CN106633190A - Preparation method and application of antibacterial agent - Google Patents

Preparation method and application of antibacterial agent Download PDF

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Publication number
CN106633190A
CN106633190A CN201610921474.9A CN201610921474A CN106633190A CN 106633190 A CN106633190 A CN 106633190A CN 201610921474 A CN201610921474 A CN 201610921474A CN 106633190 A CN106633190 A CN 106633190A
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CN
China
Prior art keywords
solution
hydrotalcite
antiseptic
preparation
antibacterial agent
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CN201610921474.9A
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Chinese (zh)
Inventor
刘凯
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Anhui Jianghuai Automobile Group Corp
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Anhui Jianghuai Automobile Group Corp
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Priority to CN201610921474.9A priority Critical patent/CN106633190A/en
Publication of CN106633190A publication Critical patent/CN106633190A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/12Adsorbed ingredients, e.g. ingredients on carriers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0806Silver
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/24Crystallisation aids

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to a preparation method and an application of an antibacterial agent. The preparation method comprises the steps of: weighing hydrotalcite and adding the hydrotalcite to a Ag2SO4 solution, and performing a reaction in a magnetic stirrer at constant temperature; adding deionized water to the solution after the reaction is finished, allowing the solution to stand, and pouring supernatant away, repeatedly washing the solution until no white precipitate is generated after a BaCl2 solution is dropwisely added to the supernatant; centrifuging the washed solution in a centrifugal machine; drying the centrifuged solid in a drying box and grinding the solid into a powdery sample to produce silver-supported hydrotalcite. The hydrotalcite is used as a carrier of the antibacterial agent, so that a conventional antibacterial agent carrier, such as artificial zeolite, montmorillonite, sepiolite and the like, is changed; and the antibacterial agent has significant antibacterial effect. The carrier greatly develops application range of antibacterial agents and has important significance.

