CN110144734A - A kind of mosquito repellent and sunscreen complex function microcapsules and preparation method thereof - Google Patents
A kind of mosquito repellent and sunscreen complex function microcapsules and preparation method thereof Download PDFInfo
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- CN110144734A CN110144734A CN201910349823.8A CN201910349823A CN110144734A CN 110144734 A CN110144734 A CN 110144734A CN 201910349823 A CN201910349823 A CN 201910349823A CN 110144734 A CN110144734 A CN 110144734A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/152—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen having a hydroxy group bound to a carbon atom of a six-membered aromatic ring
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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Abstract
The present invention relates to a kind of mosquito repellent and sunscreen complex function microcapsules and preparation method thereof, complex function microcapsules include the capsule-core for loading the cyst wall of UV absorbing material and being wrapped in cyst wall；Wherein, UV absorbing material is lignin by acid separation, and capsule-core is the mixture of plant base culicifuge and ultraviolet absorber.The synergistic function between lignin and ultraviolet absorber can be effectively utilized in the present invention, also can achieve excellent ultraviolet protection function on the basis of realizing durable mosquito repellent.The complex function microcapsules possess important application value in the fields such as summer grade clothes and daily cosmetics.
Description
Technical field
The invention belongs to function microcapsules field, in particular to a kind of mosquito repellent and sunscreen complex function microcapsules and its preparation side
Method.
Background technique
Microcapsules technology promotes it to lead in weaving in the advantage that active material (such as plants essential oil) is protected and controlled in release
Domain is widely used, such as mosquito repellent, fragrance, uvioresistant and phase-change microcapsule, is prepared for a series of functions on this basis
Textile improves the added value of traditional textile.However, existing microcapsules are mostly simple function microcapsules, complex function
Preparing for microcapsules is relatively fewer.By taking pure cotton fabric as an example, the acquisition of complex function is generally required using two or more functions
Finishing agent carry out compounding arrangement or processed using more bath multistep processes techniques (such as: CN109440449A and
CN104842594A).The exploitation of complex function microcapsules then can simplify the process flow of complex function textile with application, drop
Low-resource loss.
The enhancing of the wildness and ultraviolet radioactive of summer mosquito proposes the requirement of mosquito repellent and uvioresistant to summer grade clothes, designs
Synthesizing mosquito repellent and sunscreen complex function microcapsules has theory significance and practical value for the exploitation of summer grade function textile, at present
The related patents that there is no the complex function microcapsules to prepare.Synthesis culicifuge is because having the characteristics that the mosquito repellents such as quick, efficient and lasting
And the long-time service be used widely, but synthesize culicifuge also results in drug resistance, environmental pollution and the potential poison of mosquito
Property.Therefore, plant base culicifuge obtains the pass of researcher because of its safety, environment friendly and comparable repelling effect
Note, in common essential oil class culicifuge, citronella oil and lemon eucalyptus oil are the plants for obtaining US Gov Env Protection Agency and approving
Object base culicifuge (GNANKINE O etc., molecule magazine (Molecules), 2017,22 (10): 1-23；TAVARES M etc., it is international
Journal of Practical Pharmacy (International Journal of Pharmaceutics), 2018,539 (1-2): 190-209).So
And essential oil class culicifuge is generally existing volatile, and the problems such as to photo-thermal environment sensitive and not lasting mosquito repellent time, microcapsules technology
Application can then to efficiently solve such culicifuge volatile and compare sensitive issue to photo-thermal environment.
Sun-screening agent (or ultraviolet protective agent) mainly includes physical and chemical type, and wherein chemical type sun-screening agent has excellent
UV absorption effect, but their contacts with skin may cause different degrees of allergic reaction
(CN108066163A), using microcapsules technology by cladding get up the side effect that can reduce ultraviolet absorber to skin.It is existing
Having the sun-proof microcapsules prepared in technology to mostly use organic or inorganic high polymer greatly is wall material, to one or more ultraviolet absorbers
It is coated to obtain (CN103469605B, CN108066163A, CN103013180B and CN103169625B).These are sun-proof micro-
The sun-proof function of capsule can only realize that there is no ultraviolet shielded effects for wall material itself by the ultraviolet absorber being wrapped by, and
The emulsifier being added in microcapsules preparation process can partially remain in final product and generate to human body potentially hazardous.
