CN111793973A - Functional graphene loaded with turmeric extract, and preparation method and application thereof - Google Patents
Functional graphene loaded with turmeric extract, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a turmeric extract-loaded functionalized graphene, and a preparation method and application thereof, and belongs to the field of medical protective articles. The preparation method comprises the following steps: the preparation method comprises the steps of graphene oxide preparation, sulfonated graphene preparation, functionalized graphene preparation and turmeric extract loaded functionalized graphene preparation. The invention combines the hydrophobic medicine curcumin and the functionalized graphene together, fully exerts the characteristics of the nano material and the excellent antibacterial and antiviral pharmacological activity of the turmeric root extract, and simultaneously solves the problems of poor water solubility, low effective utilization rate and the like of the curcumin. In addition, the functional graphene loaded with the curcuma extract is fixed on cotton fabric to be used as a facing material by matching with an after-finishing process.
Description
Technical Field
The invention belongs to the field of medical protective articles, and particularly relates to a turmeric extract-loaded functionalized graphene, and a preparation method and application thereof.
Background
When respiratory infectious diseases are epidemic or work in the polluted environment such as dust, the mask has a good effect, and bacteria or pollutants can be filtered out in a filtering mode. However, as people pay more attention to the protection of individuals against bacteria, viruses, pollutants and the like, and as the mask is mostly made of cloth or paper and the like, especially the mask is generally used for medical surgery, water vapor exhaled by a human body or sweat discharged by the human body can adhere to the surface of the mask in the long-term wearing process, and a proper growing condition is provided for filtering the bacteria or pollutants on the surface of the mask. Therefore, such masks should not be used for too long a continuous time and not be recommended to be reused.
In the prior art, a sterilization mask for killing bacteria by adding a sterilization antiviral agent on the surface layer of the mask is provided. However, if the sterilizing mask is made of volatile sterilizing antiviral agents such as ethanol and hypochlorite, the mask has certain timeliness, and the antibacterial effect of the mask is greatly reduced along with the volatilization of the sterilizing antiviral agents. If the sterilizing mask is made of the sterilizing mask made of organic synthetic sterilizing and antiviral agents such as quaternary ammonium salts, ureas, guanidines, organic metals and the like, the sterilizing and antiviral agents directly contact with the skin of a human body, adverse reactions such as allergy and the like to people with sensitive constitution are easily caused, and the biological safety of the sterilizing and antiviral agents is uncertain.
Through data review, the Niamsa group researches that the turmeric extract has antibacterial activity on common escherichia coli, staphylococcus aureus, klebsiella pneumoniae and staphylococcus epidermidis, and can kill salmonella typhimurium, escherichia coli and certain drug-resistant strains through photodynamic therapy, and Li C J and the like discover that the turmeric extract can be used as a reverse transcriptase inhibitor to inhibit the replication process of most viruses, can block replication and proliferation of progeny viruses in host cells, and can inhibit the activity of related enzymes, so that the turmeric extract can effectively inhibit various viruses such as influenza virus, Herpes Simplex Virus (HSV), hepatitis virus (HCV), Respiratory Syncytial Virus (RSV) and the like.
The applicant has prepared the turmeric root extracting solution into the antibacterial finishing solution, and then combines the extracting solution with cotton fabrics through a post-finishing process to achieve the effects of sterilization and virus resistance. However, the extraction process in the turmeric root extract is complex and the yield is low. The post-finishing process of the cotton fabric cannot fully exert the antibacterial effect of the turmeric extract, and the effective utilization rate of the turmeric extract is low.
Disclosure of Invention
The purpose of the invention is as follows: provided are a turmeric extract-loaded functionalized graphene, a preparation method and an application thereof, so as to solve the problems involved in the background art.
The technical scheme is as follows: a preparation method of functional graphene loaded with turmeric extract comprises the following steps:
step 1, preparation of graphene oxide
Slowly adding a mixture of 10g of graphite powder and 5g of sodium nitrate into 250mL of concentrated sulfuric acid under the conditions of ice bath and stirring, continuously stirring for 2-5 min, then adding 30g of potassium permanganate powder, fully stirring until the temperature is stabilized to normal temperature, heating to 40-45 ℃, continuously stirring for 30-45 min, then slowly adding deionized water, diluting to 8-10 times of the original volume with ionized water, then adding a certain amount of hydrogen peroxide solution, filtering, cleaning a filter cake with hydrochloric acid solution, and finally drying a target product;
step 2, preparation of sulfonated graphene
Adding graphene oxide into water, forming a uniform dispersion liquid under the action of ultrasonic waves, adjusting the pH of the solution to 9-10 by using sodium carbonate, adding hydrazine hydrate, refluxing for 1-2 h at 80-100 ℃, cooling, filtering, washing a filter cake by using deionized water, drying to obtain proper black graphene powder, mixing the black graphene powder suspension and a diazonium salt solution, reacting for 2-5 h, filtering, washing the filter cake by using deionized water, and drying to obtain sulfonated graphene;
step 3, preparation of functionalized graphene
Adding 0.5g of sulfonated graphene and 9-10 g of methyl-B-cyclodextrin into 5L of water, forming a uniform dispersion liquid under the action of ultrasonic waves, then adding ammonia water, reacting for 8-12 h at 70-90 ℃, cooling, centrifuging, washing a filter cake with deionized water, and drying to obtain black functionalized graphene powder;
step 4, preparing functional graphene loaded with turmeric extract
Adding the functionalized graphene powder into a turmeric extract solution with the concentration of 0.01-0.05 mol/L, reacting for 30-60 min under ultrasonic-assisted reaction, then performing centrifugal separation, collecting a lower-layer precipitate, washing the precipitate with deionized water, and drying to obtain a target product.
