CN108677530A - antibacterial finishing agent and its preparation method and application - Google Patents

antibacterial finishing agent and its preparation method and application Download PDF

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Publication number
CN108677530A
CN108677530A CN201810464920.7A CN201810464920A CN108677530A CN 108677530 A CN108677530 A CN 108677530A CN 201810464920 A CN201810464920 A CN 201810464920A CN 108677530 A CN108677530 A CN 108677530A
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propolis
ethanol solution
solution
finishing agent
antibacterial finishing
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CN108677530B (en
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张彦
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Xinxiang Olive Branch Textile Chemical Co Ltd
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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
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • 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
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/17Natural resins, resinous alcohols, resinous acids, or derivatives thereof
    • 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
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • 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
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • 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
    • D06M2200/50Modified hand or grip properties; Softening compositions

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention belongs to the treatment fluid technical fields of after-finishing of textile products, are related to antibacterial finishing agent and its preparation method and application.The antibacterial finishing agent, including:Propolis ethanol solution and chitosan solution.The preparation method of the antibacterial finishing agent, including:Propolis ethanol solution is added in chitosan solution, is sufficiently mixed uniformly to get the antibacterial finishing agent.The present invention using propolis ethanol solution and chitosan solution as raw material, not only good anti-bacterial effect, high to fabric affinity and antibacterial durability is good, but also safe and reliable, environmentally protective, have no toxic side effect, and there is health-care effect.And preparation method is simple, and practical, easy to implement, at low cost, environmental benefit is good, application easy to spread.

Description

Antibacterial finishing agent and its preparation method and application
Technical field
The present invention relates to the treatment fluid technical fields of after-finishing of textile products, in particular to a kind of antibacterial finishing agent And its preparation method and application.
Background technology
For a long time, the health of the mankind is constantly subjected to environmental pollution, the threat of bacterial infection;So that countries in the world are to antibacterial The research of agent is more paid attention to, the research of antibacterial fabric finishing liquid (finishing agent) have become weaving, dyeing a big hot spot.
Currently, there are many antibiotic finish materials applied in the market, such as silver system anti-biotic material, natural antibacterial material, chemistry Anti-biotic material etc..Wherein, silver system anti-biotic material is mainly using nano silver, and nano silver is as a kind of highly effective inorganic antibacterial Material is widely used in fields such as medicine, biology, environmental protections, shows good antibiotic and sterilizing effect. Occur more and more curable product or material containing nano silver in the clinical treatments such as burns unit, gynaecology, dept. of dermatology, the department of stomatology Material, and achieve good medical effect.Efficient, wide spectrum, antibacterial action are strong and it is resistance to be not likely to produce bacterium due to having for nano silver The features such as pharmacological property, becomes current one of preferred antiseptic.But the toxicity research report in relation to nano silver is also more, with each The commercialization of the nano silver of kind of purposes and industrialized production, people touch nano silver more and more, and nano silver also by Breathing sucking, ingestion of medicines, skin contact and other approach enter human body.Trop etc. reports liver caused by Nanometer silver dressing Dirty enzyme increases and the case of argyrism reaction.Studies have shown that the nano silver particles of 15,100nm generate toxicity to hepatocytes. Therefore, while selecting nano silver as anti-biotic material, safety and issuable toxic effect also can not be ignored.
In chemical anti-biotic material, triclosan is common antiseptic in textile, but triclosan is under certain condition, can To generate dioxin-like compound.And at carcinogenic aspect, the hepatic sclerosis of long-term exposure triclosan meeting inducing mouse is had been reported that in early days, In the recent period, reporting triclosan again in the article of PNAS in 2014 plays the role of liver tumour accelerating agent, and Science in 2016 is miscellaneous Will also proposed the hepatotoxicity wind agitation effect of triclosan.It can be seen that anti-selecting the triclosan for living closely bound up with people to be used as While bacterium material, hepatotoxicity wind agitation effect is also very important.
Natural antibacterial material in natural antibacterial agent essentially from natural plants extraction, such as chitin, mustard, castor-oil plant Oil, horseradish etc., such anti-biotic material is using simplicity, but antibacterial action is limited, and heat resistance is poor, and sterilizing rate is low, and it is long to be unable to wide spectrum Effect uses and quantity is seldom;Also medicinal properties are also very limited for health care.In addition, chitosan is also common antibacterial in textile industry Material, it is resourceful, nontoxic, pollution-free as a kind of environmentally protective new material, there are many natural advantageous properties;But Be chitosan antibacterial effect not as good as silver or organic antibacterial agent, it is poor to the durability of fabric.
Currently, the textile industry in China has large development in yield and technology, it is attached that this allows textile industry to pursue product It is value added to have solid foundation.On the other hand, as the improvement of people's living standards, people not only increasingly pay attention to textile Aesthetic appearance, and start to pursue the comfortableness and security of textile, or even requirement also proposed to the health of textile. However, existing anti-biotic material all has certain advantage it can be seen from above, there is also some disadvantages of person, especially pacify Full property is unreliable, it is not only possible to cause some toxic side effects, with less health-care effect.Therefore, a kind of antibacterial is researched and developed Effect is good, it is environmentally protective, safe and reliable, have no toxic side effect, novel antibacterial finishing agent also with health role knits raising The further development of the added value and promotion textile industry of object plays an important role.
In consideration of it, special propose the present invention.
