CN107308918A - A kind of preparation method of rich nitride polyporous material and its in retrieving circuit board noble metal application - Google Patents
A kind of preparation method of rich nitride polyporous material and its in retrieving circuit board noble metal application Download PDFInfo
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- 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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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
- C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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Abstract
The application of noble metal the present invention relates to a kind of preparation method of rich nitride polyporous material and its in retrieving circuit board, using ethylene glycol as solvent, adds melamine and 1,4-benzoquinone, heats polycondensation, is eventually adding dimethylbenzene dehydration, obtains porous material MOPs 1.The present invention provides a kind of efficient precious metal adsorption material MOPs 1; using thiocarbamide leachate as useless circuit board treatment fluid; study the function of porous material; can noble metal in efficient absorption thiourea solution, reuse thiourea solution, so as to reach the recycling of electron wastes; reclaim the noble metal in electron wastes; and regenerated plastics, environmental protection, produce economic and social benefit.
Description
Technical field
The present invention relates to novel porous materials field, and in particular to a kind of preparation method of rich nitride polyporous material and its return
Receive the application of noble metal in circuit board.
Background technology
2016, the whole world produced up to 50,000,000 tons of waste electric appliance.Reported according to United Nations Environment Programme, China is
Two big electronic wastes produce state, and annual electronic waste is only second to 3,000,000 tons of the U.S. more than 2,300,000 tons.The whole world is annual about
3.5 hundred million tons of electronic wastes flow into China by all means.If these electronic wastes are not only caused without processing to environment
Serious influence, and will also result in the serious wasting of resources.According to statistics, average 1 ton of common electron wastes contain 490kg
Metal, 4kg electric wires, 12kg circuit boards etc..Such as without recycling, it will cause the huge waste of resource.Therefore, with electricity
Influence of the sub- discarded object to ecological environment is increasingly shown especially, and electron wastes itself huge economic value, electron wastes
Recycling reclaim and turn into global problem.
Recycling relative to plastics or other components is recycled, and metals resources are recycled to be had in technology and economic aspect
Obvious advantage.Noble metal is used for electronic product due to its excellent electric conductivity and corrosion resistance, accounts for electronic waste price
The overwhelming majority of value, is the primary economic value of recycling of WEEE.Use the electronics such as effective ways recycling computer, mobile phone
Discarded object can not only alleviate environmental pressure, and can reclaim the noble metals such as Ag, Au, Cu, alleviate world resource increasingly depleted
Pressure.
The present Research that noble metal is reclaimed in electron wastes:Since 1980s, western countries are with secondary resource
The noble metal cumulative year after year of form supply, just up to 1089 tons of the gold supplied in secondary resource form for only 1998, about then
The 43% of mineral products gold.As can be seen here, the recovery of noble metal has progressively caused the attention of people.The technology of noble metal is reclaimed at present
Mainly have:Pyrometallurgy technology, hydrometallurgical technology, biological metallurgy technology.
Pyrometallurgy technology.Pyrometallurgy technology generally comprises roasting, electric arc furnaces or blast furnace smelting, high temperature gas phase reaction
Deng.Electron wastes are subjected to melting at high temperature, make it is nonmetallic separated with metal, concentration of precious metal in metal phase or sulfonium from
And separated with other metals, then noble metal is obtained by electrorefining or pyro-refining.
The technology of pyrometallurgy processing electron wastes also has some defects mainly to have:1. electron wastes contain carbon fluorine chlorine
Compound, bromine flame retardant and organic matter, easily generate the toxic gases such as bioxin under oxidative conditions, it is therefore necessary to have strict efficient
Waste gas treatment equipment and technology, otherwise can cause serious secondary pollution;2. noble metal and copper can be realized with higher recovery
Reclaim, but other metals such as aluminium, iron, tin are then oxidized and enter clinker, so as to be difficult to reclaim;3. the pottery in electron wastes
Porcelain, glass fibre etc. also enter clinker, and the amount of slag of melting has just been significantly greatly increased in this, while also increasing noble metal and other gold
The entrainment loss of category.
Hydrometallurgical technology.For pyrometallurgy technology reclaims electron wastes, hydrometallurgical technology will be more
Complexity, technique is also more diversified.Hydrometallurgical technology generally comprises two steps:Soaked with acid or alkaline equal solvent
Go out, followed by the separation and removal of impurities of leachate.In addition, in the industrial production of hydrometallurgic recovery electron wastes, typically having machinery
It is broken to wait pretreatment.In the noble metal during electron wastes are reclaimed using hydrometallurgical processes, what leaching process was generally used
Solvent mainly includes cyanide, halide, thiocarbamide, thiosulfate etc., is then extracted again by a variety of methods from leachate
Noble metal therein.Extracting method common at present has:Solvent extraction, ion exchange, SPE-absorption method etc..
