CN103157446A - Adsorbent for separating palladium from alkali metals and alkaline-earth metals and its preparation method and use - Google Patents
Adsorbent for separating palladium from alkali metals and alkaline-earth metals and its preparation method and use Download PDFInfo
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- CN103157446A CN103157446A CN2013100763130A CN201310076313A CN103157446A CN 103157446 A CN103157446 A CN 103157446A CN 2013100763130 A CN2013100763130 A CN 2013100763130A CN 201310076313 A CN201310076313 A CN 201310076313A CN 103157446 A CN103157446 A CN 103157446A
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Abstract
The invention discloses an adsorbent for separating palladium from alkali metals and alkaline-earth metals. 4-[3-(3-benzo-15-crown-5)methyl-4-hydroxy-phenyl]methylethyl-phenolic resin is supported by carriers to form the adsorbent. The 4-[3-(3-benzo-15-crown-5)methyl-4-hydroxy-phenyl]methylethyl-phenolic resin has a structural general formula (I), wherein in the structural general formula (I), n is an integer of 7-15. The carriers are porous silica gel or large-hole SiO2 coated by a polymer. The invention also discloses a preparation method and a use of the adsorbent for separating palladium from alkali metals and alkaline-earth metals. The preparation method has simple processes. The adsorbent obtained by the preparation method has good selectivity in palladium separation. The palladium separation process adopting the adsorbent is simple. The adsorbent has high separation efficiency and can be industrially produced easily.
Description
Technical field
The present invention relates to the separation technology field of element palladium, be specifically related to a kind of from alkali and alkaline earth metal ions the adsorbent and its preparation method and application of separating element palladium.
Background technology
The element palladium is argenteous transition metal, and quality is softer, and good ductility and plasticity are arranged, energy forging, calendering and wire drawing.
The chemical property torpescence of element palladium, all stable in air and wet environment under normal temperature, be heated to 800 ℃, palladium surface formation palladium monoxide film.The erosion of element palladium energy hydrofluoric acid resistant, phosphoric acid, perchloric acid, hydrochloric acid and sulfuric acid vapor, but be soluble in chloroazotic acid and the hot concentrated sulfuric acid and red fuming nitric acid (RFNA), the NaOH of melting, sodium carbonate, sodium peroxide all have corrosiveness to the element palladium.
The reguline metal palladium can absorb a large amount of hydrogen, under normal temperature, 1 volume palladium sponge can absorb 900 volume hydrogen, 1 volume colloid palladium can absorb 1200 volume hydrogen, and after being heated to 40～50 ℃, the hydrogen of absorption is that major part is disengaged, and is widely used as gas reaction, particularly hydrogenation or dehydrogenation also can be made resistive conductor, clock and watch with alloy etc.
Granted publication number be CN100497676C disclosure of the invention a kind of method of SPE extraction and separate palladium, be used for extracting and separate palladium from the concentration of precious metal thing that platinum group metal concentrate or secondary resource obtain.Adopt a kind of bonding the polymer microsphere polymer of palladium extractant be fixing phase, make mobile phase with the hydrochloric acid solution that contains high and low metal, realize that palladium separates with metallic elements such as platinum, rhodium, iridium and copper base metal, iron, nickel, zinc, and make leacheate with watery hydrochloric acid, with a kind of can be eluent with the reagent solution of palladium complexing, and solid-phase extraction column can be regenerated with dilute hydrochloric acid solution.
Patent publication No. be CN102586607A disclosure of the invention a kind of method of extracting platinum, rhodium, palladium from inefficacy platinum alloy net, utilize the mixed solution of hydrochloric acid and nitric acid to dissolve, remove nitro, turn sodium type, suction filtration, get platinum rhodium palladium complex solution, adopt chloride precipitation method Separation of Pt, use natrium nitrosum complexing seperation palladium, rhodium, with six nitroso rhodium acid ammonium method purification rhodiums, with the inferior palladium method of dichloro two amminos purification palladium, through adding hydrazine hydrate reduction to get spongy platinum, palladium sponge and rhodium powder, through vacuum drying, roasting, again purify, obtain noble metal platinum rhodium palladium.
The element palladium is the indispensable critical materials of high-tech area and auto manufacturing such as space flight, aviation, navigation, weapons and nuclear energy; Palladium bichloride can be used for electroplating; Palladium bichloride and relevant chloride thereof are that the circulation refining utilizes thermal decomposition method to make the raw material of pure palladium sponge; Palladium monoxide (PdO) and palladium dydroxide [Pd (OH)
2] can do the source of palladium catalyst.