Description

A kind of preparation method and applications of antiseptic
Technical field
The invention belongs to technical field of polymer materials, particularly relates to a kind of preparation method and applications of antiseptic.
Background technology
Hydrotalcite is a kind of layer structure material, there is larger specific surface area, and the load and ion to metal ion is handed over Change there is provided enough spaces and time, being smoothed out beneficial to ion exchange.These special structures and performance make hydrotalcite Compared with existing inorganic carrier such as zeolite, bentonite, silica gel, the performance of more preferable adsorption antibacterial metal ion is shown, It is allowed to that there is very wide prospect in the exploitation of inorganic antibacterial agent carrier.
The content of the invention
It is an object of the invention to provide a kind of preparation method and applications of antiseptic, to improve polyolefinic antibiotic property Energy.
The present invention is achieved by the following technical solutions:
A kind of preparation method of antiseptic, comprises the following steps:
(1) weigh hydrotalcite to add to Ag2SO4Solution, reacts under conditions of 60-90 DEG C of constant temperature in magnetic stirring apparatus 2-5h;
(2) solution after the completion of reaction is added into deionized water, stands and remove supernatant liquor after 2-3h, cleaned repeatedly, until BaCl is added dropwise in supernatant liquor2Solution is generated without white depositions, and washed solution is centrifuged into 20-30min in centrifuge, The rotating speed of centrifuge is 3500-5000r/min;
(3) solid after centrifugation is dried into 2-3h in drying box, baking temperature is 165-180 DEG C, and powder is made in grinding Shape sample, that is, obtain carrying silver-colored hydrotalcite.
Hydrotalcite and Ag in step (1)2SO4The mass ratio of solution is 10-16:120-180.
Antiseptic described in any of the above-described is applied in polyolefin.
The polyolefin include polypropylene, polystyrene, polyethylene or polybutylene terephthalate (PBT) in one kind or It is various.
The invention has the beneficial effects as follows;
1st, using hydrotalcite as carrier, traditional carrier such as artificial zeolite, montmorillonite, sea are changed Afrodite etc., antibacterial effect is notable.This greatly expands the range of application of antiseptic, has very important significance.
2nd, the addition for carrying silver-colored hydrotalcite serves certain facilitation to polyolefinic crystallization, carries silver-colored hydrotalcite and act as The nucleator of polyolefin crystallization, crystallization can increase the regularity of macromolecular chain segment arrangement, strengthen intermolecular active force, Thus the raising of degree of crystallinity, make polyolefinic physical property also increase.
Specific embodiment
By the following examples describing technical scheme in detail, below example be only it is exemplary, only Can be used for explaining and illustrating technical scheme, and be not to be construed as the restriction to technical solution of the present invention.
The application provides a kind of preparation method of antiseptic, comprises the following steps:
(1) weigh hydrotalcite to add to Ag2SO4Solution, reacts under conditions of 60-90 DEG C of constant temperature in magnetic stirring apparatus 2-5h;
(2) solution after the completion of reaction is added into deionized water, stands and remove supernatant liquor after 2-3h, cleaned repeatedly, until BaCl is added dropwise in supernatant liquor2Solution is generated without white depositions, and washed solution is centrifuged into 20-30min in centrifuge, The rotating speed of centrifuge is 3500-5000r/min;
(3) solid after centrifugation is dried into 2-3h in drying box, baking temperature is 165-180 DEG C, and powder is made in grinding Shape sample, that is, obtain carrying silver-colored hydrotalcite.
Hydrotalcite and Ag in step (1)2SO4The mass ratio of solution is 10-16:120-180.
Antiseptic described in any of the above-described is applied in polyolefin.
The polyolefin includes polypropylene (PP), polystyrene (PS), polyethylene (PE) or polybutylene terephthalate One or more in ester (PBT).
Raw material used is as follows in various embodiments of the present invention:
PS (model 350), Taiwan state is tall;PP (model F401), Yangtze petrochemical industry;PE (model 5502S), wuhan petrochemical industry;PBT (model 2002U), Polyplastics;Hydrotalcite, Jingjiang extensively wins rubber and plastic;Ag2SO4, happy chemical industry is praised in Guangzhou;BaCl2, nation's promise chemical industry.
Tester used by the present invention is as follows:
ZSK30 type double screw extruders, German W&P companies;JL-1000 type tensile testing machines, the wide just experiment instrument in Guangzhou Device company produces;HTL900-T-5B type injection (mo(u)lding) machines, the production of Hai Tai plastics machineries Co., Ltd;XCJ-500 type shock-testings Machine, the production of Chengde testing machine factory;QT-1196 type tester for elongation, Dongguan City Gao Tai detecting instruments Co., Ltd;QD-GJS- B12K type homogenizers, Beijing perseverance Order instrument and meter Co., Ltd.
Embodiment 1
(1) 100g hydrotalcites, 1.2kg Ag are weighed2SO4Solution, they are put into magnetic stirring apparatus, anti-under the conditions of 60 DEG C Answer 2h.
(2) solution after the completion of reaction is added into deionized water, stands and remove supernatant liquor after 1h, cleaned repeatedly, until BaCl is added dropwise in supernatant liquor2Solution is generated without white depositions.Washed solution is centrifuged by 3500r/min of centrifugation rate 20min。
(3) solid after centrifugation is dried into 2h in drying box, powdered samples are made in 165 DEG C of baking temperature, grinding, i.e., Obtain carrying silver-colored hydrotalcite P1.
Application examples 1
Take 20 parts of P1 to be added in 80 parts of polypropylene (PP), Jing high mixers stirring 10min is subsequently added into double screw extruder In carry out blending extrusion, obtain PP composite X1.
Wherein, double screw extruder includes six humidity provinces sequentially arranging, and the temperature of the first humidity province is 70 DEG C, second The temperature of humidity province is 120 DEG C, and the temperature of the 3rd humidity province is 130 DEG C, and the temperature of the 4th humidity province is 140 DEG C, the 5th temperature The temperature in area is 140 DEG C, and the temperature of the 6th humidity province is 140 DEG C, and the head temperature of double screw extruder is 130 DEG C, and screw rod turns Speed is 120r/min.
Comparative example 1
80 parts of polypropylene (PP) are taken, Jing high mixers stirring 10min is subsequently added into double screw extruder to carry out being blended and squeezes Go out, obtain PP composite D1.
PP composites prepared by above-described embodiment 1 and comparative example 1 are made into batten with injection machine, its properties of product data It is as shown in the table:
As can be seen from the above table:
1) antibiotic property of X1 is better than D1, and this explanation adds the effect that silver-colored hydrotalcite-modified PP serves antibacterial that carries.
