CN103203219A - Phosphorus removal adsorbent for loading composite metal via active carbon fiber and preparation method of phosphorus removal adsorbent - Google Patents
Phosphorus removal adsorbent for loading composite metal via active carbon fiber and preparation method of phosphorus removal adsorbent Download PDFInfo
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- CN103203219A CN103203219A CN2013101316469A CN201310131646A CN103203219A CN 103203219 A CN103203219 A CN 103203219A CN 2013101316469 A CN2013101316469 A CN 2013101316469A CN 201310131646 A CN201310131646 A CN 201310131646A CN 103203219 A CN103203219 A CN 103203219A
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Abstract
The invention discloses a phosphorus removal adsorbent for loading composite metal via active carbon fiber and a preparation method of the phosphorus removal adsorbent. The adsorbent disclosed by the invention is loaded with lanthanum oxide and iron oxide by taking the active fiber as a substrate, wherein the total mass of the lanthanum oxide and the iron oxide is 27.6-28.4% of the mass of the active carbon fiber. The preparation method of the novel phosphorus removal adsorbent by loading the iron oxide and the lanthanum oxide on the active carbon fiber substrate in appropriate preparation manners by taking the active carbon fiber as the substrate is more reasonable and easy to achieve. By adopting the embodiment of the invention, the novel phosphorus removal adsorbent having the advantages of good economical efficiency and excellent adsorption property can be prepared; and the preparation method is novel and simple. The whole preparation process is short in time and low in energy consumption.
Description
Technical field
The present invention relates to a kind of dephosphorization adsorbent and preparation method thereof, particularly dephosphorization adsorbent of a kind of activated carbon fiber-loaded composition metal and preparation method thereof.
Background technology
The eutrophication of sealing water body has become a serious environmental problem, influences and restricting the coordinated development of society.Nitrogen and phosphorous nutrient is the main compound that causes body eutrophication.More than 56% of lake is added up owing to nitrogen and phosphorus pollution causes accounting for of eutrophication in the main lake of China according to statistics.Remove the phosphorus in the waste water effectively, pollute alleviating water, the eutrophication of eliminating rivers and lakes is significant.Therefore develop efficient cheap dephosphorization adsorbent and correlation technique has become one of urgent task in environmental protection field.
The waste water dephosphorization method of using always both at home and abroad mainly comprises chemical method dephosphorization, bioanalysis dephosphorization and absorption method dephosphorization at present.
Though the chemical dephosphorization method is very high to the clearance of phosphorus, the operating cost height; The metal remained ion not only makes effluent color dilution increase, and produces the mud that is difficult in a large number to handle, causes secondary pollution easily, and may also can produce chronic toxic action to biology; Bioanalysis dephosphorization treatment effect is difficult for stable, and it is bigger that processing procedure is influenced by extraneous factors such as temperature, dissolved oxygen, pH value, and the water outlet total phosphorus is difficult to up to standard.
Comparatively speaking, absorption method has advantages such as technology is simple, treatment effect good, easy to operate and reliable, remedy the deficiency of additive method to a certain extent, had characteristics such as dephosphorization economical and efficient, recyclable, non-secondary pollution, phosphorus removal property be stable, easy to operate.The key of absorption method dephosphorization is to seek a kind of appropriate adsorbent that is suitable for, and require the absorption property of adsorbent outstanding, can regenerate, stable performance, the mechanical strength height, material is easy to get cheap.
The molysite material is easy to get, low price, and main application in the early time generally concentrates on the chemical dephosphorization, and consumption is big, and causes secondary pollution.Iron adsorbent has adsorption and dephosphorization effect preferably, but also has certain gap with outstanding performance of the adsorbent; Active Rare Earth Lanthanum adsorbent has been proved to be in document in the past has outstanding adsorption and dephosphorization effect, and the more similar adsorbent of adsorption capacity is higher, yet rare earth material is difficult for a large amount of the acquisition, and price is more expensive, is difficult to the realization industry and uses; NACF is a kind of novel adsorption functional material, has unique pore structure, micropore prosperity, wide material sources, cheap, characterization of adsorption such as specific area big, regeneration is easy.But NACF is low to the affinity interaction power of phosphorus in the environmental wastewater, adsorption site is few, clearance is not high, only uses NACF to handle waste water and is difficult to reach mark.
Summary of the invention
The object of the present invention is to provide a kind of dephosphorization adsorbent of activated carbon fiber-loaded composition metal.
