CN108719329B - Composite material based on melamine cyanurate hydrogen bond self-assembly structure and preparation method and application thereof - Google Patents
Composite material based on melamine cyanurate hydrogen bond self-assembly structure and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a composite material based on a melamine cyanuric acid hydrogen bond self-assembly structure, a preparation method and application thereof. According to the invention, the composite material based on the melamine cyanuric acid hydrogen bond self-assembly structure is obtained by mixing the melamine aqueous solution, the metal salt solution and the cyanuric acid aqueous solution, and stirring for reaction. In the preparation method provided by the invention, the prepared chemical substances melamine capable of generating self-assembly behavior and cyanuric acid aqueous solution are mixed, the two molecules are assembled together through hydrogen bond acting force, and metal salt ions are adsorbed on the surface of the metal salt ions, so that the obtained metal ion or metal oxide composite material based on the hydrogen bond self-assembly structure has good antibacterial effect. The material has mild and simple synthesis conditions and low raw material price, and is easy to be commercially developed. The composite material based on the melamine cyanurate hydrogen bond self-assembly structure can also be applied to the antibiosis in various fields such as environmental protection, building, medicine and the like, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of self-assembly synthesis, in particular to a composite material based on a melamine cyanuric acid hydrogen bond self-assembly structure, a preparation method and application.
Background
Microorganisms are a collective term for all microorganisms that are difficult to observe by the naked eye, and are an important component of the natural ecosystem. Among microorganisms in nature, most of them are harmless to humans, some are beneficial to humans, and only a few of them can cause diseases of humans. However, the harm caused by the few microorganisms is not negligible. Pathogenic microorganisms can rapidly propagate at proper temperature and nutrients, so that the phenomena of deterioration, putrefaction, mildew, wound suppuration and infection and the like of substances are caused, and the health of human beings is seriously threatened. In recent years, microbial disaster events frequently occur, and huge economic loss and social harm are caused. And pathogenic microorganisms are continuously mutated in the transmission process, the drug resistance of the pathogenic microorganisms is stronger and stronger, and the sterilization effect of the traditional antibacterial agent is reduced. Therefore, in order to effectively and reasonably prevent antibiotics from being abused, an excellent functional antibacterial material is required in daily life.
The metal ion loaded antibacterial material is a common antibacterial material and has certain killing and inhibiting effects on most bacteria. However, because the synthesis process of the carrier is complex and the cost is high, most of the metal ion loaded antibacterial materials are difficult to meet the requirements of industrial production.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a composite material based on a melamine cyanuric acid hydrogen bond self-assembly structure.
The invention also aims to provide the composite material based on the melamine cyanurate hydrogen bond self-assembly structure, which is obtained by the preparation method.
The invention further aims to provide application of the composite material based on the melamine cyanurate hydrogen bond self-assembled structure.
The purpose of the invention is realized by the following technical scheme: a preparation method of a composite material based on a melamine cyanurate hydrogen bond self-assembly structure comprises the following steps: and mixing the melamine aqueous solution, the metal salt solution and the cyanuric acid aqueous solution, and stirring for reaction to obtain the composite material based on the melamine cyanuric acid hydrogen bond self-assembly structure.
The metal salt is preferably at least one of copper salt, silver salt, gold salt, platinum salt, iron salt, nickel salt, palladium salt and cobalt salt.
The copper salt is preferably at least one of copper sulfate, copper chloride, copper acetate and copper nitrate.
The silver salt is preferably at least one of silver nitrate and silver citrate.
The gold salt is preferably gold chloride or chloroauric acid.
The platinum salt is preferably platinum chloride.
The palladium salt is preferably at least one of palladium chloride and palladium nitrate.
The ferric salt is preferably at least one of ferric chloride, ferric nitrate, ferrous chloride and ferric sulfate.
The cobalt salt is preferably at least one of cobalt chloride and cobalt nitrate.
The nickel salt is preferably at least one of nickel nitrate and nickel chloride.