Invention content
The first object of the present invention is to provide a kind of antibacterial finishing agent, is original with propolis ethanol solution and chitosan solution Expect, not only good anti-bacterial effect, good to fabric affinity height and antibacterial durability but also safe and reliable, environmentally protective, nontoxic pair Effect, and there is health-care effect, the improvement to conduce to sleep.
The second object of the present invention is to provide a kind of preparation method of antibacterial finishing agent, easy to operate, easy to implement, at This is low, and environmental benefit is good, application easy to spread.
The third object of the present invention is to provide a kind of application of antibacterial finishing agent in textile, which has Good anti-bacterial effect, and antibacterial durability high to fabric affinity be good, it is safe and reliable, environmentally protective, have no toxic side effect, have and protect The features such as strong effect, thus can apply during the final finishing of textile.
To achieve the above object, the technical solution adopted by the present invention is:
According to an aspect of the present invention, the present invention provides a kind of antibacterial finishing agent, including:
Propolis ethanol solution and chitosan solution.
As further preferred technical solution, including following component:
The propolis ethanol solution of 8~30g/L and the chitosan solution of 1~7g/L;
Preferably, including following component:The propolis ethanol solution of 10~20g/L and the chitosan solution of 2~6g/L;
Preferably, including following component:The propolis ethanol solution of 10~15g/L and the chitosan solution of 2~5g/L.
As further preferred technical solution, in the antibacterial finishing agent, the body of propolis ethanol solution and chitosan solution Product is than being (1~100):(900~999);
Preferably, the volume ratio of propolis ethanol solution and chitosan solution is (2~90):(910~998);
Preferably, the volume ratio of propolis ethanol solution and chitosan solution is (5~50):(950~995).
As further preferred technical solution, in the propolis ethanol solution, weight and the volumetric concentration of propolis are 50% The ratio of the volume of~97% ethanol solution is 1g:(60~100) mL;
Preferably, the volumetric concentration of ethanol solution is 55%~65%;
Preferably, the volumetric concentration of ethanol solution is 60%.
According to another aspect of the present invention, the present invention provides a kind of preparation method of the antibacterial finishing agent, by propolis Ethanol solution is added in chitosan solution, is sufficiently mixed uniformly to get the antibacterial finishing agent.
As further preferred technical solution, the preparation method of propolis ethanol solution includes:
10~20g of propolis is weighed, is shredded, is added in the ethanol solution that 1000mL volumetric concentrations are 50%~97%, room The lower extraction of temperature 70~75 hours, removal impurity is to get the propolis ethanol solution;
Preferably, the preparation method of propolis ethanol solution includes:
10~15g of propolis is weighed, is shredded, is added in the ethanol solution that 1000mL volumetric concentrations are 55%~65%, room The lower extraction of temperature 72 hours, removal impurity is to get the propolis ethanol solution.
According to another aspect of the present invention, the present invention provides a kind of antibacterial finishing agent as described above resisting in textile Application in bacterium arrangement.
As further preferred technical solution, fabric is immersed in above-mentioned antibacterial finishing agent, or fabric is immersed In antibacterial finishing agent after to dilution, is impregnated or padded, then dried.
It as further preferred technical solution, pads for an immersing and rolling, pick-up is 75%~85%.
As further preferred technical solution, the temperature of drying is 120~160 DEG C.
Compared with prior art, the beneficial effects of the present invention are:
The antibacterial finishing agent of the present invention, mainly using propolis ethanol solution and chitosan solution as raw material, propolis therein is A kind of natural antiseptic with good antibacterial and anti-inflammation functions, while also having good medical care effect such as anticancer, carrying High immunity etc., it is environmentally protective, it has excellent performance, securely and reliably, can alleviate existing antiseptic there are antibacterial effects and is general, water-fast Washing property is poor, safety is poor, may cause the problem of toxic side effect.
Propolis ethanol solution and chitosan solution are used in compounding, the main peptizaiton for utilizing chitosan colloid makes bee What glue was stablized is dispersed in colloid, prevents propolis from assembling to form spot;In addition, chitosan itself also has antibacterial action, belong to Natural green environment-friendly products are used cooperatively with propolis antiseptic, can further promote the antibacterial effect of antiseptic, meanwhile, shell Glycan and propolis also have good health-care effect other than with antimicrobial and anti-inflammation efficacy.
In addition, the antibacterial finishing agent of the present invention also has pull-out capacity strong, the long period its antibacterial energy for having can be kept Power, while having water-fastness persistence, product stability is good, the features such as to human body without any injury, the fabric hand after arrangement Sense is comfortable.And its preparation and application is simple, practical, and it is at low cost, without complicated operation equipment, it is convenient for industrialized production.
Specific implementation mode
Embodiment of the present invention is described in detail below in conjunction with embodiments and examples, but this field skill Art personnel will be understood that following embodiments and embodiment are merely to illustrate the present invention, and be not construed as the model of the limitation present invention It encloses.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts Every other embodiment, shall fall within the protection scope of the present invention.The person that is not specified actual conditions, builds according to normal condition or manufacturer The condition of view carries out.
In a first aspect, a kind of antibacterial finishing agent is provided at least one embodiment, including:
Propolis ethanol solution and chitosan solution.
