CN107641970B - Animal fiber containing microcapsule and preparation method thereof - Google Patents
Animal fiber containing microcapsule and preparation method thereof Download PDFInfo
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- CN107641970B CN107641970B CN201711056318.1A CN201711056318A CN107641970B CN 107641970 B CN107641970 B CN 107641970B CN 201711056318 A CN201711056318 A CN 201711056318A CN 107641970 B CN107641970 B CN 107641970B
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Abstract
The invention discloses a preparation method of animal fiber containing microcapsules, which comprises the following steps of 1) preparing microcapsules containing traditional Chinese medicine essential oil: 2) removing cutin from animal fiber, and refining; 3) and (2) circularly heating the suspension of the microcapsules obtained in the step 1) in water and the animal fibers obtained in the step 2), preserving heat, cooling and the like, and drying to obtain the animal fibers containing the microcapsules. The invention also discloses the animal fiber containing the microcapsule prepared by the method, the microcapsule is filled into the animal fiber with the hollow structure through repeated and cyclic heating, heat preservation, cooling and soaking treatment, the filling rate is high, the toughness and the strength are high, the microcapsule is washing-resistant and is not easy to fall off, after the traditional Chinese medicine essential oil in the microcapsule is completely volatilized, the filling can be repeated, and the cost is saved.
Description
Technical Field
The invention relates to the field of animal fibers, in particular to an animal fiber containing microcapsules and a preparation method thereof.
Background
The microcapsule technology is a technology for coating solid or liquid with a film-forming material to form micro-particles, in the microcapsule, the capsule core is separated from the external environment by the capsule wall, so that the influence of external moisture, oxygen, acidity, ultraviolet rays and other factors can be avoided, the physicochemical properties of the microcapsule can be effectively maintained, and the components in the capsule core can be released by selecting a proper capsule wall material under a specific condition. At present, various microcapsules containing functional components are often added into fibers to enable the fibers to have corresponding functions, and common microcapsule filling methods include: 1. the adhering method is that the microcapsule and glue are mixed and adhered to natural fiber or artificial fiber; 2. the embedding method is that the artificial fiber is added with the microcapsule before forming the fiber, and the microcapsule is embedded in the fiber. The above two methods have some disadvantages, for example, when the attachment and adhesion method is used, because the microcapsule is attached to the surface of the fiber, it is easy to drop when washing or friction is generated, when the embedding method is used, because the microcapsule is added to the raw material of the artificial fiber, the firmness of the artificial fiber after molding is affected, and the fiber is easy to break. The above-mentioned method has the defect that the application of the fiber containing the microcapsule in real life is limited.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide animal fiber containing microcapsules and a preparation method thereof.
The purpose of the invention is realized by adopting the following technical scheme:
a method for preparing animal fiber containing microcapsule comprises the following steps:
1) preparing microcapsules: adding an emulsifier into the capsule wall material and the capsule core material for emulsification, adding an initiator for chemical reaction, and coating the capsule core material in the capsule wall material by adopting a chemical in-situ coating method to obtain microcapsules;
2) removing cutin from animal fiber, and refining;
3) adding the microcapsules prepared in the step 1) into water to form a microcapsule suspension, heating the microcapsule suspension at the speed of 2-3 ℃/min, carrying out flowing soaking on the animal fibers treated in the step 2) at the flow rate of 0.2-0.5 m/s, heating the microcapsule suspension to 70-80 ℃, carrying out heat preservation soaking for two hours, cooling to room temperature at the speed of 2-3 ℃/min, repeating the heating, heat preservation and cooling processes for 4 times to complete soaking, and filling the microcapsules into a hollow structure of the animal fibers;
4) dehydrating the animal fiber treated in the step 3) at normal temperature, and drying at 80 ℃ to obtain the animal fiber containing the microcapsules.
Further, the mass concentration of the microcapsule suspension in the step 3) is 25%.
Further, the particle size of the microcapsule is 0.8-53 μm.
Further, the animal fiber is a hair fiber or a silk fiber having a hollow structure.
Further, the hair fiber is one of wool or rabbit hair.
Further, the silk fiber is silk.
Further, the length of the silk is 3-20 cm.
Further, the emulsifier is alkylphenol polyoxyethylene ether, and the initiator is azobisisobutyronitrile.
Further, the microcapsule wall material is melamine resin, the capsule core material is traditional Chinese medicine essential oil, and the mass ratio of the melamine resin to the capsule core is as follows: 1: 1-2.
An animal fiber containing microcapsule is prepared by the above preparation method.
Compared with the prior art, the invention has the beneficial effects that: the invention provides animal fiber containing microcapsules and a preparation method thereof, wherein proper heating and cooling rates, heat preservation time and flow rate are limited through repeated cyclic heating and dynamic soaking treatment, the microcapsules are filled into the animal fiber with a hollow structure, the filling rate of the microcapsules is high, the original structure of the fiber is not damaged, the fiber can keep better toughness and strength, is washing-resistant and is not easy to fall off, the service life of Chinese herbal medicine essential oil in the microcapsules is better protected and prolonged through the tube wall of the fiber, the filling can be repeated after the Chinese herbal medicine essential oil in the microcapsules is completely volatilized, the utilization rate of raw materials is improved, and the cost is saved.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
In the present invention, all percentages are by weight unless otherwise specified, and the equipment and materials used are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art, unless otherwise specified.