Summary of the invention
An object of the present invention is to provide a kind of mosquito repellent and sunscreen complex function microcapsules and preparation method thereof, with solve because
The function of microcapsules is relatively single and is unable to satisfy disposable the problem of arranging the requirement for preparing multi-functional textile.
The second object of the present invention is to introduce UV absorbing material lignin in effect microcapsule wall, the wood in cyst wall is utilized
The synergistic function of ultraviolet absorber in quality and capsule-core assigns composite micro-capsule excellent ultraviolet protection function.
The present invention provides a kind of mosquito repellent and sunscreen complex function microcapsules, the complex function microcapsules include that load is ultraviolet
The cyst wall of absorbing material and the capsule-core being wrapped in cyst wall；Wherein, UV absorbing material is lignin by acid separation, and capsule-core is plant base
The mixture of culicifuge and ultraviolet absorber.
The cyst wall is organic polymer resin.
The organic polymer resin is the polyureas formed by hexamethylene diamine and isophorone diisocyanate through interfacial polymerization
Resin.
The plant base culicifuge is citronella oil or lemon eucalyptus oil；Ultraviolet absorber is 2- hydroxyl -4- n-octyloxy two
Benzophenone or ESCALOL 567.
The present invention also provides a kind of preparation methods of mosquito repellent and sunscreen complex function microcapsules, comprising:
(1) it weighs alkali lignin and lauryl sodium sulfate is scattered in deionized water and stirs evenly, by solution ph tune
To 11~12, filters, then solution ph is adjusted to 2~3, be uniformly mixing to obtain lignin by acid separation suspension；
(2) plant base culicifuge, ultraviolet absorber and isophorone diisocyanate are uniformly mixed as oily phase, will be walked
Suddenly the lignin by acid separation suspension dispersion that (1) obtains is used as water phase in deionized water, and oil is added in water phase and is emulsified, is obtained
To mosquito repellent and sunscreen lotion；
(3) hexamethylene diamine solution is added in the mosquito repellent and sunscreen lotion obtained to step (2), heating progress polymerization reaction obtains micro-
Capsule suspension liquid；It finally washs, filter, is dry, obtaining mosquito repellent and sunscreen complex function microcapsules.
The mass concentration of alkali lignin in the step (1) is 2%~4%；The mass concentration of lauryl sodium sulfate
It is 0.2%~0.3%.
The dosage of plant base culicifuge in the step (2) is that core material (i.e. plant base culicifuge and ultraviolet absorber) is total
The 88%-98% of quality, the dosage of ultraviolet absorber are the 2%~12% of core material gross mass.
The mass ratio of isophorone diisocyanate and core material in the step (2) is 2:3~1:5.
The mass ratio of the material of hexamethylene diamine and isophorone diisocyanate in the step (3) is 1.1:1~1.3:1.
