CN107828407A - A kind of discoloration micro-nano capsule of solid-state capsule-core and preparation method thereof - Google Patents
A kind of discoloration micro-nano capsule of solid-state capsule-core and preparation method thereof Download PDFInfo
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- CN107828407A CN107828407A CN201711264272.2A CN201711264272A CN107828407A CN 107828407 A CN107828407 A CN 107828407A CN 201711264272 A CN201711264272 A CN 201711264272A CN 107828407 A CN107828407 A CN 107828407A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
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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
- B01J13/20—After-treatment of capsule walls, e.g. hardening
- B01J13/206—Hardening; drying
Abstract
The invention discloses a kind of discoloration micro-nano capsule of solid-state capsule-core and preparation method thereof, is characterized in, using Solid state photochromism composite as capsule-core, comprising the following steps：1) after polymer, photochromic dyes, antioxidant, ultra-violet absorber and sensitizer being swelled in oil-dissolving solvent, being dissolved into homogeneous oil phase, it is added in the aqueous solution containing emulsifying agent and assistant for emulsifying agent, emulsification pretreatment obtains oil-in-water type stable emulsion；2) after adjustment emulsion temperature is maintained at 30~70 DEG C and adjusts pH value of solution, appropriate amino resins or etherification modified amino resin solution are at the uniform velocity added；3) it is warming up to certain temperature and is kept stirring for, can obtain micro-nano capsule；4) the micro-nano capsule pH of suspension prepared is adjusted to 7 or so, filtering and washing；5) capsule is dried and be heat-treated.Capsule thermostabilization prepared by this method is up to more than 300 DEG C, and mechanical performance is obviously improved, and technique is simple, can industrial production, available for fiber process, textile garment, chemical industry printing and dyeing, the field such as plastic products.
Description
Technical field
The present invention relates to a kind of photochromic micro-nano capsule, more particularly, to the photochromic micro-nano that a kind of capsule-core is solid-state
Capsule and preparation method thereof.
Background technology
Photochromic material refers to by a kind of intellectual material that color change can occur after light source activation, intelligently anti-
The multiple fields such as pseudo-, information storage, weaving dress and adornment obtain increasing application.If photochromic dyes is for a long time
Under the occasions such as ultraviolet light, oxygen or free electron presence, the chemical constitution of dyestuff can inevitably change, from
And cause the decay or unstable of discoloration.Capsule " is held with a kind of the small of core shell structure that capsule-core is wrapped up with wall material
Device ", it can be the functional materials of the liquid such as medicine, dyestuff, essence, ink or solid-state in container, be released for protecting or controlling
Capsule-core material, masking smell etc. are put, the persistent solid-state of capsule-core material is realized, greatly facilitates its application.Will be photochromic
Dye solution is wrapped in capsule, and light can be avoided to become dyestuff and contacted with the direct of ultraviolet light, oxygen and free electron, can effectively be strengthened
Its weatherability, keep excellent photochromic properties.
Pei Guang tinkling of pieces of jade et al. uses situ aggregation method in patent CN101225296A, and photochromic dyes is wrapped in into melamine
In amine-for-aldehyde resin, photochromic micro-encapsulation is prepared for.But the organic solvent that they use is that boiling point is relatively low and toxicity is stronger
Benzene, ethanol, toluene, tetrachloro-ethylene or carbon tetrachloride etc., human body or environment are damaged, limit it to a certain extent
Using.Ni Yonghao of University Of Science and Technology Of Tianjin et al. is in patent CN102875822A using spiro-pyrans, spiral shell oxazine discoloration organic matter
The thawing such as solution and cellulose family shears to obtain hydrophily latex.Photochromic material solution in emulsion droplet state, does not enter
Row protection is handled, and its weatherability and photomodification can be difficult to persistently, and its application scenario can be also restricted.