Propolis is the resin that honeybee acquires from plant gemma or trunk, is mixed into the secretion of palatine gland, wax gland thereon A kind of colloidal solid object with aromatic odor being process;It is secreted by the repairing honeycomb such as Apidae animal apis cerana The stickum of yellowish-brown or dark brown can be used as medicine.Its is mild-natured, and bitter, pungent, micro-sweet have moisturizing myogenic, the work(of anti-inflammatory analgetic Effect, can treat gastric ulcer, canker sore, burn and scald, skin Tearing Pain, the illnesss such as radiation protection.Propolis energy activating cell promotes tissue Regeneration, repairs the islet cells and tissue of disease damage, and help reduces blood glucose;It diminishes inflammation, treatment infection, prevention and treatment infectivity Complication;It reduces blood fat, softening blood vessel, improve microcirculation, diabetic, which takes propolis, can prevent visual impairment and heart and brain Vascular complication;It regains one's strength, eliminates " three-many-one-little " symptom;Diabetes patient adhere to taking propolis can reinforced immunological function, increase Strong constitution, improves the quality of living.
Active ingredient in propolis can directly be absorbed by skin.
Further speaking, propolis is not only a kind of natural antiseptic with good antibacterial and anti-inflammation functions, while There is good medical care effect, such as:
Patient with hypertension continuously takes the propolis rich in Flavonoid substances and with very strong anti-oxidation ability, not only The harm that lipid peroxidation confrontation blood vessel can be reduced prevents vascular sclerosis, and can also be effectively reduced the content of triglyceride, Platelet aggregation is reduced, improves microcirculation, excessively high blood pressure can be reduced, prevent the generation of unexpected thing.Therefore, person in middle and old age People, especially hypertension, heart disease, arteriosclerotic, often take propolis, quite have benifit to good health and a long life.
The natural materials such as flavonoids, terpenes, polysaccharide, organic acid contained in propolis have apparent inhibition to make in cancer cell With, cancer patient is after taking propolis, and not only cancer cell significantly reduces, but also can be effectively prevented cancer metastasis, and Side effect caused by chemotherapy, radiotherapy can be mitigated, moreover it is possible to so that constitution is gradually improved, blood middle leukocytes increase rapid.It is numerous to grind Study carefully proof, propolis is a kind of natural immunopotentiator, and propolis can stimulate immunity function and gamma globulin activity, increase anti- Body production quantity can enhance macrophages phagocytic capacity, to improve human body resistance, inhibit growth of cancer cells.
Propolis can play the role of immune adjuvant, help to improve the energy of antibody, make total serum protein and the third bulb The content of albumen increases, and the phagocytic activity enhancing of leucocyte and macrophage can stimulate immunity function, preferably play a role, The specificity of human body and non-characteristic immunocompetence improve.Propolis has the function of antibacterial anti-inflammatory, moreover it is possible to rough skin be made to become It is flexible, whelk and color spot can be effectively treated, after clinical practice shows that gastritis, patients w ith peptic ulcer disease eat propolis, stomach pain Pain gradually disappears, and most of patients after adhering to edible propolis, turn out cloudy by ulcer healing, Helicobacter pylori infection.Most it is worth noting , edible propolis is not in diet decline, the negative effects such as flora imbalance.
Propolis is a kind of natural anti-oxidant auxiliary agent, contains more flavonoids and polyphenols, propolis in propolis Alcohol extracting thing and phenolic compound therein have stronger antioxidation, and ultra-oxygen anion free radical and hydroxyl can be quenched Free radical.In-vitro pharmacological experiments show that propolis not only has inhibiting effect to oxygen radical, but also to Fe2+The low density lipoprotein of induction Protein oxidation modification also has very strong inhibiting effect.
Propolis is a kind of rare natural, is the important substance that the mankind keep fit, slow down aging.Bee Glue has effects that delaying human body caducity, and every function of human body is made to bring into normal play, and is conducive to the improvement of sleep, and without appointing What side effect.
As known from the above, propolis has numerous excellent effects, however does not have been reported that but before the filing date of the present application Propolis is applied in the antibiotic finish of textile.To find out its cause, there are some problems in the application of this field for propolis.Mainly It is to be practically insoluble in water because the solubility of propolis in water only has 0.036/L, and be dissolved in ethyl alcohol (alcohol) or isopropyl Alcohol, but after the dilution of the alcoholic solution of propolis, the concentration of alcohol declines, and propolis is easy to be precipitated, and applies pole during padding Easily form spot.Alcoholic solution dissolving propolis is simply used, in the actual processing of factory, first, cost is too high, second is that peace Full hidden danger is bigger.Based on this, designer of the invention by long-term exploration and research and multiple experiment and effort, Continuous reform and innovation, it is proposed that propolis ethanol solution is added in chitosan solution, to prepare the antibiotic finish of the present invention Agent.By the way that chitosan solution is added in propolis ethanol solution, using the peptizaiton of chitosan colloid, point for making propolis stablize It is dispersed in colloid, prevents propolis from assembling to form spot, solve application problem of the propolis in textile industry.
It is understood that unlike the effect for using chitosan in the antibacterial finishing agent of the prior art, the present invention The peptizaiton of chitosan is mainly utilized, to solve the application problem of propolis.Meanwhile chitosan itself also there is antibacterial to make With, belong to natural green environment-friendly products and propolis ethanol solution be used in compounding, for propolis antibacterial effect have promote make With, while chitosan and propolis also have good health-care effect other than antimicrobial and anti-inflammation efficacy.
