CN112472863B - Negative ion functional chip, preparation method and negative ion sanitary towel - Google Patents
Negative ion functional chip, preparation method and negative ion sanitary towel Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/45—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the shape
- A61F13/47—Sanitary towels, incontinence pads or napkins
- A61F13/472—Sanitary towels, incontinence pads or napkins specially adapted for female use
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/84—Accessories, not otherwise provided for, for absorbent pads
- A61F13/8405—Additives, e.g. for odour, disinfectant or pH control
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/40—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing ingredients of undetermined constitution or reaction products thereof, e.g. plant or animal extracts
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- A—HUMAN NECESSITIES
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
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- A—HUMAN NECESSITIES
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/84—Accessories, not otherwise provided for, for absorbent pads
- A61F13/8405—Additives, e.g. for odour, disinfectant or pH control
- A61F2013/8408—Additives, e.g. for odour, disinfectant or pH control with odour control
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- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/84—Accessories, not otherwise provided for, for absorbent pads
- A61F13/8405—Additives, e.g. for odour, disinfectant or pH control
- A61F2013/8408—Additives, e.g. for odour, disinfectant or pH control with odour control
- A61F2013/8435—Additives, e.g. for odour, disinfectant or pH control with odour control with plant derivatives
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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Abstract
The invention relates to an anion functional chip, a preparation method and an anion sanitary towel. The preparation method of the negative ion functional chip comprises the following steps: adding 1-10 parts of tourmaline powder, 1-10 parts of medical stone powder, 0.5-1.5 parts of carbomer or stone seed gum, 5-15 parts of carboxylated calcium lignosulfonate, 0.02-0.1 part of cupric citrate, 0.01-0.05 part of silver citrate and 0.2-0.5 part of nano titanium dioxide composite material into 50-120 parts of deionized water according to the weight part, stirring for 5-15min at the rotating speed of 100-400 rpm, and uniformly mixing to obtain negative ion finishing liquid; soaking the chip in the negative ion finishing liquid at 40-50 ℃ for 20-50min, wherein the mass ratio of the chip to the negative ion finishing liquid is 1 (3-10); and then drying at 40-60 ℃ for 1-5h to obtain the negative ion functional chip. The anion functional chip and the sanitary towel prepared by the invention have the functions of instantaneous absorption and softness, and also have the effects of lasting bacteriostasis and anion release, and can dredge qi and blood, resist bacteria and diminish inflammation and relieve menstrual discomfort symptoms.
Description
Technical Field
The invention relates to the technical field of disposable sanitary products, in particular to an anion functional chip, a preparation method and an anion sanitary towel.
Background
Sanitary napkin, also called sanitary napkin, is a substance with absorption capacity, and is mainly made of high-molecular polymer and high-molecular polymer composite paper formed by cotton, non-woven fabric, paper pulp or the composite of the above materials. Modern sanitary napkins are increasingly being developed toward versatility, such as by attaching multiple functions to a sanitary napkin core to produce a functional sanitary napkin product.
Chinese patent application CN108066808A discloses an anion sanitary towel and a preparation method thereof, wherein the anion sanitary towel comprises an anion functional chip, and the anion functional chip, a surface layer, an absorber, a bottom film, release paper, a coating film and quick and easy adhesion are processed according to the conventional sanitary towel preparation process. The sanitary towel has antibacterial and anion releasing health promoting effects, and has effects of promoting qi and blood circulation, warming channels, dispelling cold, regulating dysmenorrhea, relieving discomfort, relieving emotion, tranquilizing mind, etc.
How to keep the long-acting and stability of the effective functional components of the chip of the functional sanitary towel in the storage process is a problem to be solved.
Disclosure of Invention
In order to solve the problems of the prior art that the antibacterial performance, the negative ion release performance and the durability of the negative ion functional chip of the sanitary towel are to be improved. The invention provides an anion functional chip, a preparation method and an anion sanitary towel.
The invention is further developed on the basis of CN 108066808A. The inventors found that although the antibacterial performance of the negative ion functional chip prepared by the above invention is ideal, the durability is to be improved, and it is difficult to maintain stable antibacterial performance and negative ion release performance. In order to solve the problem of durability, the inventor primarily conceived to add components with better and more durable antibacterial effect and substances with slow release effect into the negative ion finishing liquid.
According to the inventive concept, the technical scheme of the invention is as follows:
the preparation method of the negative ion functional chip comprises the following steps:
adding tourmaline powder, medical stone powder, carbomer or stone seed gum, carboxylated calcium lignosulfonate, cupric citrate, silver citrate and nano titanium dioxide composite material into deionized water, and uniformly stirring and mixing to obtain anion finishing liquid;
and (3) immersing the chip in the negative ion finishing liquid, and drying to obtain the negative ion functional chip.