The content of the invention
In order to solve the technical problem in above-mentioned photochromic material application, its thermal stability, weather resistance, light are lifted
Cause discoloration and expand its application field.Photochromic dyes is dispersed in solid polymer, relative to will be photochromic
Dyestuff is dissolved in aqueous organic solution, can greatly promote photochromic dyes thermal stability, and this is it in Process Technology of Polymer
Application in field such as plastics or fiber is laid a good foundation., can in one layer of cyst wall of Solid state photochromism dye composition outer wrapping
The contact with external environment is avoided, while antioxidant, ultra-violet absorber and sensitizer are added in solid-state capsule-core, not only may be used
Its weatherability is effectively lifted, can also improve its photochromic properties.The invention provides a kind of discoloration micro-nano glue of solid-state capsule-core
Capsule and preparation method thereof, this method first exist polymer, photochromic dyes, antioxidant, ultra-violet absorber and sensitizer
After oil-dissolving solvent is dissolved into homogeneous oil phase, emulsification pretreatment obtains oil-in-water type stable emulsion, then carries out encapsulated bag to it
Wrap up in obtain the micro-nano capsule of oil-soluble liquid capsule-core, finally capsule is dried and is heat-treated, it is molten to remove all or part of oil in capsule-core
Property solvent, finally give capsule-core be Solid state photochromism compound micro-nano capsule.Solid-state capsule-core capsule heat prepared by this method
Equilibrium temperature up to more than 300 DEG C, mechanical performance be improved significantly, while technique is easily controlled, and is adapted to large-scale production.
A kind of discoloration micro-nano capsule preparation method of solid-state capsule-core, specifically includes following steps：
1) by mass, by 1~100 part of polymer, 1~20 part of photochromic dyes, 1~10 part of antioxidant, 1~
10 parts of ultra-violet absorbers and 1~10 part of sensitizer are added in 100 parts of oil soluble materials after being swelled, and agitating and heating dissolves to obtain
Phase oil-soluble solution；
2) by above-mentioned oil-phase solution be added to emulsifier concentration and assistant for emulsifying agent concentration be respectively 0.1~10wt% water
In solution, high speed shearing emulsification obtains emulsion oil-in-water, and emulsion droplet size scope control is in 10nm~500 μm, adjustment emulsion
PH is 4~7, and temperature control is at 30~70 DEG C；
3) by mass, takes 50~300 parts of amino resins or etherified amino resins to be diluted with water and stir evenly, is at the uniform velocity added to
In emulsion oil-in-water obtained above, 0.5~3 hour is incubated；
4) after system is warming up to 60~95 DEG C by, 0.5~3 hour micro-nano capsule that can obtain liquid oil phase capsule-core is incubated,
The micro-nano capsule pH of suspension prepared is adjusted to 7 or so, filtering and washing can obtain capsule filter cake；
5) capsule is dried and is heat-treated by, removes all or part of oil-dissolving solvent in capsule-core, it is solid-state to finally give capsule-core
The micro-nano capsule of photochromic compound.
The polymer is thermoplastic polymer, including PET, polybutylene terephthalate, is gathered
Ethene, polyvinylmethyl ethers, polyvinyl ethyl ether, ethylene propylene copolymer, EP rubbers, PVK, poly-vinegar acid second
Alkene ester, polyvinyl fluoride, polyvinylidene fluoride, polyvinyl chloride (PVC), polyvinylidene chloride, polymethyl methacrylate, polypropylene
Acetoacetic ester, poly- (α-itrile group butyl acrylate), polyacrylonitrile, polyisobutenyl rubber, poly- chloro-butadiene, neoprene, gather
Cis-Isosorbide-5-Nitrae-isoprene, poly- anti-form-1,4- isoprene, copolymer from styrene and butadiene, polycaprolactam, gather the sub- last of the ten Heavenly stems
Base formamide, polyhexamethylene adipamide, polyhexamethylene sebacamide, poly- nonylene urea, poly, poly- carbonic acid
Ester, poly- 2,6- dimethyl p-phenylene, poly- [double (methylamino) phosphine nitriles], dimethyl silicone polymer, celluloid fiber element, cellulose
At least one of ester, poly(diphenyl ether sulfone).
