CN108479780A - A kind of preparation method of optomagnetic response halloysite nanotubes hollow microsphere - Google Patents
A kind of preparation method of optomagnetic response halloysite nanotubes hollow microsphere Download PDFInfo
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- CN108479780A CN108479780A CN201810432749.1A CN201810432749A CN108479780A CN 108479780 A CN108479780 A CN 108479780A CN 201810432749 A CN201810432749 A CN 201810432749A CN 108479780 A CN108479780 A CN 108479780A
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- milliliter
- halloysite nanotubes
- optomagnetic
- ethyl alcohol
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- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052621 halloysite Inorganic materials 0.000 title claims abstract description 25
- 239000002071 nanotube Substances 0.000 title claims abstract description 25
- 239000004005 microsphere Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000019441 ethanol Nutrition 0.000 claims abstract description 16
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000006210 lotion Substances 0.000 claims abstract description 8
- 239000002105 nanoparticle Substances 0.000 claims abstract description 8
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 8
- 239000004626 polylactic acid Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 29
- 239000004408 titanium dioxide Substances 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 235000010215 titanium dioxide Nutrition 0.000 claims 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 2
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 claims 2
- MLNKXLRYCLKJSS-RMKNXTFCSA-N (2e)-2-hydroxyimino-1-phenylethanone Chemical compound O\N=C\C(=O)C1=CC=CC=C1 MLNKXLRYCLKJSS-RMKNXTFCSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims 1
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006116 polymerization reaction Methods 0.000 abstract description 4
- 238000004132 cross linking Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- 239000000839 emulsion Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000007146 photocatalysis Methods 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000011068 loading method Methods 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
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- B01J37/02—Impregnation, coating or precipitation
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- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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Abstract
A kind of preparation method of optomagnetic response halloysite nanotubes hollow microsphere, it is characterised in that include the following steps:1. tetrabutyl titanate and EtOH Sonicate are mixed to form vitreosol;2. by halloysite nanotubes, ethyl alcohol and vitreosol ultrasonic mixing, acetic acid is added dropwise and stirs evenly, is roasted 5 hours at 450 DEG C after being centrifuged with ethyl alcohol;3. surfactant TX 100 is mixed with the halloysite nanotubes after roasting, centrifuged after vacuumizing;4. 3. product that ferriferrous oxide nano-particle, step are obtained, photoinitiator 2,2 dimethoxy, 2 phenyl acetophenone, toluene and surfactant Hypermer2234 mixing, stirring forms stable emulsion, the mixed liquor of N ' N dimethacrylamide and polylactic acid is added dropwise again, it is protected from light stirring, crosslinking polymerization through ultraviolet light obtains hollow complex microsphere.Compared with the prior art, the advantages of the present invention are as follows:The lotion and uv-light polymerization stablized using the nano-particle with optomagnetic response obtain hollow microsphere, simple for process efficient, have a wide range of application.
Description
Technical field
The preparation method with photocatalysis performance and magnetic galapectite pipe hollow microsphere that the present invention relates to a kind of.
Background technology
The environmental pollution of getting worse has severely impacted the life and development of the mankind.Photocatalysis technology is with its room
Temperature reaction and it can become a kind of ideal environmental pollution directly using solar energy as light source come drive response etc. special performances and control
Reason technology and clear energy sources production technology.Photocatalytic oxidation is the advanced water technology occurred in recent years, and semiconductor light is urged
Agent titanium dioxide causes the extensive concern of people due to the high and excellent photoelectric properties of nontoxic, inexpensive, stability.And such as
What, which improves load factor and good dispersibility of the titanium dioxide on carrier, is related to photocatalysis effect and application, invention
The recyclable support type porous carrier of a kind of photocatalysis, i.e., by the titanium dichloride load with photocatalysis performance to galapectite nanometer
Itself and magnetic ferroferric oxide particle are formed the lotion that solids are stablized by pipe surface, then cross-linked polymeric forms hollow microsphere.
The complex microsphere has high specific surface area, recuperability and photocatalysis performance compared with similar products, has wide range of applications.
Invention content
The technical problem to be solved by the present invention is to, to the present situation of the prior art provide it is a kind of with photocatalytic activity can
The magnetic halloysite nanotube hollow microsphere of recycling.
