CN105709690A - Adsorbent capable of preferentially adsorbing gold and preparing method and application thereof - Google Patents
Adsorbent capable of preferentially adsorbing gold and preparing method and application thereof Download PDFInfo
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- CN105709690A CN105709690A CN201610123979.0A CN201610123979A CN105709690A CN 105709690 A CN105709690 A CN 105709690A CN 201610123979 A CN201610123979 A CN 201610123979A CN 105709690 A CN105709690 A CN 105709690A
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- adsorbent
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- thiosemicarbazides
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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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
- B01J20/02—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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses an adsorbent capable of preferentially adsorbing gold and a preparing method and application thereof and belongs to the technical field of hydrometallurgy. According to the technical scheme, the adsorbent is characterized in that 3-chloropropyl triethoxysilane reacts with thiosemicarbazide to introduce thiosemicarbazide into a silane coupling agent, then thiosemicarbazide is made to react with a multiwalled carbon nanotube coated with silicon dioxide to generate a multiwalled carbon nanotube gold adsorbent containing a thiosemicarbazide functional group, and the structure of the adsorbent is shown in the description. The invention further discloses a preparing method of the adsorbent capable of preferentially adsorbing gold and the application of the adsorbent in preferentially adsorbing gold in aqueous solution. The prepared adsorbent is novel in structure, the synthetic process is controllable and convenient to operate, and the synthesized adsorbent is high in gold adsorbing capacity, selectivity and antijamming capability and can be used for preferentially adsorbing gold in aqueous solution.
Description
Technical field
The invention belongs to technical field of wet metallurgy, be specifically related to adsorbent and the preparation side thereof of a kind of selective absorption gold
Method and application.
Background technology
Containing gold waste liquid have cyaniding waste liquid, chlorination waste liquid, chloroazotic acid waste liquid and various containing gold washes, from containing gold waste liquid
Reclaim gold significant at the aspect such as resource recycling, environmental conservation.The sides such as extraction, displacement, ion exchange and absorption
Method is usually used in from waste liquid reclaiming gold.Wherein, absorption method has low cost, the advantage such as easy and simple to handle.And conventional adsorbent is such as
Activated carbon is little to the adsorbance of gold, and poor to metal biosorption selectivitys such as common copper, nickel, lead.
Summary of the invention
Present invention solves the technical problem that and there is provided golden adsorbent of a kind of selective absorption and preparation method thereof, the party
Thiosemicarbazides is introduced silane coupler by method, then makes it prepare containing amino with the multi-wall carbon nano-tube tube reaction of coated with silica
The multi-walled carbon nano-tubes gold adsorbent of thiourea functional group, this adsorbent can be used for selective absorption gold from aqueous solution.
The present invention solves that above-mentioned technical problem adopts the following technical scheme that, the adsorbent of a kind of selective absorption gold, its
It is characterized by 3-chloropropyl triethoxysilane to react with thiosemicarbazides thiosemicarbazides introduces silane coupler, then makes
It prepares the multi-walled carbon nano-tubes gold absorption containing thiosemicarbazides functional group with the multi-wall carbon nano-tube tube reaction of coated with silica
Agent, this adsorbent has a following structure:
。
The preparation method of the adsorbent of selective absorption of the present invention gold, it is characterised in that concretely comprise the following steps:
(1) mesoporous silicon oxide cladding multi-walled carbon nano-tubes synthesis, by 2g cetyl trimethylammonium bromide ultrasonic dissolution in
In 30mL deionized water, add 100mg multi-walled carbon nano-tubes, ultrasonic 1h, add 80mL dehydrated alcohol, more ultrasonic 0.5h, then
In solution, the pH value of dropping 2mL ammonia spirit regulation solution is to 8-9, drips the anhydrous of positive silicic acid tetraacethyl under magnetic stirring
