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CN103966847B - A kind of method of plants essential oil thermal sensitive liposome finish fabric - Google Patents

A kind of method of plants essential oil thermal sensitive liposome finish fabric Download PDF

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CN103966847B
CN103966847B CN201410154101.4A CN201410154101A CN103966847B CN 103966847 B CN103966847 B CN 103966847B CN 201410154101 A CN201410154101 A CN 201410154101A CN 103966847 B CN103966847 B CN 103966847B
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essential oil
fabric
natural
finishing
sodium salt
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CN103966847A (en
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葛彦
汤佳鹏
唐虹
傅海洪
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Xinchengda Fashion Anhui Co ltd
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Nantong University
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Abstract

The invention discloses a kind of method of plants essential oil thermal sensitive liposome finish fabric, by mix and blend under tea tree ethereal oil, menthol and P-Cymene low temperature, obtain natural aromatic antiseptic; Natural aromatic antiseptic is dissolved in phosphate buffered solution; Natural phospholipid, phosphatid ylcholine, glycerophosphatide, phosphatidyl-ethanolamine, phosphatidylserine and phosphatidic acid are mixed, adds cholesterol, be dissolved in chloroform and pour in container, be at room temperature evaporated to chamber wall and form the homogeneous film of one deck; Being added by the phosphate buffer solution of natural aromatic antiseptic in ultrasonic water bath is covered with in the container of film, obtains thermal sensitive liposome suspension after sonic oscillation; Added by adhesive in thermal sensitive liposome suspension, stirring at room temperature, to dissolving completely, obtains thermal sensitivity fragrant antimicrobial finishing agent; By textile pad in dressing liquid, two leachings two are rolled, and last fabric utilizes desivac to carry out arrangement sizing.

Description

一种植物精油热敏脂质体整理织物的方法A kind of method for finishing fabric with plant essential oil thermosensitive liposome

技术领域technical field

本发明属于纺织服装、医用材料领域,具体涉及一种植物精油热敏脂质体整理织物的方法。The invention belongs to the field of textile clothing and medical materials, and in particular relates to a method for finishing fabrics with plant essential oil thermosensitive liposomes.

背景技术Background technique

随着消费观念和健康观念的转变,人们对纺织品有了更新的要求,为此具有保健作用的纺织品倍受青睐。With the change of consumption concepts and health concepts, people have new requirements for textiles, and textiles with health care effects are very popular.

目前研究较多的纳米银、纳米氧化锌、纳米陶瓷粉、TiO2等无机抗菌剂用于棉织物整理,能够获得较好的抗菌保健性能。但是金属离子容易转变为氧化物或者还原为单质而变色,影响织物色泽,特别是银离子或纳米银颗粒对生殖系统和肝脏具有潜在毒性。一些光催化的金属氧化物,在避光的皮肤表面抗菌效果不佳。另外,在织物中的金属进入环境后无法被转化或富集,因此可能导致生态失衡。季铵盐也有一些固有的缺陷,如:容易从织物浸出,与阴离子表面活性剂不相容等。DC公司已经生产了一种硅氧烷类季铵盐抗菌剂(AEM5700),可以共价结合到织物表面,具有持久的抗菌活性。然而这种季铵盐化合物的抗菌活性也会由于灰尘或死去微生物的吸附或者阳性季铵盐和阴性表面活性剂在反复洗涤过程中形成复合物而降低性能或失效。另外,双胍类对真菌的抗菌作用较弱,而且对光的耐受性不强。三氯生对细菌的抗性已经有文献报道,并受到关注。但由于其在阳光下会产生有毒的多氯二恶辛类化合物,因此被许多国家禁止在织物和许多其他产品中使用。总之,大部分的有机合成抗菌剂抗菌周期短、安全性和化学稳定性差,易产生微生物耐药性,导致它们的应用范围受限。更重要的是,金属及金属氧化物、有机抗菌剂都是由非可再生资源生产的,在资源危机的冲击下,势必造成这些抗菌剂制造成本大幅度提高,不利于抗菌整理的发展。At present, inorganic antibacterial agents such as nano-silver, nano-zinc oxide, nano-ceramic powder, and TiO2 , which have been studied more, are used in cotton fabric finishing, which can obtain better antibacterial and health-care properties. However, metal ions are easily transformed into oxides or reduced to simple substances to change color, affecting the color of fabrics, especially silver ions or nano-silver particles have potential toxicity to the reproductive system and liver. Some photocatalyzed metal oxides have poor antibacterial effects on skin surfaces protected from light. In addition, the metals in the fabric cannot be transformed or enriched after entering the environment, thus possibly causing ecological imbalance. Quaternary ammonium salts also have some inherent defects, such as: easy leaching from fabrics, incompatibility with anionic surfactants, etc. DC Company has produced a silicone-based quaternary ammonium antimicrobial agent (AEM5700), which can be covalently bonded to the surface of fabrics and has long-lasting antibacterial activity. However, the antibacterial activity of such quaternary ammonium compounds can also be reduced or lost due to the adsorption of dust or dead microorganisms or the formation of complexes between positive quaternary ammonium salts and negative surfactants during repeated washings. In addition, biguanides have weak antibacterial effects on fungi and are not very resistant to light. Triclosan's resistance to bacteria has been reported in the literature and has attracted attention. But its use in fabrics and many other products is banned in many countries due to the toxic polychlorinated dioxins it produces when exposed to sunlight. In short, most organic synthetic antibacterial agents have short antibacterial cycles, poor safety and chemical stability, and are prone to microbial resistance, which limits their application range. More importantly, metals, metal oxides, and organic antibacterial agents are all produced from non-renewable resources. Under the impact of resource crisis, the manufacturing cost of these antibacterial agents will inevitably increase significantly, which is not conducive to the development of antibacterial finishing.

一个理想的纺织品抗菌整理不仅要杀死有害菌阻止疾病的传播,同时也必须满足三个基本要求:首先,安全性:产品不应对人类和环境有过度毒性,不应引起皮肤过敏和刺激;其次,兼容性:产品必须对纺织品性能或外观不存在负面影响,必须与普通纺织品工艺兼容;第三,耐久性:产品应能耐受洗涤和干燥,且不容易从织物中浸出。为了达到这一最终目的,天然抗菌剂是最佳选择之一。因为抗菌天然活性物质能够用于生产安全、无毒、环保、对皮肤无刺激的生物活性纺织品,故其在纺织纤维的生物功能化中的应用显得越来越重要。而且天然抗菌剂来源广泛,量大种类多,作用靶点多样,抗菌谱广,不易产生耐药性。因此,有必要将抗菌天然活性物质与现代纺织品整理工艺结合起来,对棉织物进行整理,不仅有利于防止织物被微生物污损,更重要的是防止了疾病的传播,保证了人体的安全舒适,降低了公共环境的交叉感染率。这与人们追求健康、绿色、环保的理念是完全吻合的,具有重大的社会效益。An ideal textile antibacterial finish not only kills harmful bacteria and prevents the spread of diseases, but also must meet three basic requirements: first, safety: the product should not be excessively toxic to humans and the environment, and should not cause skin allergies and irritations; second , compatibility: the product must have no negative impact on textile performance or appearance, and must be compatible with common textile processes; third, durability: the product should be able to withstand washing and drying, and not easily leached from the fabric. To achieve this ultimate goal, natural antimicrobials are one of the best options. Because antibacterial natural active substances can be used to produce bioactive textiles that are safe, non-toxic, environmentally friendly, and non-irritating to the skin, their application in the biofunctionalization of textile fibers is becoming more and more important. Moreover, natural antibacterial agents have a wide range of sources, large quantities and types, diverse action targets, broad antibacterial spectrum, and are not easy to produce drug resistance. Therefore, it is necessary to combine antibacterial natural active substances with modern textile finishing techniques to finish cotton fabrics, which not only helps prevent fabrics from being fouled by microorganisms, but more importantly, prevents the spread of diseases and ensures the safety and comfort of the human body. Reduced cross-infection rates in public environments. This is completely consistent with people's pursuit of health, green and environmental protection concepts, and has significant social benefits.

