CN110468466A - A kind of fiber containing the removable active substance microcapsule of shell material - Google Patents
A kind of fiber containing the removable active substance microcapsule of shell material Download PDFInfo
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- CN110468466A CN110468466A CN201910760286.6A CN201910760286A CN110468466A CN 110468466 A CN110468466 A CN 110468466A CN 201910760286 A CN201910760286 A CN 201910760286A CN 110468466 A CN110468466 A CN 110468466A
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- Prior art keywords
- fiber
- shell material
- microcapsules
- active substance
- lotion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
Abstract
This application involves a kind of fiber containing the removable active substance microcapsule of shell material, the fiber contains the removable active substance microcapsule of shell material；Wherein the core material of the microcapsules includes active material；The shell material of the microcapsules includes removable material.The fiber containing the removable active substance microcapsule of shell material of the application, active material can be effectively protected in spinning and subsequent processing process, and the simple process economy, scrap build is small, is easy to produce in batches.
Description
Technical field
This application involves a kind of fibers containing the removable active substance microcapsule of shell material, are suitable for fibrous composite
Technical field.
Background technique
Since ancient times, people just excel at leveraging natural products very much, learn from the Nature.People constantly probe into, from plant
In object and animal tissue, effective active ingredient is extracted, and continually develop, has been suitable for production and life.On this basis,
With the progress of chemistry, biology, people also develop the chemical structure for imitating natural animal-plant extract, by artificial synthesized
Method, obtained the more excellent derivative of active material or even performance with similar effect and be also synthesized and develop
Come.
Fiber is one of most common, most widely used important foundation material.Meanwhile fibrous material is that splendid function carries
Body has various different function, if the functional fiber in terms of mechanics, optics, calorifics, electricity is in industrial production and daily life
Aspect plays the effect to become more and more important.The fibrous raw material of all kinds of active materials and for example various polymer solutions or melt is mixed
After conjunction, by spinneret, resolidification forming, this is to obtain one of important manufacturing process of functional fiber.But all kinds of activity
Substance is influenced vulnerable to physico chemical factors all kinds of in environment, and fiber fabrication process is often harsher, will lead to active material damage
Lose it is larger, or even completely loss and be unable to complete spinning.
During melt spinning, such as polyester fiber, spinning temperature is often as high as 300 DEG C, and spinning speed is fast, then
In addition vaccum dewatering process is stringenter.This just proposes requirement for the heat-resisting quantity of used active material.It is some
The more active active material of property is easy to happen volatilization, or even heated point such as the essence essential oil of plant extract under the high temperature conditions
Solution causes final retention amount in the fibre considerably less.And chemical reaction causes many difficulties there may be certain by-products.
Fiber production process is influenced, polyester molecule structure is such as caused to change, viscosity flow property changes, and spinneret is caused to block
Deng, or even can not spinning；Fiber product quality is influenced, if fiber broken end is more, strength is poor, and elongation is more low.Therefore,
How the polyester fiber containing this kind of active material, nylon or Fypro etc. obtained by melt-spinning technology, it is still fresh
It appears in the newspapers.The reliable batch production technique of such textile is obtained, is still relied at present to the fiber or containing the face of the fiber
Material, fabric etc. carry out final finishing.Postfinishing process just inevitably causes feel poor, and gas permeability is bad, durability and washable
The problems such as property is poor.
Chinese invention patent application 98115257.0 discloses the fiber containing Cedrus aroma ingredients and by this kind of fibre
Fabric obtained is tieed up, is immersed in natural fiber material by refining the essential oil containing deodar aromatised fraction that deodar obtains
In, to wish to obtain with strong insecticidal properties and there is the aroma therapeutic effect equivalent with Forest Bath.The essence of this method
It is by immersion fiber or fabric, active material to be made to enter the micro gap of fiber itself active material Cedarwood extract,
Or between fiber, in the micro gap between fabric.But it is protected since active material lacks, in further working process,
Such as sizing, dyeing and finishing, in water-washing process, it will greatly lost or destroyed.
Chinese invention patent application 201810589040.2 proposes a kind of based on supercritical CO2Fluid technique makes cellulose fiber
Tie up the processing method with whitening function.This method use is from resveratrol, the bright peaceful alkali of fructus piperis longi, pantolactone or tetrahydro methylpyrimidine
Cellulose is first swollen by the whitening medicaments such as carboxylic acid as active material, then supercritical CO2Cellulose fiber is brought in drug dissolution into
Dimension, whitening medicaments rest on inside cellulose fibre in unformed area after pressure release.The invention active material is not protected, and is spun
It will receive seriously affecting for soda acid, and easily leak or loss in following process, storage and use during silk.
Chinese utility model application 201020287481.6 discloses a kind of insect-preventing mosquito-expellant fiber of core-sheath composite structure, skin
Layer is PET, and pyrethroids pest repellant and PP, which are blended, is used as sandwich layer.However, about 180 DEG C of PP melting temperature, spinning temperature is 220 DEG C, should
Pest repellant will thermally decompose in the blending stage, cause the retention ratio of blended slice active material pest repellant extremely low or manufacture
Efficiency is extremely low and cost is high.And 300 DEG C are up into core-sheath spinning stage PET spinning temperature, active material pest repellant
It will further decompose.It can be seen that technology controlling and process is very difficult, active material loss late therein will be very high, or even can make fibre
Dimension loses functionality.
