CN110477006A - A kind of Antimicrobial preservative erosion nanosphere and preparation method thereof - Google Patents
A kind of Antimicrobial preservative erosion nanosphere and preparation method thereof Download PDFInfo
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- CN110477006A CN110477006A CN201910820183.4A CN201910820183A CN110477006A CN 110477006 A CN110477006 A CN 110477006A CN 201910820183 A CN201910820183 A CN 201910820183A CN 110477006 A CN110477006 A CN 110477006A
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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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
Abstract
The present invention relates to a kind of Antimicrobial preservative erosion nanospheres and preparation method thereof, and using graphene and silver ion as core, organic polymer is that the Antimicrobial preservative of shell loses nanosphere；A kind of Antimicrobial preservative erosion nanosphere produced by the present invention is combined using organic with inorganic material, stability is good, graphene and silver ion are by Coated with Organic Matter when storing state, activity will not be destroyed, when it is to be used, organic matter film automatically opens, and graphene and silver ion are released, and plays the role of good Antimicrobial preservative erosion.
Description
Technical field
The present invention relates to a kind of preparation method of nanosphere, specifically a kind of Antimicrobial preservative erosion nanosphere and its
Preparation method belongs to technical field of composite preparation.
Background technique
Corrosion is a kind of phenomenon that nature is generally existing, constitutes danger very serious to daily life and production
Evil, metal erosion is destruction of the extraneous factor to metal, and metal erosion always since expression, is internally spread, or same
Other parts extend in Shi Xiangbiao.And there is a large amount of bacterium and viral micro-organisms in environment, not only will affect the body of people
The substrates such as metal can also be caused biological corrosion by body health.
Currently, many technologies can prepare active nano microballoon reliable, that size is controllable, usually reacted in liquid-phase system
In be made, and at present nanosphere be mostly inorganic material, be easy it is affected by environment and cause nanosphere activity inactivate, thus shadow
The distinctive function of nanosphere is rung, although existing active nano antibacterial and anticorrosion microballoon reliable performance, size are controllable,
There are still a large amount of problems, especially its storage stability, and over time, nanosphere is easy to appear decomposition, reunites
The disadvantages of.
Chinese patent CN108077250A discloses the complex microsphere with efficient sterilizing performance；Its ingredient includes: acetic acid
Zinc, graphite oxide, sodium hydroxide, potassium permanganate and citric acid；Graphene has excellent mechanics and electric property in the present invention,
ZnO has suitable band structure；Contribute to form uniform particle diameter after doped graphene, the complex microsphere of large specific surface area,
To improve the contact probability of microballoon and bacterium, enhance bactericidal property；Reaction kettle high temperature, high pressure environment facilitate graphite oxide
The graphene of uniform particle diameter is quickly formed, and repeatability is high, it is at low cost；Chinese patent CN106475022A discloses one kind
The preparation method of active antibacterial microballoon, silver nitrate and ascorbic acid are dissolved in respectively in deionized water, are mixed under magnetic stirring
After conjunction, ultrasonic disperse forms microemulsion system, and hydro-thermal reaction then occurs in reaction kettle again, after centrifugation and with water and dehydrated alcohol
It is cleaned, it is dry, it makes annealing treatment under a shielding gas, active antibacterial microballoon is made.Foregoing invention obtains better performances
The problems such as nanosphere, but it is all inorganic material, there are phase tolerances with other organic materials collocation use, and show its performance compared with
It is single.
Summary of the invention
In order to solve the problems existing in the prior art, the purpose of the present invention be intended to provide a kind of Antimicrobial preservative erosion nanosphere and
Preparation method.
Graphene has the specific surface of good thermal conductivity [3000W/ (mK)], very high intensity (110GPa) and super large
Product (2630mz/g) and good Corrosion Protection；And silver ion has good sterilization antibacterial activity.