The concentration of the metal salt solution is preferably 0.0001-1000mmol/L, specifically 0.0001mmol/L, 0.0005mmol/L, 0.001mmol/L, 0.005mmol/L, 0.01mmol/L, 0.05mmol/L, 0.1mmol/L, 0.5mmol/L, 1mmol/L, 5mmol/L, 10mmol/L, 50mmol/L, 100mmol/L, 500mmol/L, 1000 mmol/L; more preferably 5 to 10 mmol/L.
The concentration of the melamine aqueous solution is preferably 0.01-50mmol/L, and specifically can be 0.01mmol/L, 0.05mmol/L, 0.1mmol/L, 0.5mmol/L, 1mmol/L, 5mmol/L, 10mmol/L, 20mmol/L, 30mmol/L, 40mmol/L, 50 mmol/L; more preferably 5 to 10 mmol/L.
The concentration of the cyanuric acid aqueous solution is preferably 0.01-50mmol/L, and specifically can be 0.01mmol/L, 0.05mmol/L, 0.1mmol/L, 0.5mmol/L, 1mmol/L, 5mmol/L, 10mmol/L, 20mmol/L, 30mmol/L, 40mmol/L and 50 mmol/L; more preferably 5 to 10 mmol/L.
The melamine and the cyanuric acid are preferably mixed according to the molar ratio of 1: 1.
The metal salt and the melamine are preferably mixed according to the molar ratio of 1-10: 100.
The stirring reaction time is preferably 0.1-48h, and specifically can be 0.1h, 0.5h, 1h, 5h, 10h, 15h, 20h, 25h, 30h, 35h, 40h and 48 h; more preferably 1 to 24 hours.
The temperature of the stirring reaction is preferably 0-100 ℃, and specifically can be 0 ℃, 10 ℃, 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ and 100 ℃; more preferably 10 to 80 ℃; most preferably 20 to 80 ℃.
A composite material based on a melamine cyanurate hydrogen bond self-assembly structure is obtained by the preparation method.
The composite material based on the melamine cyanurate hydrogen bond self-assembly structure is applied to the antibacterial field.
Compared with the prior art, the invention has the following advantages and effects:
in the preparation method provided by the invention, the prepared chemical substances melamine capable of generating self-assembly behavior and cyanuric acid aqueous solution are mixed, the two molecules are assembled together through hydrogen bond acting force, and metal salt ions are adsorbed on the surface of the metal salt ions, so that the obtained metal ion or metal oxide composite material based on the hydrogen bond self-assembly structure has good antibacterial effect. The material has mild and simple synthesis conditions and low raw material price, and is easy to be commercially developed. The composite material based on the melamine cyanurate hydrogen bond self-assembly structure can also be applied to the antibiosis in various fields such as environmental protection, building, medicine and the like, and has wide application prospect.
Drawings
FIG. 1 is a graph showing the inhibitory effect on Staphylococcus aureus in a qualitative test of a composite material based on a melamine cyanurate hydrogen bond self-assembled structure prepared in example 1; in which panel A is a blank group and panel B is a test group.
FIG. 2 is a graph showing the effect of inhibiting Escherichia coli in a qualitative test of the composite material based on the hydrogen bond self-assembled structure of melamine cyanurate prepared in example 1; in which panel A is a blank group and panel B is a test group.
FIG. 3 is a graph showing the inhibitory effect on Staphylococcus aureus in the quantitative test of the composite material based on the hydrogen bond self-assembled structure of melamine cyanurate prepared in example 1; in which panel A is a blank group and panel B is a test group.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The Staphylococcus aureus used was Staphylococcus aureus ATCC6538 standard strain, Kyoto Cyclochey Microscience and technology, Inc.
Coli used was the E.coli 55989/EAEC E.coli strain, Biovector Co., LTD.
Example 1
(1) Preparation of silver-containing composite material based on melamine cyanuric acid hydrogen bond self-assembly structure
Mixing 100mL of melamine (10mmol/L) aqueous solution and 100mL of cyanuric acid (10mmol/L) aqueous solution, adding 1mL of silver nitrate (100mmol/L), stirring at normal temperature for 1 hour, carrying out solid-liquid separation, and drying to obtain the silver-containing composite material based on the melamine cyanuric acid hydrogen bond self-assembly structure.
