CN114703658A - europium-SA nano aggregate cross-linked fluorescent sensing fabric, method and application - Google Patents
europium-SA nano aggregate cross-linked fluorescent sensing fabric, method and application Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 16
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- 229940005550 sodium alginate Drugs 0.000 claims abstract description 73
- 239000000661 sodium alginate Substances 0.000 claims abstract description 73
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 71
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 71
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 12
- 238000010382 chemical cross-linking Methods 0.000 claims abstract description 3
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 3
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 58
- 229910052693 Europium Inorganic materials 0.000 claims description 30
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 28
- TXBBUSUXYMIVOS-UHFFFAOYSA-N thenoyltrifluoroacetone Chemical compound FC(F)(F)C(=O)CC(=O)C1=CC=CS1 TXBBUSUXYMIVOS-UHFFFAOYSA-N 0.000 claims description 23
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 20
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 14
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- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical group [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims description 13
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- 238000012986 modification Methods 0.000 claims description 12
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- PUVAFTRIIUSGLK-UHFFFAOYSA-M trimethyl(oxiran-2-ylmethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1CO1 PUVAFTRIIUSGLK-UHFFFAOYSA-M 0.000 claims description 2
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 claims description 2
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- LTVDFSLWFKLJDQ-UHFFFAOYSA-N α-tocopherolquinone Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(C)(O)CCC1=C(C)C(=O)C(C)=C(C)C1=O LTVDFSLWFKLJDQ-UHFFFAOYSA-N 0.000 description 6
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/13—Alginic acid or derivatives thereof
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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Abstract
The invention discloses a europium-SA nano aggregate cross-linked fluorescence sensing fabric, a method and application thereof. Preparing a fluorescent nano aggregate, and then finishing the sodium alginate nano aggregate on the surface of the treated cotton fabric by utilizing a chemical cross-linking agent through the covalent bond combination effect to obtain the wearable fluorescent cotton fabric; sterilizing the fluorescent cotton fabric for 30 minutes under ultraviolet rays, and co-culturing the fluorescent cotton fabric with escherichia coli and staphylococcus aureus for 18 hours to observe an obvious inhibition zone and a fluorescence quenching phenomenon; preparing various metal ion solutions, respectively dripping different amounts of the metal ion solutions on fluorescent cotton fabrics with uniform cutting sizes, and observing that part of transition metal ions have obvious fluorescence quenching effect on the fluorescent cotton fabrics. The fluorescent cotton fabric prepared by the invention has high fluorescence intensity, high sensitivity to bacteria and metal ions and no toxicity, and is a novel wearable fluorescent sensor integrating antibacterial and sensing functions.
Description
Technical Field
The invention relates to the technical field of fluorescent sensing fabrics, in particular to a europium-SA nano aggregate cross-linked fluorescent sensing fabric, a method and application thereof.
Background
The nano silver has special properties of surface effect, small-size effect, quantum size effect, macroscopic quantum tunneling effect and the like, and is widely applied to the fields of antibacterial and deodorizing materials, antistatic materials, nonlinear optical materials and the like. It is currently believed that AgNPs attach to cell walls and membranes, and intracellular biomolecular and structural damage caused by AgNPs and silver ions, and AgNPs and silver ion-induced oxidative stress are involved in the antibacterial action of AgNPs, either alone or in combination. The antibacterial mechanism of the nano silver enables the antibacterial effect to have broad spectrum and durability. However, the antibacterial activity of the silver nanoparticles is significantly influenced by physicochemical properties such as surface chemistry, size, shape and the like, particularly, the high surface energy of the silver nanoparticles can cause agglomeration among the particles, so that the dispersibility is poor, and the dispersibility of the silver nanoparticles can be improved by modifying or coating the silver nanoparticles with a hydrophilic polymer.
After the rare earth ions and the ligand with high light absorption coefficient form a rare earth complex, strong characteristic fluorescence of the rare earth ions can be emitted. Among rare earth ions, Eu3+Under the excitation of 365nm ultraviolet light, visible red characteristic fluorescence is emitted, and the fluorescence intensity is increased along with the coordination of the organic ligand. Europium ions are widely used in fluorescence sensing. However, the coordination of europium ion and organic ligand makes it insoluble in water medium and incompatible with biological environment, and limits its in-situ generationApplication in the field of things.