Preferably, the diazonium salt solution is prepared as follows: under the ice bath condition, sodium sulfanilate and sodium nitrite are respectively dissolved in an aqueous solution of hydrochloric acid, then a sodium nitrite aqueous solution is slowly added into the sodium nitrite solution, the reaction is carried out for 1-2 hours under the ice bath condition, a diazonium salt solution is obtained, and finally, redundant sodium nitrite is removed through urea.
Preferably, the effective component of the turmeric root extract is xanthorrhizol, and the structural formula is as follows:
preferably, the extraction process of the xanthorrhizol is as follows:
step 1, processing, namely cleaning a certain amount of turmeric, crushing, adding acid for hydrolysis, and performing centrifugal treatment to separate solid hydrolysate;
step 2, extracting, namely performing reflux extraction by taking ethyl acetate as an extracting agent, wherein the volume mass ratio of the extracting agent to the solid hydrolysate is (2-5) to 1 during extraction, and extracting for 2-4 hours; then adjusting the pH value of the purified solution to 8-9 by ammonia water; taking the supernatant and ethyl acetate as an extractant, and performing reflux extraction to obtain a turmeric root extracting solution;
step 3, separating, namely concentrating the turmeric root extract to 1/3-1/2 of the original volume, performing silica gel column chromatography, eluting for 3-5 hours by using No. 6 gasoline and chloroform in a volume ratio of (40-50): 1 as a solvent, and collecting a xanthogen diol crude crystal at 230nm by using an ultraviolet detector according to a peak;
and 4, purifying, dissolving the xanthorrhizol crude crystals with ethanol solutions respectively, filtering, concentrating the filtrate to 4-6 times of the weight of the crude crystals, standing, cooling, evaporating, recrystallizing and drying to obtain the xanthorrhizol crystals.
Preferably, the silica gel column chromatography adopts 200-300 mesh silica gel, the column is flushed by ethanol after the elution is finished, and the column chromatography silica gel column can be repeatedly used for 2-5 times.
Preferably, the preparation method of the turmeric extract solution is: the preparation method comprises the steps of taking sodium dodecyl benzene sulfonate and tween-80 in a mass ratio of 2:1 as an emulsifier, and emulsifying curcumol, xanthogen diol or a mixture of the curcumol and the xanthogen diol into emulsion with the concentration of 8-10% by weight.
The invention also provides an antibacterial material obtained by the preparation method of the functional graphene loaded with the turmeric extract.
The invention also provides application of the antibacterial material obtained by the preparation method of the functional graphene loaded with the turmeric extract in preparation of a facing material or as a facing material component, and is characterized in that the application method comprises the following steps:
step 1, adding functional graphene loaded with turmeric extract, a penetrating agent JFC and a dispersing agent NNO into water, and forming uniform dispersion liquid under the action of ultrasonic waves;
step 2, placing the cotton fabric in an aqueous solution of sodium carbonate and sodium aminobenzenesulfonate, boiling for 15-30 min, and then washing and drying for later use;
step 3, mixing cotton fabric and the functional graphene dispersion liquid loaded with the curcuma extract according to a bath ratio of (40-50): 1, placing the mixture in an infrared dyeing machine, dyeing the fabric with the functional graphene loaded with the curcuma extract under a preset condition, taking out the cotton fabric after finishing, removing redundant moisture through a padder, and finally drying the cotton fabric at 50-60 ℃;
and 4, immersing the fabric into a sodium hydrosulfite aqueous solution, stirring for 5-10 min, washing twice, and naturally drying to obtain the facing material.
Preferably, the predetermined condition is: heating to 75-80 ℃ according to the heating rate of 2-3 ℃/min, adding sodium chloride and a leveling agent, heating to 110-130 ℃ according to the heating rate of 0.8-1.2 ℃/min, preserving heat for 30-45 min, and finally cooling to room temperature.
