WO2011057536A1 - Antibacterial and wrinkle-proof fabric with blumea oil microcapsule and producing method thereof - Google Patents

Antibacterial and wrinkle-proof fabric with blumea oil microcapsule and producing method thereof Download PDF

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Publication number
WO2011057536A1
WO2011057536A1 PCT/CN2010/078310 CN2010078310W WO2011057536A1 WO 2011057536 A1 WO2011057536 A1 WO 2011057536A1 CN 2010078310 W CN2010078310 W CN 2010078310W WO 2011057536 A1 WO2011057536 A1 WO 2011057536A1
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Prior art keywords
fabric
wrinkle
eucalyptus oil
oil microcapsule
antibacterial
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PCT/CN2010/078310
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French (fr)
Chinese (zh)
Inventor
李鹂
区伟文
汪国成
钟慧仪
李毅
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香港理工大学
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Publication of WO2011057536A1 publication Critical patent/WO2011057536A1/en

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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M23/00Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/12Processes in which the treating agent is incorporated in microcapsules
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/20Treatment influencing the crease behaviour, the wrinkle resistance, the crease recovery or the ironing ease

Definitions

  • the invention relates to an anti-wrinkle fabric of a eucalyptus oil microcapsule and a preparation method thereof. Background technique
  • Microencapsule is a semi-permeable or hermetic microcapsule with a polymer wall shell that can embed and protect certain substances.
  • Microcapsule technology uses natural or synthetic polymeric materials (often referred to as wall materials) to encapsulate dispersed solid material particles, droplets or gases (often referred to as core materials) in a film to form tiny capsules.
  • wall materials natural or synthetic polymeric materials
  • core materials dispersed solid material particles, droplets or gases
  • a technique in which the diameter is generally from 1 to 1000 ⁇ m.
  • Microcapsules have many unique functions, such as protecting the core material from environmental influences, reducing toxicity, masking bad taste, controlling core release, prolonging the effect of the drug, extending the storage period, changing the state of matter for portability and transportation, and changing the physical properties. Incompatible ingredients are evenly mixed and other functions.
  • Ai Ye is one of the commonly used medicines in traditional Chinese medicine. It is the dry leaf of the perennial herb Ai. Ai Ye, as a commonly used traditional Chinese medicine with a long history in China, has been receiving attention for thousands of years.
  • the main active ingredient of Artemisia argyi is volatile oil, which is eucalyptus oil.
  • Ai Ye oil has antibacterial, antiviral, antitussive and antitussive, enhanced cellular immune function, hemostasis and anticoagulation, anti-allergic, sedative, liver and gallbladder, complement activation and other effects, especially It has inhibitory effects on Streptococcus pneumoniae, Staphylococcus aureus, Escherichia coli, Respiratory syncytial virus, and influenza virus.
  • Ai Ye oil is also widely used in the treatment of rheumatic pain.
  • Aiye oil has strong volatility, strong odor, unstable active ingredients, easy loss, and inconvenience in storage, transportation and various dosage forms. It limits its scope of application.
  • Textile finishing has become one of the important ways to improve the added value of products and improve the function of textiles.
  • the use of microcapsule technology to make textiles have special functions is currently a hot spot.
  • microcapsules for post-finishing of fabrics, such as aroma, flame retardant, antibacterial, deodorant, thermal storage, hair removal, anti-virus, anti-fog, anti-fouling, anti-wrinkle, anti-shrinkage, Soft, UV resistant, etc.
  • the application of microcapsule technology in textiles is mainly in the printing and finishing, most of which are applied to fibers or fabrics by coating or blending, but in the coating, the microcapsules and the fabric only pass the adhesive.
  • the physical adhesion, the washability, breathability and comfort performance are not at a practical level.
  • the object of the present invention is to provide an anti-wrinkle fabric of a eucalyptus oil microcapsule and a preparation method thereof.
  • the method combines the traditional wormwood and fabric to produce a new type of fabric, which not only can stabilize the eucalyptus oil component, control the release of eucalyptus oil, prolong the effect of the drug, mask the bad taste, and clean and hygienic, the fabric can also be made.
  • the fabric produced by the method has antibacterial health care and anti-wrinkle function.
  • a method for preparing an anti-wrinkle fabric of a eucalyptus oil microcapsule comprising the following steps:
  • the fabric is treated with the prepared eucalyptus oil microcapsule antibacterial anti-wrinkle fabric finishing agent to obtain an anti-wrinkle fabric of the eucalyptus oil microcapsule.
  • a method for preparing an anti-wrinkle fabric of a eucalyptus oil microcapsule wherein in the step 1), the wall material is a mixed solution of gelatin and gum arabic, wherein the emulsification process and conditions are: at a rotational speed of 800 5 ⁇ 5 % (w/v), the amount of eucalyptus oil and wall material is emulsified in a constant temperature water bath at 40 ° C for 10 to 15 minutes, wherein the concentration of the wall material is 0.5% ⁇ 5 % (w / v) 0 ⁇ 2. 0 ⁇ The ratio is 0. 5 ⁇ 2. 0.
  • the re-agglomeration reaction process and conditions are: adjusting the ra of the emulsification reaction system to PH3 with a 10% HAC (acetic acid) solution 5 ⁇ 4. 5, then reduce the speed, remove the system from the water bath, and continue to agglomerate at room temperature for 10 to 15 minutes.
  • the emulsification stirring speed when adjusting ra is 800 ⁇ iooo rpm, and the ra value of the system is adjusted to 3. 5 ⁇
  • a method for preparing an anti-wrinkle fabric of a eucalyptus oil microcapsule according to the present invention in step 3), The cross-linking curing reaction process and conditions are as follows: the system is cooled to 0 to 5 ° C in an ice bath, the system is adjusted to neutral with 10% HAC solution, then the curing crosslinking agent is added, and the ice bath is cured for 30 minutes. After further moving into a constant temperature water bath at 50 ° C for 2 to 3 hours, a microcapsule emulsion of eucalyptus oil was obtained.
  • the amount of the curing agent to be added varies depending on the case, and for example, it may be added in an amount of from 1 to 100 ml.
  • the curing crosslinking agent is selected from the group consisting of formaldehyde, glyoxal, glutaraldehyde or a mixture thereof.
  • the eucalyptus oil microcapsule is a spherical granule having a particle diameter of 1 to 50 ⁇ ra.
  • the amounts of the anti-wrinkle crosslinking agent, the catalyst and the penetrating agent added in the step 4) are respectively:
  • the method for producing an anti-wrinkle anti-wrinkle fabric of a eucalyptus oil microcapsule according to the present invention, wherein the anti-wrinkle cross-linking agent is selected from the group consisting of 2D resin, 2D etherified resin, tetrabutyltetracarboxylic acid, or a mixture thereof.
  • the catalyst is selected from a metal salt, an inorganic acid or a mixture thereof.
  • the metal salt is selected from the group consisting of a magnesium salt, a sodium salt and a potassium salt.
  • the inorganic acid is selected from the group consisting of hydrochloric acid and phosphoric acid.
  • the penetrating agent is a fatty alcohol polyoxyethylene ether.
  • the step 5) further includes:
  • a eucalyptus oil microcapsule antibacterial anti-wrinkle fabric wherein the antibacterial anti-wrinkle fabric is treated by the foregoing method, wherein the fabric is coated with microcapsules formed from eucalyptus oil.
  • the microcapsule of the invention uses the eucalyptus oil as the core material, the gelatin and the gum arabic as the wall material, and the micro-encapsulation of the eucalyptus oil by the complex coacervation method, the preparation process is simple and easy, and the cost is relatively high. Low, it provides microencapsulation technology suitable for industrial production for Aiyan oil microcapsules.
  • the prepared microcapsules have a particle size ranging from 1 to 50 ⁇ m, and have a good appearance and a smooth spherical shape, and have good coating effect, dispersibility and sustained release property.
  • the eucalyptus oil microcapsule antibacterial fabric of the invention is prepared by using a eucalyptus oil microcapsule emulsion, an anti-wrinkle cross-linking agent, a catalyst and a penetrating agent as a fabric finishing agent, and adopting a padding finishing process to prepare the cotton and linen fabric. Since there are many reactive hydroxyl groups on the surface of the gelatin-arabino microcapsules, and the particle size of the microcapsules is small enough, the soaking and adhering not only on the surface of the yarn but also penetrates and adheres to the surface of each fiber constituting the yarn, permeating.
  • an anti-wrinkle cross-linking agent such as 2D resin
  • cross-link the reaction between the anti-wrinkle cross-linking agent and the cotton-wool fabric and the eucalyptus oil microcapsules by the action of the catalyst.
  • Forming an ether bond connection thereby overcoming the disadvantage of poor adhesion resistance of the adhesive, greatly improving the adhesion effect of the fabric and the microcapsule, enhancing the durability of the antibacterial function, and imparting anti-wrinkle and ironing resistance to the fabric, and further crosslinking and etherification It also reduces the amount of formaldehyde released from 2D resin.
