CN107652518A - A kind of preparation method of novel antibacterial material - Google Patents
A kind of preparation method of novel antibacterial material Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of novel antibacterial material, polyethylene, Cu MOF Al2O3Nano material, Ethyl formate, PLA, sodium carbonate, lauryl betaine, sodium tripolyphosphate and sodium xylene sulfonate are primary raw material, double-decker platform is built by MOF organic ligands, it will be hidden on polyethylene under " clean " surface of a stable against biological contamination, under dry conditions, the dehydration of outermost molecular brush surface is caved in, the antibacterial polymer of inside is set to be killed in a manner of contact sterilization by gas, the bacterium that the approach such as drop are propagated, in aqueous phase condition, outer layer amphiphilic polymers form hydrated sheath, the adhesion of bacterium in effective suppression solution, improve the anti-microbial property of material, the preparation method of the present invention is green, have fewer environmental impacts, and the material prepared is respectively provided with preferable antibacterial effect to Escherichia coli and staphylococcus.
Description
Technical field
Invention is related to a kind of preparation method of novel antibacterial material, belongs to medical material preparation field.
Background technology
With the raising of human life quality, the research of anti-biotic material has obtained fast development, but presently used anti-
The anti-microbial property of bacterium material is unsatisfactory, and general antibiotic rate can reach 80%, and with the continuous progress of technology, for antibacterial material
The requirement of material also more and more higher, therefore it is stronger to need to develop a kind of excellent combination property, anti-microbial property, while to life entity or ring
The harmless medical material in border.
The content of the invention
It is an object of the invention to provide a kind of novel antibacterial material and preparation method thereof, the material prepared by this method
With excellent antibacterial effect.
A kind of preparation method of novel antibacterial material, this method comprise the following steps：
Step 1, by 65 parts of polyethylene, 13 parts of Cu-MOF-Al2O3Nano material, 3 parts of Ethyl formates and 5 parts of PLAs are added to
In reactor, 1 part of sodium carbonate, 5 parts of lauryl betaines, 1 part of sodium tripolyphosphate and 0.8 part of sodium xylene sulfonate are dissolved in 30 parts
In water, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is
150 revs/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then rise
Temperature stirring reaction 30 minutes, obtains head product to 130 DEG C；
Step 2,1.5 parts of antioxidant BHTs and 1.3 parts of aid anti-oxidants DLTP are added in the head product that step 1 obtains, in temperature
Spend to be uniformly mixed under the conditions of 80 DEG C, mixing speed is 200 revs/min, and mixing time is 30 minutes；
Step 3, the mixture for obtaining step 2 are extruded in double screw extruder, and extrusion condition is after twin screw extruder barrel
Duan Wendu divides three stage control, controls respectively at 180 DEG C, 185 DEG C and 190 DEG C, barrel front-end temperature divides three stage control, controls respectively
At 195 DEG C, 200 DEG C and 210 DEG C, head temperature is divided to two sections of controls, controls respectively in 230 DEG C and 236 DEG C, finally gives medical receive
Nano antibacterial composite.
Described Cu-MOF-Al2O3Preparation method of nano material is as follows：
Step 1, by 10 parts of alumina powders, 0.3 part of Sodium Polyacrylate, 19.4 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part of yittrium oxide
Mixing is put into flask, the uniform stirring at 75 DEG C, obtains slurry；
Step 2, slurry poured into mould, placed at -16 DEG C, obtain being shaped to the aluminum oxide porous particle preform of column；
Step 3, by aluminum oxide porous particle preform first 12h is placed at -16 DEG C, then put it into freeze drier -
6h is dried under the conditions of 60 DEG C, high temperature sintering is finally carried out with 4 DEG C/min speed heating, is warming up to 1000 DEG C, is incubated 3h, cooling
After obtain porous oxidation aluminum substrate；
Step 4,4.2 parts of trimesic acids are taken, be added in the ethanol solution of 25 parts of mass fractions 95%, treated as ligand solution
With；
Step 5, the porous oxidation aluminum substrate prepared impregnated into 5h in enough above-mentioned ligand solutions；
Step 6, the nitric acid that enough concentration is 0.5 mol/L will be put into after the good porous oxidation aluminum substrate filtering of above-mentioned dipping
In copper solution, 22h is reacted in 80 DEG C of oil baths and under the conditions of condensing reflux, is filtered, is dried（Dry temperature is 100 DEG C）,
The dry time is 12h）After obtain Cu-MOF-Al2O3Nano material.