Sodium Alginate (SA) is one of natural polysaccharides, and the molecules of the Sodium Alginate (SA) are formed by alternately connecting beta-D-mannuronic acid (M unit) and alpha-L-guluronic acid (G unit) according to 1, 4-glycosidic bonds to form a block linear polymer. The molecular chain of the SA has rich carboxyl and hydroxyl, can generate coordination with polyvalent metal ions, has the characteristics of hydrophilicity, biocompatibility, biodegradability and the like, has rich SA resources and low cost, and has great application value in the fields of food, textile, biotechnology, medical engineering and the like.
Disclosure of Invention
The invention aims to provide a europium-SA nano-aggregate crosslinked fluorescent sensing fabric, a method and application. The silver nitrate solution with positive electricity and the europium complex with positive electricity are coated into nano aggregate particles by utilizing sodium alginate with negative charge, and the nano aggregate particles are arranged on the surface of the cotton fabric through a crosslinking effect. The prepared cotton fabric can be co-cultured with escherichia coli and staphylococcus aureus to observe an obvious inhibition zone and a fluorescence quenching phenomenon, and can also be observed after being contacted with a certain amount of metal ions.
A preparation method of europium-sodium alginate nano-aggregates and a fluorescent sensing fabric, (1) preparation of fluorescent nano-aggregates: mixing a sodium alginate solution with a silver nitrate solution, and carrying out oil bath reaction for a certain time to obtain small-sized nano silver particles; preparing an europium complex solution, adding the europium complex solution into a sodium alginate solution containing nano-silver, and fully stirring and reacting for 2-4h to obtain europium-induced sodium alginate nano-aggregates; (2) preparing a wearable fluorescent sensing cotton fabric: the method comprises the following steps of firstly, desizing (10g/L NaOH, 1g/L JFC penetrant, bath ratio of 1: 50) and surface cation modification treatment of cotton fabric, heating a chemical cross-linking agent (15g/L PER +1g/L JFC penetrant, bath ratio of 1: 50) to 60-90 ℃, treating the cotton fabric for 1-4 hours, then adding the prepared sodium alginate nano aggregate into the solution, continuing heating treatment, taking out the cotton fabric, carrying out desizing on the cotton fabric by using an air pressure electric padder, and drying to obtain the fluorescent cotton fabric.
The preparation method controls the concentration of the sodium alginate to be 1mg/mL-5mg/mL and the concentration of the silver nitrateThe concentration is controlled to be 0.01-0.5mol/L, and the pH value of the sodium alginate is adjusted to be 7-8 by 1mol/L NaOH before the sodium alginate is mixed with silver nitrate; the dosage ratio of the sodium alginate to the silver nitrate and europium complex is 0.05-0.25 mol: 10-6-5×10-5mol：9×10-8-1.8×10-5mol。
The preparation method comprises the step of slowly dripping the silver nitrate solution into the sodium alginate solution at the stirring speed of 500-800rpm, wherein the temperature of the mixing reaction is 60-90 ℃, and the time is 30-90 min.
The preparation method uses europium nitrate (Eu (NO) as europium complex3)3) The preparation method comprises the following steps of (1) dissolving, 2-thenoyltrifluoroacetone (TTA) solution and 1, 10-phenanthroline (Phen) solution in a molar ratio of 1: 3: 1 or 1: 1: 1 or no Phen, in a europium nitrate: TTA ═ 1: 3 or europium nitrate: TTA ═ 1: 1, control c (Eu)3+)＝0.0001-0.02mol/L。
In the preparation method, the europium complex is slowly dripped into the sodium alginate solution containing the nano-silver at the stirring speed of 800-1200rpm, and then the stirring is continued for 2-4 hours.
According to the preparation method, the used cationic modifier is one of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride (CHPTAC), 2, 3-epoxypropyl trimethyl ammonium chloride (GTA) and methacryloyloxyethyl trimethyl ammonium chloride (DMC), and the bath ratio of the cotton fabric to the cationic modification liquid is 1: 20-50, and the concentration of the prepared modified liquid is 50-80 g/L.
