CN103741496B - The preparation method of long-acting height is affine essence microcapsule softener and application - Google Patents
The preparation method of long-acting height is affine essence microcapsule softener and application Download PDFInfo
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Abstract
The invention provides the softener preparations and applicatio of the affine essence microcapsule of a kind of long-acting height, be first prepared into composite dispersing agent with non-ionic surface active agent and amphiphilic macromolecular, essence is core, and etherification melamine resin is wall material, prepares essence microcapsule; Again with it for the affine aromatic micro-capsule softener of a kind of long-acting height prepared by raw material; Provide the application process of the affine aromatic micro-capsule softener of this long-acting height.Effect of the present invention is adopt a kind of preparation method of easy environmental protection to obtain essence microcapsule, go for the softener of various ionic system, liquid detergent etc., its essence content can reach 20%-30%, solid content can reach 22-35%, compare other essence microcapsule product solid contents commercially available and can improve 10%-15%, can 60%-70% be reached to essence encapsulation ratio, and there is good stability.Meanwhile, the aromatic micro-capsule softener that the long-acting height prepared for raw material with this essence microcapsule is affine is respond well to going to temple to pray of fabric, and fabric fragrance remaining time is long, and standing lasting can reach 6 months, has fragrance explosive force after rubbing.
Description
Technical field
The invention belongs to spinning post-finishing technical field, be specifically related to one and be prepared into composite dispersing agent with non-ionic surface active agent and amphiphilic macromolecular, essence is core, etherification melamine resin is wall material, the long-acting height prepared by interfacial polymerization is affine essence microcapsule softener, can be adapted to the softener of various ionic system, liquid detergent etc.
Background technology
Microcapsules technology refers to and utilizes macromolecular material that is natural or synthesis, by method that is chemical or physics, object is wherein coated, forms the technology of the fine particle of the nucleocapsid structure of diameter 0.1-1000 μm.Microcapsules have the impact of Protective substances from environment, reduce toxicity, shelter disagreeable taste, and control core discharges, and extends storage period, and change states of matter easy to carry and transport, change physical property and uniform composition that can not be compatible is mixed, be easy to the performances such as degraded.
Essence and flavoring agent has antibacterial expelling parasite, covering smell, makes the effects such as body and mind is comfortable, thus obtains generally liking of people.In recent years, more because the appearance of aromatotherapy and various functional form essence and flavoring agent makes the consumption of annual essence and flavoring agent all in the state of increasing substantially.But as a kind of biologically active prod, very easily in the process of transport, storage, use, occur a large amount of waste, or go bad the odor type change caused.By microcapsules technology, can address this problem well.
R.T.Codge company of the U.S. mainly researchs and develops " wipe and the smell " T-shirt of microencapsulation and lady's knitted fabric, and application original position interfacial polymerization techniques manufactures capsule.Product the former washable 8 ~ 20 times, depending on the activating agent of encapsulating; And the latter is up to 10 times.Also can resistance to tumble dryer.CelessenceIntenational company of Britain applies the basic fundamental of gelatin or synthesis encapsulated perfume, in case the evaporation of content, oxidation and pollution.Spices, vitamin, wetting agent, even pest repellant can be added in capsule.Cyst wall can be made with polymeric materials such as such as urea-formaldehyde resins, but contained formaldehyde amount is atomic, lower than cosmetics, even lower than the industrial limit index of oral hygiene prods.Availablely to pad, to exhaust or centrifugal dehydration technology puts on textiles, ability is up to 30 washings.The formaldehyde binder that connected applications is suitable and softener, further improve washability and feel.Matsuishikiso chemical company of Japan develops the method for set perfume microcapsule.Fabric is first used cationic nitrogenous compound treatment, the cyst wall of manufacture is adhered on this processing layer.Manufacture capsule by interface or in-situ polymerization technology, its encapsulation object comprises Moschus, civetta, ambergris, pine wood oil and lemon wet goods spices.This kind of perfume microcapsule is sold good.Application carbamide system, microcapsules containing perfumery oil have been prepared by Pusan national university of Korea S, diameter up to 10 μm, washable 15 times.Aero company of Slovenia produce containing microencapsulation essential oil such as cloves, Salvia japonica and rosemary, Xue MingRosma rinus officinalis similar paper or nonwoven products, as sock and shoe-pad to control smell.
