CN104592803B - Organic-silicon-modified phase-change microcapsule and preparation method thereof - Google Patents
Organic-silicon-modified phase-change microcapsule and preparation method thereof Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The present invention relates to a kind of organic-silicon-modified phase-change microcapsule and preparation method thereof, building coating is can be applied to, it is prepared by the raw material that following weight matches according to following the step of sequentially carrying out：1) pre-emulsification：50 70 parts of paraffin, 14 19 parts of styrene, 0.3 1 parts of organosilicon modifiers, 5 8.5 parts of methacrylic acids, 55 82 parts of deionized waters, 24 parts of anion emulsifiers, 0.5 1.5 parts of nonionic emulsifiers and 0.25 1 parts of initiators are added in pre-emulsification reactor, at a temperature of higher than 3 15 DEG C of melting point of paraffin wax, under 800 1200r/min rotating speeds disperse, pre-emulsification 10 40 minutes, obtains pre-emulsion；2) emulsion polymerization；3) post-process；It can improve the stability of phase-change microcapsule polymer emulsion, reduce the collision cohesion between phase-change microcapsule emulsion particle, improve dispersiveness of the emulsion particle in coating.
Description
Technical field
The present invention relates to a kind of phase-change microcapsule and preparation method thereof, more particularly to a kind of organic-silicon-modified phase-change microcapsule
And preparation method thereof, building coating is can be applied to, belongs to feature technical field of phase-change energy storage.
Background technology
With the development of society and the progress of science, the energy becomes the big obstacle for hindering human development progress, improves energy
Source utilization rate has become the emphasis of people's Recent study, and phase-change material is as a kind of hot storage material for improving energy utilization rate
It is widely used, its cardinal principle is that substantial amounts of latent heat is absorbed and discharged in phase transition process using phase-change material, can be reached
Temperature control and energy saving purpose, but this kind of material is in phase transition process, it is readily flowed particularly in liquid phase, in practical applications
It is restricted.
In the 1970s, with the maturation of microcapsules technology, phase-change microcapsule technology obtains development and application.Phase transformation
Microcapsules are the particles for being wrapped up phase-change material with natural or synthesis polymeric material, so as to avoid phase-change material and its
The contact of his material.Phase-change microcapsule is made of cyst wall and capsule-core two parts, and capsule-core is phase-change material, common solid-liquid phase change
Material has crystalline hydrate salt, eutectic hydrated salt, paraffin class, polyethylene glycol, linear paraffin, fatty acid etc..Cyst wall is generally height
Molecularly Imprinted Polymer, often select it is common have polyureas, polyamide, Lauxite, melamine formaldehyde resin, polyurethane or it
Compound system.
In recent years, existing substantial amounts of report discloses phase-change microcapsule and its technology of preparing.2004, patent
CN1513938A Wang Lixins et al. use melamine formaldehyde resin to select direct-connected alkane, fatty alcohol and organosilane ester for wall material
Compound is phase-change material, and phase-change microcapsule material has been made.2006, patent CN1903971A Liu Yong stood erect et al. using straight
The method that lotion is prepared in alkaline carbamide performed polymer is connected on, the shell speed of growth is controlled by controlling reaction temperature
Prepare phase-change microcapsule.2013, patent CN103468222A is seductive and bewitching et al. to use 46#Paraffin, liquid paraffin, lauryl alcohol and
Butyl stearate be low temperature phase change core, using methyl methacrylate, methacrylic acid, acrylic acid polymer as wall material,
A kind of microcapsules of low temperature phase change are synthesized.2014, patent CN103937461A side benefited the nation et al. with methyl methacrylate
For wall material, a kind of phase-change microcapsule of clothes temperature adjustment has been synthesized by core of the mixture of n-octadecane and hexadecane.