Ethanol solution, wherein positive silicic acid tetraacethyl is 1:40 with the volume ratio of dehydrated alcohol, then magnetic agitation 12h, and centrifugation is also used
Ethanol cyclic washing, until washing liquid is neutrality, is subsequently adding 60mL dehydrated alcohol and 2mL hydrochloric acid solution, and magnetic agitation 10h is removed
Cetyl trimethylammonium bromide, repeatedly with absolute ethanol washing and be washed with deionized water, is vacuum dried 24h systems in 80 DEG C subsequently
Obtain mesoporous silicon oxide cladding multi-walled carbon nano-tubes;
(2) thiosemicarbazides modifies the synthesis of silane coupler, by 12.04mL 3-chloropropyl triethoxysilane and 4.557g ammonia
Base thiourea is added separately in 60mL DMF, and the lower heating reflux reaction 12h of nitrogen protection prepares thiosemicarbazides
Modify silane coupler;
(3) synthesis of the multi-walled carbon nano-tubes gold adsorbent containing thiosemicarbazides functional group, the thiosemicarbazides prepared to step (2)
Modify and silane coupler adds mesoporous silicon oxide cladding multi-walled carbon nano-tubes and the 80mL volume ratio that 0.5g step (1) prepares
For DMF and the mixed solution of toluene of 1:7, the lower heating reflux reaction 12h of nitrogen protection, after reaction terminates
Product be the N of 1:1, N-dimethyl formyl and the mixed solution of toluene, N by volume ratio successively, N-dimethyl formyl, anhydrous second
Alcohol and ether washing, then prepare the multi-walled carbon nano-tubes gold absorption containing thiosemicarbazides functional group in 80 DEG C of vacuum drying 24h
Agent.
Application in the adsorbent selective absorption gold in aqueous of selective absorption of the present invention gold.
Sorbent structure prepared by the present invention is novel, building-up process is controlled and easy and simple to handle, and gold is inhaled by the adsorbent of synthesis
Attached amount is big, selectivity is strong and capacity of resisting disturbance strong, can be used for selective absorption gold from aqueous solution.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the prepared multi-walled carbon nano-tubes gold adsorbent containing thiosemicarbazides functional group;
Fig. 2 is the scanning electron microscope (SEM) photograph of multi-walled carbon nano-tubes;
Fig. 3 is the scanning electron microscope (SEM) photograph of the prepared multi-walled carbon nano-tubes gold adsorbent containing thiosemicarbazides functional group;
Fig. 4 is the selective absorption figure of the prepared multi-walled carbon nano-tubes gold adsorbent containing thiosemicarbazides functional group;
Fig. 5 is the adsorption time influence curve to the multi-walled carbon nano-tubes gold adsorbent gold containing thiosemicarbazides functional group.
Detailed description of the invention
By the following examples the foregoing of the present invention is described in further details, but this should be interpreted as this
The scope inventing above-mentioned theme is only limitted to below example, and all technology realized based on foregoing of the present invention belong to this
Bright scope.
Embodiment
1, the multi-walled carbon nano-tubes gold adsorbent (TSC-mSiO containing thiosemicarbazides functional group2@MWCNTs) synthesis
(1) mesoporous silicon oxide cladding multi-walled carbon nano-tubes (mSiO2@MWCNTs) synthesis
By in 2g cetyl trimethylammonium bromide ultrasonic dissolution to 30mL deionized water, add 100mg multi-walled carbon nano-tubes, super
Sound 1h, adds 80mL dehydrated alcohol, more ultrasonic 0.5h, then drips the pH value of 2mL ammonia spirit regulation solution in solution extremely
8-9, drips the ethanol solution (v:v=1:40) of positive silicic acid tetraacethyl, then magnetic agitation 12h under magnetic stirring, centrifugal point
From and with ethanol cyclic washing until washing liquid is neutrality, be subsequently adding 60mL dehydrated alcohol and 2mL concentrated hydrochloric acid, magnetic agitation 10h
Remove cetyl trimethylammonium bromide, repeatedly with absolute ethanol washing and be washed with deionized water, subsequently in 80 DEG C of vacuum drying
24h is worth mesoporous SiO2Cladding multi-walled carbon nano-tubes, is labeled as mSiO2@MWCNTs。
(2) thiosemicarbazides modifies the synthesis of silane coupler
12.04mL 3-chloropropyl triethoxysilane and 4.557g thiosemicarbazides are added separately to the N that 60mL is dried, N-bis-
In methylformamide, the lower heating reflux reaction 12h of nitrogen protection prepares product (1) thiosemicarbazides and modifies silane coupler.
