WO2019011265A1

WO2019011265A1 - Method for preparing antibacterial down

Info

Publication number: WO2019011265A1
Application number: PCT/CN2018/095242
Authority: WO
Inventors: 毛军; 陈红霞; 陆鹏; 丁可敬
Original assignee: 江苏金太阳纺织科技股份有限公司
Priority date: 2017-07-13
Filing date: 2018-07-11
Publication date: 2019-01-17
Also published as: CN107190518B; CN107190518A; AU2018299537A1; AU2018102132A4

Abstract

Disclosed is a method for preparing antibacterial down, the method comprising firstly preparing a natural antibacterial microcapsule auxiliary by adopting a microcapsule coating method, and then performing pre-oxidation modification on the down product, and finally, grafting the antibacterial microcapsule auxiliary onto the down product by adopting an enzymatic crosslinking reaction of glutamine transaminase, thereby realizing a long-lasting, environmentally-friendly and broad-spectrum antibacterial effect for the down product.

Description

Preparation method of antibacterial down

Technical field

The invention belongs to the technical field of textile materials, and in particular relates to a preparation method of antibacterial down.

Background technique

In recent years, down products have been more and more popular among consumers because of their excellent light and warmth. In the field of clothing and home textiles, the market for down jackets, duvets, down pillows and other products is growing. The acceptance of the people is also getting higher and higher. At present, the down feathers commonly found on the market are duck down and goose down. Both of them belong to protein fiber. They are natural nutrients of bacteria and mold, and are easy to breed bacteria. Especially some fabrics are used in order to obtain better anti-drilling performance. The high-density method, supplemented by special finishing techniques, reduces the breathability of the fabric, and the bacteria are usually anaerobic, so bacteria are more likely to grow in a less permeable environment. With the constant pursuit of environmental protection and healthy living, more consumers have begun to pay attention to the antibacterial and antibacterial properties of the products. Therefore, some antibacterial and antibacterial technologies have appeared in the field of down products, and more and more researchers are committed to antibacterial. Development of antibacterial down products.

CN103882723A discloses a method for padding a solution containing silver-coated nano antibacterial agent; CN105862434A discloses a method for impregnating or antibacterial down fiber by utilizing the antibacterial property of natural antibacterial substance chitin by impregnating or spraying a solution of chitin. . The existing antibacterial and antibacterial down technology mostly utilizes the method of spraying the impregnating agent to treat the antibacterial agent on the surface of the down fiber. Although the method can impart a certain antibacterial property to the down in a short period of time, the surface of the down fiber has a dense water repellent effect. The structural layer makes the antibacterial agent unable to penetrate into the interior of the down fiber, and the antibacterial down has poor washing durability and long-term durability, which cannot meet the needs of consumers. CN104947209A discloses a method for finishing chitin and nano titanium dioxide onto a down fiber by using a binder. The method is that the down fiber can obtain long-lasting antibacterial effect, but the bulkiness of the down product after the treatment of the adhesive is greatly increased. Reduced, seriously affecting the warmth and comfort of down products.

Summary of the invention

The invention aims at the above problems, and provides an antibacterial down and a preparation method thereof. The method firstly prepares a natural antibacterial nano microcapsule auxiliary by a microcapsule coating method, and then pre-oxidizes the down product, and finally the antibacterial The microcapsule auxiliary is grafted onto the down product by the enzymatic crosslinking reaction of glutamine transaminase, thereby realizing the long-acting, environmentally-friendly and broad-spectrum antibacterial effect of the down product.

In order to achieve the above effects, the technical solution of the present invention is as follows:

A preparation method of antibacterial down, comprising the following steps:

Step 1, the cleaning of the down, mixing the down, water and degreasing agent, and washing with water;

Step 2, pre-oxidation of the down, mixing the down, water and oxidant after washing in step 1 to perform pre-oxidation;

Step 3: preparing and dispersing the antibacterial nano microcapsule, preparing the antibacterial nano microcapsule by using the compound extract or the essential oil with antibacterial activity, and then preparing the antibacterial nano microcapsule into a dispersion;

Step 4, cross-linking of the down, mixing the pre-oxidized down in step 2, the dispersion obtained in step 3, water and glutamine transaminase, and reacting, that is, obtaining.

Further, the mass ratio of water to down in step 1 is 1:40 to 60, the amount of degreaser is 3 to 5 g/L, the washing time is 30 min, and the temperature is 30 to 50 °C.

Further, the degreasing agent is a nonionic surfactant selected from the group consisting of fatty alcohol polyoxyethylene ether, ethylene diamine polyoxyethylene polyoxypropylene block polyether, polysiloxane polyether copolymer, alkyl alcohol amide or One or more of alkyl glycosides 1618.