Preferably, the preparation method of the anion functional chip comprises the following steps:
adding 1-10 parts of tourmaline powder, 1-10 parts of medical stone powder, 0.5-1.5 parts of carbomer or stone seed gum, 5-15 parts of carboxylated calcium lignosulfonate, 0.02-0.1 part of cupric citrate, 0.01-0.05 part of silver citrate and 0.2-0.5 part of nano titanium dioxide composite material into 50-120 parts of deionized water according to the weight part, stirring for 5-15min at the rotating speed of 100-400 rpm, and uniformly mixing to obtain negative ion finishing liquid;
soaking the chip in the negative ion finishing liquid at 40-50 ℃ for 20-50min, wherein the mass ratio of the chip to the negative ion finishing liquid is 1 (3-10); and then drying at 40-60 ℃ for 1-5h to obtain the negative ion functional chip.
The chip is rectangular pure cotton non-woven fabric with the length of 10-18cm and the width of 5-8 cm. Preferably, the chip is a rectangular pure cotton non-woven fabric with the length of 15cm and the width of 7 cm.
Tourmaline powder is a powdery product obtained by processing tourmaline. The tourmaline has complex chemical components, is a silicate mineral with a ring structure and characterized by boron, and has unique properties such as piezoelectricity, pyroelectric property, conductivity, far infrared radiation, anion release property and the like. The tourmaline has a permanent spontaneous electrode, and the generated electrostatic field has adsorption effect on heavy metal ions in water and is sufficient for ionizing air, so that adjacent air water molecules are ionized and converted into air anions, and the sterilization effect is achieved.
The medical stone powder is a natural silicate mineral medical stone powder product, and is nontoxic. The medical stone powder particles are in a coral reef sponge shape, are porous, have large specific surface area and strong adsorption capacity, have good dissolution property, and have adsorption and sustained release effects on metal ions.
After the cupric citrate and the silver citrate are dissolved in water, copper ions and silver ions are released, and the sterilizing and disinfecting capabilities are achieved. In particular, silver ions can strongly attract sulfhydryl (-SH) groups on proteases in bacterial bodies, and can be quickly combined with the proteases, so that the proteases lose activity and the bacteria die. After the bacteria are killed by silver ions, the silver ions are dissociated from the bacterial corpse and then contact with other bacterial colonies, so that a lasting sterilization effect is achieved.
The nano titanium dioxide composite material is prepared from nano titanium dioxide and (reduced graphene oxide and/or bismuth tungstate) by a hydrothermal method.
Preferably, the nano titanium dioxide composite material is prepared from nano titanium dioxide and reduced graphene oxide by a hydrothermal method.
The preparation method of the nano titanium dioxide composite material comprises the following steps: and (3) placing the nano titanium dioxide and the reduced graphene oxide in deionized water according to the mass ratio of 100 (3-9), performing ultrasonic dispersion, uniformly stirring, heating for 1-15 hours at the temperature of 80-240 ℃ for hydrothermal reaction, and naturally cooling, vacuum filtering, washing to neutrality, drying and grinding after the reaction is finished to obtain the nano titanium dioxide composite material.
Preferably, the nano titanium dioxide composite material is prepared from nano titanium dioxide, reduced graphene oxide and bismuth tungstate by a hydrothermal method.
The preparation method of the nano titanium dioxide composite material comprises the following steps: the nano titanium dioxide, the reduced graphene oxide and the bismuth tungstate are mixed according to the mass ratio of 100 (4-6): (0.5-1.5), placing in deionized water for ultrasonic dispersion, stirring uniformly, heating for 1-15 hours at 80-240 ℃ for hydrothermal reaction, naturally cooling, vacuum filtering, washing to neutrality, drying and grinding after the reaction is finished, thus obtaining the nano titanium dioxide composite material.
The chemical formula of the nano titanium dioxide is TiO 2 Is white loose powder, is nontoxic, has good dispersibility and weather resistance, and has good ultraviolet masking effect and antibacterial capability. The antibacterial action mechanism is as follows: tiO in a water and air system under irradiation of sunlight, particularly ultraviolet light 2 Self-breaking down free mobile negatively charged electrons and positively charged holes to form hole-electron pairs. Adsorbed on TiO 2 The dissolved oxygen-trapping electrons on the surface become O 2- The holes will adsorb TiO 2 OH of the surface - And H 2 O is oxidized to OH. O. 2- And OH can react with bacterial organic matters to decompose the bacterial organic matters into CO 2 And H 2 O, thus can kill bacteria rapidly. However, since the hole-electron pair formed is easily recombined, tiO is affected 2 Is effective in killing bacteria.
The reduced graphene oxide is a derivative of graphene, has a two-dimensional layered structure, large specific surface area, rich oxygen-containing functional groups and excellent mechanical, thermal and electrical properties, and is an ideal nanomaterial composite carrier.