(2) Detection of bacteriostatic effects
1) Research on qualitative antibacterial performance of material
Staphylococcus aureus and Escherichia coli are respectively selected as gram-positive bacteria and gram-negative bacteria as research objects. The appropriate amount of sterilized LB agar medium was poured into the sterilized petri dish and allowed to solidify. Taking the known concentration (about 10)10CFU/mL) onto the solidified solid medium, and repeatedly spreading the bacterial suspension on the surface of the agar with a spreader to uniformly distribute the bacterial suspension on the surface of the solid medium. Weighing 1mg of the silver-containing composite material based on the melamine cyanurate hydrogen bond self-assembled structure prepared in the step (1) of the embodiment, placing the silver-containing composite material in the center of a flat plate, simultaneously setting a control group without the silver-containing composite material, and performing inverted culture at 37 +/-1 ℃ for 24 h. As a result, as shown in FIGS. 1 and 2, the surface of the LB plate was covered with the bacteria of the control group, and the composite material was placed on the surface of the LB plate to form a zone of inhibition around the composite material. Therefore, the silver-containing composite material based on the melamine cyanuric acid hydrogen bond self-assembly structure has good effect of inhibiting staphylococcus aureus and escherichia coli.
2) Research on quantitative antibacterial performance of material
The melamine cyanurate based hydrogen bonding prepared in example 1 was reacted with10mg of the silver-containing composite material of the assembled structure was ultrasonically dispersed in 100mL of sterile water to obtain solution A. 1mL of solution A was added to a 49mL suspension of Staphylococcus aureus (about 10)8CFU/mL) to obtain a sample solution of a test group. At the same time, a blank set of samples, 1mL of sterile water, was added to a suspension containing 49mL of Staphylococcus aureus (about 10)8CFU/mL). Fixing the triangular flask containing the sample solution of the test group and the sample solution of the blank group on a shaking table of a constant-temperature shaking incubator, and carrying out shaking culture at the temperature of 37 +/-1 ℃ at the speed of 150r/min for 24 h. Then, a certain amount of culture solution is taken to coat a sterilized LB plate, and inverted culture is carried out for 24h at 37 +/-1 ℃. As shown in fig. 3, a colony grows on an LB plate from a blank sample solution, and a sterile colony is generated from a test sample solution, and it can be seen that 2mg/L of the silver-containing composite material based on the melamine cyanurate hydrogen bond self-assembled structure prepared in example 1 can inhibit bacteria by 100%;
10mg of the silver-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure prepared in example 1 was ultrasonically dispersed in 100mL of sterile water to obtain solution B. 1mL of the above solution was added to 49mL of E.coli suspension (about 10)8CFU/mL) to obtain a sample solution of a test group. At the same time, a blank sample solution, i.e., 1mL of sterile water, was added to 49mL of E.coli suspension (about 10)8CFU/mL). Fixing the triangular flask containing the sample solution of the test group and the sample solution of the blank group on a shaking table of a constant-temperature shaking incubator, and carrying out shaking culture at the temperature of 37 +/-1 ℃ at the speed of 150r/min for 24 h. Then, a certain amount of culture solution is taken to coat a sterilized LB plate, and inverted culture is carried out for 24h at 37 +/-1 ℃. The result shows that 2mg/L of the silver-containing composite material based on the melamine cyanurate hydrogen bond self-assembled structure prepared in the example 1 can inhibit bacteria by 100%;
example 2
(1) Preparation of copper-containing composite material based on melamine cyanurate hydrogen bond self-assembly structure
Mixing 100mL of melamine (10mmol/L) aqueous solution and 100mL of cyanuric acid (10mmol/L) aqueous solution, adding 1mL of copper nitrate (10mmol/L), stirring at normal temperature for 2 hours, carrying out solid-liquid separation, and drying to obtain the copper-containing composite material based on the melamine cyanuric acid hydrogen bond self-assembly structure.