Further, the mass ratio of water to down in step 2 is 1:20 to 40, the amount of oxidizing agent is 1 to 2 g/L, the pre-oxidation time is 30 min, the temperature is 20 to 25 ° C, and the pH is 3.5.

Further, the oxidizing agent is H ₂ O ₂ .

Further, the wall material of the antimicrobial nanocapsule in step 3 is selected from the group consisting of casein, gelatin, soy protein or whey protein.

Further, the plant extract or essential oil having antibacterial activity is thyme, clove, cinnamon, star anise, cypress, mugwort, aloe, licorice, tea, pomegranate peel, berberine, Litsea cubeba, rosemary, surimi Extracts of grass, rhubarb, astragalus, Daqingye, Phellodendron, Scrophulariaceae, Forsythia, Zhimu, Verbena, Wumei, Pulsatilla, Capillaris or dandelion or essential oils.

Further, the mass fraction of the antimicrobial nanocapsules in the dispersion obtained in the step 3 is 10 to 20%.

Further, the dispersing agent in the dispersion obtained in the step 3 is used in an amount of 1 to 3% by mass of the antibacterial nanocapsule, and the dispersing agent is selected from sodium hexametaphosphate, glyceryl stearate or stearate.

Further, in step 4, the mass ratio of the dispersion, the down, and the water is 0.1 to 0.2:1:10 to 20, the amount of the glutamine transaminase is 0.3 to 0.5 g/L, the reaction temperature is 45 to 55 ° C, and the reaction time is 1h.

Beneficial effects:

1. The micro-capsule coating technology is used to make the natural antibacterial agent into the antibacterial nano microcapsule, and then the antibacterial nano microcapsule is treated and bonded to the pre-oxidized down fiber, and the antibacterial agent is directly treated by the adhesive to the conventional one. Compared with the technique of down fiber, the down fiber of the invention has a longer-lasting antibacterial effect and a longer-lasting antibacterial property by utilizing the sustained release property of the microcapsule coating technology, and at the same time, the natural antibacterial agent is preferable to the conventional inorganic and organic. Synthetic antibacterial agents are more environmentally friendly and have less impact on human health.

2. The microcapsule wall material of the present invention is preferably a natural protein as a raw material, and the microcapsule particles are grafted onto the surface of the down fiber by the enzymatic crosslinking reaction of glutamine transaminase, and the combination between the microcapsule and the down fiber is more firm. It can further enhance the antibacterial effect of natural antibacterial agents and improve the utilization efficiency of antibacterial agents. In addition, glutamine transaminase can also catalyze the enzymatic cross-linking reaction between down-protein fibers, which can prevent the fluffiness of down fibers due to pre-oxidation pretreatment.

Detailed ways

The invention will now be further described in detail by way of specific embodiments. However, those skilled in the art will understand that the following examples are merely illustrative of the invention and should not be construed as limiting the scope of the invention. Where specific techniques or conditions are not indicated in the examples, they are carried out according to the techniques or conditions described in the literature in the art or in accordance with the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are conventional products that can be obtained commercially.

Example 1

A preparation method of antibacterial down, comprising the following steps:

Step 1. Water washing: A mixture of water and down mass ratio of 40:1 was added to a water washing machine, and a degreaser fatty alcohol polyoxyethylene ether 3 g/L was added thereto at a temperature of 30 ° C and washed with water for 30 minutes.

Step 2, pre-oxidation: the water-washed down is added to the water washing machine according to the mass ratio of water and down, and the amount of H ₂ O ₂ added is 1 g/L, the temperature is room temperature, the pH is 3.5, and the rotation is performed. 30min.

Step 3: Preparation and dispersion of microcapsules: Antibacterial microcapsules are prepared by a multiphase emulsion method, the microcapsule wall material is casein, and the core material is a mixture of essential oils of thyme, clove, cinnamon and anise, in a ratio of 1:1:1: 1. The prepared natural antibacterial microcapsules were dispersed on an ultrasonic apparatus, wherein the mass fraction of the microcapsules was 10%, and the amount of the dispersing agent was 1% of the mass of the microcapsules.

Step 4, enzyme cross-linking: the microcapsule auxiliary, pre-oxidized down and water are added to the washing machine in a mass ratio of 0.1:1:10, the amount of glutamine transaminase is 0.3 g/L, and the reaction temperature is 45-55. °C, the washing time is 1h.

Example 2

A preparation method of antibacterial down, comprising the following steps:

Step 1, water washing: a mixture of water and down mass ratio of 50:1 was added to a water washing machine, and a degreaser fatty alcohol polyoxyethylene ether 3 g/L was added thereto at a temperature of 30 ° C and washed with water for 30 minutes.

