CN107552096A - A kind of nano titanium oxide aerogel material for catalytic degradation antibiotic and preparation method thereof - Google Patents
A kind of nano titanium oxide aerogel material for catalytic degradation antibiotic and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of nano titanium oxide aerogel material for catalytic degradation antibiotic and preparation method thereof, belong to water harnessing technical field, the matrix of aerogel material is titanium dioxide galapectite hydrophobic porous carboxymethyl cellulose composite, and it is loaded with Nano Silver and graphene on the matrix of aerogel material, aerogel material light weight prepared by the present invention, intensity is high, and antibiotic adsorption capacity is big, oleophobic property is good, can be achieved to remove the in situ of antibiotic in cultivation water.
Description
Technical field
The invention belongs to water harnessing technical field, and in particular to a kind of nano titanium oxide for catalytic degradation antibiotic
Aerogel material and preparation method thereof.
Background technology
China is the country that unique aquaculture in the world is higher than fishery output, extensive, high density, intensive cultivation
Pattern, causes various fish disease evil getting worses, and various antibiotic are widely used in anti-disease in aquaculture, improve feed
Utilization rate and promote growth of animal and due to the guidance and constraint general lack of laws and regulations during production and use,
The abuse of antibiotic uses phenomenon serious with illegal, and on the one hand water ecological environment is polluted, on the other hand causes aquatic products
Drug residue, by food chain transmission, threaten human health.Effective removal of antibiotic turns into problem urgently to be resolved hurrily.
The content of the invention
It is an object of the invention to provide a kind of matrix tack and excellent adsorption, and porosity is high, and oleophobic property is good, and absorption is anti-
Raw plain capacity is big, and adsorption rate is fast, can be achieved to be used for catalytic degradation antibiosis to the one kind in situ removed of antibiotic in breeding water body
Nano titanium oxide aerogel material of element and preparation method thereof.
The scheme taken to achieve the above object of the present invention is：A kind of nanometer titanium dioxide for catalytic degradation antibiotic
Titanium aerogel material, the matrix of aerogel material is titanium dioxide-galapectite-hydrophobic porous carboxymethyl cellulose composite,
And Nano Silver and graphene are loaded with the matrix of aerogel material, by by physisorphtion and Photocatalyst knot
Close, carrying nano silver and graphene on its gel rubber material, improve the photocatalysis effect of aerogel material, aerogel material can be realized
The in situ of antibiotic in cultivation water is removed.
A kind of preparation method of nano titanium oxide aerogel material for catalytic degradation antibiotic, specific steps are such as
Under：
1）Butyl titanate, galapectite powder, hydrophobic porous carboxymethyl cellulose, absolute ethyl alcohol, toluene are mixed in mass ratio
Close, obtained solution A；Absolute ethyl alcohol, 0.5 ~ 1.5mol/L glacial acetic acid are mixed in mass ratio with water, obtained solution B；It is right
Solution A carries out supersonic oscillations processing at 50 ~ 60 DEG C, solution B is added drop-wise in the solution A of 2 times of quality；Simultaneously to solution A
Middle addition quality is 0.02 ~ 0.03 times of sodium bicarbonate powder of solution A and quality is solution A 0.001-0.002 times change
Property agent, after continuing 0.5 ~ 1h of stirring, be made sol solutionses；
2）Silver nitrate, graphene are added into sol solutionses and is stirred, salpeter solution is then added dropwise into sol solutionses to colloidal sol
The pH of liquid is 5, and sol solutionses are heated into 45 ~ 55 DEG C under the conditions of lucifuge and are incubated 1 ~ 2h, unreacted is washed with water to sol solutionses
After material, sodium borohydride and urethanes are added into sol solutionses under agitation, while sodium hydroxide solution is added dropwise
Sol solutionses pH is controlled between 7 ~ 8, is made after being washed with water and carries silver sol liquid；
3）Silver sol liquid 24 ~ 48h of aging at room temperature will be carried, then adding n-hexane into load silver sol liquid carries out solvent displacement
36 ~ 60h, n-hexane is separated off, obtains carrying silver gel, with the mixed solution of organo-silicon compound and n-hexane to carrying silver gel
Oleophobic modification is carried out, aerogel material is made after vacuum drying.