Usually it is low to there is essence content in current microcapsules on the market, and essence encapsulation ratio is low, and fragrance remaining time is short, can not control the shortcomings such as the release of fragrance very well.The more important thing is, the downstream product of adaptation different ions system that can not be good.For the shortcoming of above essence microcapsule, adopting nonionic compound dispersing agent, is that wall material carries out microencapsulation to oil soluble perfume by interfacial polymerization with etherification melamine resin.This essence microcapsule has high essence content and encapsulation ratio, and have good affinity between energy and various fabrics fiber, can anchor on cotton-textile fibres securely, lasting ability and Co ntrolled release function admirable, have and rub release property.All there is adaptability to the downstream product of the softener, liquid detergent etc. of various ionic system simultaneously.Therefore, the accommodation that how can increase substantially essence service efficiency and widen microcapsule essence is urgently developed.
Summary of the invention
The object of the invention is the preparation method and the application that provide the affine essence microcapsule softener of a kind of long-acting height, composite dispersing agent is prepared into non-ionic surface active agent and amphiphilic macromolecular, essence is core, and etherification melamine resin is wall material, prepares essence microcapsule.With it for the affine aromatic micro-capsule softener of a kind of long-acting height prepared by raw material.Provide the application process of the affine aromatic micro-capsule softener of this long-acting height.The easy environmental protection of preparation method of essence microcapsule, decreases volatilization and the spoilage problems of essence, can the well suited softener in various ionic system, liquid detergent etc., reliable and stable.Meanwhile, the aromatic micro-capsule softener that the long-acting height prepared for raw material with this essence microcapsule is affine is gone to temple to pray to fabric, can extend fragrance remaining time, and makes to release perfume (or spice) and have controllability, has fragrance explosive force after rubbing.
For achieving the above object, the technical scheme of employing is to provide the preparation method of the affine essence microcapsule softener of a kind of long-acting height, comprises the steps:
(1) preparation of composite dispersing agent
Take 100 portions of non-ionic surface active agents and 900 parts of deionized waters, stir at 50 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%;
Take 100 parts of nonionic amphiphilic macromoleculars and 900 parts of deionized waters, stir at 90 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%;
Take 50-300 part nonionic surfactant water-soluble liquid and 1-50 part nonionic amphiphilic macromolecular aqueous solution is uniformly mixed at 50 DEG C, obtain composite dispersing agent, for subsequent use;
(2) preparation of etherification melamine resin solution
70-110 part etherification melamine resin and 50-80 part deionized water are stirred in beaker miscible after, obtain etherification melamine resin dispersion liquid, for subsequent use;
(3) preparation of essence microcapsule emulsion
The composite dispersing agent of preparation in 50-350 part (1), 300-650 part deionized water, 150-350 part essence, 10-20 part glacial acetic acid solution are placed in beaker jointly, and under the rotating speed of 5000-15000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtain core material emulsion;
Core material emulsion is moved in four-hole bottle, under agitation, be added dropwise to the etherification melamine resin solution of preparation in 120-170 part (2), drip off rear dispersion 10-30min.In backflow, be warming up to 65-80 DEG C under stirring condition, solidification 0.5-2 hour, then by concentration be 30% NaOH solution pH is adjusted to neutrality and makes it stablize.Temperature fall, namely obtains etherification melamine resin essence microcapsule emulsion;
(4) preparation of aromatic micro-capsule softener
Take the obtained essence microcapsule emulsion of 1-5 part (3) and 500-1500 part containing the softener of essence, be fully uniformly mixed at 40 DEG C, obtained long-acting aromatic micro-capsule softener.
Be applied in by described aromatic micro-capsule softener in the Final finishing application of COTTON FABRIC, concrete grammar is:
Take 5-20 part aromatic micro-capsule softener and 1000-5000 part clear water, dispersed with stirring.At room temperature COTTON FABRIC is soaked 3-5min, to ensure the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC.Take out natural drying, the fabric through the submissive arrangement of long-acting fragrance can be obtained.
Effect of the present invention is:
(1) the affine essence microcapsule of long-acting height adopts nonionic system completely, compares other essence microcapsules commercially available and has adaptive capacity more widely, can applications well in the anion such as softener, CATION, amphoteric and nonionic matrix.
(2) the essence content of the affine essence microcapsule of long-acting height can reach 20%-30%, and solid content can reach 22-35%, and comparing other essence microcapsule product solid contents commercially available can improve 10%-15%, and it can reach 60%-70% to the encapsulation ratio of essence.
(3) adopt composite dispersing agent, make the building-up process of essence microcapsule be more prone to control, there is good storage stability.Meanwhile, the aromatic micro-capsule softener that the long-acting height prepared for raw material with this essence microcapsule is affine is respond well to going to temple to pray of fabric, and fabric fragrance remaining time is long, and standing lasting can reach 6 months, has fragrance explosive force after rubbing.