  • the eucalyptus oil microcapsule antibacterial fabric prepared by the technique has antibacterial and anti-inflammatory properties, promotes blood circulation, and has excellent skin.
  • the health care function at the same time, the prepared fabric also has anti-wrinkle and non-iron function, and has better washing durability. Can be used to make patients and daily care health clothing.
  • the preparation process of the eucalyptus oil microcapsule antibacterial fabric of the invention mainly comprises five steps of embedding oil emulsification reaction, re-coagulation reaction, cross-linking curing process, compounding process and fabric finishing, wherein each step is:
  • Cross-linking curing process cool down to 0 ⁇ 5 °C in ice bath, adjust pH to neutral, add curing agent for 30 minutes, then transfer to 5CTC constant temperature water bath to continue curing for 2 ⁇ 3 hours to obtain Aiye oil microcapsule emulsion;
  • Finishing process of the fabric The fabric to be finished is immersed in the above-mentioned compound finishing agent, and finished by the two-dip two-rolling process, the rolling ratio is 100%, 100 ° C drying, 150 ° C ⁇ 190 ° C Shaped baking for 2 minutes to get the Aiye oil microcapsule antibacterial fabric.
  • w/v represents mass/volume.
  • microcapsules having different particle diameters can be formed by using different wall system concentrations and different stirring speeds.
  • the wall material concentration and the stirring speed are selected according to the final needs, and the prepared microcapsules have a particle size ranging from 1 to 50 ⁇ m.
  • the method for determining the coverage of the microcapsules of the present invention accurately: 1000 g of the newly prepared eucalyptus oil microcapsule sample, and immersed in absolute ethanol for 24 hours to extract the eucalyptus oil in the microcapsule, and filtered.
  • the filtrate was determined by gas chromatography to determine the peak value of a component of the oil of the leaves of the leaves, and the standard curve of the oil of the leaves of the leaves was used to obtain the content of the leaves of the leaves, and the coverage of the microcapsules was obtained.
  • the coating ratio of the eucalyptus oil microcapsules was determined by this method to be 30% to 80%.
  • the temperature of the microcapsules of the present invention is as follows: 0. 0 ° C, humidity is 24 0 % , 0 ° O lg sample was dissolved in 5 mL of absolute ethanol soaked for 24 hours to extract the remaining eucalyptus oil in the microcapsules, and the remaining content of eucalyptus oil in the extract was determined by gas chromatography. It was found that the drug release rate of the microcapsules in the initial stage was faster, and then the release rate gradually became stable and had a good release effect.
  • the antibacterial test method for the antibacterial fabric of the eucalyptus oil microcapsule prepared by the method of the invention adopts the oscillating flask method to imitate the wearing condition of the human body, and makes the bacteria contact with the antibacterial agent in the fabric under the shaking condition (300 rpm), and shakes for l-6h. Thereafter, the percentage of bacterial reduction was calculated by bacterial culture counting to determine the magnitude of the antibacterial property.
  • the test strains were selected from the most commonly distributed Staphylococcus aureus and Escherichia coli in nature and human skin mucous membranes as representative strains.
  • the method for testing the washing durability of the fabric of the invention using 2% soapy water or a commercially available washing powder, according to the instructions, the washing liquid is prepared, the fabric is put into the washing machine and stirred, and stirred once every 10 minutes, and can be washed 0, 5, 10 20, 30, 50 times, each time should be rinsed in clean water and then stirred, and then the antibacterial rate of the washed fabric is measured.
  • the invention adopts the water extraction method (GB/T2912.1-1998) to determine the residual formaldehyde content of the finished fabric; the flatness of the fabric is determined according to the flatness test method of the fabric style test method (FZ/T 01054.6-1999); according to GB/T3819 -1997 standard, the crease recovery angle of the fabric was measured using a YGB type wrinkle tester; the rupture retention rate of the fabric was measured on a constant speed elongation machine using a burr yarn method (GB/T 3923.1-1997).
  • the eucalyptus oil microcapsule of the invention is applied to antibacterial finishing of fabrics, and can obtain an antibacterial fabric with high efficiency, broad spectrum, safety, washing resistance and certain preventive and medical effects, and also has excellent anti-wrinkle and non-scalding functions.
  • Emulsification of Artemisia argyi oil Weigh 0.50g gelatin and 0.50g gum arabic in a 250mL three-necked flask, add 100mL of distilled water, install a mechanical stirrer, put it in a 40°C water bath, stir and dissolve it, and prepare it into gelatin. A mixture of gum arabic system, the concentration is 0.5% (W / V), and then added 1. OraL Ai oil, emulsified for 10 minutes at a stirring speed of 800 rpm;
  • Re-coagulation reaction Keep the stirring speed and the bath temperature unchanged during the emulsification, gradually add 10% HAC solution to the above emulsion to adjust the pH value of the system to 4.0, reduce the stirring speed to 300 rpm, and remove Water bath, stirring at room temperature for 10 minutes;
  • Fabric Property Test The properties of the fabric produced in Example 1 were tested by the method described above. Finished cotton fabric flatness grade 3. 7, dry wrinkle recovery angle 3120, breaking strength retention rate of 68%, formaldehyde emission of 40ppm, fabric antibacterial rate and washability effect are shown in the following table:
  • Emulsification of Artemisia argyi oil Weigh 1.00g gelatin and 1. 00g gum arabic in a 250mL three-necked flask, add 100mL of distilled water, install a mechanical stirrer, put it in a 40°C water bath, stir and dissolve, add 1 OmL eucalyptus oil, emulsified for 15 minutes at a stirring speed of 800 rpm;
  • Re-coagulation reaction Keep the stirring speed and the water bath temperature unchanged during the emulsification, gradually add 10% HAC solution to the emulsion to adjust the pH of the system to 4.0, and reduce the stirring speed to 250 rpm. , remove the water bath, continue stirring at room temperature for 10 minutes;
  • Example 3 The properties of the fabrics produced in Example 2 were tested using the methods described above. After finishing, the cotton fabric has a flatness grade of 3.5, a dry wrinkle recovery angle of 2980, a breaking strength retention rate of 72%, and a formaldehyde release of 0 ppm.
  • the antibacterial rate and the washing durability of the fabric are as follows: Example 3
  • Emulsion of eucalyptus oil Weigh 5.00g gelatin and 5. 00g gum arabic in a 250mL three-necked flask, add 100mL of distilled water, install a mechanical stirrer, put it in a 40 °C water bath, stir and dissolve, add 5 0 mL of eucalyptus oil was emulsified for 20 minutes under the conditions of a stirring speed of 1000 rpm.
  • (2) agglomeration reaction maintaining the stirring speed of the emulsification and the temperature of the water bath, gradually adding 10% HAC solution to the above emulsion to adjust the ra value of the system to 4.0, and reducing the stirring speed to 600 rpm, Remove the water bath and continue stirring for 10 minutes at room temperature;
  • Fabric Property Test The properties of the fabric obtained in Example 3 were tested by the method described above.
  • the finished cotton fabric has a flatness rating of 3. 4, a dry wrinkle recovery angle of 3000, a breaking strength retention rate of 74%, and a formaldehyde release of 40 ppm.
  • the fabric antibacterial rate and water wash resistance are as follows:
  • the eucalyptus oil antibacterial anti-wrinkle fabric of the present invention has excellent antibacterial effects even after washing a plurality of times, and has a particularly excellent antibacterial effect against Staphylococcus aureus and Escherichia coli.

Abstract

A method for producing an antibacterial and wrinkle-proof fabric with blumea oil microcapsule is disclosed. The method includes: 1) emulsifying the blumea oil in an emulsifier formed by a wall material for the microcapsule, 2) complex-coacervating the emulsified blumea oil, 3) cross-linking and curing the complex-coacervated emulsion to form an emulsion containing blumea oil microcapsule, 4) adding a shrink-resistant crosslinking agent, a catalyst, and a penetrating agent to the obtained emulsion containing blumea oil microcapsule to form an antibacterial and wrinkle-proof fabric finishing agent containing blumea oil microcapsule, 5) processing the fabric with the obtained finishing agent to obtain the antibacterial and wrinkle-proof fabric with blumea oil microcapsule. An antibacterial and wrinkle-proof fabric with blumea oil microcapsule, which is produced by the method, is also disclosed. The antimicrobial and wrinkle-proof fabric with blumea oil microcapsule has antibacterial and antiphlogistic function, shrink-resistance, wash and wear performance, and good wash-resistance effect.