To sum up, antibacterial finishing agent of the invention mainly utilizes antibacterial, anti-inflammatory, anticancer, raising immunity of propolis etc. multiple Healthcare function, while there is water-fastness persistence;Since propolis is not soluble in water, so wash durability is good, it is solid to enhance it Put forth effort and Durability of antimicrobial effect, product stability obtained are good.Meanwhile chitosan has good colloidal dispersion, or it is a kind of Excellent antiseptic, chitosan are naturally occurring unique alkaline polysaccharides, are a kind of safe and non-toxic, biodegradable natural height Molecule not only has biocompatibility, and has the effects that antibacterial, hemostasis, inhibits cancer metastasis.In addition, chitosan is also With moisture-absorbing moisture-keeping function, there is cosmetic result.
Since propolis is not soluble in water, but it is dissolved in ethyl alcohol, with the active ingredient in ethyl alcohol bee glue extracting, while removing some not The unhelpful impurity of dissolubility;And the ethanol solution of propolis is added in chitosan dispersion colloid, it stirs, you can prepare Obtain uniform and stable propolis-chitosan dispersion.In addition, chitosan also has the heavy metal lead in chelating propolis, propolis is avoided In effect of the impurity to the harm of human body.
In a preferred embodiment, the antibacterial finishing agent includes following component:
The propolis ethanol solution of 8~30g/L and the chitosan solution of 1~7g/L;
Preferably, including following component:The propolis ethanol solution of 10~20g/L and the chitosan solution of 2~6g/L;
Preferably, including following component:The propolis ethanol solution of 10~15g/L and the chitosan solution of 2~5g/L.
In above-mentioned antibacterial finishing agent, the mass concentration of propolis ethanol solution is typical but non-limiting can be 8g/L, 10g/L, 12g/L, 15g/L, 16g/L, 18g/L, 20g/L, 22g/L, 24g/L, 25g/L, 26g/L or 30g/L;Chitosan solution Mass concentration it is typical but non-limiting can be 1g/L, 2g/L, 3g/L, 4g/L, 5g/L, 6g/L or 7g/L.
Using the propolis ethanol solution in above-mentioned concentration range, if being because of excessive concentration, final fabric is felt hard, It can increase cost simultaneously;If concentration is too low, antibiotic property, health properties and washing fastness of final fabric etc. cannot all reach reason The effect thought.
It is because the dispersibility of chitosan is mainly utilized in the present invention using the chitosan solution in above-mentioned concentration range Can, when the excessive excessive concentration of the dosage of chitosan, the feel for the fabric that can influence that treated, and the too small concentration of the dosage of chitosan When too low, then good dispersion performance is not had.Chitosan is in addition to good dispersion performance, chelating ability and anti-microbial property In addition, also performance of keeping humidity has cosmetic result.
In particular by propolis ethanol solution concentration within the scope of 10~15g/L and the concentration of chitosan solution 2~ Within the scope of 5g/L formed compound system, the antibacterial finishing agent prepared, can reach ideal antibacterial and health-care effect and Can be so that propolis ethyl alcohol be easy uniform dispersion, working solution has excellent storage stability, is not in floccule, after arrangement Fabric hand feel it is good, will not the appearance such as spottiness.
It should be noted that the present invention is not particularly limited the source of chitosan and molecular weight, such as chitosan Molecular weight can may further be enumerated as 1500~5000≤5000.In addition, the general solubility of chitosan in water It is relatively low, as long as selected chitosan can dissolve and form the chitosan solution in above-mentioned concentration range in water.
In a preferred embodiment, in the antibacterial finishing agent, the body of propolis ethanol solution and chitosan solution Product is than being (1~100) mL:(900~999) mL;
Preferably, the volume ratio of propolis ethanol solution and chitosan solution is (2~90) mL:(910~998) mL;
Preferably, the volume ratio of propolis ethanol solution and chitosan solution is (5~50) mL:(950~995) mL.
It should be noted that the propolis ethanol solution of aforementioned proportion range is to apply to weaving with chitosan solution Product impregnate or the concentration during padding.
When in use, the antibacterial finishing agent that can also be first formulated as follows in proportional region:
The volume ratio of propolis ethanol solution and chitosan solution is (15~35) mL:100mL;
Preferably, the volume ratio of propolis ethanol solution and chitosan solution is (22~32) mL:100mL;
It is further preferred that the volume ratio of propolis ethanol solution and chitosan solution is (20~30) mL:100mL;
Then the antibacterial finishing agent in the prepared proportional region is diluted 10~50 times again, then fabric is carried out It impregnates or pads, then dry.
In a preferred embodiment, in the propolis ethanol solution, weight and the volumetric concentration of propolis are 50% The ratio of the volume of~97% ethanol solution is 1g:(60~100) mL;
Preferably, the volumetric concentration of ethanol solution is 55%~65%;
Preferably, the volumetric concentration of ethanol solution is 60%.
Prepare propolis ethanol solution used by ethanol solution raw material preferably use volumetric concentration for 50%~97% second Alcoholic solution, it is typical but non-limiting, the volumetric concentration of ethanol solution can be 50%, 55%, 56%, 58%, 60%, 62%, 64%, 65%, 70%, 75%, 80%, 85%, 90%, 95% or 97%, most preferably use volumetric concentration for 60% ethanol solution.Because the solubility of propolis in ethanol is relatively high, using 60% ethanol solution, in propolis Beneficiating ingredient extracting flavonoids are most advantageous, if the concentration of ethyl alcohol is too low, the solubility of flavones is relatively low, and the excessive concentration of ethyl alcohol When, impurity such as some wax solubility in propolis are also correspondingly improved, although the solubility of flavones increases, impurity Solubility is also improving, and the purity of flavones is caused to decline.Further, wax content is high in the ethanol solution of propolis, by ethyl alcohol After solution dilution, the concentration of ethyl alcohol declines, and wax is precipitated, and floccule is formed in working solution, even if in the solution of chitosan, Can not uniformly it disperse, the fabric after arrangement will appear irregular blotches.