Beneficial effect：The invention provides a kind of brand-new nano anti-biotic material, the material use Woelm Alumina and Cu-
MOF is in-situ cross-linked to form the matrices of composite material with network structure, and in matrix material forming process, in matrix material
Copper ion may be homogenously dispersed in the network structure of matrix crosslinking, improve the antibacterial stability of material；MOF organic ligands structure is double
Rotating fields platform, it will be hidden on polyethylene under " clean " surface of a stable against biological contamination, it is outermost under dry conditions
The dehydration of molecular brush surface is caved in, and the antibacterial polymer of inside is killed in a manner of contact sterilization and is propagated by approach such as gas, drops
Bacterium, in aqueous phase condition, outer layer amphiphilic polymers form hydrated sheath, in effective suppression solution（Such as blood, urine）Bacterium
Adhesion；In addition, Cu-MOF-Al2O3Coating can directly be contacted with isolated cell, blood constitutent with stenlizing layer, improve antibacterial
The biocompatibility on surface；The preparation method of the present invention is green, has fewer environmental impacts, and the material prepared is to large intestine bar
Bacterium and staphylococcus are respectively provided with preferable antibacterial effect.
Embodiment
Embodiment 1
A kind of preparation method of novel antibacterial material, this method comprise the following steps：
Step 1, by 65 parts of polyethylene, 13 parts of Cu-MOF-Al2O3Nano material, 3 parts of Ethyl formates and 5 parts of PLAs are added to
In reactor, 1 part of sodium carbonate, 5 parts of lauryl betaines, 1 part of sodium tripolyphosphate and 0.8 part of sodium xylene sulfonate are dissolved in 30 parts
In water, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is
150 revs/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then rise
Temperature stirring reaction 30 minutes, obtains head product to 130 DEG C；
Step 2,1.5 parts of antioxidant BHTs and 1.3 parts of aid anti-oxidants DLTP are added in the head product that step 1 obtains, in temperature
Spend to be uniformly mixed under the conditions of 80 DEG C, mixing speed is 200 revs/min, and mixing time is 30 minutes；
Step 3, the mixture for obtaining step 2 are extruded in double screw extruder, and extrusion condition is after twin screw extruder barrel
Duan Wendu divides three stage control, controls respectively at 180 DEG C, 185 DEG C and 190 DEG C, barrel front-end temperature divides three stage control, controls respectively
At 195 DEG C, 200 DEG C and 210 DEG C, head temperature is divided to two sections of controls, controls respectively in 230 DEG C and 236 DEG C, finally gives medical receive
Nano antibacterial composite.
Described Cu-MOF-Al2O3Preparation method of nano material is as follows：
Step 1, by 10 parts of alumina powders, 0.3 part of Sodium Polyacrylate, 19.4 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part of yittrium oxide
Mixing is put into flask, the uniform stirring at 75 DEG C, obtains slurry；
Step 2, slurry poured into mould, placed at -16 DEG C, obtain being shaped to the aluminum oxide porous particle preform of column；
Step 3, by aluminum oxide porous particle preform first 12h is placed at -16 DEG C, then put it into freeze drier -
6h is dried under the conditions of 60 DEG C, high temperature sintering is finally carried out with 4 DEG C/min speed heating, is warming up to 1000 DEG C, is incubated 3h, cooling
After obtain porous oxidation aluminum substrate；
Step 4,4.2 parts of trimesic acids are taken, be added in the ethanol solution of 25 parts of mass fractions 95%, treated as ligand solution
With；
Step 5, the porous oxidation aluminum substrate prepared impregnated into 5h in enough above-mentioned ligand solutions；
Step 6, the nitric acid that enough concentration is 0.5 mol/L will be put into after the good porous oxidation aluminum substrate filtering of above-mentioned dipping
In copper solution, 22h is reacted in 80 DEG C of oil baths and under the conditions of condensing reflux, is filtered, is dried（Dry temperature is 100 DEG C）,
The dry time is 12h）After obtain Cu-MOF-Al2O3Nano material.
