CN108262026A - A kind of improved silica nano adsorber and its preparation method and application - Google Patents
A kind of improved silica nano adsorber and its preparation method and application Download PDFInfo
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- CN108262026A CN108262026A CN201810006543.2A CN201810006543A CN108262026A CN 108262026 A CN108262026 A CN 108262026A CN 201810006543 A CN201810006543 A CN 201810006543A CN 108262026 A CN108262026 A CN 108262026A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003463 adsorbent Substances 0.000 claims abstract description 50
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 46
- 239000007787 solid Substances 0.000 claims abstract description 46
- 239000000243 solution Substances 0.000 claims abstract description 39
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 36
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000000926 separation method Methods 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002245 particle Substances 0.000 claims abstract description 16
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims abstract description 11
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 11
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000005864 Sulphur Substances 0.000 claims abstract description 11
- 238000005119 centrifugation Methods 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000004821 distillation Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims abstract description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 28
- 229910052763 palladium Inorganic materials 0.000 claims description 14
- 238000002372 labelling Methods 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000005543 nano-size silicon particle Substances 0.000 claims description 6
- 238000002386 leaching Methods 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 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
- 238000000034 method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 13
- 239000000047 product Substances 0.000 description 8
- 230000009514 concussion Effects 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- CPBHJGWJMLDUNB-UHFFFAOYSA-N ethenoxysilane Chemical compound [SiH3]OC=C CPBHJGWJMLDUNB-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
Classifications
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- 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
- B01J20/28002—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 physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/48—Isomerisation; Cyclisation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The present invention discloses a kind of improved silica nano adsorber and its preparation method and application, belongs to technical field of nanometer material preparation.Nanometer silicon dioxide particle is added to V（Absolute ethyl alcohol）：V（Water）It is 1:In 1 mixed solution, and vinyltriethoxysilane is added in, vacuum drying obtains TXL SNPs after solid-liquor separation, washing, centrifugation after back flow reaction；Obtained TXL SNPs are added to the N dissolved with acrylonitrile, N dimethyl formamide solutions add in azodiisobutyronitrile, and solid-liquor separation, washing are dried in vacuo after centrifuging after back flow reaction under nitrogen atmosphere, will obtain ALT SNPs；After obtained ALT SNPs are mixed with sulphur powder, it is added in the mixed solution of ethylenediamine and toluene, solid-liquor separation after back flow reaction is dried in vacuo after taking out solid matter ethyl alcohol and distillation water washing centrifugation, obtains final modified manometer silicon dioxide adsorbent ELD SNPs.The modified manometer silicon dioxide adsorbent can adsorb the palladium ion in acid solution, and the cost of material is low, and technique prepares simple, is easily detached with aqueous solution, have high adsorption and reusable.
Description
Technical field
The present invention relates to a kind of improved silica nano adsorbers and its preparation method and application, belong to nano material system
Standby technical field.
Background technology
The reserves of palladium on earth are rare, and more difficult, category rare precious metal series is smelted in digging.Palladium is space flight, aviation, boat
The indispensable critical materials of high-tech areas and auto manufacturing such as sea, weapons and nuclear energy and International Precious Metals investment
Non-negligible investment instrument in the market.
Absorption method be most widely used at present put forward palladium method, have efficient, equipment and easy to operate, adsorbent can
Regeneration and Reusability, it is low in the pollution of the environment many advantages, such as, the active charcoal of common adsorbent and ion exchange resin, wherein living
Property charcoal absorption because of limited sorption capacity, poor selectivity, consumption charcoal amount is high, and broken abrasion easily causes palladium loss, using being restricted.And
Ion exchange resin carries in palladium amount better than activated carbon in adsorption rate and saturation, and resin have high mechanical strength, it is wear-resistant,
The characteristics of anti-extrusion and easy desorption, but cannot selectively extract palladium.
Based on this, the present invention uses for reference nano material in the successful application of absorbent fields, proposes a kind of modified nano-silica
SiClx adsorbent, preparation method and applications, the modified manometer silicon dioxide adsorbent can adsorb the palladium in acid leaching solution
Ion.This method is simply clear, and the cost of material is low, and technique is prepared simply, and adsorbent is reusable, has preferable application
Prospect.
