CN114794147A - Preparation method of antibacterial agent, composite material containing antibacterial agent and preparation method of composite material - Google Patents
Preparation method of antibacterial agent, composite material containing antibacterial agent and preparation method of composite material Download PDFInfo
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- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/06—Aluminium; Calcium; Magnesium; Compounds thereof
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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
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- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
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- C08L25/06—Polystyrene
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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Abstract
The invention discloses a preparation method of an antibacterial agent, a composite material containing the antibacterial agent and a preparation method of the composite material, wherein the preparation method of the antibacterial agent comprises the following steps: (1) adding magnesium nitrate, absolute ethyl alcohol, chitosan, sodium hydroxide and deionized water into a reaction vessel, and reacting at 50-70 ℃ for 10-16h to obtain a solution A; (2) filtering and washing the solution A, and drying in a vacuum drying oven to obtain a solid B; (3) and calcining the solid B in a muffle furnace, and cooling to obtain the MgO/chitosan type antibacterial agent. The magnesium nitrate is used as a magnesium source, the sodium borohydride is used as a reducing agent, a novel MgO/chitosan type antibacterial agent is synthesized, the antibacterial performance of the thermoplastic plastic can be improved by modifying the thermoplastic plastic with the MgO/chitosan type antibacterial agent, and the MgO/chitosan type antibacterial agent has great popularization significance.
Description
Technical Field
The invention relates to the technical field of antibacterial agents, and particularly relates to a preparation method of an antibacterial agent, a composite material containing the antibacterial agent and a preparation method of the composite material.
Background
An antimicrobial agent is a substance that effectively controls the growth of microorganisms or that can kill microorganisms directly. An agent which kills or inhibits the growth of pathogenic microorganisms without interfering with the normal growth of plants. Fungicides can be classified according to mode of action, source of raw material and chemical composition. Internationally, they are generally referred to as agents for controlling various types of pathogenic microorganisms. Along with the development of bactericides, virucides, algicides and other subclasses are distinguished.
The metal element antibacterial agent is metal and compounds thereof, mainly contains Ag, Cu, Zn and other elements, wherein the antibacterial property of Ag is about 1000 times that of Zn. These metals or their compounds are combined with inorganic porous carrier minerals such as zeolite, glass, apatite, calcium phosphate, zirconium phosphate, etc. to synthesize antibacterial materials by ion exchange or adsorption, among which silver-based antibacterial agents have been widely used. In practical application, the inorganic antibacterial material adopts various inorganic metal complexing agents. There are patent reports AB 2 O 4 A composite antibacterial agent in the form of a coating on a porous honeycomb-shaped article, wherein A is a divalent metal ion of Mg, Zn, Mn, Ni, Co or Fe, B is a trivalent metal ion of Al, Cr, Mn or Fe, and O is an oxygen element, has excellent antibacterial properties.
However, no MgO/chitosan-type antibacterial agent has been reported so far.
Disclosure of Invention
The invention aims to provide a preparation method of an antibacterial agent, a composite material containing the antibacterial agent and a preparation method of the composite material.
The technical problem to be solved by the invention is realized by the following technical scheme:
a method for preparing an antibacterial agent comprising the steps of:
(1) adding magnesium nitrate, absolute ethyl alcohol, chitosan, sodium hydroxide and deionized water into a reaction vessel, and reacting at 50-70 ℃ for 10-16h to obtain a solution A;
(2) filtering and washing the solution A, and drying the solution A in a vacuum drying oven to obtain a solid B;
(3) and calcining the solid B in a muffle furnace, and cooling to obtain the MgO/chitosan type antibacterial agent.
Preferably, in the above technical scheme, the mass ratio of magnesium nitrate, absolute ethyl alcohol, chitosan, sodium hydroxide and deionized water in step (1) is (30-40): (50-60): (24-32): (18-24): (120-160).
Preferably, in the above technical solution, the drying conditions in step (2) are: drying in a vacuum drying oven at 70-90 deg.C for 10-16 h.
