reduced and (significantly increases to the absorption of electromagnetic wave), repair rate is obviously improved, and matrix is endowed well
Self-repair function and inhale wave energy.
Detailed description of the invention
Fig. 1 is the microcapsule preparation process flow diagram of the embodiment of the present invention；
The microcapsules and common microcapsule that Fig. 2 is the embodiment of the present invention 2 are to the reflection loss curve of electromagnetic wave；
Fig. 3 is the grading curve figure of the embodiment of the present invention 2；
Fig. 4 is the surface of microcapsule topography scan electron microscope of the embodiment of the present invention 2；
Fig. 5 is the microcapsules formula microscope figure of the embodiment of the present invention 2.
Specific embodiment
For a better understanding of the invention, below with reference to embodiment and attached drawing, the present invention is further illustrated, but this hair
Bright claimed range is not limited to the scope of the embodiments.
The process flow chart of the embodiment of the present invention 1~5 is referring to attached drawing 1.
Embodiment 1:
0.5 part of 2.5 parts of gelatin, lauryl sodium sulfate are weighed, and is stirred for temperature is dissolved in being 545 parts of 70 DEG C
It is used as water phase in water, and is cooled to 25 DEG C；6 parts of ethyl celluloses and 5 parts of epoxy resin E-44s are dissolved in 90 parts simultaneously
In methylene chloride, 5 parts of carbonyl iron dusts are added after it is completely dissolved, and by mixed liquor ultrasound and stir 10min, the mixing of formation
Liquid is as oily phase；Oil is mutually poured slowly into water phase again and is stirred with 100r/min, spherical emulsion oil-in-water is formed, at 25 DEG C
4h is stirred, microcapsule wall material has gradually lost deformability at this time, forms microcapsules blank.Temperature is risen to 43 DEG C to continue to stir
1h is mixed, so that solvent sufficiently volatilizees, solidifies microcapsules；Finally suspension obtained after solidification is cooled to room temperature, and is gone
Except the waste residue and filtering for swimming in upper layer, obtained sediment is washed with distilled water, and air-dries obtain inhaling wave-certainly at room temperature
Repair microcapsules.Gained microcapsules are spherical shape, and Microcapsules Size is 30~350 μm.
Embodiment 2:
20 parts of gelatin are weighed, and are stirred for temperature is dissolved in being in 70 DEG C of 600 parts of water as water phase, and its is cold
But to 25 DEG C；5 parts of ethyl celluloses and 5 parts of epoxy resin E-51 are dissolved in 90 parts of methylene chloride simultaneously, it is completely molten to it
5 parts of carbonyl iron dusts are added after solution, and by mixed liquor ultrasound and stir 10min, the mixed liquor of formation is as oily phase；It again will be oily mutually slow
Slowly it pours into water phase and is stirred with 200r/min, form spherical emulsion oil-in-water, 4h is stirred at 30 DEG C, at this time microcapsule wall material
Deformability has been gradually lost, microcapsules blank is formd.Temperature is risen to 43 DEG C to continue to stir 1h, so that solvent is sufficiently waved
Hair, solidifies microcapsules；Finally suspension obtained after solidification is cooled to room temperature, and removal swims in the waste residue on upper layer simultaneously
Filtering, obtained sediment is washed with distilled water, and air-dries obtain inhaling wave-self-repairing microcapsule at room temperature.The micro- glue of gained
Capsule is spherical (see Fig. 4 and Fig. 5), and Microcapsules Size is 30~700 μm (see Fig. 3).
Reflection loss of the suction wave-self-repairing microcapsule and common microcapsule of testing example 2 to electromagnetic wave.Test sample
It is prepared for microcapsules and paraffin 9:1 in mass ratio, wherein paraffin is the adhesive of fixed microcapsules.Mix common microcapsule preparation
Thickness of sample is 2mm, mix embodiment 2 suction wave-self-repairing microcapsule thickness of sample be respectively 2mm, 4mm, 6mm, 8mm and
10mm.Test result is shown in Fig. 2.