2) tensile strength of X1, bending strength, cantilever beam impact strength are bigger than D1, and this explanation is added and carries silver-colored neatly Stone act as the nucleator of polyolefin crystallization, promote the heterogeneous nucleation of PP, improve the physical property of PP composites.
Embodiment 2
(1) 160g hydrotalcites, 1.8kg Ag are weighed2SO4Solution, they are put into magnetic stirring apparatus, anti-under the conditions of 90 DEG C Answer 5h.
(2) solution after the completion of reaction is added into deionized water, stands and remove supernatant liquor after 3h, cleaned repeatedly, until BaCl is added dropwise in supernatant liquor2Solution is generated without white depositions.Washed solution is centrifuged by 5000r/min of centrifugation rate 30min。
(3) solid after centrifugation is dried into 3h in drying box, powdered samples are made in 180 DEG C of baking temperature, grinding, i.e., Obtain carrying silver-colored hydrotalcite P2.
Application examples 2
Take 20 parts of P2 to be added in 80 parts of PS, Jing high mixers stirring 10min, being subsequently added into double screw extruder is carried out altogether Mixed extrusion, obtains PS composite X2.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 100 DEG C, the The temperature of two humidity provinces is 220 DEG C, and the temperature of the 3rd humidity province is 230 DEG C, and the temperature of the 4th humidity province is 230 DEG C, and the 5th is warm The temperature in degree area is 230 DEG C, and the temperature of the 6th humidity province is 240 DEG C, and the head temperature of double screw extruder is 200 DEG C, screw rod Rotating speed is 300r/min.
Comparative example 2
80 parts of PS, Jing high mixers stirring 10min are taken, being subsequently added into double screw extruder carries out blending extrusion, obtains PS Composite D2.
PS composites prepared by above-described embodiment 2 and comparative example 2 are made into batten with injection machine, its properties of product data It is as shown in the table:
As can be seen from the above table:
1) antibiotic property of X2 is better than D2, and this explanation adds the effect that silver-colored hydrotalcite-modified PS serves antibacterial that carries.
2) tensile strength of X2, bending strength, cantilever beam impact strength are bigger than D2, and this explanation is added and carries silver-colored neatly Stone act as the nucleator of polyolefin crystallization, promote the heterogeneous nucleation of PS, improve the physical property of PS composites.
Embodiment 3
(1) 130g hydrotalcites, 1.5kg Ag are weighed2SO4Solution, they are put into magnetic stirring apparatus, anti-under the conditions of 75 DEG C Answer 3.5h.
(2) solution after the completion of reaction is added into deionized water, stands and remove supernatant liquor after 2h, cleaned repeatedly, until BaCl is added dropwise in supernatant liquor2Solution is generated without white depositions.Washed solution is centrifuged by 4250r/min of centrifugation rate 25min。
(3) solid after centrifugation is dried into 2.5h in drying box, powder sample is made in 172.5 DEG C of baking temperature, grinding Product, that is, obtain carrying silver-colored hydrotalcite P3.
Application examples 3
Take 20 parts of P3 to be added in 80 parts of PE, Jing high mixers stirring 10min, being subsequently added into double screw extruder is carried out altogether Mixed extrusion, obtains PE composite X3.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 100 DEG C, the The temperature of two humidity provinces is 190 DEG C, and the temperature of the 3rd humidity province is 190 DEG C, and the temperature of the 4th humidity province is 190 DEG C, and the 5th is warm The temperature in degree area is 190 DEG C, and the temperature of the 6th humidity province is 190 DEG C, and the head temperature of double screw extruder is 190 DEG C, screw rod Rotating speed is 260r/min.
Comparative example 3
80 parts of PE, Jing high mixers stirring 10min are taken, being subsequently added into double screw extruder carries out blending extrusion, obtains PE Composite D3.
PE composites prepared by above-described embodiment 3 and comparative example 3 are made into batten with injection machine, its properties of product data It is as shown in the table:
As can be seen from the above table:
1) antibiotic property of X3 is better than D3, and this explanation adds the effect that silver-colored hydrotalcite-modified PE serves antibacterial that carries.
2) tensile strength of X3, bending strength, cantilever beam impact strength are bigger than D3, and this explanation is added and carries silver-colored neatly Stone act as the nucleator of polyolefin crystallization, promote the heterogeneous nucleation of PE, improve the physical property of PE composites.
Embodiment 4
(1) 120g hydrotalcites, 1.4kg Ag are weighed2SO4Solution, they are put into magnetic stirring apparatus, anti-under the conditions of 70 DEG C Answer 3h.
(2) solution after the completion of reaction is added into deionized water, stands and remove supernatant liquor after 2h, cleaned repeatedly, until BaCl is added dropwise in supernatant liquor2Solution is generated without white depositions.Washed solution is centrifuged by 4200r/min of centrifugation rate 20min。
(3) solid after centrifugation is dried into 2h in drying box, powdered samples are made in 170 DEG C of baking temperature, grinding, i.e., Obtain carrying silver-colored hydrotalcite P4.
Application examples 4
Take 20 parts of P4 to be added in 80 parts of PBT, Jing high mixers stirring 10min, being subsequently added into double screw extruder is carried out Blending extrusion, obtains PBT composite 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 200 DEG C, and the temperature of the 3rd humidity province is 200 DEG C, and the temperature of the 4th humidity province is 200 DEG C, and the 5th is warm The temperature in degree 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 Rotating speed is 250r/min.
Comparative example 4
80 parts of PBT, Jing high mixers stirring 10min are taken, being subsequently added into double screw extruder carries out blending extrusion, obtains PBT composite D4.
PBT composite prepared by above-described embodiment 4 and comparative example 4 is made into batten with injection machine, its properties of product number According to as shown in the table:
As can be seen from the above table:
1) antibiotic property of X4 is better than D4, and this explanation adds the effect that silver-colored hydrotalcite-modified PBT serves antibacterial that carries.
2) tensile strength of X4, bending strength, cantilever beam impact strength are bigger than D4, and this explanation is added and carries silver-colored neatly Stone act as the nucleator of polyolefin crystallization, promote the heterogeneous nucleation of PBT, improve the physical property of PBT composite.
The above is only the description of the preferred embodiment of the present invention, it is noted that due to the finiteness of literal expression, and Objectively there is unlimited concrete structure, for those skilled in the art, without departing from the principle of the invention On the premise of, some improvements and modifications can also be made, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (4)