To avoid high temperature from influencing, also someone attempts wet spinning technology.Such as Chinese invention patent application
2009100115145.8 disclose a kind of preparation method of mosquito and insect expelling viscose, are by the way that mosquito and insect expelling agent to be configured to
Solution in the alkali cellulose after being added to yellow, makes it sufficiently dissolve, mix, and mosquito and insect expelling viscose is made.But viscose glue
Spinning solution is to work under high alkalinity environment, and coagulating bath is peracidity.As the oil of Cymbopogon winterianus of active material, be containing
Easily with acid or alkali the chemical reactions such as esterification, hydrolysis occur for the mixture of the groups such as a large amount of alcohol, aldehyde, ketone, phenol, so as to cause spinning
Yarn quality decline, as yield is not high, the decline of fiber mechanics intensity；And since disclosed method is yellow again by active matter Macrodilution
Change and be modified, has had a greatly reduced quality for Anti-mosquito disinsectization effect；Pulp curing even occurs substantially to accelerate, block spinneret, causes
It can not spinning.
In order to solve this problem, there has been proposed microcapsules technologies.Chinese invention patent application 201710334526.7
Propose a kind of mosquito repellent nylon-6 fiber and preparation method thereof.This method proposes that first going out lemongrass, wormwood etc. from plant extract extracts
Object, then capsule is made in extract, then capsule is handled to obtain mosquito repellent slice with attapulgite, a kind of drive is obtained through melt spinning
Mosquito nylon fibre.However this method does not disclose the partial size of the microcapsules, the technological parameters such as spinning temperature.According to its capsule wall
Material is Arabic gum and gelatin, and in conjunction with current existing research document, such capsule grain diameter is often larger (tens of to arrive hundreds of microns),
It will cause serious spinning plate blocking for spinning；And the temperature tolerance of such capsule does not refer to, but according to the temperature of extrusion spinning
300 DEG C of suppositions, still will cause active material in capsule and seriously affect.More importantly how core material active material discharges,
Corresponding technique could not be provided by how playing effect.
Chinese invention patent application 201310449590.1 provides a kind of nano controlled-release aromatic micro-capsule cellulose fibre
And its production method, the additional amount of this method nano controlled-release aromatic micro-capsule are the 0.1-15% of cellulose sulfonate solution, system
At nanometer fragrant microcapsules cellulose sulfonate spinning solution.The patent proposes the spinning techniques that active material is encapsulated, but
For microcapsules critical process, such as the selection of wall material, specific size controlling etc. is not referred to.
Chinese invention patent application 201811474226.X proposes a kind of regenerated cellulose containing ceramide microcapsules
Ceramide is prepared into microcapsules using microcapsule coated technology by fiber and preparation method thereof, then microcapsules is added to viscous
It is prepared in glue spinning solution with skin care moisturizing viscose rayon.The technical solution is using gelatin as wall material, glycerol and ceramide
As core material, although providing microcapsules safeguard measure for active material, its spinning process is effectively carried out；But also it neglects
In use process depending on fiber, active material can not effectively play a role due to being isolated always.
It can be seen that active material is more active from above-mentioned example, in the high temperature and pressure that spinning and post-processing are handled, acid,
Under the action of the inorganic agents such as alkali, easily it is lost.And by the methods of microcapsules, after active material is protected, although can
To guarantee to be protected in spinning and post-processing processing, but in the use process that processing is completed, active material is again by micro- glue
Cyst wall material and the external world keep apart, and it is due can not to play the role of expection.
In summary, in the prior art without occurring for removable shell material being used for the precedent of functional fibre.
Summary of the invention
Present applicant proposes a kind of fiber containing the removable active substance microcapsule of shell material, active material therein exists
It can be effectively protected in spinning and subsequent processing process, and can be released effectively active material after the completion of spinning,
The simple process economy, scrap build is small, is easy to produce in batches.
According to a kind of fiber containing the removable active substance microcapsule of shell material of the application, the fiber contains shell material
Removable microcapsules；Wherein the core material of the microcapsules includes active material；The shell material of the microcapsules includes that can remove material
Material.
Preferably, preparation method the following steps are included:
A. it is added in continuous phase using active material as dispersion and obtains lotion；Wherein, in lotion at least 90% dispersion
Jing≤2.50 micron phase Li；
B. the shell material or shell material prepolymer of above-mentioned emulsion will be added to solidify at the oil-water interfaces in lotion, obtain described
Active substance microcapsule；Wherein, the shell material or the quality of shell material performed polymer are the 0.05%- of quality of the emulsion described in step A
50.00%；
C. by active substance microcapsule obtained by step B and spinning polymer or polymer solution spun, dispersion liquid is formed,
It is 0.10%-45.00% that middle active substance microcapsule, which accounts for spinning polymer mass fraction,；
D. dispersion liquid described in step C is extruded from spinneret orifice and forms thread, fiber is made through solidification or solvent volatilization；
E. by fiber obtained by step D or containing the product of the fiber, use can dissolve the shell material but not dissolve described
The washing of the cleaning solution of core material and fiber, the shell material of the microcapsules is partly or entirely removed.