Description

一种艾叶油微胶囊抗菌防皱织物及其制备方法 技术领域  Aiye oil microcapsule antibacterial anti-wrinkle fabric and preparation method thereof
本发明涉及一种艾叶油微胶囊抗菌防皱织物及其制备方法。 背景技术  The invention relates to an anti-wrinkle fabric of a eucalyptus oil microcapsule and a preparation method thereof. Background technique
微胶囊(microencapsule )是一种能包埋和保护某些物质的具有聚合物壁 壳的半透性或密封性的微型胶囊。微胶囊技术是利用天然的或合成的高分子材 料(通常称为壁材)把分散的固体物质颗粒、 液滴或气体(通常称为芯材)包 封在一层膜中从而形成微小胶囊的一种技术, 它的直径一般为 1〜1000μιιι。 微 胶囊具有许多独特的功能, 如具有保护芯材物质免受环境影响, 降低毒性, 掩 蔽不良味道, 控制芯材释放, 延长药效, 延长存储期, 改变物态便于携带和运 输, 改变物性使不相容的成分均匀混合等功能。这些特殊的功能使微胶囊技术 在医药、 食品、 农药、 伺料、 涂料、 油墨、 粘合剂、 化妆品、 洗涤剂、 感光材 料、 纺织品功能整理众多工业领域中得到了广泛的应用。 艾叶是中医常用药之一, 为菊科多年生草本植物艾的干燥叶。艾叶作为我 国历史悠久的常用中药, 千百年来一直受到人们的关注。艾叶的主要有效成分 是挥发性油, 即艾叶油。大量的药理研究证明艾叶油具有抗菌抗病毒、 平喘镇 咳祛痰、 增强细胞免疫功能、 止血与抗凝血、 抗过敏、 镇静、、 护肝利胆、 补 体激活等多种功效作用, 尤其对肺炎链球菌、 金黄色葡萄球菌、 大肠杆菌、 呼 吸道合胞病毒、流感病毒等均有抑制作用。此外, 艾叶油在治疗风湿痹痛方面 的应用也较为广泛。成都中医药大学孙竹娟将艾叶挥发油通过加热透入相关穴 位配合针刺治疗类风湿关节炎,进一步证明了艾叶挥发油在类风湿关节炎的治 疗过程中, 能够提高针刺改善关节疼痛、控制病情以及改善患者关节功能和生 活质量的作用。从文献报道来看, 艾叶挥发油治疗类风湿关节炎为临床治疗这 类慢性自身免疫性疾病提供了一个新的途径。 由上可知艾叶油具有抗菌消炎、 抗过敏和促进血液循环等多种功效作用, 然而艾叶油的挥发性较强, 气味较浓, 有效成分不稳定, 容易损失, 不便于贮 藏、 运输和剂型多样化, 限制了其应用范围。 近年来, 随着人民生活水平的提高, 人们对纺织品的舒适性和功能性要求 越来越高。纺织品后整理已成为提高产品附加值和改善纺织品功能的重要途径 之一 , 利用微胶囊技术使纺织品具有特种功能是目前发展的热点。 各种织物 后整理剂都可以制成微胶囊后用于织物的后整理,如芳香、阻燃、抗菌、防臭、 蓄热保温、 脱毛、 防毒、 防雾、 抗污、 防皱、 防缩、 柔软、 防紫外线等。 微胶囊技术在纺织上的应用主要是在印染和后整理方面,绝大多数以涂层或共 混纺丝的方式施加于纤维或织物上,但在涂层中微胶囊与织物仅仅通过粘接剂 的物理粘接, 其耐洗性、透气性及舒适性能均达不到可以实用的水平。如中国 专利 CN 85100799 A提供的浸渍微胶囊织物及中国专利 CN 1966849A提供的无 机包覆纳米载银抗菌复合聚脲微胶囊防蚊面料。而共混纺丝投资设备巨大, 技 术含量高, 尚未得到大规模推广。 发明内容 Microencapsule is a semi-permeable or hermetic microcapsule with a polymer wall shell that can embed and protect certain substances. Microcapsule technology uses natural or synthetic polymeric materials (often referred to as wall materials) to encapsulate dispersed solid material particles, droplets or gases (often referred to as core materials) in a film to form tiny capsules. A technique in which the diameter is generally from 1 to 1000 μm. Microcapsules have many unique functions, such as protecting the core material from environmental influences, reducing toxicity, masking bad taste, controlling core release, prolonging the effect of the drug, extending the storage period, changing the state of matter for portability and transportation, and changing the physical properties. Incompatible ingredients are evenly mixed and other functions. These special features make microcapsule technology widely used in many industrial fields such as medicine, food, pesticides, materials, coatings, inks, adhesives, cosmetics, detergents, photographic materials, and textile finishing. Ai Ye is one of the commonly used medicines in traditional Chinese medicine. It is the dry leaf of the perennial herb Ai. Ai Ye, as a commonly used traditional Chinese medicine with a long history in China, has been receiving attention for thousands of years. The main active ingredient of Artemisia argyi is volatile oil, which is eucalyptus oil. A large number of pharmacological studies have proven that Ai Ye oil has antibacterial, antiviral, antitussive and antitussive, enhanced cellular immune function, hemostasis and anticoagulation, anti-allergic, sedative, liver and gallbladder, complement activation and other effects, especially It has inhibitory effects on Streptococcus pneumoniae, Staphylococcus aureus, Escherichia coli, Respiratory syncytial virus, and influenza virus. In addition, Ai Ye oil is also widely used in the treatment of rheumatic pain. Sun Zhujuan of Chengdu University of Traditional Chinese Medicine has treated the volatile oil of Artemisia argyi with heat and penetrated into relevant acupuncture points to treat rheumatoid arthritis, which further proves that the volatile oil of Artemisia argyi in rheumatoid arthritis During the treatment, it can improve the effect of acupuncture on improving joint pain, controlling the condition and improving the joint function and quality of life of patients. According to literature reports, the treatment of rheumatoid arthritis with volatile oil of Artemisia argyi provides a new way for clinical treatment of such chronic autoimmune diseases. It can be seen from the above that Ai Ye oil has many functions such as antibacterial, anti-allergic, anti-allergic and promoting blood circulation. However, Aiye oil has strong volatility, strong odor, unstable active ingredients, easy loss, and inconvenience in storage, transportation and various dosage forms. It limits its scope of application. In recent years, with the improvement of people's living standards, people have become more and more demanding for the comfort and functionality of textiles. Textile finishing has become one of the important ways to improve the added value of products and improve the function of textiles. The use of microcapsule technology to make textiles have special functions is currently a hot spot. Various fabric finishing agents can be used as microcapsules for post-finishing of fabrics, such as aroma, flame retardant, antibacterial, deodorant, thermal storage, hair removal, anti-virus, anti-fog, anti-fouling, anti-wrinkle, anti-shrinkage, Soft, UV resistant, etc. The application of microcapsule technology in textiles is mainly in the printing and finishing, most of which are applied to fibers or fabrics by coating or blending, but in the coating, the microcapsules and the fabric only pass the adhesive. The physical adhesion, the washability, breathability and comfort performance are not at a practical level. Such as the impregnated microcapsule fabric provided by Chinese patent CN 85100799 A and the inorganic coated nano-silver antibacterial composite polyurea microcapsule anti-mosquito fabric provided by Chinese patent CN 1966849A. The blending and spinning investment equipment is huge and has high technical content, which has not been widely promoted. Summary of the invention
本发明的目的在于提供一种艾叶油微胶囊抗菌防皱织物及其制备方法。该 方法将传统的艾叶和织物相结合, 从而产生一种新型的织物, 不仅能达到稳定 艾叶油成分, 控制艾叶油释放、 延长药效, 掩蔽不良味道, 干净卫生的作用, 此织物还可以制作成衣物, 医疗用品以及其他纺织品, 使得传统的艾灸, 艾敷 等治疗方法, 通过纺织品这个媒介, 产生一种新的治疗和保健方法; 采用所述 的方法制得的织物具有抗菌保健和防皱功能。 The object of the present invention is to provide an anti-wrinkle fabric of a eucalyptus oil microcapsule and a preparation method thereof. The method combines the traditional wormwood and fabric to produce a new type of fabric, which not only can stabilize the eucalyptus oil component, control the release of eucalyptus oil, prolong the effect of the drug, mask the bad taste, and clean and hygienic, the fabric can also be made. Into clothing, medical supplies and other textiles, so that traditional moxibustion, Aifu and other treatments, through the medium of textiles, to create a new treatment and health care methods; The fabric produced by the method has antibacterial health care and anti-wrinkle function.
