CN103741496A - Preparation and application methods of long-acting high-affinity softener prepared from essence microcapsules - Google Patents

Preparation and application methods of long-acting high-affinity softener prepared from essence microcapsules Download PDF

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CN103741496A
CN103741496A CN201310749536.9A CN201310749536A CN103741496A CN 103741496 A CN103741496 A CN 103741496A CN 201310749536 A CN201310749536 A CN 201310749536A CN 103741496 A CN103741496 A CN 103741496A
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essence
softener
long
preparation
melamine resin
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CN103741496B (en
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费学宁
张宝莲
赵洪宾
谷迎春
于妙卓
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Tianjin Chengjian University
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Tianjin Chengjian University
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Abstract

The invention provides preparation and application of a long-acting high-affinity softener prepared from essence microcapsules. The long-acting high-affinity essence microcapsule softener is prepared in the following steps: preparing a compound dispersant by using a nonionic surfactant and amphiphilic macromolecules, and preparing the essence microcapsules by taking essence as a core material and taking etherified melamine resin as a wall material; and preparing a fragrant microcapsule softener by taking the essence microcapsules as a raw material. The invention further provides an application method of the long-acting high-affinity fragrant microcapsule softener. The essence microcapsules prepared by a simple, convenient and environment-friendly method can be suitable for softeners, laundry detergents and the like of various ionic systems, the essence content can be 20-30 percent, and the solid content can be 22-35 percent. Compared with other commercially-available essence microcapsule, the solid content of the essence microcapsules can be 10-15 percent higher than that of the commercially available essence microcapsule products, the essence coating rate can be 60-70 percent, and the stability is good. Meanwhile, the long-acting high-affinity fragrant microcapsule softener prepared by taking the essence microcapsules as a raw material is good in the perfuming effect on fabrics and long in fragrance lasting time on fabrics, the fragrance can last for six months in a standing state, and high fragrance explosive power can be achieved by rubbing.