Embodiment 3:
30 parts of gelatin, 0.5 part of lauryl sodium sulfate are weighed, and is stirred for temperature is dissolved in being 700 parts of 70 DEG C
It is used as water phase in water, and is cooled to 25 DEG C；10 parts of ethyl celluloses and 10 parts of epoxy resin E-55 are dissolved in 180 simultaneously
In part chloroform, 10 parts of carbonyl iron dusts, 0.05 part of graphene are added after it is completely dissolved, and by mixed liquor ultrasound and stir
10min, the mixed liquor of formation is as oily phase；Oil is mutually poured slowly into water phase again and is stirred with 600r/min, spherical water packet is formed
Water emulsion stirs 4h at 35 DEG C, and microcapsule wall material has gradually lost deformability at this time, forms microcapsules blank.It will
Temperature, which rises to 43 DEG C and continues to stir 1h, so that solvent sufficiently volatilizees solidifies microcapsules；It is obtained suspended after finally solidifying
Liquid is cooled to room temperature, and removes waste residue and the filtering for swimming in upper layer, obtained sediment is washed with distilled water, and in room temperature
Lower air-dry obtains inhaling wave-self-repairing microcapsule.Gained microcapsules are spherical shape, and Microcapsules Size is 30~630 μm.
Embodiment 4:
Weigh 30 parts of gelatin, 0.3 part of neopelex, and be stirred for be dissolved in temperature be 70 DEG C 600
It is used as water phase in part water, and is cooled to 25 DEG C；30 parts of ethyl celluloses and 30 parts of epoxy resin REF-170 are dissolved simultaneously
In 200 parts of organic solvents (100 parts of methylene chloride, 100 parts of dehydrated alcohol), 40 parts of carbonyl iron dusts are added after it is completely dissolved
With 0.5 part of graphene oxide, and by mixed liquor ultrasound and 10min is stirred, the mixed liquor of formation is as oily phase；It is again that oil is mutually slow
It pours into water phase and is stirred with 1500r/min, form spherical emulsion oil-in-water, 4h is stirred at 30 DEG C, at this time microcapsule wall material
Deformability has been gradually lost, microcapsules blank is formd.Temperature is risen to 43 DEG C to continue to stir 3h, so that solvent is sufficiently waved
Hair, solidifies microcapsules；Finally suspension obtained after solidification is cooled to room temperature, and removal swims in the waste residue on upper layer simultaneously
Filtering, obtained sediment is washed with distilled water, and air-dries obtain inhaling wave-self-repairing microcapsule at room temperature.The micro- glue of gained
Capsule is spherical shape, and Microcapsules Size is 30~700 μm.
Embodiment 5:
35 parts of gelatin are weighed, and are stirred for temperature is dissolved in being in 70 DEG C of 695 parts of water as water phase, and its is cold
But to 25 DEG C；20 parts of ethyl celluloses and 20 parts of epoxy resin E-51 are dissolved in 200 parts of methylene chloride simultaneously, completely to it
20 parts of carbonyl iron dusts and 10 parts of ferroso-ferric oxide powder are added after dissolution, and by mixed liquor ultrasound and stir 10min, the mixing of formation
Liquid is as oily phase；Oil is mutually poured slowly into water phase again and is stirred with 1500r/min, spherical emulsion oil-in-water is formed, at 30 DEG C
Lower stirring 4h, microcapsule wall material has gradually lost deformability at this time, forms microcapsules blank.Temperature is risen into 45 DEG C of continuation
Stirring 3h solidifies microcapsules so that solvent sufficiently volatilizees；Finally suspension obtained after solidification is cooled to room temperature, and
Removal swims in waste residue and the filtering on upper layer, and obtained sediment is washed with distilled water, and air-dries obtain inhaling wave-at room temperature
Self-repairing microcapsule.Gained microcapsules are spherical shape, and Microcapsules Size is 30~700 μm.