The photochromic dyes is by naphtho- spirooxazine, spiro-pyrans class, diarylethene, azobenzene, fulgenic acid
Any or any mixing group in liquor-saturated class and aphthopyrans class, transition metal oxide, metal halide and rare earth compounding
Into.
The antioxidant is butylhydroxy anisole (BHA), dibutyl hydroxy toluene (BHT), the tert-butyl group to benzene two
Phenol (TBHQ), propylgallate (PG), ascorbyl palmitate (AP), thiodipropionic acid dilauryl cinnamic acid ester (DLTP), 4-
Any one or several mixture in hexyl resorcin (4-HR).
The ultra-violet absorber be salicylic acid esters, benzophenone class, benzotriazole, group-substituted acrylonitrile, triazines and
Phenyl salicylate, 2- (2 '-hydroxyl -5 '-aminomethyl phenyl) BTA, 2,4-DihydroxyBenzophenone, 2- in hindered amines
Hydroxyl -4- methoxy benzophenones, 2-hydroxy-4-n-octoxybenzophenone, 2- (2 '-hydroxyl -3 ', 5 '-two tertiary phenyl) -5-
Chlorination BTA, single benzoic acid resorcinol, 2,2 '-thiobis (4- t-octyl phenol epoxide) nickel, three (1,2,2,6,6- five
Methyl piperidine base) phosphite ester, 4- benzoyloxys -2,2,6,6- tetramethyl piperidines, 2,4,6- tri- (2 '-n-butoxyphenyls) -
At least one of 1,3,5-triazines and HMPA etc..
The sensitizer is the naphthoate of 1- hydroxyls -2 in aromatic series or aliphatic esters, ethanedioic acid dibenzyl ester and right
At least one of benzylbiphenyl etc..
The oil soluble material be alkanes in isopentane, pentane, petroleum ether (main pentane and hexanes mixtures), oneself
Alkane, hexamethylene, isooctane, trimethylpentane, pentamethylene, heptane and dioxanes；Methylamine, dimethylamine, 1,1- bis- in alkane derivatives
Chloromethanes, 1,1,1- chloroform, nitromethane, chloroform, chlorotrifluoroethane, carbon tetrachloride, trichloro ethylene, dichloride second
Alkene, butyl chloride, DMF, DMA, N-METHYLFORMAMIDE, dimethylformamide and diformazan are sub-
Sulfone；Isopropanol, isobutanol, n-butanol, propyl ether, diethyl ether and phenol in alcohol and ether etc.；Aldehyde and ketone include methylisobutylketone and
Methyl ethyl ketone etc.；Organic acid is mainly alkyl acid such as stearic acid etc.；Organic ester such as ethyl acetate, butyl acetate and stearic acid are just
Butyl ester etc.；Benzene includes one kind or several in benzene,toluene,xylene, paraxylene, meta-xylene, chlorobenzene, o-dichlorohenzene and aniline
The mixture of kind.
The emulsifying agent is selected from least one of following material：Polymerization of carboxylic acid in ionic surface active agent such as anionic
Polyacrylic acid, Sodium Polyacrylate, polyacrylamide and styrene maleic anhydride copolymer sodium salt solution in salt；Sodium alkyl benzene sulfonate
Such as neopelex, alkylsulfonate, aliphatic acid sulfoalkyl ester, sulfoalkyl acid amides, sulphosuccinates, alkylnaphthalene
Sulfonate such as nekal, the formaldehyde condensation products of alkylnaphthalene sulfonate, lignosulfonates, alkyl glycerol ether sulfonic acid
Salt；Fatty alcohol sulfate salt and secondary alkyl sulphate such as lauryl sodium sulfate；Phosphate ester salt；APES formaldehyde
Condensate sulfate；Alkyl naphthalene sulfonic acid formaldehyde condensation products and its similar compound；Phenol formaldehyde condensate sulfonate and its similar product
Kind, phenol sulfonic acid naphthalene sulfonic acid-formaldehyde condensation product sodium salt, phenol formaldehyde condensate sulfonate sodium, phenol-melocol condensate sulfonates, contracting
Methylcellulose and its derivative, xanthan gum, desugar sodium lignin sulfonate M-9 in lignosulfonates etc.；Nonionic table
Face activating agent, such as APES, higher alcohols AEO, aliphatic amine polyoxyethylene ether and fatty acid polyglycol
Oxygen vinyl acetate.