Has the advantages that: the invention relates to a turmeric extract-loaded functionalized graphene, a preparation method and application thereof. In addition, the functional graphene loaded with the curcuma extract is fixed on cotton fabric to be used as a facing material by matching with an after-finishing process.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
In the prior art, a sterilizing mask for killing bacteria by adding a sterilizing antiviral agent to the surface layer of the mask has been developed. However, if the sterilizing mask is made of volatile sterilizing antiviral agents such as ethanol and hypochlorite, the mask has certain timeliness, and the antibacterial effect of the mask is greatly reduced along with the volatilization of the sterilizing antiviral agents. If the sterilizing mask is made of the sterilizing mask made of organic synthetic sterilizing and antiviral agents such as quaternary ammonium salts, ureas, guanidines, organic metals and the like, the sterilizing and antiviral agents directly contact with the skin of a human body, adverse reactions such as allergy and the like to people with sensitive constitution are easily caused, and the biological safety of the sterilizing and antiviral agents is uncertain.
The natural antibacterial agent is mainly an extract of natural plants, has broad-spectrum antibacterial effect and has advantages in safety, durability, heat resistance and the like, so that the application and research of the natural antibacterial agent are more and more paid attention by people. The applicant selects the extract of aloe, honeysuckle, mugwort, aloe, sorb, turmeric and other plants as the antibacterial agent. Firstly, selecting a commercially available plant extract for an antibacterial test, wherein the aloe extract has stronger bactericidal and bacteriostatic properties on escherichia coli and staphylococcus aureus, but has weaker resistance on candida albicans, haemophilus influenzae, pneumococcal bacteria and influenza viruses; the honeysuckle has stronger inhibitive performance on staphylococcus aureus, escherichia coli and candida albicans, but has weaker resistance on candida albicans, haemophilus influenzae, pneumococcal bacteria and influenza virus; the mugwort is used as a fabric of the Compositae, the air temperature of the mugwort has the effects of stabilizing mood, relaxing body and mind, resisting allergy and promoting blood circulation, and the mugwort has stronger antibacterial effect on most bacteria, but has smaller effect on influenza virus; sorbic acid extracted from sorbus has higher antibacterial performance, inhibits the growth and the propagation of mould, has obvious inhibiting effect on influenza virus, but has larger irritation on skin and eyes; the Curcuma longa extract is a natural terpenoid, and has antiinflammatory, antioxidant, anticancer, antibacterial and antiviral effects.
Through data review, the Niamsa group researches that the turmeric extract has antibacterial activity on common escherichia coli, staphylococcus aureus, klebsiella pneumoniae and staphylococcus epidermidis, and can kill salmonella typhimurium, escherichia coli and certain drug-resistant strains through photodynamic therapy, and Li C J and the like discover that the turmeric extract can be used as a reverse transcriptase inhibitor to inhibit the replication process of most viruses, can block replication and proliferation of progeny viruses in host cells, and can inhibit the activity of related enzymes, so that the turmeric extract can effectively inhibit various viruses such as influenza virus, Herpes Simplex Virus (HSV), hepatitis virus (HCV), Respiratory Syncytial Virus (RSV) and the like. Theoretically, the turmeric extract can have certain inhibition effect on most of respiratory diseases such as bacteria and viruses.
The turmeric root extracting solution comprises two effective components of turmeric root alcohol and turmeric root diol, wherein the combination degree of the turmeric root diol and graphene is better, in the invention, the turmeric root diol is preferred, and the structural formula is as follows:
the applicant entrusts Nanjing university of traditional Chinese medicine to extract effective components in turmeric, and the extraction method comprises the following steps: step 1, processing, namely cleaning a certain amount of turmeric, crushing, adding acid for hydrolysis, and performing centrifugal treatment to separate solid hydrolysate; step 2, extracting, namely performing reflux extraction by taking ethyl acetate as an extracting agent, wherein the volume mass ratio of the extracting agent to the solid hydrolysate is (2-5) to 1 during extraction, and extracting for 2-4 hours; then adjusting the pH value of the purified solution to 8-9 by ammonia water; taking the supernatant and ethyl acetate as an extractant, and performing reflux extraction to obtain a turmeric root extracting solution; step 3, separating, namely concentrating the turmeric root extract to 1/3-1/2 of the original volume, performing silica gel column chromatography, eluting for 3-5 hours by using No. 6 gasoline and chloroform in a volume ratio of (40-50): 1 as a solvent, and collecting a xanthogen diol crude crystal at 230nm by using an ultraviolet detector according to a peak; and 4, purifying, dissolving the xanthorrhizol crude crystals with ethanol solutions respectively, filtering, concentrating the filtrate to 4-6 times of the weight of the crude crystals, standing, cooling, evaporating, recrystallizing and drying to obtain the xanthorrhizol and xanthorrhizol crystals. The silica gel column chromatography adopts 200-300 mesh silica gel, ethanol is adopted to wash the column after the elution is finished, and the column chromatography silica gel column can be repeatedly used for 2-5 times.
