CN109232988A - A kind of antibacterial agent and preparation method thereof - Google Patents
A kind of antibacterial agent and preparation method thereof Download PDFInfo
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- CN109232988A CN109232988A CN201810988003.9A CN201810988003A CN109232988A CN 109232988 A CN109232988 A CN 109232988A CN 201810988003 A CN201810988003 A CN 201810988003A CN 109232988 A CN109232988 A CN 109232988A
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- coral reef
- antibacterial agent
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- C—CHEMISTRY; METALLURGY
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- 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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/015—Biocides
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Abstract
The present invention relates to a kind of antibacterial agent and preparation method thereof, antibacterial agent is that coral reef carries Ag+The antibacterial agent of type, using -2 pyrrolidones of 1- methyl as stabilizer, 2- hydroxyl ethyl mercaptan is reducing agent, Ag+With -2 pyrrolidones of 1- methyl formed complex by stable dispersion in a solvent, Ag+Zeroth order is reduced to from positive monovalence by 2- hydroxyl ethyl mercaptan, and is constantly gathered under the synergistic effect of -2 pyrrolidones of 1- methyl on " core " on coral reef surface, the stone that grows into coral reef carries Ag+The antibacterial agent of type.
Description
Technical field
The invention belongs to technical field of polymer materials, a kind of antibacterial agent and preparation method thereof is particularly related to.
Background technique
Antibacterial agent refers to that some microorganisms are highly sensitive, and material antimicrobial properties can be assigned by being added in material on a small quantity
Chemical substance.The technical program has innovatively synthesized a kind of novel antibacterial agent, can be good at promoting polyolefin using it
The anti-microbial property of composite material.This antibacterial agent not yet sees report so far, this has the type and application that extend antibacterial agent
There is very important realistic meaning.
Summary of the invention
The object of the present invention is to provide a kind of antibacterial agents and preparation method thereof, to improve existing composite polyolefine material
Anti-microbial property.
The present invention is achieved by the following technical solutions:
A kind of antibacterial agent carries Ag for coral reef+The antibacterial agent of type.
A kind of preparation method of antibacterial agent, comprising the following steps:
(1) a certain amount of coral reef, the concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 16-20h under room temperature, must change
Property coral reef A；
(2) modified coral reef A is placed in Muffle furnace, heating reaction 10-14h, obtains modified coral in 500-700 DEG C
Reef B；
(3) a certain amount of modified coral reef B, deionized water, Klorvess Liquid are weighed, is stirred to react 6- at 30-40 DEG C
8h is washed so dry that be modified coral reef C；
(4) weigh a certain amount of modified coral reef C, deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl,
Silver nitrate solution is stirred to react 10-16h under room temperature, is filtered, washed, dries to obtain modified coral reef D；
(5) it will be modified the coral reef D dry 12-16h at 60-80 DEG C in a vacuum drying oven, roasted at 200-280 DEG C
6-10h is burnt, cooling grinding crosses 500 meshes, both obtains antibacterial agent.
The mass ratio of coral reef and the concentrated sulfuric acid in step (1) is (20-30): (120-160).
The mass ratio of modification coral reef B, deionized water and Klorvess Liquid in step (3) are (40-60): (180-
240): (6-8).
Modification coral reef C, deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl and nitric acid in step (4)
The mass ratio of silver-colored solution is (30-50)；(120-160): (6-12): (3-5): (4-8).
The beneficial effects of the present invention are:
Using -2 pyrrolidones of 1- methyl as stabilizer, 2- hydroxyl ethyl mercaptan is reducing agent, Ag+With -2 pyrrolidones of 1- methyl
Formed complex by stable dispersion in a solvent, Ag+Zeroth order is reduced to from positive monovalence by 2- hydroxyl ethyl mercaptan, and in 1- first
On " core " for constantly gathering coral reef surface under the synergistic effect of -2 pyrrolidones of base, the stone that grows into coral reef carries Ag+Type
Antibacterial agent.