Invention content
For the above-mentioned prior art there are the problem of and deficiency, the purpose of the present invention is to provide a kind of modified nano-silicas
SiClx adsorbent, the modified manometer silicon dioxide adsorbent can adsorb the palladium ion in acid solution, and the cost of material is low, technique
It prepares simple, is easily detached with aqueous solution, there is high adsorption and reusable.The invention is realized by the following technical scheme.
A kind of improved silica nano adsorber, structural formula are：
, in formulaFor nanometer silicon dioxide particle.
It is specific to walk another object of the present invention is to provide a kind of preparation method of improved silica nano adsorber
It is rapid as follows：
（1）Nanometer silicon dioxide particle is added to V（Absolute ethyl alcohol）：V（Water）It is 1:In 1 mixed solution, and add in three second of vinyl
Oxysilane, solid-liquor separation after back flow reaction take out after solid matter wash centrifugation with absolute ethyl alcohol and are dried in vacuo, general
The Product Labeling arrived is TXL-SNPs.
（2）By step（1）Obtained TXL-SNPs is added to the N,N-dimethylformamide solution dissolved with acrylonitrile
（DMF）In, azodiisobutyronitrile is added in, solid-liquor separation after back flow reaction under nitrogen atmosphere takes out solid matter and washed with distillation
It is dried in vacuo after washing centrifugation, is ALT-SNPs by obtained Product Labeling.
（3）By step（2）After obtained ALT-SNPs is mixed with sulphur powder, it is added to the mixed solution of ethylenediamine and toluene
In, solid-liquor separation after back flow reaction is dried in vacuo after taking out solid matter ethyl alcohol and distillation water washing centrifugation, obtains most
Whole modified manometer silicon dioxide adsorbent, labeled as ELD-SNPs.
Step of the present invention（1）Medium vinyl triethoxysilane is 1 with nanometer silicon dioxide particle liquid-solid ratio:1~2:1
The mixed solution of ml/g, absolute ethyl alcohol and water is 10 with nanometer silicon dioxide particle liquid-solid ratio:1~17:1 ml/g.
Step of the present invention（2）Middle acrylonitrile solution is 3 with TXL-SNPs liquid-solid ratioes:1~5:1 ml/g, N, N- dimethyl methyls
Amide solution is 46 with TXL-SNPs liquid-solid ratioes:1~50:The mass ratio of 1 ml/g, azodiisobutyronitrile and TXL-SNPs is
0.05:1~0.08:1。
Step of the present invention（3）Middle ethylenediamine solution is 2.3 with ALT-SNPs liquid-solid ratioes:1~3.4:1 ml/g, toluene solution
It is 50 with ALT-SNPs liquid-solid ratioes:1~53.4:1 ml/g, sulphur powder are 1 with ALT-SNPs mass ratioes:28~1:31.
Step of the present invention（1）Middle back flow reaction condition is：40 ~ 50 h of back flow reaction under the conditions of 60 ~ 70 DEG C.
Step of the present invention（2）Middle back flow reaction condition is：40 ~ 50 h of back flow reaction under the conditions of 70 ~ 80 DEG C.
Step of the present invention（3）Middle back flow reaction condition is：40 ~ 50 h of back flow reaction under the conditions of 75 ~ 85 DEG C.
Modified manometer silicon dioxide adsorbent of the present invention can in acid leaching solution adsorbing separation palladium.
Organic reagent and inorganic reagent of the present invention are all pure for analysis purchased in market.
Beneficial effects of the present invention：
（1）The modified manometer silicon dioxide adsorbent that the present invention is prepared is mainly used for the adsorbing separation palladium from acid leaching solution
Ion pair palladium ion has higher adsorbance.
（2）Preparation method of the invention is simple and direct, cost is relatively low, has preferable application and economic value.
（3）The nano silicon dioxide adsorbent of the present invention is nontoxic, and performance is stablized, and is easily isolated, and repeats and utilizes, right
Environment does not cause secondary pollution.
In conclusion absorption of the nano silicon dioxide adsorbent ELD-SNPs of the adsorbing separation palladium of the present invention in palladium ion
There are very big potentiality in terms of separation.
Specific embodiment
With reference to embodiment, the invention will be further described, but protection scope of the present invention is not limited to
The content.
Embodiment 1
The modified manometer silicon dioxide adsorbent, structural formula are：
, in formulaFor nanometer silicon dioxide particle.