Because the water solubility of the xanthorrhizol is poor and the xanthorrhizol cannot be directly utilized, the applicant emulsifies the effective components to form the antibacterial agent, compounds the antibacterial agent into the antibacterial finishing liquid, and combines the extracting solution with the cotton fabric through a post-finishing process to achieve the effects of sterilization and virus resistance. However, the extraction process in the turmeric root extract is complex and the yield is low. The post-finishing process of the cotton fabric cannot fully exert the antibacterial effect of the turmeric extract, and the effective utilization rate of the turmeric extract is low.
The graphene oxide has the advantages of low cost, easy modification, large surface area and the like, and is an excellent drug carrier and a novel antibacterial nano material. Therefore, the graphene oxide material is subjected to surface modification, the functionalized graphene has the effect of efficiently resisting respiratory bacteria and viruses, can efficiently load the xanthogen diol, and solves the problems that the xanthogen diol cannot be contacted with water and is difficult to contact with bacteria and viruses, and the drug effect is difficult to give full play. Finally realizing the synergistic effect of the radix astragali II and the nano material. The preparation method comprises the following steps: the preparation method of the functional graphene loaded with the turmeric extract is characterized by comprising the following steps: slowly adding a mixture of 10g of graphite powder and 5g of sodium nitrate into 250mL of concentrated sulfuric acid under the conditions of ice bath and stirring, continuously stirring for 2-5 min, then adding 30g of potassium permanganate powder, fully stirring until the temperature is stabilized to normal temperature, heating to 40-45 ℃, continuously stirring for 30-45 min, then slowly adding deionized water, diluting to 8-10 times of the original volume with ionized water, then adding a certain amount of hydrogen peroxide solution, filtering, cleaning a filter cake with hydrochloric acid solution, and finally drying a target product; adding graphene oxide into water, forming a uniform dispersion liquid under the action of ultrasonic waves, adjusting the pH of the solution to 9-10 by using sodium carbonate, adding hydrazine hydrate, refluxing for 1-2 h at 80-100 ℃, cooling, filtering, washing a filter cake by using deionized water, drying to obtain proper black graphene powder, mixing the black graphene powder suspension and a diazonium salt solution, reacting for 2-5 h, filtering, washing the filter cake by using deionized water, and drying to obtain sulfonated graphene; adding 0.5g of sulfonated graphene and 9-10 g of methyl-B-cyclodextrin into 5L of water, forming a uniform dispersion liquid under the action of ultrasonic waves, then adding ammonia water, reacting for 8-12 h at 70-90 ℃, cooling, centrifuging, washing a filter cake with deionized water, and drying to obtain black functionalized graphene powder; adding the functionalized graphene powder into a turmeric extract solution with the concentration of 0.01-0.05 mol/L, reacting for 30-60 min under ultrasonic-assisted reaction, then performing centrifugal separation, collecting a lower-layer precipitate, washing the precipitate with deionized water, and drying to obtain a target product.
Since aromatic benzene rings in the functionalized graphene loaded with the curcuma longa extract all contain oxygen-containing groups, similar to the structure of the vat dye, hydrogen bonding and van der waals force exist between graphene sheet layers and fibers, and therefore the functionalized graphene loaded with the curcuma longa extract can be used for adsorbing and fixing the surface of cotton fibers in a traditional dyeing mode. Through orthogonal experiments, the applicant further optimizes the fixation process, comprising the following steps: firstly, adding functional graphene loaded with turmeric extract, a penetrating agent JFC and a dispersing agent NNO into water, and forming uniform dispersion liquid under the action of ultrasonic waves; then placing the cotton fabric in an aqueous solution of sodium carbonate and sodium aminobenzenesulfonate, boiling for 15-30 min, and then washing and drying for later use; mixing cotton fabric and the functional graphene dispersion liquid loaded with the turmeric extract according to a bath ratio of (40-50): 1, placing the mixture in an infrared dyeing machine, heating to 75-80 ℃ according to a heating rate of 2-3 ℃/min, adding sodium chloride and a leveling agent, heating to 110-130 ℃ according to a heating rate of 0.8-1.2 ℃/min, preserving heat for 30-45 min, cooling to room temperature, dyeing the fabric with the functional graphene loaded with the turmeric extract, taking out the cotton fabric after finishing, removing excessive moisture through a padder, and finally drying at 50-60 ℃; and then immersing the fabric into a sodium hydrosulfite aqueous solution, stirring for 5-10 min, washing twice, and naturally drying to obtain the facing material.
The invention will now be further described with reference to the following examples, which are intended to be illustrative of the invention and are not to be construed as limiting the invention.
Example 1
Extracting effective components in the turmeric: cleaning 2kg of Curcuma rhizome, pulverizing, hydrolyzing with acid, centrifuging, and separating solid hydrolysate; performing reflux extraction by using ethyl acetate as an extractant, wherein the volume-to-mass ratio of the extractant to the solid hydrolysate is 4:1 during extraction, and extracting for 3 hours; then adjusting the pH value of ammonia water in the purified liquid to 8.5; taking the supernatant and ethyl acetate as an extractant, and performing reflux extraction to obtain a turmeric root extracting solution; concentrating the turmeric root extract to 1/3 of the original volume, performing 200-mesh silica gel column chromatography, eluting with No. 6 gasoline and chloroform at a volume ratio of 40:1 as solvent for 4h, and collecting the xanthogen diol crude crystals at 230nm by using an ultraviolet detector; dissolving the xanthorrhizol crude crystals with ethanol solution respectively, filtering, concentrating the filtrate to 5 times of the weight of the crude crystals, standing, cooling, evaporating, recrystallizing, and drying to obtain 19.5g of xanthorrhizol crystals.
