CN105964228A - P2O4-loaded sodium alginate composite microsphere adsorbent l as well as preparation method and application thereof - Google Patents
P2O4-loaded sodium alginate composite microsphere adsorbent l as well as preparation method and application thereof 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
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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- C22B34/1259—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching treatment or purification of titanium containing solutions or liquors or slurries
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Abstract
The invention relates to a P2O4-loaded sodium alginate composite microsphere adsorbent as well as a preparation method and application thereof, and belongs to the technical field of environmental material preparation. According to the technical scheme adopted by the invention, the preparation method comprises the following steps: taking brown seaweed powder, treating the brown seaweed powder with formaldehyde and a sodium carbonate solution to obtain a mixture, and cooking the mixture at a temperature of 50-60 DEG C until the mixture is pasty; filtering the mixture, and adding a little distilled water into the mixture to obtain a sodium alginate solution; adding a saponified P2O4 solution into the sodium alginate solution to obtain a mixed solution, and stirring the mixed solution for 20-24 hours; and adding the mixed solution of sodium alginate and P2O4 into CaCl2 drop by drop by use of an injector, continuously stirring the solution for 10-12 hours, carrying out filtering and washing, and carrying out drying at a temperature of 50-60 DEG C to obtain the P2O4-loaded sodium alginate composite microsphere adsorbent. The adsorbent prepared by the preparation method is used for adsorbing titanium from a solution containing titanium, and has the advantages of being wide in raw material source, low in cost, energy-saving and environment-friendly, great in titanium adsorption amount, and the like.
Description
Technical field
The invention belongs to preparation and the rare metal extractive technique field of green adsorbent, be specifically related to a kind of load P204The preparation method of the sodium alginate composite microsphere adsorbent of (di-(2-ethylhexyl)phosphoric acid ester) and utilize its separation and concentration titanium.
Background technology
Titanium is silver gray metal, and matter is soft, has ductility and paramagnetism, but conducts electricity and poor thermal conductivity.There is due to it features such as high temperature resistant, corrosion-resistant, high intensity, low-density and good biocompatibility, be " space metal " by good reputation.It is widely used in Aero-Space, defence and military, petrochemical industry, pharmaceutical field and the aspect such as medical apparatus and instruments, sea water desalinating unit.Titanium is extremely wide in distributed in nature, and the abundance in the earth's crust is 0.56%, occupies the tenth, is only second to ferrum in a metal, silver, magnesium occupy the 4th, but owing to occurrence status disperses, and often and other element associations, separation and Extraction is difficult.So the titanium in all kinds of ore deposit of efficient recovery is the problem merited attention.
The method for separating and concentrating of titanium is divided into pyrogenic process and wet method at present.Pyrogenic process has electric furnace smelting process, carbonizatin method, selective chlorination, reduction grinding method, reduced ilmenite method etc..Wet method has the sedimentation method, extraction and ion exchange etc..Wherein extraction is main method for separating and concentrating, uses acidic organophosphorus extractant (such as D2EHPA etc.), neutral organophosphorus extractant (such as TOPO, Cyanex923 etc.), amine extractant (such as N1923 etc.) more.But, all there is the response rate low, and do not meet the objective of energy-saving and emission-reduction in the most traditional method extracting titanium.As can be seen here, the technology seeking more effectively separation and extraction Titanium is problem demanding prompt solution.
Summary of the invention
The problem existed for prior art, the present invention is by extractant P204Being immersed in sodium alginate surface, synthesize that a kind of preparation method is simple, pollution-free, the NEW TYPE OF COMPOSITE microsphere adsorbing agent of low cost, this adsorbent has higher adsorption capacity to titanium, reuses the advantage such as often, has practical application.
Technical scheme is as follows: a kind of load P204Sodium alginate composite microsphere adsorbent, preparation method comprises the steps:
1) take Brown algae powder and join in formalin, soak 4-6h, filter, in filtrate, add Na2CO3Solution, boils at 50-60 DEG C to pasty state, filters, add a small amount of distilled water, obtain sodium alginate soln in filtrate；
2) by the P after saponification204Mix with sodium alginate soln, stir 20-24h, by P204It is added dropwise to CaCl with the mixed solution syringe of sodium alginate2In solution, stirring 10-12h, filter, gained solid washs, and is dried, obtains target product.
Above-mentioned a kind of load P204Sodium alginate composite microsphere adsorbent, described Brown algae powder is: by Thallus Laminariae (Thallus Eckloniae) or Alga Sgrgassi Enerves cleaning, drying, be crushed to 60-80 mesh.