为此, 本发明采用以下的技术方案: 一种艾叶油微胶囊抗菌防皱织物的制 备方法, 其中, 所述的方法包括以下步骤:  To this end, the present invention adopts the following technical solution: A method for preparing an anti-wrinkle fabric of a eucalyptus oil microcapsule, wherein the method comprises the following steps:
1 ) 在以壁材形成的乳化剂中乳化艾叶油;  1) emulsifying eucalyptus oil in an emulsifier formed of a wall material;
2 ) 使乳化的艾叶油发生复凝聚反应;  2) re-agglomerating the emulsified eucalyptus oil;
3 ) 在乳化剂中加入固化交联剂, 交联固化复凝聚反应后的乳液, 以得到 艾叶油微胶囊乳液;  3) adding a curing crosslinking agent to the emulsifier, crosslinking and curing the emulsion after the re-agglomeration reaction to obtain a eucalyptus oil microcapsule emulsion;
4 ) 在得到的艾叶油微胶囊乳液中加入反应量的防皱交联剂、 催化剂和渗 透剂, 以制成艾叶油微胶囊抗菌防皱织物整理剂;  4) adding a reactive anti-wrinkle cross-linking agent, a catalyst and a penetrating agent to the obtained eucalyptus oil microcapsule emulsion to prepare an anti-wrinkle fabric finishing agent for the eucalyptus oil microcapsule;
5 ) 将织物用制成的艾叶油微胶囊抗菌防皱织物整理剂进行处理以得到艾 叶油微胶囊抗菌防皱织物。  5) The fabric is treated with the prepared eucalyptus oil microcapsule antibacterial anti-wrinkle fabric finishing agent to obtain an anti-wrinkle fabric of the eucalyptus oil microcapsule.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法, 在步骤 1 ) 中, 所 述的壁材是明胶和阿拉伯胶的混合溶液,其中所述的乳化过程和条件为:在转 速为 800〜1000转 /分, 恒温水浴 40°C的条件下乳化 10〜15分钟, 其中, 所 述的壁材的浓度为 0. 5 %〜5 % (w/v),艾叶油与壁材的用量比例为 0. 5〜2. 0。  A method for preparing an anti-wrinkle fabric of a eucalyptus oil microcapsule according to the present invention, wherein in the step 1), the wall material is a mixed solution of gelatin and gum arabic, wherein the emulsification process and conditions are: at a rotational speed of 800 5〜〜5 % (w/v), the amount of eucalyptus oil and wall material is emulsified in a constant temperature water bath at 40 ° C for 10 to 15 minutes, wherein the concentration of the wall material is 0.5% ~ 5 % (w / v) 0〜2. 0。 The ratio is 0. 5~2. 0.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法, 在步骤 2) 中, 所 述的复凝聚反应过程和条件为: 用 IO%HAC (乙酸)溶液把乳化反应体系的 ra 调至 PH3. 5〜4. 5, 然后降低转速, 把系统移出水浴, 继续在室温搅拌进行复 凝聚 10〜15分钟。  The preparation method of the anti-wrinkle fabric of the eucalyptus oil microcapsule according to the present invention, in the step 2), the re-agglomeration reaction process and conditions are: adjusting the ra of the emulsification reaction system to PH3 with a 10% HAC (acetic acid) solution 5~4. 5, then reduce the speed, remove the system from the water bath, and continue to agglomerate at room temperature for 10 to 15 minutes.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法,在复凝聚反应过程 中,调节 ra时的乳化搅拌速度为 800〜iooo转 /分,在把系统 ra值调至 3. 5〜 According to the preparation method of the anti-wrinkle fabric of the eucalyptus oil microcapsule according to the present invention, in the process of the re-coagulation reaction, the emulsification stirring speed when adjusting ra is 800~iooo rpm, and the ra value of the system is adjusted to 3. 5~
4. 5后, 把搅拌速度降低到 250〜400 转 /分。 After 4. 5, reduce the stirring speed to 250~400 rpm.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法, 在步 3 ) 中, 所述 的交联固化反应过程和条件为: 采用冰浴将系统降温至 0〜5°C, 用 10 %HAC 溶液把系统的 ra调节至中性, 接着加入固化交联剂, 冰浴固化 30分钟, 再移 入 50°C恒温水浴继续固化 2〜3小时后, 得到艾叶油微胶囊乳液。 其中加入的 固化剂的量随不同情况而定, 例如可以加入的量为 l_100ml。 A method for preparing an anti-wrinkle fabric of a eucalyptus oil microcapsule according to the present invention, in step 3), The cross-linking curing reaction process and conditions are as follows: the system is cooled to 0 to 5 ° C in an ice bath, the system is adjusted to neutral with 10% HAC solution, then the curing crosslinking agent is added, and the ice bath is cured for 30 minutes. After further moving into a constant temperature water bath at 50 ° C for 2 to 3 hours, a microcapsule emulsion of eucalyptus oil was obtained. The amount of the curing agent to be added varies depending on the case, and for example, it may be added in an amount of from 1 to 100 ml.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法,所述的固化交联剂 选自甲醛、 乙二醛、 戊二醛或其混合物。  According to the preparation method of the eucalyptus oil microcapsule antibacterial anti-wrinkle fabric according to the present invention, the curing crosslinking agent is selected from the group consisting of formaldehyde, glyoxal, glutaraldehyde or a mixture thereof.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法,在所述制成的艾叶 油微胶囊乳液中, 艾叶油微胶囊为球形颗粒, 其粒径在 1-50 μ ra之间。  According to the preparation method of the eucalyptus oil microcapsule antibacterial anti-wrinkle fabric according to the present invention, in the prepared eucalyptus oil microcapsule emulsion, the eucalyptus oil microcapsule is a spherical granule having a particle diameter of 1 to 50 μ ra.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法, 在步骤 4) 中加入 的防皱交联剂、 催化剂和渗透剂的量分别为:  According to the method for preparing an anti-wrinkle fabric of a eucalyptus oil microcapsule according to the present invention, the amounts of the anti-wrinkle crosslinking agent, the catalyst and the penetrating agent added in the step 4) are respectively:
3-20% (w/v) 的防皱交联剂;  3-20% (w/v) anti-wrinkle crosslinker;
1-3% (w/v) 的催化剂;  1-3% (w/v) of catalyst;
0. 5-1. 5% (w/v) 的渗透剂。  0. 5-1. 5% (w/v) penetrant.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法, 所述的防皱交联 剂选自 2D树脂、 2D醚化树脂、 丁垸四羧酸中或其混合物。  The method for producing an anti-wrinkle anti-wrinkle fabric of a eucalyptus oil microcapsule according to the present invention, wherein the anti-wrinkle cross-linking agent is selected from the group consisting of 2D resin, 2D etherified resin, tetrabutyltetracarboxylic acid, or a mixture thereof.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法, 所述的催化剂选 自金属盐、 无机酸或其混合物。  According to the method for producing an anti-wrinkle fabric of a eucalyptus oil microcapsule according to the present invention, the catalyst is selected from a metal salt, an inorganic acid or a mixture thereof.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法, 所述的金属盐选 自镁盐、 钠盐和钾盐。  According to the method for producing an anti-wrinkle fabric of a eucalyptus oil microcapsule according to the present invention, the metal salt is selected from the group consisting of a magnesium salt, a sodium salt and a potassium salt.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法, 所述的无机酸选 自盐酸和磷酸。  According to the method for producing an anti-wrinkle fabric of a eucalyptus oil microcapsule according to the present invention, the inorganic acid is selected from the group consisting of hydrochloric acid and phosphoric acid.
根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法, 所述的渗透剂为 脂肪醇聚氧乙烯醚。 根据本发明的艾叶油微胶囊抗菌防皱织物的制备方法, 所述的步骤 5 ) 进一步包括: According to the preparation method of the eucalyptus oil microcapsule antibacterial anti-wrinkle fabric according to the present invention, the penetrating agent is a fatty alcohol polyoxyethylene ether. According to the method for preparing an anti-wrinkle fabric of a eucalyptus oil microcapsule according to the present invention, the step 5) further includes:
a) 将织物在得到的艾叶油微胶囊抗菌防皱织物整理剂中二浸二轧; b ) 取出织物, 其中织物的带液率 70〜100 % ; a) immersing the fabric in the obtained eucalyptus oil microcapsule antibacterial anti-wrinkle fabric finishing agent; b) removing the fabric, wherein the fabric has a liquid-liquid ratio of 70-100% ;
c ) 在 85〜100°C下, 预烘 3〜5分钟;  c) pre-bake at 85~100 °C for 3~5 minutes;
d) 在 150〜190°C下, 定型焙烘 2〜5分钟;  d) at 150~190 ° C, stereotype baking for 2 to 5 minutes;
e ) 水洗后烘干, 以制成艾叶油微胶囊抗菌防皱织物。  e) Drying after washing to make antibacterial anti-wrinkle fabric of Aiye oil microcapsules.
一种艾叶油微胶囊抗菌防皱织物, 所述的抗菌防皱织物经前述的方法处 理而成, 其中, 所述的织物上包覆有以艾叶油形成的微胶囊。  A eucalyptus oil microcapsule antibacterial anti-wrinkle fabric, wherein the antibacterial anti-wrinkle fabric is treated by the foregoing method, wherein the fabric is coated with microcapsules formed from eucalyptus oil.
