CN106732384A - A kind of modified silica nanoparticle, preparation method and application - Google Patents
A kind of modified silica nanoparticle, preparation method and application Download PDFInfo
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- CN106732384A CN106732384A CN201611078771.8A CN201611078771A CN106732384A CN 106732384 A CN106732384 A CN 106732384A CN 201611078771 A CN201611078771 A CN 201611078771A CN 106732384 A CN106732384 A CN 106732384A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000007787 solid Substances 0.000 claims abstract description 52
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 33
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000003463 adsorbent Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 18
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims abstract description 11
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims abstract description 11
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims abstract description 11
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical class CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- MWVTWFVJZLCBMC-UHFFFAOYSA-N 4,4'-bipyridine Chemical group C1=NC=CC(C=2C=CN=CC=2)=C1 MWVTWFVJZLCBMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims description 28
- 235000019441 ethanol Nutrition 0.000 claims description 24
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 22
- 229910052763 palladium Inorganic materials 0.000 claims description 11
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical class CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000002372 labelling Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 4
- 239000005543 nano-size silicon particle Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 39
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 abstract description 22
- 238000001179 sorption measurement Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- MCTWTZJPVLRJOU-UHFFFAOYSA-O 1-methylimidazole Chemical compound CN1C=C[NH+]=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-O 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- 241000165940 Houjia Species 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229960000074 biopharmaceutical Drugs 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229920001429 chelating resin Polymers 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003564 dental alloy Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000005303 weighing Methods 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to a kind of modified silica nanoparticle, preparation method and application, belong to technical field of nanometer material preparation.Nanometer silicon dioxide particle and 3 chloropropyl triethoxysilanes are added in ethanol solution first, solid matter are taken out after back flow reaction and is labeled as COTS SNPs；The COTS SNPs that will be obtained are added in 4,4 bipyridyl solutions, then sequentially add vinyl chloride, toluene and CuCl, solid matter is taken out after back flow reaction and is labeled as VC SNPs；The VC SNPs that will be obtained are added in ethanol solution, are subsequently adding triethylamine and 1 methylimidazole, solid matter is taken out after back flow reaction and obtains final modified silica nanoparticle, labeled as MDZ SNPs.The modified silica nanoparticle can be used as adsorbent, and the palladium ion in adsorbent solution, material is cheap, it is easy to synthesize, and is easily separated with the aqueous solution, with high adsorption and reusable edible.
Description
Technical field
The present invention relates to a kind of modified silica nanoparticle, preparation method and application, belong to nano material preparation
Technical field.
Background technology
Palladium be it is a kind of can be used to electroplating, the platinum group metal of catalyst, dental alloy, brazing alloy and various contact materials,
With unique physics and chemical property, chemical industry catalysis, Aero-Space, microelectric technique, waste gas purification and metallurgy are widely used in
The multiple fields such as industry, rise in the most advanced branches of science and the modern industry such as petrochemical industry, electric, environmental protection, bio-pharmaceuticals, national defence
Crucial and central role.Palladium in nature generally with other element associations, and grade is low.With increasingly weighing for environmental protection
Will, and catalyst deeply developing and applying, the demand of Metal Palladium rapidly increases.Sustainable use and gold in face of resource
Belong to the rise successively of palladium price, separation and recovery palladium has great from the catalyst of failure and various waste materials, the waste liquid containing palladium
Economic benefit and social benefit.Adsorbing separation concentration method the features such as selectivity is good, simple to operate due to being generally taken seriously.Mesh
The wide adsorbent of preceding application has nano silicon, activated carbon, polyurethane foam plastics, chelating resin etc..In order to adapt to
Various purposes and requirement, the effort of people's research and development new adsorbent were never interrupted.Wherein, silica nano material by
It is the choosing of the ideal of sorbent material in there is high-specific surface area, inexpensive, modified, environmental protection is readily synthesized.
