CN103741496B - The preparation method of long-acting height is affine essence microcapsule softener and application - Google Patents

Abstract

The invention provides the preparation and application of a softener using long-acting high-affinity essence microcapsules. Firstly, a composite dispersant is prepared with nonionic surfactant and amphiphilic macromolecule, essence is the core material, and etherified melamine resin is the wall. The fragrance microcapsules are prepared from the material; then a long-acting and high-affinity aromatic microcapsule softener is prepared using it as a raw material; an application method of the long-acting and high-affinity aromatic microcapsule softener is provided. The effect of the present invention is to adopt a simple and environmentally friendly preparation method to obtain essence microcapsules, which can be applied to softeners and laundry detergents of various ionic systems. The essence content can reach 20%-30%, and the solid content can reach 22-35%. %, compared with other flavor microcapsule products on the market, the solid content can be increased by 10%-15%, and the fragrance encapsulation rate can reach 60%-70%, and it has good stability. At the same time, the long-acting and high-affinity aromatic microcapsule softener prepared from this essence microcapsule has a good fragrance effect on fabrics, and the fabric has a long fragrance retention time, which can last up to 6 months after standing. Explosive aroma.

Description

Preparation method and application of long-acting high-affinity essence microcapsule softener

technical field

The invention belongs to the technical field of textile finishing, and specifically relates to a composite dispersant prepared from nonionic surfactants and amphiphilic macromolecules, with essence as the core material and etherified melamine resin as the wall material, which is prepared by an interfacial polymerization method The long-acting high-affinity essence microcapsule softener can be adapted to softeners and laundry detergents of various ionic systems.

Background technique

Microcapsule technology refers to the technology of using natural or synthetic polymer materials to coat the target object with chemical or physical methods to form tiny particles with a core-shell structure with a diameter of 0.1-1000 μm. Microcapsules have the functions of protecting substances from environmental influences, reducing toxicity, masking bad taste, controlling core release, prolonging storage period, changing physical state for easy portability and transportation, changing physical properties to make incompatible ingredients evenly mixed, and easy to degrade.

Flavors and fragrances have the functions of antibacterial and insect repellent, masking peculiar smell, and making body and mind comfortable, so they are generally loved by people. In recent years, due to the emergence of aromatherapy and various functional flavors and fragrances, the annual consumption of flavors and fragrances has increased significantly. However, as an active product, it is very easy to cause a lot of waste in the process of transportation, storage and use, or the change of fragrance caused by deterioration. Through microcapsule technology, this problem can be well solved.

R.T.Codge of the United States mainly researches and develops microencapsulated "wipe and sniff" short-sleeved T-shirts and knitted fabrics for women, and uses in-situ interfacial polymerization technology to manufacture capsules. The former product can be washed 8 to 20 times, depending on the encapsulated active agent; while the latter can be washed up to 10 times. It is also resistant to tumble drying. The British Celessence International company has applied the basic technology of gelatin or synthetic capsule encapsulation of spices to prevent evaporation, oxidation and pollution of the contents. Fragrances, vitamins, moisturizers, and even insect repellants can be added to the capsules. The capsule wall can be made of polymer materials such as urea-formaldehyde resin, but the amount of formaldehyde contained is very small, which is lower than the industrial limit index of cosmetics and even lower than the industrial limit index of oral hygiene products. It can be applied to textiles by padding, suction, or centrifugal dehydration techniques, and can withstand up to 30 washes. Wash resistance and hand are further improved with the application of appropriate formaldehyde-free binders and softeners. Japan's Matsuishikiso Chemical Company has developed a method for immobilizing spice microcapsules. The fabric is first treated with a nitrogen-containing cationic compound to make the walls of the capsules adhere to the treated layer. Capsules are manufactured using interfacial or in situ polymerization techniques, and their encapsulates include spices such as musk, civet, ambergris, pine oil, and lemon oil. Such spice microcapsules are sold well. Pusan National University in South Korea has prepared microcapsules containing perfume oil using a melamine-formaldehyde system, with a diameter of up to 10 μm and a washability of 15 times. The Slovenian company Aero produces paper-like or non-woven products containing microencapsulated essential oils such as clove, sage and rosemary for shoe linings and insoles for odor control.

At present, the microcapsules on the market usually have the disadvantages of low essence content, low essence encapsulation rate, short fragrance retention time, and inability to control the release of fragrance well. More importantly, it cannot be well adapted to downstream products of different ion systems. In view of the shortcomings of the above essence microcapsules, a non-ionic composite dispersion system is used to microencapsulate the oil-soluble essence by interfacial polymerization with etherified melamine resin as the wall material. The essence microcapsule has high essence content and encapsulation rate, has good affinity with various fabric fibers, can be firmly fixed on cotton fabric fibers, has excellent fragrance retention and controlled release performance, and has rubbing release properties. At the same time, it has good adaptability to downstream products such as softeners and laundry detergents of various ionic systems. Therefore, how to greatly improve the use efficiency of the essence and widen the scope of application of the microcapsule essence needs to be developed urgently.