Mosquito repellent and sunscreen complex function microcapsules of the present invention be to load the carbamide resin of lignin by acid separation as cyst wall,
Using culicifuge and ultraviolet absorber as capsule-core, it is prepared by interfacial polymerization.In lignin and lauryl sodium sulfate
Mixed ammonium/alkali solutions in, due to phenolic hydroxyl group and carboxyl ionization generate electrostatic repulsion promote lignin macromolecular network structure to unfold
And it is soluble in water, under hydrophobic forces, Long carbon chain in lauryl sodium sulfate molecule and the lignin macromolecular to trail
Chain weave in forms compound micella.With the addition of hydrochloric acid, the phenolic hydroxyl group and carboxyl in lignin molecule structure are by matter
Sonization, the electrostatic repulsion between macromolecular skeleton weaken, the hydrophobic forces and Hyarogen-bonding between lignin macromolecular
Promote its macromolecular skeleton to shrink aggregation, lauryl sodium sulfate molecule is fixed in wooden cellulose aggregate.Due to dodecane
Base sodium sulphate still keeps complete ionization in low ph environment, and this guarantees the surfaces of lignin by acid separation particle with big
The negative electrical charge of amount ensure that the stability of lignin by acid separation suspension.Under high speed shear active force, above-mentioned oil is mutually dispersed into
Small drop, so that lignin by acid separation particle can at the interface formed between many oil phase drops and water phase in emulsification system
Rapidly to move on these new interfaces, and stable interfacial film is formed on the surface of oil droplet, lignin particles surface
Electrostatic repulsion between emulsion droplet caused by negative electrical charge further enhances emulsion intercalation method.When acidity is added in hexamethylene diamine
Lotion in, amino is positively charged in conjunction with proton, and under electrostatic attraction effect, hexamethylene diamine is migrated to oil-water interfaces, and and isocyanide
Sudden reaction occurs for acid esters, obtains complex function microcapsules.The ultraviolet absorber in lignin and capsule-core in cyst wall is mutually assisted
Together, reach uvioresistant effect of enhancing, at the same time, the plant base culicifuge slow release in capsule-core reaches lasting mosquito repellent
The effect of.
Beneficial effect
(1) function of driving mosquitoes and sun-screening function are combined the micro- glue for being prepared for having mosquito repellent and sunscreen complex function by the present invention
Capsule solves the problems, such as that the functionality of existing microcapsules is relatively single, and meets disposable arrangement and prepare multifunctional textile product
Requirement；
(2) present invention introduces UV absorbing material lignin in effect microcapsule wall, utilizes the lignin and capsule in cyst wall
The synergistic function of ultraviolet absorber in core can assign composite micro-capsule superior ultraviolet protection function.
(3) preparation method simple process of the present invention is easily-controllable, low in cost；Prepared complex function Microcapsules Size is equal
It is even, have many advantages, such as that repelling effect is lasting, UVResistant effect is excellent and stability is good, is led in summer grade clothes and household chemicals etc.
Domain possesses important application value.
Detailed description of the invention
Fig. 1 is the ultraviolet-visible absorption spectroscopy of various concentration lignin by acid separation suspension；
Fig. 2 is the optical microscope picture of mosquito repellent and sunscreen lotion in embodiment 1；
Fig. 3 is the electron scanning micrograph of mosquito repellent and sunscreen complex function microcapsules in embodiment 3；
Fig. 4 is the electron scanning micrograph of mosquito repellent and sunscreen complex function microcapsules in embodiment 4；
Fig. 5 is the grain size distribution of mosquito repellent and sunscreen complex function microcapsules in embodiment 6；
Fig. 6 is the grain size distribution of mosquito repellent and sunscreen complex function microcapsules in embodiment 9.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) preparation of lignin by acid separation
The lauryl sodium sulfate of the alkali lignin particle and 0.06g that weigh 0.6g is scattered in 30mL deionized water, is adopted
It is stirred evenly with magnetic stirring apparatus, solution ph is adjusted to 11 or so using the NaOH solution of 4mol/L, is removed by filtration not
Solution ph is adjusted to 2~3 using the hydrochloric acid of 1mol/L later by solubility impurity, is uniformly mixing to obtain lignin by acid separation suspension,
For use.
(2) preparation of mosquito repellent and sunscreen lotion
Take two isocyanide of isophorone of the citronella oil of 7.84g, the ESCALOL 567 of 0.16g and 2.52g
Acid esters is uniformly mixed, this is oily phase.Lignin by acid separation suspension in step (1) is distributed in 26mL deionized water, this is
Water phase.Oil is mutually slowly added into water phase, and acts on emulsified 10min in 10000r/min high speed shear, it is anti-to obtain mosquito repellent
Shine lotion.