Solvent extraction is because of its good separating effect, and production capacity is big, is easy to quick continuous operation, during amount of storage it is small,
More safely, it is easily achieved the advantages of automatically controlling and is more applied, but extraction will expect that development is then main faster
Dependent on efficiently, be easy to get, cost is low, loss few extractant is succeeded in developing and reasonable employment.
Ion-exchange is simple because of its synthetic method, and performance is stable, and exchange capacity is big, the advantages of reusable and by compared with
Apply more.But the separation selectivity of the ion similar with Chemical Physics performance to like charges ion is not good, high adsorption capacity
Resin leaching regeneration is difficult.Therefore, need to further develop and modified resin, optimization, improve separation and elution technique, with promote from
Son exchanges the larger development of separating-purifying noble metal technology.
Compared with traditional liquid-liquid technique, solid phase extraction has the following advantages:(1) operating procedure is simple, point
Analyse speed fast, shorten pretreatment time;(2) organic solvent consumption is few, reduces experimental cost, while reducing to environment
Pollution.Solid phase extraction is used as a kind of new Sample Pretreatment Technique, it has also become the most commonly used method for separating and concentrating, because
This, was developed quickly in recent years, and was widely used in many fields such as environment, medicine, food, life, especially in absorption weight
There is relatively broad Research Significance in metal, precious metal ion field.
Biological metallurgy method.Biotechnology, which has been employed successfully in from ore, extracts noble metal and copper.With traditional metallurgical work
Skill is compared, and biological adsorption process has many advantages, and such as technique is simple, expense is low, easy to operate, chemical and biosolids by-product
Thing is few, the advantages of wastewater toxicity is small.Mainly leaching time is long, the raw material DeGrain high to tenor.
Studies in China achievement.The method of molten gold and silver is soaked from ore by the former Russian scholar in nineteen forty-one with acid thiourea solution
Propose.The theory and technique to thiourea gold extraction have carried out extensive research in the world.After nineteen sixty, some metallargists were once
Many theoretical and application research has been carried out to it, lab scale factory is established.In the 1980s, Gold Leaching In Thiourea Solutions just cause individually
The attention of developed country.Over nearly 30 years, the country such as the former Soviet Union, South Africa has done substantial amounts of experimental study to Leaching of Gold by Thiourea.China
Many beneficial explorations have also been carried out in terms of Leaching of Gold by Thiourea experimental study in recent years, larger progress is obtained.In small-sized examination
On the basis of testing, the commerical test of daily 2 tons of scales has successively been carried out on Yu' erya, Zhangjiakou Gold Mine mountain;Imperial water gold mine processing is every
Once put into production in the thiourea gold extraction workshop of its 10 tons of scales.
Last decade, the country is that complexing agent, ferric iron are that catalyst, hydrogen peroxide are that (or thiocarbamide is oxidant using thiocarbamide
Complexing agent, air are oxidant) acid, alkaline thiourea leaching gold is studied.The researcher of Donghua University uses sulphur cyanogen
Hydrochlorate is that complexing agent, manganese dioxide are that oxidant also obtains very good effect, and gold leaching rate is up to 96%~99%.
However, how to apply mechanically the problem that treatment fluid is waste electric appliance handling process.If place can be adsorbed by inventing a kind of material
Noble metal in liquid is managed, treatment fluid is reusable, will be greatly cost-effective, discharge of wastewater is reduced, economical and environmentally friendly benefit is produced.
The present invention provides a kind of efficient precious metal adsorption material, using thiocarbamide leachate as useless circuit board treatment fluid, research porous material
Function.
In a word, the porous material of synthesizing efficient, adsorbs precious metal ion, reuses old metal treatment fluid, recycling electricity
The noble metal and plastics of sub- discarded object, environmental protection produce economic and social benefit.
The content of the invention
The purpose of invention is that method easy to use synthesizes a kind of rich nitride polyporous material MOPs-1, with its adsorb noble metal from
Old metal treatment fluid is used for multiple times in son, simplification of flowsheet, reduces noble metal cost recovery, and realization is turned waste into wealth, reduces pollution
The target of discharge, meets environmental protection and green environment requirement, it is contemplated that the material can be obtained greatly in industrialized production from now on
The application of scale.
For achieving the above object, the technical scheme that provides of the present invention is:
A kind of rich nitride polyporous material, its preparation methods steps are:Using ethylene glycol as solvent, melamine is added and to benzene
Quinone, heats polycondensation, is eventually adding dimethylbenzene dehydration, obtains porous material MOPs-1.