The present invention relates to a kind of Antimicrobial preservatives to lose nanosphere, and preparation method is as follows:
A, by weight, by 0.2~0.8 part of azodiisobutyronitrile be added to 8.5~16.0 parts of silane coupling agents, 10.0~
Stirring and dissolving in 20.0 parts of hydroxyethyl meth acrylate phosphates, 12.0~25.0 parts of castor oil, then with 10.0~16.0
The ethanol solution mixing of part polyethylene pyrrole network alkanone, is heated to 85 DEG C under nitrogen protection and is stirred to react 14.0~18.0h
Organic nano microballoon is obtained, then with ethanol washing organic nano microballoon and is dried in vacuo；
B, 3.0~7.0 parts of silver nitrates are added in the sulfuric acid of 4.0~8.0 parts of 1mol/L, 0.5~1.0h of ultrasonic disperse, then
10.0~20.0 parts of ethyl alcohol are added, are slow added into 20.0~40.0 parts of deionized waters, 3.5~9.0 parts of sodium hydroxides, 25~
35 DEG C of stirrings are lower to react 3.0~5.0h, 3.0~5.5 parts of hydrogen peroxide is then added, 5.0~8.0h is stirred by ultrasonic to get solution X；
C, it will be filled with nitrogen in autoclave that solution X is transferred to, reaction kettle is put into 130~150 DEG C of baking oven and is reacted
It is taken out after 24.0~28.0h, naturally cools to room temperature, then washed with deionized water and dehydrated alcohol, be dried in vacuo, obtain solid
Ⅰ；
D, resulting solid I, organic nano microballoon and 3.5~8.0 parts of graphene oxides are added to 50.0~80.0 part two
In methyl sulfoxide, ultrasonic disperse is filled with nitrogen in the autoclave then transferred the solution into, reaction kettle is put into 140~
It is taken out after reacting 12.0~16.0h in 160 DEG C of baking ovens, naturally cools to room temperature, then with deionized water and ethanol washing to get anti-
Bacterium anticorrosive nano microballoon.
The graphene oxide is prepared by Hummers method, Staudemaier method or Brodie method；Further, it is
The graphene oxide of Hummers method preparation.
The silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxy third
The combination of one or more of base trimethoxy silane, vinyltriethoxysilane, vinyltrimethoxysilane.
A kind of Antimicrobial preservative erosion nanosphere produced by the present invention has the advantage that
1), a kind of Antimicrobial preservative erosion nanosphere produced by the present invention has antibacterial and anticorrosion dual function, with graphite
Alkene and silver ion are core, and organic polymer is that the Antimicrobial preservative of shell loses nanosphere.
2), a kind of Antimicrobial preservative erosion nanosphere produced by the present invention is combined using organic with inorganic material, stability
Can be good, by Coated with Organic Matter, activity will not be destroyed, when it is to be used, organic for graphene and silver ion when storing state
Object film automatically opens, and graphene and silver ion are released, and plays the role of good Antimicrobial preservative erosion.
Specific embodiment
Present invention combination following instance further retouches the preparation of antibacterial anticorrosive nano microballoon and preparation method thereof
It states.
Embodiment 1
A kind of Antimicrobial preservative erosion nanosphere, preparation method are as follows:
A, 0.5 part of azodiisobutyronitrile by weight, is added to 12.0 parts of vinyltriethoxysilane, 14.0 parts of hydroxyl second
Stirring and dissolving in methyl acrylate phosphate, 18.0 parts of castor oil, it is then anhydrous with 12.0 parts of polyethylene pyrrole network alkanones
Ethanol solution mixing, is heated to 85 DEG C and is stirred to react 16h obtaining organic nano microballoon under nitrogen protection, then uses ethanol washing
Organic nano microballoon is simultaneously dried in vacuo；
B, 5.0 parts of silver nitrates are added in the sulfuric acid of 6.0 parts of 1mol/L, ultrasonic disperse 1.0h, 15.0 parts of ethyl alcohol are then added,
30.0 parts of deionized waters, 6.2 parts of sodium hydroxides are slow added into, react 4.0h under 25~35 DEG C of stirrings, are then added 4.0 parts
7.0h is stirred by ultrasonic to get solution X in hydrogen peroxide；
C, it will be filled with nitrogen in autoclave that solution X is transferred to, reaction kettle is put into after reacting 28h in 140 DEG C of baking oven
It takes out, naturally cools to room temperature, then washed with deionized water and dehydrated alcohol, be dried in vacuo, obtain solid I；
D, resulting solid I, organic nano microballoon and 6.0 parts of graphene oxides are added in 65.0 parts of dimethyl sulfoxides,
Ultrasonic disperse is filled with nitrogen in the autoclave then transferred the solution into, reaction kettle is put into 160 DEG C of baking ovens and is reacted
It is taken out after 14.0h, naturally cools to room temperature, then lose nanosphere with deionized water and ethanol washing to get Antimicrobial preservative.