Alternatively, preparation method the following steps are included:
A. it is added in continuous phase using active material as dispersion and obtains lotion；In the dispersed phase or the continuous phase
Shell material or shell material prepolymer is added, or shell material or shell material prepolymer are added during forming the lotion；Wherein, lotion
In at least 90% Jing≤2.50 micron dispersed phase Li, the quality of the shell material or shell material performed polymer is quality of the emulsion
0.05%-50.00%；
B. solidify at the oil-water interfaces by shell material or shell material prepolymer in lotion, obtain the micro- glue of active material
Capsule；
C. by active substance microcapsule obtained by step B and spinning polymer or polymer solution spun, dispersion liquid is formed,
It is 0.10%-45.00% that middle active substance microcapsule, which accounts for spinning polymer mass fraction,；
D. dispersion liquid described in step C is extruded from spinneret orifice and forms thread, fiber is made through solidification or solvent volatilization；
E. by fiber obtained by step D or containing the product of the fiber, use can dissolve the shell material but not dissolve described
The washing of the cleaning solution of core material and fiber, the shell material of the microcapsules is partly or entirely removed.
Preferably, forming the lotion uses the hydrolysis salt for containing maleic groups copolymer or copolymer as surface
Activating agent, wherein the hydrolysis salt of maleic groups copolymer or copolymer accounts for copolymer quality ratio not less than 25%, including second
Alkene-copolymer-maleic anhydride, styrene-maleic anhydride copolymer, fatty alkene-copolymer-maleic anhydride or above-mentioned copolymer water
Solve salt.
Preferably, the active material is the extract or imitation natural extract chemical structure of natural plants or animal
Synthetic material and its derivative.Preferably, the active material include flavors and fragrances, mosquito-repellent, octyl salicylate, bar
In pine 1789, Octocrylene, benzophenone-3, the different monooctyl ester of methoxy cinnamic acid, vitamins oil, anti-tumor drug or whitening medicaments
It is at least one.
Preferably, the removable material is soluble in water, nonoxidizing diluted acid (for example, dilute sulfuric acid, dilute hydrochloric acid etc.)
Or paraffin, metal oxide, hydroxide, carbonate, polyvinyl alcohol, water soluble starch, the inorganic oxide of ketone benzene aquatic solution
Or at least one of linear polystyrene.
The application's has the beneficial effect that:
1, for the deficiency of current fibre, a kind of fiber containing the removable active substance microcapsule of shell material is provided.
The shell material of microcapsules makes active material that can be effectively protected in spinning and subsequent processing process, and in fiber and
It is functional significant in the use process of its product；
2, technical scheme use scope is extensive, is not only suitable for wet spinning, is also applied for melt spinning, can subtract
Few process procedure energy consumption, promotes economic benefit；
3, this application provides a kind of removable complex function microcapsules of shell material, while providing a kind of removal of shell material
Technique；The simple process economy, scrap build is small, and degree of cooperation is high, is easy to produce in batches.
4, the shell material that technical scheme provides removes scheme, compared to traditional handicraft, due to going for microcapsules shell material
It removes, so that active material accounting improves, provides a kind of active material fiber of higher amount higher performance.
Detailed description of the invention
Fig. 1 is the particle diameter distribution test curve of the mosquito repellent microcapsules prepared in embodiment 1.
Fig. 2 is the electron scanning micrograph of prepared viscose rayon cross section.
Fig. 3 is that the shell material prepared in embodiment 2 can remove the partial size test curve of Peppermint essential oil microcapsules.
Fig. 4 is the electron scanning micrograph of prepared Lyocell fibers cross section.
Fig. 5 is the scanning electron microscopic picture that prepared shell material can remove Peppermint essential oil microcapsules.
Fig. 6 is the scanning electron microscope that prepared shell material can remove that Peppermint essential oil microcapsules were washed through 1 hour ketone benzene aquatic solution
Picture.
Fig. 7 is the grading curve of microcapsules obtained by step B in embodiment 3.
Specific embodiment
It, hereinafter will be to embodiments herein for the purposes, technical schemes and advantages of the application are more clearly understood
It is described in detail.It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can
With mutual any combination.
The application proposes a kind of functional fibre that economy is succinct, is specifically to provide one kind and contains the removable active matter of shell material
The fiber of matter microcapsules.Contain active material in the fiber of the application, these provide the active material of functions in spinning and subsequent
It can be effectively protected in processing operation without losing, and functional aobvious in the use process of fiber and its products
It writes.
According to a kind of fiber containing the removable active substance microcapsule of shell material of the application, the fiber contains shell material
Removable active substance microcapsule；Wherein the core material of the microcapsules includes active material；The shell material of the microcapsules includes
Removable material.