Description

With softener preparation and the application process of the affine essence microcapsule of long-acting height
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 softener preparation of the affine essence microcapsule of the long-acting height of use preparing by interfacial polymerization and application process, can be adapted to the softener, liquid detergent of various ionic systems etc.
Background technology
Microcapsules technology refers to utilizes natural or synthetic macromolecular material, by the method for chemistry or physics, object is coated wherein, forms the technology of the fine particle of the nucleocapsid structure of diameter 0.1-1000 μ m.Microcapsules have the impact that Protective substances is avoided environment, reduce toxicity, shelter disagreeable taste, and control core discharges, and extend storage period, and change states of matter easy to carry and transport, change physical property and make evenly to mix by compatible composition, are 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, thereby has obtained generally liking of people.In recent years, more because the appearance of aromatotherapy and various functional form essence and flavoring agents makes the consumption of annual essence and flavoring agent all be the state of increasing substantially.But as a kind of biologically active prod, very easily in the process of transportation, storage, use, occur a large amount of wastes, or go bad the odor type change causing.By microcapsules technology, can address this problem well.
U.S. R.T.Codge company mainly researchs and develops microencapsulation and " wipes and smell " T-shirt and lady's knitted fabric, and application original position interfacial polymerization technology is manufactured capsule.Product the former washable 8~20 times, depending on the activating agent of sealing; And the latter is up to 10 times.Also can the drying of resistance to rotating cage.Britain Celessence Intenational company has applied the basic fundamental of gelatin or synthetic capsule encapsulated perfume, in case the evaporation of content, oxidation and pollution.Can add spices, vitamin, wetting agent, even pest repellant 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 pad, exhaust or centrifugal dehydration technology puts on textiles, ability is up to 30 washings.In conjunction with application suitable formaldehyde binder and softener, washability and feel have further been improved.Japan Matsui shikiso chemical company has developed the method for set perfume microcapsule.Fabric is first used to cationic nitrogenous compound treatment, the cyst wall of manufacturing is adhered on this processing layer.By interface or in-situ polymerization technology, manufacture capsule, its encapsulation object comprises Moschus, civetta, ambergris, pine wood oil and lemon wet goods spices.This kind of perfume microcapsule sold good.The microcapsules that Korea S Pusan national university has prepared application carbamide system, contained perfumery oil, diameter is up to 10 μ m, washable 15 times.Slovenia Aero company produced containing microencapsulation essential oil for example cloves, Salvia japonica and rosemary, Xue MingRosma rinus officinalis similar paper or nonwoven products, as sock and shoe-pad to control smell.
The shortcomings such as at present microcapsules on the market exist essence content low conventionally, and essence encapsulation ratio is low, and fragrance remaining time is short, release that can not fine control fragrance.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, adopt nonionic compound dispersing agent, by interfacial polymerization, take etherification melamine resin as wall material, oil soluble perfume is carried out to microencapsulation.This essence microcapsule has high essence content and encapsulation ratio, can and various fabrics fiber between there is good affinity, can anchor at securely on COTTON FABRIC fiber, lasting ability and control release performance good, there is the release property of rubbing.The downstream product of the softener to various ionic systems, liquid detergent etc. all has adaptability simultaneously.The accommodation that therefore, how can increase substantially essence service efficiency and widen microcapsule essence is urgently developed.
Summary of the invention
The object of the invention is to provide softener preparation and the application process of the affine essence microcapsule of the long-acting height of a kind of use, with non-ionic surface active agent and amphiphilic macromolecular, be prepared into composite dispersing agent, essence is core, and etherification melamine resin is wall material, prepares essence microcapsule.Take it as raw material, prepared the affine aromatic micro-capsule softener of a kind of long-acting height.The application process of the affine aromatic micro-capsule softener of this long-acting height is provided.The easy environmental protection of preparation method of essence microcapsule, has reduced volatilization and the spoilage problems of essence, can the well suited softener in various ionic systems, liquid detergent etc., and reliable and stable.Meanwhile, the affine aromatic micro-capsule softener of long-acting height of preparing take this essence microcapsule as raw material 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 softener preparation and the application process of the affine essence microcapsule of the long-acting height of a kind of use, comprises the steps:
(1) preparation of composite dispersing agent
Take 100 portions of non-ionic surface active agents and 900 parts of deionized waters, at 50 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution;
Take 100 parts of nonionic amphiphilic macromoleculars and 900 parts of deionized waters, at 90 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution;
Take 50-300 part nonionic surfactant water-soluble liquid and 1-50 part nonionic amphiphilic macromolecular aqueous solution is uniformly mixed at 50 ℃, obtain composite dispersing agent, standby;
(2) preparation of etherification melamine resin solution
By 70-110 part etherification melamine resin and 50-80 part deionized water in beaker, stir miscible after, obtain etherification melamine resin dispersion liquid, standby;
(3) preparation of essence microcapsule emulsion
Composite dispersing agent, 300-650 part deionized water, 150-350 part essence, 10-20 part glacial acetic acid solution of preparation in 50-350 part (1) are placed in to beaker jointly, and with high-shearing dispersion emulsifying machine, under the rotating speed of 5000-15000r/min, carry out emulsification, obtain core emulsion;
Core emulsion is moved in four-hole bottle, under stirring condition, be added dropwise to the etherification melamine resin solution of preparation in 120-170 part (2), drip off rear dispersion 10-30min.Refluxing, being warming up to 65-80 ℃ under stirring condition, solidify 0.5-2 hour, then the NaOH solution that is 30% with concentration is adjusted to neutrality by pH it is stablized.Naturally cooling, obtains etherification melamine resin essence microcapsule emulsion;
(4) preparation of aromatic micro-capsule softener and application process
Take essence microcapsule emulsion that 1-5 part (3) makes and 500-1500 part containing the softener of essence, at 40 ℃, be fully uniformly mixed, make long-acting aromatic micro-capsule softener.This aromatic micro-capsule softener is applied in the rear arrangement application of COTTON FABRIC, concrete grammar 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 to 3-5min, to guarantee the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC.Take out natural drying, can obtain the fabric through the submissive arrangement of long-acting fragrance.
Effect of the present invention is:
(1) the affine essence microcapsule of long-acting height adopts nonionic system completely, compares commercially available other essence microcapsules 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%, compares commercially available other essence microcapsule product solid contents and 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 take this essence microcapsule as raw material 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.