During preparing propolis ethanol solution, the weight of the propolis used and volumetric concentration for 60% ethanol solution body Long-pending ratio is preferably 1g:(60~100) mL;If ratio is less than 1:60, then the active ingredient dissolving in propolis is insufficient, if than Example is higher than 1:100, then the impurity in propolis start to dissolve into ethyl alcohol, lead to, when concentration of alcohol declines, there is the cotton-shaped of wax Object occurs.
Second aspect provides a kind of preparation method of antibacterial finishing agent at least one embodiment, and propolis ethyl alcohol is molten Liquid is added in chitosan solution, is sufficiently mixed uniformly to get the antibacterial finishing agent.
The preparation method of the antibacterial finishing agent is usually first to prepare certain density propolis ethanol solution and certain dense respectively Then the chitosan solution of degree measures the propolis ethanol solution of certain volume, adds it in prepared chitosan solution, It is mixed evenly.
Because propolis is not soluble in water, the organic solvents such as ethyl alcohol are dissolved in, therefore it is preferred that using ethyl alcohol as the molten of dissolving propolis Agent, and ethyl alcohol is nontoxic and volatile, will not cause the residual on fabric, and in a sense, ethyl alcohol is also environmentally protective Product.
Above-mentioned preparation manipulation is simple, practical, easy to implement, efficient, at low cost, without complicated operation equipment, industry Change large-scale production.
In a preferred embodiment, the preparation method of propolis ethanol solution includes:
10~20g of propolis is weighed, is shredded, is added in the ethanol solution that 1000mL volumetric concentrations are 50%~97%, room The lower extraction of temperature 70~75 hours, removal impurity is to get the propolis ethanol solution;Wherein, extraction time is typical but unrestricted It can be 70 hours, 71 hours, 72 hours, 73 hours, 74 hours or 75 hours;
Preferably, the preparation method of propolis ethanol solution includes:
10~15g of propolis is weighed, is shredded, is added in the ethanol solution that 1000mL volumetric concentrations are 55%~65%, room The lower extraction of temperature 72 hours, removal impurity is to get the propolis ethanol solution.
Above-mentioned propolis ethanol solution is in process for preparation, and since propolis dissolving is slow, propolis and ethyl alcohol after chopping can It comes into full contact with, by extraction in 72 hours or so, the benefit materials in propolis can adequately dissolve in ethanol, so that Beneficiating ingredient in propolis is fully utilized.
As previously described, because the solubility of propolis in ethanol is relatively high, it is molten using 60% ethyl alcohol in process for preparation Liquid, most advantageous for the beneficiating ingredient extracting flavonoids in propolis, if the concentration of ethyl alcohol is too low, the solubility of flavones is relatively low, and When the excessive concentration of ethyl alcohol, impurity such as some wax solubility in propolis are also correspondingly improved, although the solubility of flavones increases Add, but the solubility of impurity is also improving, and the purity of flavones is caused to decline.Further, wax in the ethanol solution of propolis Matter content is high, and after ethanol solution is diluted, the concentration of ethyl alcohol declines, and wax is precipitated, and floccule is formed in working solution, even if In the solution of chitosan, can not uniformly it disperse, the fabric after arrangement will appear irregular blotches.
The ratio of the volume for the ethanol solution that the weight and volumetric concentration of propolis are 60% is preferably 1g:(60~100) mL; If ratio is less than 1:60, then the active ingredient dissolving in propolis is insufficient, causes the waste of propolis, if ratio is higher than 1:100, then Impurity in propolis starts to dissolve into ethyl alcohol, causes to have when concentration of alcohol declines the floccule of wax to occur, working solution Stability declines.
The extraction time of propolis is preferably 72 hours, and after 72 hours, the content of propolis does not become significantly in ethyl alcohol Change, extends the time also without actual meaning;If being less than 72 hours, the time is too short, then the beneficiating ingredient in propolis cannot be abundant Dissolving, the utilization rate of propolis is insufficient, causes to waste.
It is propagated everywhere it is worth noting that, wind, rain are easiest to carrying pollutant, it should be noted that prevent wind, rain to propolis in case Pollution.The propolis taken out from beehive wants properly pack, keeping.Lead-containing materials should not be used on beehive.Produce bee glue product Enterprise and bee farm establish cooperative relationship, can also be conducive to reinforce preventing lead contamination.Lead is a kind of polyaffinity poisonous metal, Have accumulative in human body, is not easy to excrete.If lead excess is accumulated, can be to the immune system, nervous system, Digestive of human body It unites, function and heart, kidney etc. is caused to damage.
And cause in propolis raw material the reason of containing heavy metal it is main there are two:First, incorrect take gluing method, i.e., from bee Case wire gauze covers the propolis of scraping, and lead tolerance is higher.Another reason is the huge sum of money in the pollution of environment, such as air, soil Belonging to lead and other elements can be entered by the sorption enhanced of plant in propolis ingredient.The former is the main original for causing propolis lead content high Cause.Furthermore propolis raw material cannot be directly used, i.e., the hair glue bought from bee-keeper there.This hair glue is if it is with gauze screen Acquisition, unprocessed, often lead tolerance is exceeded.This hair glue is directly made the products such as propolis liquid by some retailers in alcohol It sells, is easy to generate harm to human body.Therefore, when selecting propolis raw material, above-mentioned phenomenon is avoided as possible.