Above-mentioned a kind of load P204Sodium alginate composite microsphere adsorbent, it is preferred that it is the formalin of 1% that every gram of Brown algae powder adds 10-15g concentration expressed in percentage by volume.
Above-mentioned a kind of load P204Sodium alginate composite microsphere adsorbent, it is preferred that it is the Na of 15-20g/L that every gram of Brown algae powder adds 15-20g concentration2CO3Solution.
Above-mentioned a kind of load P204Sodium alginate composite microsphere adsorbent, it is preferred that the P after saponification204It is 1:1-3:1 with the mass ratio of sodium alginate soln.
Above-mentioned a kind of load P204Sodium alginate composite microsphere adsorbent, it is preferred that CaCl2Solution concentration is 0.5-0.7mol/L.
Above-mentioned a kind of load P204Sodium alginate composite microsphere adsorbent, it is preferred that by volume, P204Mixed solution with sodium alginate: CaCl2=1:4-6.
Above-mentioned a kind of load P204Sodium alginate composite microsphere adsorbent, it is preferred that the described P after saponification204Preparation method: take P204Join in separatory funnel with normal heptane, then add NaOH solution, rock 15-20min, bleed off bottom NaOH solution, be neutral with distilled water cyclic washing to effluent.
Load P prepared by the present invention204Sodium alginate composite microsphere adsorbent can from titaniferous feed liquid high efficiency separation enrichment titanium in application.Method is as follows: taking the solution of titaniferous, regulation solution acidity is 0.56-3mol/L, adds above-mentioned load P204Sodium alginate composite microsphere adsorbent, the ratio of adding is 2-18g/L, at 25-35 DEG C concussion reach adsorption equilibrium.Use 2MH2SO4-20%H2O2Mixed solution as eluant.
The invention has the beneficial effects as follows:
1. abundant raw material: the yield China Brown algae accounts for the 80% of world's Brown algae total output, abundance is cheap, has practical application.
2. method is simple: the present invention passes through infusion process by saponification P204Loading on sodium alginate, chemical treatment synthetic method is simple, can from containing aluminum, ferrum mixed liquor separation and concentration titanium.
The most pollution-free: this method reaction terminate rear unharmful substance discharge, the remaining solvent of other steps can Reusability, thus without to environment.
4. low cost: processing cost is greatly lowered, processing cost is the 10-20% of traditional treatment method.
5., in the present invention, under certain acidity, sodium alginate micro ball adsorbent is 58.72mg/g to the maximal absorptive capacity of titanium.
6. the present invention combines extraction ability and the high adsorption capacity of biological material, abundance, the double effects of low cost of extractant, is prepared for load P204Sodium alginate composite microsphere adsorbent, for separation and concentration trace amount of titanium from the leachate of high-sulfur bauxite roasting grog, there is not been reported for the recycle of titanium for current the method.
Accompanying drawing explanation
Fig. 1 is the IR figure of the sodium alginate composite microsphere adsorbent titanium of embodiment 1 preparation.
Fig. 2 is the XRD figure of the sodium alginate composite microsphere adsorbent titanium of embodiment 1 preparation.
Fig. 3 is the SEM figure of the sodium alginate composite microsphere adsorbent titanium of embodiment 1 preparation.
Fig. 4 is the sodium alginate composite microsphere adsorbent titanium of embodiment 1 preparation, XPS figure total before and after absorption.
Fig. 4 a is the enlarged drawing of titanium peak, Ti2p position XPS spectrum figure after absorption in Fig. 4.
Fig. 4 b is the front P of absorption in Fig. 42pXPS swarming spectrogram.
Fig. 4 c be in Fig. 4 absorption after P2pXPS swarming spectrogram.
Fig. 5 is the sodium alginate composite microsphere adsorbent of the embodiment 1 preparation adsorption rate to Ti (IV) under condition of different pH.
Fig. 6 is the sodium alginate composite microsphere adsorbent of the embodiment 1 preparation separating effect to the titanium in actual feed liquid under conditions of different solid ratio.
Detailed description of the invention
1 one kinds of load P of embodiment204Sodium alginate composite microsphere adsorbent
(1) preparation method is as follows:
1. Brown algae powder: take Alga Sgrgassi Enerves, cleaning, drying, is crushed to 60-80 mesh.
2. take Brown algae powder 6g, add the formalin of 72g 1% (v/v), filter, in filtrate, add 103g 15-20g/L Na2CO3Solution, boils at 50-60 DEG C to pasty state, filters, and adds 10-15ml distilled water, mix homogeneously, obtain sodium alginate soln (SA) in filtrate.