The present invention is using titanium dioxide-galapectite-hydrophobic porous carboxymethyl cellulose composite as matrix, and on matrix
It is loaded with Nano Silver and graphene, the galapectite in matrix is made up of countless fine tubuloses or fibrous crystal, titanium dioxide
Titanium and there is high stability, high transparency, high activity and polymolecularity, non-toxic and colour effect, hydrophobic porous methylol
Cellulose aqueous solution has the effects such as thickening, film forming, gluing, water tariff collection, colloid protection, emulsification and suspension, and three is mixed
The aerogel material matrix being prepared into afterwards has very strong ageing-resistant, adsorption effect, using special ultrasonic oscillation method system
Standby matrix, significantly improves the matrix porosity of preparation, and intensity is good, and matrix has unexpected absorption and bond effect,
Silver and graphene are uploaded in the matrix being prepared, and graphene soilless sticking phenomenon makes the photocatalysis effect of aerogel material notable
Enhancing, aeroge can occur pi-pi bond effect with the phenyl ring of antibiotic, the degradation rate of antibiotic be significantly improved, especially to supporting
Grow aromatic pollution naphthalene in water and 1- naphthols adsorption effects are obvious.
Preferably, to adding the magnetic ball with 0.1T-0.2T in solution A ultrasonic oscillation processing procedure in solution A, surpass
Acoustic power is 150w-200w, solution A is handled using ultrasonic oscillation technology when preparing matrix, solution A is in ultrasound
Solution composition stable reaction in the presence of ripple and the magnetic magnetic ball of tool, the suction of matrix is obtained by magnetized and ultrasonic oscillation
Attached effect and bond effect are greatly improved, and are advantageous to lift suction of the aerogel material being finally prepared to antibiotic
Attached effect.
Preferably, modifying agent is by stearic acid 2-3 parts by weight, erucyl amide 5-7 parts by weight and bipentaerythrite 0.5-0.7 parts
Composition, after stirring 0.5 ~ 1h under the conditions of 70-94 DEG C, sol solutionses are made, sodium bicarbonate powder is added in matrix preparation process
And modifying agent, the decomposition temperature of sodium bicarbonate powder is improved, shortens and decomposes section, beneficial to the preparation time for shortening matrix, is gone forward side by side
Matrix high-temperature resistant result prepared by the lifting of one step.
Preferably, butyl titanate, galapectite powder, hydrophobic porous carboxymethyl cellulose, absolute ethyl alcohol, toluene are pressed into quality
Than 1:0.1~0.2:0.05~0.1:15~35:0.03 ~ 0.045 is mixed, obtained solution A；By absolute ethyl alcohol, 0.5 ~
1.5mol/L glacial acetic acid and water in mass ratio 10 ~ 15:3~5:1 is mixed, obtained solution B, is prepared using aforementioned proportion
Matrix porosity is high, but intensity is also high, easily shaping, and the hole of galapectite is specific to self structure, not by crosslinking
Gained, therefore the lifting to base-material intensity has effect, and base-material is not easy by illumination ageing in cultivation water well.
Preferably, the silver nitrate of 0.1-0.15 times of butyl titanate quality, butyl titanate quality 0.07- are added in sol solutionses
0.1 times of graphene, loading nano silvery and graphene on matrix, the Nano Silver and graphene in aeroge are in practice
Titanium dioxide can be coordinated further to lift the photocatalysis effect of aeroge, the aeroge absorption and photocatalytic degradation for realizing preparation resist
The effect of raw element.
Preferably, the addition of sodium borohydride is 0.003-0.007 times of butyl titanate quality in sol solution, carbamic acid
The addition of ethyl ester is 0.004-0.008 times of butyl titanate quality, adds the sodium borohydride and ammonia of above-mentioned dosage in the base
Base Ethyl formate can effectively lift load capacity and adsorption effect of the aerogel material to silver and graphene.
Preferably, organo-silicon compound and n-hexane volume ratio are 2-3 in step 3:1, organo-silicon compound are hexamethyl
In disiloxane, diisopropyl azodiformate, bisphenol A type epoxy resin, MTMS, trim,ethylchlorosilane
One kind, aeroge of the invention are the antibiotic adsorbed in cultivation water, it is necessary to which adsorptivity improves the suction to antibiotic well
Attached and degradation effect, and oily matter is avoided by the adsorbance of aeroge Adsorption Effect antibiotic, therefore in step 3 to gas
Gel rubber material carries out oleophobic modification.