(3) the multi-walled carbon nano-tubes gold adsorbent (TSC-mSiO containing thiosemicarbazides functional group2@MWCNTs) synthesis
0.5g mSiO is added in product (1)2The N,N-dimethylformamide that@MWCNTs and 80mL is dried and the toluene being dried
Mixed solution (v:v=1:7), the lower heating reflux reaction 12h of nitrogen protection, the product after reaction terminates uses N, N-dimethyl successively
The mixed solution (v:v=1:1) of formyl and toluene, N, N-dimethyl formyl, dehydrated alcohol and ether washing, then true in 80 DEG C
The empty 24h that is dried prepares the multi-walled carbon nano-tubes gold adsorbent containing thiosemicarbazides functional group, is labeled as TSC-mSiO2@MWCNTs。
The adsorbent TSC-mSiO of preparation2The infrared spectrum of@MWCNTs is as it is shown in figure 1, characteristic absorption peak 1642cm-1Corresponding amino
Functional group, this illustrates adsorbent TSC-mSiO2@MWCNTs successfully synthesizes.
The multi-walled carbon nano-tubes of preparation and adsorbent TSC-mSiO2The scanning electron microscope of@MWCNTs as shown in Figures 2 and 3, by scheming
Understanding multi-walled carbon nano-tubes to introduce after thiosemicarbazides functional group, pattern there occurs substantially change.
2, Choice tests
It is 50 μ g/mL, volume 50mL, 30mg adsorbent TSC-mSiO at metal ion initial concentration2@MWCNTs, during vibration
Between 4h, temperature 30 DEG C, under conditions of hunting speed 160rpm/min, result of the test is shown in Fig. 4.As shown in Figure 4, the adsorbent of preparation
TSC-mSiO2@MWCNTs is far longer than the adsorbance to copper, lead, cadmium and chromium, adsorbent TSC-mSiO to the adsorbance of gold2@
MWCNTs presents the characteristic of high-selectivity adsorption gold.
3, interference test
Au3+It is 50 μ g/mL with coexistent metallic ion concentration, simulates Au respectively3+- Cu2+, Au3+- Cr6+, Au3+- Pb2+, Au3 +- Cd2+, Au3+- Mn2+, Au3+- Mg2+, Au3+- Co2+, Au3+- Ni2+, Au3+- Zn2+Coexisting body Deng gold with other metal
System, at solution 50mL, 20mg adsorbent TSC-mSiO2@MWCNTs, 30 DEG C, vibration absorption 6h under conditions of 160 r/min, as
Shown in table 1, common metal ion such as Cu2+、Cr6+、Pb2+、Cd2+、Mn2+、Mg2+、Co2+、Ni2+、Zn2+Deng to adsorbent TSC-
mSiO2@MWCNTS adsorbs Au3+Almost without interference, and less to other metal adsorption that coexists, adsorbent TSC-is described
mSiO2@MWCNTs capacity of resisting disturbance is strong, and selectivity is preferable.
Table 1 interference test result.
4, adsorption dynamics adsorption kinetics
Gold initial concentration 50 μ g/mL, volume 50mL, 20mg adsorbent TSC-mSiO2@MWCNTs, temperature 30 DEG C, hunting speed
160rpm/min, result of the test is shown in Fig. 5, adsorbs the initial stage as shown in Figure 5, and adsorption rate is fast, 4h adsorbent TSC-mSiO2@
The absorption of MWCNTs reaches balance.