Embodiment 1
A kind of viscose rayon containing removable shell material mosquito repellent microcapsules, preparation process are as follows:
A. using oil of Cymbopogon winterianus as dispersed phase, deionized water is continuous phase, it is warming up to 40 DEG C, is with molecular weight Mn
The ethylene maleic acid anhydride copolymer (wherein maleic anhydride mass fraction is 35%-78%) of 25000-95000 is used as surface-active
Agent obtains dispersion liquid emulsion；Wherein, dispersed phase and the mass ratio of continuous phase are 0.1-1.1, and emulsion particle diameter D90≤1.230 are micro-
Rice；
B. styrene is added into lotion described in step A, then be added initiator benzoyl peroxide, be warming up to 55 DEG C-
70 DEG C, 2.5-5 hours are kept the temperature, a kind of suspension of removable shell material mosquito repellent microcapsules is obtained；Wherein, the quality of the styrene
It is the 5.00%-50.00% of quality of the emulsion obtained by step A；
C. active substance microcapsule obtained by step B and viscose glue pulp are uniformly mixed, as spinning dispersion liquid, wherein driving
The quality of mosquito microcapsules is the 5%-45.00% of cellulose quality in viscose glue pulp；Viscose glue pulp in the application can be example
Such as by the raw material of cellulose (such as trees, fiber crops, bamboo plant) such as 90 DEG C or so high temperature, 6%-15% soda bath
Middle dissolution is made, and this pulp can be used to spinning, papermaking etc., belong to any technique commonly known term；
D. dispersion liquid described in step C is extruded from spinneret orifice and forms thread, fiber is made through acid bath solidification；
E. fiber obtained by step D or the product containing the fiber are washed using 40 DEG C -50 DEG C of ketone benzene aquatic solution, by institute
The shell material for stating composite micro-capsule partly or entirely removes to get fine to a kind of viscose glue for having both antibacterial functions and phase-changing and temperature-regulating function
Dimension；In the ketone benzene aquatic solution, butanone and toluene mass ratio 0.05-1.0, the total mass fraction that the two accounts for ketone benzene aquatic solution are
3.50%-6.00%.
As shown in Figure 1, being the particle diameter distribution test curve of prepared mosquito repellent microcapsules, partial size D50 is 0.821 micro-
Rice, D90 are 1.230 microns.As shown in Fig. 2, being the electron scanning micrograph of prepared viscose rayon cross section, it is seen that fine
Pore size on dimension cross section is about to meet between 1 micron to 2 microns with Microcapsules Size distribution.
Oil of Cymbopogon winterianus has excellent repelling effect, and effective component is citronellal, terpinol, terpinene etc. and its derives
Object, such as alcohol, ketone.Such physical property is active, and readily volatilized.Conventional method will lead to oil of Cymbopogon winterianus in product fiber and stay
It is extremely low to deposit rate, loss greatly, leads to product fiber functionality almost without that or even can not carry out effective spinning to this substance.
The application gives effective solution to this problem.
By the ketone benzene aquatic solution that gained viscose rayon mass fraction is 4.5% in the present embodiment, after washing different time,
According to reference GB/T 13917.9-2009 " the 9th part of agriculture chemical registration hygienic insecticide indoor pharmacodynamic test and evaluation: repellant "
With GB/T 30126-2013 " detection and evaluation of the mosquito-proof performance of textile " for trying insect: aedes albopictus (Aedes
Albopictus), the female insect experimental condition that do not suck blood for 3-5 days after emergence: temperature is 26 DEG C, and relative humidity 57% is surveyed
Its mosquito-proof performance, is summarized in the following table 1.
The viscose rayon synthesis of 1 embodiment 1 of table is tested
As shown in Table 1, sample S01 is the viscose rayon washed without ketone benzene aquatic solution, very to the repellent effect of mosquito
Difference, scattering ratio only 3.77%.Although being wrapped in capsule it can be seen that fiber S01 contains oil of Cymbopogon winterianus, can not play a role.
And sample S02, after washing in 60 minutes, as the shell material of partial capsules is removed, fiber shows certain synthesis,
Scattering ratio is 32.04%, is rated C grades；Sample S03 is the capsule shell material quilt after the washing of 180 minutes ketone benzene aquatic solutions
Further removal, the synthesis of fiber are further promoted, and scattering ratio rises to 52.83%, are had good repellent effect, are commented
Grade has reached B grades.The fiber and its products are processed in garment material, and the fields such as home textile articles, outdoor sports, health care have
Important application.
Embodiment 2
A kind of Lyocell fibers containing the removable Peppermint essential oil microcapsules of shell material, preparation process are as follows:
A. it using Peppermint essential oil as dispersed phase, adds styrene and forms dispersion liquid；Wherein, the quality of the styrene is
The 5.00%-45.00% of dispersion liquid quality；Mixed solvent (the wherein water of -3 butyl imidazole villaumite of water and ionic liquid 1- methyl
Amount is 15%, and ionic liquid is surplus) it is continuous phase, it is warming up to 40 DEG C, is the benzene second of 500-1500 with molecular weight Mn
Alkene-copolymer-maleic anhydride sodium salt hydrolysate (wherein maleic anhydride mass fraction is 15%-30%) is used as surfactant, obtains
To dispersion liquid emulsion；Wherein, dispersed phase and the mass ratio of continuous phase are 0.1-1.1, emulsion particle diameter D90≤2.396 micron；
B. crosslinking agent divinylbenzene is added into lotion described in step A, initiator benzoyl peroxide, heating is then added
To 65 DEG C -80 DEG C, 2.5-5 hours are kept the temperature, a kind of suspension of removable shell material Peppermint essential oil microcapsules is obtained；Wherein, described
The quality of crosslinking agent divinylbenzene is the 2.50%-15.00% of styrene quality；
C. cellulose is dissolved in -3 butyl imidazole villaumite of ionic liquid 1- methyl and forms cellulose ionic liquid solution, then
Complex function microcapsule suspensions obtained by step B and cellulose ionic liquid solution are uniformly mixed, spinning dispersion liquid is formed,
Wherein the quality of complex function microcapsules is the 15%-45.00% of cellulose quality
D. spinning dispersion liquid described in step C is extruded from spinneret orifice and forms thread, fibre is made through solvent volatilization solidification
Dimension；
E. it by fiber obtained by step D or containing the product of the fiber, is washed using 40 DEG C -50 DEG C of ketone benzene aquatic solutions, it will
The shell material part removal of the composite micro-capsule contains the Lay containing the removable Peppermint essential oil microcapsules of shell material to get to a kind of
Sai Er fiber；Wherein, in ketone benzene aquatic solution, the mass ratio of butanone and toluene is 1.0-2.5, gross mass shared by butanone and toluene
Score is 2.0%-4.0%.