Preferably, oleophobic modification temperature is 30 ~ 45 DEG C, modification time 20-40h in step 3, to lift aerogel material
Oleophobic effects, said temperature and time are defined, significantly improve the oleophobic property of aerogel material.
Compared with prior art, beneficial effects of the present invention are：The present invention is by by physisorphtion and photocatalytic degradation
Technology combines, carrying nano silver and graphene on its gel rubber material, improves the photocatalysis effect of aerogel material, aerogel material
It can be achieved to remove the in situ of antibiotic in cultivation water, with the phenyl ring of antibiotic pi-pi bond effect can occur for aeroge, to antibiotic
Degradation rate significantly improve, it is especially obvious to the aromatic pollution naphthalene in cultivation water and 1- naphthols adsorption effects, by magnetic
Change and ultrasonic oscillation obtains the adsorption effect of matrix and bond effect is greatly improved, aeroge prepared by the present invention
Quality of materials is light, and intensity is high, and antibiotic adsorption capacity is big, and oleophobic property is good.
Embodiment
The present invention is described in further detail with reference to embodiments：
Embodiment 1：
A kind of nano titanium oxide aerogel material for catalytic degradation antibiotic, the matrix of aerogel material is titanium dioxide
Titanium-galapectite-hydrophobic porous carboxymethyl cellulose composite, and Nano Silver and graphite are loaded with the matrix of aerogel material
Alkene.
A kind of preparation method of nano titanium oxide aerogel material for catalytic degradation antibiotic, specific steps are such as
Under：
1）By butyl titanate, galapectite powder, hydrophobic porous carboxymethyl cellulose, absolute ethyl alcohol, toluene in mass ratio 1:0.14:
0.06:24:0.034 is mixed, obtained solution A；Absolute ethyl alcohol, 0.8mol/L glacial acetic acid and water are mixed in mass ratio
Close, obtained solution B；Supersonic oscillations processing is carried out at 52 DEG C to solution A, the magnetic ball with 0.15T is added in solution A,
Ultrasonic power is 150w, solution B is added drop-wise in the solution A of 2 times of quality；Quality is added into solution A simultaneously as solution A
0.02 ~ 0.03 times of sodium bicarbonate powder and quality is 0.0015 times of modifying agent of solution A, and 0.6h is stirred under the conditions of 78 DEG C
Afterwards, sol solutionses are made；Modifying agent is made up of 0.55 part of the parts by weight of stearic acid 2, the parts by weight of erucyl amide 6 and bipentaerythrite；
2）The silver nitrate of 0.12 times of butyl titanate quality, the graphene of 0.08 times of butyl titanate quality are added into sol solutionses and is stirred
Mix uniformly, the pH that salpeter solution is then added dropwise into sol solutionses to sol solutionses is 5, and sol solutionses are heated into 47 under the conditions of lucifuge
DEG C and be incubated 1h, after unreacting substance is washed with water to sol solutionses, under agitation into sol solutionses add butyl titanate matter
0.004 times of sodium borohydride of amount and 0.005 times of urethanes of butyl titanate quality, while sodium hydroxide solution control is added dropwise
Sol solutionses pH processed is made between 7.1 ~ 7.5, after being washed with water and carries silver sol liquid；
3）Silver sol liquid aging 27h at room temperature will be carried, then adding n-hexane into load silver sol liquid carries out solvent displacement
40h, n-hexane is separated off, obtains carrying silver gel, entered with the mixed solution of organo-silicon compound and n-hexane to carrying silver gel
Row oleophobic is modified, and oleophobic modification temperature is 37 DEG C, modification time 28h, and organo-silicon compound are 2 with n-hexane volume ratio:1,
Aerogel material is made after 74 DEG C of vacuum drying, organo-silicon compound are HMDO.
Embodiment 2：
A kind of nano titanium oxide aerogel material for catalytic degradation antibiotic, the matrix of aerogel material is titanium dioxide
Titanium-galapectite-hydrophobic porous carboxymethyl cellulose composite, and Nano Silver and graphite are loaded with the matrix of aerogel material
Alkene.