Embodiment above describes the ultimate principle of the present invention, principal character and advantage, the technical staff of the industry should
Understanding, the present invention is not restricted to the described embodiments, and the simply explanation present invention's described in above-described embodiment and description is former
Reason, under the scope without departing from the principle of the invention, the present invention also has various changes and modifications, and these changes and improvements each fall within
In the scope of protection of the invention.
Claims (3)
1. the adsorbent of a selective absorption gold, it is characterised in that: by 3-chloropropyl triethoxysilane and thiosemicarbazides
Thiosemicarbazides is introduced silane coupler by reaction, then makes it prepare containing ammonia with the multi-wall carbon nano-tube tube reaction of coated with silica
The multi-walled carbon nano-tubes gold adsorbent of base thiourea functional group, this adsorbent has a following structure:
。
2. the preparation method of the adsorbent of the selective absorption gold described in a claim 1, it is characterised in that concretely comprise the following steps:
(1) mesoporous silicon oxide cladding multi-walled carbon nano-tubes synthesis, by 2g cetyl trimethylammonium bromide ultrasonic dissolution in
In 30mL deionized water, add 100mg multi-walled carbon nano-tubes, ultrasonic 1h, add 80mL dehydrated alcohol, more ultrasonic 0.5h, then
In solution, the pH value of dropping 2mL ammonia spirit regulation solution is to 8-9, drips the anhydrous of positive silicic acid tetraacethyl under magnetic stirring
Ethanol solution, wherein positive silicic acid tetraacethyl is 1:40 with the volume ratio of dehydrated alcohol, then magnetic agitation 12h, and centrifugation is also used
Ethanol cyclic washing, until washing liquid is neutrality, is subsequently adding 60mL dehydrated alcohol and 2mL hydrochloric acid solution, and magnetic agitation 10h is removed
Cetyl trimethylammonium bromide, repeatedly with absolute ethanol washing and be washed with deionized water, is vacuum dried 24h systems in 80 DEG C subsequently
Obtain mesoporous silicon oxide cladding multi-walled carbon nano-tubes;
(2) thiosemicarbazides modifies the synthesis of silane coupler, by 12.04mL 3-chloropropyl triethoxysilane and 4.557g ammonia
Base thiourea is added separately in 60mL DMF, and the lower heating reflux reaction 12h of nitrogen protection prepares thiosemicarbazides
Modify silane coupler;
(3) synthesis of the multi-walled carbon nano-tubes gold adsorbent containing thiosemicarbazides functional group, the thiosemicarbazides prepared to step (2)
Modify and silane coupler adds mesoporous silicon oxide cladding multi-walled carbon nano-tubes and the 80mL volume ratio that 0.5g step (1) prepares
For DMF and the mixed solution of toluene of 1:7, the lower heating reflux reaction 12h of nitrogen protection, after reaction terminates
Product be the N of 1:1, N-dimethyl formyl and the mixed solution of toluene, N by volume ratio successively, N-dimethyl formyl, anhydrous second
Alcohol and ether washing, then prepare the multi-walled carbon nano-tubes gold absorption containing thiosemicarbazides functional group in 80 DEG C of vacuum drying 24h
Agent.
3. the application in the adsorbent selective absorption gold in aqueous of the selective absorption gold described in claim 1.