Embodiment 2
A kind of Antimicrobial preservative erosion nanosphere, preparation method are as follows:
A, 0.4 part of azodiisobutyronitrile by weight, is added to 8.5 parts of γ-glycidyl ether oxygen propyl trimethoxy silicon
Alkane, 13.0 parts of hydroxyethyl meth acrylate phosphates, stirring and dissolving in 16.0 parts of castor oil, then with 11.0 parts of polyethylene pyrroles
The ethanol solution of network alkanone mixes, and is heated to 85 DEG C under nitrogen protection and is stirred to react 18.0h obtaining organic nano microballoon,
Then it with ethanol washing organic nano microballoon and is dried in vacuo；
B, 6.0 parts of silver nitrates are added in the sulfuric acid of 6.0 parts of 1mol/L, ultrasonic disperse 1.0h, 18.0 parts of ethyl alcohol are then added,
32.0 parts of deionized waters, 6.5 parts of sodium hydroxides are slow added into, react 4.0h under 25~35 DEG C of stirrings, are then added 3.5 parts
6.0h is stirred by ultrasonic to get solution X in hydrogen peroxide；
C, it will be filled with nitrogen in autoclave that solution X is transferred to, reaction kettle is put into 145 DEG C of baking oven and reacts 28.0h
After take out, naturally cool to room temperature, then washed with deionized water and dehydrated alcohol, be dried in vacuo, obtain solid I；
D, resulting solid I, organic nano microballoon and 4.5 parts of graphene oxides are added in 65.0 parts of dimethyl sulfoxides,
Ultrasonic disperse is filled with nitrogen in the autoclave then transferred the solution into, reaction kettle is put into 160 DEG C of baking ovens and is reacted
It is taken out after 14.0h, naturally cools to room temperature, then lose nanosphere with deionized water and ethanol washing to get Antimicrobial preservative.
Embodiment 3
A kind of Antimicrobial preservative erosion nanosphere, preparation method are as follows:
A, 0.6 part of azodiisobutyronitrile by weight, is added to 16.0 parts of γ-methacryloxypropyl trimethoxy
Silane, 11.0 parts of hydroxyethyl meth acrylate phosphates, stirring and dissolving in 20.0 parts of castor oil, then with 14.0 parts of polyethylene
The ethanol solution of pyrrole network alkanone mixes, and is heated to 85 DEG C under nitrogen protection and is stirred to react 16.0h to obtain organic nano micro-
Then ball with ethanol washing organic nano microballoon and is dried in vacuo；
B, 6.5 parts of silver nitrates are added in the sulfuric acid of 7.0 parts of 1mol/L, ultrasonic disperse 1.0h, 18.0 parts of ethyl alcohol are then added,
35.0 parts of deionized waters, 7.3 parts of sodium hydroxides are slow added into, react 5.0h under 25~35 DEG C of stirrings, are then added 5.0 parts
8.0h is stirred by ultrasonic to get solution X in hydrogen peroxide；
C, it will be filled with nitrogen in autoclave that solution X is transferred to, reaction kettle is put into 150 DEG C of baking oven after reaction 26.0
It takes out, naturally cools to room temperature, then washed with deionized water and dehydrated alcohol, be dried in vacuo, obtain solid I；
D, resulting solid I, organic nano microballoon and 7.0 parts of graphene oxides are added in 72.0 parts of dimethyl sulfoxides,
Ultrasonic disperse is filled with nitrogen in the autoclave then transferred the solution into, reaction kettle is put into 160 DEG C of baking ovens and is reacted
It is taken out after 14.0h, naturally cools to room temperature, then lose nanosphere with deionized water and ethanol washing to get Antimicrobial preservative.