The content of the invention
For problem and deficiency that above-mentioned prior art is present, a kind of modified silica nanoparticle of offer of the invention,
Preparation method and application.The modified silica nanoparticle can be used as adsorbent, and the palladium ion in adsorbent solution, material is honest and clean
Valency, it is easy to synthesize, easily separates with the aqueous solution, with high adsorption and reusable edible.The present invention is real by the following technical programs
It is existing.
A kind of modified silica nanoparticle, its structural formula is：
, in formulaIt is nanometer silicon dioxide particle.
A kind of preparation method of modified silica nanoparticle, it is comprised the following steps that：
（1）Nanometer silicon dioxide particle and 3- chloropropyl triethoxysilanes are added in ethanol solution first, are flowed back
Take out solid matter after reaction to be vacuum dried with after absolute ethanol washing centrifugation, the Product Labeling that will be obtained is COTS-
SNPs；
（2）By step（1）The COTS-SNPs for obtaining is added in 4,4- bipyridyl solutions, then sequentially adds vinyl chloride, toluene
And CuCl, taken out after back flow reaction after solid matter washs centrifugation with ethanol solution and be vacuum dried, the product that will be obtained
Substance markers are VC-SNPs；
（3）By step（2）The VC-SNPs for obtaining is added in ethanol solution, is subsequently adding triethylamine and 1- methylimidazoles,
Taken out after back flow reaction after solid matter washs centrifugation with ethanol solution and be vacuum dried, be finally modified titanium dioxide
Nano silicon particles, labeled as MDZ-SNPs.
The step（1）Middle 3- chloropropyl triethoxysilanes are 1.6 with nanometer silicon dioxide particle liquid-solid ratio:1~
1.8:1ml/g, ethanol solution is 16 with nanometer silicon dioxide particle liquid-solid ratio:1~18:1ml/g.
The step（2）Middle 4,4- bipyridyl solutions are 20 with the liquid-solid ratio of COTS-SNPs:1~30:1ml/g, vinyl chloride
It is 2 with the liquid-solid ratio of COTS-SNPs:1~3:1ml/g, toluene is 10 with the liquid-solid ratio of COTS-SNPs:1~15:1, CuCl with
COTS-SNPs mass ratioes are 1:30~1:50.
The step（3）Middle absolute ethyl alcohol is 15 with the liquid-solid ratio of VC-SNPs:1~25:1ml/g, triethylamine and VC-
The liquid-solid ratio of SNPs is 1:1~1:1.5ml/g, 1- methylimidazole are 1 with the mass ratio of VC-SNPs:1.6~1:1.8.
The step（1）42~54h of back flow reaction under the conditions of 65~80 DEG C.
The step（2）42~54h of back flow reaction under the conditions of 80~90 DEG C.
The step（3）42~54h of back flow reaction under the conditions of 80~90 DEG C.
A kind of modified silica nanoparticle as palladium adsorbent application.
Above-mentioned organic reagent and inorganic reagent are all for analysis purchased in market is pure.
The modified silica nanoparticle adsorbent that the present invention is prepared is mainly used in adsorbing separation palladium ion, and existing
There is technology to compare, have the following advantages that：
（1）Adsorption rate to palladium ion is high.
（2）Raw material of the invention are cheap, be readily synthesized.
（3）Nano SiO 2 particle adsorbent of the invention is nontoxic, stable performance, it is easy to separate, and repeats profit
With not causing secondary pollution to environment.
（4）With preferably application and economic worth.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
The modified silica nanoparticle, its structural formula is：
, in formulaIt is nanometer silicon dioxide particle.