A kind of preparation method of nano titanium oxide aerogel material for catalytic degradation antibiotic, specific preferred steps
It is as follows：
1）By butyl titanate, galapectite powder, hydrophobic porous carboxymethyl cellulose, absolute ethyl alcohol, toluene in mass ratio 1:0.14:
0.07:20:0.038 is mixed, obtained solution A；Absolute ethyl alcohol, 0.8mol/L glacial acetic acid and water are mixed in mass ratio
Close, obtained solution B；Supersonic oscillations processing is carried out at 51 DEG C to solution A, the magnetic ball with 0.2T is added in solution A, is surpassed
Acoustic power is 180w, solution B is added drop-wise in the solution A of 2 times of quality；Quality is added into solution A simultaneously as solution A
0.02 ~ 0.03 times of sodium bicarbonate powder and quality is 0.002 times of modifying agent of solution A, and 0.5h is stirred under the conditions of 82 DEG C
Afterwards, sol solutionses are made；Modifying agent is made up of 0.54 part of the parts by weight of stearic acid 2, the parts by weight of erucyl amide 5 and bipentaerythrite；
2）The silver nitrate of 0.12 times of butyl titanate quality, the graphene of 0.08 times of butyl titanate quality are added into sol solutionses and is stirred
Mix uniformly, the pH that salpeter solution is then added dropwise into sol solutionses to sol solutionses is 5, and sol solutionses are heated into 48 under the conditions of lucifuge
DEG C and be incubated 2h, after unreacting substance is washed with water to sol solutionses, under agitation into sol solutionses add butyl titanate matter
0.004 times of sodium borohydride of amount and 0.005 times of urethanes of butyl titanate quality, while sodium hydroxide solution control is added dropwise
Sol solutionses pH processed is made between 7.4-7.6, after being washed with water and carries silver sol liquid；
3）Silver sol liquid aging 40h at room temperature will be carried, then adding n-hexane into load silver sol liquid carries out solvent displacement
38h, n-hexane is separated off, obtains carrying silver gel, entered with the mixed solution of organo-silicon compound and n-hexane to carrying silver gel
Row oleophobic is modified, and oleophobic modification temperature is 42 DEG C, modification time 28h, and organo-silicon compound are 3 with n-hexane volume ratio:1,
Aerogel material is made after 83 DEG C of vacuum drying, organo-silicon compound are diisopropyl azodiformate.
Embodiment 3：
A kind of nano titanium oxide aerogel material for catalytic degradation antibiotic, the matrix of aerogel material is titanium dioxide
Titanium-galapectite-hydrophobic porous carboxymethyl cellulose composite, and Nano Silver and graphite are loaded with the matrix of aerogel material
Alkene.
A kind of preparation method of nano titanium oxide aerogel material for catalytic degradation antibiotic, specific steps are such as
Under：
1）By butyl titanate, galapectite powder, hydrophobic porous carboxymethyl cellulose, absolute ethyl alcohol, toluene in mass ratio 1:0.14:
0.08:22:0.037 is mixed, obtained solution A；Absolute ethyl alcohol, 1mol/L glacial acetic acid and water are mixed in mass ratio
Close, obtained solution B；Supersonic oscillations processing is carried out at 55 DEG C to solution A, the magnetic ball with 0.2T is added in solution A, is surpassed
Acoustic power is 150w, solution B is added drop-wise in the solution A of 2 times of quality；Quality is added into solution A simultaneously as solution A
0.02 ~ 0.03 times of sodium bicarbonate powder and quality is 0.0018 times of modifying agent of solution A, and 1h is stirred under the conditions of 92 DEG C
Afterwards, sol solutionses are made；Modifying agent is made up of 0.6 part of the parts by weight of stearic acid 3, the parts by weight of erucyl amide 6 and bipentaerythrite；
2）The silver nitrate of 0.12 times of butyl titanate quality, the graphene of 0.08 times of butyl titanate quality are added into sol solutionses and is stirred
Mix uniformly, the pH that salpeter solution is then added dropwise into sol solutionses to sol solutionses is 5, and sol solutionses are heated into 52 under the conditions of lucifuge
DEG C and be incubated 2h, after unreacting substance is washed with water to sol solutionses, under agitation into sol solutionses add butyl titanate matter
0.005 times of sodium borohydride of amount and 0.006 times of urethanes of butyl titanate quality, while sodium hydroxide solution control is added dropwise
Sol solutionses pH processed is made between 7.7-8.0, after being washed with water and carries silver sol liquid；
3）Silver sol liquid aging 27h at room temperature will be carried, then adding n-hexane into load silver sol liquid carries out solvent displacement
38h, n-hexane is separated off, obtains carrying silver gel, entered with the mixed solution of organo-silicon compound and n-hexane to carrying silver gel
Row oleophobic is modified, and oleophobic modification temperature is 34 DEG C, modification time 27h, and organo-silicon compound are 3 with n-hexane volume ratio:1,
Aerogel material is made after 72 DEG C of vacuum drying, organo-silicon compound are bisphenol A type epoxy resin.