Preferably, in the above technical scheme, the calcination conditions in step (3) are as follows: calcining at 800-860 ℃ for 10-12 h.
An antibacterial agent prepared by the preparation method of the antibacterial agent.
A composite material comprises the following components in parts by weight: thermoplastic 96, and an antimicrobial agent 4 prepared according to the method of preparing the antimicrobial agent.
Preferably, in the above technical solution, the thermoplastic is Polyethylene (PE), polypropylene (PP), Polystyrene (PS), polybutylene terephthalate (PBT) or polyamide 6(PA 6).
A method of making a composite material comprising the steps of:
and mixing the antibacterial agent and the thermoplastic plastic in parts by weight, stirring for 10min by a high-speed mixer, adding into a double-screw extruder, and performing blending extrusion to obtain the composite material.
Preferably, in the above technical solution, the twin-screw extruder comprises six temperature zones arranged in sequence, the temperature of the first temperature zone is 230 ℃ C., the temperature of the second temperature zone is 260 ℃ C., the temperature of the third temperature zone is 260 ℃ C., the temperature of the fourth temperature zone is 260 ℃ C., the temperature of the fifth temperature zone is 260 ℃ C., the temperature of the sixth temperature zone is 260 ℃ C., the temperature of the head of the twin-screw extruder is 180 ℃ C., 260 ℃ C., and the screw rotation speed is 320r/min at 200 ℃ C. -.
The antibacterial mechanism of the synthesized MgO/chitosan type antibacterial agent is as follows:
on the one hand, when Mg ions come into contact with the microbial cell membrane having negative charges, the ions are tightly adsorbed on the cell membrane surface due to coulomb's force, resulting in coagulation of proteins and inactivation of enzyme activity, and thus cell division is inhibited, thereby causing death of bacteria. On the other hand, chitosan itself also has a certain antibacterial property. Thereby greatly improving the antibacterial rate.
Mg(NO3)2+2NaOH→2NaNO 3 +Mg(OH) 2 ；
Mg(OH) 2 →MgO+H 2 O。
The technical scheme of the invention has the following beneficial effects:
the application takes magnesium nitrate as a magnesium source and sodium borohydride as a reducing agent to synthesize a novel MgO/chitosan type antibacterial agent, and the antibacterial property of the thermoplastic plastic can be improved by modifying the thermoplastic plastic with the novel MgO/chitosan type antibacterial agent, so that the application has great popularization significance.
Detailed Description
Various exemplary embodiments of the present invention will now be described in detail. It should be noted that: the relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise.
The raw materials used in the examples of the invention are as follows:
magnesium nitrate, chemical Limited, Jinchuan, Jinan; absolute ethanol, hoja, suzhou, chemical ltd; chitosan, qingdao huizhi bioengineering ltd; sodium hydroxide, jingning cyanxing chemical ltd; deionized water, Shanghai Joint test chemical reagents, Inc.; PBT (model 2002U), Japan treaty; PP (model Z30S), mazineb petrochemical; PE (model 5070), brocade ethylene; PA6 (model CM1017), eastern japan; PS (model 350), taiwan george.
The test instrument used in the present invention is as follows:
model ZSK30 twin-screw extruder, W & P, Germany; JL-1000 type tensile testing machine, produced by Guangzhou Youcai laboratory instruments; HTL900-T-5B injection molding machine, manufactured by Haita plastics machinery, Inc.; XCJ-500 impact tester, manufactured by Chengde tester; QT-1196 tensile tester, Gaotai detection instruments, Inc. of Dongguan; QD-GJS-B12K model high-speed mixer, HengOde instruments, Beijing.
Example 1
Preparation example 1
A method for preparing an antibacterial agent comprising the steps of:
(1) 300g of magnesium nitrate (Mg (NO3)2), 500g of absolute ethyl alcohol, 240g of chitosan, 180g of sodium hydroxide and 1.2kg of deionized water are weighed and added into a reaction vessel to react for 10 hours at 50 ℃ to obtain a solution A.