Specific embodiment
Carry out the technical solution that the present invention will be described in detail by the following examples, embodiment below is merely exemplary, only
It can be used to explanation and illustration technical solution of the present invention, and be not to be construed as the limitation to technical solution of the present invention.
Raw material used in embodiments herein is as follows:
PBT (model 2002U), Polyplastics；Coral reef, the Lingshou wing reach mineral products processing factory；The concentrated sulfuric acid, Zouping day deer
Chemical Co., Ltd.；Deionized water, hundred Aurion of Beijing win Science and Technology Ltd.；Klorvess Liquid, Jiaozhuo dimension connection fine chemistry industry；2-
Hydroxyl ethyl mercaptan, Shanghai Jia Chen Chemical Co., Ltd.；- 2 pyrrolidones of 1- methyl, Shanghai Bang Jing Industrial Co., Ltd.；Silver nitrate
Solution, chemical products Co., Ltd among Zhengzhou hundred million；Antioxidant (model Irganox168, Irganox1010,
Irganox1330), Switzerland's Ciba.
Test equipment used herein is as follows:
ZSK30 type double screw extruder, German W&P company；JL-1000 type tensile testing machine, the wide just experiment instrument in Guangzhou
The production of device company；HTL900-T-5B type injection (mo(u)lding) machine, the production of Hai Tai plastics machinery Co., Ltd；XCJ-500 type shock-testing
Machine, the production of Chengde testing machine factory；QT-1196 type tester for elongation, Dongguan City Gao Tai detecting instrument Co., Ltd；QD-GJS-
B12K type high-speed mixer, Beijing perseverance Order instrument and meter Co., Ltd.
The application provides a kind of antibacterial agent, carries Ag for coral reef+The antibacterial agent of type.
The application also provides a kind of preparation method of antibacterial agent, comprising the following steps:
(1) a certain amount of coral reef, the concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 16-20h under room temperature, must change
Property coral reef A；The mass ratio of coral reef and the concentrated sulfuric acid is (20-30): (120-160).
(2) modified coral reef A is placed in Muffle furnace, heating reaction 10-14h, obtains modified coral in 500-700 DEG C
Reef B.
(3) a certain amount of modified coral reef B, deionized water, Klorvess Liquid are weighed, is stirred to react 6- at 30-40 DEG C
8h is washed so dry that be modified coral reef C；The mass ratio of modified coral reef B, deionized water and Klorvess Liquid are (40-
60): (180-240): (6-8).
(4) weigh a certain amount of modified coral reef C, deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl,
Silver nitrate solution is stirred to react 10-16h under room temperature, is filtered, washed, dries to obtain modified coral reef D；Modified coral reef C,
Deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl and silver nitrate solution mass ratio be (30-50)；(120-
160): (6-12): (3-5): (4-8).
(5) it will be modified the coral reef D dry 12-16h at 60-80 DEG C in a vacuum drying oven, roasted at 200-280 DEG C
6-10h is burnt, cooling grinding crosses 500 meshes, both obtains antibacterial agent.
Embodiment 1
(1) 200g coral reef, the 1.2kg concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 16h under room temperature, obtain modification
Coral reef A.
(2) modified coral reef A is placed in Muffle furnace, heating reaction 10h, obtains modified coral reef B in 500 DEG C.
(3) 400g modified coral reef B, 1.8kg deionized water, 60g Klorvess Liquid are weighed, is stirred to react at 30 DEG C
6h is washed so dry that be modified coral reef C.
(4) 300g modified coral reef C, 1.2kg deionized water, 60g2- hydroxyl ethyl mercaptan, -2 pyrrole of 30g1- methyl are weighed
Pyrrolidone, 40g silver nitrate solution are stirred to react 10h under room temperature, are filtered, washed, dry to obtain modified coral reef D.
(5) it will be modified the coral reef D dry 12h at 60 DEG C in a vacuum drying oven, 6h is roasted at 200 DEG C, it is cooling
500 meshes are crossed in grinding, both obtain antibacterial agent P1.