The performance such as following table of aerogel material prepared by embodiment 1-3：
| Porosity | Specific surface area | Density | Inhale antibiotic multiplying power | Tensile strength | |
| Embodiment 1 | 93% | 531 m2/g | 3.92 Kg/m3 | 16 | 26.3Gpa |
| Embodiment 2 | 97% | 572 m2/g | 3.61 Kg/m3 | 13 | 27.1Gpa |
| Embodiment 3 | 95% | 553 m2/g | 3.74 Kg/m3 | 14 | 26.6Gpa |
Raw materials used in the present invention, equipment, it is the conventional raw material, equipment of this area unless otherwise noted；It is used in the present invention
Method, it is the conventional method of this area unless otherwise noted.
Routine operation in above-described embodiment 1-3 is well known to those skilled in the art, herein without repeating.
Technical scheme is described in detail embodiment described above, it should be understood that it is described above only
For the specific embodiment of the present invention, it is not intended to limit the invention, all any modifications made in the spirit of the present invention,
Supplement or similar fashion replacement etc., should be included in the scope of the protection.
Claims (9)
- A kind of 1. nano titanium oxide aerogel material for catalytic degradation antibiotic, it is characterised in that：The airsetting glue material The matrix of material is titanium dioxide-galapectite-hydrophobic porous carboxymethyl cellulose composite, and is born on the matrix of aerogel material It is loaded with Nano Silver and graphene.
- 2. the preparation method of a kind of nano titanium oxide aerogel material for catalytic degradation antibiotic, it is characterised in that following Step：1）Butyl titanate, galapectite powder, hydrophobic porous carboxymethyl cellulose, absolute ethyl alcohol, toluene are mixed in mass ratio Close, obtained solution A；Absolute ethyl alcohol, 0.5 ~ 1.5mol/L glacial acetic acid are mixed in mass ratio with water, obtained solution B；It is right Solution A carries out supersonic oscillations processing at 50 ~ 60 DEG C, solution B is added drop-wise in the solution A of 2 times of quality；Simultaneously to solution A Middle addition quality is 0.02 ~ 0.03 times of sodium bicarbonate powder of solution A and quality is solution A 0.001-0.002 times change Property agent, after continuing 0.5 ~ 1h of stirring, be made sol solutionses；2）Silver nitrate, graphene are added into sol solutionses and is stirred, salpeter solution is then added dropwise into sol solutionses to colloidal sol The pH of liquid is 5, and sol solutionses are heated into 45 ~ 55 DEG C under the conditions of lucifuge and are incubated 1 ~ 2h, unreacted is washed with water to sol solutionses After material, sodium borohydride and urethanes are added into sol solutionses under agitation, while sodium hydroxide solution is added dropwise Sol solutionses pH is controlled between 7 ~ 8, is made after being washed with water and carries silver sol liquid；3）Silver sol liquid 24 ~ 48h of aging at room temperature will be carried, then adding n-hexane into load silver sol liquid carries out solvent displacement 36 ~ 60h, n-hexane is separated off, obtains carrying silver gel, with the mixed solution of organo-silicon compound and n-hexane to carrying silver gel Oleophobic modification is carried out, aerogel material is made after vacuum drying.
- A kind of 3. preparation of nano titanium oxide aerogel material for catalytic degradation antibiotic according to claim 2 Method, it is characterised in that：To the magnetic ball with 0.1T-0.2T is added in solution A ultrasonic oscillation processing procedure in solution A, Ultrasonic power is 150w-200w.