(3) preparation of mosquito repellent and sunscreen complex function microcapsules
The mosquito repellent and sunscreen lotion prepared in step (2) is transferred in 35 DEG C of water bath with thermostatic control, be slowly added dropwise 7.4g oneself two
Amine aqueous solution, keeps the temperature 20min after being added dropwise, be warming up to 60 DEG C later, polymerization reaction 2h obtains microcapsule suspensions.To microcapsules
Suspension is washed, is filtered, and gained filter cake is placed in freeze drier dry for 24 hours up to the micro- glue of mosquito repellent and sunscreen complex function
Capsule.
In the complex function microcapsules, the clad ratio of citronella oil is 93.5%, after being arranged using complex function microcapsules
The UPF of pure cotton woven fabric (UPF of original cloth be 7.8) can achieve 104.
Embodiment 2
(1) preparation of lignin by acid separation
The lauryl sodium sulfate of the alkali lignin particle and 0.09g that weigh 1.2g is scattered in 30mL deionized water, is adopted
It is stirred evenly with magnetic stirring apparatus, solution ph is adjusted to 11 or so using the NaOH solution of 4mol/L, is removed by filtration not
Solution ph is adjusted to 2~3 using the hydrochloric acid of 1mol/L later by solubility impurity, is uniformly mixing to obtain lignin by acid separation suspension,
For use.
(2) preparation of mosquito repellent and sunscreen lotion
Take two isocyanide of isophorone of the citronella oil of 7.84g, the ESCALOL 567 of 0.16g and 2.52g
Acid esters is uniformly mixed, this is oily phase.Lignin by acid separation suspension in step (1) is distributed in 26mL deionized water, this is
Water phase.Oil is mutually slowly added into water phase, and acts on emulsified 10min in 10000r/min high speed shear, it is anti-to obtain mosquito repellent
Shine lotion.
(3) preparation of mosquito repellent and sunscreen complex function microcapsules
The mosquito repellent and sunscreen lotion prepared in step (2) is transferred in 35 DEG C of water bath with thermostatic control, be slowly added dropwise 7.4g oneself two
Amine aqueous solution, keeps the temperature 20min after being added dropwise, be warming up to 60 DEG C later, polymerization reaction 2h obtains microcapsule suspensions.To microcapsules
Suspension is washed, is filtered, and gained filter cake is placed in freeze drier dry for 24 hours up to the micro- glue of mosquito repellent and sunscreen complex function
Capsule.
In the complex function microcapsules, the clad ratio of citronella oil is 88.2%, after being arranged using complex function microcapsules
The UPF of pure cotton woven fabric (UPF of original cloth be 7.8) can achieve 93.
Embodiment 3
(1) preparation of lignin by acid separation
The lauryl sodium sulfate of the alkali lignin particle and 0.06g that weigh 0.6g is scattered in 30mL deionized water, is adopted
It is stirred evenly with magnetic stirring apparatus, solution ph is adjusted to 11 or so using the NaOH solution of 4mol/L, is removed by filtration not
Solution ph is adjusted to 2~3 using the hydrochloric acid of 1mol/L later by solubility impurity, is uniformly mixing to obtain lignin by acid separation suspension,
For use.
(2) preparation of mosquito repellent and sunscreen lotion
Take two isocyanide of isophorone of the citronella oil of 7.36g, the ESCALOL 567 of 0.64g and 2.52g
Acid esters is uniformly mixed, this is oily phase.Lignin by acid separation suspension in step (1) is distributed in 26mL deionized water, this is
Water phase.Oil is mutually slowly added into water phase, and acts on emulsified 10min in 10000r/min high speed shear, it is anti-to obtain mosquito repellent
Shine lotion.