As shown in figure 3, can remove the partial size test curve of Peppermint essential oil microcapsules, partial size D50 for prepared shell material
It is 1.505 microns, D90 is 2.396 microns.As shown in figure 4, being the scanning electron microscope of prepared Lyocell fibers cross section
Photo, it is seen that the pore size on fiber cross section is about several microns, is met with Microcapsules Size distribution.
As shown in figure 5, can remove the scanning electron microscopic picture of Peppermint essential oil microcapsules for prepared shell material.As shown in fig. 6,
It can remove the scanning electron microscopic picture that Peppermint essential oil microcapsules were washed through 1 hour ketone benzene aquatic solution for prepared shell material.As it can be seen that through
After crossing the washing of ketone benzene aquatic solution, there are some holes in the surface of microcapsules, and occurs between capsule a degree of viscous
Even, this declaratives shell material is removed.
The Lyocell fibers for present embodiments providing a kind of removable Peppermint essential oil microcapsules of shell material, pass through the application method
The shell material of microcapsules in removable fibrous, further increases the content of Peppermint essential oil in fiber.The Lyocell fibers and its product,
It is led in garment material processing, bedding manufacture, health care, electronic instrument, agricultural production, building material, device fabrication etc.
There is important application in domain.
In addition, this shell material prepolymer of styrene, this method quilt are just had been added in the present embodiment in dispersion liquid
Shell material prepolymer is added in interior phase (dispersed phase), becomes a part of interior phase by referred to as interior addition.Corresponding,
The Adding Way that prepolymer styrene is added in embodiment 1 in the lotion that step B is formed is referred to as outer addition.Two methods are equal
The purpose of the application may be implemented.
Embodiment 3
A kind of polyester fiber containing the removable Octocrylene microcapsules of shell material, technical solution are as follows:
A. using Octocrylene as dispersed phase, deionized water is continuous phase, it is warming up to 40 DEG C, is with molecular weight Mn
The ethylene maleic acid anhydride copolymer (wherein maleic anhydride mass fraction is 55%-78%) of 25000-45000 is used as surface-active
Agent obtains lotion；Wherein, dispersed phase and the mass ratio of continuous phase are 0.1-1.1, emulsion particle diameter D90≤1.991 micron；
B. the CaCl that mass fraction is 8% is added into lotion described in step A2Then aqueous solution is slowly dripped into lotion
Adding mass fraction is 8% NaCO3Aqueous solution is slowly stirred 6 hours at 75 DEG C, is obtained using calcium carbonate as shell material, is contained resistanceization
Agent and phase-changing and temperature-regulating complex function microcapsule suspensions；Wherein, CaCl2Aqueous solution and NaCO3Aqueous solution mass ratio is 1:1, the two
Quality sum is the 5.00%-45.00% of quality of the emulsion obtained by step A, Bao Wen 2.5-5 hours, obtains a kind of removable shell material
Octocrylene microcapsules suspension, it is spray-dried to obtain microscapsule powder；
C. Octocrylene microscapsule powder obtained by step B and polyester pelletizing are uniformly mixed, are made through 270-310 DEG C of blending
Grain, obtains compound pelletizing, wherein the quality of Octocrylene microcapsules is the 5%-45.00% of polyester quality；
D. compound pelletizing described in step C is extruded from spinneret orifice and forms thread, fiber is made through cooled and solidified；
E. by fiber obtained by step D or containing the product of the fiber, the fiber is using 40 DEG C -50 DEG C of mass fraction
5% salt acid elution, the shell material of the composite micro-capsule is partly or entirely removed, by the shell material part of the microcapsules or entirely
Portion's removal is to get to a kind of viscose rayon for having both antibacterial functions and phase-changing and temperature-regulating function.
As shown in fig. 7, Microcapsules Size D90 is 1.991 microns for the grading curve of microcapsules obtained by step B.This
Microcapsules decomposition temperature described in embodiment is 344 DEG C, is higher than polyester melt spinning temperature, can be used for melt spinning.
Octocrylene is a kind of efficient sun-screening agent and anti ultraviolet agent.Octocrylene microencapsulation is made it by the present embodiment
It avoids being destroyed in the high temperature harsh environment of melt spinning, while after the completion of spinning, microcapsules shell material can be removed or portion
Divide removal, to be released effectively.Microcapsules obtained by the present embodiment and fiber are in textile product, outdoor sports, health protection
There is important application in equal fields.