- A kind of 4. preparation of nano titanium oxide aerogel material for catalytic degradation antibiotic according to claim 2 Method, it is characterised in that：Modifying agent is by stearic acid 2-3 parts by weight, erucyl amide 5-7 parts by weight and bipentaerythrite 0.5-0.7 Part composition, after stirring 0.5 ~ 1h under the conditions of 70-94 DEG C, sol solutionses are made.
- A kind of 5. preparation of nano titanium oxide aerogel material for catalytic degradation antibiotic according to claim 2 Method, it is characterised in that：Butyl titanate, galapectite powder, hydrophobic porous carboxymethyl cellulose, absolute ethyl alcohol, toluene are pressed into matter Measure ratio 1:0.1~0.2:0.05~0.1:15~35:0.03 ~ 0.045 is mixed, obtained solution A；By absolute ethyl alcohol, 0.5 ~ 1.5mol/L glacial acetic acid and water in mass ratio 10 ~ 15:3~5:1 is mixed, obtained solution B.
- A kind of 6. preparation of nano titanium oxide aerogel material for catalytic degradation antibiotic according to claim 2 Method, it is characterised in that：The silver nitrate of 0.1-0.15 times of butyl titanate quality, butyl titanate quality 0.07- are added in sol solutionses 0.1 times of graphene.
- A kind of 7. preparation of nano titanium oxide aerogel material for catalytic degradation antibiotic according to claim 2 Method, it is characterised in that：The addition of sodium borohydride is 0.003-0.007 times of butyl titanate quality in sol solution, amino first The addition of acetoacetic ester is 0.004-0.008 times of butyl titanate quality.
- A kind of 8. preparation of nano titanium oxide aerogel material for catalytic degradation antibiotic according to claim 2 Method, it is characterised in that：Organo-silicon compound and n-hexane volume ratio are 2-3 in the step 3:1, the organo-silicon compound For HMDO, diisopropyl azodiformate, bisphenol A type epoxy resin, MTMS, trimethyl chlorine One kind in silane.
- A kind of 9. preparation of nano titanium oxide aerogel material for catalytic degradation antibiotic according to claim 2 Method, it is characterised in that：Oleophobic modification temperature is 30 ~ 45 DEG C in the step 3, modification time 20-40h.
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| CN112108133A (en) * | 2020-09-23 | 2020-12-22 | 济南市畜产品质量安全监测中心 | Surface-modified polyimide aerogel and preparation method and application thereof |
| CN112121769A (en) * | 2020-08-18 | 2020-12-25 | 江苏大学 | Biomass-based composite material with double-layer structure and application of biomass-based composite material to tellurium separation in complex environment |
| CN112438274A (en) * | 2020-04-03 | 2021-03-05 | 祁海强 | Preparation method of high-dispersion anti-discoloration nano-silver antibacterial agent material |
| CN115304222A (en) * | 2022-08-24 | 2022-11-08 | 南京工大环境科技有限公司 | Treatment process of oil-containing storage wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109513425A (en) * | 2018-09-25 | 2019-03-26 | 山东大学 | A kind of peanut shell graphene composite aerogel oil absorption material and preparation method thereof |
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| CN109775926A (en) * | 2019-02-02 | 2019-05-21 | 常熟理工学院 | A kind of small-sized livestock breeding wastewater integrated treatment combination unit and application method |
| CN112438274A (en) * | 2020-04-03 | 2021-03-05 | 祁海强 | Preparation method of high-dispersion anti-discoloration nano-silver antibacterial agent material |
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| CN112121769B (en) * | 2020-08-18 | 2023-03-21 | 江苏大学 | Biomass-based composite material with double-layer structure and application of biomass-based composite material to tellurium separation in complex environment |
| CN112108133A (en) * | 2020-09-23 | 2020-12-22 | 济南市畜产品质量安全监测中心 | Surface-modified polyimide aerogel and preparation method and application thereof |
| CN115304222A (en) * | 2022-08-24 | 2022-11-08 | 南京工大环境科技有限公司 | Treatment process of oil-containing storage wastewater |
| CN115304222B (en) * | 2022-08-24 | 2023-08-15 | 南京工大环境科技有限公司 | Treatment process of oil-containing storage wastewater |
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Application publication date: 20180109 |