It should be noted that the preparation for chitosan solution is not particularly limited.Such as a certain amount of shell can be weighed Glycan powder, is added to the water, and is mixed evenly to get chitosan solution.
The third aspect provides a kind of antibiotic finish of the antibacterial finishing agent in textile at least one embodiment In application.
The antibacterial finishing agent of the present invention has good anti-bacterial effect, and antibacterial durability high to fabric affinity good, safe Reliably, environmentally protective, have no toxic side effect, have the characteristics that health-care effect, applied during the final finishing of textile, it is right In reduction disease, health, the life style for meeting people's pursuit high quality is protected to have great importance.
In a preferred embodiment, above-mentioned antibacterial finishing agent is diluted 10~50 times, obtains antibiotic finish Fabric is immersed in antibiotic finish dispersion liquid by dispersion liquid;Alternatively, fabric is directly immersed in prepared antibacterial finishing agent In, it is impregnated or is padded, then dried.
It is understood that in above-mentioned antibacterial finishing agent, usually by the propolis ethanol solution and 100mL of (20~30) mL Chitosan solution be mixed to get;In practical applications, can by the antibiotic finish dilution agent 10~50 times obtain antibiotic finish Then dispersion liquid is impregnated or is padded to fabric, the shell of the propolis solution and certain volume of certain volume can also be directly taken Glycan solution is configured to the antibiotic finish dispersion liquid after dilution, and then fabric is impregnated or padded.
In a preferred embodiment, it pads for an immersing and rolling, pick-up is 75%~85%.Using an immersing and rolling Mode, easy to operate, excellent effect, save the energy;Pick-up it is typical but unrestricted can be 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84% or 85%, preferably 80%.
In a preferred embodiment, the temperature of drying is 120~160 DEG C.The mode of drying is not done excessively Limitation, by the way of commonly used in the art;It is typical but unrestricted, the temperature of drying can be 120 DEG C, 125 DEG C, 130 DEG C, 135 DEG C, 140 DEG C, 145 DEG C, 150 DEG C, 155 DEG C or 160 DEG C.
With reference to specific embodiment, comparative example, the invention will be further described.
Embodiment 1
A kind of antibacterial finishing agent, including following component:
The propolis ethanol solution of 15g/L and the chitosan solution of 5g/L.
Wherein, the preparation method of propolis ethanol solution includes:
Propolis 15g is weighed, is shredded, is added in the ethanol solution that 1000mL volumetric concentrations are 60%, extracts 72 at room temperature Hour, removal impurity is to get propolis ethanol solution.
The application process of the antibacterial finishing agent includes:
The propolis ethanol solution 5mL for measuring prepared 15g/L, is added in the chitosan solution of the 5g/L of 995mL, fills Divide and stir evenly, obtains antibiotic finish dispersion liquid, which is equivalent to the propolis 60% of 0.5% (volume fraction) Ethanol solution.The satin fabrics of pure cotton 40s/144 × 96 are padded, by the way of an immersing and rolling, pick-up 80%, at 120 DEG C Lower drying.It pads rear remaining working solution to retain, places the stability of observation working solution.
Embodiment 2
Difference lies in the present embodiment with embodiment 1:
The application process of antibacterial finishing agent includes:
The propolis ethanol solution 1mL for measuring prepared 15g/L, is added in the chitosan solution of the 5g/L of 999mL, fills Divide and stir evenly, obtains antibiotic finish dispersion liquid, which is equivalent to the propolis 60% of 0.1% (volume fraction) Ethanol solution.The satin fabrics of pure cotton 40s/144 × 96 are padded, by the way of an immersing and rolling, pick-up 80%, at 120 DEG C Lower drying.It pads rear remaining working solution to retain, places the stability of observation working solution.
Embodiment 3
A kind of antibacterial finishing agent, including following component:
The propolis ethanol solution of 10g/L and the chitosan solution of 2g/L.
Wherein, the preparation method of propolis ethanol solution includes:
Propolis 10g is weighed, is shredded, is added in the ethanol solution that 1000mL volumetric concentrations are 60%, extracts 72 at room temperature Hour, removal impurity is to get propolis ethanol solution.
The application process of the antibacterial finishing agent includes:
The propolis ethanol solution 50mL for measuring prepared 10g/L, is added in the chitosan solution of the 2g/L of 950mL, It stirs, obtains antibiotic finish dispersion liquid, which is equivalent to the propolis 60% of 5% (volume fraction) Ethanol solution.The satin fabrics of pure cotton 40s/144 × 96 are padded, by the way of an immersing and rolling, pick-up 80%, at 160 DEG C Lower drying.It pads rear remaining working solution to retain, places the stability of observation working solution.
Embodiment 4
Difference lies in the present embodiment with embodiment 3:
The application process of antibacterial finishing agent includes:
The propolis ethanol solution 10mL for measuring prepared 10g/L, is added in the chitosan solution of the 2g/L of 990mL, It stirs, obtains antibiotic finish dispersion liquid, which is equivalent to the propolis 60% of 1% (volume fraction) Ethanol solution.The satin fabrics of pure cotton 40s/144 × 96 are padded, by the way of an immersing and rolling, pick-up 80%, at 160 DEG C Lower drying.It pads rear remaining working solution to retain, places the stability of observation working solution.
