CN104532596B - A kind of Oleum Cinnamomi microcapsule fabric finishing liquid and its preparation method and application - Google Patents
A kind of Oleum Cinnamomi microcapsule fabric finishing liquid and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to Micro-Encapsulation Technique and textile technology field, disclose a kind of Oleum Cinnamomi microcapsule fabric finishing liquid, its preparation method and fabric finishing method.With chitosan quaternary ammonium salt and arabic gum for wall material, Oleum Cinnamomi is core, uses complex coacervation to prepare Oleum Cinnamomi microcapsule emulsion.Obtained microcapsule emulsion compounds with wrinkle resistant cross-linking agent, catalyst, penetrating agent and obtains Oleum Cinnamomi microcapsule fabric finishing agent, its component is as follows: Oleum Cinnamomi microcapsule 15～30%, wrinkle resistant cross-linking agent 6～12%, catalyst 2～3.5%, penetrating agent 0.5～2% and excess water.Using chemical crosslink technique that fabric is carried out Multifunctional finishing, microcapsule, as bridge, is cross-linked by chemical bond by cross-linking agent with fabric, and the fabric after arrangement has more preferable wash durability, more longlasting antibiotic health care and crease resistant functions.
Description
Technical field
The invention belongs to Micro-Encapsulation Technique and textile technology field, be specifically related to a kind of Oleum Cinnamomi microcapsule textile whole
Reason agent and its preparation method and application.
Background technology
Textile is requisite articles for use during people live, but, all kinds of textiles are noxious bacteria, fungus, virus
Etc. microbial growth procreation and the suitable place of propagation, pathogenic bacterium multiply the most in a large number and fibre not only can be made to become
Color, mouldy, degraded, more can be spread disease by indirectly mode, human lives is caused harm.Along with health of people keeps healthy
The enhancing day by day of consciousness, the demand of people's textile to having antibacterial functions is more and more urgent, therefore, to antibacterial fabric
Research, exploitation tool are of great significance.
In antibacterial textile industry, a lot of antibiotic substance have been used on various fabric, such as inorganic salt compound, organic
Metallic compound, nitro compound, formaldehyde derivatives, but human body is not only caused certain injury by major part antibacterial, and
Can not degrade, environment is impacted.If antibacterial that can be natural, nontoxic by some such as Oleum Folium Artemisiae Argyi, patchouli oil, Oleum Cinnamomi
Deng Chinese herbal medicine oil, arrange on fabric by certain method, the application of Chinese herbal medicine oil can not only be widened, improve product
Added value, and complied with the healthy living theory of modern consumer, also meet people's demand to health care textile.
Oleum Cinnamomi is called for short cassia oil, is mainly extracted by Cortex cinnamomi japonici (Ramulus Cinnamomi), Laurus nobilis, Ramulus Cinnamomi etc. and obtains, generally yellow or amber color liquid,
Main chemical compositions is trans-cinnamic aldehyde (70～80%), trans o-methoxy cinnamic aldehyde (5～12%) and cinnamyl acetate etc..Make
For the main active of Cortex Cinnamomi, research shows, Oleum Cinnamomi has strong suppression or kills the characteristic of microorganism, to antibacterial,
Yeast and mold all has the strongest inhibitory action, is incorporated on textile as antibacterial, can give textile excellent
Anti-microbial property.But Oleum Cinnamomi has strong fragrance and acrid odors, there is stronger volatility, meet light and heat instability,
Pharmacological action on volatile oil creates certain impact, directly applies it to textile and does not reaches ideal effect, need to find
Oleum Cinnamomi cladding is got up by effective ways so that it is avoid and extraneous contact.
Microcapsule technology is to utilize natural or synthesis polymer that some have reactivity, sensitivity or volatility
Liquid, solid and gas be encapsulated, formed fine particle a kind of technology, the particle of formation is referred to as microcapsule.Microcapsule
The main advantage changed has: (1) protection sensitive composition, improves the stability of material；(2) cover the pessimal stimulation abnormal smells from the patient of material, expand
The range of big core material；(3) control the release of core, there is targeting.Therefore, if by Oleum Cinnamomi micro encapsulation,
The most effectively weaken the volatilization of Oleum Cinnamomi, cover its overpowering odor, protect its effective pharmaceutical component further, and meat can be made
Cassia oil carries out slow release, extends drug effect, expands the Oleum Cinnamomi range of application in antibacterial fabric industry.
Antibacterial fabric is mainly prepared by spin processes and finishing method, and microcapsule technology is as after-finishing of textile products
A kind of effective means, because of the feature of its excellence, has obtained the favor of textile industry, be widely used in production have antibacterial,
Wrinkle resistant, anophelifuge, the textile of the function such as fire-retardant, fragrant.At present, textile is arranged and mainly passes through binding agent by microcapsule
Bonded on fabric (see Fig. 1).As Chinese patent CN85100799 discloses a kind of fabrics impregnated with microcapsules, micron size
Bead shaped particle or crystal grain by spray and liquid adhesive fabric is arranged.Chinese patent CN101324026 discloses
A kind of nano traditional Chinese medicine microcapsule fabric finishing agent, preparation method and fabric finishing method, with extracts of Chinese herbal medicine and polylactic acid system
Become capsule of nano solution, compound with aqueous polyurethane and obtain fabric finishing agent, put into fabric finishing agent soaks and dry just
Prepare anti-bacteria and anti-virus textile.Chinese patent CN102704280A discloses a kind of VE microcapsule fabric finishing liquid and production thereof
Process and the method for sorting to fabric.Using polyurethane is wall material, and VE is core, prepares VE microcapsule breast by interfacial polymerization
Liquid, adds softening agent CGF toward it and binding agent 101 compounds after obtaining fabric finishing liquor and fabric is carried out finishing functions.Although it is viscous
The use of mixture can make textile obtain different functions, but it uses, and not only can make the breathability of textile, comfortableness
Reduce, and because microcapsule is poor with the affinity of fiber so that textile resistance to water is relatively low, the functions of textile fabrics list produced
One, the demand of society can not be met.
