CN108677530B - Antibacterial finishing agent and preparation method and application thereof - Google Patents
Antibacterial finishing agent and preparation method and application thereof Download PDFInfo
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- CN108677530B CN108677530B CN201810464920.7A CN201810464920A CN108677530B CN 108677530 B CN108677530 B CN 108677530B CN 201810464920 A CN201810464920 A CN 201810464920A CN 108677530 B CN108677530 B CN 108677530B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating 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
- D06M15/03—Polysaccharides or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating 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
- D06M15/17—Natural resins, resinous alcohols, resinous acids, or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Abstract
The invention belongs to the technical field of treatment fluid for textile after-treatment, and relates to an antibacterial finishing agent, and a preparation method and application thereof. The antibacterial finishing agent comprises: propolis ethanol solution and chitosan solution. The preparation method of the antibacterial finishing agent comprises the following steps: and adding the propolis ethanol solution into the chitosan solution, and fully and uniformly mixing to obtain the antibacterial finishing agent. The invention takes the propolis ethanol solution and the chitosan solution as raw materials, has good antibacterial effect, high affinity to fabrics and good antibacterial durability, is safe and reliable, is green and environment-friendly, has no toxic or side effect, and has health care effect. And the preparation method is simple, practical, easy to implement, low in cost, good in environmental protection benefit and easy to popularize and apply.
Description
Technical Field
The invention relates to the technical field of treatment liquid for textile after-treatment, and particularly relates to an antibacterial finishing agent and a preparation method and application thereof.
Background
For a long time, human health is threatened by environmental pollution and bacterial infection; the research on the antibacterial agent in various countries in the world is more important, and the research on the antibacterial fabric finishing liquid (finishing agent) becomes a hot spot in the textile and printing and dyeing industries.
At present, various antibacterial finishing materials are applied in the market, such as silver antibacterial materials, natural antibacterial materials, chemical antibacterial materials and the like. The silver-based antibacterial material mainly adopts nano silver, and the nano silver is used as a novel high-efficiency inorganic antibacterial material, is widely applied to the fields of medicine, biology, environmental protection and the like, and shows good antibacterial and bactericidal effects. More and more medical products or materials containing nano-silver appear in clinical medical treatment of burn surgery, gynecology, dermatology, stomatology and the like, and good medical effect is achieved. The nano silver is one of the first-choice antibacterial agents at present due to the characteristics of high efficiency, broad spectrum, strong antibacterial action, difficult generation of bacterial drug resistance and the like. However, there are many reports about the toxicity of nano-silver, and people increasingly contact with nano-silver along with the commercialization and industrial production of nano-silver for various purposes, and nano-silver also enters human body through respiratory inhalation, drug uptake, skin contact and other approaches. Trop et al reported cases of elevated liver enzymes and silver poisoning reactions caused by nano-silver dressings. Research shows that the silver nanoparticles of 15 nm and 100nm generate toxicity to rat liver cells. Therefore, the safety and the possible toxic effect of the nano silver are not ignored while the nano silver is selected as the antibacterial material.
In the chemical antibacterial material, triclosan is a commonly used antibacterial agent in textiles, but triclosan can generate dioxin compounds under certain conditions. While in carcinogenesis, it was reported earlier that chronic exposure to triclosan induced liver cirrhosis in mice, recently, the PNAS article in 2014 reported again the role of triclosan as a liver tumor promoter, and the Science journal in 2016 also proposed the hepatotoxic effect of triclosan. Therefore, the liver toxicity effect of the triclosan closely related to the life of people is not negligible while the triclosan is used as an antibacterial material.
The natural antibacterial materials in the natural antibacterial agent are mainly extracted from natural plants, such as chitin, mustard, castor oil, horseradish and the like, are simple and convenient to use, but have limited antibacterial action, poorer heat resistance, low sterilization rate, no broad-spectrum long-acting use and few quantity; health care and medical performance are also limited. In addition, chitosan is also a common antibacterial material in the textile industry, is used as a green and environment-friendly new material, has rich resources, no toxicity, no pollution and many natural excellent properties; however, chitosan has an antibacterial effect inferior to silver or organic antibacterial agents and has poor durability to fabrics.
At present, the textile industry in China has great development in yield and technology, so that the textile industry has a solid foundation for pursuing the additional value of products. On the other hand, with the improvement of living standard of people, people not only pay more and more attention to the aesthetic appearance of the textile, but also pursue the comfort and the safety of the textile, and even put forward the requirements on the health care performance of the textile. However, as can be seen from the above, the existing antibacterial materials all have certain advantages, and also have some disadvantages, especially unreliable safety, which may not only cause some toxic and side effects, but also have no health-care effect. Therefore, a novel antibacterial finishing agent which has good antibacterial effect, is green and environment-friendly, safe and reliable, has no toxic or side effect and has a health-care effect is researched and developed, and the novel antibacterial finishing agent has important effects on improving the added value of the fabric and promoting the further development of the textile industry.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide an antibacterial finishing agent, which takes a propolis ethanol solution and a chitosan solution as raw materials, has good antibacterial effect, high affinity to fabrics, good antibacterial durability, safety, reliability, environmental protection, no toxic or side effect, health-care effect and contribution to sleep improvement.
