CN108906064A - A kind of preparation method for the modified nano zinc oxide that photocatalytic degradation is strong - Google Patents
A kind of preparation method for the modified nano zinc oxide that photocatalytic degradation is strong Download PDFInfo
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- CN108906064A CN108906064A CN201810834633.0A CN201810834633A CN108906064A CN 108906064 A CN108906064 A CN 108906064A CN 201810834633 A CN201810834633 A CN 201810834633A CN 108906064 A CN108906064 A CN 108906064A
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 24
- 238000013033 photocatalytic degradation reaction Methods 0.000 title claims abstract description 21
- 238000012545 processing Methods 0.000 claims abstract description 47
- 239000000706 filtrate Substances 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 30
- 230000008569 process Effects 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 239000002041 carbon nanotube Substances 0.000 claims description 11
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 229960004756 ethanol Drugs 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000003760 magnetic stirring Methods 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 7
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 229910016874 Fe(NO3) Inorganic materials 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 5
- 229960001763 zinc sulfate Drugs 0.000 claims description 5
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- YFDKVXNMRLLVSL-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid;sodium Chemical compound [Na].CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O YFDKVXNMRLLVSL-UHFFFAOYSA-N 0.000 claims description 2
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 4
- 239000000047 product Substances 0.000 abstract description 4
- 238000002715 modification method Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- -1 Graphite alkene Chemical class 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- MSNWSDPPULHLDL-UHFFFAOYSA-K ferric hydroxide Chemical compound [OH-].[OH-].[OH-].[Fe+3] MSNWSDPPULHLDL-UHFFFAOYSA-K 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- B01J35/39—
Abstract
The invention discloses a kind of preparation methods of modified nano zinc oxide that photocatalytic degradation is strong, include the following steps：（1）Mixed liquor A preparation,（2）Roll processing,（3）Mixed liquid B preparation,（4）Mixed liquor C preparation,（5）Filtrate D preparation,（6）Mixed processing,（7）Filtrate E preparation,（8）Mixture F preparation,（9）Finished product preparation.The present invention provides a kind of modification method for preparing that nano zine oxide is special, and a kind of ZnO/a-Fe has been made2O3The particle size of nano-heterogeneous structure, this substance is small, and for average grain diameter in 30 rans, photocatalytic degradation is excellent, and comprehensive service performance is good, the great market competitiveness and application value.
Description
Technical field
The invention belongs to inorganic material processing technique fields, and in particular to a kind of modified Nano oxygen that photocatalytic degradation is strong
Change the preparation method of zinc.
Background technique
Nano zine oxide is as a kind of high-performance semiconductor material since it is with unique small-size effect, surface effect
It answers, quantum size effect, macro quanta tunnel effect and Dielectric confinement effect, therefore in anti-biotic material, luminescent material, piezoresistive material
There is very extensive application in material, ultraviolet shielding material, self-cleaning material, the cell calibration fields such as material and nanocatalyst
Prospect.Characteristic possessed by zinc oxide nano-particle and the physical features of its own have more close relationship.How to select to close
Suitable coating material prepares the controllable nano zinc oxide material of size and shape by solution chemical processes, expands its application
Field, the fabulous nanometer product of the performance that is applied are one of the hot issues of current nano zinc oxide material research.
Research at present for nano zine oxide in catalytic degradation technology field is also still immature, does not obtain substantially preferably
Application have very important significance for the recycling tool of environmental pollution resource there is huge development space.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of modified nano zinc oxide that photocatalytic degradation is strong is provided
Preparation method.