Embodiment 4
A kind of acrylic fiber of the removable Microencapsulated Phase Change Materials containing adriamycin of shell material, preparation process are as follows:
A. the adriamycin and tetradecyl alchohol that mass ratio is 0.01-1.0 are as dispersed phase, and deionized water is continuous phase, by it
40 DEG C are warming up to, is ethylene maleic acid anhydride copolymer (the wherein maleic anhydride mass fraction of 25000-40000 with molecular weight Mn
It is used as surfactant for 35%-78%), obtains lotion；Wherein, dispersed phase and the mass ratio of continuous phase are 0.1-1.1, lotion
Partial size D90≤2.230 micron；
B. styrene is added into lotion described in step A, then be added initiator benzoyl peroxide, be warming up to 55 DEG C-
70 DEG C, 2.5-5 hours are kept the temperature, a kind of suspension of removable shell material mosquito repellent microcapsules is obtained；Wherein, the quality of the styrene
It is the 5.00%-50.00% of quality of the emulsion obtained by step A；
C. the sodium sulfocyanate water for the polyacrylonitrile for being 25-55% by active substance microcapsule obtained by step B and mass fraction
Solution is uniformly mixed, and as spinning dispersion liquid, wherein the quality of complex function microcapsules is the 5%- of polyacrylonitrile quality
45.00%；
D. dispersion liquid described in step C is extruded from spinneret orifice and forms thread, solidify to obtain complex function through coagulating bath
Acrylic fiber；
E. it by fiber obtained by step D, is washed using 40 DEG C -50 DEG C of ketone benzene aquatic solutions, by the shell of the composite micro-capsule
Material, which partly or entirely removes, has both fire-retardant and phase-changing and temperature-regulating function acrylic fiber to get to a kind of described in the present embodiment；Ketone
In benzene aquatic solution, the mass ratio 0.5-2.0 of butanone and toluene, the total mass fraction that the two accounts for ketone benzene aquatic solution is 1.5%-
4.0%
Adriamycin is a kind of antitumor antibiotics, can inhibit the synthesis of RNA and DNA, most strong to the inhibiting effect of RNA, is resisted
Tumor spectrum is wider, has effect to kinds of tumors, belongs to cell cycle nonspecific agent (CCNSA), kill to the tumour cell of various growth cycles
The effect of going out.
Sodium thiocyanate solution used in acrylic spinning is intensive polar solvent, is easy to cause adverse effect to active material,
Flocculation or crystallization are such as generated, further spinning is interfered.By adriamycin microencapsulation in the present embodiment, solves the problems, such as this.
Tetradecyl alchohol is introduced in the present embodiment simultaneously, as phase-change material, can play the role of carrying out temperature adjusting to microenvironment.Association
It helps adriamycin to act on, suitable working environment is provided, improve drug effect.
The application can effectively solve the above problems, the fiber and its products, in health care, garment material processing, home textile
There is important application in the fields such as articles, bedding, jewelry, construction material, the manufacture of equipment instrument.
Embodiment 5
A kind of composite micro-capsule Lyocell fibers can remove facial treatment essence and phase-change material containing shell material, preparation process
Are as follows:
A. phase-change material selects n-tetradecane, and Radix Rhodiolae extract is added, forms it into W/O lotion i.e. Radix Rhodiolae extract
Dispersion liquid in the tetradecane；Wherein, the 5.00-45.00% that Radix Rhodiolae extract is opposite tetradecane mass fraction is added；
B. using dispersion liquid obtained by step A as dispersed phase, the N-methylmorpholine-N- oxide that mass fraction is 95% is water-soluble
Liquid is continuous phase, obtains double emulsion；Wherein, dispersed phase and the mass ratio of continuous phase are 0.1-1.2, emulsion particle diameter D90≤1.90
Micron；
C. styrene is added into lotion described in step B, then be added initiator benzoyl peroxide, be warming up to 55 DEG C-
70 DEG C, 2.5-5 hours are kept the temperature, a kind of suspension of removable shell material mosquito repellent microcapsules is obtained；Wherein, the quality of the styrene
It is the 5.00%-50.00% of dispersion liquid quality obtained by step A；
D. cellulose is dissolved in N-methylmorpholine-N- oxide, forms cellulose ionic liquid solution, then by step C institute
It obtains complex function microcapsules and cellulose ionic liquid solution is uniformly mixed, form spinning dispersion liquid, wherein complex function is micro-
The quality of capsule is the 15%-45.00% of cellulose quality；
E. the spinning dispersion liquid of the microcapsules containing complex function described in step D is extruded from spinneret orifice and forms thread, through molten
Agent volatilization solidifies and becomes fiber；
F. fiber described in step E is washed using 40 DEG C -50 DEG C of ketone benzene aquatic solution, by the shell material of the composite micro-capsule
Contain the Lyocell fibers containing the removable Peppermint essential oil microcapsules of shell material to get to a kind of in part；Wherein, ketone benzene aquatic solution
In, the mass ratio of butanone and toluene is 1.0-2.5, and total mass fraction shared by butanone and toluene is 2.0%-4.0%.Obtain
A kind of Lyocell fibers simultaneously containing Radix Rhodiolae extract with temperature adjustment function.
The scientific name of Radix Rhodiolae has the function of moisture-keeping nutrient wherein containing crude protein for Selaginella tamariscina.It can be used as medicine simultaneously, can control
Knife wound, traumatic injury, ulcer, stomachache, toothache, abscess of throat etc..But Radix Rhodiolae extract is highly soluble in water.And cellulose spinning
With will use a large amount of water in last handling process, this allows for retardant and inevitably largely loses.The addition of microcapsule wall material
It can play the role of that outside water is isolated to it, but in subsequent use process, such as fail to remove shell, its moisturizing will be made to seek
It supports or physiotheraping effect is had a greatly reduced quality.The application can effectively solve the above problems, the fiber and its products, in cosmetics, medical wave
The manufacture of case garment material, home textile articles, bedding, jewelry, construction material, equipment instrument etc., processing, transport, storage,
There is important application in the fields such as transport.