The chemical formula of the bismuth tungstate is Bi 2 O 12 W 3 Is a visible light catalyst antibacterial material, the photocatalysis mechanism of which is similar to that of titanium dioxide, and can generate hole-electron pairs under the irradiation of visible light, and the hole-electron pairs are contacted with dissolved oxygen and water in the air to generate O 2- And OH, capable of reacting with bacterial organics to decompose them into CO 2 And H 2 O, thereby rapidly killing the bacteria. Although its visible light absorption performance is good, the generated photogenerated electrons and photogenerated holes are easy to recombine, resulting in lower actual electron efficiency.
Experiments show that after the nano titanium dioxide composite material is added, the antibacterial performance and durability of the negative ion functional chip are greatly improved. Analyzing the reason:
antibacterial properties: first, tiO 2 And Bi (Bi) 2 O 12 W 3 The graphene oxide has strong sterilization effect, and the reduced graphene oxide has excellent conductivity, so that TiO 2 And Bi (Bi) 2 O 12 W 3 After the composite material is compounded with the reduced graphene oxide, the photocatalysis efficiency is further improved, the antibacterial effect is obviously improved, the composite material has a superposition effect with the antibacterial effect of tourmaline, silver ions and copper ions, and the acting speed is faster than that of the silver ions and the copper ions. Secondly, tiO 2 And Bi (Bi) 2 O 12 W 3 The photocatalysis antibacterial function of the silver ion and the copper ion have synergistic effect: tiO (titanium dioxide) 2 And Bi (Bi) 2 O 12 W 3 After forming hole-electron pair, copper ion and silver ion are good electron acceptors, so as to reduce the recombination of hole and electron and improve TiO 2 And Bi (Bi) 2 O 12 W 3 Is used for the antibacterial efficiency of the composition. In addition, in the presence of silver ions and copper ions, the control of TiO is also facilitated 2 Growth of crystalline phase, broadening TiO 2 Is possible to expand TiO 2 The light reaction range and the reactivity are improved.
Experiments show that the ultraviolet light is not generated, and the antibacterial effect and the negative ion release capability of the negative ion functional chip are obviously enhanced when the visible light is irradiated. Possible reasons forThe method comprises the following steps: bi (Bi) 2 O 12 W 3 The interface of the photo-generated charge is tightly contacted with the interface of the reduced graphene oxide, so that the transmission efficiency and the separation efficiency of photo-generated charge are improved, the reactive sites are increased, and the light absorption intensity is improved due to the excellent conductive property of the reduced graphene oxide. Further, due to the electric field effect of tourmaline and the conductivity of reduced graphene oxide, bi 2 O 12 W 3 Generating hole-electron pairs, inducing TiO 2 Formation of upper hole-electron pairs to cause TiO 2 The absorption range of (2) is extended to the visible light region, and the reactivity is improved. On the other hand, the tourmaline particles in the finishing liquid can have the positive and negative poles connected end to end, so that the capability of generating air anions is reduced. The negative oxygen ions on the surface of the nano titanium dioxide composite material and the negative oxygen ions on the surface of tourmaline particles generate electrostatic repulsive force, so that an effective dispersion state can be formed with tourmaline powder particles in the finishing liquid, and the antibacterial capability and the negative ion releasing capability of the tourmaline powder are improved.
Durable antimicrobial properties: tiO (titanium dioxide) 2 And Bi (Bi) 2 O 12 W 3 The antibacterial effect is achieved through the photocatalysis, the molecular structure of the antibacterial agent is not lost in the sterilization process, the antibacterial agent is a durable and long-acting antibacterial agent like tourmaline and silver ions, and the antibacterial agent, the tourmaline and the silver ions can be mutually complemented, so that the chip can continuously and stably exert the long-acting antibacterial performance. For example: the tourmaline powder has weak antibacterial capability, and silver ions can circularly act to achieve lasting antibacterial effect, but in the process of killing bacteria, when part of silver ions are combined with bacterial protease to act, the effective silver ion quantity in the finishing liquid is reduced, and the sterilizing effect is reduced. After the nano titanium dioxide composite material is added, even if silver ions do not kill bacteria yet and are released from bacterial carcasses, the nano titanium dioxide composite material and tourmaline powder can play a good antibacterial role, and the antibacterial performance of the chip is maintained.
Experiments also find that in the prior art, silver ions are easily converted into elemental silver or Ag under the conditions of illumination and the like 2 O, causing discoloration of the chip and reduction of antibacterial performance. After the nano titanium dioxide composite material is added, the nano titanium dioxide composite material has excellent propertiesThe ultraviolet resistance function can effectively control the color change problem, delay the falling of active ingredients caused by the sun aging of the cotton fiber chip, and enhance the lasting antibacterial property and the anion release function of the chip.