The present invention is achieved by the following technical solutions：
A kind of preparation method for the modified nano zinc oxide that photocatalytic degradation is strong, includes the following steps：
（1）By zinc sulfate and dehydrated alcohol according to weight ratio 1:4 ~ 6, which carry out mixing, is put into agitator tank, and high-speed stirred processing 1 ~
Taken out after 2h mixed liquor A is spare；
（2）Carbon nanotubes is put into roller and roll processing, is taken out after 20 ~ 22min spare；
（3）By step（2）Carbon nanotubes that treated and N-Methyl pyrrolidone are according to weight ratio 1:10 ~ 14 carry out mixing investment
Into homogeneous blender, taken out after 2 ~ 2.5h of stir process mixed liquid B is spare；
（4）By step（3）Resulting mixed liquid B is put into reaction kettle, then into reaction kettle be added mixed liquid B gross mass 2 ~
4% disodium ethylene diamine tetraacetate, 4 ~ 6% silane coupling agent, 0.3 ~ 0.5% lanthanum nitrate, 5 ~ 7% dodecyl benzene sulfonic acid
Sodium takes out after being then ultrasonically treated 20 ~ 25min, it is spare to obtain mixed liquor C；
（5）By step（1）Resulting mixed liquor A is put into beaker, and mixed liquor A gross mass 7 ~ 10% is then added into beaker
Potassium carbonate, then place the beaker on magnetic stirring apparatus, centrifugal filtration is taken out after 45 ~ 50min of stir process, and to obtain filtrate D standby
With；
（6）By step（5）Resulting filtrate D is put into beaker, and 7 ~ 9 times of filtrate D gross mass is then added into beaker
N-hexane, 2 ~ 4 times the step of（4）Mixed liquor C obtained, then places the beaker on magnetic stirring apparatus, and stir process 1 ~
It is spare after 1.2h；
（7）To step（6）Treated, and beaker is heated, and keeping temperature is 450 ~ 460 DEG C, and continuous stir process, and 1
Substance in beaker is put into after ~ 1.5h in the dehydrated alcohol of 4 ~ 6 times of its gross mass, it is spare that centrifugal filtration obtains filtrate E；
（8）By Fe(NO3)39H2O, ethyl alcohol according to weight ratio 1:5 ~ 6, which carry out mixing, is put into reaction kettle, then again to reaction
The sodium hydroxide of its gross mass 24 ~ 28% is added in kettle, is taken out after being stirred continuously 2 ~ 3h of processing, is then placed in natural at room temperature
It is spare that mixture F is obtained after 8 ~ 10h of aging process；
（9）By step（7）Resulting filtrate E and step（8）Resulting mixture F is according to weight ratio 1:3 ~ 5 carry out mixing throwing
Enter into reaction kettle, taken out after being stirred continuously 14 ~ 16h of processing, after washed once respectively with ethyl alcohol and deionized water, then is put
Enter into Muffle furnace 2 ~ 3h of calcination processing, finally takes out.
Further, step（1）Described in high-speed stirred processing speed of agitator be 2000 ~ 2200 revs/min.
Further, step（2）Described in pressure when rolling processing in control roller be 700 ~ 720kgf/
cm2。
Further, step（3）Described in stir process when speed of agitator be 1000 ~ 1200 revs/min.
Further, step（4）Described in silane coupling agent be silane coupling agent kh550, silane coupling agent kh560,
Any one in silane coupling agent kh570.
Further, step（4）Described in ultrasonic treatment frequency be 530 ~ 560kHz, ultrasonic power be 1500 ~
1700W。
Further, step（8）Described in stir process when speed of agitator be 600 ~ 800 revs/min.
Further, step（9）Described in calcination processing when control Muffle furnace in temperature be 490 ~ 510 DEG C, during which
Keep oxygen sufficient.
The present invention has carried out special modification to nano zine oxide, and effectively improve nano zine oxide uses product
Matter imparts its novel characteristic.Wherein, be first prepared for a kind of mixed liquor C ingredient, be using carbon nanotubes as base matter,
Carry out it is processing modified made of Sheet Graphite alkene solution, in subsequent preparation process, this Sheet Graphite alkene is used as template, receives
Rice zinc oxide nucleus absorption is fixed in Sheet Graphite alkene, and by the size of the structure of Sheet Graphite alkene limitation nucleation and growth side
To effectively reducing the particle size of nano zine oxide, while the silane coupling agent ingredient in mixed liquor C can be avoided nanometer
Zinc oxide, which is reunited, influences preparation effect, and disodium ethylene diamine tetraacetate can enhance the absorption fixed effect to nano zine oxide, nitre
Sour lanthanum plays the role of catalysed promoted nucleus and generates, grows, and the filtrate E being eventually fabricated is that one kind has largely loaded nano oxygen
Change the Sheet Graphite alkene particle of zinc, has prepared a kind of mixture F again later, be a kind of ferric hydroxide gel, then by filtrate E
It is immersed in mixture F and is stirred to react, so that mutually absorption is combined iron hydroxide molecule in template with nano zine oxide, finally
It is handled by high-temperature calcination, and this Sheet Graphite alkene template full combustion is fallen, finally obtained a kind of short grained ZnO/a-
Fe2O3Nano-heterogeneous structure, partial size are uniformly distributed in 30 ran ranges, and have fabulous photocatalytic degradation.