Nonionic surface active agent of the assistant for emulsifying agent including short chain alcohol or suitable HLB value, alkylol such as n-butanol,
Isobutanol, n-amyl alcohol, isoamyl alcohol, ethanol, ethylene glycol, propane diols, glycerine, erythrol, xylitol, hexitol, TWEEN Series
At least one of emulsifying agent and polyglycerol ester.
The amino resins is at least one in melamine resin, Lauxite and benzoguanamine resin etc.
Kind；The etherified amino resins be methanol etherification amino resins, n-butanol etherified amino resins, isobutanol etherified amino resins and
A kind of or arbitrarily several mixture in the amino resins of the alkylols such as ethanol etherified amino resins etherificate.
The discoloration micro-nano capsule of solid-state capsule-core prepared by the present invention, first by polymer, photochromic dyes, antioxidant,
Ultra-violet absorber and sensitizer carry out encapsulated parcel to it and obtain oil-soluble after oil-dissolving solvent is dissolved into homogeneous oil phase
The micro-nano capsule of liquid capsule-core, then capsule is heat-treated, all or part of oil-dissolving solvent in capsule-core is removed, finally gives capsule-core
For the micro-nano capsule of Solid state photochromism compound.The photochromic capsule-core of solid-state improves its heat endurance and its machining
Performance, antioxidant, ultra-violet absorber effectively extend the weatherability of photochromic dyes, sensitizer in encapsulated and capsule-core
Have to its discoloration and be obviously improved, this greatly promotes its performance and expands its application field.
Brief description of the drawings
Fig. 1 is the discoloration micro-nano capsule surface topography map of solid-state capsule-core prepared by embodiment 1；
Fig. 2 is the discoloration micro-nano capsule internal microstructure figure for the solid-state capsule-core that embodiment 1 synthesizes.
Embodiment
Technical scheme is described in detail below in conjunction with drawings and examples.
Embodiment 1
By 2g PLAs, 1g Luo oxazine organic photochromic dyestuffs, 0.5g dibutyl hydroxy toluenes, 0.3g2- hydroxyls -4-
Oxy-octyl benzophenone and the naphthoate of 0.3g1- hydroxyls -2 are dissolved in 20g ethyl acetate, and it is dense to be then added to 200g
Spend for 2wt% Sodium Polyacrylate aqueous copolymers solutions, while add 2g n-amyl alcohols, emulsified at a high speed under 5000rpm rotating speeds
10min, after the emulsion oil-in-water of stabilization is made, emulsion droplet size is measured as 1~5 micron through observation by light microscope, will be above-mentioned
Emulsion oil-in-water is transferred in three-necked flask, and the pH for adjusting emulsion is 4, and temperature is set as 50 DEG C.Weigh 10g parts methyl ether
Change melamino-formaldehyde performed polymer and with 5g distilled water dilutings into uniform solution, peristaltic pump is used while stirring under 350rpm speed
It is added drop-wise in homogeneous emulsion, after 75 DEG C are warming up to after dripping off and is incubated 120min, the micro-nano capsule that can obtain liquid capsule-core suspends
Liquid.Suspension is filtered, washs and obtains filter cake.By filter cake after vacuum drying, then handled 2 hours at 120 DEG C, you can
To the photochromic micro-nano capsule dry powder of solid-state capsule-core.