The preparation method is characterized in that the time for treating the fabric by the sodium alginate nano aggregate is 1-4 hours.
The preparation method is characterized in that the air pressure for treating the cotton fabric by the pneumatic mini-padder is 0.2-0.5Mpa, and the rotating speed is 2.5-5 m/min.
The preparation method comprises the steps of firstly drying the processed cotton fabric in an oven at 80 ℃ for 5-15min and then drying the cotton fabric in an oven at 140-180 ℃ for 2-3 min.
The wearable strong-fluorescence cotton fabric prepared by any method.
After the fluorescent cotton fabric is co-cultured with escherichia coli and staphylococcus aureus for 18-24 hours, an obvious inhibition zone and a fluorescent cotton fabric fluorescence quenching phenomenon can be observed. Therefore, the fluorescent cotton fabric has an antibacterial effect, and can detect existence of escherichia coli and staphylococcus aureus.
Preparing various metal ion solutions, respectively dropwise adding the metal ion solutions with different amounts to the fluorescent cotton fabric with uniform cutting size, and observing that part of transition metal ions have obvious fluorescence quenching effect on the fluorescent cotton fabric, which indicates that the fluorescent cotton fabric has the function of sensing the metal ions.
Drawings
FIG. 1 is a TEM image of EISAs.
FIG. 2 is a fluorescence spectrum of EISAs
FIG. 3 shows the inhibition zone generated after the cotton fabric treated by SA and EISAs and staphylococcus aureus are co-cultured for 18 hours, and the fluorescence emission spectra of the fabric before and after co-culture.
FIG. 4 shows fluorescent cotton fabric and different molar amounts of Ni metal+The change spectrogram of fluorescence intensity after contact is shown in the graph with the fluorescence intensity and Ni+Linear dependence of usage.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
(1) Sodium hydroxide is weighed to prepare 10mL of 1mol/L sodium hydroxide solution for standby. Weighing silver nitrate to prepare 10mL0.1mol/L silver nitrate solution for later use. Weighing sodium alginate, adding into distilled water to prepare 9mL of 1mg/mL sodium alginate solution, and standing for one hour after the sodium alginate is completely dissolved under magnetic stirring. Putting a sodium alginate solution into a round-bottom flask, dropwise adding 1mol/L NaOH solution to adjust the pH value to be 7-8, preheating in 70 ℃ oil bath, measuring 100 mu L of silver nitrate solution, dropwise adding the silver nitrate solution into the sodium alginate solution under the stirring condition, and reacting in 70 ℃ oil bath for 1h to obtain the nano-silver solution.
(2) According to the proportion of europium nitrate: TTA: phen ═ 1: 3: 1, the medicines are weighed according to the proportion and are sequentially added into an absolute ethyl alcohol solution, the concentration of europium ions is 0.01mol/L, and the mixture is fully stirred and reacts for 2 hours to obtain Eu (TTA)3Phen. Taking 900 μ L Eu (TTA)3Phen is slowly added dropwise toAnd fully stirring the obtained nano silver solution for 2 hours at the rotating speed of 800r/min to obtain the europium-induced sodium alginate nano aggregate EISAs solution.
FIG. 1 is a TEM image of EISAs, which shows that EISAs are regular spheres and have an average particle size of 66.86 nm.
FIG. 2 is a fluorescence spectrum of EISAs, and the obtained nanoagglomerates show characteristic fluorescence of europium ion at 612 nm.
(3) Preparing 50mL of 10g/L NaOH solution, adding 0.05g of JFC solution (keeping the JFC concentration at 1g/L), uniformly stirring, heating to 80 ℃ for later use, soaking 1g of cotton fabric in the solution for boiling, and keeping for 30min, wherein the bath ratio is 1: 50, washing twice with hot water at the temperature of 80-90 ℃, washing twice with warm water at the temperature of 50-60 ℃, finally completely washing the cotton cloth with room-temperature water to be neutral, taking out the treated cotton cloth and drying in an oven at the temperature of 80 ℃ to obtain desized cotton cloth.