茶树精油,是澳洲互叶白千层叶片经水蒸气蒸馏获得的油性提取物,具有特殊的芳香气味。茶树精油具有显著的抑菌活性和广泛的抗菌谱范围,对常见的革兰氏阳性菌、革兰氏阴性菌和真菌都具有强烈的抑制作用,与化学抑菌剂相比,具有副作用和残留毒性小的独特优势,对皮肤无刺激作用。茶树精油具有净化空气、杀菌、免疫、防腐、提供细胞营养等用途,可以作为安全有效的医用敷料抗菌剂。Tea tree essential oil is an oily extract obtained from the leaves of Melaleuca alternifolia through steam distillation, and has a special aromatic smell. Tea tree essential oil has significant antibacterial activity and broad antibacterial spectrum range, and has a strong inhibitory effect on common Gram-positive bacteria, Gram-negative bacteria and fungi. Compared with chemical antibacterial agents, it has side effects and residual The unique advantage of low toxicity, no irritation to the skin. Tea tree essential oil has the functions of purifying air, sterilizing, immunizing, antisepsis, providing cell nutrition, etc. It can be used as a safe and effective antibacterial agent for medical dressings.

艾叶精油是从艾草的叶子、茎的提取物,挤压法和溶剂提取法提炼萃取的挥发性芳香物质。艾叶精油的主治功效,理气血,温经脉,祛寒湿,止痛,抗菌,消炎,激励消化腺,镇咳化痰,促循环,补气,提升免疫力。Artemisia argyi essential oil is a volatile aromatic substance extracted from the leaves and stems of wormwood, extruded and solvent extracted. The main therapeutic effects of Artemisia argyi essential oil are regulating qi and blood, warming meridians, dispelling cold and dampness, relieving pain, antibacterial, anti-inflammatory, stimulating digestive glands, relieving cough and reducing phlegm, promoting circulation, replenishing qi, and improving immunity.

薄荷醇,有机化合物,无色针状结晶或粒状。为薄荷和欧薄荷精油中的主要成分,以游离和酯的状态存在。薄荷醇有8种异构体,它们的呈香性质各不相同,左旋薄荷醇具有薄荷香气并有清凉的作用,消旋薄荷醇也有清凉作用,其他的异构体无清凉作用。可用作牙膏、香水、饮料和糖果等的赋香剂。在医药上用作刺激药,作用于皮肤或粘膜,有清凉止痒作用;内服可用于头痛及鼻、咽、喉炎症等。Menthol, organic compound, colorless needle crystal or granular. It is the main component of peppermint and peppermint essential oils, and exists in free and ester states. There are 8 isomers of menthol, and their aroma properties are different. Levomenthol has a mint aroma and has a cooling effect, racemic menthol also has a cooling effect, and other isomers have no cooling effect. It can be used as flavoring agent for toothpaste, perfume, beverage and candy. It is used as a stimulating drug in medicine, acts on the skin or mucous membrane, and has a cooling and antipruritic effect; it can be used for headache, nose, pharynx, and laryngitis when taken orally.

在研究的各种新型脂质体中,热敏脂质体是一个很有发展前途的分支,它有效利用了脂质体和热疗的双重优势来提高治疗效果,降低毒副作用,增加了靶向性。在正常的环境温度下,脂质体膜呈致密排列的胶晶态,药物很难透过脂质体膜而扩散出来。当脂质体在膜相变温度以上环境时,局部的高温使磷脂分子运动加强,脂质体膜的结构发生变化,原来排列整齐致密的胶晶态磷脂双分子层在较高温度下变成疏松混乱的液晶态,药物即被释放出来。Among the various new liposomes studied, thermosensitive liposomes are a promising branch, which effectively utilizes the dual advantages of liposomes and thermotherapy to improve the therapeutic effect, reduce toxic side effects, and increase the number of targets. tropism. At normal ambient temperature, the liposome membrane is in a densely arranged colloidal crystal state, and it is difficult for drugs to diffuse out through the liposome membrane. When the liposome is in the environment above the membrane phase transition temperature, the local high temperature will strengthen the movement of phospholipid molecules, and the structure of the liposome membrane will change. In the loose and chaotic liquid crystal state, the drug is released.

因此,将植物精油及其组分通过热敏脂质体技术结合起来能够发挥两者的优势,制备出具有良好抗菌性能的抗菌剂,并应用到对织物的抗菌整理中,具有重要的应用价值和发展前景。Therefore, the combination of plant essential oils and their components through thermosensitive liposome technology can give full play to the advantages of the two, prepare antibacterial agents with good antibacterial properties, and apply them to the antibacterial finishing of fabrics, which has important application value and development prospects.

发明内容Contents of the invention

本发明所要解决的技术问题是提供一种带有薄荷香味的植物精油热敏脂质体整理织物的方法。The technical problem to be solved by the present invention is to provide a method for finishing fabrics with plant essential oil thermosensitive liposomes with mint fragrance.

为解决上述技术问题,本发明采用的技术方案如下:In order to solve the problems of the technologies described above, the technical scheme adopted in the present invention is as follows:

一种植物精油热敏脂质体整理织物的方法,包括如下步骤:A method for finishing fabrics with plant essential oil thermosensitive liposomes, comprising the steps of:

(1)将茶树精油、薄荷醇和艾叶精油低温下混合搅拌,得天然芳香抗菌剂;(1) Mix tea tree essential oil, menthol and mugwort essential oil at low temperature to obtain a natural aromatic antibacterial agent;

(2)将步骤(1)得到的天然芳香抗菌剂溶于磷酸盐缓冲溶液中;(2) dissolving the natural aromatic antibacterial agent obtained in step (1) in a phosphate buffer solution;

(3)将天然磷脂、磷脂酰胆碱、甘油磷脂、磷脂酰乙醇胺、磷脂酰丝氨酸和磷脂酸混合,加入胆固醇,溶于氯仿倒入容器(所述的容器例如圆底烧瓶)中,在室温下蒸发至容器壁形成一层均一的薄膜;(3) Mix natural phospholipids, phosphatidylcholine, glycerophospholipids, phosphatidylethanolamine, phosphatidylserine and phosphatidic acid, add cholesterol, dissolve it in chloroform and pour it into a container (such as a round-bottomed flask), at room temperature Evaporate down to the container wall to form a uniform film;

(4)在超声水浴中将步骤(2)得到的天然芳香抗菌剂的磷酸缓冲溶液加入步骤(3)得到的覆有薄膜的容器中,超声振荡后得热敏脂质体悬液;(4) adding the phosphate buffer solution of the natural aromatic antibacterial agent obtained in step (2) into the film-covered container obtained in step (3) in an ultrasonic water bath, and obtaining a heat-sensitive liposome suspension after ultrasonic oscillation;

(5)将胶粘剂加入步骤(4)得到的热敏脂质体悬液中,室温搅拌至完全溶解,制得热敏性芳香抗菌整理剂;(5) Add the adhesive to the heat-sensitive liposome suspension obtained in step (4), stir at room temperature until completely dissolved, and prepare a heat-sensitive aromatic antibacterial finishing agent;

(6)将织物浸轧在整理液中,二浸二轧,最后织物利用冻干法进行整理定型。(6) The fabric is dipped in the finishing solution, two dips and two pads, and finally the fabric is finished and shaped by freeze-drying.