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Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106179281A (en) * | 2016-08-15 | 2016-12-07 | 河南师范大学 | A kind of gold ion solid extracting agent and its preparation method and application |
CN106435210A (en) * | 2016-09-27 | 2017-02-22 | 宁波大地化工环保有限公司 | Preparation method of trapping agent special for precious metal |
CN106700006A (en) * | 2017-01-05 | 2017-05-24 | 昆明理工大学 | Nano-silica compound material, and preparation method and application thereof |
CN106824112A (en) * | 2017-03-06 | 2017-06-13 | 济南大学 | A kind of preparation of 2 mercaptopyrimidine modified magnetic cotton stalk skins adsorbent |
CN107088403A (en) * | 2017-06-07 | 2017-08-25 | 河南师范大学 | A kind of thiosemicarbazides bonding PDA@MWCNTs adsorbents and its preparation method and application |
CN107583453A (en) * | 2017-09-18 | 2018-01-16 | 东莞市联洲知识产权运营管理有限公司 | A kind of method of low-cost processes VOCs waste gas |
CN107744796A (en) * | 2017-11-09 | 2018-03-02 | 中国工程物理研究院核物理与化学研究所 | It is a kind of to be used for adsorbent of uranium extraction and preparation method thereof in water body |
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 |
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 |
CN112295549A (en) * | 2020-09-11 | 2021-02-02 | 中南大学 | Adsorbent for selectively separating gold and preparation method and application thereof |
CN113403478A (en) * | 2021-06-15 | 2021-09-17 | 苏州市富荣环保科技有限公司 | Method for separating metals in electronic waste based on nano carbon material |
CN114887592A (en) * | 2022-04-22 | 2022-08-12 | 江苏第二师范学院 | Preparation and application of thiosemicarbazone silicon dioxide microsphere material |
CN116272879A (en) * | 2023-02-15 | 2023-06-23 | 浙江大学衢州研究院 | Green efficient preparation method of electronic grade lithium salt |
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Cited By (17)
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CN106179281A (en) * | 2016-08-15 | 2016-12-07 | 河南师范大学 | A kind of gold ion solid extracting agent and its preparation method and application |
CN106435210A (en) * | 2016-09-27 | 2017-02-22 | 宁波大地化工环保有限公司 | Preparation method of trapping agent special for precious metal |
CN106700006A (en) * | 2017-01-05 | 2017-05-24 | 昆明理工大学 | Nano-silica compound material, and preparation method and application thereof |
CN106824112A (en) * | 2017-03-06 | 2017-06-13 | 济南大学 | A kind of preparation of 2 mercaptopyrimidine modified magnetic cotton stalk skins adsorbent |
CN107088403B (en) * | 2017-06-07 | 2019-11-05 | 河南师范大学 | A kind of thiosemicarbazides bonding PDA@MWCNTs adsorbent and its preparation method and application |
CN107088403A (en) * | 2017-06-07 | 2017-08-25 | 河南师范大学 | A kind of thiosemicarbazides bonding PDA@MWCNTs adsorbents and its preparation method and application |
CN107583453A (en) * | 2017-09-18 | 2018-01-16 | 东莞市联洲知识产权运营管理有限公司 | A kind of method of low-cost processes VOCs waste gas |
CN107744796A (en) * | 2017-11-09 | 2018-03-02 | 中国工程物理研究院核物理与化学研究所 | It is a kind of to be used for adsorbent of uranium extraction and preparation method thereof in water body |
CN107744796B (en) * | 2017-11-09 | 2020-01-07 | 中国工程物理研究院核物理与化学研究所 | Adsorbent for extracting uranium from water body and preparation method thereof |
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 |
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 |
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 |
CN112295549A (en) * | 2020-09-11 | 2021-02-02 | 中南大学 | Adsorbent for selectively separating gold and preparation method and application thereof |
CN113403478A (en) * | 2021-06-15 | 2021-09-17 | 苏州市富荣环保科技有限公司 | Method for separating metals in electronic waste based on nano carbon material |
CN113403478B (en) * | 2021-06-15 | 2024-01-26 | 苏州市富荣环保科技有限公司 | Method for separating metal from electronic waste based on nano carbon material |
CN114887592A (en) * | 2022-04-22 | 2022-08-12 | 江苏第二师范学院 | Preparation and application of thiosemicarbazone silicon dioxide microsphere material |
CN116272879A (en) * | 2023-02-15 | 2023-06-23 | 浙江大学衢州研究院 | Green efficient preparation method of electronic grade lithium salt |
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Application publication date: 20160629 |