CN114342940A - Preparation method of novel nano composite antibacterial material - Google Patents
Preparation method of novel nano composite antibacterial material Download PDFInfo
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- CN114342940A CN114342940A CN202210084263.XA CN202210084263A CN114342940A CN 114342940 A CN114342940 A CN 114342940A CN 202210084263 A CN202210084263 A CN 202210084263A CN 114342940 A CN114342940 A CN 114342940A
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- Prior art keywords
- pyrithione
- standing
- nano composite
- attapulgite
- antibacterial material
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
Abstract
The invention discloses a preparation method of a novel nano composite antibacterial material, which comprises the steps of S1, preparing a sodium pyrithione aqueous solution with a certain concentration; s2, dispersing a certain amount of attapulgite in the aqueous solution of sodium pyrithione, stirring and mixing, and standing the mixed solution for 30min after stirring; s3, separating the solution after standing, dispersing the solid obtained by separation again by using clear water, standing again after dispersion, filtering and separating again after standing for 30 min; s4, washing off the free sodium pyrithione on the surface after separation; s5, drying the obtained composite material at 60-120 ℃. According to the preparation method of the novel nano composite antibacterial material, metal ions such as Mg, Zn and Al in the attapulgite are utilized to carry out in-situ compounding with the pyrithione copper salt, so that the using amount of metal salts is reduced, the nanostructure of the attapulgite can be used for obtaining the pyrithione salt with the nanostructure, and the broad spectrum and the bactericidal effect of sterilization are improved.
Description
Technical Field
The invention relates to the technical field related to preparation of antibacterial materials, in particular to a preparation method of a novel nano composite antibacterial material.
Background
The attapulgite clay is a clay mineral containing attapulgite as main component. Attapulgite is a crystalline hydrated magnesium aluminum silicate mineral, has unique layer chain structure characteristics, has lattice displacement in the structure, and contains variable amount of crystalNa+、Ca2+、Mg2+、Fe3+、Al3+The crystal is needle-shaped, fibrous or fiber-aggregated, and the attapulgite has the shape of a nanorod crystal, the length of the attapulgite is 1-5 mu m, and the diameter of the attapulgite is 20-70 nm; the pyrithione compound has mildew-proof and corrosion-proof effects, comprises N-oxidation-2-mercaptopyridine (PT) and salts thereof, and is widely researched by PT, N-oxidation-2-mercaptopyridine sodium salt (sodium pyrithione, SPT for short), N-oxidation-2-mercaptopyridine zinc salt (zinc pyrithione, ZPT for short) and N-oxidation-2-mercaptopyridine copper salt (copper pyrithione, CPT for short), and the products are widely used in the fields of daily chemical industry, medicines, plastics, coatings, pesticides and the like; in general, zinc pyrithione, magnesium pyrithione, and the like are prepared by replacing sodium pyrithione with ZnSO4, MgCl2, and then obtaining pyrithione salt powder with a suitable particle size distribution by means of a jet mill, a ball mill, an air classification mill, and the like, which has some problems:
as mentioned above, the general bactericide needs to use a large amount of metal salt, and the prepared bactericide has an insufficient broad-spectrum effect, cannot be well used in various places, and is inconvenient.
Disclosure of Invention
The invention aims to provide a preparation method of a novel nano composite antibacterial material, which aims to achieve the aim of utilizing the metal ion structure in attapulgite to carry out in-situ composite with pyrithione (or sodium pyrithione) in the background technology, not only reducing the using amount of metal salt, but also obtaining the nano composite bactericide which takes the attapulgite as a matrix and has wider spectrum effect by means of the nano structure of the attapulgite.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a novel nano composite antibacterial material comprises the following steps:
s1, firstly, preparing a sodium pyrithione aqueous solution with a certain concentration;
s2, dispersing a certain amount of attapulgite in the aqueous solution of sodium pyrithione, stirring and mixing, and standing the mixed solution for 30min after stirring;
s3, separating the solution after standing, dispersing the solid obtained by separation again by using clear water, standing again after dispersion, filtering and separating again after standing for 30 min;
s4, washing off the free sodium pyrithione on the surface after separation;
s5, drying the obtained composite material at 60-120 ℃;
and S6, drying to obtain the nano composite bacteriostatic agent taking the attapulgite as the matrix.