Due to the extensive use of element palladium in every field, need to provide effective method that element palladium and other element are carried out separating-purifying, simultaneously, in order to extract the element palladium from the trade waste that contains the element palladium, carry out the utilization of element recovery of palladium, also needing to provide simple method to carry out the separation of element palladium.
The high activity liquid waste that the spentnuclear fuel post processing produces (HLLW) is a kind of peracidity, high radioactivity and highly toxic mixed solution, and in the separation process of heating element Cs and heating element Sr, gained alkali and alkaline earth metal ions solution generally may contain NaNO
3, KNO
3, RbNO
3, CsNO
3, Sr (NO
3)
2, Ba (NO
3)
2And a certain amount of palladium, also do not have a kind of effective method the palladium in this solution effectively can be separated in prior art.
Summary of the invention
The invention provides a kind of adsorbent and application thereof of separating element palladium from alkali and alkaline earth metal ions, the preparation method of adsorbent is simple, and is selectively good during the adsorbent separating element palladium that obtains, simple to operate during using adsorbent separating element palladium, separative efficiency is high, is easy to suitability for industrialized production.
A kind of from alkali and alkaline earth metal ions the adsorbent of separating element palladium, by 4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] Methylethyl-phenolic resin loads on carrier and makes, described 4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] Methylethyl-phenolic resin has general structure (I)
N is 7～15 integer.
As preferably, described carrier is the macro-pore SiO of Bio-sil or coating polymer
2
Described Bio-sil can adopt the commercially available prod, for example can be the Bio-sil of the various models that are applied to packed column, the not strict restriction such as its aperture.The macro-pore SiO of described coating polymer
2Be SiO
2-styrene-divinylbenzene polymer (SiO
2-P), be a class novel inorganic/organic carrier, in US Patent No. 6843921, SiO is disclosed
2-styrene-divinylbenzene polymer, SiO
2-P is a kind of organic high polymer complex carrier that contains the porous silica carrier granular, and its preparation method is:
(1) with the SiO of macropore
2Be washed till neutrality with red fuming nitric acid (RFNA) washing, suction filtration, deionized water, repeat drying more than 10 times.
(2) vacuum and having under the argon shield condition is solvent with 1,2,3-trichloropropane and m-dimethylbenzene, to macro-pore SiO
2In add the m/p-formyl styrene of 48.7g, 8.9g the m/p-divinylbenzene, 72.2g dioctyl faces phthalic acid ester, 54.0g benzoin methyl acid sodium, 0.56g α, α-even bis-isobutyronitrile and 0.57g1,1 '-even dicyclohexyl amine-1-nitrile, progressively be heated to 90 ° of C by room temperature, and kept 13 hours, afterwards, progressively be cooled to room temperature.
(3) use respectively acetone and methanol wash, the above-mentioned product of suction filtration, repeat drying more than 10 times.
As preferably, the quality of described carrier is 4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] 0.5～40 times of the quality of Methylethyl-phenolic resin.Further preferred, the quality of described carrier is 4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] 1～20 times of the quality of Methylethyl-phenolic resin.
As preferably, in general structure (I), n is 8～12 integer.
The value of n will affect 4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] number of crown ether in Methylethyl-phenolic resin, utilize adsorbent of the present invention from alkali and alkaline earth metal ions during the separating element palladium, utilize the specific adsorption of crown ether and element palladium to carry out, if the quantity of crown ether is very few, the efficient of separating element palladium will reduce greatly, if the quantity of crown ether is too much, the corresponding shielding action that occurs between crown ether, separative efficiency also can reduce.
The present invention also provides the preparation method of described adsorbent, comprise: add 2 in trichloroacetic acid, 2-two (4-hydroxyphenyl)propanes and phendioxin 5-hat 5, the stirring and dissolving wiring solution-forming, then paraformaldehyde is added and react in this solution and generate sediment, isolate this sediment, dissolve in after drying in carrene, add carrier, after stirring, drying obtains described adsorbent again.
Trichloroacetic acid and 2,2-, two (4-hydroxyphenyl)propanes, the mass ratio of phendioxin 5-hat 5 and paraformaldehyde is: 100:7～15:7～15:3～8.