The Dan Huazi gel is a water extract of the seeds of the flower. The stone flower seeds are also called seeds of the ice powder seed system pseudo-wintercherry, and are named as pseudo-wintercherry seeds. The water extract mainly contains low-ester pectin, and the water solution is gelatinous and has good film forming property and antibacterial property. And can be combined with metal divalent ions to form an egg lattice structure, so that the compactness is greatly improved. Has effects of clearing heat and annealing, promoting urination, dispelling pathogenic wind, and relieving inflammation.
The Dan Huazi glue is prepared by the following method: and (3) putting 1 part by weight of the stone flower seeds into 3-5 parts by weight of water, stirring for 5-10min at 25-55 ℃ at a stirring speed of 100-300r/min, separating liquid phase from solid phase, and taking liquid phase for freeze drying for 5-10h to obtain the stone flower seed glue. Wherein said Dan Huazi, latin's name Nicandra physaioides (L) Gaertn.
Further preferably, the Dan Huazi glue is prepared by the following method:
and (3) putting 1 part by weight of the flower seeds into 3-5 parts by weight of water, stirring for 5-10min at 25-55 ℃ at a stirring speed of 100-300r/min, separating liquid phase from solid phase, taking the liquid phase, purifying by a lead salt precipitation method to obtain a purified solution, and freeze-drying the purified solution for 5-10h to obtain the flower seed gum.
The lead salt precipitation method comprises the following specific steps:
precipitation: at room temperature, adding saturated neutral lead acetate solution into the liquid phase until precipitation is complete, and filtering to obtain crude and pure liquid;
lead removal: introducing hydrogen sulfide gas into the crude pure liquid until precipitation is complete, completely removing lead at the moment, and filtering to obtain lead-free liquid;
desulfurizing: and (3) placing the lead-removing liquid in an evaporation vessel, heating in a water bath at 65 ℃ until the lead-removing liquid has no odor of the odorless eggs, and removing hydrogen sulfide in the lead-removing liquid to obtain a purified liquid.
The stone flower seed gum obtained by lead salt precipitation method has the advantages of removing impurities such as organic acid, protein, amino acid, mucilage, tannin, resin, acid saponin, etc., and obtaining the effective component-low ester pectin with higher content and purity.
Experiments also find that after carbomer is replaced by the stone seed gum, the antibacterial performance of the negative ion finishing liquid, the negative ion release performance and the durability of the negative ion functional chip are improved, and the analysis reasons are probably due to the fact that the stone seed gum can be combined with Ca in the finishing liquid 2+ ，Cu 2+ The egg lattice structure is formed, so that the finishing liquid is tighter, the interaction between the active ingredients is promoted, and the active ingredients are slowly released, so that better lasting performance is achieved.
The invention also provides a negative ion functional chip which is prepared by adopting the method.
The invention also provides an application of the negative ion functional chip in preparing the negative ion sanitary towel.
The invention also provides a negative ion sanitary towel which comprises the negative ion functional chip.
The negative ion functional chip and the sanitary towel prepared by the invention have lasting antibacterial effect and can release negative ions continuously. According to the invention, the antibacterial effect of the negative ion finishing liquid and the negative ion release performance of the functional chip under different preparation process conditions are researched, so that the optimal production process of the negative ion functional sanitary towel chip is obtained, and the prepared sanitary towel product not only has the basic functions of instantaneous absorption softness and the like, but also has the effects of lasting antibacterial and negative ion release, and can be used for ventilating blood, resisting bacteria, diminishing inflammation and relieving menstrual discomfort symptoms.
Detailed Description
Antibacterial performance test:
the specific formula of the beef extract peptone agar medium for bacterial culture is as follows: 3.0g of beef extract, 10g of peptone, 5.0g of sodium chloride, 20g of agar and 1000mL of water are heated and melted, and the pH value is adjusted to 7.5. Packaging, and sterilizing under high pressure and humidity (121deg.C, 20 min).
And (3) strain: staphylococcus aureus ATCC25923, escherichia coli ATCC8739.
All the test strains are transferred to the corresponding test tube slant culture medium, and each strain is inoculated with multiple strains repeatedly. Bacteria were placed in a biochemical incubator at 37℃for 24 hours, and mold was placed in a biochemical incubator at 28℃for 48 hours. 2 strains are taken for experiment, and the rest are refrigerated for standby.
Picking each colony, inoculating to a plate, culturing for 24 hr, eluting with sterile physiological saline, and preparing into bacteria-containing 10 7 CFU/mL of bacterial suspension. The preparation method comprises the following steps: respectively picking a small amount of bacterial spores to be washed out in sterile physiological saline, scattering glass beads to prepare bacterial suspension, and adjusting the concentration of the bacterial suspension to be 10 7 CFU/mL, ready for use.