Example 1
The preparation method of the animal fiber containing the microcapsule comprises the following specific operation steps:
1) preparing microcapsules containing traditional Chinese medicine essential oil: weighing 50g of melamine resin serving as a capsule wall material and 150g of Chinese herbal medicine essential oil serving as a capsule core material with the mass concentration of 30% and adding the mixture into an emulsifier alkylphenol polyoxyethylene ether for emulsification, emulsifying at normal temperature for 30min, adding an initiator azobisisobutyronitrile for chemical reaction, and coating the Chinese herbal medicine essential oil in the melamine resin wall material by adopting a chemical in-situ coating method to obtain a microcapsule containing the Chinese herbal medicine essential oil;
2) removing cutin of silk by using industrial hydrogen peroxide and refining;
3) adding the microcapsules prepared in the step 1) into water to form a microcapsule suspension with the mass concentration of 25%, heating the microcapsule suspension at the speed of 2 ℃/min, carrying out flowing soaking on the silk processed in the step 2) at the flow rate of 0.2m/s, heating the microcapsule suspension to 70 ℃, carrying out heat preservation soaking for two hours, cooling to room temperature at the speed of 2 ℃/min, repeating the heating, heat preservation and cooling processes for 4 times to complete soaking, and continuing the thermal cycle process for 48 hours;
4) dehydrating the silk treated in the step 3) at normal temperature, and drying at 80 ℃ to obtain the silk containing microcapsules.
Example 2
The preparation method of the animal fiber containing the microcapsule comprises the following specific operation steps:
1) preparing microcapsules containing traditional Chinese medicine essential oil: weighing 60g of melamine resin serving as a capsule wall material and 240g of Chinese herbal medicine essential oil serving as a capsule core material with the mass concentration of 30%, adding an emulsifier alkylphenol polyoxyethylene ether for emulsification, emulsifying at normal temperature for 30min, adding an initiator azobisisobutyronitrile for chemical reaction, and coating the Chinese herbal medicine essential oil in the melamine resin wall material by adopting a chemical in-situ coating method to obtain microcapsules containing the Chinese herbal medicine essential oil;
2) refining the rabbit hair by using a sulfuric acid solution to remove cutin;
3) adding the microcapsules prepared in the step 1) into water to form a microcapsule suspension with the mass concentration of 25%, heating the microcapsule suspension at the speed of 2.5 ℃/min, carrying out flowing soaking on the rabbit hair processed in the step 2) at the flow rate of 0.5m/s, heating the microcapsule suspension to 75 ℃, carrying out heat preservation soaking for two hours, cooling to room temperature at the speed of 2 ℃/min, repeating the heating, heat preservation and cooling processes for 4 times to complete soaking, and continuing the thermal cycle process for 48 hours;
4) dehydrating the rabbit hair treated in the step 3) at normal temperature, and drying at 80 ℃ to obtain the rabbit hair containing the microcapsules.
Example 3
The preparation method of the animal fiber containing the microcapsule comprises the following specific operation steps:
1) preparing microcapsules containing traditional Chinese medicine essential oil: weighing 120g of melamine resin serving as a capsule wall material and 600g of Chinese herbal medicine essential oil serving as a capsule core material with the mass concentration of 30% and adding the mixture into an emulsifier alkylphenol ethoxylate for emulsification, emulsifying at normal temperature for 30min, adding an initiator azobisisobutyronitrile for chemical reaction, and coating the Chinese herbal medicine essential oil in the melamine resin wall material by adopting a chemical in-situ coating method to obtain a microcapsule containing the Chinese herbal medicine essential oil;
2) carrying out cutin removal refining on wool by using a hydrochloric acid solution;
3) adding the microcapsules prepared in the step 1) into water to form a microcapsule suspension with the mass concentration of 25%, heating the microcapsule suspension at the speed of 3 ℃/min, carrying out flowing soaking on the wool processed in the step 2) at the flow rate of 0.4m/s, heating the microcapsule suspension to 80 ℃, carrying out heat preservation soaking for two hours, cooling to room temperature at the speed of 3 ℃/min, repeating the heating, heat preservation and cooling processes for 4 times to complete soaking, and carrying out the thermal cycle process for 48 hours;
4) dehydrating the wool treated in the step 3) at normal temperature, and drying at 80 ℃ to obtain the wool containing microcapsules.
Comparative example 1
The comparative example is silk with microcapsules adhered to the surface of the silk by an adhesion method to obtain the silk with microcapsules adhered to the surface.
Comparative example 2
The difference between the fibers of the comparative example and the fibers of the example 1 is that the suspension containing the microcapsules in the step 3) of the preparation process of the fibers of the comparative example is added into silk at one time, does not flow and keeps static, and the silk is soaked, and the circulation processes of temperature rise, heat preservation, temperature reduction and the like are the same as the example 1.