(2) Detection of bacteriostatic effects
1) Research on qualitative antibacterial performance of material
Staphylococcus aureus and Escherichia coli are respectively selected as gram-positive bacteria and gram-negative bacteria as research objects. The appropriate amount of sterilized LB agar medium was poured into the sterilized petri dish and allowed to solidify. Taking the known concentration (about 10)10CFU/mL) onto the solidified solid medium, and repeatedly spreading the bacterial suspension on the surface of the agar with a spreader to uniformly distribute the bacterial suspension on the surface of the solid medium. Weighing 1mg of the copper-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure prepared in the step (1) of the embodiment, placing the copper-containing composite material in the center of a flat plate, setting a control group without the copper-containing composite material, and performing inverted culture at 37 +/-1 ℃ for 24 hours. The results showed that the bacteria of the control group spread over the surface of the LB plate, and the composite was placed in the plate, forming a zone of inhibition around the composite. Therefore, the copper-containing composite material based on the melamine cyanuric acid hydrogen bond self-assembly structure has good effect of inhibiting staphylococcus aureus and escherichia coli.
2) Research on quantitative antibacterial performance of material
10mg of the copper-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure prepared in example 2 was ultrasonically dispersed in 100mL of sterile water to obtain solution A. 1mL of solution A was added to a 49mL suspension of Staphylococcus aureus (about 10)8CFU/mL) to obtain a sample solution of a test group. At the same time, a blank set of samples, 1mL of sterile water, was added to a suspension containing 49mL of Staphylococcus aureus (about 10)8CFU/mL). Fixing the triangular flask containing the sample solution of the test group and the sample solution of the blank group on a shaking table of a constant-temperature shaking incubator, and carrying out shaking culture at the temperature of 37 +/-1 ℃ at the speed of 150r/min for 24 h. Then, a certain amount of culture solution is taken to coat a sterilized LB plate, and inverted culture is carried out for 24h at 37 +/-1 ℃. The result shows that 2mg/L of the copper-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure prepared in the example 2 can inhibit bacteria by 100%.
The preparation of example 2 based on trimerization10mg of the copper-containing composite material with the cyanamide cyanuric acid hydrogen bond self-assembly structure is taken and ultrasonically dispersed in 100mL of sterile water to obtain a solution B. 1mL of solution B was added to 49mL of E.coli suspension (about 10)8CFU/mL) to obtain a sample solution of a test group. At the same time, a blank sample solution, i.e., 1mL of sterile water, was added to 49mL of E.coli suspension (about 10)8CFU/mL). Fixing the triangular flask containing the sample solution of the test group and the sample solution of the blank group on a shaking table of a constant-temperature shaking incubator, and carrying out shaking culture at the temperature of 37 +/-1 ℃ at the speed of 150r/min for 24 h. Then, a certain amount of culture solution is taken to coat a sterilized LB plate, and inverted culture is carried out for 24h at 37 +/-1 ℃. The result shows that 2mg/L of the copper-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure prepared in the example 2 can inhibit bacteria by 100%.
Example 3
(1) Preparation of iron-containing composite material based on melamine cyanurate hydrogen bond self-assembly structure
Mixing 100mL of melamine (10mmol/L) aqueous solution and 100mL of cyanuric acid (10mmol/L) aqueous solution, adding 1mL of ferric chloride (100mmol/L), stirring at normal temperature for 24 hours, carrying out solid-liquid separation, and drying to obtain the iron-containing composite material based on the melamine cyanuric acid hydrogen bond self-assembly structure.