Detailed description of the invention
In conjunction with embodiment, the preparation method of the affine essence microcapsule softener of long-acting height of the present invention and application are described in detail.
The preparation method of the affine essence microcapsule softener of a kind of long-acting height of the present invention, the method comprises the following steps:
(1) preparation of composite dispersing agent
Take 100 portions of non-ionic surface active agents and 900 parts of deionized waters, stir at 50 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%;
Take 100 parts of nonionic amphiphilic macromoleculars and 900 parts of deionized waters, stir at 90 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%;
Take 50-300 part nonionic surfactant water-soluble liquid and 1-50 part nonionic amphiphilic macromolecular aqueous solution is uniformly mixed at 50 DEG C, obtain composite dispersing agent, for subsequent use;
(2) preparation of etherification melamine resin solution
70-110 part etherification melamine resin and 50-80 part deionized water are stirred in beaker miscible after, obtain etherification melamine resin dispersion liquid, for subsequent use;
(3) preparation of essence microcapsule emulsion
The composite dispersing agent of preparation in 50-350 part (1), 300-650 part deionized water, 150-350 part essence, 10-20 part glacial acetic acid solution are placed in beaker jointly, and under the rotating speed of 5000-15000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtain core material emulsion;
Core material emulsion is moved in four-hole bottle, under agitation, be added dropwise to the etherification melamine resin solution of preparation in 120-170 part (2), drip off rear dispersion 10-30min.In backflow, be warming up to 65-80 DEG C under stirring condition, solidification 0.5-2 hour, then by concentration be 30% NaOH solution pH is adjusted to neutrality and makes it stablize.Temperature fall, namely obtains etherification melamine resin essence microcapsule emulsion;
(4) preparation of aromatic micro-capsule softener
Take the obtained essence microcapsule emulsion of 1-5 part (3) and 500-1500 part containing the softener of essence, be fully uniformly mixed at 40 DEG C, obtained long-acting aromatic micro-capsule softener.
Described non-ionic surface active agent is Tween series, and OP series, nonionic amphiphilic macromolecular is polyvinyl alcohol, polyethylene glycol, Carboxymethyl Cellulose, hydroxyethylcellulose, hydroxypropyl cellulose, ethylene oxide-propylene oxide block copolymer.Described etherification melamine resin is methyl-etherified melamine resin, n-butyl ether melamine resin, isobutyl etherification melamine resin, mixed etherification melamine resin.Described softener is anionic, cationic, both sexes quaternary and nonionic softener.Described essence is oil-soluble daily chemical essence.
Be applied in by described aromatic micro-capsule softener in the Final finishing application of COTTON FABRIC, Final finishing is applied as infusion process, and embody rule method is as follows:
Take 5-20 part aromatic micro-capsule softener and 1000-5000 part clear water, dispersed with stirring.At room temperature COTTON FABRIC is soaked 3-5min, to ensure the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC.Take out natural drying, the fabric through the submissive arrangement of long-acting fragrance can be obtained.
Embodiment:
Embodiment 1
Take 10 portions of non-ionic surface active agents and 90 parts of deionized waters, stir at 50 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%; Take 1 part of nonionic amphiphilic macromolecular and 9 parts of deionized waters, stir at 90 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%; The two is uniformly mixed at 50 DEG C, obtains composite dispersing agent.
Prepared composite dispersing agent, 490 parts of deionized waters, 250 parts of essence, 10 parts of glacial acetic acid solutions are jointly placed in beaker, and under the rotating speed of 8000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtains core material emulsion.Core material emulsion is moved in four-hole bottle, under agitation, be added dropwise to and fully stir miscible etherification melamine resin dispersion liquid by 70 parts of etherification melamine resin and 80 parts of deionized waters, drip off rear dispersion 10min.In backflow, be warming up to 70 DEG C under stirring condition, solidify 1 hour, then by concentration be 30% NaOH solution pH is adjusted to neutrality and makes it stablize.Temperature fall, namely obtains etherification melamine resin essence microcapsule emulsion; The solid content 23.93% of this microcapsule emulsion, essence encapsulation ratio 68.93%.
Finally, take essence microcapsule obtained by 2 parts and 500 parts not containing the softener of essence, be fully uniformly mixed at 40 DEG C, obtain long-acting aromatic micro-capsule softener.Joined in 1000 parts of clear water by 5 parts of aromatic micro-capsule softeners, dispersed with stirring, at room temperature soaks 3min by COTTON FABRIC, to ensure the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC.Take out natural drying, the fabric through the submissive arrangement of long-acting fragrance can be obtained.