Embodiment 2
Step 1, by 50 parts of polyethylene, 16 parts of Cu-MOF-Al2O3Nano material, 4 parts of Ethyl formates and 5 parts of PLAs are added to
In reactor, 1 part of sodium carbonate, 5 parts of lauryl betaines, 1 part of sodium tripolyphosphate and 0.8 part of sodium xylene sulfonate are dissolved in 30 parts
In water, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is
150 revs/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then rise
Temperature stirring reaction 30 minutes, obtains head product to 130 DEG C；
Remaining is prepared and embodiment 1 is identical.
Embodiment 3
Step 1, step 1, by 45 parts of polyethylene, 23 parts of Cu-MOF-Al2O3Nano material, 6 parts of Ethyl formates and 5 parts of PLAs
It is added in reactor, 1 part of sodium carbonate, 5 parts of lauryl betaines, 1 part of sodium tripolyphosphate and 0.8 part of sodium xylene sulfonate is molten
In 30 parts of water, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the stirring speed being uniformly mixed
To spend for 150 revs/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes,
130 DEG C are warming up to again, stirring reaction 30 minutes, obtain head product；
Remaining is prepared and embodiment 1 is identical.
Embodiment 4
Step 1, by 38 parts of polyethylene, 19 parts of Cu-MOF-Al2O3Nano material, 3 parts of Ethyl formates and 5 parts of PLAs are added to
In reactor, 1 part of sodium carbonate, 5 parts of lauryl betaines, 1 part of sodium tripolyphosphate and 0.8 part of sodium xylene sulfonate are dissolved in 30 parts
In water, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is
150 revs/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then rise
Temperature stirring reaction 30 minutes, obtains head product to 130 DEG C；
Remaining is prepared and embodiment 1 is identical.
Embodiment 5
Step 1, by 17 parts of polyethylene, 3 parts of Cu-MOF-Al2O3Nano material, 3 parts of Ethyl formates and 5 parts of PLAs are added to instead
Answer in kettle, 1 part of sodium carbonate, 5 parts of lauryl betaines, 1 part of sodium tripolyphosphate and 0.8 part of sodium xylene sulfonate are dissolved in 30 parts of water
In, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is 150
Rev/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then heat up
To 130 DEG C, stirring reaction 30 minutes, head product is obtained；
Remaining is prepared and embodiment 1 is identical.
Embodiment 6
Step 1, by 65 parts of polyethylene, 13 parts of Cu-MOF-Al2O3Nano material, 5 parts of Ethyl formates and 1 part of PLA are added to
In reactor, 4 parts of sodium carbonate, 3 parts of lauryl betaines, 6 parts of sodium tripolyphosphates and 0.8 part of sodium xylene sulfonate are dissolved in 30 parts
In water, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is
150 revs/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then rise
Temperature stirring reaction 30 minutes, obtains head product to 130 DEG C；
Remaining is prepared and embodiment 1 is identical.
Embodiment 7
Step 1, by 34 parts of polyethylene, 23 parts of Cu-MOF-Al2O3Nano material, 8 parts of Ethyl formates and 5 parts of PLAs are added to
In reactor, 1 part of sodium carbonate, 5 parts of lauryl betaines, 1 part of sodium tripolyphosphate and 0.8 part of sodium xylene sulfonate are dissolved in 30 parts
In water, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is
150 revs/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then rise
Temperature stirring reaction 30 minutes, obtains head product to 130 DEG C；
Remaining is prepared and embodiment 1 is identical.
Embodiment 8
Step 1, by 34 parts of polyethylene, 17 parts of Cu-MOF-Al2O3Nano material, 3 parts of Ethyl formates and 5 parts of PLAs are added to
In reactor, 1 part of sodium carbonate, 5 parts of lauryl betaines, 6 parts of sodium tripolyphosphates and 4 parts of sodium xylene sulfonates are dissolved in 30 parts of water
In, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is 150
Rev/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then heat up
To 130 DEG C, stirring reaction 30 minutes, head product is obtained；
Remaining is prepared and embodiment 1 is identical.
Embodiment 9
Step 1, by 65 parts of polyethylene, 23 parts of Cu-MOF-Al2O3Nano material, 3 parts of Ethyl formates and 5 parts of PLAs are added to
In reactor, 3 parts of sodium carbonate, 1 part of lauryl betaine, 1 part of sodium tripolyphosphate and 2.1 parts of sodium xylene sulfonates are dissolved in 30 parts
In water, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is
150 revs/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then rise
Temperature stirring reaction 30 minutes, obtains head product to 130 DEG C；
Remaining is prepared and embodiment 1 is identical.