The second purpose of the invention is to provide a preparation method of the antibacterial finishing agent, which has the advantages of simple operation, easy implementation, low cost, good environmental protection benefit and easy popularization and application.
The third purpose of the invention is to provide an application of the antibacterial finishing agent in textiles, and the antibacterial finishing agent has the characteristics of good antibacterial effect, high affinity to fabrics, good antibacterial durability, safety, reliability, environmental protection, no toxic or side effect, health care effect and the like, so that the antibacterial finishing agent can be applied in the after-finishing process of textiles.
In order to achieve the purpose, the invention adopts the technical scheme that:
according to one aspect of the invention, there is provided an antimicrobial finish comprising:
propolis ethanol solution and chitosan solution.
As a further preferable technical scheme, the method comprises the following components:
8-30 g/L of propolis ethanol solution and 1-7 g/L of chitosan solution;
preferably, the following components are included: 10-20 g/L of propolis ethanol solution and 2-6 g/L of chitosan solution;
preferably, the following components are included: 10-15g/L of propolis ethanol solution and 2-5g/L of chitosan solution.
According to a further preferable technical scheme, in the antibacterial finishing agent, the volume ratio of the propolis ethanol solution to the chitosan solution is (1-100): (900-999);
preferably, the volume ratio of the propolis ethanol solution to the chitosan solution is (2-90): (910 to 998);
preferably, the volume ratio of the propolis ethanol solution to the chitosan solution is (5-50): (950 to 995).
As a further preferable technical scheme, in the propolis ethanol solution, the ratio of the weight of propolis to the volume of the ethanol solution with the volume concentration of 50-97% is 1 g: (60-100) mL;
preferably, the volume concentration of the ethanol solution is 55-65%;
preferably, the ethanol solution has a concentration of 60% by volume.
According to another aspect of the invention, the invention provides a preparation method of the antibacterial finishing agent, which comprises the steps of adding the propolis ethanol solution into the chitosan solution, and fully and uniformly mixing to obtain the antibacterial finishing agent.
As a further preferable technical scheme, the preparation method of the propolis ethanol solution comprises the following steps:
weighing 10-20 g of propolis, cutting, adding into 1000mL of 50-97% ethanol solution, extracting at room temperature for 70-75 hours, and removing impurities to obtain the propolis ethanol solution;
preferably, the preparation method of the propolis ethanol solution comprises the following steps:
weighing 10-15g of propolis, chopping, adding into 1000mL of 55-65% ethanol solution, extracting at room temperature for 72 hours, and removing impurities to obtain the propolis ethanol solution.
According to another aspect of the invention, there is provided the use of an antimicrobial finish as described above in the antimicrobial finishing of textiles.
As a further preferable technical scheme, the fabric is immersed in the antibacterial finishing agent, or immersed in the diluted antibacterial finishing agent, impregnated or padded, and then dried.
As a further preferable technical scheme, the padding is one-dipping-one-rolling, and the rolling residual rate is 75-85%.
As a further preferred technical scheme, the drying temperature is 120-160 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the antibacterial finishing agent mainly takes the propolis ethanol solution and the chitosan solution as raw materials, wherein the propolis is a natural antibacterial agent with good antibacterial and anti-inflammatory effects, has good medical and health-care effects such as cancer resistance, immunity improvement and the like, is green and environment-friendly, has excellent performance, is safe and reliable, and can relieve the problems of common antibacterial effect, poor water washing resistance, poor safety and possible toxic and side effects of the existing antibacterial agent.
The propolis ethanol solution and the chitosan solution are compounded for use, and the dispersion effect of chitosan colloid is mainly utilized to ensure that the propolis is stably dispersed in the colloid and prevent the propolis from aggregating to form spots; in addition, the chitosan has an antibacterial effect, belongs to a natural green environment-friendly product, can be used together with a propolis antibacterial agent to further improve the antibacterial effect of the antibacterial agent, and simultaneously has a good health-care effect besides the antibacterial and anti-inflammatory effects of the chitosan and the propolis.
In addition, the antibacterial finishing agent disclosed by the invention has strong adhesion, can keep the antibacterial capability for a long time, has the characteristics of durability of water washing resistance, good product stability, no harm to human bodies and the like, and the finished fabric has comfortable hand feeling. And the preparation and use methods are simple and practical, the cost is low, complex operation equipment is not needed, and the industrial production is facilitated.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to embodiments and examples, but those skilled in the art will understand that the following embodiments and examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Those who do not specify the conditions are performed according to the conventional conditions or the conditions recommended by the manufacturer.
In a first aspect, there is provided in at least one embodiment an antimicrobial finish comprising:
propolis ethanol solution and chitosan solution.