Capsule pattern such as Fig. 1, capsule micro-structure diagram are as shown in Figure 2 made from present case.From fig. 1, it can be seen that this reality
Apply example preparation micro-nano capsule particle diameter distribution it is uniform, in regular spherical shape, particle diameter distribution is at 1 μm~50 μm.In Fig. 2 capsule
Rupture in photo, it can be seen that its internal microstructure, not hollow shell structure, but be made up of irregular solid matter.
Embodiment 2
By 1kg thermoplastic polyurethanes, 1kg spiro-pyrans organic photochromic dyestuffs, 60g TBHQs, the mono- benzene of 50g
Formic acid resorcinol and 30g ethanedioic acid dibenzyl esters are dissolved in 20kg toluene, are then added to 100kg lauryl sodium sulfate
In solution, wherein 1kg containing lauryl sodium sulfate, n-octyl alcohol 1kg, polysorbate60 dosage 2kg is newborn at a high speed under 9000rpm rotating speeds
Change 60min, after the emulsion oil-in-water of stabilization is made, emulsion droplet size is measured as 2~15 microns through observation by light microscope, will be upper
Emulsion oil-in-water is stated to be transferred in three-necked flask, and the pH for adjusting emulsion is 4.9, temperature is set as 50 DEG C.Weigh 5kg butyl ether
Change melamino-formaldehyde performed polymer and with 5kg distilled water dilutings into uniform solution, while stirring with wriggling under 1000rpm speed
Pump is added drop-wise in homogeneous emulsion, and after 90 DEG C are warming up to after dripping off and is incubated 120min, the micro-nano capsule that can obtain liquid capsule-core is hanged
Supernatant liquid.Suspension is filtered, washs and obtains filter cake.By filter cake after vacuum drying, then handled 2 hours at 120 DEG C, you can
Obtain the discoloration micro-nano capsule dry powder of solid-state capsule-core.It is regular spherical with Electronic Speculum measurement capsule grain diameter, particle diameter distribution is micro- 2~17
In the range of rice.The starting weightless temperature that solid-state capsule-core discoloration capsule is measured with thermogravimetric analysis instrument is 320 DEG C, and heat resistance is excellent
It is good.
Embodiment 3
By 20g polybutylene terephthalate (PBT)s, 10g2,2- bis- (4- Fonnylphenyls) aphthopyrans, 0.3g dibutyl
Hydroxy-methylbenzene, 0.5g2- hydroxyl -4- oxy-octyl benzophenones and the naphthoate of 0.1g1- hydroxyls -2 are dissolved in 50g chloroforms
In, it is 5wt% polyacrylamide solutions to be then added to 500g concentration, emulsifies 15min at a high speed under 10000rpm rotating speeds, system
After the emulsion oil-in-water that must stablize, emulsion droplet is measured as 0.5~5 micron through observation by light microscope, by above-mentioned oil-in-water type breast
Liquid is transferred in three-necked flask, and the pH for adjusting emulsion is 6, and temperature is set as 30 DEG C.It is molten to weigh 100g phenolic resin performed polymers
Liquid, it is added drop-wise to while stirring in homogeneous emulsion under 1000rpm speed, can after 60 DEG C are warming up to after dripping off and is incubated 120min
Obtain the micro-nano capsule suspension of liquid capsule-core.Suspension is filtered, washs and obtains filter cake.By filter cake after vacuum drying,
Handled 2 hours at 90 DEG C again, you can obtain the discoloration micro-nano capsule dry powder of solid-state capsule-core.With laser particle analyzer analysis measurement glue
Capsule particle diameter distribution is in 1~8 micrometer range.The starting weightless temperature of solid-state capsule-core discoloration capsule is measured with thermogravimetric analysis instrument
For 380 DEG C, there is very high heat endurance.