The specific embodiment
In conjunction with embodiment, softener preparation and the application process of the affine essence microcapsule of the long-acting height of use of the present invention are elaborated.
Softener preparation and the application process of the affine essence microcapsule of the long-acting height of a kind of use 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, at 50 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution;
Take 100 parts of nonionic amphiphilic macromoleculars and 900 parts of deionized waters, at 90 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution;
Take 50-300 part nonionic surfactant water-soluble liquid and 1-50 part nonionic amphiphilic macromolecular aqueous solution is uniformly mixed at 50 ℃, obtain composite dispersing agent, standby;
(2) preparation of etherification melamine resin solution
By 70-110 part etherification melamine resin and 50-80 part deionized water in beaker, stir miscible after, obtain etherification melamine resin dispersion liquid, standby;
(3) preparation of essence microcapsule emulsion
Composite dispersing agent, 300-650 part deionized water, 150-350 part essence, 10-20 part glacial acetic acid solution of preparation in 50-350 part (1) are placed in to beaker jointly, and with high-shearing dispersion emulsifying machine, under the rotating speed of 5000-15000r/min, carry out emulsification, obtain core emulsion;
Core emulsion is moved in four-hole bottle, under stirring condition, be added dropwise to the etherification melamine resin solution of preparation in 120-170 part (2), drip off rear dispersion 10-30min.Refluxing, being warming up to 65-80 ℃ under stirring condition, solidify 0.5-2 hour, then the NaOH solution that is 30% with concentration is adjusted to neutrality by pH it is stablized.Naturally cooling, obtains etherification melamine resin essence microcapsule emulsion;
(4) preparation of aromatic micro-capsule softener and application process
Take essence microcapsule emulsion that 1-5 part (3) makes and 500-1500 part containing the softener of essence, at 40 ℃, be fully uniformly mixed, make long-acting aromatic micro-capsule softener.This aromatic micro-capsule softener is applied in the rear arrangement application of COTTON FABRIC, rear arrangement is applied as infusion process, and concrete application process 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 to 3-5min, to guarantee the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC.Take out natural drying, can obtain the fabric through the submissive arrangement of long-acting fragrance.
Described non-ionic surface active agent is Tween series, OP series, and 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.
Embodiment:
Embodiment 1
Take 10 portions of non-ionic surface active agents and 90 parts of deionized waters, at 50 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution; Take 1 part of nonionic amphiphilic macromolecular and 9 parts of deionized waters, at 90 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution; The two is uniformly mixed at 50 ℃, 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 placed in to beaker jointly, and under the rotating speed of 8000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtain core emulsion.Core emulsion is moved in four-hole bottle, under stirring condition, be added dropwise to by 70 parts of etherification melamine resin and 80 parts of deionized waters and fully stir miscible etherification melamine resin dispersion liquid, drip off rear dispersion 10min.Refluxing, being warming up to 70 ℃ under stirring condition, solidify 1 hour, then the NaOH solution that is 30% with concentration is adjusted to neutrality by pH it is stablized.Naturally cooling, obtains etherification melamine resin essence microcapsule emulsion; The solid content 23.93% of this microcapsule emulsion, essence encapsulation ratio 68.93%.
Finally, take 2 parts of prepared essence microcapsules and 500 parts not containing the softener of essence, at 40 ℃, be fully uniformly mixed, obtain long-acting aromatic micro-capsule softener.5 parts of aromatic micro-capsule softeners are joined in 1000 parts of clear water, and dispersed with stirring, at room temperature soaks 3min by COTTON FABRIC, to guarantee the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC.Take out natural drying, can obtain the fabric through the submissive arrangement of long-acting fragrance.
The affine aromatic micro-capsule softener of long-acting height of preparation 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, at 50 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution; Take 5 parts of nonionic amphiphilic macromoleculars and 45 parts of deionized waters, at 90 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution; The two is uniformly mixed at 50 ℃, 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 placed in to beaker jointly, and under the rotating speed of 10000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtain core emulsion.Core emulsion is moved in four-hole bottle, under stirring condition, be added dropwise to by 110 parts of etherification melamine resin and 50 parts of deionized waters and fully stir miscible etherification melamine resin dispersion liquid, drip off rear dispersion 30min.Refluxing, being warming up to 75 ℃ under stirring condition, solidify 2 hours, then the NaOH solution that is 30% with concentration is adjusted to neutrality by pH it is stablized.Naturally cooling, obtains etherification melamine resin essence microcapsule emulsion; The solid content 28.90% of this microcapsule emulsion, essence encapsulation ratio 63.51%.
Finally, take 3 parts of prepared essence microcapsules and 1000 parts not containing the softener of essence, at 40 ℃, be fully uniformly mixed, obtain long-acting aromatic micro-capsule softener.8 parts of aromatic micro-capsule softeners are joined in 2000 parts of clear water, and dispersed with stirring, at room temperature soaks 4min by COTTON FABRIC, to guarantee the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC.Take out natural drying, can obtain the fabric through the submissive arrangement of long-acting fragrance.
The affine aromatic micro-capsule softener of long-acting height of preparation 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, at 50 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution; Take 3 parts of nonionic amphiphilic macromoleculars and 27 parts of deionized waters, at 90 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution; The two is uniformly mixed at 50 ℃, 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 placed in to beaker jointly, and under the rotating speed of 15000r/min, carry out emulsification with high-shearing dispersion emulsifying machine, obtain core emulsion.Core emulsion is moved in four-hole bottle, under stirring condition, be added dropwise to by 80 parts of etherification melamine resin and 70 parts of deionized waters and fully stir miscible etherification melamine resin dispersion liquid, drip off rear dispersion 20min.Refluxing, being warming up to 72 ℃ under stirring condition, solidify 1.5 hours, then the NaOH solution that is 30% with concentration is adjusted to neutrality by pH it is stablized.Naturally cooling, obtains etherification melamine resin essence microcapsule emulsion; The solid content 27.20% of this microcapsule emulsion, essence encapsulation ratio 65.34%.
Finally, take 5 parts of prepared essence microcapsules and 1500 parts not containing the softener of essence, at 40 ℃, be fully uniformly mixed, obtain long-acting aromatic micro-capsule softener.20 parts of aromatic micro-capsule softeners are joined in 5000 parts of clear water, and dispersed with stirring, at room temperature soaks 5min by COTTON FABRIC, to guarantee the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC.Take out natural drying, can obtain the fabric through the submissive arrangement of long-acting fragrance.
The affine aromatic micro-capsule softener of long-acting height of preparation 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 (5)

