CN109575362A - 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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- CN109575362A CN109575362A CN201811496316.9A CN201811496316A CN109575362A CN 109575362 A CN109575362 A CN 109575362A CN 201811496316 A CN201811496316 A CN 201811496316A CN 109575362 A CN109575362 A CN 109575362A
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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
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Abstract
The present invention relates to a kind of antibacterial agents and preparation method thereof, to load Pr3+Fe2O3Antibacterial agent.The technical program has synthesized a kind of load Pr3+Fe2O3The antibacterial agent of antibacterial agent, Pr3+It is attached to Fe2O3In crystal structure, there is part Pr3+Form Pr6O11, Pr6O11There is certain inhibiting effect to bacterium, its energy and Fe2O3The synergistic effect that antibacterial can be arrived shows better antibacterial effect, it can be good at improving the antibiotic property with regard to composite polyolefine material, this has great importance.
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, which refers to, to be killed bacterium using chemically or physically method or interferes bacterial growth breeding and its active process, right
In that can kill or interfere microbial growth and its active material to be known as anti-biotic material, most critical has in anti-biotic material
Imitating ingredient is antibacterial agent.
The technical program has synthesized a kind of load Pr3+Fe2O3Antibacterial agent, using it can be good at promoted polyolefin
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 the antibiotic property of composite polyolefine material
Energy.
The present invention is achieved by the following technical solutions:
A kind of antibacterial agent, to load Pr3+Fe2O3Antibacterial agent.
A kind of preparation method of antibacterial agent, comprising:
(1) a certain amount of potassium hydroxide, deionized water, six chloride hydrate praseodymiums and FeCl are weighed3·6H2O is added them into
Into reaction vessels, it is stirred to react 1-3h under room temperature, obtains solution A；
(2) a certain amount of solution A and polypropylene tetramer benzene sulfonic acid sodium salt are weighed, is added them into reaction vessels, 40-60 DEG C
Mechanic whirl-nett reaction 1-3h is down to room temperature ultrasonic reaction 2-4h, obtains solution B；
(3) solution B is transferred in microwave dissolver, carries out micro-wave digestion and react 3-5h, obtains solution C；
(4) solution C is filtered, washed, dried, ground, sieving must both load Pr3+Fe2O3Antibacterial agent.
Potassium hydroxide, deionized water, six chloride hydrate praseodymiums and FeCl in step (1)3·6H2The mass ratio of O is (1-3):
(180-240): (20-30): (70-90).
The mass ratio of solution A and polypropylene tetramer benzene sulfonic acid sodium salt is (40-60) in step (2): (1-3).
The micro-wave digestion reaction temperature of microwave dissolver is 140-160 DEG C in step (3).
The beneficial effects of the present invention are as follows:
1、Pr3+It is attached to Fe2O3In crystal structure, there is part Pr3+Form Pr6O11, Pr6O11There is certain suppression to bacterium
Production is used, its energy and Fe2O3The synergistic effect that antibacterial can be arrived shows better antibacterial effect.
2, the technical program has synthesized a kind of load Pr3+Fe2O3The antibacterial agent of antibacterial agent, it can be good at changing
The kind antibiotic property with regard to composite polyolefine material, this has great importance.
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.
The application provides a kind of antibacterial agent, to load Pr3+Fe2O3Antibacterial agent.
The application also provides a kind of preparation method of antibacterial agent, comprising:
(1) a certain amount of potassium hydroxide, deionized water, six chloride hydrate praseodymiums and FeCl are weighed3·6H2O is added them into
Into reaction vessels, it is stirred to react 1-3h under room temperature, obtains solution A；Potassium hydroxide, deionized water, six chloride hydrate praseodymiums and
FeCl3·6H2The mass ratio of O is (1-3): (180-240): (20-30): (70-90).
(2) a certain amount of solution A and polypropylene tetramer benzene sulfonic acid sodium salt are weighed, is added them into reaction vessels, 40-60 DEG C
Mechanic whirl-nett reaction 1-3h is down to room temperature ultrasonic reaction 2-4h, obtains solution B；The mass ratio of solution A and polypropylene tetramer benzene sulfonic acid sodium salt
It is (40-60): (1-3).
(3) solution B is transferred in microwave dissolver, carries out micro-wave digestion and react 3-5h, obtains solution C；Microwave dissolver
Micro-wave digestion reaction temperature be 140-160 DEG C.
(4) solution C is filtered, washed, dried, ground, sieving must both load Pr3+Fe2O3Antibacterial agent.