Application examples 1
It takes 4 parts of P1 to be added in 96 parts of polypropylene (PP), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PP composite material X1.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 170 DEG C, the
The temperature of two humidity provinces is 220 DEG C, and the temperature of third humidity province is 230 DEG C, and the temperature of the 4th humidity province is 240 DEG C, the 5th temperature
The temperature for spending area is 240 DEG C, and the temperature of the 6th humidity province is 240 DEG C, and the head temperature of double screw extruder is 230 DEG C, screw rod
Revolving speed is 220r/min.
Comparative example 1
96 parts of polypropylene (PP) are taken, stir 10min through high mixer, is subsequently added into double screw extruder be blended and squeeze
Out, PP composite material D1 is obtained.
The anti-microbial property data of PP composite material prepared by above application examples 1 and comparative example 1 are as shown in the table:
As can be seen from the above table, antibiotic property of the X1 than D1 is good, this illustrates after the antibacterial agent of this programme is added, PP composite material
Anti-microbial property it is more preferable.
Embodiment 2
(1) 300g coral reef, the 1.6kg concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 20h under room temperature, obtain modification
Coral reef A.
(2) modified coral reef A is placed in Muffle furnace, heating reaction 14h, obtains modified coral reef B in 700 DEG C.
(3) 600g modified coral reef B, 2.4kg deionized water, 80g Klorvess Liquid are weighed, is stirred to react at 40 DEG C
8h is washed so dry that be modified coral reef C.
(4) 500g modified coral reef C, 1.6kg deionized water, 120g2- hydroxyl ethyl mercaptan, -2 pyrrole of 50g1- methyl are weighed
Pyrrolidone, 80g silver nitrate solution are stirred to react 16h under room temperature, are filtered, washed, dry to obtain modified coral reef D.
(5) it will be modified the coral reef D dry 16h at 80 DEG C in a vacuum drying oven, 10h is roasted at 280 DEG C, it is cooling
500 meshes are crossed in grinding, both obtain antibacterial agent P2.
Application examples 2
Take 4 parts of P2 to be added in 96 parts of polybutylene terephthalate (PBT)s (PBT), stir 10min through high mixer, then plus
Enter and carry out blending extrusion in double screw extruder, obtains PBT composite X2.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 200 DEG C, the
The temperature of two humidity provinces is 260 DEG C, and the temperature of third humidity province is 260 DEG C, and the temperature of the 4th humidity province is 260 DEG C, the 5th temperature
The temperature for spending area is 260 DEG C, and the temperature of the 6th humidity province is 260 DEG C, and the head temperature of double screw extruder is 260 DEG C, screw rod
Revolving speed is 300r/min.
Comparative example 2
96 parts of PBT are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain
PBT composite D2.
The anti-microbial property data of PBT composite prepared by above application examples 2 and comparative example 2 are as shown in the table:
As can be seen from the above table, antibiotic property of the X2 than D2 is good, this illustrates after the antibacterial agent of the technical program is added that PBT is multiple
The anti-microbial property of condensation material is more preferable.
Embodiment 3
(1) 250g coral reef, the 1.4kg concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 18h under room temperature, obtain modification
Coral reef A.
(2) modified coral reef A is placed in Muffle furnace, heating reaction 12h, obtains modified coral reef B in 600 DEG C.
(3) 500g modified coral reef B, 2.1kg deionized water, 70g Klorvess Liquid are weighed, is stirred to react at 35 DEG C
7h is washed so dry that be modified coral reef C.
(4) 400g modified coral reef C, 1.4kg deionized water, 90g2- hydroxyl ethyl mercaptan, -2 pyrrole of 40g1- methyl are weighed
Pyrrolidone, 60g silver nitrate solution are stirred to react 13h under room temperature, are filtered, washed, dry to obtain modified coral reef D.