Cation modification treatment: the desized cotton cloth was immersed in 20mL CHPTAC (60g/L) solution heated to 70 ℃ at a bath ratio of 1: 20, soaking for 10min, adding NaOH (15g/L), and continuously maintaining the temperature for 50 min. Taking out after 50min, washing with cold water to neutrality, and drying to obtain cotton fabric subjected to cationic modification.
Preparing 50mL of 15g/L pentaerythritol solution, adding a JFC penetrating agent (with the final concentration of 1g/L) to prepare a finishing liquid, uniformly stirring, and immersing the cotton fabric subjected to cationic modification treatment in the finishing liquid, wherein the bath ratio is 1: 50, heated to 80 ℃ for 1 hour. Adding 30mL of EISAs solution prepared in the step (1) into 20mL of finishing liquid soaked with cotton fabrics, and controlling the bath ratio to be 1: and 50, continuously reacting for 4 hours at 80 ℃, taking out the cotton fabric after 4 hours, treating the cotton fabric by using a pneumatic electric padder, wherein the air pressure is 0.2Mpa, the rotating speed is 3m/min, then drying the cotton fabric for 5min at 80 ℃, and drying the cotton fabric for 2min at 180 ℃ to obtain the fluorescent cotton fabric.
Example 2
Compared with the embodiment 1, the concentration of the sodium alginate is increased, and a bacteriostasis test and metal ion detection are carried out.
(1) Sodium hydroxide is weighed to prepare 10mL of 1mol/L sodium hydroxide solution for standby. Weighing silver nitrate to prepare 10mL0.1mol/L silver nitrate solution for later use. Preparing 9mL of 3mg/mL sodium alginate solution, weighing the sodium alginate, adding the sodium alginate into distilled water, stirring by magnetic force to completely dissolve the sodium alginate, and standing for one hour for later use. Putting a sodium alginate solution into a round-bottom flask, dropwise adding 1mol/L NaOH solution to adjust the pH value to be 7-8, preheating in 70 ℃ oil bath, measuring 100 mu L of silver nitrate solution, dropwise adding the silver nitrate solution into the sodium alginate solution under the stirring condition, and reacting in 70 ℃ oil bath for 1 h.
(2) According to the proportion of europium nitrate: TTA: phen ═ 1: 3: 1, the medicines are weighed according to the proportion and are sequentially added into an absolute ethyl alcohol solution, the concentration of europium ions is 0.01mol/L, and the mixture is fully stirred and reacts for 2 hours to obtain Eu (TTA)3Phen. Taking 900 μ L Eu (TTA)3Phen is slowly dripped into the prepared nano silver solution, and is fully stirred for 2 hours at the rotating speed of 800r/min, so as to prepare the europium-induced sodium alginate nano-aggregate EISAs solution.
(3) Preparing 50mL of 10g/L NaOH solution, adding 0.05g of JFC solution (keeping the JFC concentration at 1g/L), uniformly stirring, heating to 80 ℃ for later use, soaking 1g of cotton fabric into the solution, boiling, and keeping for 30min, wherein the bath ratio is 1: 50, washing twice with hot water at the temperature of 80-90 ℃, washing twice with warm water at the temperature of 50-60 ℃, finally completely washing the cotton cloth to be neutral with room temperature water, taking out the treated cotton cloth and drying in an oven at the temperature of 80 ℃ for later use.
The desized cotton was immersed in 20mL CHPTAC (60g/L) solution heated to 80 ℃ at a bath ratio of 1: 20, soaking for 10min, adding NaOH (15g/L), and continuously maintaining the temperature for 50 min. Taking out after 50min, washing with cold water to neutrality, and oven drying for use.