A round blank filter paper sheet with the diameter of 60mm is subjected to dry heat sterilization at 160 ℃ and then is preserved for standby under aseptic conditions. 0.1mL of each experimental bacterial suspension which is activated and adjusted in bacterial liquid concentration is sucked by a sterile pipettor and added into a culture dish with a poured culture medium, and the bacterial suspension is uniformly coated by a self-made glass coater which is sterilized by dry heat. And then, each filter paper sheet is clamped by using sterile forceps and placed on different bacteria-containing culture dishes, 10 mu L of negative ion finishing liquid is sucked onto each filter paper sheet by using a sterile pipettor, and two dishes are made for each bacteria in parallel. Deionized water was then used as a negative control. Culturing bacteria in a biochemical incubator at 37 ℃ for 24 hours, measuring the diameter of a bacteriostasis ring by a crisscross method, and taking an average value.
And (3) testing negative ion release performance: the method is used for testing the negative ion generation amount of the JCT 1016-2006 material. The testing instrument adopts an anion tester with the model of ITC-201A provided by Beijing midbody Instrument friend communication technology Co.
Durability test: sealing the negative ion finishing liquid at normal temperature and pressure for 2 months, and testing antibacterial performance; and sealing the prepared negative ion functional chip, storing for 2 months at normal temperature and normal pressure, and testing the negative ion release performance.
In the embodiment, the pure cotton non-woven fabric is specifically 100% pure cotton spunlaced non-woven fabric provided by Wu Jianghao textile Co., ltd, and the gram weight is 60g/m 2 。
The tourmaline powder in the embodiment is 8000 mesh tourmaline powder provided by mineral product processing factories in Yingshou county, hebei province.
In the embodiment, the medical stone powder is specifically medical stone powder with the particle size of 200 nanometers provided by Tianjin wild goose Tianshan stone industry nanometer technology Co.
Carbomers, CAS number: 54182-57-9, in particular cosmetic grade carbomer 940 from Hubei, as supplied by the company of bioengineering, inc.
Copper citrate, CAS number: 10402-15-0.
Silver citrate, CAS number: 314040-92-1.
The preparation method of carboxylated calcium lignosulfonate in the examples is the same as that of the carboxylated calcium lignosulfonate in the example 1 of the patent application CN 201711381045.8. Wherein the raw material calcium lignosulfonate is MG-3 calcium lignosulfonate provided by Shanghai Yun Zhe new material technology Co.Ltd.
In the examples, the sharp nano titanium dioxide, CAS number: 1317-80-2. Provided by Xuan Chengjing Rui New Material Co., ltd., model: vK-TA18, purity > 99.8%, particle size: 20nm, specific surface area: 80m 2 /g。
Reduced graphene oxide in the examples is provided by Shanghai Ditong nanotechnology Inc., manufacturer: graphene Supermarket, product number: HDT0345 has a purity of 98% and a specific surface area of 400m 2 /g。
Bismuth tungstate, CAS no: 13595-87-4.
Lead acetate (trihydrate), CAS number: 6080-56-4.
Hydrogen sulfide, CAS number: 7783-06-4.
In the examples carbon dioxide, CAS number: 124-38-9.
Example 1
(1) Placing anatase nano titanium dioxide and reduced graphene oxide in deionized water according to a mass ratio of 100:6 for ultrasonic dispersion, wherein the mass ratio of solid to liquid is 1:80, stirring uniformly, heating for 5 hours at 100 ℃ to perform hydrothermal reaction, naturally cooling, vacuum filtering, washing to neutrality, drying and grinding after the reaction is finished, thus obtaining the titanium dioxide composite material.
(2) Adding 5 parts of tourmaline powder, 4 parts of medical stone powder, 1 part of carbomer 940, 10 parts of carboxylated calcium lignosulfonate, 0.07 part of cupric citrate, 0.03 part of silver citrate and 0.4 part of titanium dioxide composite material into 90 parts of deionized water, stirring for 10min at the rotating speed of 300r/min, and uniformly mixing to obtain the negative ion finishing liquid.
(3) And (3) soaking the chip in negative ion finishing liquid at 45 ℃ for 30min and drying at 50 ℃ for 3 hours, wherein the mass ratio of the chip to the negative ion finishing liquid is 1:5, so as to obtain the negative ion functional chip.
The chip is rectangular pure cotton non-woven fabric with the length of 15cm and the width of 7 cm.
Example 2
(1) Placing anatase nano titanium dioxide and bismuth tungstate in deionized water according to a mass ratio of 100:6 for ultrasonic dispersion, wherein the mass ratio of solid to liquid is 1:80, stirring uniformly, heating for 5 hours at 100 ℃ to perform hydrothermal reaction, naturally cooling, vacuum filtering, washing to neutrality, drying and grinding after the reaction is finished, thus obtaining the titanium dioxide composite material.
(2) Adding 5 parts of tourmaline powder, 4 parts of medical stone powder, 1 part of carbomer 940, 10 parts of carboxylated calcium lignosulfonate, 0.07 part of cupric citrate, 0.03 part of silver citrate and 0.4 part of titanium dioxide composite material into 90 parts of deionized water, stirring for 10min at the rotating speed of 300r/min, and uniformly mixing to obtain the negative ion finishing liquid.