实施本发明具有以下有益效果: 本发明的微胶囊以艾叶油为芯材, 以明 胶和阿拉伯胶为壁材,采用复凝聚法对艾叶油进行微胶囊化, 该制备工艺简单 易行, 成本较低, 为艾叶油微胶囊提供了适合于工业化生产的微胶囊化技术。 制备出的微胶囊粒径在 1〜50 μ ιιι范围,外观形态良好,呈光滑球形,包覆效果、 分散性、 缓释性良好。 本发明的艾叶油微胶囊抗菌织物以艾叶油微胶囊乳液、 防皱交联剂、催化剂、 渗透剂为织物整理剂, 采用浸轧整理工艺对棉麻织物进 行整理而成。 由于明胶 -阿拉伯胶微胶囊表面存在很多反应性的羟基, 且微胶 囊的粒径足够小,浸透和附着不仅在纱线表面,还能渗透和附着到构成纱线的 每根纤维的表面, 渗透到棉麻纤维无定形区, 故可以使用防皱交联剂 (如 2D 树脂), 通过在催化剂的作用下发生交联反应, 使防皱交联剂与棉麻织物及艾 叶油微胶囊之间形成醚键连接, 从而克服了使用粘胶剂耐洗性差的缺点,大大 提高织物与微胶囊的附着效果, 增强抗菌功能的耐久性, 同时赋予织物防皱免 烫性能, 此外交联醚化作用还能降低 2D树脂甲醛的释放量。而且, 利用这种技 术制备的艾叶油微胶囊抗菌织物具有抗菌消炎、促进血液循环、对皮肤有优良 的保健功能,同时所制备的织物还具有防皱免烫功能,并有较好的耐洗性效果。 可用于制作病人及日常护理保健服装。 The invention has the following beneficial effects: the microcapsule of the invention uses the eucalyptus oil as the core material, the gelatin and the gum arabic as the wall material, and the micro-encapsulation of the eucalyptus oil by the complex coacervation method, the preparation process is simple and easy, and the cost is relatively high. Low, it provides microencapsulation technology suitable for industrial production for Aiyan oil microcapsules. The prepared microcapsules have a particle size ranging from 1 to 50 μm, and have a good appearance and a smooth spherical shape, and have good coating effect, dispersibility and sustained release property. The eucalyptus oil microcapsule antibacterial fabric of the invention is prepared by using a eucalyptus oil microcapsule emulsion, an anti-wrinkle cross-linking agent, a catalyst and a penetrating agent as a fabric finishing agent, and adopting a padding finishing process to prepare the cotton and linen fabric. Since there are many reactive hydroxyl groups on the surface of the gelatin-arabino microcapsules, and the particle size of the microcapsules is small enough, the soaking and adhering not only on the surface of the yarn but also penetrates and adheres to the surface of each fiber constituting the yarn, permeating. To the amorphous area of cotton and linen fibers, it is possible to use an anti-wrinkle cross-linking agent (such as 2D resin) to cross-link the reaction between the anti-wrinkle cross-linking agent and the cotton-wool fabric and the eucalyptus oil microcapsules by the action of the catalyst. Forming an ether bond connection, thereby overcoming the disadvantage of poor adhesion resistance of the adhesive, greatly improving the adhesion effect of the fabric and the microcapsule, enhancing the durability of the antibacterial function, and imparting anti-wrinkle and ironing resistance to the fabric, and further crosslinking and etherification It also reduces the amount of formaldehyde released from 2D resin. Moreover, the eucalyptus oil microcapsule antibacterial fabric prepared by the technique has antibacterial and anti-inflammatory properties, promotes blood circulation, and has excellent skin. The health care function, at the same time, the prepared fabric also has anti-wrinkle and non-iron function, and has better washing durability. Can be used to make patients and daily care health clothing.
具体实施方式 detailed description
下面将详细描述本发明的具体制作例。应当注意,这里描述的制作例只用 于举例说明, 并不用于限制本发明。  Specific production examples of the present invention will be described in detail below. It should be noted that the fabrication examples described herein are for illustrative purposes only and are not intended to limit the invention.
本发明的艾叶油微胶囊抗菌织物其制备工艺主要包括艾叶油乳化反应、复 凝聚反应、 交联固化过程、 复配过程和织物的后整理五个步骤, 其中的各个步 骤分别为:  The preparation process of the eucalyptus oil microcapsule antibacterial fabric of the invention mainly comprises five steps of embedding oil emulsification reaction, re-coagulation reaction, cross-linking curing process, compounding process and fabric finishing, wherein each step is:
1、 艾叶油的乳化: 在系统浓度为 0. 1 %〜1. 5 % (w/v) 的明胶, 阿拉伯 胶混合溶液中加入 0. 1 %〜1. 5 % (w/v) 的艾叶油, 在转速为 800〜1000转 / 分, 恒温水浴 40 °C的条件下乳化 10〜15分钟; 1 %〜1. 5 % (w/v) 埃叶Oil, emulsified for 10 to 15 minutes at a speed of 800~1000 rpm, in a constant temperature water bath at 40 °C;
2、 复凝聚反应: 用 10 %HAC (乙酸)调节体系 ra至 3. 5〜4. 5, 然后降低 转速 250〜400转 /分, 移出水浴, 室温继续搅拌复凝聚 10〜15分钟; 2, re-coagulation reaction: with 10% HAC (acetic acid) to adjust the system ra to 3. 5~4. 5, then reduce the speed of 250~400 rev / min, remove the water bath, continue to stir and re-agglomerate at room temperature for 10~15 minutes;
3、 交联固化过程: 冰浴降温至 0〜5°C, 调节 PH至中性, 加入固化剂固 化 30分钟, 后移入 5CTC恒温水浴继续固化 2〜3小时, 得到艾叶油微胶囊乳 液; 3. Cross-linking curing process: cool down to 0~5 °C in ice bath, adjust pH to neutral, add curing agent for 30 minutes, then transfer to 5CTC constant temperature water bath to continue curing for 2~3 hours to obtain Aiye oil microcapsule emulsion;
4、 复配以制成多功能织物整理剂: 在上述制备的艾叶油微胶囊乳液中加 入 5 %〜20 % (w/v) 的防皱交联树脂, 1〜3% (w/v )催化剂, 0. 5%〜2% (w/v) 渗透剂脂肪醇聚氧乙烯醚 (JFC) , 复配成多功能织物整理剂; 4. Compounding to make multi-functional fabric finishing agent: Add 5%~20% (w/v) anti-wrinkle cross-linking resin, 1~3% (w/v) to the eucalyptus oil microcapsule emulsion prepared above. Catalyst, 0. 5%~2% (w/v) penetrant fatty alcohol polyoxyethylene ether (JFC), compounded into a multifunctional fabric finishing agent;
5、 织物的后整理过程: 将待整理织物浸入到上述复配整理剂中, 用二浸 二轧工艺进行整理, 轧余率为 100 %, 100°C烘干, 150°C〜190°C定型焙烘 2 分钟得艾叶油微胶囊抗菌织物。 其中, 在上述歩骤中, w/v表示质量 /体积。 5. Finishing process of the fabric: The fabric to be finished is immersed in the above-mentioned compound finishing agent, and finished by the two-dip two-rolling process, the rolling ratio is 100%, 100 ° C drying, 150 ° C ~ 190 ° C Shaped baking for 2 minutes to get the Aiye oil microcapsule antibacterial fabric. Wherein, in the above step, w/v represents mass/volume.
在本发明微胶囊制备技术方案中,采用不同的壁材体系浓度和不同的搅拌 速度可形成不同粒径的微胶囊。壁材浓度和搅拌速度的选择根据最终的需要而 定, 制备的微胶囊粒径范围为 1〜50 μ πι。  In the microcapsule preparation technical scheme of the present invention, microcapsules having different particle diameters can be formed by using different wall system concentrations and different stirring speeds. The wall material concentration and the stirring speed are selected according to the final needs, and the prepared microcapsules have a particle size ranging from 1 to 50 μm.
本发明微胶囊包覆率的测定方法:准确称取 0. 1000g新制备的艾叶油微胶 囊样品, 用无水乙醇浸泡 24小时萃取微胶囊中的艾叶油, 过滤。 取滤液用气 相色谱法测定萃取液中艾叶油某组分的峰面值,对照艾叶油溶液标准曲线,根 据外标法得到艾叶油的含量,从而可以得到微胶囊的包覆率。经此方法测定艾 叶油微胶囊的包覆率为 30 %〜80 %。  The method for determining the coverage of the microcapsules of the present invention: accurately: 1000 g of the newly prepared eucalyptus oil microcapsule sample, and immersed in absolute ethanol for 24 hours to extract the eucalyptus oil in the microcapsule, and filtered. The filtrate was determined by gas chromatography to determine the peak value of a component of the oil of the leaves of the leaves, and the standard curve of the oil of the leaves of the leaves was used to obtain the content of the leaves of the leaves, and the coverage of the microcapsules was obtained. The coating ratio of the eucalyptus oil microcapsules was determined by this method to be 30% to 80%.