Preparing 50mL of 15g/L pentaerythritol solution, adding a JFC penetrating agent (with the final concentration of 1g/L) to prepare a finishing liquid, uniformly stirring, and immersing the cotton fabric subjected to cationic modification treatment in the finishing liquid, wherein the bath ratio is 1: 50, heated to 80 ℃ for 1 hour. Adding 30mL of EISAs solution prepared in the step (1) into 20mL of finishing liquid soaked with cotton fabrics, and controlling the bath ratio to be 1: and 50, continuously reacting for 4 hours at the temperature of 80 ℃, taking out the cotton fabric after 4 hours, treating the cotton fabric by using a pneumatic electric padder at the rotating speed of 3m/min under the pressure of 0.2Mpa, then drying the cotton fabric for 5 minutes at the temperature of 80 ℃, and drying the cotton fabric for 2 minutes at the temperature of 180 ℃ to obtain the fluorescent cotton fabric.
(4) Preparing the cotton fabric grafted with SA according to the steps, cutting the cotton fabric treated by SA and EISAs into round pieces with the diameter of 1cm, putting the round pieces into a disposable culture dish, and sterilizing the two sides of the round pieces by irradiation under an ultraviolet lamp for 30 min. 100. mu.L of Staphylococcus aureus (ATCC29213) solution was aspirated and uniformly spread on LB solid medium. The sample was picked up with sterile forceps and placed on the surface of the medium and gently pressed with forceps to make full contact, and the dish was placed in a constant temperature incubator at 37 ℃ for 18 h. After the culture is finished, taking out the culture medium, taking a picture by using a common camera, and measuring and recording the size of the inhibition zone by using a cross method.
(5) Mixing NiCl3·6H2O10 ml of 0.1mol/L aqueous solution is prepared for standby. Cutting the prepared fluorescent cotton fabric into 1.5cm by 1.5cm square fluorescent cotton fabric for later use, respectively taking metal ion solutions with different volumes by using a pipette gun and dropwise adding the metal ion solutions onto the cotton fabric, and testing the fluorescence change of the fluorescent cotton fabric by using a full-spectrum microspectrophotometer.
FIG. 3 shows the inhibition zone generated after the cotton fabric treated by SA and EISAs and staphylococcus aureus are co-cultured for 18 hours, and the fluorescence emission spectra of the fabric before and after co-culture. Test results show that no inhibition zone (a) is generated after the SA-treated cotton fabric and staphylococcus aureus are co-cultured, which indicates that sodium alginate has no inhibition effect on staphylococcus aureus. After the cotton fabric treated by EISAs and staphylococcus aureus are cultured together for 18 hours, an 8mm antibacterial ring (b) is generated, which shows that the fluorescent cotton fabric has an obvious antibacterial effect on staphylococcus aureus. As can be seen from the fluorescence spectrum, the fluorescent cotton fabric has a strong characteristic fluorescence emission peak at 612nm, but after the fluorescent cotton fabric is co-cultured with staphylococcus aureus, the fluorescence is quenched (c), namely the staphylococcus aureus has an obvious 'on-off' effect on the fluorescence of the fluorescent cotton fabric, and whether the fluorescent cotton fabric is polluted by the staphylococcus aureus can be judged through the point.
FIG. 4 shows fluorescent cotton fabric and different molar amounts of Ni metal+The change spectrogram of fluorescence intensity after contact is shown in the graph with the fluorescence intensity and Ni+Linear dependence of usage. The fluorescence intensity of the cotton fabric can be seen along with Ni+Is increased and decreased, indicating fluorescent cotton fabricTo Ni+Has obvious fluorescent sensing effect on Ni+Has a detection limit of 40 μ M and Ni+The fluorescent intensity influence on the cotton fabric follows a certain linear function relationship, and the fitting variance is R2＝0.9768。
Example 3
Compared to example 1, the cationic modifier was replaced.
(1) Sodium hydroxide is weighed to prepare 10mL of 1mol/L sodium hydroxide solution for standby. Weighing silver nitrate to prepare 10mL0.1mol/L silver nitrate solution for later use. Preparing 9mL of 1mg/mL sodium alginate solution, weighing the sodium alginate, adding the sodium alginate into distilled water, stirring by magnetic force to completely dissolve the sodium alginate, and standing for one hour for later use. Putting a sodium alginate solution into a round-bottom flask, dropwise adding 1mol/L NaOH solution to adjust the pH value to be 7-8, preheating in 70 ℃ oil bath, measuring 100 mu L of silver nitrate solution, dropwise adding the silver nitrate solution into the sodium alginate solution under the stirring condition, and reacting in 70 ℃ oil bath for 1 h.