After dried sediment dissolves in carrene, initial stage carrene content is more, the load of vavuum pump when alleviating the later stage vacuum drying, can first about 45 ℃ stirrings under normal pressure, make carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The present invention also provides the method for described adsorbent separating element palladium from alkali and alkaline earth metal ions, comprise the steps: that the aqueous solution that will contain alkali nitrates, alkaline earth nitrate and palladium nitrate contacts with described adsorbent, make the element palladium be adsorbed agent absorption and separate.
Described alkali nitrates comprises NaNO
3, KNO
3, RbNO
3, CsNO
3, described alkaline earth nitrate comprises Sr (NO
3)
2, Ba (NO
3)
2, in the aqueous solution, alkali nitrates, alkaline earth nitrate and palladium nitrate can ionize, and therefore, in esse in the aqueous solution is alkali metal ion, alkaline-earth metal ions, palladium ion and nitrate ion.
With can have trace impurity in the aqueous solution that adsorbent contacts, do not affect the separating effect of element palladium, the solute in the aqueous solution can only be comprised of alkali metal ion, alkaline-earth metal ions, palladium ion and nitrate ion.
Na in the aqueous solution
+, K
+, Rb
+, Cs
+, Sr
+, Ba
2+And Pb
2+Concentration range be 1 * 10
-3～5.0 * 10
-3Mol/L.
Can regulate the concentration of nitric acid in the aqueous solution by adding nitric acid, reach the optimum efficiency of adsorbent adsorbing separation element palladium, preferably, in the described aqueous solution, concentration of nitric acid is 0.4～6mol/L.
Also will affect the separating effect of element palladium the time of contact of adsorbent and the aqueous solution, time of contact is too short, the element palladium not yet is adsorbed agent and adsorbs fully, time of contact is long, reduce separative efficiency, preferably, be 100～1000min the time of contact of the aqueous solution and described adsorbent, further preferred, be 350～750min the time of contact of the aqueous solution and described adsorbent.
The inventive method at room temperature operates and gets final product.
Adsorbent of the present invention does not need to use the diluent with property to dilute or dissolve in adsorption process, do not need to add other organic compounds yet, the complexity of minishing method, be easy in industrial popularization, and environmentally friendly, utilize adsorbent selectively good during the separating element palladium from alkali and alkaline earth metal ions, separating rate is fast.
Description of drawings
Fig. 1 is the graph of a relation that utilizes the distribution coefficient of adsorbent separating element palladium from alkali and alkaline earth metal ions that the present invention prepares to change with concentration of nitric acid;
Fig. 2 is the graph of a relation that utilizes the distribution coefficient of adsorbent separating element palladium from alkali and alkaline earth metal ions that the present invention prepares to change with time of contact.
The specific embodiment
4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] preparation of Methylethyl-phenolic resin
add 3.42g(15mmol in the 30g trichloroacetic acid) 2, 2-two (4-hydroxyphenyl)propanes and 3.49g(13mmol) phendioxin 5-hat 5, 90 ℃ of lower stirring and dissolving, wiring solution-forming, then in 4.5 hours, 1.79g paraformaldehyde (containing 60mmol formaldehyde) is added in this solution, add and reaction temperature is risen to 140 ℃ after completing, react and began to occur precipitation in 4 hours in the afterreaction system, quality to be precipitated no longer increases, reaction system is cooled to room temperature, add 150mL methyl alcohol in the reactant liquor of gained, make the precipitation atomizing, through crushing, filtration obtains solid state powder, continue with this solid state powder of 50mL methanol wash, the repeated washing several times to cleaning fluid (being methyl alcohol) without change color, finally obtain brown powder, be 4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] Methylethyl-phenolic resin (be called for short: poly-two 15 are preced with 5 resins), it is 70% that drying under reduced pressure obtains the 4.88g(yield).
N in the present embodiment is 8, can be as required by changing the ratio of each raw material, the value of regulating n.
The 4-[3-that uses in following examples (3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] Methylethyl-phenolic resin all prepares by the method.