Compared to coating or the infusion process of use binding agent, chemical crosslink technique can make microcapsule technology because of its advantage
Textile finishing has wider application.Chemical crosslink technique selects suitable cross-linking agent as the bridge of textile Yu microcapsule
Beam, is grafted onto microcapsule on fiber by ehter bond or ester bond.Dressing liquid generally comprises microcapsule suspensions, cross-linking agent, catalysis
Agent, softening agent and other auxiliary agents, finishing technique generally comprises an immersing and rolling or two leachings two are rolled, preliminary drying, bake three operations.Micro-glue
Chemical crosslinking between capsule and textile, not only makes the water resistance of function textile strengthen, and it is more preferable to give textile
Crease resistance.
Summary of the invention
In order to overcome the shortcoming of prior art with not enough, it is an object of the invention to provide a kind of energy and give the cotton after arranging
Fabric has the Oleum Cinnamomi microcapsule fabric finishing liquid that fastness to washing is good, antibacterial action is lasting, wrinkle resistant ability is strong, can meet weaving
The needs of product function finishing.
Further object is that the preparation method that above-mentioned Oleum Cinnamomi microcapsule fabric finishing liquid is provided.The method
First it is core using natural macromolecular material chitosan quaternary ammonium salt and arabic gum as the wall material of microcapsule, Oleum Cinnamomi, uses
Complex coacervation prepares Oleum Cinnamomi microcapsule emulsion.Then by cross-linking agent applicable with interpolation for above-mentioned Oleum Cinnamomi microcapsule emulsion, urge
Agent, softening agent and penetrating agent are compounding obtains a kind of multi-functional Oleum Cinnamomi microcapsule fabric finishing liquid.
It is yet a further object of the present invention to provide above-mentioned Oleum Cinnamomi microcapsule fabric finishing liquid answering in finish fabric
With.Use chemical crosslink technique that fabric carries out finishing functions, give the lasting antibiotic health care of fabric and crease resistant functions.
The purpose of the present invention is achieved by following technology:
A kind of Oleum Cinnamomi microcapsule fabric finishing liquid, this Oleum Cinnamomi microcapsule fabric finishing liquid by following by mass percentage
The component composition of meter:
Described Oleum Cinnamomi microcapsule emulsion prepares in accordance with the following methods:
(1) so that every liter of acetum to add in terms of 10～20g chitosan quaternary ammonium salts, chitosan quaternary ammonium salt is dissolved in acetic acid molten
In liquid, stirring makes it be completely dissolved, and is configured to chitosan quaternary ammonium saline solution；
(2) so that every liter of distilled water to add in terms of 10～20g arabic gums, arabic gum is dissolved in distilled water and is configured to Ah
Draw primary sol solution, add Oleum Cinnamomi and emulsifying agent carries out emulsification pretreatment, obtain acacia emulsions；
(3) water bath with thermostatic control temperature is adjusted to 40～50 DEG C, by step (2) gained under low whipping speed 400～600r/min
Acacia emulsions is added drop-wise in step (3) gained chitosan quaternary ammonium saline solution, after mix homogeneously, regulates reaction system with alkaline agent
PH value to 5～6, complex coacervation 30min；
(4) above-mentioned reactant liquor is cooled to 0～5 DEG C, adds firming agent, hand under the mixing speed of 400～600r/min
After connection solidification 0.5～1h, system pH is regulated to 6.5～7.0, then reaction system is moved into the constant temperature that temperature is 40～50 DEG C
In water-bath, solidification 1.5～2h i.e. obtains Oleum Cinnamomi microcapsule emulsion further.
Step (1) described chitosan quaternary ammonium salt is 1:1～3 with the mass ratio of step (2) described arabic gum；
The volume fraction of step (1) described acetum is 0.5～1.0%；
The temperature of step (2) described distilled water is 40 DEG C；Described emulsifying agent is any one in following two kinds of emulsifying agents, its
Middle a kind of emulsifying agent is made up of span-80 and tween 80 mixed in equal amounts, and another kind of emulsifying agent is OP-10, the consumption of emulsifying agent
1～2g emulsifying agent is used to calculate with every 100ml reaction system；The addition of described Oleum Cinnamomi, with chitosan quaternary ammonium salt and I
It is 1 that primary both glue adds the mass ratio of total amount:
0.5～3；The speed of described emulsification pretreatment is 2000～3500r/min, and the time is 5～10min；
Alkaline agent described in step (3) be volume fraction be the sodium hydroxide solution of 5～10%；
Step (4) described firming agent is glutaraldehyde, Biformyl or glutaraldehyde and the mixture of bis-phenol starch, firming agent
Addition and chitosan quaternary ammonium salt+arabic gum+Oleum Cinnamomi three to add the mass ratio of total amount be 1:0.5～3；Gained Cortex Cinnamomi
In oil microcapsule emulsion, Microcapsules Size is 4～12 μm, and drug loading is up to 38.1%.