(5) it will be modified the coral reef D dry 14h at 70 DEG C in a vacuum drying oven, 8h is roasted at 240 DEG C, it is cooling
500 meshes are crossed in grinding, both obtain antibacterial agent P3.
Application examples 3
It takes 4 parts of P3 to be added in 96 parts of polyethylene (PE), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PE composite material X3.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 120 DEG C, the
The temperature of two humidity provinces is 180 DEG C, and the temperature of third humidity province is 180 DEG C, and the temperature of the 4th humidity province is 180 DEG C, the 5th temperature
The temperature for spending area is 180 DEG C, and the temperature of the 6th humidity province is 180 DEG C, and the head temperature of double screw extruder is 180 DEG C, screw rod
Revolving speed is 300r/min.
Comparative example 3
96 parts of PE are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain PE
Composite material D3.
The anti-microbial property data of PE composite material prepared by above application examples 3 and comparative example 3 are as shown in the table:
As can be seen from the above table, antibiotic property of the X3 than D3 is good, this illustrates after the antibacterial agent of the technical program is added that PE is compound
The anti-microbial property of material is more preferable.
Embodiment 4
(1) 220g coral reef, the 1.5kg concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 17h under room temperature, obtain modification
Coral reef A.
(2) modified coral reef A is placed in Muffle furnace, heating reaction 13h, obtains modified coral reef B in 560 DEG C.
(3) 460g modified coral reef B, 2.2kg deionized water, 75g Klorvess Liquid are weighed, is stirred to react at 38 DEG C
6h is washed so dry that be modified coral reef C.
(4) 360g modified coral reef C, 1.5kg deionized water, 110g2- hydroxyl ethyl mercaptan, -2 pyrrole of 45g1- methyl are weighed
Pyrrolidone, 75g silver nitrate solution are stirred to react 15h under room temperature, are filtered, washed, dry to obtain modified coral reef D.
(5) it will be modified the coral reef D dry 14h at 65 DEG C in a vacuum drying oven, 10h is roasted at 200 DEG C, it is cooling
500 meshes are crossed in grinding, both obtain antibacterial agent P4.
Application examples 4
It takes 4 parts of P4 to be added in 96 parts of polyamide 6s (PA6), stirs 10min through high mixer, be subsequently added into twin-screw extrusion
Blending extrusion is carried out in machine, obtains PA6 composite material X4.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 230 DEG C, the
The temperature of two humidity provinces is 260 DEG C, and the temperature of third humidity province is 260 DEG C, and the temperature of the 4th humidity province is 260 DEG C, the 5th temperature
The temperature for spending area is 260 DEG C, and the temperature of the 6th humidity province is 260 DEG C, and the head temperature of double screw extruder is 250 DEG C, screw rod
Revolving speed is 320r/min.
Comparative example 4
96 parts of PA6 are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain
PA6 composite material D4.
The anti-microbial property data of PA6 composite material prepared by above application examples 4 and comparative example 4 are as shown in the table:
As can be seen from the above table, antibiotic property of the X4 than D4 is good, this illustrates after the antibacterial agent of the technical program is added that PA6 is multiple
The anti-microbial property of condensation material is more preferable.
Embodiment 5
(1) 290g coral reef, the 1.3kg concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 17h under room temperature, obtain modification
Coral reef A.
(2) modified coral reef A is placed in Muffle furnace, heating reaction 11h, obtains modified coral reef B in 550 DEG C.
(3) 550g modified coral reef B, 2.0kg deionized water, 65g Klorvess Liquid are weighed, is stirred to react at 38 DEG C
8h is washed so dry that be modified coral reef C.
(4) 450g modified coral reef C, 1.3kg deionized water, 80g2- hydroxyl ethyl mercaptan, -2 pyrrole of 50g1- methyl are weighed
Pyrrolidone, 55g silver nitrate solution are stirred to react 12h under room temperature, are filtered, washed, dry to obtain modified coral reef D.