In the preparation method of report phase-change microcapsule, majority is wall material with melamine resin, Lauxite, phenolic resin,
By its Effect of Materials, removing residue formaldehyde becomes inevitable in cyst wall.In addition, using the method for emulsion polymerization, conventional emulsion used
Agent is attached to emulsion particle surface in a manner of physical absorption, so as to fulfill the stability to emulsion system, this conventional emulsifier
Molecule easily is influenced to desorb by external environment, causes emulsion particle collision cohesion.And often contain APE (alkyl in emulsifying agent
Phenol polyethenoxy ether) and formaldehyde harmful substance, in addition, using methyl methacrylate, methacrylic acid polymer as wall material, though
Without harmful substances such as formaldehyde, but the heat endurance of phase-change microcapsule is poor, and resistance to elevated temperatures is poor, and resistance to acid and alkali is poor.
The content of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provides a kind of organic-silicon-modified phase-change microcapsule
And preparation method thereof, the organic-silicon-modified phase-change microcapsule prepared by the present invention can improve the steady of phase-change microcapsule polymer emulsion
It is qualitative, the collision cohesion between phase-change microcapsule emulsion particle is reduced, improves dispersiveness of the emulsion particle in coating.In addition, also have
There is outstanding weatherability, make phase-change microcapsule with good stability and resistance to acid and alkali.
Technical solution of the present invention is as follows：
One) scheme one：
A kind of organic-silicon-modified phase-change microcapsule, the raw material that it is matched by following weight is according to following the step of sequentially carrying out
It is prepared：
1) pre-emulsification：
By 50-70 parts of paraffin, 14-19 parts of styrene, 0.3-1 parts of organosilicon modifiers, 5-8.5 parts of methacrylic acids, 55-
82 parts of deionized waters, 2-4 parts of anion emulsifiers, 0.5-1.5 parts of nonionic emulsifiers and 0.25-1 parts of initiators are added to pre-
In emulsion reactor, at a temperature of higher than 3-15 DEG C of melting point of paraffin wax, under 800-1200r/min rotating speeds disperse, pre-emulsification
10-40 minutes, obtain pre-emulsion；
2) emulsion polymerization：
30-45 parts of deionized waters are added in polymer reactor, are heated to 78 DEG C -82 DEG C, step 1) is obtained pre-
Emulsion droplet is added in polymer reactor, is added dropwise 50-100 minutes, afterwards when reaction 5.5-6.5 is small at a temperature of 78 DEG C -82 DEG C,
Obtain polymer emulsion；
3) post-process：
The obtained polymer emulsion of step 2) is separated by filtration, after washing 2-5 times, that is, obtains the micro- glue of organic-silicon-modified phase transformation
Capsule；
The melting point of paraffin wax is 30-60 DEG C.
The organosilicon modifier is siloxanes, vinyl trimethoxy containing single methacryloxy functional side group
One kind in silane, γ-methacryloxypropyl trimethoxy silane.
The nonionic emulsifier uses the polyethenoxy ether class containing acrylic.
The cationic emulsifier uses the salt containing acrylic.
The initiator is using azodiisobutyronitrile, benzoyl peroxide, azobisisoheptonitrile, ammonium persulfate, persulfuric acid
One kind in potassium.
Two) scheme two：A kind of preparation method for being used to prepare the organic-silicon-modified phase-change microcapsule described in scheme one, the party
Method includes the step of next coming in order carry out：
1) pre-emulsification：
By 50-70 parts of paraffin, 14-19 parts of styrene, 0.3-1 parts of organosilicon modifiers, 5-8.5 parts of methacrylic acids, 55-
82 parts of deionized waters, 2-4 parts of anion emulsifiers, 0.5-1.5 parts of nonionic emulsifiers and 0.25-1 parts of initiators are added to pre-
In emulsion reactor, at a temperature of higher than 3-15 DEG C of melting point of paraffin wax, under 800-1200r/min rotating speeds disperse, pre-emulsification
10-40 minutes, obtain pre-emulsion；
2) emulsion polymerization：
30-45 parts of deionized waters are added in polymer reactor, are heated to 78 DEG C -82 DEG C, step 1) is obtained pre-
Emulsion droplet is added in polymer reactor, is added dropwise 50-100 minutes, afterwards when reaction 5.5-6.5 is small at a temperature of 78 DEG C -82 DEG C,
Obtain polymer emulsion；
3) post-process：
The obtained polymer emulsion of step 2) is separated by filtration, after washing 2-5 times, that is, obtains the micro- glue of organic-silicon-modified phase transformation
Capsule；
The melting point of paraffin wax is 30-60 DEG C.