步骤(1)中,所述的茶树精油、薄荷醇和艾叶精油的质量比为1~3.5:1:1~3,搅拌温度为0~4℃,搅拌转速为30~120转/分。In step (1), the mass ratio of the tea tree essential oil, menthol and mugwort essential oil is 1-3.5:1:1-3, the stirring temperature is 0-4°C, and the stirring speed is 30-120 rpm.

步骤(2)中,磷酸盐缓冲溶液按如下方法配制得到:氯化钠8g/L,氯化钾0.2g/L,磷酸氢二钠1.44g/L,磷酸氢二钾0.24g/L,溶剂为水,用盐酸调pH值至6.5,加入终浓度为6v/v%的吐温80。In step (2), the phosphate buffer solution was prepared as follows: sodium chloride 8g/L, potassium chloride 0.2g/L, disodium hydrogen phosphate 1.44g/L, dipotassium hydrogen phosphate 0.24g/L, solvent For water, adjust the pH value to 6.5 with hydrochloric acid, and add Tween 80 with a final concentration of 6v/v%.

步骤(2)中,天然芳香抗菌剂以15~30g/L的浓度加入磷酸盐缓冲溶液。In step (2), the natural aromatic antibacterial agent is added to the phosphate buffer solution at a concentration of 15-30 g/L.

步骤(3)中,所述的天然磷脂选自大豆卵磷脂或蛋黄卵磷脂;所述的磷脂酰胆碱选自1-肉豆蔻酰基-2-硬脂酰基卵磷脂、二棕榈酰基卵磷脂、二硬脂酰基卵磷脂或1-棕榈酰基-2-硬脂酰基卵磷脂;所述的甘油磷脂选自二棕榈酰磷脂酰甘油钠盐或二硬脂酰磷脂酰甘油钠盐;所述的磷脂酰乙醇胺选自二肉豆蔻酰磷脂酰乙醇胺、二棕榈酰磷脂酰乙醇胺或二硬脂酰磷脂酰乙醇胺;所述的磷脂酰丝氨酸选自二棕榈酰磷脂酰丝氨酸钠盐或二硬脂酰磷脂酰丝氨酸钠盐;所述的磷脂酸选自二肉豆蔻酰磷脂酸钠盐、二棕榈酰磷脂酸钠盐或二肉豆蔻酰磷脂酸钠盐;所述的天然磷脂、磷脂酰胆碱、甘油磷脂、磷脂酰乙醇胺、磷脂酰丝氨酸以及磷脂酸以物质的量之比为1:1:1:1:1:1混合;天然磷脂、磷脂酰胆碱、甘油磷脂、磷脂酰乙醇胺、磷脂酰丝氨酸和磷脂酸的混合物与胆固醇的质量比为4~9:1。In step (3), the natural phospholipid is selected from soybean lecithin or egg yolk lecithin; the phosphatidylcholine is selected from 1-myristoyl-2-stearoyl lecithin, dipalmitoyl lecithin, Distearoyl lecithin or 1-palmitoyl-2-stearoyl lecithin; the glycerophospholipid is selected from dipalmitoylphosphatidylglycerol sodium salt or distearoylphosphatidylglycerol sodium salt; the phospholipid Acylethanolamine is selected from dimyristoylphosphatidylethanolamine, dipalmitoylphosphatidylethanolamine or distearoylphosphatidylethanolamine; described phosphatidylserine is selected from dipalmitoylphosphatidylserine sodium salt or distearoylphosphatidylethanolamine Serine sodium salt; the phosphatidic acid is selected from dimyristoyl phosphatidic acid sodium salt, dipalmitoyl phosphatidic acid sodium salt or dimyristoyl phosphatidic acid sodium salt; the natural phospholipids, phosphatidylcholine, glycerophospholipid , phosphatidylethanolamine, phosphatidylserine and phosphatidic acid are mixed in a ratio of 1:1:1:1:1:1; natural phospholipids, phosphatidylcholine, glycerophospholipids, phosphatidylethanolamine, phosphatidylserine and The mass ratio of phosphatidic acid mixture to cholesterol is 4-9:1.

步骤(4)中,在55℃超声水浴中将含有天然芳香抗菌剂的磷酸缓冲溶液预热至55℃,并加入覆有薄膜的容器中,超声振荡10~50分钟得热敏脂质体悬液,超声频率为400MHz,振荡频率为200转/分;天然芳香抗菌剂与薄膜的质量比为3:2~1。薄膜的质量可按照磷脂混合物与胆固醇总质量计。In step (4), preheat the phosphate buffer solution containing the natural aromatic antibacterial agent to 55°C in an ultrasonic water bath at 55°C, put it into a container covered with a film, and vibrate ultrasonically for 10 to 50 minutes to obtain a thermosensitive liposome suspension. liquid, the ultrasonic frequency is 400MHz, and the oscillation frequency is 200 rpm; the mass ratio of the natural aromatic antibacterial agent to the film is 3:2-1. The mass of the film can be calculated according to the total mass of phospholipid mixture and cholesterol.

步骤(5)中,所述的胶粘剂选自淀粉、壳聚糖、海藻酸钠、羧甲基纤维素、糊精或聚乙烯醇;胶粘剂相对于热敏脂质体悬液的加入量为15~30g/L。In step (5), the adhesive is selected from starch, chitosan, sodium alginate, carboxymethyl cellulose, dextrin or polyvinyl alcohol; the amount of the adhesive relative to the thermosensitive liposome suspension is 15 ~30g/L.

步骤(6)中,将织物按浴比(即整理液与织物的质量比)为3~5:1浸轧在整理液中,二浸二轧,轧辊压力为0.1~0.25MPa,轧余率为80~100%。In step (6), the fabric is dipped in the finishing solution at a bath ratio (that is, the mass ratio of the finishing solution to the fabric) of 3 to 5:1, two dipping and two rolling, the roll pressure is 0.1 to 0.25 MPa, and the excess rate 80-100%.

步骤(6)中,所述的冻干法程序为:首先从室温以1℃/分钟的速率下降至-80℃,然后打开真空泵,进行冻干,真空度小于13Pa,-80℃维持24h,再以0.5℃/分钟的速率升温至-55℃,将氮气注入冻干室使气压回到1个大气压下,以自然升温速率恢复至室温,拿出冻干织物。In step (6), the procedure of the freeze-drying method is as follows: first, drop from room temperature to -80°C at a rate of 1°C/min, then turn on the vacuum pump for freeze-drying, the vacuum degree is less than 13Pa, and maintain at -80°C for 24h, Then raise the temperature to -55°C at a rate of 0.5°C/min, inject nitrogen gas into the freeze-drying chamber to return the air pressure to 1 atmosphere, return to room temperature at a natural heating rate, and take out the freeze-dried fabric.

上述方法制备得到的织物也在本发明的保护范围之内。该职务可制备医用材料、抗菌材料、纺织服装材料等,广泛应用于生物医学、纺织工业、医用抗菌保健等领域。The fabric prepared by the above method is also within the protection scope of the present invention. This position can prepare medical materials, antibacterial materials, textile and clothing materials, etc., which are widely used in biomedicine, textile industry, medical antibacterial health care and other fields.