Described wrinkle resistant cross-linking agent is more than one in 2D resin, etherified 2D resin, BTCA (BTCA)；
Described catalyst is magnesium chloride, sodium citrate, sodium hypophosphite or disodium hydrogen phosphate；
Described penetrating agent is fatty alcohol-polyoxyethylene ether (JFC)；
Described softening agent is amido silicon oil；
Described water is distilled water.
The preparation method of above-mentioned Oleum Cinnamomi microcapsule fabric finishing liquid, according to following operating procedure: by wrinkle resistant cross-linking agent, urge
After agent, penetrating agent, softening agent and water mix homogeneously, under 400～550r/min mixing speeds, by Oleum Cinnamomi microcapsule emulsion
Join in above-mentioned mixed liquor, after stirring, obtain Oleum Cinnamomi microcapsule fabric finishing liquid.
The application in finish fabric of the above-mentioned Oleum Cinnamomi microcapsule fabric finishing liquid.
Described application is according to following steps:
(1) first fabric to be arranged is soaked in 8～10g/L sodium carbonate liquors 30～45min and carry out pretreatment；
(2) by after the fabric of pretreatment is put into and soaked 0.5～1h in Oleum Cinnamomi microcapsule fabric finishing liquid, it is placed in all
Arranging with two leaching two roll process on even laboratory mangle, pick-up rate is 70～100%, then is placed in baking oven in 70～90 DEG C of temperature
Middle preliminary drying 2～4min, finally bakes 1～3min in shaping drying at a temperature of 140～160 DEG C, is cooled to room temperature, water
Wash, dry, obtain microcapsule textile.
Microcapsule mode of appearance prepared by the present invention is good, in complete spherical, and favorable dispersibility, particle diameter is 4～12 μm,
Drug loading is up to 38.1%, and sustained release performance is good, by Oleum Cinnamomi micro encapsulation, the performance of Oleum Cinnamomi will not be caused bigger shadow
Ring, expand the Oleum Cinnamomi range of application in antibacterial fabric industry.
The present invention utilizes Oleum Cinnamomi microcapsule fabric finishing liquid to Cotton Fabric, and its method relates to a kind of microcapsule chemistry
Cross-linking method, is specifically described as follows:
The present invention has selected chitosan quaternary ammonium salt and arabic gum to be wall material when preparing microcapsule, and both of which contains in a large number
Active hydroxyl and amino, these active groups are under the effect of catalyst, with 2D resin, etherified 2D resin, BTCA
Deng cross-linking agent, esterification or etherification reaction (reaction principle is shown in Fig. 2 and Fig. 3) can occur, thus by chemical crosslinking, microcapsule be transferred
Receive on fabric, not only increase the water-wash resistance of fabric, impart the antibacterial functions that fabric is more longlasting, and give fabric more
Excellent crease resistant functions.In addition, use 2D resin or etherified 2D resin as cross-linking agent, the free formaldehyde of they releases
Can again solidify microcapsule as the firming agent of microcapsule so that microcapsule better tightness, the slow release effect of core more preferably,
And considerably reduce the burst size of fabric formaldehyde after arrangement.
In the present invention, the clad ratio of Oleum Cinnamomi microcapsule and the calculating of drug loading are carried out according to below equation:
Wherein:
The mensuration of microcapsule always oil: taking a certain amount of microcapsule product, it is ultrasonic that addition absolute ether is placed in sonic oscillation instrument
10min, makes Oleum Cinnamomi be dissolved in organic facies, is repeated several times to water layer oil-free, and organic facies merges, concentrates, and is placed in by concentrated solution
In the dry beaker weighed, volatilize residue ether to constant weight.
The mensuration of surface of microcapsule oil: take the microcapsule product of equivalent in centrifuge tube, adds absolute ether, acutely shakes
1min, centrifugal 5min (4000r/min), be repeated several times, and supernatant merges, concentrates, and concentrated solution is placed in the dry burning weighed
In Bei, volatilize residue ether to constant weight.
The method of testing of the release performance of microcapsule Oleum Cinnamomi of the present invention: accurately weigh three parts freshly prepared and measured initial
The dry microcapsule product of drug loading is respectively placed in 24.0%RH, 37 DEG C of climatic chambers, the most accurately weighs
Quantitatively microcapsule sample is in absolute ether, according to microcapsule always oil and the assay method of surface of microcapsule oil, measures microcapsule
Remaining drug loading, residue drug loading and the ratio of initial drug loading, it is simply that relative surplus drug loading, thus can try to achieve microcapsule
Relative accumulation burst size within certain time period.
Oleum Cinnamomi microcapsule textile anti-microbial property test prepared by the present invention is carried out according to GB/T 20944.3-2008 standard
Measure.The burst size of fabric formaldehyde after being arranged by GB/T 2912.1-2009 (aqueous extraction method) standard test.According to GB/T
3819-1997 standard uses LLY-02 type wrinkle recovery angle of woven fabrics using viscoelasticity theory tester to measure wrinkle recovery angle of woven fabrics using viscoelasticity theory.