The inventive principle of the present invention is as follows：
The present invention using styrene, methacrylic acid, organosilicon modifier as monomer, with the salt containing acrylic and
Polyoxyethylene ether containing acrylic is emulsifying agent, using the method for emulsion polymerization, styrene, metering system during the reaction
Acid, organosilicon modifier are moved to water-oil interface direction, and synthetic polymer, has successfully wrapped up phase-change material paraffin, of the invention
The functional group that the anion emulsifier and nonionic emulsifier that organic-silicon-modified phase-change microcapsule is selected contain can be directly and single
Precursor reactant, greatly improves the stability of polymer emulsion, reduce between emulsion particle collision cohesion, in coating in application,
Facilitation is dispersed among coating to phase-change microcapsule.
The cyst material of microcapsules is formed by styrene and methacrylic polymeric, without formaldehyde, with traditional ureaformaldehyde tree
Fat, phenolic resin cyst wall are compared to more environmentally-friendly.It is organic-silicon-modified to cyst material progress to add organosilicon modifier, adds micro-
The dispersiveness of capsule, improves the thermal stability of cyst wall, weatherability, heat-resisting quantity and acid-proof alkaline.
Compared with prior art, the present invention have the following advantages：
Organic-silicon-modified phase-change microcapsule prepared by the present invention is free of formaldehyde, polymerizable using polymerizable emulsifying agent
Emulsifying agent can both play emulsifying agent in emulsion polymerization in itself, and can participate in polymerization process, itself and polymerisation list
Body can greatly improve the stability of polymer emulsion with Covalent bonding together, reduce the collision cohesion between emulsion particle,
Improve dispersiveness of the emulsion particle in coating.In addition, the present invention is modified phase-change microcapsule wall material using organosilicon, due to Si-O
The very high bond energy of key, outstanding weatherability make phase-change microcapsule with good stability and resistance to acid and alkali.
1) phase-change microcapsule prepared by the present invention, cyst material is formed by styrene and methacrylic polymeric, without first
Aldehyde, and with organic-silicon-modified, improve the thermal stability of cyst wall, weatherability, heat-resisting quantity and acid-proof alkaline.
2) phase-change microcapsule prepared by the present invention participates in monomer using the environment-friendly type emulsifying agent that may participate in polymerization, emulsifying agent
Polymerization process in, greatly improve the stability of polymer emulsion, reduce the reunion between phase-change microcapsule, it is micro- to improve phase transformation
Dispersion performance of the capsule in coating.
3) phase-change microcapsule prepared by the present invention, preparation process is simple, and production efficiency is high, more efficiently.
4) the phase-change microcapsule particle diameter prepared can be directly appended in building coating at 1-5 μm, not influence the painting of coating
Film effect, oil-proof, microcapsule stability is good, and resistance to acid and alkali is good, has been greatly improved the heat preservation and insulation of coating, can also answer
For various aspects such as field of textiles, military fields.
5) present invention prepares the solid content of gained lotion up to more than 50%, and core accounts for microcapsules proportion in phase-change microcapsule
Up to more than 70%, production efficiency and the heat-insulating property of microcapsules, more energy conservation and environmental protection are greatly improved, is widely used.
Embodiment
Present invention is described in detail with reference to embodiment, embodiment：
(1) embodiment
A kind of organic-silicon-modified phase-change microcapsule, the raw material that it is matched by following weight is according to following the step of sequentially carrying out
It is prepared：
1) pre-emulsification：
By 50-70 parts of paraffin, 14-19 parts of styrene, 0.3-1 parts of organosilicon modifiers, 5-8.5 parts of methacrylic acids, 55-
82 parts of deionized waters, 2-4 parts of anion emulsifiers, 0.5-1.5 parts of nonionic emulsifiers and 0.25-1 parts of initiators are added to pre-
In emulsion reactor, at a temperature of higher than 3-15 DEG C of melting point of paraffin wax, under 800-1200r/min rotating speeds disperse, pre-emulsification
10-40 minutes, obtain pre-emulsion；
2) emulsion polymerization：
30-45 parts of deionized waters are added in polymer reactor, are heated to 78 DEG C -82 DEG C, step 1) is obtained pre-
Emulsion droplet is added in polymer reactor, is added dropwise 50-100 minutes, afterwards when reaction 5.5-6.5 is small at a temperature of 78 DEG C -82 DEG C,
Obtain polymer emulsion；
3) post-process：
The obtained polymer emulsion of step 2) is separated by filtration, after washing 2-5 times, that is, obtains the micro- glue of organic-silicon-modified phase transformation
Capsule；
The melting point of paraffin wax is 30-60 DEG C.
