CN115806297A - Preparation method of antibacterial hydrophobic silica aerogel composite material - Google Patents
Preparation method of antibacterial hydrophobic silica aerogel composite material Download PDFInfo
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- CN115806297A CN115806297A CN202211527426.3A CN202211527426A CN115806297A CN 115806297 A CN115806297 A CN 115806297A CN 202211527426 A CN202211527426 A CN 202211527426A CN 115806297 A CN115806297 A CN 115806297A
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- copper
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- acid
- composite material
- silica aerogel
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 56
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 43
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 20
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 18
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000012986 modification Methods 0.000 claims abstract description 6
- 230000004048 modification Effects 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 239000004964 aerogel Substances 0.000 claims description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 150000001879 copper Chemical class 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000017 hydrogel Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 5
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 5
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 5
- SCGJLFGXXZTXSX-UHFFFAOYSA-N copper;ethanol Chemical compound [Cu].CCO SCGJLFGXXZTXSX-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- ZKXWKVVCCTZOLD-UHFFFAOYSA-N copper;4-hydroxypent-3-en-2-one Chemical compound [Cu].CC(O)=CC(C)=O.CC(O)=CC(C)=O ZKXWKVVCCTZOLD-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000499 gel Substances 0.000 abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000011068 loading method Methods 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000010703 silicon Substances 0.000 abstract description 3
- 239000000741 silica gel Substances 0.000 abstract description 2
- 229910002027 silica gel Inorganic materials 0.000 abstract description 2
- 238000011282 treatment Methods 0.000 abstract description 2
- 238000007605 air drying Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000010586 diagram Methods 0.000 description 8
- 210000004027 cell Anatomy 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 238000003795 desorption Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001963 growth medium Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008827 biological function Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- YDRFJPRPCBJKCM-UHFFFAOYSA-L dichlorocopper ethanol Chemical compound C(C)O.[Cu](Cl)Cl YDRFJPRPCBJKCM-UHFFFAOYSA-L 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of an antibacterial hydrophobic silica aerogel composite material, which comprises the steps of taking tetraethyl orthosilicate as a silicon source, adding deionized water and absolute ethyl alcohol to prepare silica gel, and carrying out five subsequent treatments of silica framework aging, solvent exchange, gel surface hydrophobic modification, normal pressure forced air drying, copper ion loading and the like at a certain temperature to obtain the antibacterial hydrophobic silica aerogel composite material.
Description
Technical Field
The invention belongs to the technical field of antibacterial composite materials, and particularly relates to a preparation method of an antibacterial hydrophobic silica aerogel composite material.
Background
Silica aerogel is a highly cross-linked porous network material whose structure is substantially filled with gas and is also the most representative aerogel material. Silica aerogel plays an important role in the fields of thermal, optical, environmental protection, electricity, catalyst carriers and the like because of the characteristics of high specific surface area, high porosity, low thermal conductivity, low density and the like. However, the performance of the silica aerogel is reduced due to the fact that microorganisms are easily attached to the material structure of the silica aerogel, and the silica aerogel is difficult to be applied to a humid environment in which microorganisms are easily bred.
Copper salt is widely used as the most common antibacterial agent with low cost, and the antibacterial action mode of copper ions is that bacterial cells can enrich the copper ions, the copper ions adsorbed on the surfaces of the bacteria destroy the functions of cell membranes and enter the interior of the cells, certain cell components escape, the cell metabolic process is interfered or the action of various enzymes is interfered, the cells lose the due biological functions, and finally the cells die. The composite material is prepared by carrying out hydrophobic modification on the silicon dioxide aerogel and loading copper ions, so that the silicon dioxide aerogel is endowed with an antibacterial function, and the silicon dioxide aerogel is suitable for protecting precision instruments and applying antibacterial coatings in more environments, such as a humid environment.
At present, the development aiming at the antibacterial function of the aerogel is mainly based on the research of composite materials of noble metals such as nano silver. Compared with nano silver, the cost of copper is relatively low, and the method is more suitable for industrial production. The market lacks a technology for producing antibacterial aerogel by combining aerogel preparation technology with copper ions.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of an antibacterial hydrophobic silica aerogel composite material.