Embodiment 4
10g acetyl celluloses are weighed, 10g1- ethoxys -3,3- dimethyl-nitroindoline quinoline spiro-pyrans light becomes dyestuff,
1g thiodipropionic acid dilauryl cinnamic acid esters, 0.5g4- benzoyloxys -2,2,6,6- tetramethyl piperidines and 0.3g are molten to benzylbiphenyl
For solution in 100g butyl acetates, it is 4wt% APES formaldehyde condensation products sulfats to be then added to 800g concentration
The aqueous solution, 30min is emulsified at a high speed under 30000rpm rotating speeds, after the emulsion oil-in-water of stabilization is made, emulsion droplet size is through optics
Micro- sem observation is measured as 0.1~2 micron, and above-mentioned emulsion oil-in-water is transferred in three-necked flask, and adjusts the pH of emulsion
For 5, temperature is set as 45 DEG C.80g melamine-ureas-formaldehyde prepolymer uniform solution is weighed, is stirred below in 200rpm speed
Mix side to be added drop-wise in homogeneous emulsion with peristaltic pump, after 70 DEG C are warming up to after dripping off and is incubated 120min, can obtain liquid capsule-core
Micro-nano capsule suspension.Suspension is filtered, washs and obtains filter cake.By filter cake after vacuum drying, then the vacuum at 100 DEG C
Drying process 5 hours, you can obtain the discoloration micro-nano capsule dry powder of solid-state capsule-core.The weightless starting point of test capsule is 420 DEG C,
It can apply to fibers melt spinning and plastic extrusion manufacture field.
Claims (10)
1. the discoloration micro-nano capsule preparation method of a kind of solid-state capsule-core, it is characterised in that comprise the following steps：
1) by mass, by 1~100 part of polymer, 1~20 part of photochromic dyes, 1~10 part of antioxidant, 1~10 part
Ultra-violet absorber and 1~10 part of sensitizer are added in 100 parts of oil soluble materials after being swelled, and agitating and heating dissolves to obtain homogeneous oil
Soluble solution；
2) by above-mentioned oil-phase solution be added to emulsifier concentration and assistant for emulsifying agent concentration be respectively 0.1~10wt% the aqueous solution
In, high speed shearing emulsification obtains emulsion oil-in-water, and emulsion droplet size scope control is being 4 in 10nm~500 μm, adjustment emulsion pH
~7, temperature control is at 30~70 DEG C；
3) by mass, takes 50~300 parts of amino resins or etherified amino resins to be diluted with water and stir evenly, is at the uniform velocity added to above-mentioned
In obtained emulsion oil-in-water, 0.5~3 hour is incubated；
4) after system is warming up to 60~95 DEG C by, 0.5~3 hour micro-nano capsule that can obtain liquid oil phase capsule-core is incubated, will be made
The micro-nano capsule pH of suspension got ready is adjusted to 7 or so, and filtering and washing can obtain capsule filter cake；
5) capsule is dried and is heat-treated by, removes all or part of oil-dissolving solvent in capsule-core, and it is photic for solid-state to finally give capsule-core
The micro-nano capsule of discoloration compound.
2. preparation method as claimed in claim 1, it is characterised in that the polymer is thermoplastic polymer, including poly- to benzene
Dioctyl phthalate second diester, polybutylene terephthalate, polyethylene, polyvinylmethyl ethers, polyvinyl ethyl ether, ethylene propylene copolymer
Thing, EP rubbers, PVK, polyvinyl acetate, polyvinyl fluoride, polyvinylidene fluoride, polyvinyl chloride (PVC), gather
Vinylidene chloride, polymethyl methacrylate, polyethyl acrylate, poly- (α-itrile group butyl acrylate), polyacrylonitrile, poly- isobutyl
Alkenyl rubber, poly- chloro-butadiene, neoprene, gather cis-Isosorbide-5-Nitrae-isoprene, poly- anti-form-1,4- isoprene, styrene
And butadiene copolymer, polycaprolactam, poly- decylene formamide, polyhexamethylene adipamide, polyhexamethylene sebacamide, gather sub- nonyl
Base urea, poly, makrolon, poly- 2,6- dimethyl p-phenylene, poly- [double (methylamino) phosphine nitriles], gather
At least one of dimethyl siloxane, celluloid fiber element, cellulose esters, poly(diphenyl ether sulfone).