(2) And filtering and washing the solution A, and placing the solution A in a vacuum drying oven at 70 ℃ for 10 hours to obtain a solid B.
(3) And (3) calcining the solid B in a muffle furnace at 800 ℃ for 10h, and cooling to obtain the MgO/chitosan type antibacterial agent P1.
Application example 1
A method of making a composite material comprising the steps of:
and adding 4 parts of P1 into 96 parts of PP, stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PP composite material X1.
The double-screw extruder comprises six temperature zones which are sequentially arranged, wherein the temperature of the first temperature zone is 200 ℃, the temperature of the second temperature zone is 230 ℃, the temperature of the third temperature zone is 230 ℃, the temperature of the fourth temperature zone is 230 ℃, the temperature of the fifth temperature zone is 230 ℃, the temperature of the sixth temperature zone is 230 ℃, the head temperature of the double-screw extruder is 230 ℃, and the screw rotating speed is 200 r/min.
Comparative example 1
And (3) taking 96 parts of PP, stirring for 10min by using a high-speed mixer, and then adding the PP into a double-screw extruder for blending and extruding to obtain the PP composite material D1.
The antibacterial performance data of the PP composite materials prepared in the application example 1 and the comparative example 1 are shown in the following table (table 1):
TABLE 1
As can be seen from the above table, X1 has better antibacterial property than D1, which indicates that the PP composite material has better antibacterial property after the antibacterial agent of the present application is added.
Example 2
Preparation example 2
A method for preparing an antibacterial agent comprising the steps of:
(1) 350g of magnesium nitrate (Mg (NO3)2), 550g of absolute ethyl alcohol, 280g of chitosan, 210g of sodium hydroxide and 1.4kg of deionized water are weighed and added into a reaction vessel to react for 13 hours at the temperature of 60 ℃ to obtain a solution A.
(2) And filtering and washing the solution A, and placing the solution A in a vacuum drying oven at 80 ℃ for 13h to obtain a solid B.
(3) And (3) calcining the solid B in a muffle furnace at 830 ℃ for 11h, and cooling to obtain the MgO/chitosan type antibacterial agent P2.
Application example 2
A method of making a composite material comprising the steps of:
adding 4 parts of P2 into 96 parts of polybutylene terephthalate (PBT), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PBT composite material X2.
The double-screw extruder comprises six temperature zones which are sequentially arranged, wherein the temperature of the first temperature zone is 200 ℃, the temperature of the second temperature zone is 260 ℃, the temperature of the third temperature zone is 260 ℃, the temperature of the fourth temperature zone is 260 ℃, the temperature of the fifth temperature zone is 260 ℃, the temperature of the sixth temperature zone is 260 ℃, the head temperature of the double-screw extruder is 260 ℃, and the screw rotating speed is 300 r/min.
Comparative example 2
And (3) taking 96 parts of PBT, stirring for 10min by using a high-speed mixer, and then adding the PBT into a double-screw extruder for blending and extruding to obtain the PBT composite material D2.
The antibacterial performance data of the PBT composite materials prepared in application example 2 and comparative example 2 are shown in the following table (table 2):
TABLE 2
As can be seen from the above table, X2 has better antibacterial property than D2, which shows that the antibacterial property of the PBT composite material is better after the antibacterial agent is added.
Example 3
Preparation example 3
(1) Weighing 400g of magnesium nitrate (Mg (NO3)2), 600g of absolute ethyl alcohol, 320g of chitosan, 240g of sodium hydroxide and 1.6kg of deionized water, adding into a reaction vessel, and reacting at 70 ℃ for 16h to obtain a solution A.
(2) And filtering and washing the solution A, and placing the solution A in a vacuum drying oven at 90 ℃ for 16 hours to obtain a solid B.
(3) And calcining the solid B in a muffle furnace at 860 ℃ for 12h, and cooling to obtain the MgO/chitosan type antibacterial agent P3.