Preparing functional graphene loaded with turmeric extract: under the conditions of ice bath and stirring, slowly adding a mixture of 10g of graphite powder and 5g of sodium nitrate into 250mL of concentrated sulfuric acid, continuously stirring for 5min, then adding 30g of potassium permanganate powder, fully stirring until the temperature is stabilized to normal temperature, heating to 42 ℃, continuously stirring for 40min, then slowly adding deionized water, diluting to 9 times of the original volume with ionized water, then adding a certain amount of hydrogen peroxide solution, filtering, cleaning a filter cake with hydrochloric acid solution, and finally drying graphene oxide; adding 0.15g of graphene oxide into 150mL of water, forming uniform dispersion under the action of ultrasonic waves, adjusting the pH of the solution to 10 by using sodium carbonate, adding hydrazine hydrate, refluxing for 2h at 80 ℃, cooling, filtering, washing a filter cake by using deionized water, drying to obtain proper black graphene powder, then mixing 150mL of black graphene powder suspension with 20mL of diazonium solution (under the ice bath condition, respectively dissolving sodium sulfanilate and sodium nitrite into the aqueous solution of hydrochloric acid, then slowly adding the aqueous solution of sodium nitrite into the sodium nitrite solution, reacting for 1-2 h under the ice bath condition to obtain the diazonium solution, finally removing the excessive sodium nitrite by using urea), mixing, reacting for 2h, filtering, washing the filter cake by using the deionized water, and drying to obtain sulfonated graphene; adding 0.1g of sulfonated graphene and 0.9g of methyl-B-cyclodextrin into 100mL of water, forming uniform dispersion liquid under the action of ultrasonic waves, then adding ammonia water, reacting for 12h at 80 ℃, cooling, centrifuging, washing a filter cake with deionized water, and drying to obtain black functionalized graphene powder; adding the functionalized graphene powder into a turmeric extract solution with the concentration of 0.02 mol/L, reacting for 45min under ultrasonic-assisted reaction, then carrying out centrifugal separation, collecting a lower-layer precipitate, washing the precipitate with deionized water, and drying to obtain a target product.
Adsorption of functional graphene loaded with turmeric extract: firstly, 2g of functional graphene loaded with turmeric extract, 0.5g of penetrating agent JFC and 0.2g of dispersing agent NNO are added into 100mL of water to form uniform dispersion liquid under the action of ultrasonic waves; then placing the cotton fabric in an aqueous solution of sodium carbonate and sodium aminobenzenesulfonate for boiling for 30min, and then washing and drying the cotton fabric for later use; mixing cotton fabric and the functional graphene dispersion liquid loaded with the curcuma longa extract according to a bath ratio of 45:1, placing the mixture in an infrared dyeing machine, heating to 78 ℃ according to a heating rate of 2 ℃/min, adding sodium chloride and a leveling agent, heating to 125 ℃ according to a heating rate of 0.8 ℃/min, preserving heat for 30min, finally cooling to room temperature, dyeing the fabric loaded with the functional graphene loaded with the curcuma longa extract, taking out the cotton fabric after finishing, removing excessive moisture through a padder, and finally drying at 55 ℃; and then immersing the fabric into a sodium hydrosulfite aqueous solution, stirring for 8min, then washing twice, and naturally drying in air to obtain the finishing material.
Example 2
Extracting effective components in the turmeric: the same as in example 1.
Preparing functional graphene loaded with turmeric extract: under the conditions of ice bath and stirring, slowly adding a mixture of 10g of graphite powder and 5g of sodium nitrate into 250mL of concentrated sulfuric acid, continuously stirring for 3min, then adding 30g of potassium permanganate powder, fully stirring until the temperature is stabilized to normal temperature, heating to 40 ℃, continuously stirring for 45min, then slowly adding deionized water, diluting to 8 times of the original volume with ionized water, then adding a certain amount of hydrogen peroxide solution, filtering, cleaning a filter cake with hydrochloric acid solution, and finally drying graphene oxide; adding 0.15g of graphene oxide into 150mL of water, forming a uniform dispersion liquid under the action of ultrasonic waves, adjusting the pH of the solution to 10 by using sodium carbonate, adding hydrazine hydrate, refluxing for 1h at 100 ℃, cooling, filtering, washing a filter cake by using deionized water, drying to obtain proper black graphene powder, mixing 150mL of black graphene powder suspension with 20mL of diazonium salt solution (same as in example 1), reacting for 2h, filtering, washing the filter cake by using deionized water, and drying to obtain sulfonated graphene; adding 0.1g of sulfonated graphene and 0.9g of methyl-B-cyclodextrin into 100mL of water, forming uniform dispersion liquid under the action of ultrasonic waves, then adding ammonia water, reacting for 12h at 80 ℃, cooling, centrifuging, washing a filter cake with deionized water, and drying to obtain black functionalized graphene powder; adding the functionalized graphene powder into a turmeric extract solution with the concentration of 0.05mol/L, reacting for 30min under ultrasonic-assisted reaction, then carrying out centrifugal separation, collecting a lower-layer precipitate, washing the precipitate with deionized water, and drying to obtain a target product.