Embodiment 6
A kind of viscose rayon of the Vitamin E contained micro capsule containing removable shell material, preparation process are as follows:
A. 58# paraffin is warming up to 65 DEG C is completely melt it, it is uniformly mixed with vitamin E as dispersed phase (its
In, the quality that vitamin E is added is the 0.10-150.00% of 58# Quality of Paraffin Waxes；), deionized water is continuous phase, it is risen
Temperature is styrene-maleic anhydride copolymer sodium salt (the wherein maleic anhydride mass fraction of 500-5000 with molecular weight Mn to 65 DEG C
It is used as surfactant for 35%-78%), obtains lotion；Wherein, dispersed phase and the mass ratio of continuous phase are 0.1-1.3, lotion
Partial size D90≤2.110 micron；
B. above-mentioned emulsion is stirred evenly, is slow cooling to room temperature, cool and solidify 58# paraffin, formed shell material, obtain institute
The Vitamin E contained micro capsule suspension containing removable shell material stated；
C. Vitamin E contained micro capsule obtained by step B and viscose glue pulp are uniformly mixed, as spinning dispersion liquid, wherein institute
The quality for stating microcapsules is the 5%-45.00% of cellulose quality in viscose glue pulp；
D. the spinning dispersion liquid described in step C containing Vitamin E contained micro capsule is extruded from spinneret orifice and forms thread, through acid bath
It solidifies and becomes fiber；
E. using 60 DEG C -80 DEG C of water washing, the shell material of the microcapsules is part or all of by fiber described in step D
It removes to get a kind of viscose rayon of Vitamin E contained micro capsule containing removable shell material is arrived.
In the present embodiment, thermo-sensitive material 58# paraffin can be used as phase-change material presence, also plays package protection and lives
The effect of property Vitamins E.In health care or beauty, when such as hot compress Ankang thermotherapy, phase-change material can play adjusting temperature
The effect of degree extends physiotheraping effect, helps preferably to play drug effect.
Embodiment 7
A kind of viscose rayon containing the removable function of driving mosquitoes of shell material, technical solution are as follows:
Culicifuge in step A is replaced with to artificial synthesized culicifuge DEET (Metadelphene), remaining is the same as embodiment 1.
Gained Microcapsules Size D90 is 2.03 microns, and gained fiber or fabric, can after washing in ketone benzene aquatic solution 3 hours
Obtain the excellent repelling effect of scattering ratio 73.2%, the mosquito repellent viscose rayon that mosquito repellent level ratings are A grades.
Embodiment 8
A kind of acrylic fiber containing the removable whitening function microcapsules of shell material, technical solution are as follows:
Adriamycin in step A and tetradecyl alchohol are replaced with into whitening medicaments resveratrol, remaining is the same as embodiment 4.
Gained Microcapsules Size D90 is 2.26 microns, and gained fiber or fabric can be had after the washing of ketone benzene aquatic solution
There is the acrylic fiber of release whitening medicaments resveratrol effect.
Embodiment 9
A kind of Lyocell fibers containing shell material removable Rosa Damascana and Lavender essential oil microcapsule, preparation process
Are as follows:
Peppermint essential oil in step A is replaced with the composite essential oil containing Rosa Damascana, Lavender (Rosa Damascana and to smoke
Clothing grass essential oil mass ratio 1:1), remaining is the same as embodiment 2.Fiber is washed using 40 DEG C -50 DEG C of ketone benzene aquatic solution, it will be described micro-
The shell material part removal of capsule contains energy sustained release rose scent and lavender Lyocell fibers to get to a kind of.
Although embodiment disclosed by the application is as above, the content is only to facilitate understanding the application and adopting
Embodiment is not limited to the application.Technical staff in any the application technical field is not departing from this
Under the premise of the disclosed spirit and scope of application, any modification and change can be made in the implementing form and in details,
But the scope of patent protection of the application, still should be subject to the scope of the claims as defined in the appended claims.
Claims (8)
1. a kind of fiber containing the removable active substance microcapsule of shell material, which is characterized in that the fiber contains shell material can
The active substance microcapsule of removal；Wherein the core material of the microcapsules includes active material；The shell material of the microcapsules includes can
Remove material.
2. the fiber of active substance microcapsule according to claim 1, which is characterized in that preparation method includes following step
It is rapid:
A. it is added in continuous phase using active material as dispersion and obtains lotion；Wherein, in lotion at least 90% dispersed phase grain
Jing≤2.50 micron；
B. the shell material or shell material prepolymer of above-mentioned emulsion will be added to solidify at the oil-water interfaces in lotion, obtain the activity
Substance microcapsules；Wherein, the shell material or the quality of shell material performed polymer are the 0.05%- of quality of the emulsion described in step A
50.00%；
C. by active substance microcapsule obtained by step B and spinning polymer or polymer solution spun, dispersion liquid is formed, wherein living
Property substance microcapsules account for spinning polymer mass fraction be 0.10%-45.00%；
D. dispersion liquid described in step C is extruded from spinneret orifice and forms thread, fiber is made through solidification or solvent volatilization；
E. by fiber obtained by step D or containing the product of the fiber, use can dissolve the shell material but not dissolve the core material
It is washed with the cleaning solution of fiber, the shell material of the microcapsules is partly or entirely removed.