有益效果:本发明制备方法与现有技术相比,具有以下优点:Beneficial effect: compared with the prior art, the preparation method of the present invention has the following advantages:

1、本发明整理的织物,在35-40℃实现“智能开关”功能,利用它一方面可以起到按温度高低自动调节精油组分释放,实现穿着服用过程中靶向抗菌,可在极短时间内快速杀灭微生物,提高抗菌效率;另一方面该织物在精油组分挥发时能够带走一部分体表热量,而且体表上温度较高,散热较多的部位,其凉感效果更加明显。1. The fabric finished by the present invention realizes the function of "smart switch" at 35-40°C. On the one hand, it can automatically adjust the release of essential oil components according to the temperature, and realize targeted antibacterial in the process of wearing and taking. It can be used in a very short time. Quickly kill microorganisms within a short period of time and improve antibacterial efficiency; on the other hand, the fabric can take away part of the body surface heat when the essential oil components volatilize, and the body surface has a higher temperature and more heat dissipation, and its cooling effect is more obvious .

2、与其他抗菌整理相比,本发明利用具有天然抗菌剂和生物相容性好的胶粘剂组成芳香抑菌整理剂,该整理剂是一种优越的无毒无害、可生物循环、透气性好的且在织物表面可成膜的新型整理剂,降低了化学试剂对人体皮肤造成的不良影响。2. Compared with other antibacterial finishes, the present invention uses natural antibacterial agents and adhesives with good biocompatibility to form an aromatic antibacterial finishing agent. A good new finishing agent that can form a film on the surface of the fabric, which reduces the adverse effects of chemical reagents on human skin.

3、综合了植物精油和脂质体两者的优势,结合冻干固化作用,将精油脂质体嵌入纤维中,不会破坏脂质体结构使精油脂质体更加稳定,抗菌活性强,热敏释放效果明显,广谱抑菌作用显著;3. Combining the advantages of both plant essential oils and liposomes, combined with freeze-drying and solidification, the essential oil liposomes are embedded in the fibers without destroying the liposome structure, making the essential oil liposomes more stable, with strong antibacterial activity and heat The sensitive release effect is obvious, and the broad-spectrum antibacterial effect is remarkable;

4、制备的织物具有一定的薄荷香味,能够一定程度优化环境,净化空气,还能加速消除人的神经紧张,缓解压力,愉悦心情,满足人们精神上的享受;4. The prepared fabric has a certain mint fragrance, which can optimize the environment to a certain extent, purify the air, and can also accelerate the elimination of people's nervous tension, relieve pressure, delight the mood, and satisfy people's spiritual enjoyment;

5、用途广泛,可用作医用材料、抗菌材料、纺织服装材料、保健卫生、抗菌护理等。5. It has a wide range of uses, and can be used as medical materials, antibacterial materials, textile and clothing materials, health care, antibacterial care, etc.

附图说明Description of drawings

图1织物中薄荷醇含量随时间变化曲线。Figure 1 Curve of menthol content in fabrics as a function of time.

图2织物热敏精油释放特性的测定曲线。Fig. 2 Determination curves of the release characteristics of fabric heat-sensitive essential oils.

具体实施方式Detailed ways

根据下述实施例,可以更好地理解本发明。然而,本领域的技术人员容易理解,实施例所描述的内容仅用于说明本发明,而不应当也不会限制权利要求书中所详细描述的本发明。The present invention can be better understood from the following examples. However, those skilled in the art can easily understand that the content described in the embodiments is only for illustrating the present invention, and should not and will not limit the present invention described in the claims.

实施例1:Example 1:

一种植物精油热敏脂质体整理织物的方法,包括如下步骤:A method for finishing fabrics with plant essential oil thermosensitive liposomes, comprising the steps of:

(1)将茶树精油、薄荷醇和艾叶精油按照质量比为1:1:1的比例在0℃下混合搅拌,搅拌转速为30转/分,即得天然芳香抗菌剂。(1) Mix tea tree essential oil, menthol and mugwort essential oil at a mass ratio of 1:1:1 at 0°C with a stirring speed of 30 rpm to obtain a natural aromatic antibacterial agent.

(2)配制磷酸盐缓冲溶液:氯化钠8g/L,氯化钾0.2g/L,磷酸氢二钠1.44g/L,磷酸氢二钾0.24g/L,用盐酸调pH至6.5,加入终浓度为6%v/v的吐温80。将天然芳香抗菌剂溶于上述磷酸盐缓冲溶液中,使得天然芳香抗菌剂的浓度为15g/L。(2) Prepare phosphate buffer solution: sodium chloride 8g/L, potassium chloride 0.2g/L, disodium hydrogen phosphate 1.44g/L, dipotassium hydrogen phosphate 0.24g/L, adjust pH to 6.5 with hydrochloric acid, add The final concentration was 6% v/v Tween 80. Dissolve the natural fragrance antibacterial agent in the above-mentioned phosphate buffer solution, so that the concentration of the natural fragrance antibacterial agent is 15g/L.

(3)将大豆卵磷脂、1-肉豆蔻酰基-2-硬脂酰基卵磷脂、二棕榈酰磷脂酰甘油钠盐、二肉豆蔻酰磷脂酰乙醇胺、二棕榈酰磷脂酰丝氨酸钠盐以及二肉豆蔻酰磷脂酸钠盐以物质的量之比为1:1:1:1:1:1混合。取磷脂混合物100mg与胆固醇25mg,溶于氯仿倒入圆底烧瓶中,在室温下旋蒸至瓶壁形成一层均一的薄膜。(3) Soybean lecithin, 1-myristoyl-2-stearoyl lecithin, dipalmitoylphosphatidylglycerol sodium salt, dimyristoylphosphatidylethanolamine, dipalmitoylphosphatidylserine sodium salt and dimeat The sodium myristoyl phosphatidic acid is mixed in a ratio of 1:1:1:1:1:1. Take 100 mg of phospholipid mixture and 25 mg of cholesterol, dissolve in chloroform and pour into a round bottom flask, and rotate at room temperature until a uniform film is formed on the wall of the bottle.

(4)在55℃超声水浴中将含有天然抗菌剂的磷酸盐缓冲溶液预热至55℃,并加入覆有薄膜的圆底烧瓶中,超声振荡10分钟,超声频率为400MHz,振荡频率为200转/分,天然芳香抗菌剂(不包括磷酸盐缓冲溶液的质量)与薄膜的质量比为3:1,制得热敏脂质体悬液。(4) Preheat the phosphate buffer solution containing natural antibacterial agents to 55°C in an ultrasonic water bath at 55°C, add it into a round-bottomed flask covered with a film, and oscillate ultrasonically for 10 minutes at a frequency of 400MHz and an oscillation frequency of 200 rev/min, the mass ratio of natural aromatic antibacterial agent (excluding the mass of phosphate buffer solution) to film is 3:1, and a heat-sensitive liposome suspension is prepared.

(5)将糊精作为胶粘剂以15g/L的浓度加入热敏脂质体悬液,室温搅拌至完全溶解,制得热敏性芳香抗菌整理剂;(5) Add dextrin as an adhesive to the heat-sensitive liposome suspension at a concentration of 15 g/L, stir at room temperature until completely dissolved, and obtain a heat-sensitive aromatic antibacterial finishing agent;

(6)将织物按浴比为3:1浸轧在整理液中,二浸二轧,轧辊压力为0.1MPa,轧余率为80%;最后织物从室温以1℃/分的速率下降至-80℃,然后打开真空泵,进行冻干,真空度小于13Pa,-80℃维持24h,再以0.5℃/分的速率升温至-55℃,将氮气注入冻干室使气压回到1个大气压下,以自然升温速率恢复至室温,拿出冻干织物。(6) Pad the fabric in the finishing solution with a bath ratio of 3:1, two dipping and two rolling, the roll pressure is 0.1MPa, and the excess rate is 80%; finally, the fabric drops from room temperature at a rate of 1°C/min to -80°C, then turn on the vacuum pump for freeze-drying, the vacuum degree is less than 13Pa, maintain at -80°C for 24 hours, then raise the temperature to -55°C at a rate of 0.5°C/min, inject nitrogen into the freeze-drying chamber to return the air pressure to 1 atmosphere Return to room temperature at a natural heating rate, and take out the freeze-dried fabric.