本发明微胶囊芯材释放性能的测试方法:准确称取 0. 5000g已测定包覆率 的艾叶油微胶囊织物样品置于恒温恒湿箱, 设定温度为 50. 0 °C, 湿度为 24. 0 % , 每隔 1小时取出 0. O lg样品溶于 5mL的无水乙醇泡浸 24小时萃取微胶囊 中剩余的艾叶油,采用气相色谱法测定萃取液中艾叶油的剩余含量。经测试发 现初始阶段微胶囊的药物释放速率较快, 随后释放速率逐渐趋于稳定,具有良 好的释放效果。  The temperature of the microcapsules of the present invention is as follows: 0. 0 ° C, humidity is 24 0 % , 0 ° O lg sample was dissolved in 5 mL of absolute ethanol soaked for 24 hours to extract the remaining eucalyptus oil in the microcapsules, and the remaining content of eucalyptus oil in the extract was determined by gas chromatography. It was found that the drug release rate of the microcapsules in the initial stage was faster, and then the release rate gradually became stable and had a good release effect.
本发明的方法制备的艾叶油微胶囊抗菌织物抗菌性测试方法:采用振荡烧 瓶法模仿人体的穿着条件, 使细菌在振荡条件 (300 转 /分) 下与织物内抗菌 剂接触, 振荡 l-6h之后, 经细菌培养计数, 计算细菌减少百分率, 从而确定 抗菌性能大小。测试菌种选取自然界及人体皮肤粘膜中最常分布的金黄色葡萄 球菌和大肠杆菌作为代表菌种。  The antibacterial test method for the antibacterial fabric of the eucalyptus oil microcapsule prepared by the method of the invention adopts the oscillating flask method to imitate the wearing condition of the human body, and makes the bacteria contact with the antibacterial agent in the fabric under the shaking condition (300 rpm), and shakes for l-6h. Thereafter, the percentage of bacterial reduction was calculated by bacterial culture counting to determine the magnitude of the antibacterial property. The test strains were selected from the most commonly distributed Staphylococcus aureus and Escherichia coli in nature and human skin mucous membranes as representative strains.
本发明织物耐洗性测试方法: 用 2%肥皂水或市售的洗衣粉, 按说明配成 洗涤液, 将织物放入洗衣机内搅动, 以每 10分钟一次搅动, 可洗 0、 5、 10、 20、 30、 50次, 每次应在清水中漂净再搅拌, 然后再测定洗后织物的抗菌率。 本发明采用水萃取法( GB/T2912.1-1998)测定整理后织物残留甲醛 含量; 根据织物风格试验方法平整度试验方法 (FZ/T 01054.6-1999) 测定织 物的平整度; 依据 GB/T3819-1997标准, 使用 YGB型折皱测试仪测定织物折痕 回复角; 采用扯边纱条样法(GB/T 3923.1-1997)在等速伸长强力机上测定织 物的断裂保留率。 The method for testing the washing durability of the fabric of the invention: using 2% soapy water or a commercially available washing powder, according to the instructions, the washing liquid is prepared, the fabric is put into the washing machine and stirred, and stirred once every 10 minutes, and can be washed 0, 5, 10 20, 30, 50 times, each time should be rinsed in clean water and then stirred, and then the antibacterial rate of the washed fabric is measured. The invention adopts the water extraction method (GB/T2912.1-1998) to determine the residual formaldehyde content of the finished fabric; the flatness of the fabric is determined according to the flatness test method of the fabric style test method (FZ/T 01054.6-1999); according to GB/T3819 -1997 standard, the crease recovery angle of the fabric was measured using a YGB type wrinkle tester; the rupture retention rate of the fabric was measured on a constant speed elongation machine using a burr yarn method (GB/T 3923.1-1997).
本发明的艾叶油微胶囊应用于织物抗菌整理, 可获得高效、 广谱、 安全、 耐洗且有一定预防和医疗效果的抗菌织物, 同时还具有优良的防皱免烫功能。  The eucalyptus oil microcapsule of the invention is applied to antibacterial finishing of fabrics, and can obtain an antibacterial fabric with high efficiency, broad spectrum, safety, washing resistance and certain preventive and medical effects, and also has excellent anti-wrinkle and non-scalding functions.
实施例 1  Example 1
(1) 艾叶油的乳化: 分别称取 0.50g明胶和 0.50g阿拉伯胶于 250mL的 三口烧瓶中, 加入 lOOmL蒸馏水, 装上机械搅拌器, 置于 40°C水浴中搅拌溶 解后配制成明胶 -阿拉伯胶体系的混合液,浓度均为 0.5%(W/V),再加入 1. OraL 艾叶油, 在搅拌速度为 800转 /分的条件下乳化 10分钟;  (1) Emulsification of Artemisia argyi oil: Weigh 0.50g gelatin and 0.50g gum arabic in a 250mL three-necked flask, add 100mL of distilled water, install a mechanical stirrer, put it in a 40°C water bath, stir and dissolve it, and prepare it into gelatin. A mixture of gum arabic system, the concentration is 0.5% (W / V), and then added 1. OraL Ai oil, emulsified for 10 minutes at a stirring speed of 800 rpm;
(2) 复凝聚反应: 保持乳化时的搅拌速度和水浴温度不变, 在上述乳化 液中逐渐滴加 10%HAC溶液调节体系的 PH值至 4.0, 把搅拌速度降低到 300 转 /分, 移出水浴, 室温继续搅拌 10分钟;  (2) Re-coagulation reaction: Keep the stirring speed and the bath temperature unchanged during the emulsification, gradually add 10% HAC solution to the above emulsion to adjust the pH value of the system to 4.0, reduce the stirring speed to 300 rpm, and remove Water bath, stirring at room temperature for 10 minutes;
(3)交联固化:将上述凝聚化的微胶囊悬浮液用冰水浴 30分钟降温至 0〜 5°C,然后用 10%NaOH溶液调节体系 PH值至 7.0,滴加入 2mL 25%戊二醛溶液, 在搅拌速度 400转 /分的条件下继续冰浴 30分钟; 移入 50°C的水浴中继续交 联固化 2小时得到艾叶油微胶囊乳液;  (3) Cross-linking curing: The above-mentioned coagulated microcapsule suspension was cooled to 0 to 5 ° C in an ice water bath for 30 minutes, then the pH of the system was adjusted to 7.0 with a 10% NaOH solution, and 2 mL of 25% glutaraldehyde was added dropwise. The solution was incubated at a stirring speed of 400 rpm for 30 minutes; the mixture was transferred to a water bath at 50 ° C to continue crosslinking and solidification for 2 hours to obtain a eucalyptus oil microcapsule emulsion;
(4) 艾叶油微胶囊抗菌防皱织物整理剂的制备: 在上述制得的微胶囊乳 液中加入 20克含量 100%的 2D树脂, 3克氯化镁催化剂, l.Og渗透剂 JFC, 搅拌均匀, 得到叶油微胶囊抗菌防皱织物整理剂;  (4) Preparation of antibacterial anti-wrinkle fabric finishing agent of Aiye oil microcapsules: 20 g of 100% 2D resin, 3 g of magnesium chloride catalyst, l.Og penetrant JFC, and evenly stirred, are added to the microcapsule emulsion prepared above. Obtaining an antibacterial anti-wrinkle fabric finishing agent for leaf oil microcapsules;
(5)抗菌织物的整理: 将待整理织物 (100%棉) 浸入到上述制备的整理 剂中, 二浸二轧, 轧液率重量比为 100 %, 然后在 10CTC烘箱中预烘 3分钟, 再在 16CTC烘培 2分钟, 冷却至室温即得艾叶油微胶囊抗菌防皱织物。 (5) Finishing of antibacterial fabric: Dip the fabric to be finished (100% cotton) into the above preparation In the agent, the second immersion and two rolling, the rolling solution weight ratio is 100%, and then pre-baked in a 10CTC oven for 3 minutes, and then baked at 16CTC for 2 minutes, and cooled to room temperature to obtain the eucalyptus oil microcapsule antibacterial anti-wrinkle fabric.