3. preparation method as claimed in claim 1, it is characterised in that the photochromic dyes is by naphtho- spirooxazine, spiral shell pyrrole
Mutter the liquor-saturated class of class, diarylethene, azobenzene, fulgenic acid, aphthopyrans class, transition metal oxide, metal halide with
And any or any mix forms in rare earth compounding.
4. preparation method as claimed in claim 1, it is characterised in that the antioxidant is butylhydroxy anisole
(BHA), dibutyl hydroxy toluene (BHT), TBHQ (TBHQ), propylgallate (PG), ascorbic acid palm
Any one or several mixing in acid esters (AP), thiodipropionic acid dilauryl cinnamic acid ester (DLTP) and 4- hexyl resorcins (4-HR)
Thing.
5. preparation method as claimed in claim 1, it is characterised in that the ultra-violet absorber is salicylic acid esters, benzophenone
Phenyl salicylate, 2- (2 '-hydroxyls -5 '-methylbenzene in class, benzotriazole, group-substituted acrylonitrile, triazines and hindered amines
Base) BTA, 2,4-DihydroxyBenzophenone, ESCALOL 567,2- hydroxyl -4- n-octyloxies two
Benzophenone, 2- (2 '-hydroxyl -3 ', 5 '-two tertiary phenyl) -5- chlorinations BTA, single benzoic acid resorcinol, 2,2 '-it is thio
Double (4- t-octyl phenol epoxide) nickel, three (1,2,2,6,6- pempidine base) phosphite esters, 4- benzoyloxys -2,2,6,6- tetra-
Methyl piperidine, 2,4,6- tri- (2 '-n-butoxyphenyl)-at least one of 1,3,5-triazines and HMPA.
6. preparation method as claimed in claim 1, it is characterised in that the sensitizer is in aromatic series or aliphatic esters
The naphthoate of 1- hydroxyls -2, ethanedioic acid dibenzyl ester and at least one of benzylbiphenyl.
7. preparation method as claimed in claim 1, it is characterised in that the oil soluble material is isopentane, positive penta in alkanes
Alkane, petroleum ether, hexane, hexamethylene, isooctane, trimethylpentane, pentamethylene, heptane, dioxanes；Methylamine, two in alkane derivatives
Methylamine, 1,1- dichloromethane, 1,1,1- chloroform, nitromethane, chloroform, chlorotrifluoroethane, carbon tetrachloride, three chloroethenes
Alkene, ethylene dichloride, butyl chloride, DMF, DMA, N-METHYLFORMAMIDE, dimethyl methyl
Acid amides and dimethyl sulfoxide；Isopropanol, isobutanol, n-butanol, propyl ether, diethyl ether and phenol in alcohol and ether；Aldehyde and ketone；It is organic
Acid；Organic ester；Benzene includes one kind in benzene,toluene,xylene, paraxylene, meta-xylene, chlorobenzene, o-dichlorohenzene and aniline
Or several mixture.
8. preparation method as claimed in claim 1, it is characterised in that the emulsifying agent is selected from least one of following material：From
Polyacrylic acid, Sodium Polyacrylate, polyacrylamide and styrene in polymerization of carboxylic acid salt in sub- surfactant such as anionic
Copolymer-maleic anhydride sodium salt solution；Sodium alkyl benzene sulfonate such as neopelex, alkylsulfonate, aliphatic acid sulfoalkyl
Ester, sulfoalkyl acid amides, sulphosuccinates, alkylnaphthalene sulfonate such as nekal, the formaldehyde of alkylnaphthalene sulfonate
Condensation product, lignosulfonates, alkyl glyceryl ether sulfonate；Fatty alcohol sulfate salt and secondary alkyl sulphate such as dodecyl sulphur
Sour sodium；Phosphate ester salt；APES formaldehyde condensation products sulfat；Alkyl naphthalene sulfonic acid formaldehyde condensation products and its similarization
Compound；Phenol formaldehyde condensate sulfonate and its similar kind, phenol sulfonic acid naphthalene sulfonic acid-formaldehyde condensation product sodium salt, phenol formaldehyde condensate sulphur
Acid sodium-salt, phenol-melocol condensate sulfonates, contracting methylcellulose and its derivative, xanthan gum, in lignosulfonates
Desugar sodium lignin sulfonate M-9；Nonionic surfactant such as APES, higher alcohols aliphatic alcohol polyethenoxy
Ether, aliphatic amine polyoxyethylene ether and polyoxyethylene carboxylate.