The technical scheme of the invention is as follows:
a preparation method of an antibacterial hydrophobic silica aerogel composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) Sequentially stirring tetraethyl orthosilicate, deionized water and absolute ethyl alcohol while adding into a reaction vessel for mixing, then adding an acid solution to adjust the pH value to acidity, stirring until sol is formed, adding an alkali solution to adjust the pH value to alkalinity, and standing to obtain silicon dioxide hydrogel;
(2) Aging the silica hydrogel for 10-50h at 10-100 ℃ under normal pressure, then carrying out solvent exchange by using an organic solvent, then placing the silica hydrogel in a hydrophobic modifier for carrying out surface hydrophobic modification for 10-50h, and finally drying to obtain silica aerogel; wherein the hydrophobic modifier consists of the organic solvent and trimethylchlorosilane in a volume ratio of 1-20: 1;
(3) Standing the silicon dioxide aerogel in a copper salt ethanol solution with the copper ion solubility of 50-100mmol/L, and drying to obtain the antibacterial hydrophobic silicon dioxide aerogel composite material; wherein the copper salt is at least one selected from copper acetate, copper chloride, copper sulfate, copper nitrate and copper acetylacetonate.
In a preferred embodiment of the invention, the volume ratio of the tetraethyl orthosilicate, the deionized water and the absolute ethyl alcohol is 1: 0.1-5: 0.1-3.
Further preferably, the volume ratio of the tetraethyl orthosilicate to the deionized water to the absolute ethyl alcohol is 1: 3-3.12: 0.47-0.5.
In a preferred embodiment of the present invention, the acid in the acid solution is selected from at least one of hydrochloric acid, sulfuric acid, nitric acid, carbonic acid, phosphoric acid, sulfurous acid, and acetic acid.
In a preferred embodiment of the present invention, the alkali in the alkali solution is selected from at least one of sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide and ammonia water.
In a preferred embodiment of the present invention, the organic solvent is n-hexane, cyclohexane, n-heptane, toluene or ethanol.
Further preferably, the number of solvent exchanges is 1 to 5, each for 5 to 10 hours.
In a preferred embodiment of the present invention, the drying in the step (2) is: blowing and drying at normal pressure for 10-50h at 10-120 deg.C.
In a preferred embodiment of the present invention, the drying in the step (3) is: drying by blowing under normal pressure or vacuum for 1-15 hr at 10-120 deg.C.
In a preferred embodiment of the invention, the concentration of copper ions in the copper salt ethanol solution is 75-100mmol/L.
The invention has the beneficial effects that: the antibacterial hydrophobic silica aerogel composite material is prepared by taking tetraethyl orthosilicate as a silicon source, adding deionized water and absolute ethyl alcohol to prepare silica gel, and performing five subsequent treatments of silica framework aging, solvent exchange, gel surface hydrophobic modification, normal-pressure air blowing drying, copper ion loading and the like at a certain temperature.
Drawings
Fig. 1 is an antibacterial experimental result diagram of the antibacterial hydrophobic silica aerogel composite material prepared in example 1 of the present invention, wherein a is an antibacterial experimental result diagram of a blank control group, and b is an antibacterial experimental result diagram of the antibacterial hydrophobic silica aerogel composite material.
Fig. 2 is an antibacterial experimental result diagram of the antibacterial hydrophobic silica aerogel composite prepared in example 4 of the present invention, wherein a is an antibacterial experimental result diagram of a blank control group; b is an antibacterial experiment result chart of the antibacterial hydrophobic silica aerogel composite material.
Fig. 3 is a nitrogen adsorption and desorption graph and a pore size distribution graph of the antibacterial hydrophobic silica aerogel composite materials prepared in examples 1 and 4 of the present invention, wherein a is the nitrogen adsorption and desorption graph, the graph labeled "1" is the nitrogen adsorption and desorption graph of the antibacterial hydrophobic silica aerogel composite material prepared in example 1 of the present invention, and the graph labeled "2" is the nitrogen adsorption and desorption graph of the antibacterial hydrophobic silica aerogel composite material prepared in example 4 of the present invention; b is a pore size distribution diagram, wherein the one marked with "1" is the pore size distribution diagram of the antibacterial hydrophobic silica aerogel composite material prepared by the method of example 1, and the one marked with "2" is the pore size distribution diagram of the antibacterial hydrophobic silica aerogel composite material prepared by the method of example 4. The BET characterization test was carried out using a nitrogen adsorption analyzer from Kang Da, USA, at 77K, with a degassing temperature of 150 ℃ and a degassing time of 8h.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description in conjunction with the accompanying drawings.