Embodiment 10
Step 1, by 75 parts of polyethylene, 37 parts of Cu-MOF-Al2O3Nano material, 3 parts of Ethyl formates and 5 parts of PLAs are added to
In reactor, 1 part of sodium carbonate, 8 parts of lauryl betaines, 1 part of sodium tripolyphosphate and 0.8 part of sodium xylene sulfonate are dissolved in 30 parts
In water, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is
150 revs/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then rise
Temperature stirring reaction 30 minutes, obtains head product to 130 DEG C；
Remaining is prepared and embodiment 1 is identical.
Embodiment 11
Step 1, by 65 parts of polyethylene, 13 parts of Cu-MOF-Al2O3Nano material, 8 parts of modified carbon fibers, 3 parts of Ethyl formates and 5
Part PLA is added in reactor, by 1 part of sodium carbonate, 5 parts of lauryl betaines, 1 part of sodium tripolyphosphate and 0.8 part of dimethylbenzene
Sodium sulfonate is dissolved in 30 parts of water, is then added in reactor, is uniformly mixed under the conditions of 50 DEG C, wherein being uniformly mixed
Mixing speed be 150 revs/min, incorporation time be 30 minutes, then vacuum be 0.01MPa under be warming up to 80 DEG C, stir
Mix 20 minutes, then be warming up to 130 DEG C, stirring reaction 30 minutes, obtain head product；
Remaining is prepared and embodiment 1 is identical.
Described modified carbon fiber preparation method is as follows：
Carbon fiber is placed in acetone soln and soaks 12h, is filtered, deionized water is washed 3 times, is dried in 120 DEG C of blast driers
4h, with 60% nitric acid reflux oxidation carbon fiber 7h, filtering, deionized water washing PH=6, dried extremely in 120 DEG C of blast driers
Constant weight；The carbon fiber of nitric acid oxidation is placed in polyvinylpyrrolidone, lauryl sodium sulfate and equivalent to its total weight parts
In the solution of 12 times of deionized water configuration, ultrasonic 50min, 60 DEG C of dryings, the carbon fiber of surface modification is obtained.
Reference examples 1
It is with the difference of embodiment 1：In the step 2 of antimicrobial nano material, by 2 parts of antioxidant BHTs and 0.3 part of aid anti-oxidants
DLTP is added in the head product that step 1 obtains, and remaining step is identical with embodiment 1.
Reference examples 2
It is with the difference of embodiment 1：In the step 2 of antimicrobial nano material, by 0.3 part of antioxidant BHT and 2 parts of aid anti-oxidants
DLTP is added in the head product that step 1 obtains, and remaining step is identical with embodiment 1.
Reference examples 3
It is with the difference of embodiment 1：In the step 3 of antimicrobial nano material, the three sections of controls of twin screw extruder barrel back segment temperature point
System, is controlled at 150 DEG C, 155 DEG C and 160 DEG C, remaining step is identical with embodiment 1 respectively.
Reference examples 4
It is with the difference of embodiment 1：In the step 3 of antimicrobial nano material, the three sections of controls of twin screw extruder barrel back segment temperature point
System, is controlled at 190 DEG C, 195 DEG C and 200 DEG C, remaining step is identical with embodiment 1 respectively.
Reference examples 5
It is with the difference of embodiment 1：Cu-MOF-Al2O3In step 1 prepared by nano material, 8 parts of alumina powders, 3 parts are gathered
PAA, 14 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part of yittrium oxide mixing are put into flask, the uniform stirring at 75 DEG C, are obtained
It is identical with embodiment 1 to slurry, remaining step.
Reference examples 6
It is with the difference of embodiment 1：Cu-MOF-Al2O3In step 1 prepared by nano material, by 16 parts of alumina powders, 0.1
Part Sodium Polyacrylate, 6 parts of camphenes, 9 parts of tert-butyl alcohols and 3 parts of yittrium oxide mixing are put into flask, the uniform stirring at 75 DEG C, are obtained
Slurry, remaining step are identical with embodiment 1.
Reference examples 7
It is with the difference of embodiment 1：Cu-MOF-Al2O3Nano material prepare step 3 in, be put into freeze drier-
6h is dried under the conditions of 60 DEG C, high temperature sintering is finally carried out with 15 DEG C/min speed heating, 1000 DEG C is warming up to, is incubated 3h, its
Remaining step is identical with embodiment 1.