(2) embodiment：
Embodiment 1
A kind of organic-silicon-modified phase-change microcapsule, the raw material that it is matched by following weight is according to following the step of sequentially carrying out
It is prepared：
1) pre-emulsification：
By 55 parts of paraffin, 18.55 parts of styrene, 0.5 part of 32 organic-silicon-modified additive of DOW CORNING, 6.35 parts of methyl-props
Olefin(e) acid, 60 parts of deionized waters, 3.1 parts of propenyl ether sulfonate, 1.18 parts of acrylic polyoxyethylene ether and 0.5 part of two isobutyl of azo
Nitrile is added in pre-emulsification reactor, and heating water bath is to 45 DEG C, and in the case where 900r/min rotating speeds disperse, pre-emulsification 20 minutes, obtains
Pre-emulsion；
2) emulsion polymerization：
30 parts of deionized waters are added in polymer reactor, 80 DEG C are heated to, by the obtained pre-emulsification drop of step 1)
It is added in polymer reactor, is added dropwise 80 minutes, afterwards when reaction 6 is small at a temperature of 80 DEG C, obtains polymer emulsion；
3) post-process：
The obtained polymer emulsion of step 2) is separated by filtration, after washing 2-5 times, that is, obtains the micro- glue of organic-silicon-modified phase transformation
Capsule；
The melting point of paraffin wax is 37 DEG C.
Embodiment 2
A kind of organic-silicon-modified phase-change microcapsule, the raw material that it is matched by following weight is according to following the step of sequentially carrying out
It is prepared：
1) pre-emulsification：
By 70 parts of paraffin, 23.25 parts of styrene, 1 part of figure A-171 organo functional silanes advanced in years, 8.08 parts of methacrylic acids,
82 parts of deionized waters, 4.0 parts of propenyl ether sulfonate, 1.5 parts of acrylic polyoxyethylene ether and 1 part of azodiisobutyronitrile are added to
In pre-emulsification reactor, heating water bath is to 50 DEG C, and in the case where 900r/min rotating speeds disperse, pre-emulsification 20 minutes, obtains pre-emulsion；
2) emulsion polymerization：
44 parts of deionized waters are added in the reactor, are heated to 80 DEG C, the obtained pre-emulsion of step 1) is added drop-wise to
In reactor, it is added dropwise 100 minutes, afterwards when reaction 6 is small at a temperature of 80 DEG C, obtains polymer emulsion；
3) post-process：
The obtained polymer emulsion of step 2) is separated by filtration, after washing 2-5 times, that is, obtains the micro- glue of organic-silicon-modified phase transformation
Capsule；
The melting point of paraffin wax is 42 DEG C.
Embodiment 3
A kind of organic-silicon-modified phase-change microcapsule, the raw material that it is matched by following weight is according to following the step of sequentially carrying out
It is prepared：
1) pre-emulsification：
By 50 parts of paraffin, 15.57 parts of styrene, 0.3 part of figure A-174NT organo functional silanes advanced in years, 5.37 parts of methyl-props
Olefin(e) acid, 54 parts of deionized waters, 3.5 parts of propenyl ether sulfonate, 0.8 part of acrylic polyoxyethylene ether and 0.25 part of benzoyl peroxide first
Acyl is added in pre-emulsification reactor, and heating water bath is to 45 DEG C, and in the case where 900r/min rotating speeds disperse, pre-emulsification 20 minutes, obtains
Pre-emulsion；
2) emulsion polymerization：
30 parts of deionized waters are added in the reactor, are heated to 80 DEG C, the obtained pre-emulsion of step 1) is added drop-wise to
In reactor, it is added dropwise 60 minutes, afterwards when reaction 6 is small at a temperature of 80 DEG C, obtains polymer emulsion；
3) post-process：
The obtained polymer emulsion of step 2) is separated by filtration, after washing 2-5 times, that is, obtains the micro- glue of organic-silicon-modified phase transformation
Capsule；
The melting point of paraffin wax is 31 DEG C.