The preparation method of the modified manometer silicon dioxide adsorbent, is as follows：
（1）It is 10 by liquid-solid ratio:Nanometer silicon dioxide particle is added to V by the ratio of 1ml/g（Absolute ethyl alcohol）：V（Water）It is 1:1 mixing
In solution, vinyltriethoxysilane is added（Vinyltriethoxysilane is with nanometer silicon dioxide particle liquid-solid ratio
1.5:1ml/g）, the solid-liquor separation after reflux 40h under the conditions of 70 DEG C taken out after solid matter wash with absolute ethyl alcohol and centrifuge
Obtained Product Labeling is TXL-SNPs by vacuum drying.
（2）By step（1）Obtained TXL-SNPs is added to the N,N-dimethylformamide solution dissolved with acrylonitrile
（DMF）In（TXL-SNPs and acrylonitrile liquid-solid ratio 3:The liquid-solid ratio of 1ml/g, n,N-Dimethylformamide solution and TXL-SNPs
46:1 ml/g）, azodiisobutyronitrile is added in, the wherein mass ratio of azodiisobutyronitrile and TXL-SNPs is 0.05:1；At 70 DEG C
Under the conditions of solid-liquor separation after back flow reaction 50h in nitrogen atmosphere, take out solid matter and be washed with distilled water vacuum after centrifugation
It is dry, it is ALT-SNPs by obtained Product Labeling.
（3）It is 1 according to sulphur powder and ALT-SNPs mass ratioes:28 ratio is by step（2）Obtained ALT-SNPs and sulphur powder
It after mixing, is added in the mixed solution of ethylenediamine and toluene, wherein ethylenediamine solution and ALT-SNPs liquid-solid ratioes are 3:1 ml/
G, toluene solution are 52 with ALT-SNPs liquid-solid ratioes:1 ml/g, 50h solid-liquor separations after back flow reaction, take out under the conditions of 75 DEG C
Solid matter ethyl alcohol and distillation water washing are dried in vacuo after centrifuging, and obtain final modified manometer silicon dioxide adsorbent,
Labeled as ELD-SNPs.
Adsorb palladium ion performance measurement：
It takes in the palladium ion solution that 20mg ELD-SNPs adsorbents input initial concentration is 100mg/L after 1 h of concussion absorption, from
Heart separating adsorbent, it is 23.8mg/L to measure remaining palladium ion concentration in filtrate with ICP-OES, adsorption rate 76.2%.It will absorption
The adsorbent of palladium ion is crossed in thiourea solution（8 wt%）Then middle 4 h of agitator treating is washed with distilled water 5 times, finally will absorption
Agent is dried in vacuo 14 h at 60 DEG C.It is in the palladium ion solution of 100 mg/L to take above-mentioned 20 mg of adsorbent inputs initial concentration
After 1 h of concussion absorption, adsorbent is centrifuged, it is 24.3 mg/L to measure remaining palladium ion concentration in filtrate with ICP-OES, is inhaled
Attached rate is 75.7 %.Illustrate that the nano silicon dioxide adsorbent ELD-SNPs of the adsorbing separation palladium of the present invention can be recycled.
Embodiment 2
The modified manometer silicon dioxide adsorbent, structural formula are：
The preparation method of the modified manometer silicon dioxide adsorbent, is as follows：
（1）It is 17 by liquid-solid ratio:Nanometer silicon dioxide particle is added to V by the ratio of 1 ml/g（Absolute ethyl alcohol）：V（Water）It is 1:1 it is mixed
It closes in solution, adds vinyltriethoxysilane（Vinyltriethoxysilane and nanometer silicon dioxide particle liquid-solid ratio
It is 1:1ml/g）, the solid-liquor separation after reflux 50h under the conditions of 60 DEG C taken out after solid matter wash with absolute ethyl alcohol and centrifuge
Obtained Product Labeling is TXL-SNPs by vacuum drying.
（2）By step（1）Obtained TXL-SNPs is added to the N,N-dimethylformamide solution dissolved with acrylonitrile
（DMF）In（TXL-SNPs and acrylonitrile liquid-solid ratio 4:The liquid-solid ratio of 1ml/g, n,N-Dimethylformamide solution and TXL-SNPs
50:1 ml/g）, azodiisobutyronitrile is added in, the wherein mass ratio of azodiisobutyronitrile and TXL-SNPs is 0.08:1；At 80 DEG C
Under the conditions of solid-liquor separation after back flow reaction 40h in nitrogen atmosphere, take out solid matter and be washed with distilled water vacuum after centrifugation
It is dry, it is ALT-SNPs by obtained Product Labeling.
