CN108754152A - A method of recycling silver from silver ion adsorbant - Google Patents
A method of recycling silver from silver ion adsorbant Download PDFInfo
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- CN108754152A CN108754152A CN201810661954.5A CN201810661954A CN108754152A CN 108754152 A CN108754152 A CN 108754152A CN 201810661954 A CN201810661954 A CN 201810661954A CN 108754152 A CN108754152 A CN 108754152A
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- silver
- silver ion
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- argentiferous
- regenerant
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- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- 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
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Abstract
The method that the present invention provides a kind of to recycle silver from silver ion adsorbant, the adsorbent for adsorbing silver ion is mixed with alcohols solvent, after ultrasonic disperse, thermal reduction reaction is carried out at 45~75 DEG C, obtains argentiferous regenerant.The adsorbent for adsorbing silver ion is dispersed in alcohols solvent by the present invention by ultrasound, then destroys the key between adsorbent and silver ion by thermal reduction reaction, while by silver ion reduction, obtaining argentiferous regenerant.The recovery method has advantage simple for process, easily operated.Meanwhile the experimental results showed that, the content of silver-colored simple substance is more than 52% in the argentiferous regenerant that the silver-colored method of recycling provided by the present invention obtains, and has higher recycle value.
Description
Technical field
The present invention relates to the technical field of heavy metal recovery more particularly to a kind of sides recycling silver from silver ion adsorbant
Method.
Background technology
Silver is a kind of argenteous transition metal.It has good ductility, has highest lead in all metals
Electrical and conductivity of heat.Silver is commonly used to make the high physical apparatus element of sensitivity, and electronic apparatus is the maximum industry of silver consuming amount,
Its use is divided into contact material, composite material and welding material.In the compound of silver, photosensitive silve halide material is silver consuming amount
One of maximum field, the current maximum several photosensitive materials of production and selling amount are rollfilms, printing paper, x-ray film, glimmering
Optical information recording piece, electron micrograph film and lithographic film etc..In addition, two masters of the silver in terms of chemical material
It to apply and be：First, silver catalyst, is such as widely used in redox and polymerisation, the industrial waste gas for handling sulfur compound
Deng；Second is that electronics finishing industrial preparation, such as silver paste, silver potassium cyanide.It is widely used due to containing silver products, these products are being made
It is standby, use and will produce after discarding a large amount of argentiferous waste, can not recycle, cause a large amount of wasting of resources.And silver ion into
It but will do harm to huamn body when entering in environment.Silver ion can react the protein for making human body with hemoglobin and various enzymes become
Property, it is more than the silver-colored spot precipitation that 0.8g will cause blue on the skin into internal silver ion.Since silver ion has very by force
Oxidisability, so can also cause the symptoms such as internal organs oedema into the silver ion in human body, causing death when serious.Human body
Without effectively arranging silver-colored mechanism, so once intake silver ion is just mainly accumulated in bone and liver.Silver ion is as heavy metal
The removal recycling of ion and be noble metal, selectivity is of great significance and economic value.
Ag is recycled from waste water+Conventional method include precipitation, electrolysis, ion exchange, UF membrane, absorption.In above-mentioned side
In method, adsorbs since easy to operate, low energy consumption, efficient, be a kind of technology of great development prospect.Many is developed at present
For detaching Ag+Adsorbent, including modified silica nanoparticle, activated carbon, waste coffee dregs, chelating resin, ion print
Mark polymer etc..It is handled by the way of absorption in water body after silver ion, the technique that tradition recycles silver from adsorbent is profit
The method eluted with solvent destroys the active force between adsorbent and silver ion using a large amount of acid or alkalinity method, from
And release silver ion, but this procedure is cumbersome, takes longer.
Invention content
The method that the purpose of the present invention is to provide a kind of to recycle silver from silver ion adsorbant, this method is simple for process,
It is easily operated.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The method that the present invention provides a kind of to recycle silver from silver ion adsorbant, includes the following steps：
The adsorbent for being adsorbed with silver ion is mixed with alcohols solvent, after ultrasonic disperse, heat is carried out at 45~75 DEG C also
Original reaction, obtains argentiferous regenerant.
Preferably, the adsorbent is Rhodanine derivates polymer.
Preferably, the alcohols solvent is methanol.
Preferably, the quality of the adsorbent of the absorption silver ion and the ratio between the volume of alcohols solvent are 1mg:1~3mL.
Preferably, the power of the ultrasonic disperse is 20~28kHz, and the time of the ultrasonic disperse is 2~5min.
Preferably, the temperature of the thermal reduction reaction is 55~65 DEG C.
Preferably, the time of the thermal reduction reaction is 10~30min.