The present invention compared with prior art has such advantages as and beneficial effect:
(1) present invention is with chitosan quaternary ammonium salt and arabic gum for wall material, with Oleum Cinnamomi as core, uses complex coacervation legal system
Standby Oleum Cinnamomi microcapsule.Complex coacervation preparation condition is gentle, and operating process is simple, low for equipment requirements, abundant raw material source, side
Just implement, it is easier to industrialized production.Prepared microcapsule good dispersion, size is uniform, and stability of emulsion is high, cladding
Rate, drug loading and slow release effect all reach more satisfactory state.Chitosan quaternary ammonium salt wall material has good bacteria resistance, nontoxic
The advantage such as property, biodegradability, biocompatibility, and the Oleum Cinnamomi being wrapped by has multiple pharmacological function, as antibacterial, disease-resistant
Characteristic, chitosan quaternary ammonium salt and the Oleum Cinnamomi such as poison, blood pressure lowering and antitumor all have good antibiotic property, and both are combined in one
Rising, synergism can make the antibiotic property of microcapsule strengthen, and antimicrobial spectrum is widened, and by microcapsule to textile finishing, gives fabric more
Excellent antibacterial functions.In addition, by Oleum Cinnamomi micro encapsulation, not only make its effective ingredient obtain good protection, make
Its stability strengthens, and masks the Chinese herbal medicine oil taste that Oleum Cinnamomi is special, expands the Oleum Cinnamomi application in textile industry
Scope.
(2) different from conventional coatings adhesive bonding method, the present invention uses chemical crosslink technique to arrange fabric, is effectively improved
The water-wash resistance of function fabric, the breathability of fabric and overcome the monistic deficiency of fabric functional, make prepared fabric with
Time there is lasting antibacterial and wrinkle resistant performance.The Oleum Cinnamomi Microcapsules Size that the present invention prepares is sufficiently small, affine with fabric
Power is good, not only can adhere to the surface of fabric, and under the effect of penetrating agent, moreover it is possible to penetrate between fiber and fiber,
Under the effect of catalyst, microcapsule, fiber and cross-linking agent crosslink reaction, thus further increase the water-fastness of fabric
Property.The use of softening agent amido silicon oil, substantially increases the wettability of finish fabric, before making the comfort level of fabric reach to arrange
Effect.
(3) Oleum Cinnamomi microcapsule fabric finishing liquid is applied in the Final finishing of the crease-resistant function of antibacterial fabric, height can be obtained
Effect, wide spectrum, safe, washable antibacterial and wrinkle resistant multifunctional fabric, not only increase the added value of textile, and can expire
Foot people's demand to multifunctional fabric.
Accompanying drawing explanation
Fig. 1 is fabric scanning electron microscope (SEM) figure arranged with binding agent.
Fig. 2 is chemical crosslink reaction figure that may be present between 2D resin and microcapsule and cotton-textile fibres.
Fig. 3 is chemical crosslink reaction figure that may be present between BTCA and microcapsule and cotton-textile fibres.
Fig. 4 is scanning electron microscope (SEM) figure of the embodiment of the present invention 1 Oleum Cinnamomi microcapsule.
Fig. 5 is the grain size distribution of the embodiment of the present invention 1 Oleum Cinnamomi microcapsule.
Fig. 6 is the scanning electron microscope (SEM) of the bafta after the embodiment of the present invention 1 Oleum Cinnamomi microcapsule fabric finishing liquid arranges
Figure.
Fig. 7 is the grain size distribution of the embodiment of the present invention 2 Oleum Cinnamomi microcapsule.
Fig. 8 is the scanning electron microscope (SEM) of the bafta after the embodiment of the present invention 2 Oleum Cinnamomi microcapsule fabric finishing liquid arranges
Figure.
Fig. 9 is the grain size distribution of the embodiment of the present invention 3 Oleum Cinnamomi microcapsule.
Figure 10 is the scanning electron microscope of the bafta after the embodiment of the present invention 3 Oleum Cinnamomi microcapsule fabric finishing liquid arranges
(SEM) figure.
Figure 11 is the grain size distribution of the embodiment of the present invention 4 Oleum Cinnamomi microcapsule.
Figure 12 is the scanning electron microscope of the bafta after the embodiment of the present invention 4 Oleum Cinnamomi microcapsule fabric finishing liquid arranges
(SEM) figure.
Figure 13 is scanning electron microscope (SEM) figure of untrimmed fabric.
Detailed description of the invention
Below in conjunction withspecific examples and drawings the present invention is described in further detail, but the implementation of the present invention
Flexibly, the concrete operations mode described in this example it is not limited only to.
Embodiment 1
1, the preparation of Oleum Cinnamomi microcapsule
1.1 chitosan quaternary ammonium saline solution: 1.5g chitosan quaternary ammonium salt (HACC) is dissolved in 150mL 0.5% acetum
In, it is 1.0% chitosan quaternary ammonium saline solution that stirring make it be completely dissolved i.e. to obtain concentration.
The emulsifying of 1.2 Oleum Cinnamomi: take 3.0g arabic gum (GA) and be dissolved in 150mL distilled water, adds 1.5g tween 80 and mixes
After closing mixing, add the mixture of 2.25g Oleum Cinnamomi and the span-80 of 1.5g, in 2000r/min rotating speed down cut emulsifying
10min。
1.3 complex coacervations: above-mentioned acacia emulsions is instilled in chitosan quaternary ammonium saline solution, after its mix homogeneously
Adjusting pH value to 5.0 with 10% sodium hydroxide (NaOH), in 45 DEG C of heating in water bath 30min, mixing speed is 400r/min.
1.4 cross-linking reactions: be placed in ice bath by above-mentioned reactant liquor and be cooled to 0～5 DEG C, add 5g 25% glutaraldehyde solution,
Under 400r/min mixing speed after crosslinking curing 1h, move in 40 DEG C of water-baths by reactant liquor again after system pH is adjusted to 6.5
One step solidification 2h i.e. obtains Oleum Cinnamomi microcapsule emulsion, centrifugal sedimentation, sucking filtration, dried Oleum Cinnamomi microscapsule powder.