（3）It is 1 according to sulphur powder and ALT-SNPs mass ratioes:31 ratio is by step（2）Obtained ALT-SNPs and sulphur powder
It after mixing, is added in the mixed solution of ethylenediamine and toluene, wherein ethylenediamine solution and ALT-SNPs liquid-solid ratioes are 3.4:1
Ml/g, toluene solution are 53.4 with ALT-SNPs liquid-solid ratioes:1 ml/g, the solid-liquor separation after back flow reaction 50h under the conditions of 75 DEG C,
It is dried in vacuo after taking out solid matter ethyl alcohol and distillation water washing centrifugation, obtains final modified manometer silicon dioxide absorption
Agent, labeled as ELD-SNPs.
Adsorb palladium ion performance measurement：
It takes in the palladium ion solution that 20mg ELD-SNPs adsorbents input initial concentration is 100 mg/L after concussion absorption 1h, from
Heart separating adsorbent, it is 25.1 mg/L to measure remaining palladium ion concentration in filtrate with ICP-OES, and adsorption rate is 74.9 %.It will inhale
The attached adsorbent for crossing palladium ion is in thiourea solution（10 wt%）Then middle 5 h of agitator treating is washed with distilled water 5 times, finally will
Adsorbent is dried in vacuo 14 h at 60 DEG C.Take the palladium ion that above-mentioned 20 mg of adsorbent inputs initial concentration is 100 mg/L molten
In liquid after 1 h of concussion absorption, adsorbent is centrifuged, it is 24.8 mg/ to measure remaining palladium ion concentration in filtrate with ICP-OES
L, adsorption rate are 75.2 %.Illustrate that the nano silicon dioxide adsorbent ELD-SNPs of the adsorbing separation palladium of the present invention is recycled profit
With.
Embodiment 3
The modified manometer silicon dioxide adsorbent, structural formula are：
The preparation method of the modified manometer silicon dioxide adsorbent, is as follows：
（1）It is 15 by liquid-solid ratio:Nanometer silicon dioxide particle is added to V by the ratio of 1 ml/g（Absolute ethyl alcohol）：V（Water）It is 1:1 it is mixed
It closes in solution, adds vinyltriethoxysilane（Vinyltriethoxysilane and nanometer silicon dioxide particle liquid-solid ratio
It is 2:1ml/g）, the solid-liquor separation after reflux 45h under the conditions of 65 DEG C taken out after solid matter wash with absolute ethyl alcohol and centrifuge
Obtained Product Labeling is TXL-SNPs by vacuum drying.
（2）By step（1）Obtained TXL-SNPs is added to the N,N-dimethylformamide solution dissolved with acrylonitrile
（DMF）In（TXL-SNPs and acrylonitrile liquid-solid ratio 5:The liquid-solid ratio of 1ml/g, n,N-Dimethylformamide solution and TXL-SNPs
48:1ml/g）, azodiisobutyronitrile is added in, the wherein mass ratio of azodiisobutyronitrile and TXL-SNPs is 0.06:1；At 75 DEG C
Under the conditions of solid-liquor separation after back flow reaction 45h in nitrogen atmosphere, take out solid matter and be washed with distilled water vacuum after centrifugation
It is dry, it is ALT-SNPs by obtained Product Labeling.
（3）It is 1 according to sulphur powder and ALT-SNPs mass ratioes:30 ratio is by step（2）Obtained ALT-SNPs and sulphur powder
It after mixing, is added in the mixed solution of ethylenediamine and toluene, wherein ethylenediamine solution and ALT-SNPs liquid-solid ratioes are 2.3:1
Ml/g, toluene solution are 50 with ALT-SNPs liquid-solid ratioes:1 ml/g, solid-liquor separation after back flow reaction 40h, takes under the conditions of 85 DEG C
It is dried in vacuo after going out solid matter ethyl alcohol and distillation water washing centrifugation, obtains final modified manometer silicon dioxide absorption
Agent, labeled as ELD-SNPs.