Embodiment 5
A kind of antibacterial finishing agent, including following component:
The propolis ethanol solution of 12g/L and the chitosan solution of 3g/L.
Wherein, the preparation method of propolis ethanol solution includes:
Propolis 12g is weighed, is shredded, is added in the ethanol solution that 1000mL volumetric concentrations are 55%, extracts 73 at room temperature Hour, removal impurity is to get propolis ethanol solution.
The application process of the antibacterial finishing agent includes:
The propolis ethanol solution 20mL for measuring prepared 12g/L, is added in the chitosan solution of the 3g/L of 980mL, It stirs, obtains antibiotic finish dispersion liquid, which is equivalent to the propolis 55% of 2% (volume fraction) Ethanol solution.The satin fabrics of pure cotton 40s/144 × 96 are padded, by the way of an immersing and rolling, pick-up 85%, at 150 DEG C Lower drying.It pads rear remaining working solution to retain, places the stability of observation working solution.
Embodiment 6-7
A kind of antibacterial finishing agent, with embodiment difference lies in:
The volumetric concentration for the ethanol solution that propolis ethanol solution uses in preparation process is respectively 65% and 80%;
Remaining is same as Example 1.
Embodiment 8-9
A kind of antibacterial finishing agent, with embodiment difference lies in:
The time that propolis ethanol solution extracts in preparation process is respectively 70 hours and 75 hours;
Remaining is same as Example 1.
Embodiment 10
A kind of antibacterial finishing agent, including following component:
The propolis ethanol solution of 11g/L and the chitosan solution of 4g/L.
Wherein, the preparation method of propolis ethanol solution includes:
Propolis 11g is weighed, is shredded, is added in the ethanol solution that 1000mL volumetric concentrations are 60%, extracts 72 at room temperature Hour, removal impurity is to get propolis ethanol solution.
The application process of the antibacterial finishing agent includes:
The propolis ethanol solution 80mL for measuring prepared 11g/L, is added in the chitosan solution of the 4g/L of 920mL, It stirs, obtains antibiotic finish dispersion liquid, which is equivalent to the propolis 60% of 8% (volume fraction) Ethanol solution.The satin fabrics of pure cotton 40s/144 × 96 are padded, by the way of an immersing and rolling, pick-up 78%, at 140 DEG C Lower drying.It pads rear remaining working solution to retain, places the stability of observation working solution.
Comparative example 1
A kind of antibacterial finishing agent includes the chitosan solution of 5g/L.
The application process of the antibacterial finishing agent includes:
The chitosan solution for taking the 5g/L of 1000mL pads the satin fabrics of pure cotton 40s/144 × 96, using an immersing and rolling Mode, pick-up 80% are dried at 120 DEG C.It pads rear remaining working solution to retain, places the stabilization of observation working solution Property.
Difference lies in only add chitosan solution, be added without propolis this comparative example with embodiment 1 in antibacterial finishing agent Ethanol solution.
Comparative example 2
A kind of antibacterial finishing agent includes the propolis ethanol solution of 15g/L.
The application process of the antibacterial finishing agent includes:
Propolis ethyl alcohol (60% ethanol solution) the solution 5mL for taking 15g/L, is added in the water of 995mL, pads pure cotton The satin fabrics of 40s/144 × 96, by the way of an immersing and rolling, pick-up 80% is dried at 120 DEG C.Residue after padding Working solution retain, place observation working solution stability.
Difference lies in only add propolis ethanol solution, be added without shell this comparative example with embodiment 1 in antibacterial finishing agent Glycan solution.
Comparative example 3
A kind of antibacterial finishing agent, including following component:
The chitosan solution of propolis 60% ethanol solution and 3g/L of 32g/L.
Difference lies in the concentration of propolis ethanol solution is not in the present invention in antibacterial finishing agent with embodiment 1 for this comparative example In the range of restriction.
Comparative example 4
A kind of antibacterial finishing agent, including following component:
The chitosan solution of propolis 60% ethanol solution and 5g/L of 5g/L.
Difference lies in the concentration of propolis ethanol solution is not in the present invention in antibacterial finishing agent with embodiment 1 for this comparative example In the range of restriction.
Comparative example 5
A kind of antibacterial finishing agent, including following component:
The propolis ethanol solution of 10g/L and the chitosan solution of 0.5g/L.
Difference lies in the concentration of chitosan solution does not limit this comparative example in the present invention in antibacterial finishing agent with embodiment 1 In fixed range.
The main operating parameters of each embodiment and comparative example, as shown in table 1.
The main operating parameters of 1 each embodiment and comparative example of table
Performance test
The fabric obtained after being arranged respectively to each embodiment and comparative example carries out anti-microbial property test, with reference to GB/ T20944.3-2008《The evaluation of antibacterial textile performance》Carry out anti-microbial property test.