织物性能测试: 用上述的方法对实施例 1中制成的织物的性能进行测试。 整理后的棉织物平整度等级 3. 7, 干折皱回复角 3120, 断裂强力保留率 68%, 甲醛释放为 40ppm, 织物抗菌率及耐洗性效果见下表:  Fabric Property Test: The properties of the fabric produced in Example 1 were tested by the method described above. Finished cotton fabric flatness grade 3. 7, dry wrinkle recovery angle 3120, breaking strength retention rate of 68%, formaldehyde emission of 40ppm, fabric antibacterial rate and washability effect are shown in the following table:
实施例 2:  Example 2:
( 1 ) 艾叶油的乳化: 分别称取 1. 00g明胶和 1. 00g阿拉伯胶于 250mL的 三口烧瓶中, 加入 lOOmL蒸馏水, 装上机械搅拌器, 置于 40°C水浴中搅拌溶 解, 加入 1. OmL艾叶油, 在搅拌速度为 800转 /分的条件下乳化 15分钟;  (1) Emulsification of Artemisia argyi oil: Weigh 1.00g gelatin and 1. 00g gum arabic in a 250mL three-necked flask, add 100mL of distilled water, install a mechanical stirrer, put it in a 40°C water bath, stir and dissolve, add 1 OmL eucalyptus oil, emulsified for 15 minutes at a stirring speed of 800 rpm;
( 2 ) 复凝聚反应: 保持乳化时的搅拌速度和水浴温度不变, 在上述乳化 液中逐渐滴加 10 %HAC溶液调节体系的 PH值至 4. 0, 把搅拌速度降低到 250 转 /分, 移出水浴, 室温继续搅拌 10分钟;  (2) Re-coagulation reaction: Keep the stirring speed and the water bath temperature unchanged during the emulsification, gradually add 10% HAC solution to the emulsion to adjust the pH of the system to 4.0, and reduce the stirring speed to 250 rpm. , remove the water bath, continue stirring at room temperature for 10 minutes;
( 3 )交联固化: 将上述凝聚化的悬浮液用冰水浴 30分钟降温至 0〜5°C, 然后用 10%NaOH溶液调节体系 ίΉ值至 7. 0, 滴加入 4mL25 %戊二醛溶液,在搅 拌速度 300转 /分的条件下继续冰浴 30分钟; 移入 50°C的水浴中继续交联固 化 2小时得艾叶油微胶囊乳液;  (3) Cross-linking curing: The above-mentioned coagulated suspension was cooled to 0 to 5 ° C in an ice water bath for 30 minutes, and then the system was adjusted to 7. 0 with a 10% NaOH solution, and 4 mL of a 25% glutaraldehyde solution was added dropwise. , the ice bath was continued for 30 minutes under the stirring speed of 300 rpm; the mixture was transferred into a water bath at 50 ° C to continue crosslinking and solidification for 2 hours to obtain a eucalyptus oil microcapsule emulsion;
(4 ) 艾叶油微胶囊抗菌防皱织物整理剂的制备: 在上述制成的微胶囊乳 液中加入 5克丁垸四羧酸(BTCA)防皱交联剂, 1克磷酸二氢钠催化剂, 0. 5gJFC 渗透剂, 搅拌均匀即得复配整理剂;  (4) Preparation of antibacterial anti-wrinkle fabric finishing agent of Aiye oil microcapsule: 5 g of butyl bromide tetracarboxylic acid (BTCA) anti-wrinkle cross-linking agent and 1 g of sodium dihydrogen phosphate catalyst were added to the microcapsule emulsion prepared above. 0. 5gJFC penetrant, evenly mixed to obtain a finishing agent;
( 5 )抗菌织物的整理: 将待整理织物 (100%棉) 浸入到上述制备的整理 剂中, 二浸二轧, 轧液率重量比为 100 %, 然后在 85°C烘箱中预烘 3分钟, 再 在 18CTC烘培 2分钟, 冷却至室温即得艾叶油微胶囊抗菌防皱织物。 (5) Finishing of antibacterial fabric: Dip the fabric to be finished (100% cotton) into the above preparation In the agent, the second dip and two rolling, the rolling solution weight ratio is 100%, and then pre-baked in an oven at 85 ° C for 3 minutes, and then baked at 18 CTC for 2 minutes, cooled to room temperature to obtain the anti-wrinkle fabric of the micro-capsule .
织物性能测试: 采用上述的方法对实施例 2 中制成的织物的性能进行测 试。整理后棉织物平整度等级 3. 5,干折皱回复角 2980, 断裂强力保留率 72%, 甲醛释放为 0ppm, 织物抗菌率及耐洗性效果见下表:
Figure imgf000012_0001
实施例 3
Fabric Performance Test: The properties of the fabrics produced in Example 2 were tested using the methods described above. After finishing, the cotton fabric has a flatness grade of 3.5, a dry wrinkle recovery angle of 2980, a breaking strength retention rate of 72%, and a formaldehyde release of 0 ppm. The antibacterial rate and the washing durability of the fabric are as follows:
Figure imgf000012_0001
Example 3
( 1 ) 艾叶油的乳化: 分别称取 5. 00g明胶和 5. 00g阿拉伯胶于 250mL的 三口烧瓶中, 加入 lOOmL蒸馏水, 装上机械搅拌器, 置于 40°C水浴中搅拌溶 解, 加入 5. 0mL艾叶油, 在搅拌速度为 1000转 /分的条件下乳化 20分钟。  (1) Emulsion of eucalyptus oil: Weigh 5.00g gelatin and 5. 00g gum arabic in a 250mL three-necked flask, add 100mL of distilled water, install a mechanical stirrer, put it in a 40 °C water bath, stir and dissolve, add 5 0 mL of eucalyptus oil was emulsified for 20 minutes under the conditions of a stirring speed of 1000 rpm.
( 2 ) 凝聚反应: 保持乳化时的搅拌速度和水浴温度不变, 在上述乳化液 中逐渐滴加 10 %HAC溶液调节体系的 ra值至 4. 0, 把搅拌速度降低到 600转 / 分, 移出水浴, 室温继续搅拌 10分钟;  (2) agglomeration reaction: maintaining the stirring speed of the emulsification and the temperature of the water bath, gradually adding 10% HAC solution to the above emulsion to adjust the ra value of the system to 4.0, and reducing the stirring speed to 600 rpm, Remove the water bath and continue stirring for 10 minutes at room temperature;
( 3 )交联固化: 将上述凝聚化的悬浮液用冰水浴 30分钟降温至 0〜5°C, 然后用 10%NaOH溶液调节体系 PH值至 7. 0, 滴加入 10mL25 %戊二醛溶液, 在 搅拌速度 350转 /分的条件下继续冰浴 30分钟; 移入 50°C的水浴中继续交联 固化 2小时得到艾叶油微胶囊乳液;  (3) Cross-linking curing: The above-mentioned coagulated suspension was cooled to 0 to 5 ° C in an ice water bath for 30 minutes, and then the pH of the system was adjusted to 7.0 with a 10% NaOH solution, and 10 mL of a 25% glutaraldehyde solution was added dropwise. , the ice bath was continued for 30 minutes under the stirring speed of 350 rpm; the mixture was transferred to a 50 ° C water bath to continue crosslinking and solidification for 2 hours to obtain a eucalyptus oil microcapsule emulsion;
(4) 艾叶油微胶囊抗菌防皱织物整理剂的制备: 在上述制成的微胶囊乳 液中加入 20克含量 100 %的 2D树脂, 6克氯化镁, l. Og渗透剂 JFC, 搅拌均 匀, 即得复配整理剂。 ( 5 )抗菌织物的整理: 将待整理织物 (100%棉) 浸入到上述制得的稀释 4倍的整理液中, 二浸二轧, 轧液率重量比为 100 %, 然后在 85°C烘箱中预烘 3分钟,再在 15CTC烘培 3分钟,冷却至室温即得艾叶油微胶囊抗菌防皱织物。 (4) Preparation of antibacterial anti-wrinkle fabric finishing agent of Aiye oil microcapsule: Add 20 g of 100% 2D resin, 6 g of magnesium chloride, 1.0 g of penetrant JFC to the microcapsule emulsion prepared above, and mix well, ie It is necessary to compound the finishing agent. (5) Finishing of antibacterial fabric: The fabric to be finished (100% cotton) is immersed in the above-mentioned diluted 4 times of the finishing liquid, the second dip and the second rolling, the rolling solution weight ratio is 100%, and then at 85 ° C The oven was prebaked for 3 minutes, then baked at 15 CTC for 3 minutes, and cooled to room temperature to obtain the eucalyptus oil microcapsule antibacterial anti-wrinkle fabric.
织物性能测试: 采用上述的方法对实施例 3中制得织物的性能进行测试。 对整理后棉织物平整度等级 3. 4, 干折皱回复角 3000, 断裂强力保留率 74%, 甲醛释放为 40ppm, 织物抗菌率和耐水洗性见下表:  Fabric Property Test: The properties of the fabric obtained in Example 3 were tested by the method described above. The finished cotton fabric has a flatness rating of 3. 4, a dry wrinkle recovery angle of 3000, a breaking strength retention rate of 74%, and a formaldehyde release of 40 ppm. The fabric antibacterial rate and water wash resistance are as follows:
Figure imgf000013_0001
从以上实施例的数据可以看出, 即使是在洗涤多次之后, 本发明的艾叶油 抗菌防皱织物仍然具有优良的抗菌效果,特别对金黄色葡萄球菌和大肠杆菌有 着较好的抗菌效果。
Figure imgf000013_0001
As can be seen from the data of the above examples, the eucalyptus oil antibacterial anti-wrinkle fabric of the present invention has excellent antibacterial effects even after washing a plurality of times, and has a particularly excellent antibacterial effect against Staphylococcus aureus and Escherichia coli.