(3) preparation of mosquito repellent and sunscreen complex function microcapsules
The mosquito repellent and sunscreen lotion prepared in step (2) is transferred in 35 DEG C of water bath with thermostatic control, be slowly added dropwise 7.4g oneself two
Amine aqueous solution, keeps the temperature 20min after being added dropwise, be warming up to 60 DEG C later, polymerization reaction 2h obtains microcapsule suspensions.To microcapsules
Suspension is washed, is filtered, and gained filter cake is placed in freeze drier dry for 24 hours up to the micro- glue of mosquito repellent and sunscreen complex function
Capsule.
From the figure 3, it may be seen that gained microcapsules, in spherical, wherein the clad ratio of citronella oil is 95.4%, micro- using complex function
The UPF of pure cotton woven fabric (UPF of original cloth is 7.8) after capsule arrangement can achieve 184.
Embodiment 4
(1) preparation of lignin by acid separation
The lauryl sodium sulfate of the alkali lignin particle and 0.06g that weigh 0.6g is scattered in 30mL deionized water, is adopted
It is stirred evenly with magnetic stirring apparatus, solution ph is adjusted to 11 or so using the NaOH solution of 4mol/L, is removed by filtration not
Solution ph is adjusted to 2~3 using the hydrochloric acid of 1mol/L later by solubility impurity, is uniformly mixing to obtain lignin by acid separation suspension,
For use.
(2) preparation of mosquito repellent and sunscreen lotion
Take the isophorone two of the lemon eucalyptus oil of 7.60g, the ESCALOL 567 of 0.40g and 2.52g
Isocyanates is uniformly mixed, this is oily phase.Lignin by acid separation suspension in step (1) is distributed in 26mL deionized water,
This is water phase.Oil is mutually slowly added into water phase, and acts on emulsified 10min in 10000r/min high speed shear, is driven
Mosquito ultra light sun block lotion.
(3) preparation of mosquito repellent and sunscreen complex function microcapsules
The mosquito repellent and sunscreen lotion prepared in step (2) is transferred in 35 DEG C of water bath with thermostatic control, be slowly added dropwise 7.4g oneself two
Amine aqueous solution, keeps the temperature 20min after being added dropwise, be warming up to 60 DEG C later, polymerization reaction 2h obtains microcapsule suspensions.To microcapsules
Suspension is washed, is filtered, and gained filter cake is placed in freeze drier dry for 24 hours up to the micro- glue of mosquito repellent and sunscreen complex function
Capsule.
As shown in Figure 4, gained microcapsules are in uniform spherical, and wherein the clad ratio of lemon eucalyptus oil is 94.6%, are used
The UPF of pure cotton woven fabric (UPF of original cloth is 7.8) after the arrangement of complex function microcapsules can achieve 126.
Embodiment 5
(1) preparation of lignin by acid separation
The lauryl sodium sulfate of the alkali lignin particle and 0.06g that weigh 0.6g is scattered in 30mL deionized water, is adopted
It is stirred evenly with magnetic stirring apparatus, solution ph is adjusted to 11 or so using the NaOH solution of 4mol/L, is removed by filtration not
Solution ph is adjusted to 2~3 using the hydrochloric acid of 1mol/L later by solubility impurity, is uniformly mixing to obtain lignin by acid separation suspension,
For use.
(2) preparation of mosquito repellent and sunscreen lotion
Take the isophorone two of the citronella oil of 7.84g, the 2-hydroxy-4-n-octoxybenzophenone of 0.16g and 2.52g different
Cyanate is uniformly mixed, this is oily phase.Lignin by acid separation suspension in step (1) is distributed in 26mL deionized water, this
For water phase.Oil is mutually slowly added into water phase, and acts on emulsified 10min in 10000r/min high speed shear, obtains mosquito repellent
Ultra light sun block lotion.
(3) preparation of mosquito repellent and sunscreen complex function microcapsules
The mosquito repellent and sunscreen lotion prepared in step (2) is transferred in 35 DEG C of water bath with thermostatic control, be slowly added dropwise 7.4g oneself two
Amine aqueous solution, keeps the temperature 20min after being added dropwise, be warming up to 60 DEG C later, polymerization reaction 2h obtains microcapsule suspensions.To microcapsules
Suspension is washed, is filtered, and gained filter cake is placed in freeze drier dry for 24 hours up to the micro- glue of mosquito repellent and sunscreen complex function
Capsule.