The preparation method of the modified silica nanoparticle, it is comprised the following steps that：
（1）It is 1.6 to be first according to liquid-solid ratio:1ml/g mixes nanometer silicon dioxide particle with 3- chloropropyl triethoxysilanes
Uniformly, according to ethanol solution and nanometer silicon dioxide particle liquid-solid ratio it is then 16:1ml/g is added to ethanol solution
In, centrifugation is taken out solid matter and is vacuum dried with after absolute ethanol washing centrifugation after 65 DEG C of back flow reaction 42h, will
The Product Labeling for obtaining is COTS-SNPs；
（2）It is 20 according to liquid-solid ratio:1ml/g is by step（1）The COTS-SNPs for obtaining is added in 4,4- bipyridyl solutions, so
After sequentially add vinyl chloride, toluene and CuCl, wherein vinyl chloride and the liquid-solid ratio of COTS-SNPs is 2:1ml/g, toluene with
The liquid-solid ratio of COTS-SNPs is 10:1, CuCl is 1 with COTS-SNPs mass ratioes:30, the centrifugation point after 80 DEG C of back flow reaction 42h
From, taking out after solid matter washs centrifugation with ethanol solution and be vacuum dried, the Product Labeling that will be obtained is VC-
SNPs；
（3）It is 15 according to liquid-solid ratio:1ml/g is by step（2）The VC-SNPs for obtaining is added in ethanol solution, Ran Houjia
Enter triethylamine and 1- methylimidazoles, wherein triethylamine and the liquid-solid ratio of VC-SNPs is 1:1ml/g, 1- methylimidazole and VC-SNPs
Mass ratio be 1:1.6, the centrifugation after 80 DEG C of back flow reaction 42h, take out solid matter washed with ethanol solution from
The heart is vacuum dried after separating, and final modified silica nanoparticle is obtained, labeled as MDZ-SNPs.
Absorption palladium ion performance measurement：
After 20mgMDZ-SNPs adsorbents input initial concentration is taken to shake absorption 2h in the palladium ion solution of 100mg/L, centrifugation
Separating adsorbent, remaining palladium ion concentration is 25.4mg/L in determining filtrate with ICP-OES, and adsorption rate is 74.6%.To adsorb
The adsorbent of palladium ion h of agitator treating 4 in thiourea solution (10wt%), then with water washing is distilled 3 times, finally by adsorbent
8h is vacuum dried at 70 DEG C.Above-mentioned adsorbent 20mg input initial concentrations are taken to be inhaled to be shaken in the palladium ion solution of 100mg/L
After attached 2h, centrifugation adsorbent, remaining palladium ion concentration is 26.1mg/L in determining filtrate with ICP-OES, and adsorption rate is
73.9%.Illustrate the modified silica nanoparticle MDZ-SNPs reusable edibles of adsorbing separation palladium of the invention.
Embodiment 2
The modified silica nanoparticle, its structural formula is：
, in formulaIt is nanometer silicon dioxide particle.
The preparation method of the modified silica nanoparticle, it is comprised the following steps that：
（1）It is 1.7 to be first according to liquid-solid ratio:1ml/g mixes nanometer silicon dioxide particle with 3- chloropropyl triethoxysilanes
Uniformly, according to ethanol solution and nanometer silicon dioxide particle liquid-solid ratio it is then 17:1ml/g is added to ethanol solution
In, centrifugation is taken out solid matter and is vacuum dried with after absolute ethanol washing centrifugation after 70 DEG C of back flow reaction 48h, will
The Product Labeling for obtaining is COTS-SNPs；
（2）It is 25 according to liquid-solid ratio:1ml/g is by step（1）The COTS-SNPs for obtaining is added in 4,4- bipyridyl solutions, so
After sequentially add vinyl chloride, toluene and CuCl, wherein vinyl chloride and the liquid-solid ratio of COTS-SNPs is 2.5:1ml/g, toluene with
The liquid-solid ratio of COTS-SNPs is 12.5:1, CuCl is 1 with COTS-SNPs mass ratioes:40, it is centrifuged after 85 DEG C of back flow reaction 48h
Separate, take out after solid matter washs centrifugation with ethanol solution and be vacuum dried, the Product Labeling that will be obtained is VC-
SNPs；
（3）It is 20 according to liquid-solid ratio:1ml/g is by step（2）The VC-SNPs for obtaining is added in ethanol solution, Ran Houjia
Enter triethylamine and 1- methylimidazoles, wherein triethylamine and the liquid-solid ratio of VC-SNPs is 1:1.25ml/g, 1- methylimidazole and VC-
The mass ratio of SNPs is 1:1.7, the centrifugation after 85 DEG C of back flow reaction 48h is taken out solid matter and is washed with ethanol solution
It is vacuum dried after washing centrifugation, final modified silica nanoparticle is obtained, labeled as MDZ-SNPs.