(2) According to the proportion of europium nitrate: TTA: phen ═ 1: 3: 1, the medicines are weighed according to the proportion and are sequentially added into an absolute ethyl alcohol solution, the concentration of europium ions is 0.01mol/L, and the mixture is fully stirred and reacts for 2 hours to obtain Eu (TTA)3Phen. Taking 900 μ L Eu (TTA)3Phen is slowly dripped into the prepared nano silver solution, and is fully stirred for 2 hours at the rotating speed of 800r/min, so that the europium-induced sodium alginate nano-aggregate is prepared.
(3) Preparing 50mL of 10g/L NaOH solution, adding 0.05g of JFC solution (keeping the JFC concentration at 1g/L), uniformly stirring, heating to 80 ℃ for later use, soaking 1g of cotton fabric into the solution, boiling, and keeping for 30min, wherein the bath ratio is 1: 50, washing twice with hot water at the temperature of 80-90 ℃, washing twice with warm water at the temperature of 50-60 ℃, finally completely washing the cotton cloth with room-temperature water to be neutral, taking out the treated cotton cloth and drying in an oven at the temperature of 80 ℃ for later use. The desized cotton cloth was immersed in 20mL of a mixed solution of GTA (60g/L) and NaOH (6g/L) heated to 90 ℃ at a bath ratio of 1: 20, the temperature is maintained for 30 min. Taking out after 30min, washing with cold water to neutrality, and oven drying for use. Preparing 50mL of 15g/L pentaerythritol solution, adding a JFC penetrating agent (with the final concentration of 1g/L) to prepare a finishing liquid, uniformly stirring, and immersing the cotton fabric subjected to cationic modification treatment in the finishing liquid, wherein the bath ratio is 1: 50, heated to 80 ℃ for 1 hour. Adding 30mL of EISAs solution prepared in the step (1) into 20mL of finishing liquid soaked with cotton fabrics, and controlling the bath ratio to be 1: and 50, continuously reacting for 4 hours at 80 ℃, taking out the cotton fabric after 4 hours, treating the cotton fabric by using a pneumatic electric padder, wherein the air pressure is 0.2Mpa, the rotating speed is 3m/min, then drying the cotton fabric for 5min at 80 ℃, and drying the cotton fabric for 2min at 180 ℃ to obtain the fluorescent cotton fabric.
Example 4
Compared with example 1, the preparation ratio of the europium complex is changed, and the europium nitrate: TTA: phen ═ 1: 3: 1, changing into europium nitrate: TTA: phen ═ 1: 1: 1.
(1) sodium hydroxide is weighed to prepare 10mL of 1mol/L sodium hydroxide solution for standby. Weighing silver nitrate to prepare 10mL0.1mol/L silver nitrate solution for later use. Preparing 9mL of 1mg/mL sodium alginate solution, weighing the sodium alginate, adding the sodium alginate into distilled water, stirring by magnetic force to completely dissolve the sodium alginate, and standing for one hour for later use. Putting a sodium alginate solution into a round-bottom flask, dropwise adding 1mol/L NaOH solution to adjust the pH value to be 7-8, preheating in 70 ℃ oil bath, measuring 100 mu L of silver nitrate solution, dropwise adding the silver nitrate solution into the sodium alginate solution under the stirring condition, and reacting in 70 ℃ oil bath for 1 h.
(2) According to the proportion of europium nitrate: TTA: phen ═ 1: 1: 1, the medicines are weighed according to the proportion and are sequentially added into an absolute ethyl alcohol solution, the concentration of europium ions is 0.01mol/L, and the mixture is fully stirred and reacts for 2 hours to obtain Eu (TTA)3Phen. Taking 900 μ L Eu (TTA)3Phen is slowly dripped into the prepared nano silver solution, and is fully stirred for 2 hours at the rotating speed of 800r/min, so that the europium-induced sodium alginate nano-aggregate is prepared.