Propolis is a colloidal solid with aromatic odor obtained by collecting resin from plant spore or trunk, and mixing with secretion of palate gland and ceriferous gland; is a yellow brown or black brown viscous substance secreted by repairing nidus Vespae of Apidae such as Apis cerana Fabricius. It has mild property, bitter, pungent and slightly sweet taste, has effects of moistening skin, promoting granulation, diminishing inflammation and relieving pain, and can be used for treating gastric ulcer, oral ulcer, burn and scald, skin pain, and radiation protection etc. Propolis can activate cells, promote tissue regeneration, repair damaged islet cells and tissues, and help to reduce blood sugar; eliminating inflammation, treating infection, and preventing and treating infectious complications; reducing blood lipid, softening blood vessel, and improving microcirculation, and can be used for preventing visual deterioration and cardiovascular and cerebrovascular complications for diabetic patients; recovering physical strength, and eliminating the symptoms of more than three and one less; the diabetes patients insist on taking the propolis can strengthen the immune function, strengthen the physique and improve the life quality.
The effective components in propolis can be directly absorbed through skin.
Furthermore, propolis is not only a natural antibacterial agent with good antibacterial and anti-inflammatory effects, but also has good health care effects, such as:
the propolis rich in flavonoids and having strong antioxidant capacity is continuously taken by patients suffering from hypertension, so that the harm of lipid peroxide to blood vessels can be reduced, angiosclerosis can be prevented, the content of triglyceride can be effectively reduced, platelet aggregation can be reduced, microcirculation can be improved, the hypertension can be reduced, and accidents can be prevented. Therefore, the middle-aged and the elderly people, especially patients with hypertension, heart disease and arteriosclerosis, often take propolis, which is beneficial to health and longevity.
The propolis contains natural substances such as flavonoids, terpenes, polysaccharides and organic acids, which have obvious inhibiting effect on cancer cells, and can be used for cancer patients to take the propolis, so that the cancer cells are obviously reduced, the cancer cell metastasis can be effectively prevented, the side effects caused by chemotherapy and radiotherapy can be alleviated, the physique can be gradually improved, and the white blood cells in blood can be rapidly increased. A plurality of researches prove that the propolis is a natural immunopotentiator, can stimulate the immune function and the gamma globulin activity, increase the antibody production amount and enhance the phagocytic capacity of macrophages, thereby improving the body resistance and inhibiting the growth of cancer cells.
Propolis has immunity adjuvant effect, and is helpful for increasing antibody energy, increasing serum total protein and gamma globulin content, enhancing phagocytic ability of leukocyte and macrophage, stimulating immunity, and improving specific and nonspecific immunity of organism. The propolis has the effects of resisting bacteria and diminishing inflammation, can enable rough skin to become elastic, and can effectively treat whelk and color spots. Most notably, eating propolis does not have the negative effects of diet reduction, flora imbalance and the like.
Propolis is a natural antioxidant auxiliary agent, contains more flavonoids and polyphenols, and has strong antioxidation effect on ethanol extract and phenolic compounds therein, and can quench superoxide anion free radicals and hydroxyl free radicals. In vitro pharmacological test shows that propolis not only has inhibition effect on oxygen free radical, but also has effect on Fe2+The induced oxidation modification of low density lipoprotein has strong inhibiting effect.
Propolis is an rare natural antioxidant and is an important substance for keeping human health and delaying aging. The propolis has the effect of delaying aging of human body, enables various functions of the human body to be normally exerted, is beneficial to improving sleep, and has no side effect.
From the above, propolis has many excellent effects, however, it has not been reported to apply propolis to antibacterial finishing of textiles until the filing date of the present application. For this reason, propolis has some problems in the application in the field. The main reason is that the solubility of propolis in water is only 0.036/L, which is almost insoluble in water, but is dissolved in ethanol (alcohol) or isopropanol, but after the propolis alcohol solution is diluted, the concentration of alcohol is reduced, the propolis is easy to precipitate, and spots are easy to form when the propolis is applied in the padding process. The propolis is dissolved by adopting the alcohol solution, so that the cost is too high and the potential safety hazard is large in the actual processing of a factory. Based on this, the designers of the invention continuously innovate and innovate through long-term exploration and research, and a plurality of tests and efforts, and propose to add the propolis ethanol solution into the chitosan solution to prepare the antibacterial finishing agent of the invention. By adding the chitosan solution into the propolis ethanol solution and utilizing the dispersion effect of the chitosan colloid, the propolis is stably dispersed in the colloid, so that the propolis is prevented from aggregating to form spots, and the application problem of the propolis in the textile industry is solved.
It can be understood that the invention mainly utilizes the dispersion effect of the chitosan to solve the application problem of the propolis, which is different from the effect of adopting the chitosan in the antibacterial finishing agent in the prior art. Meanwhile, the chitosan has an antibacterial effect, belongs to a natural green environment-friendly product, is used in combination with the propolis ethanol solution, has a promoting effect on the antibacterial effect of the propolis, and has a good health-care effect besides the antibacterial and anti-inflammatory effects of the chitosan and the propolis.
In conclusion, the antibacterial finishing agent mainly utilizes multiple health care functions of the propolis, such as antibiosis, antiphlogosis, anticancer, immunity improvement and the like, and has durability of water washing resistance; because propolis is insoluble in water, the water washing resistance is good, the fixing force and the antibacterial durability are enhanced, and the prepared product has good stability. Meanwhile, chitosan has good colloid dispersibility and is an excellent antibacterial agent, the chitosan is the only naturally-occurring alkaline polysaccharide, is a safe, nontoxic and biodegradable natural polymer, has biocompatibility and has the effects of resisting bacteria, stopping bleeding, inhibiting cancer cell metastasis and the like. In addition, chitosan also has moisture absorption and retention functions, and has a beautifying effect.