Absorption palladium ion performance measurement：
After 20mgMDZ-SNPs adsorbents input initial concentration is taken to shake absorption 2h in the palladium ion solution of 100mg/L, centrifugation
Separating adsorbent, remaining palladium ion concentration is 18.8mg/L in determining filtrate with ICP-OES, and adsorption rate is 81.2%.To adsorb
The adsorbent of palladium ion agitator treating 4h in thiourea solution (10wt%), then with water washing is distilled 3 times, finally by adsorbent
8h is vacuum dried at 70 DEG C.Above-mentioned adsorbent 20mg input initial concentrations are taken to be inhaled to be shaken in the palladium ion solution of 100mg/L
After attached 2h, centrifugation adsorbent, remaining palladium ion concentration is 19.7mg/L in determining filtrate with ICP-OES, and adsorption rate is
80.3%.Illustrate the modified silica nanoparticle MDZ-SNPs reusable edibles of adsorbing separation palladium of the invention.
Embodiment 3
The modified silica nanoparticle, its structural formula is：
, in formulaIt is nanometer silicon dioxide particle.
The preparation method of the modified silica nanoparticle, it is comprised the following steps that：
（1）It is 1.8 to be first according to liquid-solid ratio:1ml/g mixes nanometer silicon dioxide particle with 3- chloropropyl triethoxysilanes
Uniformly, according to ethanol solution and nanometer silicon dioxide particle liquid-solid ratio it is then 18:1ml/g is added to ethanol solution
In, centrifugation is taken out solid matter and is vacuum dried with after absolute ethanol washing centrifugation after 80 DEG C of back flow reaction 54h, will
The Product Labeling for obtaining is COTS-SNPs；
（2）It is 30 according to liquid-solid ratio:1ml/g is by step（1）The COTS-SNPs for obtaining is added in 4,4- bipyridyl solutions, so
After sequentially add vinyl chloride, toluene and CuCl, wherein vinyl chloride and the liquid-solid ratio of COTS-SNPs is 3:1ml/g, toluene with
The liquid-solid ratio of COTS-SNPs is 15:1, CuCl is 1 with COTS-SNPs mass ratioes:50, the centrifugation point after 90 DEG C of back flow reaction 54h
From, taking out after solid matter washs centrifugation with ethanol solution and be vacuum dried, the Product Labeling that will be obtained is VC-
SNPs；
（3）It is 25 according to liquid-solid ratio:1ml/g is by step（2）The VC-SNPs for obtaining is added in ethanol solution, Ran Houjia
Enter triethylamine and 1- methylimidazoles, wherein triethylamine and the liquid-solid ratio of VC-SNPs is 1:1.5ml/g, 1- methylimidazole and VC-
The mass ratio of SNPs is 1:1.8, the centrifugation after 90 DEG C of back flow reaction 54h is taken out solid matter and is washed with ethanol solution
It is vacuum dried after washing centrifugation, final modified silica nanoparticle is obtained, labeled as MDZ-SNPs.