The following examples employ a plate colony counting method to obtain the antibacterial rate of the antibacterial hydrophobic silica aerogel composite.
Example 1
(1) Tetraethyl orthosilicate is used as a silicon source, deionized water and absolute ethyl alcohol are added and stirred, hydrochloric acid is used for adjusting the pH value of the solution to 2.5, stirring is carried out for 1.5h, ammonia water is added for adjusting the pH value to 8 after the solution forms sol, silicon dioxide gel is obtained by standing, and silicon dioxide aerogel is obtained by aging a silicon dioxide framework for 24h, exchanging a solvent for 24h for 3 times, carrying out hydrophobic modification on the surface of the gel for 24h and drying for 24h at the temperature of 50 ℃.
Wherein, the volume ratio of tetraethyl orthosilicate, deionized water and absolute ethyl alcohol is 1: 3.12: 0.47, the acid solution is hydrochloric acid, the alkali solution is ammonia water, the volume ratio of TMCS and n-hexane is 1: 9, and the solvent in solvent exchange is n-hexane.
(2) Placing 0.5g of silica aerogel in a container, adding 75mmol/L copper chloride ethanol solution, standing for 1h, drying at 80 deg.C for 4h after the solution is filled with silica aerogel, and obtaining the antibacterial hydrophobic silica aerogel composite material shown in FIG. 3.
Further, 50mg of the antibacterial hydrophobic silica aerogel composite material is measured and mixed with escherichia coli bacterial liquid, the mixture is kept still for 10min at 37 ℃, then the bacterial liquid is uniformly coated on a solid culture medium by a dilution coating plate method, and then the culture medium is cultured for 24-48h at 37 ℃, and the result is shown in fig. 1. The density of the antibacterial hydrophobic silica aerogel composite in this example was 0.112g/cm 3 Specific surface area of 1003m 2 The antibacterial rate is 99 percent per gram.
Example 2
This example is different from example 1 in that:
adjusting the pH of the solution to 7 with ammonia water, wherein the copper salt is cupric chloride, the concentration of copper ions in the ethanol solution is 100mmol/L, and the density of the antibacterial hydrophobic silica aerogel composite material in the embodiment is 0.125g/cm 3 Specific surface area of 696m 2 The antibacterial rate is 98 percent per gram.
Example 3
This example is different from example 1 in that:
the volume ratio of tetraethyl orthosilicate to deionized water to absolute ethyl alcohol is 1: 3: 0.5, copper salt is copper nitrate, the concentration of copper ions in the ethanol solution is 100mmol/L, and the density of the antibacterial hydrophobic silica aerogel composite material in the embodiment is 0.141g/cm 3 Specific surface area of 612m 2 The antibacterial rate is 91 percent per gram.
Example 4
This example is different from example 1 in that:
the aqueous alkali is aqueous sodium hydroxide solution, copper salt is the mixture of copper acetate and copper chloride in a ratio of 1: 1, the concentration of copper ions in the ethanol solution is 100mmol/L, and the density of the antibacterial hydrophobic silica aerogel composite material in the embodiment is 0.128g/cm 3 Specific surface area of 736m 2 The antibacterial rate is 71% (as shown in figure 2 and figure 3).
Example 5
This example is different from example 4 in that:
the concentration of copper ions in the ethanol solution was 75mmol/L, and the density of the antibacterial hydrophobic silica aerogel composite material in this example was 0.115g/cm 3 Specific surface area of 808m 2 The antibacterial rate is 65 percent per gram.
Example 6
This example is different from example 4 in that:
the copper salt is the mixture of copper acetate and copper nitrate in a ratio of 1: 1, the concentration of copper ions in the copper ethanol solution is 75mmol/L, and the density of the antibacterial hydrophobic silica aerogel composite material in the embodiment is 0.145g/cm 3 The specific surface area is 787m 2 The antibacterial rate is 99 percent per gram.