实施例2:Example 2:

一种植物精油热敏脂质体整理织物的方法,包括如下步骤:A method for finishing fabrics with plant essential oil thermosensitive liposomes, comprising the steps of:

(1)将茶树精油、薄荷醇和艾叶精油按照质量比为3.5:1:3的比例在4℃下混合搅拌,搅拌转速为120转/分,即得天然芳香抗菌剂;(1) Mix tea tree essential oil, menthol and mugwort essential oil at a mass ratio of 3.5:1:3 at 4°C with a stirring speed of 120 rpm to obtain a natural aromatic antibacterial agent;

(2)配制磷酸盐缓冲溶液:氯化钠8g/L,氯化钾0.2g/L,磷酸氢二钠1.44g/L,磷酸氢二钾0.24g/L,用盐酸调pH至6.5,加入终浓度为6%v/v的吐温80。将天然芳香抗菌剂溶于上述磷酸盐缓冲溶液中,使得天然芳香抗菌剂的浓度为30g/L。(2) Prepare phosphate buffer solution: sodium chloride 8g/L, potassium chloride 0.2g/L, disodium hydrogen phosphate 1.44g/L, dipotassium hydrogen phosphate 0.24g/L, adjust pH to 6.5 with hydrochloric acid, add The final concentration was 6% v/v Tween 80. Dissolve the natural fragrance antibacterial agent in the above-mentioned phosphate buffer solution, so that the concentration of the natural fragrance antibacterial agent is 30g/L.

(3)将蛋黄卵磷脂、二棕榈酰基卵磷脂、二硬脂酰磷脂酰甘油钠盐、二棕榈酰磷脂酰乙醇胺、二硬脂酰磷脂酰丝氨酸钠盐以及二棕榈酰磷脂酸钠盐以物质的量之比为1:1:1:1:1:1混合。取磷脂混合物100mg与胆固醇11.11mg,溶于氯仿倒入圆底烧瓶中,在室温下旋蒸至瓶壁形成一层均一的薄膜。(3) Egg yolk lecithin, dipalmitoyl lecithin, distearoylphosphatidylglycerol sodium salt, dipalmitoylphosphatidylethanolamine, distearoylphosphatidylserine sodium salt and dipalmitoylphosphatidic acid sodium salt as substances The volume ratio is 1:1:1:1:1:1 for mixing. Take 100 mg of phospholipid mixture and 11.11 mg of cholesterol, dissolve it in chloroform and pour it into a round bottom flask, and spin evaporate at room temperature until a uniform film is formed on the wall of the bottle.

(4)在55℃超声水浴中将含有天然抗菌剂的磷酸缓冲溶液预热至55℃,并加入覆有薄膜的圆底烧瓶中,超声振荡50分钟,超声频率为400MHz,振荡频率为200转/分,天然芳香抗菌剂(不包括磷酸盐缓冲溶液的质量)与薄膜的质量比为3:2,制得热敏脂质体悬液。(4) Preheat the phosphate buffer solution containing natural antibacterial agents to 55°C in an ultrasonic water bath at 55°C, add it to a round-bottomed flask covered with a film, and oscillate ultrasonically for 50 minutes at a frequency of 400MHz and 200 rpm /min, the mass ratio of natural aromatic antibacterial agent (not including the quality of phosphate buffer solution) to film is 3:2, and the thermosensitive liposome suspension is prepared.

(5)将聚乙烯醇作为胶粘剂以30g/L的浓度加入热敏脂质体悬液,室温搅拌至完全溶解,制得热敏性芳香抗菌整理剂;(5) Add polyvinyl alcohol as an adhesive to the heat-sensitive liposome suspension at a concentration of 30 g/L, stir at room temperature until completely dissolved, and obtain a heat-sensitive aromatic antibacterial finishing agent;

(6)将织物按浴比为5:1浸轧在整理液中,二浸二轧,轧辊压力为0.25MPa,轧余率为100%;最后织物从室温以1℃/分的速率下降至-80℃,然后打开真空泵,进行冻干,真空度小于13Pa,-80℃维持24h,再以0.5℃/分的速率升温至-55℃,将氮气注入冻干室使气压回到1个大气压下,以自然升温速率恢复至室温,拿出冻干织物。(6) Pad the fabric in the finishing solution with a bath ratio of 5:1, two dipping and two rolling, the roll pressure is 0.25MPa, and the excess rate is 100%; finally, the fabric drops from room temperature at a rate of 1°C/min to -80°C, then turn on the vacuum pump for freeze-drying, the vacuum degree is less than 13Pa, maintain at -80°C for 24 hours, then raise the temperature to -55°C at a rate of 0.5°C/min, inject nitrogen into the freeze-drying chamber to return the air pressure to 1 atmosphere Return to room temperature at a natural heating rate, and take out the freeze-dried fabric.

实施例3:Example 3:

一种植物精油热敏脂质体整理织物的方法,包括如下步骤:A method for finishing fabrics with plant essential oil thermosensitive liposomes, comprising the steps of:

(1)将茶树精油、薄荷醇和艾叶精油按照质量比为2:1:2的比例在2℃下混合搅拌,搅拌转速为60转/分,即得天然芳香抗菌剂。(1) Mix and stir tea tree essential oil, menthol and mugwort essential oil at a mass ratio of 2:1:2 at 2°C at a stirring speed of 60 rpm to obtain a natural aromatic antibacterial agent.

(2)配制磷酸盐缓冲溶液:氯化钠8g/L,氯化钾0.2g/L,磷酸氢二钠1.44g/L,磷酸氢二钾0.24g/L,用盐酸调pH至6.5,加入终浓度为6%v/v的吐温80。将天然芳香抗菌剂溶于上述磷酸盐缓冲溶液中,使得天然芳香抗菌剂的浓度为20g/L。(2) Prepare phosphate buffer solution: sodium chloride 8g/L, potassium chloride 0.2g/L, disodium hydrogen phosphate 1.44g/L, dipotassium hydrogen phosphate 0.24g/L, adjust pH to 6.5 with hydrochloric acid, add The final concentration was 6% v/v Tween 80. Dissolve the natural fragrance antibacterial agent in the above-mentioned phosphate buffer solution, so that the concentration of the natural fragrance antibacterial agent is 20g/L.

(3)将蛋黄卵磷脂、二硬脂酰基卵磷脂、二硬脂酰磷脂酰甘油钠盐、二棕榈酰磷脂酰乙醇胺、二硬脂酰磷脂酰丝氨酸钠盐以及二肉豆蔻酰磷脂酸钠盐以物质的量之比为1:1:1:1:1:1混合。取磷脂混合物100mg与胆固醇25mg,溶于氯仿倒入圆底烧瓶中,在室温下旋蒸至瓶壁形成一层均一的薄膜。(3) Egg yolk lecithin, distearoyl lecithin, distearoylphosphatidylglycerol sodium salt, dipalmitoylphosphatidylethanolamine, distearoylphosphatidylserine sodium salt and dimyristoylphosphatidic acid sodium salt The ratio of the amount of substances is 1:1:1:1:1:1. Take 100 mg of phospholipid mixture and 25 mg of cholesterol, dissolve in chloroform and pour into a round bottom flask, and rotate at room temperature until a uniform film is formed on the wall of the bottle.