Reference examples 8
It is with the difference of embodiment 1：Cu-MOF-Al2O3Nano material prepare step 3 in, be put into freeze drier-
6h is dried under the conditions of 60 DEG C, high temperature sintering is finally carried out with 25 DEG C/min speed heating, 1000 DEG C is warming up to, is incubated 3h, its
Remaining step is identical with embodiment 1.
Reference examples 9
It is with the difference of embodiment 1：Cu-MOF-Al2O3In step 3 prepared by nano material, by good porous of above-mentioned dipping
It is put into after alumina substrate filtering in the copper nitrate solution that enough concentration is 0.01mol/L, remaining step and embodiment 1 are complete
It is exactly the same.
Reference examples 10
It is with the difference of embodiment 1：Cu-MOF-Al2O3In step 3 prepared by nano material, by good porous of above-mentioned dipping
It is put into after alumina substrate filtering in the copper nitrate solution that enough concentration is 1.0mol/L, remaining step and embodiment 1 are complete
It is exactly the same.
The anti-biotic material that above example and reference examples are prepared carries out performance test, and its antibacterial after testing the 100th day
Effect is as a result as follows；
Test result
Test result indicates that novel antibacterial material provided by the invention has good antibacterial effect, material is in standard test condition
Under, Bacteria suppression rate is lower, illustrates good anti-bacterial effect, conversely, effect is poorer；Embodiment 1 arrives embodiment 10, staphylococcus and
Escherichia coli inhibiting rate changes the proportioning of each raw material composition in anti-biotic material, to the anti-microbial property of material respectively more than 85%
There are different degrees of influence, polyethylene and Cu-MOF-Al2O3Nano material quality proportioning is 5：1, other dispensing dosages are fixed
When, antibacterial effect is best；It is worth noting that embodiment 11 adds modified carbon fiber, antibacterial effect significantly improves, and antibacterial
Stability keeps unusual outstanding, illustrates modified carbon fiber to Cu-MOF-Al2O3Nanometer insulation layer structure anti-microbial property with
And stability has more preferable optimization function；Reference examples 1 to reference examples 2 change antimicrobial nano material against oxidative agent dosage, antibacterial effect
Fruit is decreased obviously, and illustrates that the dosage of antioxidant and pro-oxidant produces material impact to the antibiotic property of material；Reference examples 3 and right
As usual 4, change the height of three stage control temperature, the material bacteria inhibiting rate of synthesis is still very low, and anti-microbial property is bad；Reference examples
5 change Cu-MOF-Al to reference examples 82O3The raw material proportioning and heating rate of nano material, effect is also bad, illustrates the group of raw material
Into with temperature-rise period to Cu-MOF-Al2O3Nano material obtains compound have a major impact；Reference examples 9 and example 10 change in dipping process
The concentration of copper nitrate solution, antibacterial effect substantially reduce, illustrate copper nitrate it is excessive it is very few all can be to the Bacteria suppression rate shadow of material
Sound is very big；Therefore the novel antibacterial material prepared using the present invention has good antibacterial effect.
Claims (2)
1. a kind of preparation method of novel antibacterial material, it is characterised in that this method comprises the following steps：
Step 1, by 65 parts of polyethylene, 13 parts of Cu-MOF-Al2O3Nano material, 3 parts of Ethyl formates and 5 parts of PLAs are added to instead
Answer in kettle, 1 part of sodium carbonate, 5 parts of lauryl betaines, 1 part of sodium tripolyphosphate and 0.8 part of sodium xylene sulfonate are dissolved in 30 parts of water
In, then add in reactor, be uniformly mixed under the conditions of 50 DEG C, wherein the mixing speed being uniformly mixed is 150
Rev/min, incorporation time is 30 minutes, is then warming up to 80 DEG C in the case where vacuum is 0.01MPa, stirs 20 minutes, then heat up
To 130 DEG C, stirring reaction 30 minutes, head product is obtained；
Step 2,1.5 parts of antioxidant BHTs and 1.3 parts of aid anti-oxidants DLTP are added in the head product that step 1 obtains, in temperature
Spend to be uniformly mixed under the conditions of 80 DEG C, mixing speed is 200 revs/min, and mixing time is 30 minutes；
Step 3, the mixture for obtaining step 2 are extruded in double screw extruder, and extrusion condition is after twin screw extruder barrel
Duan Wendu divides three stage control, controls respectively at 180 DEG C, 185 DEG C and 190 DEG C, barrel front-end temperature divides three stage control, controls respectively
At 195 DEG C, 200 DEG C and 210 DEG C, head temperature is divided to two sections of controls, controls respectively in 230 DEG C and 236 DEG C, finally gives medical receive
Nano antibacterial composite.