Because propolis is insoluble in water but soluble in ethanol, the effective components in propolis are extracted by ethanol, and simultaneously, some insoluble useless impurities are removed; adding the ethanol solution of the propolis into the chitosan dispersoid, and fully and uniformly stirring to prepare the uniform and stable propolis chitosan dispersoid. In addition, the chitosan also has the function of chelating heavy metal lead in the propolis and avoiding the harm of impurities in the propolis to human bodies.
In a preferred embodiment, the antimicrobial finish comprises the following components:
8-30 g/L of propolis ethanol solution and 1-7 g/L of chitosan solution;
preferably, the following components are included: 10-20 g/L of propolis ethanol solution and 2-6 g/L of chitosan solution;
preferably, the following components are included: 10-15g/L of propolis ethanol solution and 2-5g/L of chitosan solution.
In the antibacterial finishing agent, the mass concentration of the propolis ethanol solution is typically, but not limited to, 8g/L, 10g/L, 12g/L, 15g/L, 16g/L, 18g/L, 20g/L, 22g/L, 24g/L, 25g/L, 26g/L or 30 g/L; the chitosan solution may have a mass concentration of typically, but not exclusively, 1g/L, 2g/L, 3g/L, 4g/L, 5g/L, 6g/L or 7 g/L.
The propolis ethanol solution with the concentration in the range is adopted because if the concentration is too high, the hand feeling of the final fabric becomes hard, and the cost is increased; if the concentration is too low, the antibacterial property, the health-care performance, the washing resistance and the like of the final fabric can not achieve ideal effects.
The chitosan solution with the concentration in the range is adopted because the invention mainly utilizes the dispersion performance of chitosan, when the dosage of the chitosan is too large and the concentration is too high, the hand feeling of the treated fabric is influenced, and when the dosage of the chitosan is too small and the concentration is too low, the chitosan solution cannot have good dispersion performance. The chitosan has good dispersing performance, chelating performance and antibacterial performance, also has moisturizing performance and has a beautifying effect.
Particularly, the antibacterial finishing agent prepared by adopting a compound system formed by the concentration of the propolis ethanol solution within the range of 10-15g/L and the concentration of the chitosan solution within the range of 2-5g/L can achieve ideal antibacterial and health-care effects, can ensure that the propolis ethanol is easily and uniformly dispersed, has excellent storage stability of working solution, does not generate floccules, and has good hand feeling of finished fabrics and no spots and the like.
In the present invention, the source and molecular weight of chitosan are not particularly limited, and for example, the molecular weight of chitosan may be 5000 or less, and more specifically, 1500 to 5000. In addition, chitosan generally has low solubility in water, and the chitosan selected only needs to be capable of dissolving in water to form a chitosan solution with the concentration within the range.
In a preferred embodiment, in the antibacterial finishing agent, the volume ratio of the propolis ethanol solution to the chitosan solution is (1-100) mL: (900-999) mL;
preferably, the volume ratio of the propolis ethanol solution to the chitosan solution is (2-90) mL: (910-998) mL;
preferably, the volume ratio of the propolis ethanol solution to the chitosan solution is (5-50) mL: (950-995) mL.
It should be noted that the above ratio ranges of the propolis ethanol solution and the chitosan solution are concentrations in practical application to textile dipping or padding.
When in use, the antibacterial finishing agent can be prepared in the following proportion range:
the volume ratio of the propolis ethanol solution to the chitosan solution is (15-35) mL: 100 mL;
preferably, the volume ratio of the propolis ethanol solution to the chitosan solution is (22-32) mL: 100 mL;
further preferably, the volume ratio of the propolis ethanol solution to the chitosan solution is (20-30) mL: 100 mL;
and then diluting the prepared antibacterial finishing agent within the proportion range by 10-50 times, dipping or padding the fabric, and drying.
In a preferred embodiment, in the propolis ethanol solution, the ratio of the weight of propolis to the volume of the ethanol solution with the volume concentration of 50-97% is 1 g: (60-100) mL;
preferably, the volume concentration of the ethanol solution is 55-65%;
preferably, the ethanol solution has a concentration of 60% by volume.
The ethanol solution used for preparing the propolis ethanol solution is preferably 50-97% ethanol solution, typically but not limited to, 50%, 55%, 56%, 58%, 60%, 62%, 64%, 65%, 70%, 75%, 80%, 85%, 90%, 95% or 97%, and most preferably 60% ethanol solution. Because the solubility of propolis in ethanol is relatively high, a 60% ethanol solution is most beneficial to extracting flavone which is a beneficial component in propolis, if the concentration of ethanol is too low, the solubility of flavone is low, and if the concentration of ethanol is too high, the solubility of impurities in propolis, such as wax, is correspondingly improved, and although the solubility of flavone is increased, the solubility of impurities is also improved, so that the purity of flavone is reduced. Furthermore, the content of wax in the ethanol solution of the propolis is high, after the ethanol solution is diluted, the concentration of the ethanol is reduced, the wax is separated out, floccules are formed in the working solution, even if the wax is in the solution of the chitosan, the wax cannot be uniformly dispersed, and irregular spots can appear on the finished fabric.