(4)在55℃超声水浴中将含有天然抗菌剂的磷酸缓冲溶液预热至55℃,并加入覆有薄膜的圆底烧瓶中,超声振荡15分钟,超声频率为400MHz,振荡频率为200转/分,天然芳香抗菌剂(不包括磷酸盐缓冲溶液的质量)与薄膜的质量比为2:1,制得热敏脂质体悬液。(4) Preheat the phosphate buffer solution containing natural antibacterial agents to 55°C in an ultrasonic water bath at 55°C, and add it to a round-bottomed flask covered with a film, and oscillate ultrasonically for 15 minutes at a frequency of 400MHz and 200 rpm /min, the mass ratio of natural aromatic antibacterial agent (not including the quality of phosphate buffer solution) to film is 2:1, and a thermosensitive liposome suspension is prepared.

(5)将壳聚糖作为胶粘剂以20g/L的浓度加入热敏脂质体悬液,室温搅拌至完全溶解,制得热敏性芳香抗菌整理剂。(5) Add chitosan as an adhesive to the heat-sensitive liposome suspension at a concentration of 20 g/L, stir at room temperature until completely dissolved, and obtain a heat-sensitive aromatic antibacterial finishing agent.

(6)将织物按浴比为4:1浸轧在整理液中,二浸二轧,轧辊压力为0.2MPa,轧余率为95%;最后织物从室温以1℃/分的速率下降至-80℃,然后打开真空泵,进行冻干,真空度小于13Pa,-80℃维持24h,再以0.5℃/分的速率升温至-55℃,将氮气注入冻干室使气压回到1个大气压下,以自然升温速率恢复至室温,拿出冻干织物。(6) Pad the fabric in the finishing solution with a bath ratio of 4:1, two dips and two rolls, the roll pressure is 0.2MPa, and the excess rate is 95%; finally, the fabric drops from room temperature at a rate of 1°C/min to -80°C, then turn on the vacuum pump for freeze-drying, the vacuum degree is less than 13Pa, maintain at -80°C for 24 hours, then raise the temperature to -55°C at a rate of 0.5°C/min, inject nitrogen into the freeze-drying chamber to return the air pressure to 1 atmosphere Return to room temperature at a natural heating rate, and take out the freeze-dried fabric.

对比例1:Comparative example 1:

一种植物精油整理织物的方法,包括如下步骤:A method for finishing fabrics with plant essential oils, comprising the steps of:

(1)将茶树精油、薄荷醇和艾叶精油按照质量比为2:1:2的比例在2℃下混合搅拌,搅拌转速为60转/分,即得天然芳香抗菌剂;(1) Mix tea tree essential oil, menthol and mugwort essential oil at a mass ratio of 2:1:2 at 2°C with a stirring speed of 60 rpm to obtain a natural aromatic antibacterial agent;

(2)配制磷酸缓冲盐溶液:氯化钠8g/L,氯化钾0.2g/L,磷酸氢二钠1.44g/L,磷酸氢二钾0.24g/L,用盐酸调pH至6.5,加入终浓度为6%v/v的吐温80。(2) Prepare phosphate buffered saline solution: sodium chloride 8g/L, potassium chloride 0.2g/L, disodium hydrogen phosphate 1.44g/L, dipotassium hydrogen phosphate 0.24g/L, adjust pH to 6.5 with hydrochloric acid, add The final concentration was 6% v/v Tween 80.

(3)在磷酸缓冲溶液中加入20g/L天然芳香抗菌剂和20g/L壳聚糖,室温搅拌至完全溶解,制得芳香抗菌整理剂。(3) Add 20g/L natural aromatic antibacterial agent and 20g/L chitosan to the phosphate buffer solution, stir at room temperature until completely dissolved, and obtain an aromatic antibacterial finishing agent.

(4)将织物按浴比为4:1浸轧在整理液中,二浸二轧,轧辊压力为0.2MPa,轧余率为95%;最后织物从室温以1℃/分的速率下降至-80℃,然后打开真空泵,进行冻干,真空度小于13Pa,-80℃维持24h,再以0.5℃/分的速率升温至-55℃,将氮气注入冻干室使气压回到1个大气压下,以自然升温速率恢复至室温,拿出冻干织物。(4) The fabric is dipped in the finishing solution at a bath ratio of 4:1, two dips and two rolls, the roll pressure is 0.2MPa, and the excess rate is 95%; finally, the fabric drops from room temperature at a rate of 1°C/min to -80°C, then turn on the vacuum pump for freeze-drying, the vacuum degree is less than 13Pa, maintain at -80°C for 24 hours, then raise the temperature to -55°C at a rate of 0.5°C/min, inject nitrogen into the freeze-drying chamber to return the air pressure to 1 atmosphere Return to room temperature at a natural heating rate, and take out the freeze-dried fabric.

对比例2:Comparative example 2:

一种植物精油整理织物的方法,包括如下步骤:A method for finishing fabrics with plant essential oils, comprising the steps of:

(1)将茶树精油、薄荷醇和艾叶精油按照质量比为2:1:2的比例在2℃下混合搅拌,搅拌转速为60转/分,即得天然芳香抗菌剂;(1) Mix tea tree essential oil, menthol and mugwort essential oil at a mass ratio of 2:1:2 at 2°C with a stirring speed of 60 rpm to obtain a natural aromatic antibacterial agent;

(2)配制磷酸缓冲盐溶液:氯化钠8g/L,氯化钾0.2g/L,磷酸氢二钠1.44g/L,磷酸氢二钾0.24g/L,用盐酸调pH至6.5,加入终浓度为6%v/v的吐温80。(2) Prepare phosphate buffered saline solution: sodium chloride 8g/L, potassium chloride 0.2g/L, disodium hydrogen phosphate 1.44g/L, dipotassium hydrogen phosphate 0.24g/L, adjust pH to 6.5 with hydrochloric acid, add The final concentration was 6% v/v Tween 80.

(3)在磷酸缓冲溶液中加入20g/L天然芳香抗菌剂和20g/L壳聚糖,室温搅拌至完全溶解,制得芳香抗菌整理剂。(3) Add 20g/L natural aromatic antibacterial agent and 20g/L chitosan to the phosphate buffer solution, stir at room temperature until completely dissolved, and obtain an aromatic antibacterial finishing agent.

(4)将织物按浴比为4:1浸轧在整理液中,二浸二轧,轧辊压力为0.2MPa,轧余率为95%;将二浸二轧处理的织物在110℃烘箱中烘5分钟,再经过水洗,烘干定型。(4) Pad the fabric in the finishing solution according to the bath ratio of 4:1, double dipping and second rolling, the roll pressure is 0.2MPa, and the excess rate is 95%; the fabric treated by the second dipping and second rolling is placed in an oven at 110°C Bake for 5 minutes, then wash with water and dry to set the shape.

实施例4:Example 4:

精油及薄荷醇含量测定:Determination of essential oil and menthol content:

称取一定量样品,用乙醇提取,再用265nm吸光度检定精油含量,用气相色谱测定薄荷醇含量。气相色谱方法:色谱柱为SE-5430m×0.32m×0.25μm;载气为氮气,流速为1ml/min;采用程序升温,70℃维持1min,然后以5℃/min升温,最后140℃保持1min;进样口温度为250℃,检测器温度为250℃;检测器为氢离子火焰检测器;分流比50:1;进样量为0.4μl。A certain amount of sample was weighed, extracted with ethanol, and then the content of essential oil was tested by absorbance at 265nm, and the content of menthol was determined by gas chromatography. Gas chromatography method: the chromatographic column is SE-5430m×0.32m×0.25μm; the carrier gas is nitrogen, the flow rate is 1ml/min; the temperature is programmed, 70°C is maintained for 1min, then the temperature is raised at 5°C/min, and finally 140°C is maintained for 1min ; The temperature of the injection port is 250°C, and the temperature of the detector is 250°C; the detector is a hydrogen ion flame detector; the split ratio is 50:1; the injection volume is 0.4 μl.