Absorption palladium ion performance measurement：
After 20mgMDZ-SNPs adsorbents input initial concentration is taken to shake absorption 2h in the palladium ion solution of 100mg/L, centrifugation
Separating adsorbent, remaining palladium ion concentration is 24.8mg/L in determining filtrate with ICP-OES, and adsorption rate is 75.2%.To adsorb
The adsorbent of palladium ion agitator treating 4h in thiourea solution (10wt%), then with water washing is distilled 3 times, finally by adsorbent
8h is vacuum dried at 70 DEG C.Above-mentioned adsorbent 20mg input initial concentrations are taken to be inhaled to be shaken in the palladium ion solution of 100mg/L
After attached 2h, centrifugation adsorbent, remaining palladium ion concentration is 25.5mg/L in determining filtrate with ICP-OES, and adsorption rate is
74.5%.Illustrate the modified silica nanoparticle MDZ-SNPs reusable edibles of adsorbing separation palladium of the invention.
Specific embodiment of the invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula, in the ken that those of ordinary skill in the art possess, can also do on the premise of present inventive concept is not departed from
Go out various change.
Claims (9)
1. a kind of modified silica nanoparticle, it is characterised in that：Its structural formula is：
, in formulaIt is nanometer silicon dioxide particle.
2. a kind of preparation method of modified silica nanoparticle according to claim 1, it is characterised in that specific step
It is rapid as follows：
（1）Nanometer silicon dioxide particle and 3- chloropropyl triethoxysilanes are added in ethanol solution first, are flowed back
Take out solid matter after reaction to be vacuum dried with after absolute ethanol washing centrifugation, the Product Labeling that will be obtained is COTS-
SNPs；
（2）By step（1）The COTS-SNPs for obtaining is added in 4,4- bipyridyl solutions, then sequentially adds vinyl chloride, toluene
And CuCl, taken out after back flow reaction after solid matter washs centrifugation with ethanol solution and be vacuum dried, the product that will be obtained
Substance markers are VC-SNPs；
（3）By step（2）The VC-SNPs for obtaining is added in ethanol solution, is subsequently adding triethylamine and 1- methylimidazoles,
Taken out after back flow reaction after solid matter washs centrifugation with ethanol solution and be vacuum dried, be finally modified titanium dioxide
Nano silicon particles, labeled as MDZ-SNPs.
3. the preparation method of modified silica nanoparticle according to claim 2, it is characterised in that：The step
（1）Middle 3- chloropropyl triethoxysilanes are 1.6 with nanometer silicon dioxide particle liquid-solid ratio:1~1.8:1ml/g, absolute ethyl alcohol
Solution is 16 with nanometer silicon dioxide particle liquid-solid ratio:1~18:1ml/g.
4. the preparation method of modified silica nanoparticle according to claim 2, it is characterised in that：The step
（2）Middle 4,4- bipyridyl solutions are 20 with the liquid-solid ratio of COTS-SNPs:1~30:The liquid of 1ml/g, vinyl chloride and COTS-SNPs
Gu than being 2:1~3:1ml/g, toluene is 10 with the liquid-solid ratio of COTS-SNPs:1~15:1, CuCl with COTS-SNPs mass ratioes
It is 1:30~1:50.
5. the preparation method of modified silica nanoparticle according to claim 2, it is characterised in that：The step
（3）Middle absolute ethyl alcohol is 15 with the liquid-solid ratio of VC-SNPs:1~25:1ml/g, triethylamine is 1 with the liquid-solid ratio of VC-SNPs:1~
1:1.5ml/g, 1- methylimidazole are 1 with the mass ratio of VC-SNPs:1.6~1:1.8.
6. the preparation method of modified silica nanoparticle according to claim 2, it is characterised in that：The step
（1）42~54h of back flow reaction under the conditions of 65~80 DEG C.
7. the preparation method of modified silica nanoparticle according to claim 2, it is characterised in that：The step
（2）42~54h of back flow reaction under the conditions of 80~90 DEG C.
8. the preparation method of modified silica nanoparticle according to claim 2, it is characterised in that：The step
（3）42~54h of back flow reaction under the conditions of 80~90 DEG C.