Adsorption of functional graphene loaded with turmeric extract: firstly, 2g of functional graphene loaded with turmeric extract, 0.5g of penetrating agent JFC and 0.2g of dispersing agent NNO are added into 100mL of water to form uniform dispersion liquid under the action of ultrasonic waves; then placing the cotton fabric in an aqueous solution of sodium carbonate and sodium aminobenzenesulfonate, boiling for 20min, and then washing and drying for later use; mixing cotton fabric and the functional graphene dispersion liquid loaded with the curcuma longa extract according to a bath ratio of 40:1, placing the mixture in an infrared dyeing machine, heating to 78 ℃ according to a heating rate of 3.0 ℃/min, adding sodium chloride and a leveling agent, heating to 125 ℃ according to a heating rate of 1.0 ℃/min, preserving heat for 45min, finally cooling to room temperature, dyeing the fabric loaded with the functional graphene loaded with the curcuma longa extract, taking out the cotton fabric after finishing, removing excessive moisture through a padder, and finally drying at 60 ℃; and then immersing the fabric into a sodium hydrosulfite aqueous solution, stirring for 5-10 min, washing twice, and naturally drying to obtain the facing material.
Example 3
Extracting effective components in the turmeric: the same as in example 1.
Preparing functional graphene loaded with turmeric extract: under the conditions of ice bath and stirring, slowly adding a mixture of 10g of graphite powder and 5g of sodium nitrate into 250mL of concentrated sulfuric acid, continuously stirring for 2min, then adding 30g of potassium permanganate powder, fully stirring until the temperature is stabilized to normal temperature, heating to 50 ℃, continuously stirring for 30min, then slowly adding deionized water, diluting to 10 times of the original volume with ionized water, then adding a certain amount of hydrogen peroxide solution, filtering, cleaning a filter cake with hydrochloric acid solution, and finally drying graphene oxide; adding 0.15g of graphene oxide into 150mL of water, forming a uniform dispersion liquid under the action of ultrasonic waves, adjusting the pH value of the solution to 9 by using sodium carbonate, adding hydrazine hydrate, refluxing for 1.5h at 90 ℃, cooling, filtering, washing a filter cake by using deionized water, drying to obtain proper black graphene powder, mixing 150mL of black graphene powder suspension with 20mL of diazonium salt solution (same as in example 1), reacting for 5h, filtering, washing the filter cake by using deionized water, and drying to obtain sulfonated graphene; adding 0.1g of sulfonated graphene and 0.9g of methyl-B-cyclodextrin into 100mL of water, forming uniform dispersion liquid under the action of ultrasonic waves, then adding ammonia water, reacting for 8 hours at 90 ℃, cooling, centrifuging, washing a filter cake with deionized water, and drying to obtain black functionalized graphene powder; adding the functionalized graphene powder into a turmeric extract solution with the concentration of 0.01 mol/L, reacting for 60min under ultrasonic-assisted reaction, then carrying out centrifugal separation, collecting a lower-layer precipitate, washing the precipitate with deionized water, and drying to obtain a target product.
Adsorption of functional graphene loaded with turmeric extract: firstly, 2g of functional graphene loaded with turmeric extract, 0.5g of penetrating agent JFC and 0.2g of dispersing agent NNO are added into 100mL of water to form uniform dispersion liquid under the action of ultrasonic waves; then placing the cotton fabric in an aqueous solution of sodium carbonate and sodium aminobenzenesulfonate for boiling for 30min, and then washing and drying the cotton fabric for later use; mixing cotton fabric and the functional graphene dispersion liquid loaded with the curcuma longa extract according to a bath ratio of 40:1, placing the mixture in an infrared dyeing machine, heating to 78 ℃ according to a heating rate of 2.5 ℃/min, adding sodium chloride and a leveling agent, heating to 130 ℃ according to a heating rate of 0.9 ℃/min, preserving heat for 30min, finally cooling to room temperature, dyeing the fabric loaded with the functional graphene loaded with the curcuma longa extract, taking out the cotton fabric after finishing, removing excessive moisture through a padder, and finally drying at 55 ℃; and then immersing the fabric into a sodium hydrosulfite aqueous solution, stirring for 10min, then washing twice, and naturally drying in air to obtain the finishing material.