3. the fiber of active substance microcapsule according to claim 1, which is characterized in that preparation method includes following step
It is rapid:
A. it is added in continuous phase using active material as dispersion and obtains lotion；It is added in the dispersed phase or the continuous phase
Lotion is formed after shell material or shell material prepolymer, or shell material or shell material prepolymer are added during forming the lotion；Its
In, the quality of at least 90% Jing≤2.50 micron dispersed phase Li in lotion, the shell material or shell material performed polymer is quality of the emulsion
0.05%-50.00%；
B. solidify at the oil-water interfaces by shell material or shell material prepolymer in lotion, obtain the active substance microcapsule；
C. by active substance microcapsule obtained by step B and spinning polymer or polymer solution spun, dispersion liquid is formed, wherein living
Property substance microcapsules account for spinning polymer mass fraction be 0.10%-45.00%；
D. dispersion liquid described in step C is extruded from spinneret orifice and forms thread, fiber is made through solidification or solvent volatilization；
E. by fiber obtained by step D or containing the product of the fiber, use can dissolve the shell material but not dissolve the core material
It is washed with the cleaning solution of fiber, the shell material of the microcapsules is partly or entirely removed.
4. the fiber of active substance microcapsule according to any one of claim 1-3, which is characterized in that form the cream
Liquid uses the hydrolysis salt for containing maleic groups copolymer or copolymer as surfactant, and wherein maleic groups are total
The hydrolysis salt of polymers or copolymer accounts for copolymer quality ratio not less than 25%.
5. the fiber of active substance microcapsule according to any one of claim 1-3, which is characterized in that the active matter
Matter is the extract of natural plants or animal or synthetic material and its derivative for imitating natural extract chemical structure.
6. the fiber of active substance microcapsule according to any one of claim 1-3, which is characterized in that the active matter
Matter includes flavors and fragrances, mosquito-repellent, octyl salicylate, bassoon 1789, Octocrylene, benzophenone-3, methoxy cinnamic acid
At least one of different monooctyl ester, vitamins oil, anti-tumor drug or whitening medicaments.
7. the fiber of complex function microcapsules according to any one of claim 1-3, which is characterized in that described to can remove
Material is soluble in water, the paraffin of nonoxidizing diluted acid or ketone benzene aquatic solution, metal oxide, hydroxide, carbonate, gathers
At least one of vinyl alcohol, water soluble starch, inorganic oxide or linear polystyrene.
8. the fiber of complex function microcapsules according to claim 4, which is characterized in that the maleic groups copolymerization
The hydrolysis salt of object or copolymer includes ethylene maleic acid anhydride copolymer, styrene-maleic anhydride copolymer, fatty alkene-maleic acid
The hydrolysis salt of anhydride copolymer or above-mentioned copolymer.
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| CN201910760286.6A CN110468466A (en) | 2019-08-16 | 2019-08-16 | A kind of fiber containing the removable active substance microcapsule of shell material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094419A (en) * | 2020-09-16 | 2020-12-18 | 青岛迦南美地家居用品有限公司 | Hyaluronic acid microcapsule, fiber containing hyaluronic acid microcapsule, preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103981588A (en) * | 2014-06-09 | 2014-08-13 | 青岛嘉胜隆贸易有限公司 | Antibacterial and deodorization cellulosic fiber and preparation method thereof |
| CN110004510A (en) * | 2019-04-25 | 2019-07-12 | 希肤科技（上海）有限公司 | A kind of preparation process of jade viscose rayon and mask substrate |
| CN110359108A (en) * | 2019-08-05 | 2019-10-22 | 北京宇田相变储能科技有限公司 | A kind of functional fiber cellulose fiber and the preparation method and application thereof |
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2019
- 2019-08-16 CN CN201910760286.6A patent/CN110468466A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103981588A (en) * | 2014-06-09 | 2014-08-13 | 青岛嘉胜隆贸易有限公司 | Antibacterial and deodorization cellulosic fiber and preparation method thereof |
| CN110004510A (en) * | 2019-04-25 | 2019-07-12 | 希肤科技（上海）有限公司 | A kind of preparation process of jade viscose rayon and mask substrate |
| CN110359108A (en) * | 2019-08-05 | 2019-10-22 | 北京宇田相变储能科技有限公司 | A kind of functional fiber cellulose fiber and the preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112094419A (en) * | 2020-09-16 | 2020-12-18 | 青岛迦南美地家居用品有限公司 | Hyaluronic acid microcapsule, fiber containing hyaluronic acid microcapsule, preparation method and application |
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Effective date of registration: 20210312 Address after: Room 101, building 4, 1788 Mozitan Road, high tech Zone, Hefei City, Anhui Province, 230011 Applicant after: Hefei Xinneng phase change new material technology Co.,Ltd. Address before: 201900 Room 302, No.17, Lane 188, Jufengyuan Road, Dachang Town, Baoshan District, Shanghai Applicant before: Shanghai Xinya New Material Technology Co.,Ltd. |
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Application publication date: 20191119 |