Further, the mol ratio of melamine and 1,4-benzoquinone is 3:(1.9~2.2);Mol ratio is less than 3:1.9 or it is more than
3:When 2.2, yield is substantially reduced, and material physical property is reduced.
Further, the heating polycondensation time is 5~8 hours, and the time is less than 5 hours, and reaction yield reduction, yield is more than 8
Hour, yield is not significantly improved.
Further, heating-up temperature is 160~198 DEG C, and when temperature is less than 160 DEG C, the reaction time is elongated, ethylene glycol boiling point
For 198 DEG C;It is eventually adding dimethylbenzene to be dehydrated 3~5 hours, the time was less than polycondensation in 3 hours not exclusively, low yield, more than 5 hours,
Do not significantly improve.
Further, dehydration temperaturre is 136~140 DEG C of xylene boiling point.
The present invention also announces application of the above-mentioned rich nitride polyporous material in the recovery of circuit board noble metal.
It is preferred that, sorbing material is 12~(20 with noble metal mass ratio:1).
The preferred proportion is obtained by adsorbing column test:Porous material is loaded into adsorption column, by the solution containing noble metal
Add adsorption column, adsorption column absorption precious metal ion.1% diluted hydrochloric acid aqueous solution is washed into adsorption column, noble metal parsing.
When trial scale is less than 12:When 1, absorption is incomplete;Ratio is more than 20:When 1, remaining precious metal concentration is not obvious
Reduction.Judge desorption terminal using atomic absorption spectrum.
Beneficial effect:
The recovery of noble metal can reduce pollution, provide valuable raw material, environmental protection in useless electronic device.Reclaim at present
The technology of noble metal mainly has:Pyrometallurgy technology, hydrometallurgical technology, biological metallurgy technology.Hydrometallurgical technology is due to returning
Receiving metal and plastics has good application prospect, but brings environment dirty using the strong chloroazotic acid of organic solvent or chemical corrosivity
Dye.Last decade, the country is complexing agent using thiocarbamide or rhodanate, obtains huge progress, but how to save thiocarbamide or sulphur cyanogen
Acid ammonium solution, reduces sewage discharge, is that can this method industrialized key issue.If place can be adsorbed by inventing a kind of material
Noble metal in liquid is managed, treatment fluid is reusable, will be greatly cost-effective, discharge of wastewater is reduced, economical and environmentally friendly benefit is produced.
The present invention provides a kind of efficient precious metal adsorption material MOPs-1, using thiocarbamide leachate as useless circuit board treatment fluid,
Study the function of porous material, can noble metal in efficient absorption thiourea solution, reuse thiourea solution, so as to reach electricity
The recycling of sub- discarded object, reclaims the noble metal in electron wastes, and regenerated plastics, and environmental protection produces economic and society
Benefit.
Brief description of the drawings
Fig. 1:Material MOPs-1 syntheti c routes of the present invention and absorption noble metal schematic diagram.
Fig. 2:MOPs-1,1,4-benzoquinone (A) and melamine (B) infrared spectrum.
Embodiment
With reference to specific embodiment, the invention will be further described.
A kind of efficient precious metal adsorption material MOPs-1, using thiocarbamide leachate as useless circuit board treatment fluid, reclaims electronics and gives up
Noble metal in gurry.Metal and nonmetallic ingredient are determined as follows shown in table 1 in useless electronic circuit board:
Table 1
Following reality is shown in the synthesis (embodiment 1~9) of material and the property experiment (embodiment 10~12) of material of the present invention
Apply example:The synthesis of material:
Embodiment 1
In 1L ethylene glycol, 0.20mol melamine and 0.30mol 1,4-benzoquinone are added, is heated, stirring keeps temperature
Degree is stable to react 5 hours at 180 DEG C, adds 300mL dimethylbenzene, loads onto water knockout drum, 136-140 DEG C of refluxing xylene band is leaked water
Point, polycondensation 4 hours stops stirring, and Temperature fall filters to obtain brown precipitate to room temperature, and 100mL ethanol is washed three times, and 80 DEG C are true
Sky is dried, and obtains brown blocks of solid 40.5g yields 86.5%.
Embodiment 2
In 1L ethylene glycol, 0.19mol melamine and 0.30mol 1,4-benzoquinone are added, is heated, stirring keeps temperature
Degree is stable to react 5 hours at 180 DEG C, adds 300mL dimethylbenzene, loads onto water knockout drum, 136-140 DEG C of refluxing xylene band is leaked water
Point, polycondensation 4 hours stops stirring, and Temperature fall filters to obtain brown precipitate to room temperature, and 100mL ethanol is washed three times, and 80 DEG C are true
Sky is dried, and obtains brown solid 35.6g yields 80.1%.