Application example 3
A method of making a composite material comprising the steps of:
adding 4 parts of P3 into 96 parts of Polyethylene (PE), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PE composite material X3.
The double-screw extruder comprises six temperature zones which are sequentially arranged, wherein the temperature of the first temperature zone is 120 ℃, the temperature of the second temperature zone is 180 ℃, the temperature of the third temperature zone is 180 ℃, the temperature of the fourth temperature zone is 180 ℃, the temperature of the fifth temperature zone is 180 ℃, the temperature of the sixth temperature zone is 180 ℃, the head temperature of the double-screw extruder is 180 ℃, and the screw rotating speed is 300 r/min.
Comparative example 3
And (3) taking 96 parts of PE, stirring for 10min by using a high-speed mixer, and then adding the PE into a double-screw extruder for blending and extruding to obtain the PE composite material D3.
The antibacterial performance data of the PE composite prepared in the above application example 3 and comparative example 3 are shown in the following table (table 3):
TABLE 3
As can be seen from the above table, X3 is more antibacterial than D3, which indicates that the antibacterial performance of the PE composite material is better after the antibacterial agent of the invention is added.
Example 4
Preparation example 4
(1) 325g of magnesium nitrate (Mg (NO3)2), 555g of absolute ethyl alcohol, 295g of chitosan, 195g of sodium hydroxide and 1.45kg of deionized water are weighed and added into a reaction vessel to react for 12 hours at 55 ℃ to obtain a solution A.
(2) And filtering and washing the solution A, and placing the solution A in a vacuum drying oven at 75 ℃ for 15h to obtain a solid B.
(3) And calcining the solid B in a muffle furnace at 820 ℃ for 11h, and cooling to obtain the MgO/chitosan type antibacterial agent P4.
Application example 4
A method of making a composite material comprising the steps of:
adding 4 parts of P4 into 96 parts of polyamide 6(PA6), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PA6 composite material X4.
The double-screw extruder comprises six temperature zones which are sequentially arranged, wherein the temperature of the first temperature zone is 230 ℃, the temperature of the second temperature zone is 260 ℃, the temperature of the third temperature zone is 260 ℃, the temperature of the fourth temperature zone is 260 ℃, the temperature of the fifth temperature zone is 260 ℃, the temperature of the sixth temperature zone is 260 ℃, the head temperature of the double-screw extruder is 260 ℃, and the screw rotating speed is 320 r/min.
Comparative example 4
And (3) taking 96 parts of PA6, stirring for 10min by a high-speed mixer, and then adding the PA6 into a double-screw extruder for blending and extruding to obtain the PA6 composite material D4.
The antibacterial performance data of the PA6 composite materials prepared in application example 4 and comparative example 4 above are shown in the following table (table 4):
TABLE 4
As can be seen from the above table, X4 has better antibacterial property than D4, which shows that the antibacterial property of the PA6 composite material is better after the antibacterial agent of the invention is added.
Example 5
Preparation example 5
(1) 315g of magnesium nitrate (Mg (NO3)2), 525g of absolute ethyl alcohol, 285g of chitosan, 195g of sodium hydroxide and 1.15kg of deionized water are weighed and added into a reaction vessel to react for 13 hours at the temperature of 55 ℃ to obtain a solution A.
(2) And filtering and washing the solution A, and placing the solution A in a vacuum drying oven at 85 ℃ for 15 hours to obtain a solid B.
(3) And (3) calcining the solid B in a muffle furnace at 845 ℃ for 12h, and cooling to obtain the MgO/chitosan type antibacterial agent P5.
Application example 5
A method of making a composite material comprising the steps of:
adding 4 parts of P5 into 96 Parts of Styrene (PS), stirring for 10min by a high-speed mixer, and then adding into a double-screw extruder for blending and extruding to obtain the PS composite material X5.