The present invention has the following advantages that compared with prior art：
The present invention provides a kind of modification method for preparing that nano zine oxide is special, and a kind of ZnO/a-Fe has been made2O3Nanometer is different
The particle size of matter structure, this substance is small, and for average grain diameter in 30 rans, photocatalytic degradation is excellent, comprehensive service performance
It is good, the great market competitiveness and application value.
Specific embodiment
Embodiment 1
A kind of preparation method for the modified nano zinc oxide that photocatalytic degradation is strong, includes the following steps：
（1）By zinc sulfate and dehydrated alcohol according to weight ratio 1:4, which carry out mixing, is put into agitator tank, and high-speed stirred handles 1 ~ 2h
After take out mixed liquor A is spare；
（2）Carbon nanotubes is put into roller and roll processing, is taken out after 20min spare；
（3）By step（2）Carbon nanotubes that treated and N-Methyl pyrrolidone are according to weight ratio 1:10, which carry out mixing, puts into
In homogeneous blender, taken out after stir process 2h mixed liquid B is spare；
（4）By step（3）Resulting mixed liquid B is put into reaction kettle, and mixed liquid B gross mass 2% is then added into reaction kettle
Disodium ethylene diamine tetraacetate, 4% silane coupling agent, 0.3% lanthanum nitrate, 5% neopelex, then ultrasound
It is taken out after processing 20min, it is spare to obtain mixed liquor C；
（5）By step（1）Resulting mixed liquor A is put into beaker, and the carbon of mixed liquor A gross mass 7% is then added into beaker
Sour potassium, then places the beaker on magnetic stirring apparatus, and it is spare to obtain filtrate D for taking-up centrifugal filtration after stir process 45min；
（6）By step（5）Resulting filtrate D is put into beaker, and 7 times of filtrate D gross mass is then added into beaker
The step of n-hexane, 2 times（4）Mixed liquor C obtained, then places the beaker on magnetic stirring apparatus, spare after stir process 1h；
（7）To step（6）Treated, and beaker is heated, and keeping temperature is 450 DEG C, and continuous stir process, after 1h
Substance in beaker is put into the dehydrated alcohol of 4 times of its gross mass, it is spare that centrifugal filtration obtains filtrate E；
（8）By Fe(NO3)39H2O, ethyl alcohol according to weight ratio 1:5, which carry out mixing, is put into reaction kettle, then again to reaction kettle
The interior sodium hydroxide that its gross mass 24% is added takes out after being stirred continuously processing 2h, is then placed in the processing of natural aging at room temperature
It is spare that mixture F is obtained after 8h；
（9）By step（7）Resulting filtrate E and step（8）Resulting mixture F is according to weight ratio 1:3 carry out mixing investment
Into reaction kettle, takes out after being stirred continuously processing 14h, after washed once respectively with ethyl alcohol and deionized water, then put it into
Calcination processing 2h in Muffle furnace finally takes out.
Further, step（1）Described in high-speed stirred processing speed of agitator be 2000 revs/min.
Further, step（2）Described in pressure when rolling processing in control roller be 700kgf/cm2。
Further, step（3）Described in stir process when speed of agitator be 1000 revs/min.
Further, step（4）Described in silane coupling agent be silane coupling agent kh550.
Further, step（4）Described in ultrasonic treatment frequency be 530kHz, ultrasonic power be 1500W.
Further, step（8）Described in stir process when speed of agitator be 600 revs/min.
Further, step（9）Described in calcination processing when control Muffle furnace in temperature be 490 DEG C, during which keep
Oxygen is sufficient.