In a preferred embodiment of the present invention, the aqueous solution of sodium pyrithione with a certain concentration prepared in step S1 is replaced by a dimethylsulfoxide solution of pyrithione with a certain concentration, and the pyrithione with a certain concentration is washed away in step S4.
By adopting the technical scheme, different preparation options can be provided, so that the preparation method of the nano composite bacteriostatic agent can be wider.
As a preferred embodiment of the present invention, the step S3 is repeated 2 to 4 times.
By adopting the technical scheme, the step S3 is repeated for 2-4 times, so that the free sodium pyrithione or pyrithione on the surface can be cleaned, and the using effect of the nano composite bacteriostatic agent is improved.
In a preferred embodiment of the present invention, the drying process at step S5 takes 24 hours at 60 ℃ and 6 hours at 120 ℃.
By adopting the technical scheme, the composite material can be uniformly dried for a long time by drying at 60 ℃ for 24 hours, and the manufacturing efficiency can be improved by drying at 120 ℃ for 6 hours, so that the material is rapidly dried.
Compared with the prior art, the invention has the beneficial effects that: the preparation method of the novel nano composite antibacterial material comprises the following steps:
the metal ions such as Mg, Zn, Al and the like in the attapulgite are utilized to carry out in-situ compounding with the pyridine sulfur copper sodium salt, so that the using amount of the metal salt is reduced, the pyridine sulfur copper salt with the nano structure can be obtained by means of the nano structure of the attapulgite, and the broad spectrum property and the sterilization effect of sterilization are improved.
Drawings
FIG. 1 is a comparison diagram of bacteriostatic effect data of the structured nano composite bacteriostatic agent of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a novel nano composite antibacterial material comprises the following steps:
example 1
S1, firstly, preparing a sodium pyrithione aqueous solution with a certain concentration;
s2, dispersing a certain amount of attapulgite in the aqueous solution of sodium pyrithione, stirring and mixing, and standing the mixed solution for 30min after stirring;
s3, separating the solution after standing, dispersing the solid obtained by separation again by using clear water, standing again for dispersion, performing suction filtration and separation after standing for 30min, and repeating for 2 times;
s4, washing off the free sodium pyrithione on the surface after separation;
s5, drying the obtained composite material at 60 ℃ for 24 hours;
and S6, drying to obtain the nano composite bacteriostatic agent taking the attapulgite as the matrix.
Example 2
S1, firstly, preparing a dimethyl sulfoxide solution of pyrithione with a certain concentration;
s2, dispersing a certain amount of attapulgite in the aqueous solution of sodium pyrithione, stirring and mixing, and standing the mixed solution for 30min after stirring;
s3, separating the solution after standing, dispersing the solid obtained by separation again by using clear water, standing again for dispersion, performing suction filtration and separation after standing for 30min, and repeating for 4 times;
s4, washing away the free pyrithione on the surface after separation;
s5, drying the obtained composite material at 120 ℃ for 6 hours;
and S6, drying to obtain the nano composite bacteriostatic agent taking the attapulgite as the matrix.
The aqueous solution of sodium pyrithione with a certain concentration prepared in step S1 of example 1 can be replaced by the dimethylsulfoxide solution of pyrithione with a certain concentration of example 2, and step S4 is followed by replacing the cleaned material, so that different preparation options can be provided, thereby enabling the preparation method of the nano-composite bacteriostatic agent to be more extensive.