The method that the present invention provides a kind of to recycle silver from silver ion adsorbant, will adsorb the adsorbent and alcohol of silver ion
Class solvent mixes, and after ultrasonic disperse, thermal reduction reaction is carried out at 45~75 DEG C, obtains argentiferous regenerant.The present invention passes through super
The adsorbent for adsorbing silver ion is dispersed in alcohols solvent by sound, then by thermal reduction reaction destroy adsorbent with silver from
Key between son, while by silver ion reduction, obtaining argentiferous regenerant.The recovery method have it is simple for process, it is easily operated
Advantage.Meanwhile the experimental results showed that, silver-colored simple substance contains in the argentiferous regenerant that the silver-colored method of recycling provided by the present invention obtains
Amount is more than 52%, has higher recycle value.
Description of the drawings
The XRD diagram of 1 gained argentiferous regenerant of Fig. 1 embodiments.
Specific implementation mode
The method that the present invention provides a kind of to recycle silver from silver ion adsorbant, includes the following steps：Silver will be adsorbed with
The adsorbent of ion is mixed with alcohols solvent, and after ultrasonic disperse, thermal reduction reaction is carried out at 45~75 DEG C, obtains containing silver recovery
Object.
The present invention mixes the adsorbent for adsorbing silver ion with alcohols solvent, obtains mixture.
In the present invention, the adsorbent is preferably Rhodanine derivates polymer.
In the present invention, the Rhodanine derivates polymer is preferably poly- 3- allyls rhodanine and poly- 3- cyclobutenyls sieve
At least one of tannin.
The present invention is not particularly limited the degree of polymerization of Rhodanine derivates polymer.
In the present invention, the alcohols solvent is preferably methanol.
In the present invention, the ratio between the quality of the adsorbent of the absorption silver ion and the volume of alcohols solvent preferably 1mg:
1~3mL.
After obtaining mixture, the mixture is carried out ultrasonic disperse by the present invention.It in the present invention, can by ultrasonic disperse
Adsorbent to be well-dispersed in alcohols solvent.
In the present invention, the power of the ultrasonic disperse is preferably 20~28kHz；The time of the ultrasonic disperse is preferably
2~5min.
After completing ultrasonic disperse, the mixture after ultrasonic disperse is carried out thermal reduction reaction at 45~75 DEG C by the present invention.
The present invention is not particularly limited the heating rate for being warming up to thermal reduction reaction required temperature, can be arbitrary heating
Rate.
In the present invention, the temperature of the thermal reduction reaction is preferably 55~65 DEG C.
In the present invention, the time of the thermal reduction reaction is preferably 10~30min, more preferably 15~25min；It is described
The time of thermal reduction reaction when being warming up to thermal reduction reaction required temperature preferably from counting.
After the completion of thermal reduction reaction, thermal reduction reaction products therefrom is preferably down to room temperature by the present invention, is then filtered,
Obtained solid substance is argentiferous regenerant.
In embodiments of the present invention, after the completion of the thermal reduction reaction, some metal is adhered on the wall of reactor
The substance of gloss, the present invention preferably get up the collecting material of the metallic luster on wall, with filtering obtained solid material mixing,
Obtain argentiferous regenerant.
In the present invention, silver is reduced to by thermal reduction reaction major part silver ion, the adsorbent spreads out for rhodanine
When biopolymer, part silver ion generates silver sulfide, silver sulfide and silver list with the element sulphur in Rhodanine derivates polymer
Matter is precipitated simultaneously, constitutes argentiferous regenerant.
The method provided by the invention that silver is recycled from silver ion adsorbant is carried out specifically with reference to embodiment
It is bright, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) use the poly- 3- allyls rhodanines of 20mg in 20mL concentration of silver ions 300mg/L conical flasks, concussion absorption is flat
After weighing apparatus, the front and back solution variation of absorption is measured using atomic absorption method, adsorbance method is calculated and measures adsorbent absorption silver ion
5.411mg；
(2) it is with volume ratio with methanol by the quality of the poly- 3- allyls rhodanine after absorption silver ion obtained by step (1)
1mg:After the ratio of 1mL is mixed in conical flask, ultrasonic disperse 2min under conditions of frequency is 20kHz；
(3) mixture that the step (2) ultrasonic disperse obtains is placed in 60 DEG C of water-bath, isothermal reaction 15min
Afterwards, it is down to room temperature, is filtered, is obtained silver-containing solid, while being attached with the substance of metallic luster in bottle wall, collect, with argentiferous
Solid mixes, and obtains 5mg argentiferous regenerants.
It by XRD analysis (as shown in Figure 1), can obtain, the group of the argentiferous regenerant becomes silver sulfide and silver-colored simple substance.