In the process of preparing the propolis ethanol solution, the proportion of the weight of the adopted propolis to the volume of the ethanol solution with the volume concentration of 60% is preferably 1 g: (60-100) mL; if the ratio is less than 1: 60, the effective components in the propolis are not sufficiently dissolved, and if the proportion is higher than 1: 100, the impurities in the propolis start to dissolve into ethanol, resulting in waxy flocs appearing when the ethanol concentration is reduced.
In a second aspect, in at least one embodiment, there is provided a method for preparing an antibacterial finishing agent, which comprises adding a propolis ethanol solution into a chitosan solution, and mixing the mixture thoroughly to obtain the antibacterial finishing agent.
The preparation method of the antibacterial finishing agent generally comprises the steps of preparing a propolis ethanol solution with a certain concentration and a chitosan solution with a certain concentration respectively, then measuring a certain volume of the propolis ethanol solution, adding the propolis ethanol solution into the prepared chitosan solution, and mixing and stirring uniformly.
Because propolis is insoluble in water and soluble in organic solvents such as ethanol, ethanol is preferably used as the solvent for dissolving propolis, and ethanol is nontoxic and volatile, so that residues on fabrics cannot be caused, and ethanol is a green and environment-friendly product in a certain sense.
The preparation method is simple in operation, practical, easy to implement, high in efficiency, low in cost, free of complex operation equipment and suitable for industrial large-scale production.
In a preferred embodiment, the propolis ethanol solution is prepared by a method comprising:
weighing 10-20 g of propolis, cutting, adding into 1000mL of 50-97% ethanol solution, extracting at room temperature for 70-75 hours, and removing impurities to obtain the propolis ethanol solution; wherein the extraction time may typically, but not limited to, be 70 hours, 71 hours, 72 hours, 73 hours, 74 hours, or 75 hours;
preferably, the preparation method of the propolis ethanol solution comprises the following steps:
weighing 10-15g of propolis, chopping, adding into 1000mL of 55-65% ethanol solution, extracting at room temperature for 72 hours, and removing impurities to obtain the propolis ethanol solution.
In the preparation process of the propolis ethanol solution, as the propolis is slowly dissolved, the cut propolis and the ethanol can be fully contacted, and after about 72 hours of extraction, the beneficial substances in the propolis can be fully dissolved in the ethanol, so that the beneficial components in the propolis can be fully utilized.
As mentioned above, since the solubility of propolis in ethanol is relatively high, 60% ethanol solution is used in the preparation process, which is most beneficial for extracting the flavone as a beneficial component in propolis, and if the concentration of ethanol is too low, the solubility of flavone is low, and if the concentration of ethanol is too high, the solubility of impurities in propolis, such as some waxes, is also correspondingly improved, and although the solubility of flavone is increased, the solubility of impurities is also improved, which results in the reduction of the purity of flavone. Furthermore, the content of wax in the ethanol solution of the propolis is high, after the ethanol solution is diluted, the concentration of the ethanol is reduced, the wax is separated out, floccules are formed in the working solution, even if the wax is in the solution of the chitosan, the wax cannot be uniformly dispersed, and irregular spots can appear on the finished fabric.
The ratio of the weight of propolis to the volume of an ethanol solution having a volume concentration of 60% is preferably 1 g: (60-100) mL; if the ratio is less than 1: 60, the effective components in the propolis are not fully dissolved, so that the propolis is wasted, and if the ratio is higher than 1: 100, the impurities in the propolis begin to dissolve in the ethanol, so that waxy floccules appear when the concentration of the ethanol is reduced, and the stability of the working solution is reduced.
The extraction time of the propolis is preferably 72 hours, after the extraction time exceeds 72 hours, the content of the propolis in the ethanol has no obvious change, and the extension time has no practical significance; if the time is shorter than 72 hours, the beneficial components in the propolis can not be fully dissolved, the utilization rate of the propolis is insufficient, and waste is caused.
It is worth noting that wind and rain are most easy to carry pollutants to spread everywhere, and attention is paid to prevent the pollution of the propolis in the box by the wind and rain. Propolis taken out of the beehive is properly packaged and stored. Lead-containing materials are not suitable for beehives. Enterprises producing propolis products establish cooperative relationship with a bee field, and can also help to strengthen the prevention of lead pollution. Lead is a multi-affinity harmful metal, has accumulation in the human body, and is not easy to be discharged out of the body. If lead is excessively accumulated, it may cause damage to the immune system, nervous system, digestive system, function, heart, kidney, etc. of the human body.
The reasons for the heavy metal in the propolis raw material are two main reasons: firstly, the incorrect propolis taking method is that propolis scraped from an iron gauze cover of a beehive has high lead content. Another reason is environmental pollution, such as air, heavy metal lead in soil, etc. can enter propolis components through absorption and transformation of plants. The former is the main cause of high lead content in propolis. Furthermore, the propolis raw material, i.e. the feather glue, which is purchased from bee-keepers, cannot be used directly. If the crude rubber is collected by a gauze, the crude rubber is not treated and the lead content is often over-standard. Some vendors directly make the hair glue into products such as propolis liquid in alcohol for sale, and the products are easy to harm human bodies. Therefore, the above phenomenon should be avoided as much as possible when selecting the propolis raw material.