In the complex function microcapsules, the clad ratio of citronella oil is 96.2%, after being arranged using complex function microcapsules
The UPF of pure cotton woven fabric (UPF of original cloth be 7.8) can achieve 107.
Embodiment 6
(1) preparation of lignin by acid separation
The lauryl sodium sulfate of the alkali lignin particle and 0.06g that weigh 0.6g is scattered in 30mL deionized water, is adopted
It is stirred evenly with magnetic stirring apparatus, solution ph is adjusted to 11 or so using the NaOH solution of 4mol/L, is removed by filtration not
Solution ph is adjusted to 2~3 using the hydrochloric acid of 1mol/L later by solubility impurity, is uniformly mixing to obtain lignin by acid separation suspension,
For use.
(2) preparation of mosquito repellent and sunscreen lotion
Take the isophorone of the lemon eucalyptus oil of 7.60g, the 2-hydroxy-4-n-octoxybenzophenone of 0.40g and 2.52g
Diisocyanate is uniformly mixed, this is oily phase.Lignin by acid separation suspension in step (1) is distributed to 26mL deionized water
In, this is water phase.Oil is mutually slowly added into water phase, and acts on emulsified 10min in 10000r/min high speed shear, is obtained
Mosquito repellent and sunscreen lotion.
(3) preparation of mosquito repellent and sunscreen complex function microcapsules
The mosquito repellent and sunscreen lotion prepared in step (2) is transferred in 35 DEG C of water bath with thermostatic control, be slowly added dropwise 7.4g oneself two
Amine aqueous solution, keeps the temperature 20min after being added dropwise, be warming up to 60 DEG C later, polymerization reaction 2h obtains microcapsule suspensions.To microcapsules
Suspension is washed, is filtered, and gained filter cake is placed in freeze drier dry for 24 hours up to the micro- glue of mosquito repellent and sunscreen complex function
Capsule.
Gained microcapsules are in spherical, and as shown in Figure 5, the partial size of microcapsules is 8 μm or so, and the clad ratio of lemon eucalyptus oil is
95.4%, the UPF of the pure cotton woven fabric (UPF of original cloth for 7.8) after using complex function microcapsules to arrange can achieve 154.
Embodiment 7
(1) preparation of lignin by acid separation
The lauryl sodium sulfate of the alkali lignin particle and 0.06g that weigh 0.6g is scattered in 30mL deionized water, is adopted
It is stirred evenly with magnetic stirring apparatus, solution ph is adjusted to 11 or so using the NaOH solution of 4mol/L, is removed by filtration not
Solution ph is adjusted to 2~3 using the hydrochloric acid of 1mol/L later by solubility impurity, is uniformly mixing to obtain lignin by acid separation suspension,
For use.
(2) preparation of mosquito repellent and sunscreen lotion
Take two isocyanide of isophorone of the citronella oil of 7.04g, the ESCALOL 567 of 0.96g and 2.52g
Acid esters is uniformly mixed, this is oily phase.Lignin by acid separation suspension in step (1) is distributed in 26mL deionized water, this is
Water phase.Oil is mutually slowly added into water phase, and acts on emulsified 10min in 10000r/min high speed shear, it is anti-to obtain mosquito repellent
Shine lotion.
(3) preparation of mosquito repellent and sunscreen complex function microcapsules
The mosquito repellent and sunscreen lotion prepared in step (2) is transferred in 35 DEG C of water bath with thermostatic control, be slowly added dropwise 7.4g oneself two
Amine aqueous solution, keeps the temperature 20min after being added dropwise, be warming up to 60 DEG C later, polymerization reaction 2h obtains microcapsule suspensions.To microcapsules
Suspension is washed, is filtered, and gained filter cake is placed in freeze drier dry for 24 hours up to the micro- glue of mosquito repellent and sunscreen complex function
Capsule.