The preparation of embodiment 2 adsorbents
4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl that 100 grams is had structural formula (I)] Methylethyl-phenolic resin (n is 7) is dissolved in the 1000mL carrene, mixes; Add 150 gram Bio-sils, stirring makes carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The preparation of embodiment 3 adsorbents
4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl that 100 grams is had structural formula (I)] Methylethyl-phenolic resin (n is 9) is dissolved in the 1000mL carrene, mixes; Add 200 gram Bio-sils, stirring makes carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The preparation of embodiment 4 adsorbents
4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl that 100 grams is had structural formula (I)] Methylethyl-phenolic resin (n is 11) is dissolved in the 1000mL carrene, mixes; Add 250 gram Bio-sils, stirring makes carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The preparation of embodiment 5 adsorbents
4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl that 100 grams is had structural formula (I)] Methylethyl-phenolic resin (n is 13) is dissolved in the 1000mL carrene, mixes; The macro-pore SiO that adds 300 gram coating polymer
2(SiO
2-P) stir and make carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The preparation of embodiment 6 adsorbents
4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl that 100 grams is had structural formula (I)] Methylethyl-phenolic resin (n is 15) is dissolved in the 1000mL carrene, mixes; The macro-pore SiO that adds 350 gram coating polymer
2(SiO
2-P) stir and make carrene volatilization most of to material to nearly dried state, and then nearly the material of dried state at 45 ℃ of lower vacuum drying 24h.
The separation of element palladium in embodiment 7 alkali and alkaline earth metal ions
With NaNO
3, KNO
3, RbNO
3, CsNO
3, Sr (NO
3)
2, Ba (NO
3)
2And Pd (NO
3)
2The water-soluble aqueous solution that is mixed with, NaNO in this aqueous solution
3, KNO
3, RbNO
3, CsNO
3, Sr (NO
3)
2, Ba (NO
3)
2And Pd (NO
3)
2Concentration be respectively 5.0 * 10
-3Mol/L.
Add nitric acid to regulate HNO in the aqueous solution
3Concentration is 5.0mol/L, and mixings that then aqueous solution that obtains and the adsorbent of embodiment 3 preparations contacted in container for the raising adsorption effect can be aided with concussion, is adsorbed on adsorbent the element palladium.
Adsorption separation process is that solid-liquid separates, and is set up and states solution in the 100mL conical flask, and the adsorbent with the present invention's preparation adds in the 100mL conical flask simultaneously, adsorbs concussion on TAITEC MM-10 type concussion instrument, and concussion speed is 120rpm, ambient operation.Because adsorbent has good selectively to Pd, so can and separate with other metallic elements Pd absorption, has good separating effect.
Adsorbent of the present invention has good selective to the element palladium, can and separate with other metallic elements the absorption of element palladium, has good separating effect.The separating effect spectrogram is seen Fig. 2, and can realize the fully separation of element palladium when being 750min time of contact.
Embodiment 8～14
Utilize the method for embodiment 7, only change the concentration of nitric acid in the aqueous solution, when the concentration of nitric acid is respectively 0.5mol/L, 1mol/L, 2mol/L, 3mol/L, 4mol/L, 5mol/L, 6mol/L, the gained separating resulting as shown in Figure 1, when concentration of nitric acid was 5mol/L, the effect of separating element palladium was best.
Claims (9)
1. the adsorbent of a separating element palladium from alkali and alkaline earth metal ions, it is characterized in that, by 4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] Methylethyl-phenolic resin loads on carrier and makes, described 4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] Methylethyl-phenolic resin has general structure (I)
N is 7～15 integer.
As claimed in claim 1 from alkali and alkaline earth metal ions the adsorbent of separating element palladium, it is characterized in that, described carrier is the macro-pore SiO of Bio-sil or coating polymer
2
As claimed in claim 2 from alkali and alkaline earth metal ions the adsorbent of separating element palladium, it is characterized in that, the quality of described carrier is 4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] 0.5～40 times of the quality of Methylethyl-phenolic resin.
As claimed in claim 3 from alkali and alkaline earth metal ions the adsorbent of separating element palladium, it is characterized in that, the quality of described carrier is 4-[3-(3-phendioxin 5-hat-5) methyl-4-hydroxyl-phenyl] 1～20 times of the quality of Methylethyl-phenolic resin.
As arbitrary in claim 1～4 described from alkali and alkaline earth metal ions the adsorbent of separating element palladium, it is characterized in that, in general structure (I), n is 8～12 integer.
6. the method for a utilization described adsorbent as arbitrary in claim 1～5 separating element palladium from alkali and alkaline earth metal ions, it is characterized in that, comprise the steps: that the aqueous solution that will contain alkali nitrates, alkaline earth nitrate and palladium nitrate contacts with described adsorbent, make the element palladium be adsorbed agent absorption and separate.