The preparation of the chitosan solution is not particularly limited. For example, a certain amount of chitosan powder can be weighed, added into water, and mixed and stirred uniformly to obtain the chitosan solution.
In a third aspect, there is provided in at least one embodiment a use of the antimicrobial finish in the antimicrobial finishing of a textile.
The antibacterial finishing agent has the characteristics of good antibacterial effect, high affinity to fabrics, good antibacterial durability, safety, reliability, environmental friendliness, no toxic or side effect, health-care effect and the like, and has important significance for reducing diseases, protecting human health and meeting the requirement of people on pursuing high-quality life style when being applied to the after-finishing process of textiles.
In a preferred embodiment, the antibacterial finishing agent is diluted by 10-50 times to obtain an antibacterial finishing dispersion, and the fabric is immersed in the antibacterial finishing dispersion; or directly soaking the fabric into the prepared antibacterial finishing agent, soaking or padding, and then drying.
It can be understood that, in the antibacterial finishing agent, 20-30 mL of propolis ethanol solution and 100mL of chitosan solution are generally mixed to obtain the antibacterial finishing agent; in practical application, the antibacterial finishing agent can be diluted by 10-50 times to obtain an antibacterial finishing dispersion, then the fabric is soaked or padded, or a propolis solution with a certain volume and a chitosan solution with a certain volume can be directly prepared into the diluted antibacterial finishing dispersion, and then the fabric is soaked or padded.
In a preferred embodiment, the padding is one padding and one rolling, and the rolling residual ratio is 75-85%. The method adopts a one-dipping-one-rolling mode, is convenient to operate, has excellent effect and saves energy; the percent reduction can be typically, but not limited to, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, or 85%, preferably 80%.
In a preferred embodiment, the drying temperature is 120-160 ℃. The drying mode is not limited too much, and the mode commonly used in the field is adopted; typically, but not by way of limitation, the temperature of the oven drying may 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.
The present invention will be further described with reference to specific examples and comparative examples.
Example 1
An antibacterial finishing agent comprises the following components:
15g/L of propolis ethanol solution and 5g/L of chitosan solution.
The preparation method of the propolis ethanol solution comprises the following steps:
weighing 15g of propolis, cutting, adding into 1000mL of 60% ethanol solution, extracting at room temperature for 72 hr, and removing impurities to obtain propolis ethanol solution.
The application method of the antibacterial finishing agent comprises the following steps:
weighing 5mL of prepared 15g/L propolis ethanol solution, adding into 995mL of 5g/L chitosan solution, and fully and uniformly stirring to obtain an antibacterial finishing dispersion, wherein the antibacterial finishing dispersion is equivalent to 0.5% (volume fraction) propolis 60% ethanol solution. Padding pure cotton 40s/144 multiplied by 96 satin fabric, adopting a one-padding one-rolling mode, keeping the rolling residual rate at 80 percent, and drying at 120 ℃. And (4) remaining the residual working solution after padding, and placing and observing the stability of the working solution.
Example 2
The difference from embodiment 1 is that, in this embodiment:
the application method of the antibacterial finishing agent comprises the following steps:
weighing 1mL of prepared 15g/L propolis ethanol solution, adding into 999mL of 5g/L chitosan solution, and stirring to obtain antibacterial finishing dispersion solution equivalent to 0.1% (volume fraction) propolis 60% ethanol solution. Padding pure cotton 40s/144 multiplied by 96 satin fabric, adopting a one-padding one-rolling mode, keeping the rolling residual rate at 80 percent, and drying at 120 ℃. And (4) remaining the residual working solution after padding, and placing and observing the stability of the working solution.
Example 3
An antibacterial finishing agent comprises the following components:
10g/L propolis ethanol solution and 2g/L chitosan solution.
The preparation method of the propolis ethanol solution comprises the following steps:
weighing 10g of propolis, chopping, adding into 1000mL of 60% ethanol solution, extracting at room temperature for 72 hr, and removing impurities to obtain propolis ethanol solution.
The application method of the antibacterial finishing agent comprises the following steps:
weighing 50mL of prepared 10g/L propolis ethanol solution, adding into 950mL of 2g/L chitosan solution, and stirring to obtain antibacterial finishing dispersion solution equivalent to 5% (volume fraction) propolis 60% ethanol solution. Padding pure cotton 40s/144 multiplied by 96 satin fabric, adopting a one-padding one-rolling mode, keeping the rolling residual rate at 80 percent, and drying at 160 ℃. And (4) remaining the residual working solution after padding, and placing and observing the stability of the working solution.