And step S3 in examples 1 and 2 needs to be repeated for 2-4 times, and step S3 is repeated for 2-4 times, so that the surface free sodium pyrithione or pyrithione can be cleaned, and the using effect of the nano composite bacteriostatic agent is improved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A preparation method of a novel nano composite antibacterial material is characterized by comprising the following steps:
s1, firstly, preparing a sodium pyrithione aqueous solution with a certain concentration;
s2, dispersing a certain amount of attapulgite in the aqueous solution of sodium pyrithione, stirring and mixing, and standing the mixed solution for 30min after stirring;
s3, separating the solution after standing, dispersing the solid obtained by separation again by using clear water, standing again after dispersion, filtering and separating again after standing for 30 min;
s4, washing off the free sodium pyrithione on the surface after separation;
s5, drying the obtained composite material at 60-120 ℃;
and S6, drying to obtain the nano composite bacteriostatic agent taking the attapulgite as the matrix.
2. The method for preparing a novel nano composite antibacterial material according to claim 1, characterized in that: the aqueous solution of sodium pyrithione with a certain concentration prepared in step S1 may be replaced with a dimethylsulfoxide solution of pyrithione with a certain concentration, and the step S4 washes away the pyrithione with a certain concentration.
3. The method for preparing a novel nano composite antibacterial material according to claim 1, characterized in that: the step S3 is repeated 2-4 times.
4. The method for preparing a novel nano composite antibacterial material according to claim 1, characterized in that: the step S5 takes 24 hours for the drying process at 60 ℃ and 6 hours for the drying process at 120 ℃.
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| CN202210084263.XA CN114342940A (en) | 2022-01-25 | 2022-01-25 | Preparation method of novel nano composite antibacterial material |
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| CN202210084263.XA CN114342940A (en) | 2022-01-25 | 2022-01-25 | Preparation method of novel nano composite antibacterial material |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1171207A (en) * | 1997-06-30 | 1999-03-16 | Kanae Toryo Kk | Production of ceramic including metal pyrithione |
| JP2001232215A (en) * | 2000-02-25 | 2001-08-28 | Nippon Soda Co Ltd | Photocatalyst carrying structure having antibacterial and antifungal effect |
| CN1461365A (en) * | 2000-09-01 | 2003-12-10 | 上海兰格科技发展有限公司 | Nano silver long-acting broad-spectrum antibacterial and anti-mildew granules and its preparation method |
| JP2007223917A (en) * | 2006-02-21 | 2007-09-06 | Nippon Chem Ind Co Ltd | Antimicrobial agent |
| CN101300981A (en) * | 2008-05-15 | 2008-11-12 | 兰州大学 | Nano silver-carrying concave-convex stick anti-bacteria agent and preparation thereof |
| CN103392698A (en) * | 2013-07-24 | 2013-11-20 | 广东泰宝医疗科技股份有限公司 | Attapulgite material with anti-bacterial function and preparation method thereof |
-
2022
- 2022-01-25 CN CN202210084263.XA patent/CN114342940A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1171207A (en) * | 1997-06-30 | 1999-03-16 | Kanae Toryo Kk | Production of ceramic including metal pyrithione |
| JP2001232215A (en) * | 2000-02-25 | 2001-08-28 | Nippon Soda Co Ltd | Photocatalyst carrying structure having antibacterial and antifungal effect |
| CN1461365A (en) * | 2000-09-01 | 2003-12-10 | 上海兰格科技发展有限公司 | Nano silver long-acting broad-spectrum antibacterial and anti-mildew granules and its preparation method |
| JP2007223917A (en) * | 2006-02-21 | 2007-09-06 | Nippon Chem Ind Co Ltd | Antimicrobial agent |
| CN101300981A (en) * | 2008-05-15 | 2008-11-12 | 兰州大学 | Nano silver-carrying concave-convex stick anti-bacteria agent and preparation thereof |
| CN103392698A (en) * | 2013-07-24 | 2013-11-20 | 广东泰宝医疗科技股份有限公司 | Attapulgite material with anti-bacterial function and preparation method thereof |
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