1. with softener preparation and the application process of the affine essence microcapsule 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, at 50 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution;
Take 100 parts of nonionic amphiphilic macromoleculars and 900 parts of deionized waters, at 90 ℃, stir, make it abundant dissolving, be prepared into mass fraction and be 10% the aqueous solution;
Take 50-300 part nonionic surfactant water-soluble liquid and 1-50 part nonionic amphiphilic macromolecular aqueous solution is uniformly mixed at 50 ℃, obtain composite dispersing agent, standby;
(2) preparation of etherification melamine resin solution
By 70-110 part etherification melamine resin and 50-80 part deionized water in beaker, stir miscible after, obtain etherification melamine resin dispersion liquid, standby;
(3) preparation of essence microcapsule emulsion
Composite dispersing agent, 300-650 part deionized water, 150-350 part essence, 10-20 part glacial acetic acid solution of preparation in 50-350 part step (1) are placed in to beaker jointly, and with high-shearing dispersion emulsifying machine, under the rotating speed of 5000-15000r/min, carry out emulsification, obtain core emulsion;
Core emulsion is moved in four-hole bottle, under stirring condition, be added dropwise to the etherification melamine resin solution of preparation in 120-170 part step (2), drip off rear dispersion 10-30min; Refluxing, being warming up to 65-80 ℃ under stirring condition, solidify 0.5-2 hour, then the NaOH solution that is 30% with concentration is adjusted to neutrality by pH it is stablized; Naturally cooling, obtains etherification melamine resin essence microcapsule emulsion;
(4) preparation of aromatic micro-capsule softener
Take the essence microcapsule emulsion that makes in 1-5 part step (3) and 500-1500 part containing the softener of essence, at 40 ℃, be fully uniformly mixed, make long-acting aromatic micro-capsule softener;
(5) application of long-acting aromatic micro-capsule softener
Adopt infusion process that the long-acting aromatic micro-capsule softener of preparation in step (4) is applied in the rear arrangement application of COTTON FABRIC, concrete operations are: take 5-20 part aromatic micro-capsule softener and 1000-5000 part clear water, dispersed with stirring; At room temperature COTTON FABRIC is soaked to 3-5min, to guarantee the uniformly penetrating of Aroma finishing liquid to COTTON FABRIC; Take out natural drying, can obtain the fabric through the submissive arrangement of long-acting fragrance.
2. with the softener of the affine essence microcapsule of long-acting height, prepare and application process according to claim 1, it is characterized in that: described ionic surfactant pack has been drawn together 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. according to claim 1 with softener preparation and the application process of the affine essence microcapsule of long-acting height, it 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. according to claim 1 with softener preparation and the application process of the affine essence microcapsule of long-acting height, it is characterized in that: described long-acting aromatic micro-capsule softener is anionic, cationic, both sexes quaternary and nonionic softener.
5. according to claim 1 with softener preparation and the application process of the affine essence microcapsule of long-acting height, it is characterized in that: described essence is oil-soluble daily chemical essence.
CN201310749536.9A 2013-12-27 2013-12-27 The preparation method of long-acting height is affine essence microcapsule softener and application Expired - Fee Related CN103741496B (en)

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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
CN111286414A (en) * 2019-11-28 2020-06-16 纳爱斯浙江科技有限公司 Clothing fragrance retaining bead and preparation method thereof
CN112391834A (en) * 2020-09-28 2021-02-23 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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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
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