Example 4
The difference from example 3 is that, in this example:
the application method of the antibacterial finishing agent comprises the following steps:
weighing 10mL of prepared 10g/L propolis ethanol solution, adding into 990mL of 2g/L chitosan solution, and stirring to obtain antibacterial finishing dispersion solution equivalent to 1% (volume fraction) propolis 60% ethanol solution. Padding pure cotton 40s/144 multiplied by 96 satin fabric, adopting a one-padding one-rolling mode, keeping the rolling residual rate at 80 percent, and drying at 160 ℃. And (4) remaining the residual working solution after padding, and placing and observing the stability of the working solution.
Example 5
An antibacterial finishing agent comprises the following components:
12g/L propolis ethanol solution and 3g/L chitosan solution.
The preparation method of the propolis ethanol solution comprises the following steps:
weighing 12g of propolis, cutting, adding into 1000mL of 55% ethanol solution, extracting at room temperature for 73 hr, and removing impurities to obtain propolis ethanol solution.
The application method of the antibacterial finishing agent comprises the following steps:
weighing 20mL of prepared 12g/L propolis ethanol solution, adding into 980mL of 3g/L chitosan solution, and stirring to obtain antibacterial finishing dispersion solution equivalent to 2% (volume fraction) propolis 55% ethanol solution. Padding pure cotton 40s/144 multiplied by 96 satin fabric, adopting a one-padding one-rolling mode, keeping the rolling residual rate at 85 percent, and drying at 150 ℃. And (4) remaining the residual working solution after padding, and placing and observing the stability of the working solution.
Examples 6 to 7
An antibacterial finishing agent, which is different from the embodiment:
the volume concentration of the ethanol solution adopted in the preparation process of the propolis ethanol solution is 65 percent and 80 percent respectively;
the rest is the same as in example 1.
Examples 8 to 9
An antibacterial finishing agent, which is different from the embodiment:
the extraction time of the propolis ethanol solution in the preparation process is respectively 70 hours and 75 hours;
the rest is the same as in example 1.
Example 10
An antibacterial finishing agent comprises the following components:
11g/L of propolis ethanol solution and 4g/L of chitosan solution.
The preparation method of the propolis ethanol solution comprises the following steps:
weighing 11g of propolis, cutting, adding into 1000mL of 60% ethanol solution, extracting at room temperature for 72 hr, and removing impurities to obtain propolis ethanol solution.
The application method of the antibacterial finishing agent comprises the following steps:
weighing 80mL of prepared propolis ethanol solution of 11g/L, adding into 920mL of chitosan solution of 4g/L, and stirring to obtain antibacterial finishing dispersion solution equivalent to 8% (volume fraction) propolis 60% ethanol solution. Padding pure cotton 40s/144 multiplied by 96 satin fabric, adopting a one-padding one-rolling mode, with the rolling retention rate of 78 percent, and drying at 140 ℃. And (4) remaining the residual working solution after padding, and placing and observing the stability of the working solution.
Comparative example 1
An antibacterial finishing agent comprises 5g/L of chitosan solution.
The application method of the antibacterial finishing agent comprises the following steps:
1000mL of 5g/L chitosan solution is used for padding pure cotton satin fabric for 40s/144 multiplied by 96, a one-padding one-rolling mode is adopted, the rolling residual rate is 80%, and drying is carried out at 120 ℃. And (4) remaining the residual working solution after padding, and placing and observing the stability of the working solution.
The comparative example is different from example 1 in that only the chitosan solution was added to the antibacterial finishing agent, and no propolis ethanol solution was added.
Comparative example 2
An antibacterial finishing agent comprises 15g/L propolis ethanol solution.
The application method of the antibacterial finishing agent comprises the following steps:
adding 5mL of 15g/L propolis ethanol (60% ethanol solution) solution into 995mL of water, padding pure cotton 40 s/144X 96 satin fabric, adopting a one-padding one-rolling mode, keeping the rolling residue at 80%, and drying at 120 ℃. And (4) remaining the residual working solution after padding, and placing and observing the stability of the working solution.
The difference between the comparative example and the example 1 is that only the propolis ethanol solution is added into the antibacterial finishing agent, and the chitosan solution is not added.
Comparative example 3
An antibacterial finishing agent comprises the following components:
32g/L of propolis 60% ethanol solution and 3g/L of chitosan solution.
This comparative example differs from example 1 in that the concentration of the propolis ethanol solution in the antimicrobial finish is not within the limits of the invention.
Comparative example 4
An antibacterial finishing agent comprises the following components:
5g/L of propolis 60% ethanol solution and 5g/L of chitosan solution.
This comparative example differs from example 1 in that the concentration of the propolis ethanol solution in the antimicrobial finish is not within the limits of the invention.
Comparative example 5
An antibacterial finishing agent comprises the following components:
10g/L propolis ethanol solution and 0.5g/L chitosan solution.
This comparative example differs from example 1 in that the concentration of the chitosan solution in the antimicrobial finish is not within the range defined by the present invention.
The main operating parameters of the examples and comparative examples are shown in table 1.
TABLE 1 Main operating parameters of the examples and comparative examples
Performance testing
And (3) respectively carrying out antibacterial performance tests on the fabrics obtained after finishing in the examples and the comparative examples, and carrying out the antibacterial performance tests according to GB/T20944.3-2008 'evaluation of antibacterial performance of textiles'.