Contents of the invention

The purpose of the present invention is to provide a preparation method and application of a long-acting high-affinity essence microcapsule softener. A composite dispersant is prepared from a nonionic surfactant and an amphiphilic macromolecule, the essence is the core material, and the etherified melamine resin is the wall material to prepare essence microcapsules. A long-acting and high-affinity aromatic microcapsule softener was prepared using it as a raw material. An application method of the long-acting and high-affinity aromatic microcapsule softener is provided. The preparation method of the essence microcapsules is simple and environmentally friendly, which reduces the volatilization and deterioration of the essence, and can be well applied to softeners and laundry detergents of various ionic systems, and is reliable and stable. At the same time, the long-acting and high-affinity aromatic microcapsule softener prepared with this essence microcapsule as raw material can perfume the fabric, which can prolong the fragrance retention time and make the fragrance release controllable. It has an explosive aroma after rubbing .

In order to achieve the above object, the technical solution adopted is to provide a preparation method of a long-acting high-affinity essence microcapsule softener, comprising the following steps:

(1) Preparation of composite dispersant

Weigh 100 parts of nonionic surfactant and 900 parts of deionized water, stir at 50°C to fully dissolve them, and prepare an aqueous solution with a mass fraction of 10%;

Weigh 100 parts of non-ionic amphiphilic polymers and 900 parts of deionized water, stir at 90°C to fully dissolve them, and prepare an aqueous solution with a mass fraction of 10%;

Weigh 50-300 parts of nonionic surfactant aqueous solution and 1-50 parts of nonionic amphiphilic polymer aqueous solution and stir and mix at 50°C to obtain a composite dispersant, which is set aside;

(2) Preparation of etherified melamine resin solution

Stir and mix 70-110 parts of etherified melamine resin and 50-80 parts of deionized water in a beaker to obtain a dispersion of etherified melamine resin for later use;

(3) Preparation of Essence Microcapsule Emulsion

Put 50-350 parts of the composite dispersant prepared in (1), 300-650 parts of deionized water, 150-350 parts of essence, and 10-20 parts of glacial acetic acid solution in a beaker, and use a high-shear dispersing emulsifier in the Carry out emulsification under the rotating speed of 5000-15000r/min, obtain core material emulsion;

Move the core material emulsion to a four-necked bottle, add 120-170 parts of the etherified melamine resin solution prepared in (2) dropwise under stirring conditions, and disperse for 10-30 minutes after the dropping. Under the conditions of reflux and stirring, the temperature is raised to 65-80°C, solidified for 0.5-2 hours, and then the pH is adjusted to neutral with a 30% NaOH solution to stabilize it. Cool down naturally to obtain etherified melamine resin essence microcapsule emulsion;

(4) Preparation of aromatic microcapsule softener

Weighing 1-5 parts of the fragrance microcapsule emulsion prepared in (3) and 500-1500 parts of the softening agent without fragrance, fully stirring and mixing at 40° C., to prepare the long-lasting fragrance microcapsule softening agent.

The aromatic microcapsule softening agent is applied in the after-finishing application of cotton fabrics, and the specific method is:

Weigh 5-20 parts of aromatic microcapsule softener and 1000-5000 parts of water, stir and disperse. Soak the cotton fabric for 3-5 minutes at room temperature to ensure the uniform penetration of the aromatic finishing solution on the cotton fabric. Take it out to dry naturally, and you can get the fabric with long-lasting fragrance and smooth finishing.

Effect of the present invention is:

(1) The long-acting high-affinity fragrance microcapsules completely adopt the non-ionic system, which has a wider adaptability than other commercially available fragrance microcapsules, and can be well used in anionic, cationic, amphoteric and non-ionic matrices such as softeners.

(2) The flavor content of the long-acting high-affinity flavor microcapsules can reach 20%-30%, and the solid content can reach 22-35%, which can be increased by 10%-15% compared with other commercially available flavor microcapsule products. The wrapping rate of essence can reach 60%-70%.

(3) The composite dispersant is used to make the synthesis process of the essence microcapsules easier to control and has good storage stability. At the same time, the long-acting and high-affinity aromatic microcapsule softener prepared from this essence microcapsule has a good fragrance effect on fabrics, and the fabric has a long fragrance retention time, which can last up to 6 months after standing. Explosive aroma.

detailed description

The preparation method and application of the long-acting high-affinity essence microcapsule softener of the present invention will be described in detail in combination with examples.