Adsorb palladium ion performance measurement：
It takes in the palladium ion solution that 20 mg ELD-SNPs adsorbents input initial concentration is 100 mg/L after 1 h of concussion absorption,
Adsorbent is centrifuged, it is 26.3 mg/L to measure remaining palladium ion concentration in filtrate with ICP-OES, and adsorption rate is 73.7 %.It will
The adsorbent of palladium ion was adsorbed in thiourea solution（9 wt%）Then middle 6 h of agitator treating is washed with distilled water 5 times, finally will
Adsorbent is dried in vacuo 15 h at 60 DEG C.Take the palladium ion that above-mentioned 20 mg of adsorbent inputs initial concentration is 100 mg/L molten
In liquid after 1 h of concussion absorption, adsorbent is centrifuged, it is 25.9 mg/ to measure remaining palladium ion concentration in filtrate with ICP-OES
L, adsorption rate are 74.1 %.Illustrate that the nano silicon dioxide adsorbent ELD-SNPs of the adsorbing separation palladium of the present invention is recycled profit
With.
The specific embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula within the knowledge of a person skilled in the art, can also be done under the premise of present inventive concept is not departed from
Go out various change.
Claims (9)
1. a kind of improved silica nano adsorber, structural formula are：
In formulaFor nanometer silicon dioxide particle.
2. the preparation method of modified manometer silicon dioxide adsorbent described in claim 1, which is characterized in that be as follows：
（1）Nanometer silicon dioxide particle is added to V（Absolute ethyl alcohol）：V（Water）It is 1:In 1 mixed solution, and add in three ethoxy of vinyl
Base silane, solid-liquor separation after back flow reaction, take out solid matter wash with absolute ethyl alcohol centrifuge after be dried in vacuo, will obtain
Product Labeling be TXL-SNPs；
（2）By step（1）Obtained TXL-SNPs is added in the n,N-Dimethylformamide solution dissolved with acrylonitrile, is added in
Azodiisobutyronitrile, solid-liquor separation after back flow reaction under nitrogen atmosphere are taken out after solid matter is washed with distilled water centrifugation
Obtained Product Labeling is ALT-SNPs by vacuum drying；
（3）By step（2）It after obtained ALT-SNPs is mixed with sulphur powder, is added in the mixed solution of ethylenediamine and toluene, returns
Solid-liquor separation after stream reaction takes out after solid matter ethyl alcohol is centrifuged with distillation water washing and is dried in vacuo, finally changed
Property nano silicon dioxide adsorbent, labeled as ELD-SNPs.
3. the preparation method of modified manometer silicon dioxide adsorbent according to claim 2, it is characterised in that：The step
（1）Medium vinyl triethoxysilane is 1 with nanometer silicon dioxide particle liquid-solid ratio:1~2:1 ml/g, absolute ethyl alcohol and water
Mixed solution is 10 with nanometer silicon dioxide particle liquid-solid ratio:1~17:1 ml/g.
4. the preparation method of modified manometer silicon dioxide adsorbent according to claim 2, it is characterised in that：The step
（2）Middle acrylonitrile solution is 3 with TXL-SNPs liquid-solid ratioes:1~5:1 ml/g, n,N-Dimethylformamide solution and TXL-SNPs
Liquid-solid ratio is 46:1~50:The mass ratio of 1 ml/g, azodiisobutyronitrile and TXL-SNPs are 0.05:1~0.08:1.
5. the preparation method of modified manometer silicon dioxide adsorbent according to claim 2, it is characterised in that：The step
（3）Middle ethylenediamine solution is 2.3 with ALT-SNPs liquid-solid ratioes:1~3.4:1 ml/g, toluene solution are with ALT-SNPs liquid-solid ratioes
50:1~53.4:1 ml/g, sulphur powder are 1 with ALT-SNPs mass ratioes:28~1:31.
6. the preparation method of modified manometer silicon dioxide adsorbent according to claim 2, it is characterised in that：Step（1）In
Back flow reaction condition is：40 ~ 50 h of back flow reaction under the conditions of 60 ~ 70 DEG C.
7. the preparation method of modified manometer silicon dioxide adsorbent according to claim 2, it is characterised in that：Step（2）In
Back flow reaction condition is：40 ~ 50 h of back flow reaction under the conditions of 70 ~ 80 DEG C.
8. the preparation method of modified manometer silicon dioxide adsorbent according to claim 2, it is characterised in that：Step（3）In
Back flow reaction condition is：40 ~ 50 h of back flow reaction under the conditions of 75 ~ 85 DEG C.
9. the application of modified manometer silicon dioxide adsorbent adsorbing separation palladium in acid leaching solution described in claim 1.
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| 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 |
| CN111085163A (en) * | 2018-10-23 | 2020-05-01 | 南京化学工业园环保产业协同创新有限公司 | Nano silicon dioxide adsorbent and preparation method thereof |
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