7. method as claimed in claim 6, is characterized in that, in the described aqueous solution, concentration of nitric acid is 0.4～6mol/L.
8. method as claimed in claim 6, is characterized in that, be 100～1000min the time of contact of the described aqueous solution and described adsorbent.
9. the preparation method of the adsorbent of separating element palladium from alkali and alkaline earth metal ions, it is characterized in that, comprise: add 2 in trichloroacetic acid, 2-two (4-hydroxyphenyl)propanes and phendioxin 5-hat 5, then the stirring and dissolving wiring solution-forming adds paraformaldehyde and reacts in this solution and generate sediment, isolate this sediment, dissolve in carrene after drying, then add carrier, after stirring, drying obtains described adsorbent.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104805286A (en) * | 2015-04-22 | 2015-07-29 | 浙江大学 | Polymer-based supramolecular adsorbent, preparation method and application thereof |
| CN106179273A (en) * | 2016-08-10 | 2016-12-07 | 清华大学 | A kind of adsorbent for lithium isotope separation and its preparation method and application |
| CN108531732A (en) * | 2018-01-31 | 2018-09-14 | 福州大学 | A kind of activated carbon supported ruthenium catalyst gives up the recovery method of ruthenium in agent |
| CN108998672A (en) * | 2018-08-02 | 2018-12-14 | 浙江大学 | A kind of method of separate palladium |
| CN109182776A (en) * | 2018-08-02 | 2019-01-11 | 浙江大学 | A method of the separate palladium from acidic aqueous solution |
| CN109179550A (en) * | 2018-08-02 | 2019-01-11 | 浙江大学 | A method of using adsorbent from acidic aqueous solution separate palladium |
| CN113481379A (en) * | 2021-06-18 | 2021-10-08 | 金川集团股份有限公司 | Method for removing impurities by using palladium extracting agent |
| CN115178300A (en) * | 2022-07-13 | 2022-10-14 | 安徽东至广信农化有限公司 | Hydrogenation catalyst regeneration wastewater treatment method |
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| CN104805286A (en) * | 2015-04-22 | 2015-07-29 | 浙江大学 | Polymer-based supramolecular adsorbent, preparation method and application thereof |
| CN104805286B (en) * | 2015-04-22 | 2016-11-30 | 浙江大学 | A kind of polymer-based supermolecule adsorbent and its preparation method and application |
| CN106179273A (en) * | 2016-08-10 | 2016-12-07 | 清华大学 | A kind of adsorbent for lithium isotope separation and its preparation method and application |
| CN108531732A (en) * | 2018-01-31 | 2018-09-14 | 福州大学 | A kind of activated carbon supported ruthenium catalyst gives up the recovery method of ruthenium in agent |
| CN108531732B (en) * | 2018-01-31 | 2019-05-17 | 福州大学 | A kind of activated carbon supported ruthenium catalyst gives up the recovery method of ruthenium in agent |
| CN109179550A (en) * | 2018-08-02 | 2019-01-11 | 浙江大学 | A method of using adsorbent from acidic aqueous solution separate palladium |
| CN109182776A (en) * | 2018-08-02 | 2019-01-11 | 浙江大学 | A method of the separate palladium from acidic aqueous solution |
| CN108998672A (en) * | 2018-08-02 | 2018-12-14 | 浙江大学 | A kind of method of separate palladium |
| CN108998672B (en) * | 2018-08-02 | 2019-09-20 | 浙江大学 | A kind of method of separate palladium |
| CN109182776B (en) * | 2018-08-02 | 2019-10-25 | 浙江大学 | A method of the separate palladium from acidic aqueous solution |
| CN109179550B (en) * | 2018-08-02 | 2019-10-29 | 浙江大学 | A method of using adsorbent from acidic aqueous solution separate palladium |
| CN113481379A (en) * | 2021-06-18 | 2021-10-08 | 金川集团股份有限公司 | Method for removing impurities by using palladium extracting agent |
| CN115178300A (en) * | 2022-07-13 | 2022-10-14 | 安徽东至广信农化有限公司 | Hydrogenation catalyst regeneration wastewater treatment method |
| CN115178300B (en) * | 2022-07-13 | 2024-04-16 | 安徽东至广信农化有限公司 | Hydrogenation catalyst regeneration wastewater treatment method |
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