(2) Detection of bacteriostatic effects
1) Research on qualitative antibacterial performance of material
Staphylococcus aureus and Escherichia coli are respectively selected as gram-positive bacteria and gram-negative bacteria as research objects. An appropriate amount of sterilized agar medium was poured into the sterilized petri dish and allowed to solidify. Taking the known concentration (about 10)10CFU/mL) onto the solidified solid medium, and repeatedly spreading the bacterial suspension on the surface of the agar with a spreader to uniformly distribute the bacterial suspension on the surface of the solid medium. Weighing 1mg of the iron-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure prepared in the step (1) of the embodiment, placing the iron-containing composite material in the center of a flat plate, setting a control group without the iron-containing composite material, and performing inverted culture at 37 +/-1 ℃ for 24 h. The results showed that the control group of bacteria were spread on the surface of the LB plate, and the composite material was placed on the surface of the LB plateAnd forming a bacteriostatic circle around the material. Therefore, the iron-containing composite material has good effect of inhibiting staphylococcus aureus and escherichia coli.
2) Research on quantitative antibacterial performance of material
100mg of the iron-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure prepared in example 3 was ultrasonically dispersed in 100mL of sterile water to obtain solution a. 1mL of solution A was added to a 49mL suspension of Staphylococcus aureus (about 10)8CFU/mL) to obtain a sample solution of a test group. At the same time, a blank set of samples, 1mL of sterile water, was added to a suspension containing 49mL of Staphylococcus aureus (about 10)8CFU/mL). Fixing the triangular flask containing the sample solution of the test group and the sample solution of the blank group on a shaking table of a constant-temperature shaking incubator, and carrying out shaking culture at the temperature of 37 +/-1 ℃ at the speed of 150r/min for 24 h. Then, a certain amount of culture solution is taken to coat a sterilized LB plate, and inverted culture is carried out for 24h at 37 +/-1 ℃. The result shows that 20mg/L of the iron-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure prepared in the example 3 can inhibit bacteria by 100%.
100mg of the iron-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure prepared in example 3 was ultrasonically dispersed in 100mL of sterile water to obtain solution B. 1mL of solution B was added to 49mL of E.coli suspension (about 10)8CFU/mL) to obtain a sample solution of a test group. At the same time, a blank sample solution, i.e., 1mL of sterile water, was added to 49mL of E.coli suspension (about 10)8CFU/mL). Fixing the triangular flask containing the sample solution of the test group and the sample solution of the blank group on a shaking table of a constant-temperature shaking incubator, and carrying out shaking culture at the temperature of 37 +/-1 ℃ at the speed of 150r/min for 24 h. Then, a certain amount of culture solution is taken to coat a sterilized LB plate, and inverted culture is carried out for 24h at 37 +/-1 ℃. The result shows that 20mg/L of the iron-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure prepared in the example 3 can inhibit bacteria by 100%.
Example 4
100mL of melamine (5mmol/L) aqueous solution and 100mL of cyanuric acid (5mmol/L) aqueous solution are mixed, 1mL of copper nitrate (5mmol/L) is added, and the mixture is stirred for 2 hours in a temperature control device at 80 ℃ to obtain copper-containing composite material suspension (solution No. 1) based on a melamine cyanuric acid hydrogen bond self-assembly structure.
100mL of melamine (5mmol/L) aqueous solution and 100mL of cyanuric acid (5mmol/L) aqueous solution are mixed, 1mL of water is added, and the mixture is stirred for 2 hours in a temperature control device at 80 ℃ to obtain suspension (liquid No. 2) of the melamine cyanuric acid hydrogen bond self-assembly material.
1mL of copper nitrate (5mmol/L) was added to 200mL of the aqueous solution, and the mixture was stirred in a temperature-controlled apparatus at 80 ℃ for 2 hours to obtain a copper oxide-containing nanoparticle solution (solution No. 3).
1mL of copper nitrate (5mmol/L) was added to 200mL of the aqueous solution to obtain an aqueous solution containing copper ions (solution No. 4).