(3) And (3) soaking the chip in negative ion finishing liquid at 45 ℃ for 30min and drying at 50 ℃ for 3 hours, wherein the mass ratio of the chip to the negative ion finishing liquid is 1:5, so as to obtain the negative ion functional chip.
The chip is rectangular pure cotton non-woven fabric with the length of 15cm and the width of 7 cm.
Example 3
(1) Placing anatase nano titanium dioxide, reduced graphene oxide and bismuth tungstate in deionized water according to a mass ratio of 100:5:1 for ultrasonic dispersion, wherein the mass ratio of solid to liquid is 1:80, stirring uniformly, heating for 5 hours at 100 ℃ to perform hydrothermal reaction, naturally cooling, vacuum filtering, washing to neutrality, drying and grinding after the reaction is finished, thus obtaining the titanium dioxide composite material.
(2) Adding 5 parts of tourmaline powder, 4 parts of medical stone powder, 1 part of carbomer 940, 10 parts of carboxylated calcium lignosulfonate, 0.07 part of cupric citrate, 0.03 part of silver citrate and 0.4 part of titanium dioxide composite material into 90 parts of deionized water, stirring for 10min at the rotating speed of 300r/min, and uniformly mixing to obtain the negative ion finishing liquid.
(3) And (3) soaking the chip in negative ion finishing liquid at 45 ℃ for 30min and drying at 50 ℃ for 3 hours, wherein the mass ratio of the chip to the negative ion finishing liquid is 1:5, so as to obtain the negative ion functional chip.
The chip is rectangular pure cotton non-woven fabric with the length of 15cm and the width of 7 cm.
Example 4
(1) Placing anatase nano titanium dioxide, reduced graphene oxide and bismuth tungstate in deionized water according to a mass ratio of 100:5:1 for ultrasonic dispersion, wherein the mass ratio of solid to liquid is 1:80, stirring uniformly, heating for 5 hours at 100 ℃ to perform hydrothermal reaction, naturally cooling, vacuum filtering, washing to neutrality, drying and grinding after the reaction is finished, thus obtaining the titanium dioxide composite material.
(2) Adding 5 parts of tourmaline powder, 4 parts of medical stone powder, 1 part of stone seed gum, 10 parts of carboxylated calcium lignosulfonate, 0.07 part of cupric citrate, 0.03 part of silver citrate and 0.4 part of titanium dioxide composite material into 90 parts of deionized water, stirring for 10min at the rotating speed of 300r/min, and uniformly mixing to obtain the negative ion finishing liquid.
(3) And (3) soaking the chip in negative ion finishing liquid at 45 ℃ for 30min and drying at 50 ℃ for 3 hours, wherein the mass ratio of the chip to the negative ion finishing liquid is 1:5, so as to obtain the negative ion functional chip.
The chip is rectangular pure cotton non-woven fabric with the length of 15cm and the width of 7 cm.
The Dan Huazi glue is prepared by the following method: 1 part by weight of the stone flower seed is put into 3 parts by weight of water and stirred for 5min at 40 ℃ at a stirring speed of 200r/min. Separating the liquid phase and the solid phase by using a separator after stirring, taking the liquid phase, and freeze-drying for 10 hours to obtain the stone flower seed gum.
Example 5
(1) Placing anatase nano titanium dioxide, reduced graphene oxide and bismuth tungstate in deionized water according to a mass ratio of 100:5:1 for ultrasonic dispersion, wherein the mass ratio of solid to liquid is 1:80, stirring uniformly, heating for 5 hours at 100 ℃ to perform hydrothermal reaction, naturally cooling, vacuum filtering, washing to neutrality, drying and grinding after the reaction is finished, thus obtaining the titanium dioxide composite material.
(2) Adding 5 parts of tourmaline powder, 4 parts of medical stone powder, 1 part of stone seed gum, 10 parts of carboxylated calcium lignosulfonate, 0.07 part of cupric citrate, 0.03 part of silver citrate and 0.4 part of titanium dioxide composite material into 90 parts of deionized water, stirring for 10min at the rotating speed of 300r/min, and uniformly mixing to obtain the negative ion finishing liquid.
(3) And (3) soaking the chip in negative ion finishing liquid at 45 ℃ for 30min and drying at 50 ℃ for 3 hours, wherein the mass ratio of the chip to the negative ion finishing liquid is 1:5, so as to obtain the negative ion functional chip.
The chip is rectangular pure cotton non-woven fabric with the length of 15cm and the width of 7 cm.