(3) Preparing 50mL of 10g/L NaOH solution, adding 0.05g of JFC solution (keeping the JFC concentration at 1g/L), uniformly stirring, heating to 80 ℃ for later use, soaking 1g of cotton fabric into the solution, boiling, and keeping for 30min, wherein the bath ratio is 1: 50, washing twice with hot water at the temperature of 80-90 ℃, washing twice with warm water at the temperature of 50-60 ℃, finally completely washing the cotton cloth with room-temperature water to be neutral, taking out the treated cotton cloth and drying in an oven at the temperature of 80 ℃ for later use. The desized cotton cloth was immersed in 20mL of CHPTAC (60g/L) solution heated to 60-80 ℃ at a bath ratio of 1: 20, soaking for 10min, adding NaOH (15g/L), and continuously keeping the temperature for 50 min. Taking out after 50min, washing with cold water to neutrality, and oven drying for use. 50mL of 15g/L pentaerythritol solution is added with a JFC penetrating agent (with the final concentration of 1g/L) to prepare a finishing liquid, the finishing liquid is uniformly stirred, and the cotton fabric subjected to cationic modification treatment is immersed in the finishing liquid, wherein the bath ratio is 1: 50, heated to 80 ℃ for 1 hour. Adding 30mL of EISAs solution prepared in the step (1) into 20mL of finishing liquid soaked with cotton fabrics, and controlling the bath ratio to be 1: and 50, continuously reacting for 4 hours at 80 ℃, taking out the cotton fabric after 4 hours, treating the cotton fabric by using a pneumatic electric padder, wherein the air pressure is 0.2Mpa, the rotating speed is 3m/min, then drying the cotton fabric for 5min at 80 ℃, and drying the cotton fabric for 2min at 180 ℃ to obtain the fluorescent cotton fabric.
Example 5
The configuration procedure of the europium complex reduces the use of the ligand Phen compared to example 4.
(1) Sodium hydroxide is weighed to prepare 10mL of 1mol/L sodium hydroxide solution for standby. Weighing silver nitrate to prepare 10mL0.1mol/L silver nitrate solution for later use. Preparing 9mL of 1mg/mL sodium alginate solution, weighing the sodium alginate, adding the sodium alginate into distilled water, stirring by magnetic force to completely dissolve the sodium alginate, and standing for one hour for later use. Putting a sodium alginate solution into a round-bottom flask, dropwise adding 1mol/L NaOH solution to adjust the pH value to be 7-8, preheating in 70 ℃ oil bath, measuring 100 mu L of silver nitrate solution, dropwise adding the silver nitrate solution into the sodium alginate solution under the stirring condition, and carrying out oil bath reaction at 90 ℃ for 30.
(2) According to the proportion of europium nitrate: TTA ═ 1: 1, adding the medicines into an absolute ethanol solution in sequence, wherein the concentration of europium ions is 0.01mol/L, and fully stirring for reacting for 2 hours to obtain the europium complex. And slowly dripping 900 mu L of europium complex into the prepared nano silver solution, and fully stirring at the rotating speed of 800r/min for 4 hours to prepare the europium-induced sodium alginate nano aggregate.