Embodiment 3
In 1L ethylene glycol, 0.22mol melamine and 0.30mol 1,4-benzoquinone are added, is heated, stirring keeps temperature
Degree is stable to react 5 hours at 180 DEG C, adds 300mL dimethylbenzene, loads onto water knockout drum, 136-140 DEG C of refluxing xylene band is leaked water
Point, polycondensation 4 hours stops stirring, and Temperature fall filters to obtain brown precipitate to room temperature, and 100mL ethanol is washed three times, and 80 DEG C are true
Sky is dried, and obtains brown solid 40.2g yields 85.9%.
It was found from embodiment 1-3, when the mol ratio of melamine and 1,4-benzoquinone is 1.9~2.2:When 3, reaction yield compared with
It is high.To be 2 according to the mol ratio of melamine and 1,4-benzoquinone:3, it is expanded on further in embodiment.
Embodiment 4
In 1L ethylene glycol, 0.20mol melamine and 0.30mol 1,4-benzoquinone are added, is heated, stirring keeps temperature
Degree is stable to react 5 hours at 160 DEG C, adds 300mL dimethylbenzene, loads onto water knockout drum, 136-140 DEG C of refluxing xylene band is leaked water
Point, polycondensation 4 hours stops stirring, and Temperature fall filters to obtain brown precipitate to room temperature, and 100mL ethanol is washed three times, and 80 DEG C are true
Sky is dried, and obtains brown solid 40.3g yields 86.1%.
Embodiment 5
In 1L ethylene glycol, 0.20mol melamine and 0.30mol 1,4-benzoquinone are added, is heated, stirring keeps temperature
Degree is stable to react 5 hours at 198 DEG C, adds 300mL dimethylbenzene, loads onto water knockout drum, 136-140 DEG C of refluxing xylene band is leaked water
Point, polycondensation 4 hours stops stirring, and Temperature fall filters to obtain brown precipitate to room temperature, and 100mL ethanol is washed three times, and 80 DEG C are true
Sky is dried, and obtains brown solid 40.5g yields 86.5%.
It was found from embodiment 1,4,5, when reaction temperature is at 160~198 DEG C, reaction yield is stable.Will according to 180 DEG C
It is expanded on further in embodiment.
Embodiment 6
In 1L ethylene glycol, 0.20mol melamine and 0.30mol 1,4-benzoquinone are added, is heated, stirring keeps temperature
Degree is stable to react 8 hours at 180 DEG C, adds 300mL dimethylbenzene, loads onto water knockout drum, 136-140 DEG C of refluxing xylene band is leaked water
Point, polycondensation 4 hours stops stirring, and Temperature fall filters to obtain brown precipitate to room temperature, and 100mL ethanol is washed three times, and 80 DEG C are true
Sky is dried, and obtains brown solid 40.3g yields 86.1%.
Embodiment 7
In 1L ethylene glycol, 0.20mol melamine and 0.30mol 1,4-benzoquinone are added, is heated, stirring keeps temperature
Degree is stable to react 6.5 hours at 180 DEG C, adds 300mL dimethylbenzene, loads onto water knockout drum, 136-140 DEG C of refluxing xylene band is leaked water
Point, polycondensation 4 hours stops stirring, and Temperature fall filters to obtain brown precipitate to room temperature, and 100mL ethanol is washed three times, and 80 DEG C are true
Sky is dried, and obtains brown solid 40.5g yields 86.5%.
It was found from embodiment 1,6,7, when reacted between at 5-8 hours, reaction yield is stable.It will implement according to 5 hours
It is expanded on further in example.
Embodiment 8
In 1L ethylene glycol, 0.20mol melamine and 0.30mol 1,4-benzoquinone are added, is heated, stirring keeps temperature
Degree is stable to react 5 hours at 180 DEG C, adds 300mL dimethylbenzene, loads onto water knockout drum, 136-140 DEG C of refluxing xylene band is leaked water
Point, polycondensation 3 hours stops stirring, and Temperature fall filters to obtain brown precipitate to room temperature, and 100mL ethanol is washed three times, and 80 DEG C are true
Sky is dried, and obtains brown solid 40.2g yields 85.9%.