In the complex function microcapsules, the clad ratio of citronella oil is 90.2%, after being arranged using complex function microcapsules
The UPF of pure cotton woven fabric (UPF of original cloth be 7.8) can achieve 189.
Embodiment 8
(1) preparation of lignin by acid separation
The lauryl sodium sulfate of the alkali lignin particle and 0.06g that weigh 0.6g is scattered in 30mL deionized water, is adopted
It is stirred evenly with magnetic stirring apparatus, solution ph is adjusted to 11 or so using the NaOH solution of 4mol/L, is removed by filtration not
Solution ph is adjusted to 2~3 using the hydrochloric acid of 1mol/L later by solubility impurity, is uniformly mixing to obtain lignin by acid separation suspension,
For use.
(2) preparation of mosquito repellent and sunscreen lotion
Take the different Fo Er of the lemon eucalyptus oil of 11.76g, the 2-hydroxy-4-n-octoxybenzophenone of 0.24g and 2.52g
Ketone diisocyanate is uniformly mixed, this is oily phase.Lignin by acid separation suspension in step (1) is distributed to 26mL deionized water
In, this is water phase.Oil is mutually slowly added into water phase, and acts on emulsified 10min in 10000r/min high speed shear, is obtained
Mosquito repellent and sunscreen lotion.
(3) preparation of mosquito repellent and sunscreen complex function microcapsules
The mosquito repellent and sunscreen lotion prepared in step (2) is transferred in 35 DEG C of water bath with thermostatic control, be slowly added dropwise 7.4g oneself two
Amine aqueous solution, keeps the temperature 20min after being added dropwise, be warming up to 60 DEG C later, polymerization reaction 2h obtains microcapsule suspensions.To microcapsules
Suspension is washed, is filtered, and gained filter cake is placed in freeze drier dry for 24 hours up to the micro- glue of mosquito repellent and sunscreen complex function
Capsule.
In the complex function microcapsules, the clad ratio of lemon eucalyptus oil is 93.8%, whole using complex function microcapsules
The UPF of pure cotton woven fabric (UPF of original cloth is 7.8) after reason can achieve 133.
Embodiment 9
(1) preparation of lignin by acid separation
The lauryl sodium sulfate of the alkali lignin particle and 0.06g that weigh 0.6g is scattered in 30mL deionized water, is adopted
It is stirred evenly with magnetic stirring apparatus, solution ph is adjusted to 11 or so using the NaOH solution of 4mol/L, is removed by filtration not
Solution ph is adjusted to 2~3 using the hydrochloric acid of 1mol/L later by solubility impurity, is uniformly mixing to obtain lignin by acid separation suspension,
For use.
(2) preparation of mosquito repellent and sunscreen lotion
Take two isocyanide of isophorone of the citronella oil of 7.84g, the ESCALOL 567 of 0.16g and 4.76g
Acid esters is uniformly mixed, this is oily phase.Lignin by acid separation suspension in step (1) is distributed in 17mL deionized water, this is
Water phase.Oil is mutually slowly added into water phase, and acts on emulsified 10min in 10000r/min high speed shear, it is anti-to obtain mosquito repellent
Shine lotion.
(3) preparation of mosquito repellent and sunscreen complex function microcapsules
The mosquito repellent and sunscreen lotion prepared in step (2) is transferred in 35 DEG C of water bath with thermostatic control, be slowly added dropwise 16.4g oneself two
Amine aqueous solution, keeps the temperature 20min after being added dropwise, be warming up to 60 DEG C later, polymerization reaction 2h obtains microcapsule suspensions.To microcapsules
Suspension is washed, is filtered, and gained filter cake is placed in freeze drier dry for 24 hours up to the micro- glue of mosquito repellent and sunscreen complex function
Capsule.