Oleum Cinnamomi microcapsule:
(1) mode of appearance: buff powder, spherical rule, independent completion, such as accompanying drawing 4.
(2) size: mean diameter is 10.8 μm, particle diameter is distributed such as accompanying drawing 5.
(3) envelop rate and drug loading are respectively as follows: 76.2%, and 29.3%.
(4) slow release effect: after 5 days, Oleum Cinnamomi relative accumulation burst size is 45.7%.
(5) antibacterial effect: after 5 days, staphylococcus aureus and colibacillary minimal inhibitory concentration are respectively as follows:
1.25mg/mL and 2.5mg/mL.
2, the preparation of Oleum Cinnamomi microcapsule fabric finishing liquid
2.1 weigh 60g above-mentioned Oleum Cinnamomi microcapsule emulsion, 20g cross-linking agent 2D resin, 8g catalyst magnesium chloride, and 2g permeates
Agent JFC, 10g softening agent amido silicon oil, 100g deionized water, stir and i.e. obtain 200g Oleum Cinnamomi microcapsule dressing liquid.
Oleum Cinnamomi microcapsule fabric finishing liquid:
(1) mode of appearance: emulsion form, stablizes not stratified, and 50 DEG C of heating 1h do not have obvious sediment.
(2) each constituent content of dressing liquid is as follows:
Oleum Cinnamomi microcapsule emulsion: 30%；
Cross-linking agent 2D resin: 10%；
Catalyst magnesium chloride: 4%；
Softening agent amido silicon oil: 5%；
Penetrating agent JFC: 1%；
3, the Oleum Cinnamomi microcapsule fabric finishing liquid method for sorting to bafta
The pretreatment of 3.1 baftas: under room temperature, puts into fabric (100% pure cotton grey fabric, 25cm × 25cm) containing 10g/
L sodium carbonate liquor soaks 30min, cleans up with flowing water the most again, dried for standby.
3.2 will treat finish fabric, be immersed in above-mentioned Oleum Cinnamomi microcapsule fabric finishing liquid (bath raio 1:20), dipping
30min, is placed on uniform laboratory mangle (two leachings two are rolled, and pick-up rate is 100%), is placed in 80 DEG C of preliminary drying 3min in baking oven, then fixed
In type dehydrator, 160 DEG C bake 2min, are cooled to room temperature, washing, dry, obtain microcapsule textile sample.
Bafta after arrangement:
(1) mode of appearance: microcapsule is evenly distributed on cotton fiber, spherical well, such as accompanying drawing 6.
(2) water-wash resistance: when fabric is the most scrubbed, is staphylococcus aureus and colibacillary bacteriostasis rate
100%, after fabric washing 25 times, to staphylococcus aureus, colibacillary bacteriostasis rate all more than 75%.
(3) creasy recovery angle: after washing 25 times, creasy recovery angle is 273 °.
(4) burst size of methanal: 45mg/kg.
(5) tested by FTIR spectrum, it was demonstrated that Oleum Cinnamomi microcapsule, cross-linking agent 2D resin occur with cotton fiber
Etherification reaction.
Embodiment 2
1, the preparation of Oleum Cinnamomi microcapsule
1.1 chitosan quaternary ammonium saline solution: 1.5g chitosan quaternary ammonium salt (HACC) is dissolved in 150mL 0.5% acetum
In, it is 1.0% chitosan quaternary ammonium saline solution that stirring make it be completely dissolved i.e. to obtain concentration.
The emulsifying of 1.2 Oleum Cinnamomi: take 1.5g arabic gum (GA) and be dissolved in 150mL distilled water, adds 1.5g tween 80 and mixes
After closing mixing, add the mixture of 3.0g Oleum Cinnamomi and the span-80 of 1.5g, in 3000r/min rotating speed down cut emulsifying
5min。
1.3 complex coacervations: above-mentioned acacia emulsions is instilled in chitosan quaternary ammonium saline solution, after its mix homogeneously
Adjusting pH value to 6.0 with 10% sodium hydroxide (NaOH), in 40 DEG C of heating in water bath 30min, mixing speed is 400r/min.
1.4 cross-linking reactions: be placed in ice bath by above-mentioned reactant liquor and be cooled to 0～5 DEG C, add 8g 25% glyoxal solution,
Under 500r/min mixing speed after crosslinking curing 45min, again reactant liquor is moved in 50 DEG C of water-baths after system pH is adjusted to 7.0
Further solidification 1.5h i.e. obtains Oleum Cinnamomi microcapsule emulsion, centrifugal sedimentation, sucking filtration, dried Oleum Cinnamomi microscapsule powder.
Oleum Cinnamomi microcapsule:
(1) mode of appearance: buff powder, spherical rule, independent completion, such as accompanying drawing 4.
(2) size: mean diameter is 9.57 μm, particle diameter is distributed such as accompanying drawing 5.
(3) envelop rate and drug loading are respectively as follows: 53.6%, and 37.6%.
(4) slow release effect: after 5 days, Oleum Cinnamomi relative accumulation burst size is 62.7%.
(5) antibacterial effect: after 5 days, staphylococcus aureus and colibacillary minimal inhibitory concentration are respectively as follows:
1.5mg/mL and 3.0mg/mL.