Technical solution is used by the present invention solves above-mentioned technical problem:Optomagnetic response galapectite pipe hollow microsphere,
It is characterized in that preparation method is as follows:
1. tetrabutyl titanate and EtOH Sonicate are mixed 2 hours and form vitreosol;
2. after halloysite nanotubes are mixed ultrasound with ethyl alcohol, vitreosol and acetic acid is added dropwise, stirs 24 hours, use ethyl alcohol
It is roasted 5 hours at 450 DEG C after centrifugal drying;
3. the halloysite nanotubes ultrasonic mixing of surfactant TX-100 and composite titanium dioxide 20 minutes, vacuumizes guarantor
It holds 24 hours, TX-100 is made to enter a nanometer tube cavity, it is dry after centrifugation;
4. by ferriferrous oxide nano-particle, the compound halloysite nanotubes of titanium dioxide, the photoinitiator of loading TX-100
2,2- dimethoxy -2- phenyl acetophenones and toluene are stirred, and surfactant Hypermer2234 is added, and are stirred 10 minutes
The lotion that solids are stablized is formed, then the mixed liquor of N ' N- dimethacrylamide and polylactic acid is added dropwise, is protected from light 10 points of stirring
Clock crosslinks polymerization through ultraviolet light and obtains hollow complex microsphere.
The tetrabutyl titanate (gram) and ethyl alcohol (milliliter) ratio are 0.5~2;
The ratio of the halloysite nanotubes (milligram), ethyl alcohol (milliliter) and vitreosol (milliliter) is 10:1:1~100:
10:1;Acetic acid is 0.5~2 milliliter;
The quality of the surfactant TX-100 is 0.5~3 gram;
It is the ferriferrous oxide nano-particle, the compound halloysite nanotubes of titanium dioxide for loading TX-100, light-initiated
The ratio of agent 2,2- dimethoxy -2- phenyl acetophenones, toluene and Hypermer2234 is (0.01~1) gram:(0.01~1)
Gram:(0.1~1) gram:(2~5) milliliter:(0.1~0.5) milliliter;
N ' the N- dimethacrylamide volumes are 0.1~2 milliliter, and polylactic acid volume is 0.1~2 milliliter;
50~the 100W of uv power, light application time 10~120 minutes.
Compared with prior art, hollow microsphere provided by the present invention loads compound angstrom of the titanium dioxide of surfactant
Lip river stone and modified magnetic iron particle form the lotion that solids are stablized in oil meter face, add polymer monomer and light-initiated
Agent, by photo-initiated crosslinking polymerization, making, there is the galapectite pipe of optomagnetic response, which to be cross-linked to form in oil droplets, is coated on oil droplet
On shell obtain the optomagnetic response Hollow Microspheres with micro-nano hole structure then by later stage centrifugation, washing, dry;No
Specific surface area is only substantially increased, and there is photocatalysis performance and recuperability, which prepares item
Part is mild, simple for process, and the prices of raw materials are cheap and easily-available, is easy to be extended and applied.
Specific implementation mode
Present invention is further described in detail with reference to embodiments.
1 preparation method of embodiment is as follows:
1. 3 grams of tetrabutyl titanates and 3 milliliters of EtOH Sonicates are mixed 2 hours and form vitreosol;
2. after 50 milligrams of halloysite nanotubes are mixed ultrasound with 1 milliliter of ethyl alcohol, be added dropwise 0.5 milliliter vitreosol and
0.5 milliliter of acetic acid stirs 24 hours, with roasting 5 hours under 450 degree after ethyl alcohol centrifugal drying;
3. the halloysite nanotubes ultrasonic mixing of 1 gram of surfactant TX-100 and composite titanium dioxide 20 minutes is taken out true
Sky is kept for 24 hours, makes Qula is logical to enter nanometer tube cavity, dry after centrifugation;
4. by 0.1 gram of ferriferrous oxide nano-particle, the compound halloysite nanotubes of titanium dioxide for loading TX-100,0.1
Milliliter photoinitiator 2,2- dimethoxy -2- phenyl acetophenones and 2 milliliters of toluene are stirred, and 0.1 milliliter of surface-active is added
Agent Hypermer2234 is stirred and is formed within 10 minutes the lotion that solids are stablized, then 0.1 milliliter of N ' N- dimethyl allene acyl is added dropwise
The mixed liquor of amine and 0.1 milliliter of polylactic acid is protected from light stirring 10 minutes, through ultraviolet light (power 50-100W), irradiation time 10-
It 120 minutes, crosslinks to obtain hollow complex microsphere.
It is detected through particle size analyzer, microsphere particle size is distributed between 3~20 microns.
The preparation method of embodiment 2 is as follows:
1. 4 grams of tetrabutyl titanates and 5 milliliters of EtOH Sonicates are mixed 2 hours and form vitreosol;
2. after 60 milligrams of halloysite nanotubes are mixed ultrasound with 1.5 milliliters of ethyl alcohol, be added dropwise 1 milliliter vitreosol and
0.7 milliliter of acetic acid is stirred 24 hours, is roasted 5 hours at 450 DEG C after ethyl alcohol centrifugal drying;
3. the halloysite nanotubes ultrasonic mixing of 2 grams of surfactant TX-100 and composite titanium dioxide 20 minutes is taken out true
Sky is kept for 24 hours, makes Qula is logical to enter nanometer tube cavity, dry after centrifugation;
4. by 0.2 gram of ferriferrous oxide nano-particle, the compound halloysite nanotubes of titanium dioxide for loading TX-100,0.1
Milliliter photoinitiator 2,2- dimethoxy -2- phenyl acetophenones and 32 milliliters of toluene are stirred, and 0.2 milliliter of surface-active is added
Agent Hypermer2234 is stirred and is formed within 10 minutes the lotion that solids are stablized, then 0.2 milliliter of N ' N- dimethyl allene acyl is added dropwise
The mixed liquor of amine and 0.2 milliliter of polylactic acid is protected from light stirring 10 minutes, through ultraviolet light (power 50-100W), irradiation time 10-
It 120 minutes, crosslinks to obtain hollow complex microsphere.