精油及薄荷醇含量测定结果见表1。The results of determination of essential oil and menthol content are shown in Table 1.

表1Table 1

精油含量mg/gEssential oil content mg/g 薄荷醇含量mg/gMenthol content mg/g 实施例1Example 1 5858 1818 实施例2Example 2 9595 1212 实施例3Example 3 7878 1414 对比例1Comparative example 1 7575 1313 对比例2Comparative example 2 77 11

实施例1、2、3和对比例1采用冻干后整理技术整理织物,使得大部分的精油和薄荷醇保留在织物中,而对比例2采用高温烘干整理织物,使得精油组分和薄荷醇迅速挥发,织物中仅存微量的精油和薄荷醇。Embodiment 1, 2, 3 and comparative example 1 adopt freeze-drying post-finishing technology to finish the fabric, make most of the essential oil and menthol remain in the fabric, and comparative example 2 adopts high-temperature drying to finish the fabric, make the essential oil component and peppermint Alcohol evaporates quickly, leaving only traces of essential oils and menthol in the fabric.

香气释放测定:将样品放入25℃,气压为1标准大气压,湿度50%的环境中每过一月取出样品剪下1cm×1cm方块,用乙醇提取,测定薄荷醇含量,以初始样品中的薄荷醇含量为100%计。Determination of aroma release: Put the sample in an environment of 25°C, 1 standard atmospheric pressure, and 50% humidity. Take out the sample every month, cut a 1cm×1cm square, extract with ethanol, and measure the menthol content. Menthol content is 100%.

由上述实施例和对比例所制得的五种织物,薄荷醇含量结果见图1。The results of the menthol content of the five fabrics prepared in the above examples and comparative examples are shown in FIG. 1 .

与对比例比较,实施例1、2、3采用热敏脂质体技术有效降低了薄荷醇的挥发速率,达到了长久释放香气的效果。制备的织物带有薄荷香味,随着时间的推移,芳香气味逐渐释放、减弱,这种香味能够创造怡人舒适的环境,缓解和释放压力,有助于人的身心健康。Compared with the comparative examples, the heat-sensitive liposome technology used in Examples 1, 2, and 3 effectively reduces the volatilization rate of menthol and achieves the effect of long-term release of fragrance. The prepared fabric has mint fragrance, and as time goes by, the fragrance smell is gradually released and weakened, the fragrance can create a pleasant and comfortable environment, relieve and release pressure, and contribute to people's physical and mental health.

织物热敏精油释放特性的测定:由上述实施例和对比例所制得的五种织物,取12组试管分别置于32,33,34,35,36,37,38,39,40,41,42共12组不同温度水浴中预热15min后,每支试管中各加入0.1g织物,振摇,72h后迅速从每组水浴中取出试管置于液氮中冷却,取样,用乙醇提取,分别在265nm下测定精油含量,计算释放率,作图2。The mensuration of the heat-sensitive essential oil release characteristic of fabric: by the five kinds of fabrics that above-mentioned embodiment and comparative example make, get 12 groups of test tubes and place respectively in 32,33,34,35,36,37,38,39,40,41 ,42 A total of 12 groups of water baths with different temperatures were preheated for 15 minutes, each test tube was added with 0.1g of fabric, shaken, and after 72 hours, the test tubes were quickly taken out of each group of water baths and placed in liquid nitrogen to cool, samples were taken, and extracted with ethanol. The essential oil content was measured at 265nm respectively, and the release rate was calculated, as shown in Figure 2.

实施例1、2、3采用热敏脂质体技术使得织物能够随着温度的变化将精油组分释放出来,而对比例则无此效果。Examples 1, 2, and 3 use thermosensitive liposome technology to enable the fabric to release the essential oil component as the temperature changes, while the comparative example has no such effect.

织物耐洗次数实验:由上述实施例和对比例所制得的五种织物,根据AATCC100-2004和AATCC124-2006标准检验其洗涤后对金黄色葡萄球菌、大肠杆菌、白色念珠菌、红色毛癣菌、须癣毛癣菌、絮状表皮癣菌抑菌效果见表2。Fabric washability test: by the five kinds of fabrics that above-mentioned embodiment and comparative example make, according to AATCC100-2004 and AATCC124-2006 standard test its anti-staphylococcus aureus, Escherichia coli, Candida albicans, trichophyton rubrum after washing bacteria, Trichophyton mentagrophytes, and Epidermophyton flocculus are shown in Table 2.

表2Table 2

本发明所整理后的织物,对金黄色葡萄球菌、大肠杆菌、白色念珠菌、红色毛癣菌、须癣毛癣菌、絮状表皮癣菌均有显著的抑制效果,抗菌效果缓慢释放,经过多次洗涤后保持较高的抑菌率。而对比例,经多次洗涤后,对各种微生物的抑制效果明显降低。The fabric finished by the present invention has significant inhibitory effects on Staphylococcus aureus, Escherichia coli, Candida albicans, Trichophyton rubrum, Trichophyton mentagrophytes, and Epidermophyton flocculus, and the antibacterial effect is released slowly. It maintains a high antibacterial rate after multiple washings. In the comparative example, after repeated washing, the inhibitory effect on various microorganisms was significantly reduced.

Claims (8)