2, the preparation of Oleum Cinnamomi microcapsule fabric finishing liquid
2.1 weigh 80g above-mentioned Oleum Cinnamomi microcapsule emulsion, 30g cross-linking agent BTCA (BTCA), 10g catalyst lemon
Lemon acid sodium, 2g penetrating agent JFC, 10g softening agent amido silicon oil, 68g deionized water, stir and i.e. obtain 200g Oleum Cinnamomi microcapsule
Dressing liquid.
Oleum Cinnamomi microcapsule fabric finishing liquid:
(1) mode of appearance: emulsion form, stablizes not stratified, and 50 DEG C of heating 1h do not have obvious sediment.
(2) each constituent content of dressing liquid is as follows:
Oleum Cinnamomi microcapsule emulsion: 40%；
Crosslinking agent B TCA:15%；
Catalyst magnesium chloride: 5%；
Softening agent amido silicon oil: 5%；
Penetrating agent JFC: 1%；
3, the Oleum Cinnamomi microcapsule fabric finishing liquid method for sorting to bafta
The pretreatment of 3.1 baftas: under room temperature, puts into fabric (100% pure cotton grey fabric, 25cm × 25cm) containing 10g/
L sodium carbonate liquor soaks 30min, cleans up with flowing water the most again, dried for standby.
3.2 will treat finish fabric, be immersed in above-mentioned Oleum Cinnamomi microcapsule fabric finishing liquid (bath raio 1:20), dipping
45min, is placed on uniform laboratory mangle (two leachings two are rolled, and pick-up rate is 80%), is placed in 80 DEG C of preliminary drying 4min in baking oven, then in sizing
In dehydrator, 180 DEG C bake 1.5min, are cooled to room temperature, washing, dry, obtain microcapsule textile sample.
Bafta after arrangement:
(1) mode of appearance: microcapsule is evenly distributed on cotton fiber, spherical well, such as accompanying drawing 6.
(2) water-wash resistance: when fabric is the most scrubbed, is staphylococcus aureus and colibacillary bacteriostasis rate
100%, after fabric washing 25 times, to staphylococcus aureus, colibacillary bacteriostasis rate all more than 80%.
(3) creasy recovery angle: after washing 25 times, creasy recovery angle is 286 °.
(4) tested by FTIR spectrum, it was demonstrated that Oleum Cinnamomi microcapsule, crosslinking agent B TCA there occurs with cotton fiber
Esterification.
Embodiment 3
1, the preparation of Oleum Cinnamomi microcapsule
1.1 chitosan quaternary ammonium saline solution: 3.0g chitosan quaternary ammonium salt (HACC) is dissolved in 150mL 0.5% acetum
In, it is 2.0% chitosan quaternary ammonium saline solution that stirring make it be completely dissolved i.e. to obtain concentration.
The emulsifying of 1.2 Oleum Cinnamomi: take 3.0g arabic gum (GA) and be dissolved in 150mL distilled water, adds 3g OP-10 emulsifying
After agent stirring mixing mixing, add 6g Oleum Cinnamomi, at 2500r/min rotating speed down cut emulsifying 8min.
1.3 complex coacervations: above-mentioned acacia emulsions is instilled in chitosan quaternary ammonium saline solution, after its mix homogeneously
Adjusting pH value to 5.5 with 10% sodium hydroxide (NaOH), in 45 DEG C of heating in water bath 30min, mixing speed is 500r/min.
1.4 cross-linking reactions: above-mentioned reactant liquor is placed in ice bath and is cooled to 0～5 DEG C, addition 3g 25% glutaraldehyde solution,
2g bis-phenol starch, under 500r/min mixing speed after crosslinking curing 30min, moves reactant liquor after system pH is adjusted to 6.5 again
Enter in 40 DEG C of water-baths solidification 2h further and i.e. obtain Oleum Cinnamomi microcapsule emulsion, centrifugal sedimentation, sucking filtration, dried the micro-glue of Oleum Cinnamomi
Capsule powder.
Oleum Cinnamomi microcapsule:
(1) mode of appearance: buff powder, spherical rule, independent completion, such as accompanying drawing 7.
(2) size: mean diameter is 9.66 μm, particle diameter is distributed such as accompanying drawing 8.
(3) envelop rate and drug loading are respectively as follows: 59.1%, and 38.1%.
(4) slow release effect: after 5 days, Oleum Cinnamomi relative accumulation burst size is 52.3%.
(5) antibacterial effect: after 5 days, staphylococcus aureus and colibacillary minimal inhibitory concentration are respectively as follows:
0.625mg/mL and 1.25mg/mL.
2, the preparation of Oleum Cinnamomi microcapsule fabric finishing liquid
2.1 weigh 50g above-mentioned Oleum Cinnamomi microcapsule emulsion, 20g cross-linking agent etherified 2D resin, 16g catalyst magnesium chloride, 6g
Penetrating agent JFC, 16g softening agent amido silicon oil, 92g deionized water, stir and i.e. obtain 200g Oleum Cinnamomi microcapsule dressing liquid.
Oleum Cinnamomi microcapsule fabric finishing liquid:
(1) mode of appearance: emulsion form, stablizes not stratified, and 50 DEG C of heating 1h do not have obvious sediment.
(2) each constituent content of dressing liquid is as follows:
Oleum Cinnamomi microcapsule emulsion: 25%；
Cross-linking agent etherified 2D resin: 10%；
Catalyst magnesium chloride: 8%；
Softening agent amido silicon oil: 8%；
Penetrating agent JFC: 3%；
3, the Oleum Cinnamomi microcapsule fabric finishing liquid method for sorting to bafta
The pretreatment of 3.1 baftas: under room temperature, puts into fabric (100% pure cotton grey fabric, 25cm × 25cm) containing 10g/
L sodium carbonate liquor soaks 30min, cleans up with flowing water the most again, dried for standby.