Example 7
This example is different from example 1 in that:
adjusting the pH of the solution to 8 with ammonia water, mixing copper salt of copper nitrate and copper chloride at a ratio of 1: 1, adjusting the concentration of copper ions in the ethanol solution to 100mmol/L, adding the ethanol solution of copper, and standing for 2h, wherein the density of the antibacterial hydrophobic silica aerogel composite material in the embodiment is 0.121g/cm 3 Specific surface area of 746m 2 The antibacterial rate is 97 percent.
Example 8
This example is different from example 7 in that:
after adding the ethanol solution of copper, standing for 3h, the density of the antibacterial hydrophobic silica aerogel composite material in the embodiment is 0.126g/cm 3 Specific surface area of 729m 2 The antibacterial rate is 99 percent per gram.
Example 9
This example is different from example 1 in that:
copper salt is the mixture of copper chloride, copper nitrate and copper acetate in a ratio of 1: 1, the concentration of copper ions in ethanol solution is 100mmol/L, and after the solution is filled with silicon dioxide aerogel, the mixture is filteredDrying at 70 deg.C for 4 h. The density of the antibacterial hydrophobic silica aerogel composite in this example was 0.108g/cm 3 A specific surface area of 754m 2 The antibacterial rate is 94 percent per gram.
Example 10
This example is different from example 9 in that:
after the solution is filled with the silicon dioxide aerogel, the solution is treated by vacuum drying for 4 hours at 70 ℃. The density of the antibacterial hydrophobic silica aerogel composite in this example was 0.110g/cm 3 A specific surface area of 764m 2 The antibacterial rate is 96 percent.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (10)
1. A preparation method of an antibacterial hydrophobic silica aerogel composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) Sequentially stirring tetraethyl orthosilicate, deionized water and absolute ethyl alcohol while adding the mixture into a reaction vessel for mixing, then adding an acid solution to adjust the pH to acidity, stirring the mixture until sol is formed, adding an alkali solution to adjust the pH to alkalinity, and standing the sol to obtain silicon dioxide hydrogel;
(2) Aging the silica hydrogel for 10-50h at 10-100 ℃ under normal pressure, then carrying out solvent exchange by using an organic solvent, then placing the silica hydrogel in a hydrophobic modifier for carrying out surface hydrophobic modification for 10-50h, and finally drying to obtain silica aerogel; wherein the hydrophobic modifier consists of the organic solvent and trimethylchlorosilane in a volume ratio of 1-20: 1;
(3) Standing the silicon dioxide aerogel in a copper salt ethanol solution with the copper ion solubility of 50-100mmol/L, and drying to obtain the antibacterial hydrophobic silicon dioxide aerogel composite material; wherein the copper salt is at least one selected from copper acetate, copper chloride, copper sulfate, copper nitrate and copper acetylacetonate.
2. The method of claim 1, wherein: the volume ratio of the tetraethyl orthosilicate to the deionized water to the absolute ethyl alcohol is 1: 0.1-5: 0.1-3.
3. The method of claim 2, wherein: the volume ratio of the tetraethyl orthosilicate to the deionized water to the absolute ethyl alcohol is 1: 3-3.12: 0.47-0.5.
4. The method of claim 1, wherein: the acid in the acid solution is at least one selected from hydrochloric acid, sulfuric acid, nitric acid, carbonic acid, phosphoric acid, sulfurous acid, acetic acid and the like.
5. The method of claim 1, wherein: the alkali in the alkali solution is at least one selected from sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide and ammonia water.
6. The method of claim 1, wherein: the organic solvent is n-hexane, cyclohexane, n-heptane, toluene or ethanol.
7. The method of claim 6, wherein: the number of solvent exchanges is 1-5, each time for 5-10h.
8. The method of claim 1, wherein: the drying in the step (2) is as follows: blowing and drying at normal pressure for 10-50h at 10-120 deg.C.
9. The method of claim 1, wherein: the drying in the step (3) is as follows: drying by blowing under normal pressure or vacuum for 1-15 hr at 10-120 deg.C.
10. The production method according to any one of claims 1 to 9, characterized in that: the concentration of copper ions in the copper salt ethanol solution is 75-100mmol/L.
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