Embodiment 4
A kind of Antimicrobial preservative erosion nanosphere, preparation method are as follows:
A, 0.3 part of azodiisobutyronitrile by weight, is added to 9.0 parts of vinyltrimethoxysilanes, 12.0 parts of hydroxyl second
Stirring and dissolving in methyl acrylate phosphate, 12.0 parts of castor oil, it is then anhydrous with 11.0 parts of polyethylene pyrrole network alkanones
Ethanol solution mixing, is heated to 85 DEG C and is stirred to react 16.0h obtaining organic nano microballoon under nitrogen protection, is then washed with ethyl alcohol
It washs organic nano microballoon and is dried in vacuo；
B, 3.5 parts of silver nitrates are added in the sulfuric acid of 5.5 parts of 1mol/L, 0.5~1.0h of ultrasonic disperse, are then added 13.0 parts
Ethyl alcohol is slow added into 26.0 parts of deionized waters, 6.0 parts of sodium hydroxides, reacts 5.0h under 25~35 DEG C of stirrings, is then added
3.5 parts of hydrogen peroxide ultrasonic agitation 7.0h are to get solution X；
C, it will be filled with nitrogen in autoclave that solution X is transferred to, reaction kettle is put into 150 DEG C of baking oven and reacts 26.0h
After take out, naturally cool to room temperature, then washed with deionized water and dehydrated alcohol, be dried in vacuo, obtain solid I；
D, resulting solid I, organic nano microballoon and 4.2 parts of graphene oxides are added in 60.0 parts of dimethyl sulfoxides,
Ultrasonic disperse is filled with nitrogen in the autoclave then transferred the solution into, reaction kettle is put into 160 DEG C of baking ovens and is reacted
It is taken out after 14.0h, naturally cools to room temperature, then lose nanosphere with deionized water and ethanol washing to get Antimicrobial preservative.
Although the present invention has described it in detail and cited embodiments, but for those of ordinary skill in the art, show
Various schemes, modification and the change that can so make as specified above, should be construed as being included within the scope of the claims.
Claims (3)
1. a kind of Antimicrobial preservative erosion nanosphere and preparation method thereof, preparation step is as follows:
A, by weight, by 0.2~0.8 part of azodiisobutyronitrile be added to 8.5~16.0 parts of silane coupling agents, 10.0~
Stirring and dissolving in 20.0 parts of hydroxyethyl meth acrylate phosphates, 12.0~25.0 parts of castor oil, then with 10.0~16.0
The ethanol solution mixing of part polyethylene pyrrole network alkanone, is heated to 85 DEG C under nitrogen protection and is stirred to react 14.0~18.0h
Organic nano microballoon is obtained, then with ethanol washing organic nano microballoon and is dried in vacuo；
B, 3.0~7.0 parts of silver nitrates are added in the sulfuric acid of 4.0~8.0 parts of 1mol/L, 0.5~1.0h of ultrasonic disperse, then
10.0~20.0 parts of ethyl alcohol are added, are slow added into 20.0~40.0 parts of deionized waters, 3.5~9.0 parts of sodium hydroxides, 25~
35 DEG C of stirrings are lower to react 3.0~5.0h, 3.0~5.5 parts of hydrogen peroxide is then added, 5.0~8.0h is stirred by ultrasonic to get solution X；
C, it will be filled with nitrogen in autoclave that solution X is transferred to, reaction kettle is put into 130~150 DEG C of baking oven and is reacted
It is taken out after 24.0~28.0h, naturally cools to room temperature, then washed with deionized water and dehydrated alcohol, be dried in vacuo, obtain solid
Ⅰ；
D, resulting solid I, organic nano microballoon and 3.5~8.0 parts of graphene oxides are added to 50.0~80.0 part two
In methyl sulfoxide, ultrasonic disperse is filled with nitrogen in the autoclave then transferred the solution into, reaction kettle is put into 140~
It is taken out after reacting 12.0~16.0h in 160 DEG C of baking ovens, naturally cools to room temperature, then with deionized water and ethanol washing to get anti-
Bacterium anticorrosive nano microballoon.
2. a kind of Antimicrobial preservative as described in claim 1 loses nanosphere, it is characterised in that: the graphene oxide, by
Hummers method, Staudemaier method or the preparation of Brodie method；It further, is the graphene oxide of Hummers method preparation.
3. a kind of Antimicrobial preservative as described in claim 1 loses nanosphere, it is characterised in that: the silane coupling agent is
γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, three second of vinyl
The combination of one or more of oxysilane, vinyltrimethoxysilane.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310388A (en) * | 2014-10-15 | 2015-01-28 | 宁波墨西科技有限公司 | Graphene composite powder material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310388A (en) * | 2014-10-15 | 2015-01-28 | 宁波墨西科技有限公司 | Graphene composite powder material and preparation method thereof |
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Application publication date: 20191122 |