Raw material used in each embodiment of the application is as follows:
Potassium hydroxide, Zibo Linzhou City jackshaft chemical industry；Deionized water, Xiamen Ao Quan Environmental Protection Technology Co., Ltd；PrCl3·
6H2O, Yutai Qi Xin Chemical Co., Ltd.；FeCl3·6H2O, Shanghai circumpolar Chemical Co., Ltd.；Polypropylene tetramer benzene sulfonic acid sodium salt, lake
Bei Hengjingrui Chemical Co., Ltd.；PBT (model 2002U), Polyplastics；PP (model Z30S), Maoming Petrochemical；PE (model
5070), Panjin ethylene；PA6 (model C M1017), toray；PS (model 350), state, Taiwan Province are tall.
Test equipment used in each embodiment of the application is as follows:
XH-800B type microwave dissolver, Beijing XiangHu Science and Technology Development Co., Ltd.；ZSK30 type double screw extruder, Germany
W&P company；JL-1000 type tensile testing machine, the production of Guangzhou Guang Cai laboratory apparatus company；The injection moulding of HTL900-T-5B type
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 is drawn
Stretch tester, Dongguan City Gao Tai detecting instrument Co., Ltd；QD-GJS-B12K type high-speed mixer, Beijing perseverance Order instrument instrument
Table Co., Ltd.
Embodiment 1
(1) 10g potassium hydroxide, 1.8kg deionized water, six chloride hydrate praseodymium (PrCl of 200g are weighed3·6H2O)、
700gFeCl3·6H2O is added them into reaction vessels, is stirred to react 1h under room temperature, is obtained solution A.
(2) 400g solution A, 10g polypropylene tetramer benzene sulfonic acid sodium salt are weighed, is added them into reaction vessels, 40 DEG C of machinery
It is stirred to react 1h, room temperature ultrasonic reaction 2h is down to, obtains solution B.
(3) solution B is transferred in microwave dissolver, carries out micro-wave digestion and react 3h, obtains solution C；Microwave dissolver
Micro-wave digestion reaction temperature is 140 DEG C.
(4) solution C is filtered, washed, dried, ground, crossed 300 meshes, must both load Pr3+Fe2O3Antibacterial agent
P1。
Application examples 1
It takes 4 parts of P1 to be added in 96 parts of PP, stirs 10min through high mixer, be subsequently added into double screw extruder and be total to
It is mixed to squeeze out, obtain PP composite material X1.
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 230 DEG C, and the temperature of third humidity province is 230 DEG C, and the temperature of the 4th humidity province is 230 DEG C, the 5th temperature
The temperature for spending area is 230 DEG C, and the temperature of the 6th humidity province is 230 DEG C, and the head temperature of double screw extruder is 230 DEG C, screw rod
Revolving speed is 200r/min.
Comparative example 1
96 parts of PP are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain PP
Composite material D1.
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 the technical program is added that PP is compound
The anti-microbial property of material is more preferable.
Embodiment 2
(1) 30g potassium hydroxide, 2.4kg deionized water, six chloride hydrate praseodymium (PrCl of 300g are weighed3·6H2O)、
900gFeCl3·6H2O is added them into reaction vessels, is stirred to react 3h under room temperature, is obtained solution A.
(2) 600g solution A, 30g polypropylene tetramer benzene sulfonic acid sodium salt are weighed, is added them into reaction vessels, 60 DEG C of machinery
It is stirred to react 3h, room temperature ultrasonic reaction 4h is down to, obtains solution B.
(3) solution B is transferred in microwave dissolver, carries out micro-wave digestion and react 5h, obtains solution C；Microwave dissolver
Micro-wave digestion reaction temperature is 160 DEG C.
(4) solution C is filtered, washed, dried, ground, crossed 300 meshes, must both load Pr3+Fe2O3Antibacterial 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) 20g potassium hydroxide, 2.1kg deionized water, six chloride hydrate praseodymium (PrCl of 250g are weighed3·6H2O)、
800gFeCl3·6H2O is added them into reaction vessels, is stirred to react 2h under room temperature, is obtained solution A.
(2) 500g solution A, 20g polypropylene tetramer benzene sulfonic acid sodium salt are weighed, is added them into reaction vessels, 50 DEG C of machinery
It is stirred to react 2h, room temperature ultrasonic reaction 3h is down to, obtains solution B.
(3) solution B is transferred in microwave dissolver, carries out micro-wave digestion and react 4h, obtains solution C；Microwave dissolver
Micro-wave digestion reaction temperature is 150 DEG C.