The double-screw extruder comprises six temperature zones which are sequentially arranged, wherein the temperature of the first temperature zone is 160 ℃, the temperature of the second temperature zone is 200 ℃, the temperature of the third temperature zone is 200 ℃, the temperature of the fourth temperature zone is 200 ℃, the temperature of the fifth temperature zone is 200 ℃, the temperature of the sixth temperature zone is 200 ℃, the head temperature of the double-screw extruder is 200 ℃, and the screw rotating speed is 280 r/min.
Comparative example 5
And (3) taking 96 parts of PS, stirring for 10min by using a high-speed mixer, and then adding the PS into a double-screw extruder for blending and extruding to obtain the PS composite material D5.
The antibacterial performance data of the PS composite materials prepared in the above application example 5 and comparative example 5 are shown in the following table (table 5):
TABLE 5
As can be seen from the above table, X5 is more antibacterial than D5, which indicates that the antibacterial property of the PS composite material is better after the antibacterial agent of the present invention is added.
The preparation method of the antibacterial agent and the thermoplastic plastic material prepared by the preparation method have a certain improvement in antibacterial performance, so that the types and application fields of the antibacterial agent are greatly expanded, and the preparation method has very important significance.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited thereto, and various changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the present invention.
Claims (9)
1. A method for preparing an antibacterial agent, comprising the steps of:
(1) adding magnesium nitrate, absolute ethyl alcohol, chitosan, sodium hydroxide and deionized water into a reaction vessel, and reacting at 50-70 ℃ for 10-16h to obtain a solution A;
(2) filtering and washing the solution A, and drying the solution A in a vacuum drying oven to obtain a solid B;
(3) and calcining the solid B in a muffle furnace, and cooling to obtain the MgO/chitosan type antibacterial agent.
2. The method for preparing the antibacterial agent according to claim 1, wherein the mass ratio of the magnesium nitrate, the absolute ethyl alcohol, the chitosan, the sodium hydroxide and the deionized water in the step (1) is (30-40): (50-60): (24-32): (18-24): (120-160).
3. The method for producing an antibacterial agent according to claim 1, wherein the drying conditions in the step (2) are: drying in a vacuum drying oven at 70-90 deg.C for 10-16 h.
4. The method for producing an antibacterial agent according to claim 1, wherein the calcination conditions in the step (3) are: calcining at 800-860 ℃ for 10-12 h.
5. An antibacterial agent characterized by being a MgO/chitosan type antibacterial agent produced by the method for producing an antibacterial agent according to any one of claims 1 to 4.
6. The composite material is characterized by comprising the following components in parts by weight: a thermoplastic 96 and an antibacterial agent 4, which is obtained by the method for producing an antibacterial agent according to any one of claims 1 to 4.
7. Composite according to claim 6, characterized in that the thermoplastic is polyethylene, polypropylene, polystyrene, polybutylene terephthalate or polyamide 6.
8. A method for preparing a composite material according to any one of claims 6 to 7, characterized in that it comprises the following steps:
and mixing the antibacterial agent and the thermoplastic plastic in parts by weight, stirring for 10min by a high-speed mixer, adding into a double-screw extruder, and performing blending extrusion to obtain the composite material.
9. The method as claimed in claim 8, wherein the twin-screw extruder comprises six temperature zones sequentially arranged, the first temperature zone is at a temperature of 120-.
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| CN116114709A (en) * | 2023-02-24 | 2023-05-16 | 福建安邦展示股份有限公司 | Novel antibacterial material and preparation method thereof |
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| CN110804247A (en) * | 2019-11-26 | 2020-02-18 | 泉州师范学院 | Chitosan microsphere-loaded nano-silver antibacterial polypropylene material, composite antibacterial agent and preparation method thereof |
| CN113501997A (en) * | 2021-07-22 | 2021-10-15 | 安徽江淮汽车集团股份有限公司 | Preparation method and application of antibacterial agent |
| CN113621181A (en) * | 2021-08-03 | 2021-11-09 | 安徽江淮汽车集团股份有限公司 | Preparation method of antibacterial agent, thermoplastic resin composite material and preparation method thereof |
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