A kind of preparation method of long-acting high-affinity essence microcapsule softening agent of the present invention, the method comprises the following steps:

(1) Preparation of composite dispersant

Weigh 100 parts of nonionic surfactant and 900 parts of deionized water, stir at 50°C to fully dissolve them, and prepare an aqueous solution with a mass fraction of 10%;

Weigh 100 parts of non-ionic amphiphilic polymers and 900 parts of deionized water, stir at 90°C to fully dissolve them, and prepare an aqueous solution with a mass fraction of 10%;

Weigh 50-300 parts of nonionic surfactant aqueous solution and 1-50 parts of nonionic amphiphilic polymer aqueous solution and stir and mix at 50°C to obtain a composite dispersant, which is set aside;

(2) Preparation of etherified melamine resin solution

Stir and mix 70-110 parts of etherified melamine resin and 50-80 parts of deionized water in a beaker to obtain a dispersion of etherified melamine resin for later use;

(3) Preparation of Essence Microcapsule Emulsion

Put 50-350 parts of the composite dispersant prepared in (1), 300-650 parts of deionized water, 150-350 parts of essence, and 10-20 parts of glacial acetic acid solution in a beaker, and use a high-shear dispersing emulsifier in the Carry out emulsification under the rotating speed of 5000-15000r/min, obtain core material emulsion;

Move the core material emulsion to a four-necked bottle, add 120-170 parts of the etherified melamine resin solution prepared in (2) dropwise under stirring conditions, and disperse for 10-30 minutes after the dropping. Under the conditions of reflux and stirring, the temperature is raised to 65-80°C, solidified for 0.5-2 hours, and then the pH is adjusted to neutral with a 30% NaOH solution to stabilize it. Cool down naturally to obtain etherified melamine resin essence microcapsule emulsion;

(4) Preparation of aromatic microcapsule softener

Weighing 1-5 parts of the fragrance microcapsule emulsion prepared in (3) and 500-1500 parts of the softening agent without fragrance, fully stirring and mixing at 40° C., to prepare the long-lasting fragrance microcapsule softening agent.

Described nonionic surfactant is Tween series, OP series, and nonionic amphipathic polymer is polyvinyl alcohol, polyethylene glycol, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, cyclic Ethylene oxide-propylene oxide block copolymer. The etherified melamine resins are methyl etherified melamine resins, n-butyl etherified melamine resins, isobutyl etherified melamine resins, and mixed etherified melamine resins. The softening agent is anionic, cationic, amphoteric quaternary ammonium salt and nonionic softening agent. The essence is an oil-soluble daily chemical essence.

The aromatic microcapsule softening agent is applied in the post-finishing application of cotton fabrics, and the post-finishing application is a dipping method, and the specific application method is as follows:

Weigh 5-20 parts of aromatic microcapsule softener and 1000-5000 parts of water, stir and disperse. Soak the cotton fabric for 3-5 minutes at room temperature to ensure the uniform penetration of the aromatic finishing solution on the cotton fabric. Take it out to dry naturally, and you can get the fabric with long-lasting fragrance and smooth finishing.

Example:

Example 1

Weigh 10 parts of nonionic surfactant and 90 parts of deionized water, stir at 50°C to make it fully dissolve, and prepare an aqueous solution with a mass fraction of 10%; weigh 1 part of nonionic amphiphilic polymer and 9 parts Deionized water was stirred at 90°C to fully dissolve it to prepare an aqueous solution with a mass fraction of 10%; the two were stirred and mixed at 50°C to obtain a composite dispersant.

The prepared composite dispersant, 490 parts of deionized water, 250 parts of essence, and 10 parts of glacial acetic acid solution were placed in a beaker, and emulsified with a high-shear dispersing emulsifier at a speed of 8000r/min to obtain a core material emulsion . Move the core material emulsion to a four-necked bottle, and under stirring conditions, add dropwise the etherified melamine resin dispersion that is fully stirred and miscible by 70 parts of etherified melamine resin and 80 parts of deionized water, and disperse for 10 minutes after dropping . Under the conditions of reflux and stirring, the temperature was raised to 70° C., solidified for 1 hour, and then the pH was adjusted to neutral with 30% NaOH solution to stabilize it. Cool down naturally to obtain the etherified melamine resin essence microcapsule emulsion; the solid content of the microcapsule emulsion is 23.93%, and the essence encapsulation rate is 68.93%.

Finally, 2 parts of the prepared fragrance microcapsules and 500 parts of the softening agent without fragrance were weighed, and fully stirred and mixed at 40° C. to obtain a long-lasting fragrance microcapsule softening agent. Add 5 parts of aromatic microcapsule softener to 1000 parts of clear water, stir to disperse, and soak the cotton fabric for 3 minutes at room temperature to ensure the uniform penetration of the aromatic finishing solution on the cotton fabric. Take it out to dry naturally, and you can get the fabric with long-lasting fragrance and smooth finishing.