1. a kind of preparation method of antiseptic, it is characterised in that comprise the following steps:
(1) weigh hydrotalcite to add to Ag2SO4Solution, reacts in magnetic stirring apparatus 2-5h under conditions of 60-90 DEG C of constant temperature;
(2) solution after the completion of reaction is added into deionized water, stands and remove supernatant liquor after 2-3h, cleaned repeatedly, until upper BaCl is added dropwise in layer clear liquid2Solution is generated without white depositions, and washed solution is centrifuged into 20-30min in centrifuge, is centrifuged The rotating speed of machine is 3500-5000r/min;
(3) solid after centrifugation is dried into 2-3h in drying box, baking temperature is 165-180 DEG C, and powder sample is made in grinding Product, that is, obtain carrying silver-colored hydrotalcite.
2. the preparation method of antiseptic according to claim 1, it is characterised in that the hydrotalcite and Ag in step (1)2SO4 The mass ratio of solution is 10-16:120-180.
3. a kind of application of antiseptic, it is characterised in that the antiseptic any one of the claims 1 or 2 is employed In polyolefin.
4. the application of antiseptic according to claim 3, it is characterised in that the polyolefin includes polypropylene, polyphenyl second One or more in alkene, polyethylene or polybutylene terephthalate (PBT).
CN201610921474.9A 2016-10-21 2016-10-21 Preparation method and application of antibacterial agent Pending CN106633190A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109526951A (en) * 2018-11-19 2019-03-29 椤惧缓 A kind of preparation method of antibacterial agent
CN109824974A (en) * 2018-12-24 2019-05-31 万华化学(宁波)有限公司 A kind of halogen-free flame-retardant composite material and preparation method thereof of high flowing antibacterial

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Publication number Priority date Publication date Assignee Title
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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
CN102210325A (en) * 2011-01-27 2011-10-12 深圳市源兴纳米医药科技有限公司 Composite antibacterial powder and preparation method thereof
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Publication number Priority date Publication date Assignee Title
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
CN102125055A (en) * 2010-12-02 2011-07-20 上海纳米技术及应用国家工程研究中心有限公司 Sliver-carried nano-montmorillonite antibacterial agent and preparation method thereof
CN102210325A (en) * 2011-01-27 2011-10-12 深圳市源兴纳米医药科技有限公司 Composite antibacterial powder and preparation method thereof
CN103461382A (en) * 2013-08-08 2013-12-25 广东药学院 Silver-loading modified montmorillonite antibacterial agent, preparation method and application thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109526951A (en) * 2018-11-19 2019-03-29 椤惧缓 A kind of preparation method of antibacterial agent
CN109824974A (en) * 2018-12-24 2019-05-31 万华化学(宁波)有限公司 A kind of halogen-free flame-retardant composite material and preparation method thereof of high flowing antibacterial

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Application publication date: 20170510