3.2 will treat finish fabric, be immersed in above-mentioned Oleum Cinnamomi microcapsule fabric finishing liquid (bath raio 1:20), impregnate 1h,
It is placed on uniform laboratory mangle (two leachings two are rolled, and pick-up rate is 70%), is placed in 90 DEG C of preliminary drying 2min in baking oven, then at shaping drying
In 140 DEG C bake 3min, be cooled to room temperature, washing, dry, obtain microcapsule textile sample.
Bafta after arrangement:
(1) mode of appearance: microcapsule is evenly distributed on cotton fiber, spherical well, such as accompanying drawing 9.
(2) water-wash resistance: when fabric is the most scrubbed, is staphylococcus aureus and colibacillary bacteriostasis rate
100%, after fabric washing 25 times, to staphylococcus aureus, colibacillary bacteriostasis rate all more than 70%.
(3) creasy recovery angle: after washing 25 times, creasy recovery angle is 254 °.
(4) burst size of methanal: 22mg/kg.
(5) tested by FTIR spectrum, it was demonstrated that Oleum Cinnamomi microcapsule, cross-linking agent 2D resin occur with cotton fiber
Etherification reaction.
Embodiment 4
1, the preparation of Oleum Cinnamomi microcapsule
1.1 chitosan quaternary ammonium saline solution: 2.25g chitosan quaternary ammonium salt (HACC) is dissolved in 150mL0.5% acetum
In, it is 1.5% chitosan quaternary ammonium saline solution that stirring make it be completely dissolved i.e. to obtain concentration.
The emulsifying of 1.2 Oleum Cinnamomi: take 4.5g arabic gum (GA) and be dissolved in 150mL distilled water, adds 3.0g tween 80 and mixes
After closing mixing, add the mixture of 2.25g Oleum Cinnamomi and the span-80 of 3.0g, in 3500r/min rotating speed down cut emulsifying
10min。
1.3 complex coacervations: above-mentioned acacia emulsions is instilled in chitosan quaternary ammonium saline solution, after its mix homogeneously
Adjusting pH value to 6.0 with 10% sodium hydroxide (NaOH), in 50 DEG C of heating in water bath 30min, mixing speed is 600r/min.
1.4 cross-linking reactions: be placed in ice bath by above-mentioned reactant liquor and be cooled to 0～5 DEG C, add 5g 25% glutaraldehyde solution,
Under 600r/min mixing speed after crosslinking curing 30min, again reactant liquor is moved in 50 DEG C of water-baths after system pH is adjusted to 7.0
Further solidification 1.5h i.e. obtains Oleum Cinnamomi microcapsule emulsion, centrifugal sedimentation, sucking filtration, dried Oleum Cinnamomi microscapsule powder.
Oleum Cinnamomi microcapsule:
(1) mode of appearance: buff powder, spherical rule, independent completion, such as accompanying drawing 10.
(2) size: mean diameter is 4.97 μm, particle diameter is distributed such as accompanying drawing 11.
(3) envelop rate and drug loading are respectively as follows: 81.5%, and 20.6%.
(4) slow release effect: after 5 days, Oleum Cinnamomi relative accumulation burst size is 43.6%.
(5) antibacterial effect: after 5 days, staphylococcus aureus and colibacillary minimal inhibitory concentration are respectively as follows:
1.25mg/mL and 2.5mg/mL.
2, the preparation of Oleum Cinnamomi microcapsule fabric finishing liquid
2.1 weigh 100g above-mentioned Oleum Cinnamomi microcapsule emulsion, 40g cross-linking agent BTCA (BTCA), 20g catalyst
Sodium phosphate, 4g penetrating agent JFC, 14g softening agent amido silicon oil, 22g deionized water, stir and i.e. obtain 200g Oleum Cinnamomi microcapsule
Dressing liquid.
Oleum Cinnamomi microcapsule fabric finishing liquid:
(1) mode of appearance: emulsion form, stablizes not stratified, and 50 DEG C of heating 1h do not have obvious sediment.
(2) each constituent content of dressing liquid is as follows:
Oleum Cinnamomi microcapsule emulsion: 50%；
Crosslinking agent B TCA:20%；
Catalyst magnesium chloride: 10%；
Softening agent amido silicon oil: 7%；
Penetrating agent JFC: 2%；
3, the Oleum Cinnamomi microcapsule fabric finishing liquid method for sorting to bafta
The pretreatment of 3.1 baftas: under room temperature, puts into fabric (100% pure cotton grey fabric, 25cm × 25cm) containing 10g/
L sodium carbonate liquor soaks 30min, cleans up with flowing water the most again, dried for standby.
3.2 will treat finish fabric, be immersed in above-mentioned Oleum Cinnamomi microcapsule fabric finishing liquid (bath raio 1:20), dipping
30min, is placed on uniform laboratory mangle (two leachings two are rolled, and pick-up rate is 90%), is placed in 70 DEG C of preliminary drying 4min in baking oven, then in sizing
In dehydrator, 160 DEG C bake 2min, are cooled to room temperature, washing, dry, obtain microcapsule textile sample.
Bafta after arrangement:
(1) mode of appearance: microcapsule is evenly distributed on cotton fiber, spherical well, such as accompanying drawing 12.