It is detected through particle size analyzer, microsphere particle size is distributed between 3~20 microns.
The preparation method of embodiment 3 is as follows:
1. 5 grams of tetrabutyl titanates and 7 milliliters of EtOH Sonicates are mixed 2 hours and form vitreosol;
2. after 100 milligrams of halloysite nanotubes are mixed ultrasound with 2 milliliters of ethyl alcohol, 2 milliliters of vitreosol and 1 is added dropwise
The acetic acid of milliliter is stirred 24 hours, is roasted 5 hours at 450 DEG C after ethyl alcohol centrifugal drying;
3. the halloysite nanotubes ultrasonic mixing of 3 grams of surfactant TX-100 and composite titanium dioxide 20 minutes is taken out true
Sky is kept for 24 hours, makes Qula is logical to enter nanometer tube cavity, dry after centrifugation;
4. by 0.3 gram of ferriferrous oxide nano-particle, the compound halloysite nanotubes of titanium dioxide for loading TX-100,0.2
Milliliter photoinitiator 2,2- dimethoxy -2- phenyl acetophenones and 32 milliliters of toluene are stirred, and 0.3 milliliter of surface-active is added
Agent Hypermer2234 is stirred and is formed within 10 minutes the lotion that solids are stablized, then 0.3 milliliter of N ' N- dimethyl allene acyl is added dropwise
The mixed liquor of amine and 0.3 milliliter of polylactic acid is protected from light stirring 10 minutes, through ultraviolet light (power 50-100W), irradiation time 10-
It 120 minutes, crosslinks to obtain hollow complex microsphere.
Claims (3)
1. a kind of hollow galapectite pipe microballoon of optomagnetic response, it is characterised in that preparation method is as follows:
Vitreosol is formed within 2 hours 1. tetrabutyl titanate and EtOH Sonicate are mixed, the tetrabutyl titanate (gram) and ethyl alcohol (milli
Rise) ratio be 0.5~2;
2. after halloysite nanotubes are mixed ultrasound with ethyl alcohol, vitreosol and 0.5 milliliter of acetic acid is added dropwise, stir 24 hours, uses
After ethyl alcohol centrifugal drying, roasted 5 hours at 450 DEG C;The halloysite nanotubes (milligram), ethyl alcohol (milliliter) and vitreosol
The ratio of (milliliter) is 10:1:1~100:10:1;Acetic acid is 0.5~2 milliliter;
3. the halloysite nanotubes ultrasonic mixing 20 of the surfactant TX-100 composite titanium dioxides 2. obtained with step is divided
Clock vacuumizes holding 24 hours, makes Qula is logical to enter nanometer tube cavity, dry after centrifugation;The quality of the surfactant is
0.5~3 gram;
4. by ferriferrous oxide nano-particle, the compound halloysite nanotubes of titanium dioxide, photoinitiator 2,2- dimethoxy -2- benzene
Benzoylformaldoxime and toluene are stirred, and surfactant Hypermer2234 is added, and are stirred 10 minutes and are formed oil phase
Pickering, then the mixed liquor of N ' N- dimethacrylamide and polylactic acid is added dropwise, it is protected from light stirring 10 minutes, forms solid grain
The lotion that son is stablized, crosslinks to obtain hollow complex microsphere through ultraviolet light.
2. the preparation method of optomagnetic response hollow microsphere according to claim 1, it is characterised in that step 4. in four oxygen
The compound halloysite nanotubes of titanium dioxide, the photoinitiator 2,2- dimethoxy -2- benzene changed three Fe nanometer particles, load TX-100
The ratio of benzoylformaldoxime, toluene and Hypermer2234 is (0.01~1) gram:(0.01~1) gram:(0.1~1) gram:(2~5)
Milliliter:(0.1~0.5) milliliter;N ' the N- dimethyl allenes acyl volume is 0.1~2 milliliter;Polylactic acid volume is 0.1~2 milli
It rises.
3. the preparation method of optomagnetic response hollow microsphere according to claim 1, it is characterised in that step 4. in it is ultraviolet
50~100W of luminous power, light application time 10~120 minutes.
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