The prepared long-acting and high-affinity aromatic microcapsule softener does not affect the original function of the softener, and has a good fragrance effect on fabrics. The fabric has a long fragrance retention time, and the fragrance retention can last up to 6 months. After rubbing, it has explosive fragrance.

Example 2

Weigh 30 parts of nonionic surfactant and 270 parts of deionized water, stir at 50°C to make it fully dissolved, and prepare an aqueous solution with a mass fraction of 10%; weigh 5 parts of nonionic amphiphilic polymer and 45 parts of Deionized water was stirred at 90°C to fully dissolve it to prepare an aqueous solution with a mass fraction of 10%; the two were stirred and mixed at 50°C to obtain a composite dispersant.

Put the prepared composite dispersant, 300 parts of deionized water, 350 parts of essence, and 20 parts of glacial acetic acid solution into a beaker, and emulsify with a high-shear dispersing emulsifier at a speed of 10,000 r/min to obtain a core material emulsion . Move the core material emulsion to a four-necked bottle, and under stirring conditions, add dropwise the etherified melamine resin dispersion that is fully stirred and miscible by 110 parts of etherified melamine resin and 50 parts of deionized water, and disperse for 30 minutes after dropping . Under the condition of reflux and stirring, the temperature was raised to 75° C., solidified for 2 hours, and then the pH was adjusted to neutral with 30% NaOH solution to make it stable. Cool down naturally to obtain the etherified melamine resin essence microcapsule emulsion; the solid content of the microcapsule emulsion is 28.90%, and the essence encapsulation rate is 63.51%.

Finally, 3 parts of the prepared fragrance microcapsules and 1000 parts of softener without fragrance were weighed, and fully stirred and mixed at 40° C. to obtain a long-lasting fragrance microcapsule softener. Add 8 parts of aromatic microcapsule softener to 2000 parts of clear water, stir to disperse, and soak the cotton fabric for 4 minutes at room temperature to ensure the uniform penetration of the aromatic finishing solution on the cotton fabric. Take it out to dry naturally, and you can get the fabric with long-lasting fragrance and smooth finishing.

The prepared long-acting and high-affinity aromatic microcapsule softener does not affect the original function of the softener, and has a good fragrance effect on fabrics. The fabric has a long fragrance retention time, and the fragrance retention can last up to 6 months. After rubbing, it has explosive fragrance.

Example 3

Weigh 20 parts of nonionic surfactant and 180 parts of deionized water, stir at 50°C to make it fully dissolved, and prepare an aqueous solution with a mass fraction of 10%; weigh 3 parts of nonionic amphiphilic polymer and 27 parts of Deionized water was stirred at 90°C to fully dissolve it to prepare an aqueous solution with a mass fraction of 10%; the two were stirred and mixed at 50°C to obtain a composite dispersant.

The prepared composite dispersant, 350 parts of deionized water, 300 parts of essence, and 15 parts of glacial acetic acid solution were placed in a beaker, and emulsified with a high-shear dispersing emulsifier at a speed of 15000r/min to obtain a core material emulsion . Move the core material emulsion to a four-necked bottle, and under stirring conditions, add dropwise the etherified melamine resin dispersion liquid that is fully stirred and miscible with 80 parts of etherified melamine resin and 70 parts of deionized water, and disperse for 20 minutes after dropping . Under the conditions of reflux and stirring, the temperature was raised to 72° C., solidified for 1.5 hours, and then the pH was adjusted to neutral with 30% NaOH solution to stabilize it. Cool down naturally to obtain the etherified melamine resin essence microcapsule emulsion; the solid content of the microcapsule emulsion is 27.20%, and the essence encapsulation rate is 65.34%.

Finally, 5 parts of the prepared fragrance microcapsules and 1500 parts of softener without fragrance were weighed, and fully stirred and mixed at 40° C. to obtain a long-lasting fragrance microcapsule softener. Add 20 parts of aromatic microcapsule softener to 5000 parts of clear water, stir to disperse, and soak the cotton fabric for 5 minutes at room temperature to ensure the uniform penetration of the aromatic finishing solution on the cotton fabric. Take it out to dry naturally, and you can get the fabric with long-lasting fragrance and smooth finishing.

The prepared long-acting and high-affinity aromatic microcapsule softener does not affect the original function of the softener, and has a good fragrance effect on fabrics. The fabric has a long fragrance retention time, and the fragrance retention can last up to 6 months. After rubbing, it has explosive fragrance.

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.