Argentiferous regenerant obtained by the present embodiment is dissolved using the nitric acid of a concentration of 2mol/L of 10mL, then uses NITRATE BY FLAME ATOMIC
Absorption process measures a concentration of 479.4mg/L of silver ion in the liquid for dissolving argentiferous regenerant, i.e. the rate of recovery (contains for 88.60%
The quality of silver element divided by the quality of adsorbent silver element in silver recovery object) be calculate by the following formula in argentiferous regenerant
Silver-colored simple substance quality be 3.4mg, then the content of silver-colored simple substance is 68% in argentiferous regenerant.
Wherein, mArgentiferous regenerantFor the quality of argentiferous regenerant；
mSilver in argentiferous regenerantFor the quality of the silver element in argentiferous regenerant；
MW (sulphur)For the molal weight of element sulphur；
MW (silver sulfide)For the relative molecular mass of silver sulfide.
Embodiment 2
(1) use the poly- 3- allyls rhodanines of 20mg in 20mL concentration of silver ions 300mg/L conical flasks, concussion absorption is flat
After weighing apparatus, the front and back solution variation of absorption is measured using atomic absorption method, adsorbance is calculated, calculates adsorbent Adsorption For Ag
5.864mg；
(2) step (1) gained is adsorbed to the quality of poly- 3- allyls rhodanine and the volume ratio of methanol after silver ion is
2mg:After the ratio of 3mL is mixed in conical flask, ultrasonic disperse 3min under conditions of frequency is 28kHz；
(3) mixture that the step (2) ultrasonic disperse obtains is placed in 60 DEG C of water-bath, isothermal reaction 15min
Afterwards, it is down to room temperature, is filtered, is obtained silver-containing solid, while being attached with the substance of metallic luster in bottle wall, collect, with argentiferous
Solid mixes, and obtains 5.58mg argentiferous regenerants.
It by XRD analysis (result is similar to Fig. 1), can obtain, the group of the argentiferous regenerant becomes silver sulfide and silver-colored simple substance.
Argentiferous regenerant obtained by the present embodiment is dissolved using the nitric acid of a concentration of 2mol/L of 10mL, then uses NITRATE BY FLAME ATOMIC
Absorption process measures a concentration of 523.5mg/L of silver ion in the liquid for dissolving argentiferous regenerant, i.e. the rate of recovery is 89.26%,
By the formula listed by embodiment 1 calculate silver-colored simple substance quality in argentiferous regenerant is 2.902mg, then it is silver-colored in argentiferous regenerant
The content of simple substance is 52%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of method recycling silver from silver ion adsorbant, includes the following steps：
The adsorbent for being adsorbed with silver ion is mixed with alcohols solvent, after ultrasonic disperse, carries out heat-treating at 45~75 DEG C anti-
It answers, obtains argentiferous regenerant.
2. according to the method described in claim 1, it is characterized in that, the adsorbent is Rhodanine derivates polymer.
3. according to the method described in claim 1, it is characterized in that, the alcohols solvent is methanol.
4. method according to claim 1 or 3, which is characterized in that the quality and alcohol of the adsorbent of the absorption silver ion
The ratio between volume of class solvent is 1mg:1~3mL.
5. described super according to the method described in claim 1, it is characterized in that, the power of the ultrasonic disperse is 20~28kHz
The time of sound dispersion is 2~5min.
6. according to the method described in claim 1, it is characterized in that, the temperature of the thermal reduction reaction is 55~65 DEG C.
7. according to the method described in claim 1, it is characterized in that, the time of the thermal reduction reaction is 10~30min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810661954.5A CN108754152A (en) | 2018-06-25 | 2018-06-25 | A method of recycling silver from silver ion adsorbant |
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| CN201810661954.5A CN108754152A (en) | 2018-06-25 | 2018-06-25 | A method of recycling silver from silver ion adsorbant |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113046569A (en) * | 2021-03-03 | 2021-06-29 | 南昌航空大学 | Method for selectively recovering gold from waste circuit board |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101089206A (en) * | 2007-07-09 | 2007-12-19 | 同济大学 | Methoxy-pheyl-sulfamic acid modified aniline copolymer used as silver ion absorbent |
| CN103305700A (en) * | 2013-06-27 | 2013-09-18 | 江苏省环境科学研究院 | Method for recovering silver from silver-containing wastewater |
-
2018
- 2018-06-25 CN CN201810661954.5A patent/CN108754152A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101089206A (en) * | 2007-07-09 | 2007-12-19 | 同济大学 | Methoxy-pheyl-sulfamic acid modified aniline copolymer used as silver ion absorbent |
| CN103305700A (en) * | 2013-06-27 | 2013-09-18 | 江苏省环境科学研究院 | Method for recovering silver from silver-containing wastewater |
Non-Patent Citations (1)
| Title |
|---|
| 殷晓翠: "银离子印迹聚合物和3-烯丙基罗丹宁聚合物选择性去除和回收银的性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113046569A (en) * | 2021-03-03 | 2021-06-29 | 南昌航空大学 | Method for selectively recovering gold from waste circuit board |
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