Embodiment 2
A kind of preparation method for the modified nano zinc oxide that photocatalytic degradation is strong, includes the following steps：
（1）By zinc sulfate and dehydrated alcohol according to weight ratio 1:5, which carry out mixing, is put into agitator tank, and high-speed stirred handles 1.5h
After take out mixed liquor A is spare；
（2）Carbon nanotubes is put into roller and roll processing, is taken out after 21min spare；
（3）By step（2）Carbon nanotubes that treated and N-Methyl pyrrolidone are according to weight ratio 1:12, which carry out mixing, puts into
In homogeneous blender, taken out after stir process 2.3h mixed liquid B is spare；
（4）By step（3）Resulting mixed liquid B is put into reaction kettle, and mixed liquid B gross mass 3% is then added into reaction kettle
Disodium ethylene diamine tetraacetate, 5% silane coupling agent, 0.4% lanthanum nitrate, 6% neopelex, then ultrasound
It is taken out after processing 23min, it is spare to obtain mixed liquor C；
（5）By step（1）Resulting mixed liquor A is put into beaker, and the carbon of mixed liquor A gross mass 9% is then added into beaker
Sour potassium, then places the beaker on magnetic stirring apparatus, and it is spare to obtain filtrate D for taking-up centrifugal filtration after stir process 48min；
（6）By step（5）Resulting filtrate D is put into beaker, and 8 times of filtrate D gross mass is then added into beaker
The step of n-hexane, 3 times（4）Mixed liquor C obtained, then places the beaker on magnetic stirring apparatus, stir process 1.1h standby
With；
（7）To step（6）Treated, and beaker is heated, and keeping temperature is 455 DEG C, and continuous stir process, 1.3h
Substance in beaker is put into afterwards in the dehydrated alcohol of 5 times of its gross mass, it is spare that centrifugal filtration obtains filtrate E；
（8）By Fe(NO3)39H2O, ethyl alcohol according to weight ratio 1:5.6, which carry out mixing, is put into reaction kettle, then again to reaction
The sodium hydroxide of its gross mass 26% is added in kettle, is taken out after being stirred continuously processing 2.5h, is then placed in natural aging at room temperature
It is spare that mixture F is obtained after processing 9h；
（9）By step（7）Resulting filtrate E and step（8）Resulting mixture F is according to weight ratio 1:4 carry out mixing investment
Into reaction kettle, takes out after being stirred continuously processing 15h, after washed once respectively with ethyl alcohol and deionized water, then put it into
Calcination processing 2.5h in Muffle furnace finally takes out.
Further, step（1）Described in high-speed stirred processing speed of agitator be 2100 revs/min.
Further, step（2）Described in pressure when rolling processing in control roller be 710kgf/cm2。
Further, step（3）Described in stir process when speed of agitator be 1100 revs/min.
Further, step（4）Described in silane coupling agent be silane coupling agent kh560.
Further, step（4）Described in ultrasonic treatment frequency be 550kHz, ultrasonic power be 1600W.
Further, step（8）Described in stir process when speed of agitator be 700 revs/min.
Further, step（9）Described in calcination processing when control Muffle furnace in temperature be 500 DEG C, during which keep
Oxygen is sufficient.