9. preparation method as claimed in claim 1, it is characterised in that the assistant for emulsifying agent includes short chain alcohol or suitable HLB value
Nonionic surface active agent, alkylol such as n-butanol, isobutanol, n-amyl alcohol, isoamyl alcohol, ethanol, ethylene glycol, propane diols, third
At least one of triol, erythrol, xylitol, hexitol, twain series emulsifier and polyglycerol ester.
10. preparation method as claimed in claim 1, it is characterised in that：The amino resins is melamine resin, urea
At least one of urea formaldehyde, benzoguanamine resin；The etherified amino resins are methanol etherification amino resins, n-butanol ether
Change amino resins, isobutanol etherified amino resins are a kind of in the amino resins of ethanol etherified amino resins alkylol etherificate or appoint
Anticipate several mixtures.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711264272.2A CN107828407A (en) | 2017-11-30 | 2017-11-30 | A kind of discoloration micro-nano capsule of solid-state capsule-core and preparation method thereof |
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|---|---|---|---|
| CN201711264272.2A CN107828407A (en) | 2017-11-30 | 2017-11-30 | A kind of discoloration micro-nano capsule of solid-state capsule-core and preparation method thereof |
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| CN107828407A true CN107828407A (en) | 2018-03-23 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114029011A (en) * | 2021-10-25 | 2022-02-11 | 江苏视科新材料股份有限公司 | Preparation method of organic/inorganic nano composite microsphere visible light material |
| CN115041109A (en) * | 2022-05-30 | 2022-09-13 | 江南大学 | Silicon-based modified photochromic microcapsule and preparation method thereof |
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| CN1860167A (en) * | 2003-09-29 | 2006-11-08 | 西巴特殊化学品控股有限公司 | Stabilization of photochromic systems |
| CN101225296A (en) * | 2008-02-01 | 2008-07-23 | 北京服装学院 | Method for preparing photochromic micro-encapsulation |
| CN105797660A (en) * | 2016-04-18 | 2016-07-27 | 天津工业大学 | Method for preparing capsules from oil-soluble etherified amino resin |
| CN105964196A (en) * | 2016-06-02 | 2016-09-28 | 天津工业大学 | Composite ball containing self-assembly microcapsule and preparation method thereof |
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| CN1860167A (en) * | 2003-09-29 | 2006-11-08 | 西巴特殊化学品控股有限公司 | Stabilization of photochromic systems |
| CN101225296A (en) * | 2008-02-01 | 2008-07-23 | 北京服装学院 | Method for preparing photochromic micro-encapsulation |
| CN105797660A (en) * | 2016-04-18 | 2016-07-27 | 天津工业大学 | Method for preparing capsules from oil-soluble etherified amino resin |
| CN105964196A (en) * | 2016-06-02 | 2016-09-28 | 天津工业大学 | Composite ball containing self-assembly microcapsule and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114029011A (en) * | 2021-10-25 | 2022-02-11 | 江苏视科新材料股份有限公司 | Preparation method of organic/inorganic nano composite microsphere visible light material |
| CN114029011B (en) * | 2021-10-25 | 2023-07-25 | 江苏视科新材料股份有限公司 | Preparation method of organic/inorganic nano composite microsphere optomaterial |
| CN115041109A (en) * | 2022-05-30 | 2022-09-13 | 江南大学 | Silicon-based modified photochromic microcapsule and preparation method thereof |
| CN115041109B (en) * | 2022-05-30 | 2023-08-08 | 江南大学 | Silicon-based modified photochromic microcapsule and preparation method thereof |
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