The test method specifically comprises the following steps: round test samples 1, 2, 3, 4, 5, 6, 7, 8, 9 and 10 with the diameters of 25mm +/-5 mm are respectively cut from the finished fabrics of the examples 1-10 for standby, and meanwhile, control samples 1, 2, 3, 4 and 5 with the same size are cut from the finished fabrics prepared in the comparative examples 1-5; in addition, a blank sample with the same size is cut from common 100% pure cotton cloth;
pouring 10mL of agar medium into the sterile plate, and preparing an agar plate after the agar medium is coagulated; taking 150mL of agar culture medium at 45 +/-2 ℃, adding 1mL of test bacterium liquid (with the thallus concentration of 3000cfu/mL) and uniformly mixing, then taking 5mL of test bacterium liquid and adding the test bacterium liquid into an agar plate for later use after the test bacterium liquid is coagulated; respectively placing the test sample, the reference sample and the blank sample in the center of a prepared plate by using a sterile forceps, and uniformly pressing the test sample, the reference sample and the blank sample on an agar culture medium to ensure that the test sample and the agar culture medium are in close contact; then immediately putting the culture medium into an incubator at 37 +/-2 ℃ for culturing for 18-24 h, and ensuring that the test sample and the agar culture medium are kept in good contact in the culture process; after the culture is finished, calculating the width of the bacteriostatic zone of the sample according to the following formula:
H＝(D－d)/2
in the formula: h represents the width of the bacteriostatic zone in mm; d represents the outer diameter of the antibacterial band in mm; d represents the diameter of the test specimen in mm.
After the zone of inhibition was measured, the test specimen was removed from the agar medium with tweezers, and the contact area under the test specimen was examined microscopically for the growth of bacteria, and the inhibition rate was calculated, and the test results are shown in Table 2.
TABLE 2 antibacterial Property test results
From the results, the fabric finished by the antibacterial finishing agent has better antibacterial performance, the bacteriostasis rate of the fabric to common bacteria is still kept at a higher level after 5 times of washing, the bacteriostasis rate can still reach more than 95% (the difference between the unwashed state and the 5 times of washing is about 2%), and the antibacterial effect of the fabric finished by the single chitosan antibacterial finishing agent is greatly reduced after washing and is only about 60%. The single propolis ethanol solution is unstable and is difficult to realize in actual large-scale production. In addition, within the range of the propolis ethanol solution and the chitosan solution provided by the invention, a better antibacterial effect can be achieved, and the solution beyond the range can obviously harden the hand feeling of the fabric, thereby causing the waste of propolis, increasing the cost, or reducing the stability of the working solution.
In addition, the stability of the working fluids after finishing of the respective examples and comparative examples was tested, and the results are shown in table 3.
Table 3 working fluid stability test results
As can be seen from the above, the antibacterial finishing agent has the advantages of good dispersion uniformity, good stability and convenient storage. Meanwhile, when the fabrics finished in the examples and the comparative examples are touched, the hand feeling of the fabrics of the examples is obviously better than that of the fabrics of various comparative examples.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. An antibacterial after-finishing method of fabric is characterized in that an antibacterial finishing agent compounded by a propolis ethanol solution and a chitosan solution is adopted to carry out after-finishing on the fabric; the preparation method of the antibacterial finishing agent comprises the following steps:
preparing components of the antibacterial finishing agent, weighing a certain amount of propolis, chopping, adding into an ethanol solution with the volume concentration of 55-60%, extracting at room temperature for more than 72 hours, and removing impurities to obtain a propolis ethanol solution, wherein the concentration of the propolis ethanol solution is 10-15 g/L; weighing a certain amount of chitosan powder, and dissolving in water to obtain a chitosan solution, wherein the concentration of the chitosan solution is 2-5 g/L;
compounding the antibacterial finishing agent, namely measuring a certain volume of the propolis ethanol solution, adding the propolis ethanol solution into the prepared chitosan solution, and mixing and stirring uniformly to obtain the antibacterial finishing agent, wherein the volume ratio of the propolis ethanol solution to the chitosan solution in the antibacterial finishing agent is (1-100) to (900-999);
the method for finishing the fabric by the antibacterial finishing agent comprises the following steps:
and (3) soaking the fabric into the antibacterial finishing agent, carrying out soaking or padding, and then drying.
2. The antibacterial after-finishing method of fabric according to claim 1, characterized in that the volume fraction of the propolis ethanol solution in the antibacterial finishing agent is 0.1-5%.
3. A method for the antimicrobial afterfinish of a fabric according to claim 1 wherein said ethanol solution has a concentration of 60% by volume.
4. A method for the antimicrobial post-finishing of a fabric according to any one of claims 1 to 3, wherein the padding is a padding-padding with a residual reduction of 75% to 85%.
5. A method for the antimicrobial afterfinish of a textile fabric as claimed in any one of claims 1 to 3, characterized in that said drying temperature is 120-.
6. A method for the antimicrobial afterfinish of a fabric according to any one of claims 1-3, wherein said chitosan has a molecular weight of 5000 or less.
7. A method for the antimicrobial afterfinish of a textile according to any of claims 1-3, characterized in that the textile finished by the method has a bacteriostatic ratio of more than 95% after five washes.
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