(5) it will be modified the coral reef D dry 15h at 75 DEG C in a vacuum drying oven, 9h is roasted at 270 DEG C, it is cooling
500 meshes are crossed in grinding, both obtain antibacterial agent P5.
Application examples 5
It takes 4 parts of P5 to be added in 96 parts of styrene (PS), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PS composite material X5.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 160 DEG C, the
The temperature of two humidity provinces is 200 DEG C, and the temperature of third humidity province is 200 DEG C, and the temperature of the 4th humidity province is 200 DEG C, the 5th temperature
The temperature for spending area is 200 DEG C, and the temperature of the 6th humidity province is 200 DEG C, and the head temperature of double screw extruder is 200 DEG C, screw rod
Revolving speed is 280r/min.
Comparative example 5
96 parts of PS are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain PS
Composite material D5.
The anti-microbial property data of PS composite material prepared by above application examples 5 and comparative example 5 are as shown in the table:
As can be seen from the above table, antibiotic property of the X5 than D5 is good, and after the antibacterial agent of the technical program is added in this scheme, PS is compound
The anti-microbial property of material is more preferable.
This programme describes a kind of preparation method of antibacterial agent, and with its polyolefine material obtained in anti-microbial property
Aspect is also improved to some extent, this greatly expands the type and application field of antibacterial agent, has very important significance.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And deformation, the scope of the present invention are extremely equally limited by appended claims.
Claims (5)
1. a kind of antibacterial agent, it is characterized in that: Ag is carried for coral reef+The antibacterial agent of type.
2. a kind of preparation method of antibacterial agent, which comprises the following steps:
(1) a certain amount of coral reef, the concentrated sulfuric acid are weighed, is added into reaction vessels, is reacted 16-20h under room temperature, obtain modified coral
Coral reef A；
(2) modified coral reef A is placed in Muffle furnace, heating reaction 10-14h, obtains modified coral reef in 500-700 DEG C
B；
(3) a certain amount of modified coral reef B, deionized water, Klorvess Liquid are weighed, 6-8h is stirred to react at 30-40 DEG C, washes
It washs so dry that be modified coral reef C；
(4) a certain amount of modified coral reef C, deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl, nitric acid are weighed
Silver-colored solution is stirred to react 10-16h under room temperature, is filtered, washed, dries to obtain modified coral reef D；
(5) it will be modified the coral reef D dry 12-16h at 60-80 DEG C in a vacuum drying oven, roast 6- at 200-280 DEG C
10h, cooling grinding, crosses 500 meshes, both obtains antibacterial agent.
3. the preparation method of antibacterial agent according to claim 2, which is characterized in that coral reef in step (1) with it is dense
The mass ratio of sulfuric acid is (20-30): (120-160).
4. the preparation method of antibacterial agent according to claim 2, which is characterized in that the modification coral reef in step (3)
B, the mass ratio of deionized water and Klorvess Liquid is (40-60): (180-240): (6-8).
5. the preparation method of antibacterial agent according to claim 2, which is characterized in that the modification coral reef in step (4)
C, the mass ratio of deionized water, 2- hydroxyl ethyl mercaptan, -2 pyrrolidones of 1- methyl and silver nitrate solution is (30-50)；(120-
160): (6-12): (3-5): (4-8).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548361A (en) * | 2020-05-29 | 2020-08-18 | 广东迪美生物技术有限公司 | Novel high-stability transparent silver ion complex and preparation method and application thereof |
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| CN101020078A (en) * | 2007-03-13 | 2007-08-22 | 广州麦邦生物科技有限公司 | Antibiotic silver-carrying modified artificial coral bone and its prepn process |
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Address after: 230601 No. 99 Ziyun Road, Hefei Economic and Technological Development Zone, Anhui Province Applicant after: Anhui Jianghuai Automobile Group Limited by Share Ltd Address before: 230601 No. 669 Shixin Road, Taohua Industrial Park, Hefei City, Anhui Province Applicant before: Anhui Jianghuai Automobile Group Limited by Share Ltd |
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