Embodiment 9
In 1L ethylene glycol, 0.20mol melamine and 0.30mol 1,4-benzoquinone are added, is heated, stirring keeps temperature
Degree is stable to react 5 hours at 180 DEG C, adds 300mL dimethylbenzene, loads onto water knockout drum, 136-140 DEG C of refluxing xylene band is leaked water
Point, polycondensation 5 hours stops stirring, and Temperature fall filters to obtain brown precipitate to room temperature, and 100mL ethanol is washed three times, and 80 DEG C are true
Sky is dried, and obtains brown solid 40.1g yields 85.7%.
The property experiment of material:
Embodiment 10
Above-mentioned porous material 2g is taken, addition contains gold ion 0.051wt%, thiocarbamide 20wt%, pH=2.5 water containing 3L
In solution, 30min is stirred at room temperature, filters, Atomic Absorption Spectrometry residue gold ion concentration is 16ppm, adsorption rate 96.8%.
The material of ADSORPTION OF GOLD is loaded into adsorption column, eluted using 1% hydrochloric acid solution, Atomic Absorption Spectrometry outflow salt
Stop elution when gold ion concentration is less than 3ppm in acid solution, spend hydrochloric acid 25mL.
Embodiment 11
Above-mentioned porous material 2g is taken, addition contains silver ion 0.89wt%, thiocarbamide 20wt% containing 300mL, pH=2.5's
In the aqueous solution, 30min is stirred at room temperature, filters, Atomic Absorption Spectrometry residue concentration of silver ions is 156ppm, adsorption rate
98.2%.
The material of Adsorption For Ag is loaded into adsorption column, eluted using 1% salpeter solution, Atomic Absorption Spectrometry outflow nitre
Stop elution when concentration of silver ions is less than 3ppm in acid solution, spend nitric acid 20mL.
Embodiment 12
Above-mentioned porous material 2g is taken, addition contains silver ion 0.89wt%, gold ion 215ppm, thiocarbamide containing 300mL
In 20wt%, the pH=2.5 aqueous solution, 30min is stirred at room temperature, filters, Atomic Absorption Spectrometry residue gold, silver ion concentration
Respectively 10ppm, 152ppm, adsorption rate is respectively 95.3%, 98.3%.
The material that noble metal will be adsorbed loads adsorption column, is first eluted with 20mL 1% salpeter solution, then with 10mL 1%
Hydrochloric acid solution elution, Atomic Absorption Spectrometry outflow precious metal ion concentration stops elution when being less than 3ppm.
It is described above, only it is presently preferred embodiments of the present invention, any formal limitation not is made to the present invention, it is any ripe
Professional and technical personnel is known, it is without departing from the scope of the present invention, real to more than according to the technical spirit of the present invention
Apply any simple modification, equivalent substitution that example made and improve etc., still fall within technical solution of the present invention protection domain it
It is interior.
Claims (8)
1. a kind of rich nitride polyporous material, it is characterised in that:Its preparation methods steps are:Using ethylene glycol as solvent, melamine is added
Amine and 1,4-benzoquinone, heat polycondensation, are eventually adding dimethylbenzene dehydration, obtain porous material MOPs-1.
2. rich nitride polyporous material according to claim 1, it is characterised in that:The mol ratio of the melamine and 1,4-benzoquinone
For 3:(1.9~2.2).
3. rich nitride polyporous material according to claim 1, it is characterised in that:It is 5~8 hours to heat the polycondensation time.
4. rich nitride polyporous material according to claim 1, it is characterised in that:Heating-up temperature is 160~198 DEG C.
5. rich nitride polyporous material according to claim 1, it is characterised in that:Dimethylbenzene is eventually adding to be dehydrated 3~5 hours.
6. rich nitride polyporous material according to claim 1, it is characterised in that:Dehydration temperaturre is xylene boiling point 136~140
℃。
7. application of the rich nitride polyporous material in the recovery of circuit board noble metal described in claim 1.
8. application of the rich nitride polyporous material according to claim 7 in the recovery of circuit board noble metal, it is characterised in that:Inhale
Enclosure material is 12~(20 with noble metal mass ratio:1).
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Publication number | Priority date | Publication date | Assignee | Title |
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CN108421540A (en) * | 2018-05-07 | 2018-08-21 | 南京信息工程大学 | A kind of melamine-based organic porous material and preparation method thereof |
CN108467492A (en) * | 2018-05-07 | 2018-08-31 | 南京信息工程大学 | A kind of fluorine-containing organic metal porous material and preparation method thereof |
CN108371946A (en) * | 2018-05-08 | 2018-08-07 | 南京信息工程大学 | A kind of application by bisphenol-A and the preparation method and its absorbing heavy metal ions in water of the rich nitride polyporous material of melamine polycondensation |
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