Claims (7)
1. a kind of suction wave-self-repairing microcapsule, it is characterised in that: using ethyl cellulose as wall material, wave absorbing agent is functional modifier,
Epoxy resin is core material, in parts by mass, including 6~29 parts of ethyl cellulose, 4~30 parts of wave absorbing agent, epoxy resin 5~74
Part, 3~35 parts of emulsifier, 87~236 parts of organic solvent, 542~749 parts of deionized water.
2. suction wave-self-repairing microcapsule according to claim 1, it is characterised in that: the emulsifier is gelatin, 12
One or more of sodium alkyl benzene sulfonate, lauryl sodium sulfate.
3. suction wave-self-repairing microcapsule according to claim 1, it is characterised in that: the wave absorbing agent is carbonyl iron, four
One or more of Fe 3 O, graphene, graphene oxide.
4. suction wave-self-repairing microcapsule according to claim 1, it is characterised in that: the epoxy resin is bisphenol A-type
One or more of epoxy resin, bisphenol-s epoxy resin or bisphenol f type epoxy resin.
5. suction wave-self-repairing microcapsule according to claim 1, it is characterised in that: the organic solvent is dichloromethane
One or more of alkane, benzene, toluene, ethyl alcohol, chloroform or methanol.
6. microcapsule preparation method according to any one of claim 1 to 5, it is characterised in that: the following steps are included:
(1) prepared by water phase: 3~35 parts of emulsifiers are dissolved in 542~749 parts of deionized waters as water phase；
(2) oil is mutually prepared: by 6~29 parts of ethyl celluloses, 4~30 parts of wave absorbing agents, 5~74 parts of epoxy resin and 87~236 parts
Organic solvent mixing, ultrasonic disperse dissolution；
(3) it emulsifies: oil being mutually poured slowly into water phase, 2~6h, the shape under shear action are stirred with certain temperature and certain speed
Glomeration emulsion oil-in-water；The temperature range is 25~35 DEG C, and the range of speeds is in 100r/min~1500r/min；
(4) solidify: temperature being risen to 40 DEG C~45 DEG C and continues to stir 1h~3h, so that organic solvent sufficiently volatilizees；
(5) filtration washing: suspension obtained after solidification is cooled to room temperature, and removal swims in waste residue and the filtering on upper layer,
Obtained sediment is washed with distilled water, air-dries obtain inhaling wave-self-repairing microcapsule at room temperature.
7. preparation method according to claim 6, it is characterised in that: in step 1, the emulsifier includes gelatin, will
The emulsifier is dissolved in deionized water, and is heated to 70 DEG C, stirring to dissolution, and is cooled to 25 DEG C.
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Cited By (4)
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| CN111499253A (en) * | 2020-04-15 | 2020-08-07 | 东南大学 | Microwave controlled release-based additive microcapsule and preparation method thereof |
| CN114163825A (en) * | 2021-11-08 | 2022-03-11 | 三峡大学 | Core-shell structure graphene composite particle and preparation method thereof |
| CN114774083A (en) * | 2022-03-30 | 2022-07-22 | 南昌大学 | Multifunctional microcapsule with temperature regulation and electromagnetic absorption functions and preparation method thereof |
| CN114956652A (en) * | 2022-05-06 | 2022-08-30 | 武汉理工大学 | Preparation method of microcapsule curing agent for phosphogypsum-based jetting rock-forming material |
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| CN114774083A (en) * | 2022-03-30 | 2022-07-22 | 南昌大学 | Multifunctional microcapsule with temperature regulation and electromagnetic absorption functions and preparation method thereof |
| CN114956652A (en) * | 2022-05-06 | 2022-08-30 | 武汉理工大学 | Preparation method of microcapsule curing agent for phosphogypsum-based jetting rock-forming material |
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