Comparative example 1
Extracting effective components in the turmeric: the same as in example 1.
Preparing a composite finishing liquid: the quality ratio of sodium dodecyl benzene sulfonate and tween-80 is 2:1, and the xanthene glycol is emulsified into 10% wt concentration emulsion. Then further preparing an antibacterial finishing liquid which comprises the following components: the concentration of turmeric root extract (10 wt% of effective components) is 30g/L, the concentration of mugwort extract (commercially available essential oil) is 5g/L, the concentration of cross-linking agent (a composition formed by mixing citric acid and DL-2, 3-dihydroxybenzoic acid in a molar ratio of 2: 1) is 35g/L, the concentration of sodium hypophosphite is 3g/L, the concentration of JFC is 1g/L, and the solvent is deionized water.
Antibacterial finishing: soaking the cotton fabric in the composite finishing liquid for 15min at room temperature, soaking for two times and rolling for two times, wherein the mangle expression is 80%, pre-drying for 3min at the temperature of 65 ℃ to enable the finishing liquid to fully permeate into the cotton fiber, and then baking for 8min at the temperature of 135 ℃ to fix the color; and finally, washing the cotton fabric by using deionized water, removing floating color (polybasic carboxylic acid or other fixed extracts), and naturally drying.
Comparative example 2
Untreated cotton cloth of the same size was sprayed with medical alcohol of 75% concentration, and comparative example 2 was conducted.
Example of detection
Three pieces of cotton cloth of 10X 10cm finished in examples 1 to 3 were cut out, respectively, and subjected to an antibacterial test, and an untreated cloth sample of the same size was taken as a blank.
Under aseptic operation, inoculating staphylococcus aureus, klebsiella pneumoniae and hemolytic streptococcus strains, sampling for several times at intervals, and calculating the bacteriostasis rate according to the viable count principle. Wherein, the bacteriostasis rate = (average colony number of blank case-average colony number of example or comparative example)/average colony number of blank case x 100%), the specific data are as follows: (wherein, the unit% of the inhibitory rate, in addition, 3 groups of data in each column are the inhibitory rates of Staphylococcus aureus, Klebsiella pneumoniae and Streptococcus hemolyticus, respectively)
From the table above, it can be seen that the cotton fabric treated by the functional graphene loaded with the turmeric extract has a strong inhibiting effect on staphylococcus aureus, klebsiella pneumoniae and hemolytic streptococcus, is close to the sterilization effect of medical alcohol, and has a sterilization durability far higher than that of alcohol. Although examples 1 to 3 showed similar or slightly inferior experimental effects to comparative example 1, the consumption of the turmeric extract during actual use was only about 2.7% of that of comparative example.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
Claims (9)
1. A preparation method of functional graphene loaded with turmeric extract is characterized by comprising the following steps:
step 1, preparation of graphene oxide
Slowly adding a mixture of graphite powder and sodium nitrate into concentrated sulfuric acid under the conditions of ice bath and stirring, continuously stirring for 2-5 min, then adding potassium permanganate powder, fully stirring until the temperature is stabilized to normal temperature, heating to 40-45 ℃, continuously stirring for 30-45 min, then slowly adding deionized water, diluting to 8-10 times of the original volume by using ionized water, then adding a certain amount of hydrogen peroxide solution, filtering, cleaning a filter cake by using a hydrochloric acid solution, and finally drying a target product;
step 2, preparation of sulfonated graphene
Adding graphene oxide into water, forming a uniform dispersion liquid under the action of ultrasonic waves, adjusting the pH of the solution to 9-10 by using sodium carbonate, adding hydrazine hydrate, refluxing for 1-2 h at 80-100 ℃, cooling, filtering, washing a filter cake by using deionized water, drying to obtain proper black graphene powder, mixing the black graphene powder suspension and a diazonium salt solution, reacting for 2-5 h, filtering, washing the filter cake by using deionized water, and drying to obtain sulfonated graphene;
step 3, preparation of functionalized graphene
Adding sulfonated graphene and methyl-B-cyclodextrin into water, forming uniform dispersion liquid under the action of ultrasonic waves, then adding ammonia water, reacting for 8-12 h at 70-90 ℃, cooling, centrifuging, washing a filter cake with deionized water, and drying to obtain black functionalized graphene powder;
step 4, preparing functional graphene loaded with turmeric extract
Adding the functionalized graphene powder into a turmeric extract solution with the concentration of 0.01-0.05 mol/L, reacting for 30-60 min under ultrasonic-assisted reaction, then performing centrifugal separation, collecting a lower-layer precipitate, washing the precipitate with deionized water, and drying to obtain a target product.
2. The method for preparing turmeric extract-loaded functionalized graphene according to claim 1, wherein the diazonium salt solution is prepared as follows:
under the ice bath condition, sodium sulfanilate and sodium nitrite are respectively dissolved in an aqueous solution of hydrochloric acid, then a sodium nitrite aqueous solution is slowly added into the sodium nitrite solution, the reaction is carried out for 1-2 hours under the ice bath condition, a diazonium salt solution is obtained, and finally, redundant sodium nitrite is removed through urea.