Two of purpose of the present invention is to provide this preparation of adsorbent method.
For achieving the above object, the present invention adopts following technical scheme:
A kind of dephosphorization adsorbent of activated carbon fiber-loaded composite metal oxide, it is characterized in that this adsorbent is matrix with the NACF, load has lanthana and iron oxide, and wherein the gross mass of lanthana and iron oxide is 27.6%～28.4% of NACF quality.
The mol ratio of iron ion and lanthanum ion is in the lanthana of the above and the iron oxide: 1:9～9:1.
A kind of method for preparing the dephosphorization adsorbent of above-mentioned activated carbon fiber-loaded composite metal oxide is characterized in that the concrete steps of this method are:
A. soluble ferric iron salt and solubility lanthanum salt are mixed with the mixed solution that total mol concentration is 0.02～0.2mol/L;
B. the processed active carbon fiber is shredded and be immersed in the resulting iron lanthanum of the described step a composite metal ion mixed liquor 10 minutes;
C. with the NACF of step b gained dry fully after, under ° C temperature of 400 ° of C ~ 650, activate 30 ~ 150min, to be cooled to room temperature, namely prepare the composite dephosphorization sorbent material, its sealing is preserved.
Above-mentioned soluble ferric iron salt can be ferric nitrate, iron chloride or ferric sulfate; Described solubility lanthanum salt can be lanthanum nitrate or lanthanum chloride.
The present invention compared with prior art, have following apparent outstanding substantive distinguishing features and remarkable advantage: the present invention is at certain lanthanum ion that mixes in molysite, two kinds of metal composite can significantly reduce the preparation cost of material, and can keep higher absorption property.Simultaneously because active Rare Earth Lanthanum and iron oxide generally are pulverous, be difficult to directly apply to water treatment procedure, have only it is loaded to that mechanical strength is higher, could realize operating on the carrier of easy shaping.By suitable preparation means iron oxide, lanthana are loaded to as base material with NACF that to prepare novel adsorption and dephosphorization agent on the NACF matrix more reasonable, be easy to realize.Present embodiment can prepare not only economical, but also the novel adsorption and dephosphorization agent of good absorption property is arranged, the preparation method is novel simple.The whole process of preparation time is short, and energy consumption is low.
The specific embodiment
Details are as follows to the preferred embodiments of the present invention:
Embodiment one:The concrete steps of present embodiment are:
A. be that 1:9 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.1mol/L with iron lanthanum ion mol ratio.
B. NACF is cut into 0.4～0.6cm square piece, wash with water for several times after, dipping, filtration, drying in deionized water;
C. the NACF with step b gained takes by weighing 0.2 g, adds in the resulting suspension of step a, and dipping 10min filters;
D. with 105 ℃ of dryings of solid of step c gained fully after, with 650 ℃ of activation of Muffle furnace 120min; The room temperature that reaches to be cooled namely gets adsorbent, and sealing is preserved.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment two:The technical scheme of present embodiment and embodiment one is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.1mol/L with iron lanthanum ion mol ratio.The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment three:The technical scheme of present embodiment and embodiment one is basic identical, and difference is:
In step a, be that 1:1 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.1mol/L with iron lanthanum ion mol ratio.The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment four:The technical scheme of present embodiment and embodiment one is basic identical, and difference is:
In step a, be that 7:3 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.1mol/L with iron lanthanum ion mol ratio.The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment five:The technical scheme of present embodiment and embodiment one is basic identical, and difference is:
In step a, be that 9:1 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.1mol/L with iron lanthanum ion mol ratio.The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment six:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.02mol/L with iron lanthanum ion mol ratio.The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment seven:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.05mol/L with iron lanthanum ion mol ratio.The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment eight:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.1mol/L with iron lanthanum ion mol ratio.The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment nine:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment ten:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.2mol/L with iron lanthanum ion mol ratio.The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 11:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 650 ℃ of activation of Muffle furnace 30min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 12:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, the configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L when being 3:7 with iron lanthanum ion mol ratio.In steps d, with 650 ℃ of activation of Muffle furnace 60min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 13:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 650 ℃ of activation of Muffle furnace 90min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 14:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 650 ℃ of activation of Muffle furnace 120min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 15:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 650 ℃ of activation of Muffle furnace 150min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 16:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 400 ℃ of activation of Muffle furnace activation 60min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 17:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 450 ℃ of activation of Muffle furnace 60min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 18:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 500 ℃ of activation of Muffle furnace 60min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 19:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 550 ℃ of activation of Muffle furnace 60min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 20:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 600 ℃ of activation of Muffle furnace 60min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 21:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 3:7 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 650 ℃ of activation of Muffle furnace 60min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
Embodiment 22:The technical scheme of present embodiment and previous embodiment is basic identical, and difference is:
In step a, be that 1:39.98 configuration total mol concentration is ferric nitrate and the lanthanum nitrate mixed solution 10mL of 0.15mol/L with iron lanthanum ion mol ratio.In steps d, with 600 ℃ of activation of Muffle furnace 70min.