Step 2, pre-oxidation: the water-washed down is added to the water washing machine according to the mass ratio of water and down, and the amount of H ₂ O ₂ added is 1.5 g/L, the temperature is room temperature, and the pH is 3.5. Turn for 30min.

Step 3: Preparation and dispersion of microcapsules: Antibacterial microcapsules are prepared by a multiphase emulsion method. The microcapsule wall material is casein, and the core material is a mixture of essential oils of mugwort, aloe, licorice, tea, pomegranate peel and berberine. The ratio is 1:1:1:1:1:1. The prepared natural antibacterial microcapsules were dispersed on an ultrasonic apparatus, wherein the mass fraction of the microcapsules was 15%, and the amount of the dispersing agent was 2% of the mass of the microcapsules.

Step 4, enzyme cross-linking: the microcapsule auxiliary, pre-oxidized down and water are added to the washing machine in a mass ratio of 0.15:1:15, the amount of glutamine transaminase is 0.3 g/L, and the reaction temperature is 45-55. °C, the washing time is 1h.

Example 3

A preparation method of antibacterial down, comprising the following steps:

Step 1. Water washing: A mixture of water and down mass ratio of 60:1 was added to a water washing machine, and a degreaser fatty alcohol polyoxyethylene ether 3 g/L was added thereto at a temperature of 30 ° C and washed with water for 30 minutes.

Step 2, pre-oxidation: the water-washed down is added to the water washing machine according to the mass ratio of water and down, and the amount of H ₂ O ₂ added is 2 g/L, the temperature is room temperature, the pH is 3.5, and the rotation is performed. 30min.

Step 3: Preparation and dispersion of microcapsules: Antibacterial microcapsules are prepared by a multiphase emulsion method, the microcapsule wall material is casein, and the core material is a mixture of essential oils of Cork, Scrophulariaceae, Forsythia, Anemarrhena, Verbena, and Wumei. The ratio is 1:1:1:1:1:1. The prepared natural antibacterial microcapsules were dispersed on an ultrasonic apparatus, wherein the mass fraction of the microcapsules was 20%, and the amount of the dispersing agent was 3% of the mass of the microcapsules.

Step 4, enzyme cross-linking: the microcapsule auxiliary, pre-oxidized down and water are added to the washing machine in a mass ratio of 0.2:1:20, the amount of glutamine transaminase is 0.3 g/L, and the reaction temperature is 45-55. °C, the washing time is 1h.

Comparative Example 1

The difference from Embodiment 1 is that the down is not subjected to the pre-oxidation treatment.

A preparation method of antibacterial down, comprising the following steps:

Step 1, water washing: a mixture of water and down mass ratio of 40:1 is added to the water washing machine, and a degreaser ethylenediamine polyoxyethylene polyoxypropylene block type polyether 4g/L is added, the temperature is 30 ° C, and the water is washed for 30 minutes. .

Step 2: Preparation and dispersion of microcapsules: Antibacterial microcapsules are prepared by a multiphase emulsion method. The microcapsule wall material is casein, and the core material is a mixture of essential oils of thyme, clove, cinnamon and anise, in a ratio of 1:1:1: 1. The prepared natural antibacterial microcapsules were dispersed on an ultrasonic apparatus, wherein the mass fraction of the microcapsules was 10%, and the amount of the dispersing agent was 1% of the mass of the microcapsules.

Step 3, enzyme cross-linking: the microcapsule auxiliary, pre-oxidized down and water are added to the washing machine in a mass ratio of 0.1:1:10, the amount of glutamine transaminase is 0.3 g/L, and the reaction temperature is 45-55. °C, the washing time is 1h.

Comparative Example 2

The difference from Example 2 is that no chemical cross-linking agent glutamine transaminase is added in step 2.

A preparation method of antibacterial down, comprising the following steps:

Step 4: The microcapsule auxiliary, pre-oxidized down and water were added to a water washing machine at a mass ratio of 0.15:1:15, the reaction temperature was 45-55 ° C, and the water washing time was 1 h.

Comparative Example 3

The difference from the embodiment 3 is that the antibacterial finishing liquid (without microcapsule coating) is directly added in the step 3, and the amount of the finishing liquid is the same as that of the microcapsule-coated core material of the embodiment 3.

A preparation method of antibacterial down, comprising the following steps:

Step 3: Antibacterial finishing liquid configuration: mixing the essential oils of mugwort, aloe vera, licorice, tea, pomegranate peel and berberine, and the ratio is 1:1:1:1:1:1 to form a finishing liquid.