3. The method for preparing turmeric extract-loaded functionalized graphene according to claim 1, wherein the turmeric root extract solution contains xanthorrhizol as an active ingredient, and the structural formula of the turmeric root extract solution is as follows:
4. the method for preparing turmeric extract-loaded functionalized graphene according to claim 1, wherein the extraction process of the xanthorrhizol is as follows:
step 1, processing, namely cleaning a certain amount of turmeric, crushing, adding acid for hydrolysis, and performing centrifugal treatment to separate solid hydrolysate;
step 2, extracting, namely performing reflux extraction by taking ethyl acetate as an extracting agent, wherein the volume mass ratio of the extracting agent to the solid hydrolysate is (2-5) to 1 during extraction, and extracting for 2-4 hours; then adjusting the pH value of the purified solution to 8-9 by ammonia water; taking the supernatant and ethyl acetate as an extractant, and performing reflux extraction to obtain a turmeric root extracting solution;
step 3, separating, namely concentrating the turmeric root extract to 1/3-1/2 of the original volume, performing silica gel column chromatography, eluting for 3-5 hours by using No. 6 gasoline and chloroform in a volume ratio of (40-50): 1 as a solvent, and collecting a xanthogen diol crude crystal at 230nm by using an ultraviolet detector according to a peak;
and 4, purifying, dissolving the xanthorrhizol crude crystals with ethanol solutions respectively, filtering, concentrating the filtrate to 4-6 times of the weight of the crude crystals, standing, cooling, evaporating, recrystallizing and drying to obtain the xanthorrhizol crystals.
5. The preparation method of the turmeric extract-loaded functionalized graphene according to claim 3, wherein 200-300 mesh silica gel is adopted for silica gel column chromatography, ethanol is adopted for column washing after elution is completed, and the column chromatography silica gel column can be reused for 2-5 times.
6. The method for preparing turmeric extract-loaded functionalized graphene according to claim 1, wherein the turmeric extract solution is prepared by: the preparation method comprises the steps of taking sodium dodecyl benzene sulfonate and tween-80 in a mass ratio of 2:1 as an emulsifier, and emulsifying curcumol, xanthogen diol or a mixture of the curcumol and the xanthogen diol into emulsion with the concentration of 8-10% by weight.
7. An antibacterial material obtained by the method for preparing the turmeric extract-loaded functionalized graphene according to any one of claims 1 to 6.
8. The application of the antibacterial material obtained by the preparation method of the turmeric extract-loaded functionalized graphene in the preparation of finishing materials or as a finishing material component is characterized in that the use method comprises the following steps:
step 1, adding functional graphene loaded with turmeric extract, a penetrating agent JFC and a dispersing agent NNO into water, and forming uniform dispersion liquid under the action of ultrasonic waves;
step 2, placing the cotton fabric in an aqueous solution of sodium carbonate and sodium aminobenzenesulfonate, boiling for 15-30 min, and then washing and drying for later use;
step 3, mixing cotton fabric and the functional graphene dispersion liquid loaded with the curcuma extract according to a bath ratio of (40-50): 1, placing the mixture in an infrared dyeing machine, dyeing the fabric with the functional graphene loaded with the curcuma extract under a preset condition, taking out the cotton fabric after finishing, removing redundant moisture through a padder, and finally drying the cotton fabric at 50-60 ℃;
and 4, immersing the fabric into a sodium hydrosulfite aqueous solution, stirring for 5-10 min, washing twice, and naturally drying to obtain the facing material.
9. The application of the antibacterial material prepared by the preparation method of the turmeric extract-loaded functionalized graphene as claimed in claim 8 as a facing material or as a facing material component is characterized in that the preset conditions are as follows: heating to 75-80 ℃ according to the heating rate of 2-3 ℃/min, adding sodium chloride and a leveling agent, heating to 110-130 ℃ according to the heating rate of 0.8-1.2 ℃/min, preserving heat for 30-45 min, and finally cooling to room temperature.
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| CN112411209A (en) * | 2020-10-29 | 2021-02-26 | 山东魏桥特宽幅印染有限公司 | Preparation method of color graphene fabric |
| CN117735537A (en) * | 2023-02-19 | 2024-03-22 | 烯源科技无锡有限公司 | Preparation method of high-dispersity graphene |
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| CN112411209A (en) * | 2020-10-29 | 2021-02-26 | 山东魏桥特宽幅印染有限公司 | Preparation method of color graphene fabric |
| CN117735537A (en) * | 2023-02-19 | 2024-03-22 | 烯源科技无锡有限公司 | Preparation method of high-dispersity graphene |
| CN117735537B (en) * | 2023-02-19 | 2024-05-17 | 烯源科技无锡有限公司 | Preparation method of high-dispersity graphene |
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