The adsorption capacity data of present embodiment composite dephosphorization adsorbent see Table 1.
?
Performance test methods:
Get the adsorbent of mass M and put into conical flask, in this conical flask, add concentration C then
0Be 20 mg/L phosphorus solution, measure the KH of volume V by adsorbent dosage 1.0g/L
2PO
4Solution adsorbs in constant temperature oscillator, and adsorption time is 24h, and adsorption temp is 25 ° of C, after absorption finishes, measures absorption back solution concentration C
eMeasuring method GBT11893-1989, adsorbents adsorb capacity q (mg/g)=V* (C
0-C
e)/M the results are shown in Table 1.
Table 1. embodiment experimental data table
| Experimental example | Iron lanthanum ion mol ratio (ratio mixes) | Metal ion total mol concentration mol/L | Soak time min | Activation temperature ° C | Adsorption capacity (mg/g) |
| Embodiment one | 1:9 | 0.1 | 120 | 650 | 10.9245 |
| Embodiment two | 3:7 | 0.1 | 120 | 650 | 10.4920 |
| Embodiment three | 1:1 | 0.1 | 120 | 650 | 8.58981 |
| Embodiment four | 7:3 | 0.1 | 120 | 650 | 7.55278 |
| Embodiment five | 9:1 | 0.1 | 120 | 650 | 4.23427 |
| Embodiment six | 3:7 | 0.02 | 120 | 650 | 6.45693 |
| Embodiment seven | 3:7 | 0.05 | 120 | 650 | 8.51094 |
| Embodiment eight | 3:7 | 0.10 | 120 | 650 | 11.21092 |
| Embodiment nine | 3:7 | 0.15 | 120 | 650 | 11.95141 |
| Embodiment ten | 3:7 | 0.2 | 120 | 650 | 11.74601 |
| Embodiment 11 | 3:7 | 0.15 | 30 | 650 | 12.2082 |
| Embodiment 12 | 3:7 | 0.15 | 60 | 650 | 14.6216 |
| Embodiment 13 | 3:7 | 0.15 | 90 | 650 | 12.2082 |
| Embodiment 14 | 3:7 | 0.15 | 120 | 650 | 11.7974 |
| Embodiment 15 | 3:7 | 0.15 | 150 | 650 | 11.2839 |
| Embodiment 16 | 3:7 | 0.15 | 60 | 400 | 10.7190 |
| Embodiment 17 | 3:7 | 0.15 | 60 | 450 | 10.7703 |
| Embodiment 18 | 3:7 | 0.15 | 60 | 500 | 11.6947 |
| Embodiment 19 | 3:7 | 0.15 | 60 | 550 | 11.3352 |
| Embodiment 20 | 3:7 | 0.15 | 60 | 600 | 12.0541 |
| Embodiment 21 | 3:7 | 0.15 | 60 | 650 | 11.5920 |
| Embodiment 22 | 1:39.98 | 0.15 | 60 | 600 | 13.3017 |
By table 1 as can be known: can prepare the composite dephosphorization adsorbent of different adsorption capacities by control iron lanthanum ion mol ratio (ratio mixes), metal ion total mol concentration, the soak time of Muffle furnace, the activation temperature of Muffle furnace, certain lanthanum ion mixes in molysite, two kinds of metal composite can significantly reduce the preparation cost of material, and can keep higher absorption property.Adsorbent of the present invention is matrix with the NACF, and load has iron lanthanum composite oxides, and resulting adsorbent has advantages such as high-adsorption-capacity, high dephosphorizing rate rate.Instrument required for the present invention is simple, easy to operate, has favorable industrial application prospect, and the method for composition metal is the effectively lower preparation cost of material has kept outstanding absorption property.