The Dan Huazi glue is prepared by the following method: 1 part by weight of the stone flower seed is put into 3 parts by weight of water, the stirring is carried out for 5min at 40 ℃, the stirring speed is 200r/min, then the liquid phase is separated from the solid phase, the liquid phase is taken, the purification is carried out by adopting a lead salt precipitation method to obtain a purified solution, and the purified solution is frozen and dried for 10h to obtain the stone flower seed gum.
The lead salt precipitation method comprises the following specific steps:
precipitation: at room temperature, adding saturated neutral lead acetate solution into the liquid phase until precipitation is complete, and filtering to obtain crude and pure liquid;
lead removal: introducing hydrogen sulfide gas into the crude pure liquid until precipitation is complete, completely removing lead at the moment, and filtering to obtain lead-free liquid;
desulfurizing: and (3) placing the lead-removing liquid in an evaporation vessel, heating in a water bath at 65 ℃ until the lead-removing liquid has no odor of the odorless eggs, and removing hydrogen sulfide in the lead-removing liquid to obtain a purified liquid.
Comparative example 1
(1) 5 parts of tourmaline powder, 4 parts of medical stone powder, 1 part of carbomer 940, 10 parts of carboxylated calcium lignosulfonate, 0.07 part of cupric citrate, 0.03 part of silver citrate and 0.4 part of anatase type nano titanium dioxide are added into 90 parts of deionized water by weight, and stirred for 10 minutes at the rotating speed of 300r/min, and the negative ion finishing liquid is obtained after uniform mixing.
(2) And (3) soaking the chip in negative ion finishing liquid at 45 ℃ for 30min and drying at 50 ℃ for 3 hours, wherein the mass ratio of the chip to the negative ion finishing liquid is 1:5, so as to obtain the negative ion functional chip.
The chip is rectangular pure cotton non-woven fabric with the length of 15cm and the width of 7 cm.
Comparative example 2
(1) Placing anatase nano titanium dioxide and reduced graphene oxide in deionized water according to a mass ratio of 100:6 for ultrasonic dispersion, wherein the mass ratio of solid to liquid is 1:80, stirring uniformly, heating for 5 hours at 100 ℃ to perform hydrothermal reaction, naturally cooling, vacuum filtering, washing to neutrality, drying and grinding after the reaction is finished, thus obtaining the titanium dioxide composite material.
(2) Adding 5 parts of tourmaline powder, 4 parts of medical stone powder, 10 parts of carboxylated calcium lignosulfonate, 0.07 part of cupric citrate, 0.03 part of silver citrate and 0.4 part of titanium dioxide composite material into 90 parts of deionized water, stirring for 10min at the rotating speed of 300r/min, and uniformly mixing to obtain the negative ion finishing liquid.
(3) And (3) soaking the chip in negative ion finishing liquid at 45 ℃ for 30min and drying at 50 ℃ for 3 hours, wherein the mass ratio of the chip to the negative ion finishing liquid is 1:5, so as to obtain the negative ion functional chip.
The chip is rectangular pure cotton non-woven fabric with the length of 15cm and the width of 7 cm.
Test example 1
The antibacterial properties of the negative ion finishing solutions prepared in examples 1-5 and comparative examples 1-2 were tested, and the specific results are shown in Table 1.
Table 1: antibacterial performance test data sheet
The negative ion functional chips prepared in examples 1 to 5 and comparative examples 1 to 2 were tested for negative ion release characteristics, and specific results are shown in Table 2.
Table 2: negative ion release property test
Test example 2
The negative ion finishing liquids prepared in examples 1-5 and comparative examples 1-2 were sealed and stored at normal temperature and pressure for 2 months, and the antibacterial performance was tested, and the specific results are shown in Table 3.
Table 3: antibacterial persistence test data sheet
The negative ion functional chips prepared in examples 1-5 and comparative examples 1-2 were sealed and stored at normal temperature and normal pressure for 2 months, and the negative ion release characteristics were tested, and the specific results are shown in Table 4.
Table 4: data sheet for testing durability of negative ion release
As can be seen by comparison, the ternary composite material of the reduced graphene oxide, bismuth tungstate and nano titanium dioxide in the embodiment 3 has the best antibacterial performance, anion release function and durability. Example 3 reduced graphene oxide is added on the basis of example 2, and the reduced graphene oxide, nano titanium dioxide and bismuth tungstate are compounded to form the nano titanium dioxide composite material. The charges generated by the bismuth tungstate through visible light catalysis are rapidly transmitted under the excellent conductive performance of the graphene, and the titanium dioxide is effectively excited to form a hole-electron pair, so that an antibacterial effect is realized, and the overall antibacterial capacity of the composite material is greatly improved. Example 3 bismuth tungstate is added on the basis of example 1, and the bismuth tungstate is compounded with nano titanium dioxide and reduced graphene oxide to form a nano titanium dioxide composite material. Example 1 only relies on the electric field effect of tourmaline and the conductivity of reduced graphene oxide, but the induction effect is limited although the absorption range of nano titanium dioxide can be expanded to the visible light region. After bismuth tungstate is added, the interface of the bismuth tungstate and the reduced graphene oxide is in close contact, and due to the excellent conductive performance of the reduced graphene oxide, the transmission efficiency and the separation efficiency of photo-generated charges are improved, the reactive sites are increased, and the light absorption intensity is improved. Furthermore, the bismuth tungstate forms a hole-electron pair to assist in inducing titanium dioxide to form a hole-electron pair, so that an antibacterial effect is realized, and the antibacterial capability of the composite material is improved.