The aromatic micro-capsule softener that the long-acting height of preparation is affine does not affect the original function of softener, and respond well to going to temple to pray of fabric, fabric fragrance remaining time is long, and standing lasting can reach 6 months, has fragrance explosive force after rubbing.
Embodiment 2
Take 30 portions of non-ionic surface active agents and 270 parts of deionized waters, stir at 50 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%; Take 5 parts of nonionic amphiphilic macromoleculars and 45 parts of deionized waters, stir at 90 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%; The two is uniformly mixed at 50 DEG C, obtains composite dispersing agent.
Prepared composite dispersing agent, 300 parts of deionized waters, 350 parts of essence, 20 parts of glacial acetic acid solutions are jointly placed in beaker, and under the rotating speed of 10000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtains core material emulsion.Core material emulsion is moved in four-hole bottle, under agitation, be added dropwise to and fully stir miscible etherification melamine resin dispersion liquid by 110 parts of etherification melamine resin and 50 parts of deionized waters, drip off rear dispersion 30min.In backflow, be warming up to 75 DEG C under stirring condition, solidify 2 hours, then by concentration be 30% NaOH solution pH is adjusted to neutrality and makes it stablize.Temperature fall, namely obtains etherification melamine resin essence microcapsule emulsion; The solid content 28.90% of this microcapsule emulsion, essence encapsulation ratio 63.51%.
Finally, take essence microcapsule obtained by 3 parts and 1000 parts not containing the softener of essence, be fully uniformly mixed at 40 DEG C, obtain long-acting aromatic micro-capsule softener.Joined in 2000 parts of clear water by 8 parts of aromatic micro-capsule softeners, dispersed with stirring, at room temperature soaks 4min by COTTON FABRIC, to ensure the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC.Take out natural drying, the fabric through the submissive arrangement of long-acting fragrance can be obtained.
The aromatic micro-capsule softener that the long-acting height of preparation is affine does not affect the original function of softener, and respond well to going to temple to pray of fabric, fabric fragrance remaining time is long, and standing lasting can reach 6 months, has fragrance explosive force after rubbing.
Embodiment 3
Take 20 portions of non-ionic surface active agents and 180 parts of deionized waters, stir at 50 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%; Take 3 parts of nonionic amphiphilic macromoleculars and 27 parts of deionized waters, stir at 90 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%; The two is uniformly mixed at 50 DEG C, obtains composite dispersing agent.
Prepared composite dispersing agent, 350 parts of deionized waters, 300 parts of essence, 15 parts of glacial acetic acid solutions are jointly placed in beaker, and under the rotating speed of 15000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtains core material emulsion.Core material emulsion is moved in four-hole bottle, under agitation, be added dropwise to and fully stir miscible etherification melamine resin dispersion liquid by 80 parts of etherification melamine resin and 70 parts of deionized waters, drip off rear dispersion 20min.In backflow, be warming up to 72 DEG C under stirring condition, solidify 1.5 hours, then by concentration be 30% NaOH solution pH is adjusted to neutrality and makes it stablize.Temperature fall, namely obtains etherification melamine resin essence microcapsule emulsion; The solid content 27.20% of this microcapsule emulsion, essence encapsulation ratio 65.34%.
Finally, take essence microcapsule obtained by 5 parts and 1500 parts not containing the softener of essence, be fully uniformly mixed at 40 DEG C, obtain long-acting aromatic micro-capsule softener.Joined in 5000 parts of clear water by 20 parts of aromatic micro-capsule softeners, dispersed with stirring, at room temperature soaks 5min by COTTON FABRIC, to ensure the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC.Take out natural drying, the fabric through the submissive arrangement of long-acting fragrance can be obtained.
The aromatic micro-capsule softener that the long-acting height of preparation is affine does not affect the original function of softener, and respond well to going to temple to pray of fabric, fabric fragrance remaining time is long, and standing lasting can reach 6 months, has fragrance explosive force after rubbing.