Embodiment 4
A kind of organic-silicon-modified phase-change microcapsule, the raw material that it is matched by following weight is according to following the step of sequentially carrying out
It is prepared：
1) pre-emulsification：
By 60 parts of paraffin, 19.5 parts of styrene, 0.5 part of figure A-174NT organo functional silanes advanced in years, 8 parts of methacrylic acids,
55 parts of deionized waters, 2.8 parts of propenyl ether sulfonate, 1.5 parts of acrylic polyoxyethylene ether and 0.5 part of benzoyl peroxide add
Into pre-emulsification reactor, heating water bath is to 50 DEG C, and in the case where 900r/min rotating speeds disperse, pre-emulsification 20 minutes, obtains pre-emulsification
Liquid；
2) emulsion polymerization：
30 parts of deionized waters are added in the reactor, are heated to 80 DEG C, the obtained pre-emulsion of step 1) is added drop-wise to
In reactor, it is added dropwise 60 minutes, afterwards when reaction 6 is small at a temperature of 80 DEG C, obtains polymer emulsion；
3) post-process：
The obtained polymer emulsion of step 2) is separated by filtration, after washing 2-5 times, that is, obtains the micro- glue of organic-silicon-modified phase transformation
Capsule；
The melting point of paraffin wax is 45 DEG C.
Embodiment 5
A kind of organic-silicon-modified phase-change microcapsule, the raw material that it is matched by following weight is according to following the step of sequentially carrying out
It is prepared：
1) pre-emulsification：
By 50 parts of paraffin, 19.5 parts of styrene, 0.5 part of 32 organic-silicon-modified additive of DOW CORNING, 8 parts of metering systems
Acid, 65 parts of deionized waters, 3.1 parts of propenyl ether sulfonate, 1.08 parts of acrylic polyoxyethylene ether and 0.5 part of azodiisobutyronitrile
It is added in pre-emulsification reactor, heating water bath is to 45 DEG C, and in the case where 900r/min rotating speeds disperse, pre-emulsification 20 minutes, obtains pre-
Emulsion；
2) emulsion polymerization：
35 parts of deionized waters are added in the reactor, are heated to 80 DEG C, the obtained pre-emulsion of step 1) is added drop-wise to
In reactor, it is added dropwise 60 minutes, afterwards when reaction 6 is small at a temperature of 80 DEG C, obtains polymer emulsion；
3) post-process：
The obtained polymer emulsion of step 2) is separated by filtration, after washing 2-5 times, that is, obtains the micro- glue of organic-silicon-modified phase transformation
Capsule；
The melting point of paraffin wax is 31 DEG C.
In various embodiments above：
The preferred 32 organic-silicon-modified additive of DOW CORNING of the organosilicon modifier；
The nonionic emulsifier acrylic polyoxyethylene ether is preferably the ER-10 of ADEKA productions；
The anion emulsifier allyl ether hydroxylpropyl sulfonate is preferably the COPS-1 of SOLVAY productions.
The paraffin is preferably the paraffin of Zhenjiang Runzhou Ze Zhong Wax specials factory production.
The styrene, methacrylic acid, the preferred Aladdin reagent of azodiisobutyronitrile.
Solid content, heat endurance, enthalpy, particle size, acidproof is carried out to prepared organic-silicon-modified phase-change microcapsule
The performance tests such as alkalescence.
Solid content is tested：The accurate quality for weighing the flat disk of blank is M0, 1g or so samples are weighed, sample is pacifically justified
The quality of disk is M altogether2, sample is heated into 1h in 120 ± 2 DEG C of baking ovens.It is cooled to room temperature, weighs again surplus in drier afterwards
The common M of the quality of remaining sample and flat disk1, all weighings are accurately to 0.1mg.