(3) Preparing 50mL of 10g/L NaOH solution, adding 0.05g of JFC solution (keeping the JFC concentration at 1g/L), uniformly stirring, heating to 80 ℃ for later use, soaking 1g of cotton fabric into the solution, boiling, and keeping for 30min, wherein the bath ratio is 1: 50, washing twice with hot water at the temperature of 80-90 ℃, washing twice with warm water at the temperature of 50-60 ℃, finally completely washing the cotton cloth with room-temperature water to be neutral, taking out the treated cotton cloth and drying in an oven at the temperature of 80 ℃ for later use. The desized cotton cloth was immersed in 20mL of CHPTAC (60g/L) solution heated to 60-80 ℃ at a bath ratio of 1: 20, soaking for 10min, adding NaOH (15g/L), and continuously keeping the temperature for 50 min. Taking out after 50min, washing with cold water to neutrality, and oven drying for use. 50mL of 15g/L pentaerythritol solution is added with a JFC penetrating agent (with the final concentration of 1g/L) to prepare a finishing liquid, the finishing liquid is uniformly stirred, and the cotton fabric subjected to cationic modification treatment is immersed in the finishing liquid, wherein the bath ratio is 1: 50, heated to 80 ℃ for 1 hour. Adding 30mL of EISAs solution prepared in the step (1) into 20mL of finishing liquid soaked with cotton fabrics, and controlling the bath ratio to be 1: and 50, continuously reacting for 4 hours at the temperature of 80 ℃, taking out the cotton fabric after 4 hours, treating the cotton fabric by using a pneumatic electric padder at the rotating speed of 3m/min under the pressure of 0.2Mpa, then drying the cotton fabric for 5 minutes at the temperature of 80 ℃, and drying the cotton fabric for 2 minutes at the temperature of 180 ℃ to obtain the fluorescent cotton fabric.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (10)
1. A preparation method of europium-sodium alginate nano-aggregates and a fluorescent sensing fabric is characterized by comprising the following steps: (1) preparation of fluorescent nano aggregates: mixing a sodium alginate solution with a silver nitrate solution, and performing oil bath reaction for a certain time to obtain small-sized nano silver particles; preparing a europium complex solution, adding the europium complex solution into a sodium alginate solution containing nano silver, and fully stirring for reaction for 2-4 hours to obtain europium-induced sodium alginate nano aggregates; (2) preparing a wearable fluorescent sensing cotton fabric: the method comprises the steps of desizing and surface cationic modification of cotton fabrics, heating a chemical cross-linking agent to 60-90 ℃, treating the cotton fabrics for 1-4 hours, adding the prepared sodium alginate nano-aggregates into the solution, continuing heating, taking out the sodium alginate nano-aggregates, carrying out size rolling on the cotton fabrics by using an air pressure electric padder, and drying the cotton fabrics to obtain the fluorescent cotton fabrics.
2. The method of claim 1, wherein: the concentration of sodium alginate is controlled to be 1mg/mL-5mg/mL, the concentration of silver nitrate is controlled to be 0.01-0.5mol/L, and 1mo is used before mixing the sodium alginate and the silver nitrateAdjusting the pH value to 7-8 by using L/L NaOH; the dosage ratio of the sodium alginate to the silver nitrate and europium complex is 0.05-0.25 mol: 10-6-5×10- 5mol：9×10-8-1.8×10-5mol。
3. The method of claim 1, wherein: slowly dripping the silver nitrate solution into the sodium alginate solution at the stirring speed of 500 plus 800rpm, wherein the temperature of the mixing reaction is between 60 and 90 ℃, and the time is between 30 and 90 min.
4. The method of claim 1, wherein: europium complex is europium nitrate (Eu (NO)3)3) The solution, 2-thenoyltrifluoroacetone (TTA) solution and 1, 10-phenanthroline (Phen) solution according to a molar ratio of 1: 3: 1 or 1: 1: 1 or no Phen, in a europium nitrate: TTA ═ 1: 3 or europium nitrate: TTA ═ 1: 1, control c (Eu)3+)＝0.0001-0.02mol/L。
5. The method of making fluorescent nanoagglomerates of claim 2, wherein: the europium complex is slowly dripped into the sodium alginate solution containing the nano-silver at the stirring speed of 800-1200rpm, and then the stirring is continued for 2-4 hours.
6. The method of claim 1, wherein: the used cationic modifier is one of 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride (CHPTAC), 2, 3-epoxypropyl trimethyl ammonium chloride (GTA) and methacryloyloxyethyl trimethyl ammonium chloride (DMC), and the bath ratio of the cotton fabric to the cationic modifier is 1: 20-50, and the concentration of the prepared modified liquid is 50-80 g/L.
7. The method of claim 1, wherein: the time for treating the fabric with the sodium alginate nano-aggregates is 1-4 hours.
8. A wearable intense-fluorescence sensing fabric prepared according to any of the methods of claims 1-7.
9. The wearable intense fluorescence sensing fabric of claim 8 for use in antibacterium.
10. The use of the wearable intense fluorescence sensing fabric of claim 8 in metal ion sensing.
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