Staphylococcus aureus (ATCC6538 standard strain, Kyoto Loop Microbiol. Co., Ltd.) and Escherichia coli (55989/EAEC Escherichia coli strain, Biovector Co., LTD) were selected as gram-positive bacteria and gram-negative bacteria, respectively, as the subjects of study. 1mL of solutions No. 1, 2, 3 and 4 were each transferred and ultrasonically dispersed in 100mL of sterile water to obtain solution A, B, C, D. 1mL of solution A, B, C, D was added to a 49mL suspension of Staphylococcus aureus (about 10)8CFU/mL) to obtain a sample solution of a test group. At the same time, a blank set of samples, 1mL of sterile water, was added to a suspension containing 49mL of Staphylococcus aureus (about 10)8CFU/mL). Fixing the triangular flask containing the sample solution of the test group and the sample solution of the blank group on a shaking table of a constant-temperature shaking incubator, and carrying out shaking culture at the temperature of 37 +/-1 ℃ at the speed of 150r/min for 24 h. Then, the same amount of culture solution was applied to sterilized LB plates, and inverted cultured at 37. + -. 1 ℃ for 24 hours, and 5 replicates were set. As a result, the number of colonies was found to be larger in the case of liquid No. 2 > liquid No. 3 > liquid No. 4 > liquid No. 1, and no colonies were observed on the plate coated with liquid No. 1. The result shows that the suspension (No. 2 liquid) of the melamine cyanuric acid hydrogen bond self-assembly material has no antibacterial property; the antibacterial property of the copper-containing composite material suspension (solution No. 1) based on the melamine cyanuric acid hydrogen bond self-assembly structure is obviously higher than that of a copper oxide-containing nanoparticle solution (solution No. 3) and a copper ion-containing aqueous solution (solution No. 4).
Therefore, the antibacterial performance of the copper-containing composite material based on the melamine cyanurate hydrogen bond self-assembly structure comes from the synergistic effect of the melamine cyanurate hydrogen bond self-assembly material and copper ions or copper nanoparticles. The inventors speculate that the stability of copper loading in melamine cyanurate is greatly enhanced, thereby facilitating the maintenance of its antibacterial properties.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A preparation method of a composite material based on a melamine cyanurate hydrogen bond self-assembly structure is characterized by comprising the following steps: the method comprises the following steps: mixing a melamine aqueous solution, a metal salt solution and a cyanuric acid aqueous solution, and stirring for reaction to obtain a composite material based on a melamine cyanuric acid hydrogen bond self-assembly structure;
the metal salt is copper salt; the temperature of the stirring reaction is 80 ℃.
2. The method for preparing the composite material based on the melamine cyanurate hydrogen bond self-assembled structure as recited in claim 1, wherein:
the copper salt is at least one of copper sulfate, copper chloride, copper acetate and copper nitrate.
3. The method for preparing the composite material based on the melamine cyanurate hydrogen bond self-assembled structure as recited in claim 1, wherein:
the concentration of the metal salt solution is 0.0001-1000 mmol/L;
the concentration of the melamine aqueous solution is 0.01-50 mmol/L;
the concentration of the cyanuric acid aqueous solution is 0.01-50 mmol/L.
4. The method for preparing the composite material based on the melamine cyanurate hydrogen bond self-assembled structure as recited in claim 3, wherein:
the concentration of the metal salt is 5-10 mmol/L;
the concentration of the melamine is 5-10 mmol/L;
the concentration of the cyanuric acid aqueous solution is 5-10 mmol/L.
5. The method for preparing the composite material based on the melamine cyanurate hydrogen bond self-assembled structure as recited in claim 1, wherein: the melamine and the cyanuric acid are mixed according to the molar ratio of 1: 1.
6. The method for preparing the composite material based on the melamine cyanurate hydrogen bond self-assembled structure as recited in claim 1, wherein: the metal salt and the melamine are mixed according to the molar ratio of 1-10: 100.
7. The method for preparing the composite material based on the melamine cyanurate hydrogen bond self-assembled structure as recited in claim 1, wherein:
the stirring reaction time is 0.1-48 h.
8. The utility model provides a combined material based on melamine cyanuric acid hydrogen bond self-assembly structure which characterized in that: obtained by the preparation method of any one of claims 1 to 7.
9. The use of the composite material based on melamine cyanurate hydrogen bond self-assembled structure as recited in claim 8 in the antibacterial field.
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