3. take 25mL P204Join in separatory funnel with 65mL normal heptane, then add 55mL 1mol/L NaOH solution, rock 15-20min, bleed off bottom NaOH solution, be neutral with distilled water cyclic washing to effluent, obtain the P after saponification204。
4. by the P after 8-10mL saponification204It is added in 25-30mL sodium alginate soln, stirs 20-24h；By P204150-170mL 0.6mol/L CaCl is dropwise instilled with the mixed solution syringe of sodium alginate2In solution, stirring 10-12h, filter, distilled water wash for several times, is dried at 50-60 DEG C, obtains load P204Sodium alginate composite microsphere adsorbent (SA-P204)。
(2) sign of adsorbent
1.IR analyzes: load P204Sodium alginate micro ball adsorbent (SA-P204) infrared spectrum as it is shown in figure 1,3445cm-1For-OH stretching vibration peak, 2862cm-1For CH2-(CH2)3-CH(CH2)-CH2CH3Stretching vibration peak, 1559cm-1For C=O stretching vibration peak, 1291cm-1For P=O stretching vibration peak, 1178cm-1For P-O-C stretching vibration peak, the existence at the above peak demonstrates P204Successfully it is supported on sodium alginate micro ball.
2.XRD analyzes: load P204Sodium alginate micro ball adsorbent (SA-P204) XRD as shown in Figure 2: 2 θ=30 ° are load P204The emerging peak of rear adsorbent, unsupported P204Sodium alginate micro ball then do not have the peak of 2 θ=30 ° to occur, it was demonstrated that new peak and P204Relevant, with pertinent literature phase comparison, find that the peak of 2 θ=30 ° is P204The peak of middle P element, is consistent with the result of infrared spectrum and XPS, P is described204Successfully load on sodium alginate.
3.SEM analyzes: unsupported P204Sodium alginate micro ball (SA, such as Fig. 3 (a)) and load P204Sodium alginate micro ball (SA-P204, such as Fig. 3 (b)) the SEM figure of adsorbent as it is shown on figure 3, in the scanogram of 3 (a), it can be seen that there is a large amount of pore space structure in microsphere surface and surface is the most coarse；In the scanogram of 3 (b), it can be clearly seen that load P204Adsorbent surface unusual light smooth, hole major part disappears, and P is described204Successfully load on sodium alginate.
4.XPS analyzes: visible by Fig. 4, Fig. 4 a-4c, and sodium alginate composite microsphere adsorbent occurs in that Ti peak at about 460ev after absorption titanium, substantially occurs in that P in adsorbent2PPeak, illustrates P204Successfully load on sodium alginate, and P2PPosition at peak before and after absorption, peak significantly there occurs change, illustrates that P serves pivotal role during absorption titanium.
2 one kinds of sodium alginate composite microsphere adsorbents of embodiment under different acidity to feed liquid in the adsorption effect of titanium
Take 10mg sodium alginate composite microsphere adsorbent and add different pH (pH=0.25,0.5,0.75,1,1.25) and [H]+For the solution of the 5mL of 1M, 2M, 3M, 20ppm Ti (IV), by its in vibration case with 180r/min, 30 DEG C of vibration 24h.Result is as shown in Figure 5.
As seen from Figure 5, load P204Sodium alginate composite microsphere adsorbent when pH=1, Ti (IV) is had maximum adsorption rate, be 95%, can realize Ti (IV) in actual feed liquid is adsorbed.
3 one kinds of sodium alginate composite microsphere adsorbents of embodiment separating effect of titanium in feed liquid actual to titanium ferro-aluminum under conditions of different solid ratio
Weigh 10 respectively, 20,30,40,50,60,70,80,90mg adsorbent, it is added thereto to the leachate after 5ml high-sulfur bauxite roasting (titanium 295.5mg/L, aluminum 1677mg/L, ferrum 725.2mg/L), solid-to-liquid ratio is respectively 2:1,4:1,6:1,8:1,10:1,12:1,14:1,16:1,18:1, after shaking 24 hours, measure titanium, aluminum, the concentration of iron ion in solution.Result is as shown in Figure 6.