Step 3, enzyme cross-linking: the antibacterial finishing liquid, the pre-oxidized down and water are added to the washing machine in a mass ratio of 0.1:1:10, the amount of glutamine transaminase is 0.3 g/L, and the reaction temperature is 45-55 ° C. The washing time is 1h.

The fluffiness of down is tested according to the national standard GB/T14272-2002 and the industry standard FZ/T81002-2002. Antibacterial properties of down fiber The antibacterial rate of down fiber in the examples and the comparative examples was tested by the GB/T 20944.3 standard method. The results are shown in the following table:

It can be seen from the data in the above table that after the pre-oxidized down finishing antibacterial microcapsules and the enzymatic crosslinking reaction by adding glutamine transaminase, the down has good antibacterial and antibacterial properties, and the fluffiness of the finished down is also achieved. There is also a certain degree of improvement; after the microcapsule-coated antibacterial liquid is finished onto the down, the antibacterial and antibacterial effect of the down is better, and the antibacterial effect is more durable; after 10 times of washing, the down still maintains good antibacterial properties, The bacteria performance is more durable. In addition, the pre-oxidation of the down and the enzymatic cross-linking of glutamine transaminase help to improve the antibacterial and antibacterial properties of the down, because the pre-oxidation enhances the reactivity of the surface material and increases the fixation rate of the microcapsules. The enzymatic cross-linking reaction of glutamine transaminase causes a graft reaction between the microcapsule wall material and the down, which can improve the fixing efficiency of the microcapsule and improve the antibacterial property of the down.

Claims

The invention discloses a preparation method of antibacterial down, which comprises the following steps:

Step 1, the cleaning of the down, mixing the down, water and degreasing agent, and washing with water;

Step 2, pre-oxidation of the down, mixing the down, water and oxidant after washing in step 1 to perform pre-oxidation;

Step 3: preparing and dispersing the antibacterial nano microcapsule, and preparing the antibacterial nano-capsule by using the compound extract or the essential oil with antibacterial activity, and then making the antibacterial nano microcapsule into a dispersion;

Step 4, cross-linking of the down, mixing the pre-oxidized down in step 2, the dispersion obtained in step 3, water and glutamine transaminase, and reacting, that is, obtaining.
The method for preparing an antibacterial down according to claim 1, wherein the mass ratio of water to down in step 1 is 1:40 to 60, the amount of degreaser is 3 to 5 g/L, and the washing time is 30 min. It is 30 to 50 °C.
The method for preparing an antibacterial down according to claim 1, wherein the degreasing agent is a nonionic surfactant selected from the group consisting of fatty alcohol polyoxyethylene ethers, ethylenediamine polyoxyethylene polyoxypropylene block polyethers, One or more of a polysiloxane polyether copolymer, an alkyl alcohol amide or an alkyl glycoside 1618.
The method for preparing an antibacterial down according to claim 1, wherein the mass ratio of water to down in step 2 is 1:20-40, the amount of oxidant is 1-2 g/L, the oxidation time is 30 min, and the temperature is 20 to 25 ° C, pH is 3.5.
The method of preparing an antibacterial down according to claim 1, wherein the oxidizing agent is H2O2.
The method for preparing an antibacterial down according to claim 1, wherein the wall material of the antibacterial nanocapsule in step 3 is selected from the group consisting of casein, gelatin, soy protein or whey protein.
The method for preparing an antibacterial down according to claim 1, wherein the antibacterial activity plant extract or essential oil is thyme, clove, cinnamon, anise, cypress, mugwort, aloe vera, licorice, tea, pomegranate Extracts of Pi, Huanglian, Litsea cube, Rosemary, Houttuynia, Rhubarb, Astragalus, Daqingye, Phellodendron, Scrophulariaceae, Forsythia, Zhimu, Verbena, Wumei, Pulsatilla, Capillaris or Dandelion Or essential oils.
The method for preparing an antibacterial down according to claim 1, wherein the mass fraction of the antibacterial nanocapsules in the dispersion obtained in the step 3 is 10 to 20%.
The method for preparing an antibacterial down according to claim 1, wherein the dispersing agent in the dispersion obtained in the step 3 accounts for 1 to 3% of the mass fraction of the antibacterial nanocapsule, and the dispersing agent is selected from the group consisting of sodium hexametaphosphate. , glyceryl stearate or stearate.
The method for preparing an antibacterial down according to claim 1, wherein the mass ratio of the dispersion, the down, and the water in the step 4 is 0.1 to 0.2:1:10 to 20, and the amount of the glutamine transaminase is 0.3 to 0.5. g/L, reaction temperature 45-55 ° C, reaction time 1 h.