Comparative example 3
The difference between the comparative example fiber and the example 1 is that the microcapsule suspension is heated to 70 ℃ and then is soaked in a heat preservation way in the step 3) in the preparation process of the comparative example fiber, the soaking time is the same as the total soaking time of the example 1, the cyclic cooling, heat preservation and heating treatment are not carried out in the soaking process, the soaking temperature is kept at 70 ℃, and the rest is the same.
The dry strengths of the fibers of examples 1 to 3 and comparative example 1, comparative example 2 and comparative example 3 were measured using a YG001B type single fiber strength machine according to GB/T14337-.
The silk in the embodiment 1, the comparison example 2 and the comparison example 3 is respectively weighed before and after filling the microcapsule, the filling rate is judged according to the increase degree of the mass, the filling rate of the embodiment 1 is found to be more than the comparison example 2 and the comparison example 3 through weighing, and the adoption of the cyclic heating, heat preservation and cooling soaking mode of the application is more beneficial to filling the microcapsule in the hollow structure of the animal fiber, and the filling rate is higher.
The test results show that the microcapsule-containing suspension is adopted to carry out specific heating and cooling rates, specific heat preservation time, specific flow rate and cyclic soaking period on the animal fibers, so that the filling rate of the microcapsules in the hollow structure of the animal fibers is improved, and meanwhile, the toughness and the strength of the animal fibers can be improved.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (4)
1. A method for preparing animal fiber containing microcapsules is characterized by comprising the following steps:
1) preparing microcapsules: adding an emulsifier into a capsule wall material and a capsule core material for emulsification, adding an initiator for chemical reaction, and coating the capsule core material in the capsule wall material by adopting a chemical in-situ coating method to obtain microcapsules, wherein the particle size of the microcapsules is 0.8-53 mu m;
2) removing cutin from animal fiber, and refining;
3) adding the microcapsules prepared in the step 1) into water to form a microcapsule suspension, wherein the mass concentration of the microcapsule suspension is 25%, heating the microcapsule suspension at a speed of 2-3 ℃/min, carrying out flowing soaking on the animal fibers treated in the step 2) at a flow speed of 0.2-0.5 m/s, heating the microcapsule suspension to 70-80 ℃, carrying out heat preservation soaking for two hours, cooling to room temperature at a speed of 2-3 ℃/min, repeating the heating, heat preservation and cooling processes for 4 times to complete soaking, and filling the microcapsules into a hollow structure of the animal fibers;
4) dehydrating the animal fiber treated in the step 3) at normal temperature, and drying at 80 ℃ to obtain animal fiber containing microcapsules;
the animal fiber is silk.
2. The process for preparing animal fiber containing microcapsule according to claim 1, wherein: the length of the silk is 3-20 cm.
3. The process for preparing animal fiber containing microcapsule according to claim 1, wherein: the emulsifier is alkylphenol polyoxyethylene ether, and the initiator is azobisisobutyronitrile.
4. The process for preparing animal fiber containing microcapsule according to claim 1, wherein: the microcapsule wall material is melamine resin, and the capsule core material is Chinese medicinal essential oil.
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JPS5217565Y2 (en) * | 1973-05-16 | 1977-04-20 | ||
JP3187987B2 (en) * | 1992-11-18 | 2001-07-16 | 亨 山本 | Sustained release fiber material and method for producing the same |
JPH06228880A (en) * | 1993-02-01 | 1994-08-16 | Kanebo Ltd | Textile structure having fragrance |
CN1286528C (en) * | 2004-07-22 | 2006-11-29 | 武汉理工大学 | Hollow fiber medicine carrier and its preparing method and use |
CN102746450B (en) * | 2012-07-25 | 2014-01-29 | 浙江理工大学 | A self-adhesive long-acting slow-release essential oil microcapsule and its preparation method and application |
CN103132313B (en) * | 2013-04-07 | 2015-01-21 | 江苏悦达纺织集团有限公司 | Filled type cotton fiber and preparation method thereof |
WO2015159219A1 (en) * | 2014-04-15 | 2015-10-22 | Canepa S.P.A. | Process for improving the chemical and/or physical properties of hollow-structure natural fibers |
CN104746350B (en) * | 2015-03-13 | 2016-08-17 | 常州大学 | A kind of palyacrylate binder containing Chinese medicine oil microcapsule and its preparation method and application |
CN105200802B (en) * | 2015-10-22 | 2017-08-22 | 江苏阳光股份有限公司 | A kind of preparation method of the fragrant atmosphere light and thin wool cloth with healthcare function |
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Effective date of registration: 20200914 Address after: 474668 east of Binhe Road, Chengdong, Nanzhao County, Nanyang City, Henan Province Applicant after: NANZHAO DONGFANG SILK DEVELOPMENT Co.,Ltd. Address before: Nanyang City, Henan province 474668 Zhen bin he Lu, Nanzhao County Nanhe Applicant before: NANZHAO BAINIANQING INDUSTRIAL Co.,Ltd. |
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