A kind of 2. preparation method of novel antibacterial material according to claim 1, it is characterised in that it is described,
Described Cu-MOF-Al2O3Preparation method of nano material is as follows：
Step 1, by 10 parts of alumina powders, 0.3 part of Sodium Polyacrylate, 19.4 parts of camphenes, 2.9 parts of tert-butyl alcohols and 0.5 part of yittrium oxide
Mixing is put into flask, the uniform stirring at 75 DEG C, obtains slurry；
Step 2, slurry poured into mould, placed at -16 DEG C, obtain being shaped to the aluminum oxide porous particle preform of column；
Step 3, by aluminum oxide porous particle preform first 12h is placed at -16 DEG C, then put it into freeze drier -
6h is dried under the conditions of 60 DEG C, high temperature sintering is finally carried out with 4 DEG C/min speed heating, is warming up to 1000 DEG C, is incubated 3h, cooling
After obtain porous oxidation aluminum substrate；
Step 4,4.2 parts of trimesic acids are taken, be added in the ethanol solution of 25 parts of mass fractions 95%, treated as ligand solution
With；
Step 5, the porous oxidation aluminum substrate prepared impregnated into 5h in enough above-mentioned ligand solutions；
Step 6, the nitric acid that enough concentration is 0.5 mol/L will be put into after the good porous oxidation aluminum substrate filtering of above-mentioned dipping
In copper solution, 22h to be reacted in 80 DEG C of oil baths and under the conditions of condensing reflux, is filtered, is dried, the dry time is 12h, after
To Cu-MOF-Al2O3Nano material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110157085A (en) * | 2019-05-16 | 2019-08-23 | 广州大学 | A kind of antibiotic plastic and preparation method thereof using ZIF-8 |
| CN112056313A (en) * | 2020-08-31 | 2020-12-11 | 中国科学院地球环境研究所 | Method for aqueous phase synthesis of nano Cu-MOF (copper-metal organic framework) bacteriostatic agent |
| CN112959786A (en) * | 2021-03-22 | 2021-06-15 | 四川汇利实业有限公司 | Oral liquid PET-PCTFE-PE composite hard sheet and preparation method thereof |
| CN114773864A (en) * | 2022-04-18 | 2022-07-22 | 宁波长阳科技股份有限公司 | Composite material based on zirconium-based organic framework compound and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1294145A (en) * | 1999-11-02 | 2001-05-09 | 海尔科化工程塑料国家工程研究中心有限公司 | Resin composition containing antibacterial mildew inhibitor and its preparing process |
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- 2017-10-29 CN CN201711029044.7A patent/CN107652518A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1294145A (en) * | 1999-11-02 | 2001-05-09 | 海尔科化工程塑料国家工程研究中心有限公司 | Resin composition containing antibacterial mildew inhibitor and its preparing process |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110157085A (en) * | 2019-05-16 | 2019-08-23 | 广州大学 | A kind of antibiotic plastic and preparation method thereof using ZIF-8 |
| CN112056313A (en) * | 2020-08-31 | 2020-12-11 | 中国科学院地球环境研究所 | Method for aqueous phase synthesis of nano Cu-MOF (copper-metal organic framework) bacteriostatic agent |
| CN112056313B (en) * | 2020-08-31 | 2021-11-16 | 中国科学院地球环境研究所 | Method for aqueous phase synthesis of nano Cu-MOF (copper-metal organic framework) bacteriostatic agent |
| CN112959786A (en) * | 2021-03-22 | 2021-06-15 | 四川汇利实业有限公司 | Oral liquid PET-PCTFE-PE composite hard sheet and preparation method thereof |
| CN114773864A (en) * | 2022-04-18 | 2022-07-22 | 宁波长阳科技股份有限公司 | Composite material based on zirconium-based organic framework compound and preparation method and application thereof |
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