Embodiment 3
A kind of preparation method for the modified nano zinc oxide that photocatalytic degradation is strong, includes the following steps：
（1）By zinc sulfate and dehydrated alcohol according to weight ratio 1:6, which carry out mixing, is put into agitator tank, after high-speed stirred handles 2h
Take out mixed liquor A is spare；
（2）Carbon nanotubes is put into roller and roll processing, is taken out after 22min spare；
（3）By step（2）Carbon nanotubes that treated and N-Methyl pyrrolidone are according to weight ratio 1:14, which carry out mixing, puts into
In homogeneous blender, taken out after stir process 2.5h mixed liquid B is spare；
（4）By step（3）Resulting mixed liquid B is put into reaction kettle, and mixed liquid B gross mass 4% is then added into reaction kettle
Disodium ethylene diamine tetraacetate, 6% silane coupling agent, 0.5% lanthanum nitrate, 7% neopelex, then ultrasound
It is taken out after processing 25min, it is spare to obtain mixed liquor C；
（5）By step（1）Resulting mixed liquor A is put into beaker, and mixed liquor A gross mass 10% is then added into beaker
Potassium carbonate then places the beaker on magnetic stirring apparatus, and it is spare to obtain filtrate D for taking-up centrifugal filtration after stir process 50min；
（6）By step（5）Resulting filtrate D is put into beaker, and 9 times of filtrate D gross mass is then added into beaker
The step of n-hexane, 4 times（4）Mixed liquor C obtained, then places the beaker on magnetic stirring apparatus, stir process 1.2h standby
With；
（7）To step（6）Treated, and beaker is heated, and keeping temperature is 460 DEG C, and continuous stir process, 1.5h
Substance in beaker is put into afterwards in the dehydrated alcohol of 6 times of its gross mass, it is spare that centrifugal filtration obtains filtrate E；
（8）By Fe(NO3)39H2O, ethyl alcohol according to weight ratio 1:6, which carry out mixing, is put into reaction kettle, then again to reaction kettle
The interior sodium hydroxide that its gross mass 28% is added takes out after being stirred continuously processing 3h, is then placed in the processing of natural aging at room temperature
It is spare that mixture F is obtained after 10h；
（9）By step（7）Resulting filtrate E and step（8）Resulting mixture F is according to weight ratio 1:5 carry out mixing investment
Into reaction kettle, takes out after being stirred continuously processing 16h, after washed once respectively with ethyl alcohol and deionized water, then put it into
Calcination processing 3h in Muffle furnace finally takes out.
Further, step（1）Described in high-speed stirred processing speed of agitator be 2200 revs/min.
Further, step（2）Described in pressure when rolling processing in control roller be 720kgf/cm2。
Further, step（3）Described in stir process when speed of agitator be 1200 revs/min.
Further, step（4）Described in silane coupling agent be silane coupling agent kh570.
Further, step（4）Described in ultrasonic treatment frequency be 560kHz, ultrasonic power be 1700W.
Further, step（8）Described in stir process when speed of agitator be 800 revs/min.
Further, step（9）Described in calcination processing when control Muffle furnace in temperature be 510 DEG C, during which keep
Oxygen is sufficient.
Comparative example 1
This comparative example 1 compared with Example 2, eliminates step（2）~（4）Preparation for mixed liquor C and subsequent corresponding
It uses, method and step in addition to this is all the same.
Comparative example 2
This comparative example 2 compared with Example 2, eliminates step（4）In disodium ethylene diamine tetraacetate, silane coupling agent,
Lanthanum nitrate and neopelex ingredient, method and step in addition to this are all the same.
Control group
Application No. is：201710554599.7 a kind of preparation method of disclosed nano zine oxide heterojunction structure.
In order to compare effect of the present invention, to above-described embodiment 2, comparative example 1, comparative example 2, the corresponding system of control group
Finished product be tested for the property, specifically every group takes 3 parts of samples, respectively by every group of sample be placed in aqueous solution of methylene blue,
It in methyl blue aqueous solution, rhodamine aqueous solution, is reacted 2 hours under ultraviolet light, measurement methylene blue, methyl blue and sieve
Red bright degradation rate, specific test result correlation data are as shown in table 1 below：
Table 1
The modified nano zinc oxide made from the method for the present invention it can be seen from upper table 1 has extremely strong photocatalytic degradation, using effect
It is good, the great market competitiveness and productivity effect.