Foregoing is illustrated the embodiment of the invention; but the invention is not restricted to above-described embodiment; can also make multiple variation according to the purpose of innovation and creation of the present invention; as adopt the compound of the organic metal platinum of other kinds; adopt the different microwave reaction time etc.; all according to technical solution of the present invention spiritual essence and principle under the change made; modify; substitute; combination; simplify; all should be the substitute mode of equivalence; as long as goal of the invention according to the invention; only otherwise deviate from the composite dephosphorization adsorbent preparation method's of the activated carbon fiber-loaded metal of the present invention know-why and inventive concept, all belong to protection scope of the present invention.
Claims (4)
1. the dephosphorization adsorbent of an activated carbon fiber-loaded composite metal oxide, it is characterized in that this adsorbent is matrix with the NACF, load has lanthana and iron oxide, and wherein the gross mass of lanthana and iron oxide is 27.6%～28.4% of NACF quality.
2. the dephosphorization adsorbent of activated carbon fiber-loaded composite metal oxide according to claim 1 is characterized in that the mol ratio of iron ion and lanthanum ion is in described lanthana and the iron oxide: 1:9～9:1.
3. method for preparing the dephosphorization adsorbent of activated carbon fiber-loaded composite metal oxide according to claim 1 and 2 is characterized in that the concrete steps of this method are:
A. soluble ferric iron salt and solubility lanthanum salt are mixed with the mixed solution that total mol concentration is 0.02～0.2mol/L;
B. the processed active carbon fiber is shredded and be immersed in the resulting iron lanthanum of the described step a composite metal ion mixed liquor 10 minutes;
C. with the NACF of step b gained dry fully after, under ° C temperature of 400 ° of C ~ 650, activate 30 ~ 150min, to be cooled to room temperature, namely prepare the composite dephosphorization sorbent material, its sealing is preserved.
4. method according to claim 3 is characterized in that soluble ferric iron salt is: ferric nitrate, iron chloride or ferric sulfate; Described solubility lanthanum salt is: lanthanum nitrate or lanthanum chloride.
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| CN105854806A (en) * | 2016-06-03 | 2016-08-17 | 上海大学 | Lanthanum-iron-compound-metal-oxide-loading expanded-graphite phosphate removing agent and preparing method thereof |
| CN106362688A (en) * | 2016-10-24 | 2017-02-01 | 江苏省农业科学院 | Preparation method and application of modified charcoal adsorbent based on lanthanum ferrite |
| CN106861621A (en) * | 2017-03-24 | 2017-06-20 | 华纺股份有限公司 | A kind of La2O3/Fe2O3The preparation technology of carbon fibre material |
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| CN107961760A (en) * | 2017-11-30 | 2018-04-27 | 华南理工大学 | A kind of activated carbon supported FeOOH compound adsorbent and its preparation and application |
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| CN102350306A (en) * | 2011-09-19 | 2012-02-15 | 上海大学 | Activated carbon fiber adsorbent loaded with lanthanum hydroxide and preparation method thereof |
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Cited By (8)
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| CN105854806A (en) * | 2016-06-03 | 2016-08-17 | 上海大学 | Lanthanum-iron-compound-metal-oxide-loading expanded-graphite phosphate removing agent and preparing method thereof |
| CN106362688A (en) * | 2016-10-24 | 2017-02-01 | 江苏省农业科学院 | Preparation method and application of modified charcoal adsorbent based on lanthanum ferrite |
| CN106861621A (en) * | 2017-03-24 | 2017-06-20 | 华纺股份有限公司 | A kind of La2O3/Fe2O3The preparation technology of carbon fibre material |
| CN106861605A (en) * | 2017-03-31 | 2017-06-20 | 四川农业大学 | Activated carbon supported nanometer Fe Al（Hydrogen）The preparation method and applications of oxide particle composites |
| CN107961760A (en) * | 2017-11-30 | 2018-04-27 | 华南理工大学 | A kind of activated carbon supported FeOOH compound adsorbent and its preparation and application |
| CN109082880A (en) * | 2018-07-05 | 2018-12-25 | 王伟霞 | Functional activity carbon fiber, preparation method and applications |
| CN109082880B (en) * | 2018-07-05 | 2021-07-09 | 浪达网络科技(浙江)有限公司 | Functional activated carbon fiber, preparation method and application thereof |
| CN110180498A (en) * | 2019-05-23 | 2019-08-30 | 江苏省农业科学院 | Carry the preparation method and application of lanthanum magnetism hydro-thermal charcoal adsorbent |
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