Gained microcapsules are in spherical, it will be appreciated from fig. 6 that the partial size of microcapsules is 20 μm or so, the clad ratio of citronella oil is
91.6%, the UPF of the pure cotton woven fabric (UPF of original cloth for 7.8) after using complex function microcapsules to arrange can achieve 112.
As shown in Figure 1, lignin by acid separation has absorption in ultra-violet (UV) band, and absorption intensity increases with the increase of lignin dosage
By force.It is the clad ratio of culicifuge in mosquito repellent and sunscreen microcapsules prepared by emulsifier mostly 90% or more using lignin by acid separation, it can
To guarantee preferable repelling effect.
It replaces lignin by acid separation to prepare microcapsules using lauryl sodium sulfate by emulsifier, and it is adopted in a like fashion
It arranges on pure cotton woven fabric, the UPF value of fabric is 45 or so after arrangement, and uses lignin for emulsifier preparation in the present invention
Microcapsules arrange after the UPF value of pure cotton woven fabric can achieve 100 or more, show excellent UVResistant effect, here it is
Because of the result of the ultraviolet absorber synergy in the lignin and capsule-core in cyst wall.
Claims (9)
1. a kind of mosquito repellent and sunscreen complex function microcapsules, it is characterised in that: the complex function microcapsules include loading ultraviolet suction
The capsule-core receiving the cyst wall of material and being wrapped in cyst wall；Wherein, UV absorbing material is lignin by acid separation, and capsule-core is plant base drive
The mixture of mosquito agent and ultraviolet absorber.
2. a kind of mosquito repellent and sunscreen complex function microcapsules according to claim 1, it is characterised in that: the cyst wall is organic
Macromolecule resin.
3. a kind of mosquito repellent and sunscreen complex function microcapsules according to claim 2, it is characterised in that: the organic polymer
Resin is the carbamide resin formed by hexamethylene diamine and isophorone diisocyanate through interfacial polymerization.
4. a kind of mosquito repellent and sunscreen complex function microcapsules according to claim 1, it is characterised in that: the plant base mosquito repellent
Agent is citronella oil or lemon eucalyptus oil；Ultraviolet absorber is 2-hydroxy-4-n-octoxybenzophenone or 2- hydroxyl -4- methoxyl group
Benzophenone.
5. a kind of preparation method of mosquito repellent and sunscreen complex function microcapsules, comprising:
(1) it weighs alkali lignin and lauryl sodium sulfate is scattered in deionized water and stirs evenly, solution ph is adjusted to 11
~12, filtering, then solution ph is adjusted to 2~3, it is uniformly mixing to obtain lignin by acid separation suspension；
(2) plant base culicifuge, ultraviolet absorber and isophorone diisocyanate are uniformly mixed as oily phase, by step
(1) oil is added in water phase and emulsifies, obtain in deionized water as water phase by the lignin by acid separation suspension dispersion obtained
Mosquito repellent and sunscreen lotion；
(3) hexamethylene diamine solution is added in the mosquito repellent and sunscreen lotion obtained to step (2), heating carries out polymerization reaction and obtains microcapsules
Suspension；It finally washs, filter, is dry, obtaining mosquito repellent and sunscreen complex function microcapsules.
6. preparation method according to claim 5, it is characterised in that: the quality of the alkali lignin in the step (1) is dense
Degree is 2%~4%；The mass concentration of lauryl sodium sulfate is 0.2%~0.3%.
7. preparation method according to claim 5, it is characterised in that: the use of the plant base culicifuge in the step (2)
Amount is the 88%-98% of core material gross mass, and the dosage of ultraviolet absorber is the 2%~12% of core material gross mass.
8. preparation method according to claim 5, it is characterised in that: the isophorone diisocyanate in the step (2)
The mass ratio of ester and core material is 2:3~1:5.
9. preparation method according to claim 5, it is characterised in that: hexamethylene diamine and isophorone in the step (3)
The mass ratio of the material of diisocyanate is 1.1:1~1.3:1.
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