Claims (8)
1. a kind of preparation method for the modified nano zinc oxide that photocatalytic degradation is strong, which is characterized in that include the following steps：
（1）By zinc sulfate and dehydrated alcohol according to weight ratio 1:4 ~ 6, which carry out mixing, is put into agitator tank, and high-speed stirred processing 1 ~
Taken out after 2h mixed liquor A is spare；
（2）Carbon nanotubes is put into roller and roll processing, is taken out after 20 ~ 22min spare；
（3）By step（2）Carbon nanotubes that treated and N-Methyl pyrrolidone are according to weight ratio 1:10 ~ 14 carry out mixing investment
Into homogeneous blender, taken out after 2 ~ 2.5h of stir process mixed liquid B is spare；
（4）By step（3）Resulting mixed liquid B is put into reaction kettle, then into reaction kettle be added mixed liquid B gross mass 2 ~
4% disodium ethylene diamine tetraacetate, 4 ~ 6% silane coupling agent, 0.3 ~ 0.5% lanthanum nitrate, 5 ~ 7% dodecyl benzene sulfonic acid
Sodium takes out after being then ultrasonically treated 20 ~ 25min, it is spare to obtain mixed liquor C；
（5）By step（1）Resulting mixed liquor A is put into beaker, and mixed liquor A gross mass 7 ~ 10% is then added into beaker
Potassium carbonate, then place the beaker on magnetic stirring apparatus, centrifugal filtration is taken out after 45 ~ 50min of stir process, and to obtain filtrate D standby
With；
（6）By step（5）Resulting filtrate D is put into beaker, and 7 ~ 9 times of filtrate D gross mass is then added into beaker
N-hexane, 2 ~ 4 times the step of（4）Mixed liquor C obtained, then places the beaker on magnetic stirring apparatus, and stir process 1 ~
It is spare after 1.2h；
（7）To step（6）Treated, and beaker is heated, and keeping temperature is 450 ~ 460 DEG C, and continuous stir process, and 1
Substance in beaker is put into after ~ 1.5h in the dehydrated alcohol of 4 ~ 6 times of its gross mass, it is spare that centrifugal filtration obtains filtrate E；
（8）By Fe(NO3)39H2O, ethyl alcohol according to weight ratio 1:5 ~ 6, which carry out mixing, is put into reaction kettle, then again to reaction
The sodium hydroxide of its gross mass 24 ~ 28% is added in kettle, is taken out after being stirred continuously 2 ~ 3h of processing, is then placed in natural at room temperature
It is spare that mixture F is obtained after 8 ~ 10h of aging process；
（9）By step（7）Resulting filtrate E and step（8）Resulting mixture F is according to weight ratio 1:3 ~ 5 carry out mixing throwing
Enter into reaction kettle, taken out after being stirred continuously 14 ~ 16h of processing, after washed once respectively with ethyl alcohol and deionized water, then is put
Enter into Muffle furnace 2 ~ 3h of calcination processing, finally takes out.
2. a kind of preparation method of the strong modified nano zinc oxide of photocatalytic degradation according to claim 1, feature
It is, step（1）Described in high-speed stirred processing speed of agitator be 2000 ~ 2200 revs/min.
3. a kind of preparation method of the strong modified nano zinc oxide of photocatalytic degradation according to claim 1, feature
It is, step（2）Described in pressure when rolling processing in control roller be 700 ~ 720kgf/cm2。
4. a kind of preparation method of the strong modified nano zinc oxide of photocatalytic degradation according to claim 1, feature
It is, step（3）Described in stir process when speed of agitator be 1000 ~ 1200 revs/min.
5. a kind of preparation method of the strong modified nano zinc oxide of photocatalytic degradation according to claim 1, feature
It is, step（4）Described in silane coupling agent be silane coupling agent kh550, silane coupling agent kh560, silane coupling agent
Any one in kh570.
6. a kind of preparation method of the strong modified nano zinc oxide of photocatalytic degradation according to claim 1, feature
It is, step（4）Described in ultrasonic treatment frequency be 530 ~ 560kHz, ultrasonic power be 1500 ~ 1700W.
7. a kind of preparation method of the strong modified nano zinc oxide of photocatalytic degradation according to claim 1, feature
It is, step（8）Described in stir process when speed of agitator be 600 ~ 800 revs/min.
8. a kind of preparation method of the strong modified nano zinc oxide of photocatalytic degradation according to claim 1, feature
It is, step（9）Described in calcination processing when control Muffle furnace in temperature be 490 ~ 510 DEG C, during which keep oxygen sufficient.
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| CN110725062A (en) * | 2019-09-16 | 2020-01-24 | 浙江海洋大学 | Method for preparing netting by compounding multi-strand antifouling net wire |
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