9. a kind of modified silica nanoparticle according to claim 1 to 8 any one as palladium adsorbent should
With.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107321314A (en) * | 2017-06-22 | 2017-11-07 | 北京大学深圳研究生院 | A kind of magnetic adsorbent preparation method and application of green high-efficient palladium |
| CN108262026A (en) * | 2018-01-04 | 2018-07-10 | 昆明理工大学 | A kind of improved silica nano adsorber and its preparation method and application |
| CN108642039A (en) * | 2018-06-29 | 2018-10-12 | 山东阳成生物科技有限公司 | A kind of immobilized glutamate decarboxylase and its method for producing γ-aminobutyric acid |
| CN109569547A (en) * | 2018-12-05 | 2019-04-05 | 昆明理工大学 | A kind of functional magnetic material and its preparation method and application |
| CN110394146A (en) * | 2019-07-05 | 2019-11-01 | 重庆科技学院 | A kind of preparation method and products thereof of palladium ion adsorbent material |
| US11065182B2 (en) | 2018-03-01 | 2021-07-20 | Imam Abdulrahman Bin Faisal University | Resin composite and restoration containing azole-functionalized silica |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100136319A1 (en) * | 2008-12-03 | 2010-06-03 | Keio University | Method for forming mesoporous silica layer, its porous coating, anti-reflection coating, and optical member |
| CN102847522A (en) * | 2012-09-15 | 2013-01-02 | 安徽师范大学 | Preparation method and application of functional silica nano material |
| CN106040162A (en) * | 2016-07-01 | 2016-10-26 | 昆明理工大学 | Surface modified silicon dioxide material, preparation method and application thereof |
| CN106111065A (en) * | 2016-07-01 | 2016-11-16 | 昆明理工大学 | A kind of modified activated carbon absorbent and its preparation method and application |
-
2016
- 2016-11-30 CN CN201611078771.8A patent/CN106732384B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100136319A1 (en) * | 2008-12-03 | 2010-06-03 | Keio University | Method for forming mesoporous silica layer, its porous coating, anti-reflection coating, and optical member |
| CN102847522A (en) * | 2012-09-15 | 2013-01-02 | 安徽师范大学 | Preparation method and application of functional silica nano material |
| CN106040162A (en) * | 2016-07-01 | 2016-10-26 | 昆明理工大学 | Surface modified silicon dioxide material, preparation method and application thereof |
| CN106111065A (en) * | 2016-07-01 | 2016-11-16 | 昆明理工大学 | A kind of modified activated carbon absorbent and its preparation method and application |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107321314A (en) * | 2017-06-22 | 2017-11-07 | 北京大学深圳研究生院 | A kind of magnetic adsorbent preparation method and application of green high-efficient palladium |
| CN107321314B (en) * | 2017-06-22 | 2020-02-14 | 北京大学深圳研究生院 | Preparation method and application of green high-efficiency palladium magnetic adsorbent |
| CN108262026A (en) * | 2018-01-04 | 2018-07-10 | 昆明理工大学 | A kind of improved silica nano adsorber and its preparation method and application |
| CN108262026B (en) * | 2018-01-04 | 2021-08-20 | 昆明理工大学 | Modified silicon dioxide nano adsorbent and preparation method and application thereof |
| US11065182B2 (en) | 2018-03-01 | 2021-07-20 | Imam Abdulrahman Bin Faisal University | Resin composite and restoration containing azole-functionalized silica |
| CN108642039A (en) * | 2018-06-29 | 2018-10-12 | 山东阳成生物科技有限公司 | A kind of immobilized glutamate decarboxylase and its method for producing γ-aminobutyric acid |
| CN109569547A (en) * | 2018-12-05 | 2019-04-05 | 昆明理工大学 | A kind of functional magnetic material and its preparation method and application |
| CN110394146A (en) * | 2019-07-05 | 2019-11-01 | 重庆科技学院 | A kind of preparation method and products thereof of palladium ion adsorbent material |
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