(2) water-wash resistance: when fabric is the most scrubbed, is staphylococcus aureus and colibacillary bacteriostasis rate
100%, after fabric washing 25 times, to staphylococcus aureus, colibacillary bacteriostasis rate all more than 85%.
(3) creasy recovery angle: after washing 25 times, creasy recovery angle is 296 °.
(4) tested by FTIR spectrum, it was demonstrated that Oleum Cinnamomi microcapsule, crosslinking agent B TCA there occurs with cotton fiber
Esterification.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (6)
1. an Oleum Cinnamomi microcapsule fabric finishing liquid, it is characterised in that: this Oleum Cinnamomi microcapsule fabric finishing liquid is pressed by following
The component composition of mass percent:
Described Oleum Cinnamomi microcapsule emulsion prepares in accordance with the following methods:
(1) so that every liter of acetum to add in terms of 10～20g chitosan quaternary ammonium salts, chitosan quaternary ammonium salt is dissolved in acetum
In, stirring makes it be completely dissolved, and is configured to chitosan quaternary ammonium saline solution；
(2) so that every liter of distilled water to add in terms of 10～20g arabic gums, arabic gum is dissolved in distilled water and is configured to Arab
Sol solution, adds Oleum Cinnamomi and emulsifying agent carries out emulsification pretreatment, obtains acacia emulsions；
(3) water bath with thermostatic control temperature is adjusted to 40～50 DEG C, under low whipping speed 400～600r/min by step (2) gained I
Primary latex solution is added drop-wise in step (1) gained chitosan quaternary ammonium saline solution, after mix homogeneously, with the pH of alkaline agent regulation reaction system
It is worth to 5～6, complex coacervation 30min；
(4) above-mentioned reactant liquor being cooled to 0～5 DEG C, add firming agent, under the mixing speed of 400～600r/min, crosslinking is solid
After changing 0.5～1h, system pH is regulated to 6.5～7.0, then reaction system is moved into the water bath with thermostatic control that temperature is 40～50 DEG C
In Guo, solidification 1.5～2h i.e. obtains Oleum Cinnamomi microcapsule emulsion further.
Oleum Cinnamomi microcapsule fabric finishing liquid the most according to claim 1, it is characterised in that:
Step (1) described chitosan quaternary ammonium salt is 1:1～3 with the mass ratio of step (2) described arabic gum；
The volume fraction of step (1) described acetum is 0.5～1.0%；
The temperature of step (2) described distilled water is 40 DEG C；Described emulsifying agent is any one in following two kinds of emulsifying agents, Qi Zhongyi
Planting emulsifying agent to be made up of span-80 and tween 80 mixed in equal amounts, and another kind of emulsifying agent is OP-10, the consumption of emulsifying agent is with often
100ml reaction system uses 1～2g emulsifying agent to calculate；The addition of described Oleum Cinnamomi, with chitosan quaternary ammonium salt and arabic gum
Both add the mass ratio of total amount is 1:0.5～3；The speed of described emulsification pretreatment is 2000～3500r/min, the time be 5～
10min；
Alkaline agent described in step (3) be volume fraction be the sodium hydroxide solution of 5～10%；
Step (4) described firming agent is glutaraldehyde, Biformyl or glutaraldehyde and the mixture of bis-phenol starch, adding of firming agent
Enter amount and chitosan quaternary ammonium salt+arabic gum+Oleum Cinnamomi three adding the mass ratio of total amount is 1:0.5～3；Gained Oleum Cinnamomi is micro-
In capsule emulsion, Microcapsules Size is 4～12 μm, and drug loading is up to 38.1%.
Oleum Cinnamomi microcapsule fabric finishing liquid the most according to claim 1, it is characterised in that:
Described wrinkle resistant cross-linking agent is more than one in 2D resin, etherified 2D resin, BTCA；
Described catalyst is magnesium chloride, sodium citrate, sodium hypophosphite or disodium hydrogen phosphate；
Described penetrating agent is fatty alcohol-polyoxyethylene ether；
Described softening agent is amido silicon oil；
Described water is distilled water.
The preparation method of Oleum Cinnamomi microcapsule fabric finishing liquid the most according to claim 1, it is characterised in that according to following
Operating procedure: after wrinkle resistant cross-linking agent, catalyst, penetrating agent, softening agent and water mix homogeneously, in 400～550r/min stirrings
Under speed, Oleum Cinnamomi microcapsule emulsion is joined in above-mentioned mixed liquor, obtain Oleum Cinnamomi microcapsule textile after stirring whole
Reason liquid.
The Oleum Cinnamomi microcapsule fabric finishing liquid the most according to claim 1 application in finish fabric.
Application the most according to claim 5, it is characterised in that: described application is according to following steps:
(1) first fabric to be arranged is soaked in 8～10g/L sodium carbonate liquors 30～45min and carry out pretreatment；
(2) by after the fabric of pretreatment is put into and soaked 0.5～1h in Oleum Cinnamomi microcapsule fabric finishing liquid, it is placed in the least
Arranging with two leaching two roll process on padding machine, pick-up rate is 70～100%, then is placed in baking oven in 70～90 DEG C of temperature pre-
Dry 2～4min, in shaping drying, at a temperature of 140～160 DEG C, finally bake 1～3min, be cooled to room temperature, washing, dry in the air
Dry, obtain microcapsule textile.
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| CN102405941A (en) * | 2011-08-10 | 2012-04-11 | 华南农业大学 | Isatis root oil microcapsule and functional fabric finishing agent |
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