The percentage (X) of solid content is calculated as follows：
X=100 × (M1-M0)/(M2-M0)
Twice, measurement result is averaged, report test result a to decimal for measurement.
Particle size measures：The particle size of microcapsules is observed under a scanning electron microscope.
Heat enthalpy value measures：With the heat enthalpy value of differential scanning calorimeter (DSC) test sample, test condition is：It is accurate to claim
The sample of 10mg or so is taken, in N2Under atmosphere, 10K/min temperature rates are selected, test temperature selects -20 DEG C -100 DEG C of survey
Measure scope.
Emulsion particle dispersiveness test：The phase-change microcapsule lotion of the placement 10 days of 30g is taken to be added to 100g finished product emulsion paints
In, stirred 30 minutes with the rotating speed of 900r/min.The emulsion paint sample after mixing is taken, fineness test is done on hanging plate fineness gauge.
Phase-change microcapsule thermal stability is tested：With the heat decomposition temperature of thermal gravimetric analyzer (TG) test sample, survey
Strip part is：The sample of 10mg or so is weighed, in N2Under atmosphere, selection 10K/min heating rates, 25 DEG C of test temperature selection-
600 DEG C of measurement range.
Acid resistance is tested：Hydrochloric acid is added in microcapsule emulsion and adjusts pH value to 3, is placed two days later, in flat disk
Add 1g or so sample, sample be put into 50 degrees Celsius of baking ovens 1 it is small when, touch whether have oil leakage phenomenon with feel after taking-up.
Alkali resistance is tested：Ammonium hydroxide is added in microcapsule emulsion and adjusts pH value to 10, is placed two days later, in flat disk
Add 1g or so sample, sample be put into 50 degrees Celsius of baking ovens 1 it is small when, touch whether have oil leakage phenomenon with feel after taking-up.
By the test to each embodiment, the detection data result of organic-silicon-modified phase-change microcapsule of the invention is for example following
Shown in each table：
The experimental data of each embodiment test of table one --- organic-silicon-modified phase-change microcapsule
, it is apparent that various embodiments of the present invention are respectively provided with good heat surely under difficult environmental conditions from table one
Qualitative energy and resistance to acid and alkali, for particle diameter distribution between 1-5 μm, heat enthalpy value is high, and with good stability and acidproof
Alkalescence, has good application value.
In conclusion the organic-silicon-modified phase-change microcapsule of various embodiments of the present invention has very high heat enthalpy value, therefore
With good energy-storage property, while there is good thermal stability.
Above-mentioned embodiment is simply explained in detail technical scheme, the present invention not only only office
Be limited to above-described embodiment, it will be understood by those skilled in the art that it is every according to above-mentioned principle and spirit on the basis of the present invention
Improve, substitute, all should be within protection scope of the present invention.
Claims (4)
- A kind of 1. organic-silicon-modified phase-change microcapsule, it is characterised in that：It by following weight proportioning raw material according to it is following sequentially The step of progress, is prepared：1）Pre-emulsification：By 50-70 parts of paraffin, 14-19 parts of styrene, 0.3-1 parts of organosilicon modifiers, 5-8.5 parts of methacrylic acids, 55-82 parts Deionized water, 2-4 part anion emulsifier, 0.5-1.5 parts of nonionic emulsifiers and 0.25-1 parts of initiators are added to pre-emulsification In reactor, at a temperature of higher than 3-15 DEG C of melting point of paraffin wax, under 800-1200r/min rotating speeds disperse, 10-40 points of pre-emulsification Clock, obtains pre-emulsion；2）Emulsion polymerization：30-45 parts of deionized waters are added in polymer reactor, 78 DEG C -82 DEG C are heated to, by step 1）Obtained pre-emulsification Drop is added in polymer reactor, is added dropwise 50-100 minutes, afterwards when reaction 5.5-6.5 is small at a temperature of 78 DEG C -82 DEG C, is obtained Polymer emulsion；3）Post processing：It is separated by filtration step 2）Obtained polymer emulsion, after washing 2-5 times, that is, obtains organic-silicon-modified phase-change microcapsule；The melting point of paraffin wax is 30-60 DEG C；The nonionic emulsifier uses the polyethenoxy ether class containing acrylic；The anion emulsifier uses the salt containing acrylic.