(4) solution C is filtered, washed, dried, ground, crossed 300 meshes, must both load Pr3+Fe2O3Antibacterial 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) 25g potassium hydroxide, 1.9kg deionized water, six chloride hydrate praseodymium (PrCl of 260g are weighed3·6H2O)、
780gFeCl3·6H2O is added them into reaction vessels, is stirred to react 1h under room temperature, is obtained solution A.
(2) 450g solution A, 25g polypropylene tetramer benzene sulfonic acid sodium salt are weighed, is added them into reaction vessels, 45 DEG C of machinery
It is stirred to react 3h, room temperature ultrasonic reaction 4h is down to, obtains solution B.
(3) solution B is transferred in microwave dissolver, carries out micro-wave digestion and react 3h, obtains solution C；Microwave dissolver
Micro-wave digestion reaction temperature is 145 DEG C.
(4) solution C is filtered, washed, dried, ground, crossed 300 meshes, must both load Pr3+Fe2O3Antibacterial 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 260 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) 15g potassium hydroxide, 2.0kg deionized water, six chloride hydrate praseodymium (PrCl of 270g are weighed3·6H2O)、
780gFeCl3·6H2O is added them into reaction vessels, is stirred to react 3h under room temperature, is obtained solution A.
(2) 520g solution A, 22g polypropylene tetramer benzene sulfonic acid sodium salt are weighed, is added them into reaction vessels, 45 DEG C of machinery
It is stirred to react 1h, room temperature ultrasonic reaction 4h is down to, obtains solution B.
(3) solution B is transferred in microwave dissolver, carries out micro-wave digestion and react 5h, obtains solution C；Microwave dissolver
Micro-wave digestion reaction temperature is 155 DEG C.
(4) solution C is filtered, washed, dried, ground, crossed 300 meshes, must both load Pr3+Fe2O3Antibacterial 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, this illustrates after the antibacterial agent of the technical program is added that PS is compound
The anti-microbial property of material is more preferable.
The technical program describes a kind of preparation method of antibacterial agent, and with its polyolefine material obtained in antibacterial
Aspect of performance is also improved to some extent, this has very important meaning for the type and application field of extension antibacterial agent
Justice.
Although present invention combination above embodiments are described, the present invention is not limited to above-described embodiment,
And be only defined by the appended claims, those of ordinary skill in the art easily can modify and change to it, but simultaneously
Without departing from essential idea and range of the invention.
Claims (5)
1. a kind of antibacterial agent, which is characterized in that for load Pr3+Fe2O3Antibacterial agent.
2. a kind of preparation method of antibacterial agent characterized by comprising
(1) a certain amount of potassium hydroxide, deionized water, six chloride hydrate praseodymiums and FeCl are weighed3·6H2O is added them into anti-
It answers in vessel, is stirred to react 1-3h under room temperature, obtains solution A；
(2) a certain amount of solution A and polypropylene tetramer benzene sulfonic acid sodium salt are weighed, is added them into reaction vessels, 40-60 DEG C of machinery
It is stirred to react 1-3h, room temperature ultrasonic reaction 2-4h is down to, obtains solution B；
(3) solution B is transferred in microwave dissolver, carries out micro-wave digestion and react 3-5h, obtains solution C；
(4) solution C is filtered, washed, dried, ground, sieving must both load Pr3+Fe2O3Antibacterial agent.
3. the preparation method of antibacterial agent according to claim 2, which is characterized in that potassium hydroxide, deionization in step (1)
Water, six chloride hydrate praseodymiums and FeCl3·6H2The mass ratio of O is (1-3): (180-240): (20-30): (70-90).
4. the preparation method of antibacterial agent according to claim 2, which is characterized in that solution A and polypropylene tetramer in step (2)
The mass ratio of benzene sulfonic acid sodium salt is (40-60): (1-3).
5. the preparation method of antibacterial agent according to claim 2, which is characterized in that microwave dissolver is micro- in step (3)
It is 140-160 DEG C that wave, which clears up reaction temperature,.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112136834A (en) * | 2020-09-23 | 2020-12-29 | 安徽江淮汽车集团股份有限公司 | Method for producing antibacterial agent, antibacterial agent and thermoplastic using the same |
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| CN102138569A (en) * | 2010-01-28 | 2011-08-03 | 广东炜林纳功能材料有限公司 | Rare-earth composite antibacterial agent and application thereof |
| CN102491403A (en) * | 2011-12-19 | 2012-06-13 | 班朝磊 | Method for preparing copper oxide powder by using complexed-precipitation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112136834A (en) * | 2020-09-23 | 2020-12-29 | 安徽江淮汽车集团股份有限公司 | Method for producing antibacterial agent, antibacterial agent and thermoplastic using the same |
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