1.一种植物精油热敏脂质体整理织物的方法,其特征在于,包括如下步骤:1. a method for plant essential oil thermosensitive liposome finishing fabric, is characterized in that, comprises the steps: (1)将茶树精油、薄荷醇和艾叶精油低温下混合搅拌,得天然芳香抗菌剂;(1) Mix and stir tea tree essential oil, menthol and Artemisia argyi essential oil at low temperature to obtain a natural aromatic antibacterial agent; (2)将步骤(1)得到的天然芳香抗菌剂溶于磷酸盐缓冲溶液中;(2) the natural aromatic antibacterial agent that step (1) obtains is dissolved in the phosphate buffered saline solution; (3)将天然磷脂、磷脂酰胆碱、甘油磷脂、磷脂酰乙醇胺、磷脂酰丝氨酸和磷脂酸混合,加入胆固醇,溶于氯仿倒入容器中,在室温下蒸发至容器壁形成一层均一的薄膜;(3) Mix natural phospholipids, phosphatidylcholine, glycerophospholipids, phosphatidylethanolamine, phosphatidylserine and phosphatidic acid, add cholesterol, dissolve in chloroform and pour into a container, and evaporate to the container wall at room temperature to form a uniform layer film; (4)在超声水浴中将步骤(2)得到的天然芳香抗菌剂的磷酸盐缓冲溶液加入步骤(3)得到的覆有薄膜的容器中,超声振荡后得热敏脂质体悬液;(4) Add the phosphate buffered saline solution of the natural aromatic antibacterial agent obtained in step (2) in the ultrasonic water bath to the container covered with film obtained in step (3), and obtain the thermosensitive liposome suspension after ultrasonic oscillation; (5)将胶粘剂加入步骤(4)得到的热敏脂质体悬液中,室温搅拌至完全溶解,制得热敏性芳香抗菌整理剂;(5) adding the adhesive to the heat-sensitive liposome suspension obtained in step (4), and stirring at room temperature until completely dissolved to obtain a heat-sensitive aromatic antibacterial finishing agent; (6)将织物浸轧在整理液中,二浸二轧,最后织物利用冻干法进行整理定型;(6) padding the fabric in the finishing solution, two dipping and two rolling, and finally the fabric is finished and shaped by freeze-drying; 步骤(3)中,所述的天然磷脂选自大豆卵磷脂或蛋黄卵磷脂;所述的磷脂酰胆碱选自1-肉豆蔻酰基-2-硬脂酰基卵磷脂、二棕榈酰基卵磷脂、二硬脂酰基卵磷脂或1-棕榈酰基-2-硬脂酰基卵磷脂;所述的甘油磷脂选自二棕榈酰磷脂酰甘油钠盐或二硬脂酰磷脂酰甘油钠盐;所述的磷脂酰乙醇胺选自二肉豆蔻酰磷脂酰乙醇胺、二棕榈酰磷脂酰乙醇胺或二硬脂酰磷脂酰乙醇胺;所述的磷脂酰丝氨酸选自二棕榈酰磷脂酰丝氨酸钠盐或二硬脂酰磷脂酰丝氨酸钠盐;所述的磷脂酸选自二肉豆蔻酰磷脂酸钠盐、二棕榈酰磷脂酸钠盐或二肉豆蔻酰磷脂酸钠盐;所述的天然磷脂、磷脂酰胆碱、甘油磷脂、磷脂酰乙醇胺、磷脂酰丝氨酸以及磷脂酸以物质的量之比为1:1:1:1:1:1混合;天然磷脂、磷脂酰胆碱、甘油磷脂、磷脂酰乙醇胺、磷脂酰丝氨酸和磷脂酸的混合物与胆固醇的质量比为4~9:1。In step (3), described natural phospholipid is selected from soybean lecithin or egg yolk lecithin; Described phosphatidylcholine is selected from 1-myristoyl-2-stearoyl lecithin, dipalmitoyl lecithin, Distearoyl lecithin or 1-palmitoyl-2-stearoyl lecithin; described glycerophospholipid is selected from dipalmitoylphosphatidylglycerol sodium salt or distearoylphosphatidylglycerol sodium salt; described phospholipid Acylethanolamine is selected from dimyristoylphosphatidylethanolamine, dipalmitoylphosphatidylethanolamine or distearoylphosphatidylethanolamine; described phosphatidylserine is selected from dipalmitoylphosphatidylserine sodium salt or distearoylphosphatidylethanolamine Serine sodium salt; the phosphatidic acid is selected from dimyristoyl phosphatidic acid sodium salt, dipalmitoyl phosphatidic acid sodium salt or dimyristoyl phosphatidic acid sodium salt; the natural phospholipids, phosphatidylcholine, glycerophospholipid , phosphatidylethanolamine, phosphatidylserine and phosphatidic acid are mixed in a ratio of 1:1:1:1:1:1; natural phospholipids, phosphatidylcholine, glycerophospholipids, phosphatidylethanolamine, phosphatidylserine and The mass ratio of phosphatidic acid mixture to cholesterol is 4-9:1. 2.根据权利要求1所述的植物精油热敏脂质体整理织物的方法,其特征在于,步骤(1)中,所述的茶树精油、薄荷醇和艾叶精油的质量比为1~3.5:1:1~3,搅拌温度为0~4℃,搅拌转速为30~120转/分。2. the method for plant essential oil thermosensitive liposome finishing fabric according to claim 1, is characterized in that, in step (1), the mass ratio of described tea tree essential oil, menthol and Folium Artemisiae Argyi quintessence oil is 1~3.5:1 :1~3, the stirring temperature is 0~4°C, and the stirring speed is 30~120 rpm. 3.根据权利要求1所述的植物精油热敏脂质体整理织物的方法,其特征在于,步骤(2)中,天然芳香抗菌剂以15~30g/L的浓度加入磷酸盐缓冲溶液。3. the method for finishing fabric with plant essential oil thermosensitive liposome according to claim 1, is characterized in that, in step (2), natural fragrance antibacterial agent adds phosphate buffered saline with the concentration of 15~30g/L. 4.根据权利要求1所述的植物精油热敏脂质体整理织物的方法,其特征在于,步骤(4)中,在55℃超声水浴中将含有天然芳香抗菌剂的磷酸盐缓冲溶液预热至55℃,并加入覆有薄膜的容器中,超声振荡10~50分钟得热敏脂质体悬液,超声频率为400MHz,振荡频率为200转/分;天然芳香抗菌剂与薄膜的质量比为3:2~1。4. the method for plant essential oil thermosensitive liposome finishing fabric according to claim 1, is characterized in that, in step (4), in 55 ℃ of supersonic water baths, the phosphate buffer solution preheating that will contain natural aromatic antiseptic to 55°C, and added to a container covered with a film, ultrasonically oscillating for 10 to 50 minutes to obtain a thermosensitive liposome suspension, the ultrasonic frequency is 400MHz, and the oscillation frequency is 200 rpm; It is 3:2~1. 5.根据权利要求1所述的植物精油热敏脂质体整理织物的方法,其特征在于,步骤(5)中,所述的胶粘剂选自淀粉、壳聚糖、海藻酸钠、羧甲基纤维素、糊精或聚乙烯醇;胶粘剂相对于热敏脂质体悬液的加入量为15~30g/L。5. the method for plant essential oil thermosensitive liposome finishing fabric according to claim 1, is characterized in that, in step (5), described tackiness agent is selected from starch, chitosan, sodium alginate, carboxymethyl Cellulose, dextrin or polyvinyl alcohol; the amount of the adhesive relative to the thermosensitive liposome suspension is 15-30 g/L. 6.根据权利要求1所述的植物精油热敏脂质体整理织物的方法,其特征在于,步骤(6)中,将织物按浴比为3~5:1浸轧在整理液中,二浸二轧,轧辊压力为0.1~0.25MPa,轧余率为80~100%。6. the method for plant essential oil thermosensitive liposome finishing fabric according to claim 1, it is characterized in that, in step (6), fabric is 3~5:1 padding in finishing liquid by bath ratio, two Dipping and rolling, the pressure of the roll is 0.1-0.25MPa, and the excess rate is 80-100%. 7.根据权利要求1所述的植物精油热敏脂质体整理织物的方法,其特征在于,步骤(6)中,所述的冻干法程序为:首先从室温以1℃/分钟的速率下降至-80℃,然后打开真空泵,进行冻干,真空度小于13Pa,-80℃维持24h,再以0.5℃/分钟的速率升温至-55℃,将氮气注入冻干室使气压回到1个大气压下,以自然升温速率恢复至室温,拿出冻干织物。7. the method for finishing fabric with vegetable essential oil thermosensitive liposome according to claim 1, is characterized in that, in step (6), described freeze-drying method program is: at first from room temperature with the rate of 1 ℃/minute Decrease to -80°C, then turn on the vacuum pump for freeze-drying, the vacuum degree is less than 13Pa, maintain at -80°C for 24 hours, then raise the temperature to -55°C at a rate of 0.5°C/min, inject nitrogen into the freeze-drying chamber to bring the pressure back to 1 Atmospheric pressure, return to room temperature at a natural heating rate, and take out the freeze-dried fabric. 8.权利要求1~7中任意一项所述的植物精油热敏脂质体整理织物的方法制备得到的织物。8. The fabric prepared by the method for finishing fabric with vegetable essential oil thermosensitive liposome according to any one of claims 1 to 7.
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