When carbomer is replaced by the stone seed gum in example 4, the antibacterial function of the finishing liquid, the negative ion release function of the negative ion functional chip and the durability of the function are improved, probably due to the fact that the stone seed gum can be combined with Ca in the finishing liquid 2+ ，Cu 2+ The egg lattice structure is formed, so that the finishing liquid is tighter, the interaction between the active ingredients is promoted, and the coating effect of the stone seed gum has a slow release effect on the active ingredients, so that the function durability is improved. When the purification of the stone-seed gum by the lead salt precipitation method of example 5 was carried out, the effect was further enhanced because the purity of the active ingredient in the obtained stone-seed gum was higher.
The nano titanium dioxide used alone in comparative example 1 can only form hole-electron pairs under ultraviolet irradiation, thereby realizing antibacterial effect and assisting tourmaline powder particles to disperse, so that the antibacterial performance, the anion release function and the durability are not high.
In comparative example 2, nano titanium dioxide and reduced graphene oxide are compounded, functional components in the finishing liquid are in a dispersed state due to the lack of carbomer and graphite seed glue, have weak interaction and cannot be effectively attached to a chip, and the prepared functional chip has few functional components and the functions are the weakest.
The negative ion functional chip and the sanitary towel prepared by the invention have excellent, stable and durable antibacterial performance and negative ion release performance.
Claims (6)
1. The preparation method of the negative ion functional chip is characterized by comprising the following steps of:
adding 1-10 parts of tourmaline powder, 1-10 parts of medical stone powder, 0.5-1.5 parts of stone seed gum, 5-15 parts of carboxylated calcium lignosulfonate, 0.02-0.1 part of cupric citrate, 0.01-0.05 part of silver citrate and 0.2-0.5 part of nano titanium dioxide composite material into 50-120 parts of deionized water according to the rotating speed of 100-400 rpm for 5-15min, and uniformly mixing to obtain negative ion finishing liquid;
soaking the chip in the negative ion finishing liquid at 40-50 ℃ for 20-50min, wherein the mass ratio of the chip to the negative ion finishing liquid is 1 (3-10); then drying at 40-60 ℃ for 1-5h to obtain the negative ion functional chip;
the preparation method of the nano titanium dioxide composite material comprises the following steps: the nano titanium dioxide, the reduced graphene oxide and the bismuth tungstate are mixed according to the mass ratio of 100 (4-6): (0.5-1.5), placing in deionized water for ultrasonic dispersion, stirring uniformly, heating for 1-15 hours at 80-240 ℃ for hydrothermal reaction, naturally cooling, vacuum filtering, washing to neutrality, drying and grinding after the reaction is finished, thus obtaining the nano titanium dioxide composite material;
the Dan Huazi glue is prepared by the following method: and (3) putting 1 part by weight of the stone flower seeds into 3-5 parts by weight of water, stirring for 5-10min at 25-55 ℃ at a stirring speed of 100-300r/min, separating liquid phase from solid phase, and taking liquid phase for freeze drying for 5-10h to obtain the stone flower seed glue.
2. The method for preparing the negative ion functional chip as claimed in claim 1, wherein the preparation of the Dan Huazi gel can be further purified by a lead salt precipitation method to obtain a purified solution, and the purified solution is freeze-dried;
the lead salt precipitation method comprises the following steps:
precipitation: at room temperature, adding saturated neutral lead acetate solution into the liquid phase until precipitation is complete, and filtering to obtain crude and pure liquid;
lead removal: introducing hydrogen sulfide gas into the crude pure liquid until precipitation is complete, completely removing lead at the moment, and filtering to obtain lead-free liquid;
desulfurizing: and (3) placing the lead-removing liquid in an evaporation vessel, heating in a water bath at 65 ℃ until the lead-removing liquid has no odor of the odorless eggs, and removing hydrogen sulfide in the lead-removing liquid to obtain a purified liquid.
3. The method for preparing the negative ion functional chip as claimed in claim 1, wherein the chip is a rectangular pure cotton non-woven fabric with the length of 10-18cm and the width of 5-8 cm.
4. An anion functional chip prepared by the method of any one of claims 1-3.
5. Use of the negative ion functional chip according to claim 4 for preparing a negative ion sanitary towel.
6. An anion sanitary towel comprising the anion functional chip of claim 4.
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