以上结合实施例对本发明进行了详细的说明,但是在本发明的精神和权利 要求的保护范围之内,本领域的技术人员还可以作出多种改型和变型,应当说, 这样的一些改型和变型都在本发明的保护范围之内。  The present invention has been described in detail above with reference to the embodiments, but those skilled in the art can also make various modifications and changes within the scope of the spirit of the invention and the scope of the claims. Both variations and modifications are within the scope of the invention.

Claims

权 利 要 求 Rights request
1. 一种艾叶油微胶囊抗菌防皱织物的制备方法, 其特征在于, 所述的方 法包括以下步骤: A method for preparing an anti-wrinkle fabric of a eucalyptus oil microcapsule, characterized in that the method comprises the following steps:
1 ) 在以壁材形成的乳化剂中乳化艾叶油;  1) emulsifying eucalyptus oil in an emulsifier formed of a wall material;
2 ) 使乳化的艾叶油发生复凝聚反应;  2) re-agglomerating the emulsified eucalyptus oil;
3 ) 在乳化剂中加入固化交联剂, 交联固化复凝聚反应后的乳液, 以得到 艾叶油微胶囊乳液;  3) adding a curing crosslinking agent to the emulsifier, crosslinking and curing the emulsion after the re-agglomeration reaction to obtain a eucalyptus oil microcapsule emulsion;
4 ) 在得到的艾叶油微胶囊乳液中加入防皱交联剂、 催化剂和渗透剂, 以 制成艾叶油微胶囊抗菌防皱织物整理剂;  4) adding an anti-wrinkle cross-linking agent, a catalyst and a penetrating agent to the obtained eucalyptus oil microcapsule emulsion to prepare an anti-wrinkle fabric finishing agent for the eucalyptus oil microcapsule;
5 ) 将织物用制成的艾叶油微胶囊抗菌防皱织物整理剂进行处理以得到艾 叶油微胶囊抗菌防皱织物。  5) The fabric is treated with the prepared eucalyptus oil microcapsule antibacterial anti-wrinkle fabric finishing agent to obtain an anti-wrinkle fabric of the eucalyptus oil microcapsule.
2. 如权利要求 1所述的方法, 其特征在于, 在步骤 1 ) 中, 所述的壁材 是明胶和阿拉伯胶的混合溶液, 其中, 所述的壁材的浓度 w/v为 0. 5%〜5%, 艾叶油与壁材的用量比例为 0. 5〜2. 0; 所述的乳化过程和条件为: 在转速为 800〜1000转 /分, 恒温水浴 40°C的条件下乳化 10〜15分钟。  2. The method according to claim 1, wherein in the step 1), the wall material is a mixed solution of gelatin and gum arabic, wherein the wall material has a concentration w/v of 0. 5〜2. 0; The emulsification process and conditions are as follows: at a speed of 800~1000 rpm, a constant temperature water bath of 40 ° C under the conditions of 0. 5~2. 0; Emulsify for 10 to 15 minutes.
3. 如权利要求 1所述的方法, 其特征在于, 在步骤 2 ) 中, 所述的复凝聚 反应过程和条件为: 用 10 %HAC溶液把乳化反应体系的 ra调至 ΪΉ3. 5〜4. 5, 然后降低转速, 把系统移出水浴, 继续在室温搅拌进行复凝聚 10〜15分钟。  5〜4。 The method of the emulsification reaction system was adjusted to ΪΉ 3. 5~4 5, then reduce the speed, remove the system from the water bath, continue to stir at room temperature for re-agglomeration for 10 to 15 minutes.
4. 如权利要求 3所述的方法, 其特征在于, 在复凝聚反应过程中, 调节 PH时的乳化搅拌速度为 800〜1000转 /分, 在把系统 ra值调至 3. 5〜4. 5后, 把搅拌速度降低到 250〜400 转 /分。  5〜4. The value of the system ra is adjusted to 3. 5~4. After 5, reduce the stirring speed to 250~400 rpm.
5. 如权利要求 1所述的方法, 其特征在于, 在步骤 3 ) 中, 所述的交联 固化反应过程和条件为: 采用冰浴将系统降温至 0〜5°C, 用 10 %HAC溶液把 系统的 ra调节至中性, 接着加入 l-100ml的固化交联剂, 冰浴固化 30分钟, 再移入 5CTC恒温水浴继续固化 2〜3小时后, 得到艾叶油微胶囊乳液。 5. The method according to claim 1, wherein in step 3), said crosslinking The curing reaction process and conditions are as follows: The system is cooled to 0 to 5 ° C in an ice bath, the system is adjusted to neutral with 10% HAC solution, then 1-100 ml of curing crosslinking agent is added, and the ice bath is cured for 30 minutes. Then, it was transferred to a 5 CTC constant temperature water bath to continue curing for 2 to 3 hours, and then a eucalyptus oil microcapsule emulsion was obtained.
6. 如权利要求 5所述的制备方法, 其特征在于, 所述的固化交联剂选自 甲醛、 乙二醛、 戊二醛或其混合物。  The method according to claim 5, wherein the curing crosslinking agent is selected from the group consisting of formaldehyde, glyoxal, glutaraldehyde or a mixture thereof.
7. 如权利要求 1中任意一项所述的方法, 其特征在于, 在所述制成的艾 叶油微胶囊乳液中, 艾叶油微胶囊为球形颗粒, 其粒径在 1-50 μ m之间。  The method according to any one of claims 1 to 3, wherein in the prepared eucalyptus oil microcapsule emulsion, the eucalyptus oil microcapsule is a spherical particle having a particle diameter of 1 to 50 μm. between.
8. 如权利要求 1所述的方法, 其特征在于, 在步骤 4) 中加入的防皱交 联剂、 催化剂和渗透剂的量分别为:  8. The method according to claim 1, wherein the amounts of the anti-wrinkle crosslinking agent, the catalyst and the penetrating agent added in the step 4) are respectively:
w/v为 3-20% 的防皱交联剂;  w/v is 3-20% anti-wrinkle crosslinker;
w/v为 1-3% 的催化剂;  w/v is 1-3% catalyst;
w/v为 0. 5-1. 5% 的渗透剂。  w/v is 0. 5-1. 5% penetrant.
9. 如权利要求 8所述的方法, 其特征在于, 所述的防皱交联剂选自 2D 树脂、 2D醚化树脂、 丁垸四羧酸或其混合物。  9. The method according to claim 8, wherein the anti-wrinkle crosslinking agent is selected from the group consisting of 2D resin, 2D etherified resin, tetrabutyltetracarboxylic acid or a mixture thereof.
10. 如权利要求 8所述的方法, 其特征在于, 所述的催化剂选自金属盐、 无机酸或其混合物。  10. The method of claim 8, wherein the catalyst is selected from the group consisting of metal salts, inorganic acids, or mixtures thereof.
11.如权利要求 10所述的方法, 其特征在于, 所述的金属盐选自镁盐、 钠盐和钾盐。  The method according to claim 10, wherein the metal salt is selected from the group consisting of magnesium salts, sodium salts and potassium salts.
12. 如权利要求 10所的方法, 其特征在于, 所述的无机酸选自盐酸和磷 酸。  12. The method of claim 10 wherein said mineral acid is selected from the group consisting of hydrochloric acid and phosphoric acid.
13 如权利要求 8所述的方法,其特征在于,所述的渗透剂为脂肪醇聚氧 乙烯醚。  13. The method of claim 8 wherein said penetrant is a fatty alcohol ethoxylate.
14. 如权利要求 1所述的方法,其特征在于,所述的步骤 5 )进一步包括: a ) 将织物在得到的艾叶油微胶囊抗菌防皱织物整理剂中二浸二轧; b ) 取出织物, 其中织物的带液率 70〜100 % ; 14. The method of claim 1 wherein said step 5) further comprises: a) immersing the fabric in the obtained eucalyptus oil microcapsule antibacterial anti-wrinkle fabric finishing agent; b) removing the fabric, wherein the fabric has a liquid-liquid ratio of 70-100% ;
c ) 在 85〜100°C下, 预烘 3〜5分钟;  c) pre-bake at 85~100 °C for 3~5 minutes;
d) 在 150〜190°C下, 定型焙烘 2〜5分钟;  d) at 150~190 ° C, stereotype baking for 2 to 5 minutes;
e ) 水洗后烘干,制成艾叶油微胶囊抗菌防皱织物。  e) After washing with water, it is made into an anti-wrinkle fabric of Aiye oil microcapsules.
15.—种艾叶油微胶囊抗菌防皱织物,其特征在于,所述的抗菌防皱织物 采用权利要求 1-14中任意一项所述的方法经处理后得到, 其中, 所述的织物 上包覆有以艾叶油形成的微胶囊。  15. A eucalyptus oil microcapsule antibacterial anti-wrinkle fabric, characterized in that the antibacterial anti-wrinkle fabric is obtained by treatment according to the method of any one of claims 1-14, wherein the fabric is It is coated with microcapsules formed from eucalyptus oil.
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