As seen from Figure 6, under conditions of different solid ratio, along with the increase of solid-to-liquid ratio, the adsorption rate of the titanium ion in actual feed liquid is gradually increasing by sodium alginate composite microsphere adsorbent, reach maximum when solid-to-liquid ratio is 16:1, be 88.5%, aluminum ions adsorption rate is always held at about 15.0%.It appeared that to the adsorption rate of iron ion from the beginning of solid-to-liquid ratio 10:1, be gradually increased from figure.When solid-to-liquid ratio is 12:1, sodium alginate composite microsphere adsorbent is higher to the adsorption rate of the titanium in actual feed liquid, and relatively low to the adsorption rate of aluminium ion and iron ion, therefore the adsorbent of the present invention can realize from high concentration containing Al (III), Fe (III) actual feed liquid selective absorption Ti (IV).
The application on recovery Pd of the 4 one kinds of sodium alginate composite microsphere adsorbents of embodiment
Weigh 100mg SA-P204Adsorbent adds 50mL Ti (IV) solution (concentration is 100mg/L) concussion a period of time, adsorbs saturated rear filtration, is dried.Again with 2mol/L H2SO4-20%H2O2For strippant, Ti (IV) is resolved by the ratio using solid-to-liquid ratio to be 2g:1L.Experiment records 10mg SA-P204Load capacity to titanium is 0.43mg, 2mol/LH2SO4-20%H2O2Eluting rate to titanium is about 80%, after three times circulate, and SA-P204The adsorbance of titanium is still kept about 0.5mg, the response rate can reach about 80% too, it was demonstrated that this adsorbent has good recycling ability.
Claims (10)
1. a load P2O4Sodium alginate composite microsphere adsorbent, it is characterised in that preparation method comprises the steps:
1) take Brown algae powder and join in formalin, soak 4-6h, filter；Na is added in filtrate2CO3Solution, boils at 50-60 DEG C to pasty state, filters, add a small amount of distilled water, obtain sodium alginate soln in filtrate；
2) by the P after saponification2O4Mix with sodium alginate soln, stir 20-24h, by P2O4It is added dropwise to CaCl with the mixed solution syringe of sodium alginate2In solution, stirring 10-12h, filter, gained solid washs, and is dried, obtains target product.
A kind of load P the most according to claim 12O4Sodium alginate composite microsphere adsorbent, it is characterised in that: described Brown algae powder is: by Thallus Laminariae (Thallus Eckloniae) or Alga Sgrgassi Enerves cleaning, drying, be crushed to 60-80 mesh.
A kind of load P the most according to claim 12O4Sodium alginate composite microsphere adsorbent, it is characterised in that: it is the formalin of 1% that every gram of Brown algae powder adds 10-15g concentration expressed in percentage by volume.
A kind of load P the most according to claim 12O4Sodium alginate composite microsphere adsorbent, it is characterised in that: it is the Na of 15-20g/L that every gram of Brown algae powder adds 15-20g concentration2CO3Solution.
A kind of load P the most according to claim 12O4Sodium alginate composite microsphere adsorbent, it is characterised in that: the P after saponification204It is 1:1-3:1 with the mass ratio of sodium alginate soln.
A kind of load P the most according to claim 12O4Sodium alginate composite microsphere adsorbent, it is characterised in that: CaCl2Solution concentration is 0.5-0.7mol/L.
A kind of load P the most according to claim 62O4Sodium alginate composite microsphere adsorbent, it is characterised in that: by volume, P2O4Mixed solution with sodium alginate: CaCl2=1:4-6.
A kind of load P the most according to claim 12O4Sodium alginate composite microsphere adsorbent, it is characterised in that: the described P after saponification2O4Preparation method: take P2O4Join in separatory funnel with normal heptane, then add NaOH solution, rock 15-20min, bleed off bottom NaOH solution, be neutral with distilled water cyclic washing to effluent.
9. the arbitrary described a kind of load P of claim 1-82O4The application in separation and concentration titanium of the sodium alginate composite microsphere adsorbent.
Application the most according to claim 9, it is characterised in that method is as follows: take the solution of titaniferous, regulation solution acidity is 0.56-3mol/L, adds the arbitrary described load P of claim 1-82O4Sodium alginate composite microsphere adsorbent, the ratio of adding is 2-18g/L, at 25-35 DEG C concussion reach adsorption equilibrium.
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| CN114505059A (en) * | 2021-12-27 | 2022-05-17 | 辽宁大学 | Preparation method of porous cellulose nanocrystalline-sodium alginate gel microspheres |
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| CN114505059B (en) * | 2021-12-27 | 2024-01-09 | 辽宁大学 | Preparation method of porous cellulose nanocrystalline-sodium alginate gel microsphere |
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Application publication date: 20160928 |