- 2. organic-silicon-modified phase-change microcapsule according to claim 1, it is characterised in that：The organosilicon modifier is the siloxanes containing single methacryloxy functional side group, vinyl trimethoxy silicon One kind in alkane, γ-methacryloxypropyl trimethoxy silane.
- 3. organic-silicon-modified phase-change microcapsule according to claim 1, it is characterised in that：The initiator is using in azodiisobutyronitrile, benzoyl peroxide, azobisisoheptonitrile, ammonium persulfate, potassium peroxydisulfate One kind.
- 4. a kind of preparation method for being used to prepare the organic-silicon-modified phase-change microcapsule of claim 1-3 any one of them, it is special Sign is：The organic-silicon-modified phase-change microcapsule is according to following the step of sequentially carrying out preparation：1）Pre-emulsification：By 50-70 parts of paraffin, 14-19 parts of styrene, 0.3-1 parts of organosilicon modifiers, 5-8.5 parts of methacrylic acids, 55-82 parts Deionized water, 2-4 part anion emulsifier, 0.5-1.5 parts of nonionic emulsifiers and 0.25-1 parts of initiators are added to pre-emulsification In reactor, at a temperature of higher than 3-15 DEG C of melting point of paraffin wax, under 800-1200r/min rotating speeds disperse, 10-40 points of pre-emulsification Clock, obtains pre-emulsion；2）Emulsion polymerization：30-45 parts of deionized waters are added in polymer reactor, 78 DEG C -82 DEG C are heated to, by step 1）Obtained pre-emulsification Drop is added in polymer reactor, is added dropwise 50-100 minutes, afterwards when reaction 5.5-6.5 is small at a temperature of 78 DEG C -82 DEG C, is obtained Polymer emulsion；3）Post processing：It is separated by filtration step 2）Obtained polymer emulsion, after washing 2-5 times, that is, obtains organic-silicon-modified phase-change microcapsule；The melting point of paraffin wax is 30-60 DEG C.
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| CN105396523A (en) * | 2015-12-26 | 2016-03-16 | 孝感巨核新材料科技有限公司 | Preparation method of polymer wrapped paraffin phase-change microsphere |
| US20200108367A1 (en) * | 2016-04-12 | 2020-04-09 | Croda International Plc | Microcapsules |
| CN109082120B (en) * | 2018-09-28 | 2021-06-01 | 华南协同创新研究院 | Elastic shell microcapsule phase change material and preparation method and application thereof |
| CN109261090A (en) * | 2018-10-08 | 2019-01-25 | 长春理工大学 | A kind of preparation method of phase-change microcapsule |
| CN111607300A (en) * | 2020-06-21 | 2020-09-01 | 武汉露能科技有限公司 | Durable anti-icing low-surface-energy material for wind power blade and preparation method thereof |
| CN114653314B (en) * | 2020-12-23 | 2022-11-25 | 北京化工大学 | Method for preparing self-assembly type microcapsule |
| CN115386344A (en) * | 2021-05-25 | 2022-11-25 | 中国石油天然气股份有限公司 | Paraffin-based composite phase change microcapsule and preparation method thereof |
| CN114276497B (en) * | 2021-12-28 | 2023-02-24 | 青岛理工大学 | Paraffin-modified styrene-acrylate-siloxane core-shell phase-change emulsion and preparation method and application thereof |
| CN114752217A (en) * | 2022-04-06 | 2022-07-15 | 中国民用航空飞行学院 | Flame-retardant and flexible phase-change heat storage composite material, preparation method and application |
| CN114870760B (en) * | 2022-05-13 | 2023-08-29 | 湖北大学 | Preparation method of inorganic shell material phase-change microcapsule |
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| CN101717618A (en) * | 2009-11-10 | 2010-06-02 | 天津工业大学 | Preparation method of phase-change material microcapsule |
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