Claims (6)
1. a preparation method for the affine essence microcapsule softener of long-acting height, the method comprises the following steps:
(1) preparation of composite dispersing agent
Take 100 portions of non-ionic surface active agents and 900 parts of deionized waters, stir at 50 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%;
Take 100 parts of nonionic amphiphilic macromoleculars and 900 parts of deionized waters, stir at 90 DEG C, make it abundant dissolving, be prepared into the aqueous solution that mass fraction is 10%;
Take 50-300 part nonionic surfactant water-soluble liquid and 1-50 part nonionic amphiphilic macromolecular aqueous solution is uniformly mixed at 50 DEG C, obtain composite dispersing agent, for subsequent use;
(2) preparation of etherification melamine resin solution
70-110 part etherification melamine resin and 50-80 part deionized water are stirred in beaker miscible after, obtain etherification melamine resin dispersion liquid, for subsequent use;
(3) preparation of essence microcapsule emulsion
The composite dispersing agent of preparation in 50-350 part step (1), 300-650 part deionized water, 150-350 part essence, 10-20 part glacial acetic acid solution are placed in beaker jointly, and under the rotating speed of 5000-15000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtain core material emulsion;
Core material emulsion is moved in four-hole bottle, under agitation, be added dropwise to the etherification melamine resin solution of preparation in 120-170 part step (2), drip off rear dispersion 10-30min; In backflow, be warming up to 65-80 DEG C under stirring condition, solidification 0.5-2 hour, then by concentration be 30% NaOH solution pH is adjusted to neutrality and makes it stablize; Temperature fall, namely obtains etherification melamine resin essence microcapsule emulsion;
(4) preparation of high affine essence microcapsule softener
To take in 1-5 part step (3) obtained essence microcapsule emulsion and 500-1500 part containing the softener of essence, be fully uniformly mixed at 40 DEG C, the obtained affine essence microcapsule softener of long-acting height.
2. the preparation method of the affine essence microcapsule softener of long-acting height according to claim 1, it is characterized in that: described non-ionic surface active agent includes poly yamanashi esters Tween-20, Tween-60, Tween-80, alkylphenol polyoxyethylene class OP-7, OP-10, OP-15, OP-21, nonionic amphiphilic macromolecular is polyvinyl alcohol, polyethylene glycol, Carboxymethyl Cellulose, hydroxyethylcellulose, hydroxypropyl cellulose, ethylene oxide-propylene oxide block copolymer.
3. the preparation method of the affine essence microcapsule softener of long-acting height according to claim 1, is characterized in that: described etherification melamine resin is methyl-etherified melamine resin, n-butyl ether melamine resin, isobutyl etherification melamine resin, mixed etherification melamine resin.
4. the preparation method of the affine essence microcapsule softener of long-acting height according to claim 1, is characterized in that: described long-acting height affine essence microcapsule softener is anionic, cationic, both sexes quaternary and nonionic softener.
5. the preparation method of the affine essence microcapsule softener of long-acting height according to claim 1, is characterized in that: described essence is oil-soluble daily chemical essence.
6. the application of the affine essence microcapsule softener of long-acting height obtained by long-acting height affine essence microcapsule softener preparation method according to claim 1, it is characterized in that: adopt infusion process to be applied in the Final finishing of COTTON FABRIC by the affine essence microcapsule softener of long-acting height of preparation in step (4), concrete operations are: take the affine essence microcapsule softener of the long-acting height of 5-20 part and 1000-5000 part clear water, dispersed with stirring is dressing liquid; At room temperature COTTON FABRIC is soaked 3-5min, to ensure the uniformly penetrating of described dressing liquid to COTTON FABRIC; Take out natural drying, the fabric arranged through the affine essence microcapsule softener of long-acting height can be obtained.
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| CN104975513B (en) * | 2015-05-29 | 2017-09-15 | 天津城建大学 | The preparation method of antimicrobial form chitosan essential oil microcapsules |
| CN106433976A (en) * | 2016-12-16 | 2017-02-22 | 东莞波顿香料有限公司 | Slow release microencapsulated flavor and preparation method thereof |
| CN111286414B (en) * | 2019-11-28 | 2021-04-27 | 纳爱斯浙江科技有限公司 | Clothing fragrance retaining bead and preparation method thereof |
| CN112391834B (en) * | 2020-09-28 | 2022-11-01 | 广州立白企业集团有限公司 | Composition for removing bacteria, removing peculiar smell and keeping fragrance for long time and preparation method thereof |
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| CN101928641B (en) * | 2010-09-29 | 2012-08-08 | 江南大学 | Essence microcapsule with long-term effectiveness and preparation method thereof |
| KR20130021761A (en) * | 2011-08-23 | 2013-03-06 | 김은엽 | In nature with the micro capsule of the rose oil and used this the reel of the rose oil the composition which has a theraphy function |
| CN102586017B (en) * | 2011-12-22 | 2013-05-01 | 华南师范大学 | Essence microcapsule with softening function and preparation method of essence microcapsule |
| CN103233368B (en) * | 2013-05-08 | 2015-03-04 | 天津城市建设学院 | Preparation and application of modified melamine resin essence microcapsule finishing agent |
| CN103230766B (en) * | 2013-05-08 | 2014-12-10 | 天津城市建设学院 | Preparation and application of self-adhesive double-wall essence microcapsule |
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