Test method is specifically as follows:Respectively from embodiment 1-10 arrange after fabric on a diameter of 25mm of clip ± The round test sample 1 of 5mm, test sample 2, test sample 3, test sample 4, test sample 5, test sample 6, test sample 7, test sample 8, experiment Sample 9 and test sample 10, it is spare, while from an equal amount of control of clip on the fabric after arranging prepared by comparative example 1-5 Sample 1, control sample 2, control sample 3, control sample 4 and control sample 5;In addition, from an equal amount of sky of clip on common 100% pure cotton cloth White sample;
10mL agar mediums are poured into sterilized petri dishes, wait for its condensation, agar plate is made;Take 45 DEG C ± 2 DEG C of fine jade 1mL test bacteria liquids (cell concentration 3000cfu/mL) mixing is added in fat culture medium 150mL, then takes 5mL to be added to agar flat In plate, its condensation is waited for, it is spare;Test sample, control sample, blank sample are put in the plate center made respectively with aseptic nipper, Even pressing makes to be in close contact between test sample and agar medium on agar medium;It is put into 37 DEG C ± 2 DEG C immediately after Incubator in cultivate 18-24h, ensure that test sample and agar medium keep good contact in incubation;Culture finishes, The antibacterial bandwidth of sample according to the following formula:
H=(D-d)/2
In formula:H indicates antibacterial bandwidth, unit mm;D indicates the outer diameter of antibacterial band, unit mm;D indicates the straight of test sample Diameter, unit mm.
After measuring antibacterial band, test sample is removed from agar medium with tweezers, below microexamination test sample The food supplements of contact area, calculate bacteriostasis rate, and test result is shown in Table 2.
2 anti-microbial property test result of table
As can be seen from the above results, the fabric after antibacterial finishing agent using the present invention arranges has preferable antibacterial Performance, and after washing 5 times, higher level is still maintained to the bacteriostasis rate of common bacterium, bacteriostasis rate still can reach 95% or more (do not wash with wash 5 times then probably differ 2%), and the fabric after individually chitosan antibacterial finishing agent arranges, are washing After washing, antibacterial effect substantially reduces, and only 60% or so.Individual propolis ethanol solution, it is very unstable, in actual scale It is difficult to realize in production.In addition, in the range of propolis ethanol solution provided by the invention and chitosan solution, can reach more Good antibacterial effect, can make the feel of fabric obviously be hardened more than the solution within the scope of this, cause the waste of propolis, and increase Cost, or so that the stability of working solution is declined.
In addition, the stability of the working solution after being arranged respectively to each embodiment and comparative example is tested, 3 are the results are shown in Table.
3 working solution stability test result of table
The antibacterial finishing agent dispersing uniformity of the present invention is good it can be seen from above, and stability is good, convenient for storage.Meanwhile Fabric after being arranged to various embodiments of the present invention and comparative example touches, it is found that the feel of the fabric of each embodiment is also apparent excellent In the feel of the fabric of each comparative example.
Finally it should be noted that:The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that:Its according to So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into Row equivalent replacement;And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution The range of scheme.

Claims (10)

1. a kind of antibacterial finishing agent, which is characterized in that including:
Propolis ethanol solution and chitosan solution.
2. antibacterial finishing agent according to claim 1, which is characterized in that including following component:
The propolis ethanol solution of 8~30g/L and the chitosan solution of 1~7g/L;
Preferably, including following component:The propolis ethanol solution of 10~20g/L and the chitosan solution of 2~6g/L;
Preferably, including following component:The propolis ethanol solution of 10~15g/L and the chitosan solution of 2~5g/L.
3. antibacterial finishing agent according to claim 1, which is characterized in that in the antibacterial finishing agent, propolis ethanol solution Volume ratio with chitosan solution is (1~100):(900~999);
Preferably, the volume ratio of propolis ethanol solution and chitosan solution is (2~90):(910~998);
Preferably, the volume ratio of propolis ethanol solution and chitosan solution is (5~50):(950~995).
4. according to claims 1 to 3 any one of them antibacterial finishing agent, which is characterized in that in the propolis ethanol solution, bee The ratio of the volume for the ethanol solution that the weight and volumetric concentration of glue are 50%~97% is 1g:(60~100) mL;
Preferably, the volumetric concentration of ethanol solution is 55%~65%;
Preferably, the volumetric concentration of ethanol solution is 60%.
5. such as the preparation method of Claims 1 to 4 any one of them antibacterial finishing agent, which is characterized in that propolis ethyl alcohol is molten Liquid is added in chitosan solution, is sufficiently mixed uniformly to get the antibacterial finishing agent.
6. the preparation method of antibacterial finishing agent according to claim 5, which is characterized in that the preparation side of propolis ethanol solution Method includes:
10~20g of propolis is weighed, is shredded, is added in the ethanol solution that 1000mL volumetric concentrations are 50%~97%, at room temperature Extraction 70~75 hours, removal impurity is to get the propolis ethanol solution;
Preferably, the preparation method of propolis ethanol solution includes:
10~15g of propolis is weighed, is shredded, is added in the ethanol solution that 1000mL volumetric concentrations are 55%~65%, at room temperature Extraction 72 hours, removal impurity is to get the propolis ethanol solution.
7. such as application of Claims 1 to 4 any one of them antibacterial finishing agent in the antibiotic finish of textile.
8. application according to claim 7, which is characterized in that fabric is immersed in Claims 1 to 4 any one of them In antibacterial finishing agent, or by fabric be immersed in dilution after Claims 1 to 4 any one of them antibacterial finishing agent in, into Row dipping pads, and then dries.
9. application according to claim 8, which is characterized in that pad for an immersing and rolling, pick-up is 75%~85%.
10. application according to claim 8, which is characterized in that the temperature of drying is 120~160 DEG C.
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