CN104034842A - Simple and easy method for judging reaction activity of iron materials - Google Patents
Simple and easy method for judging reaction activity of iron materials Download PDFInfo
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- CN104034842A CN104034842A CN201410243599.1A CN201410243599A CN104034842A CN 104034842 A CN104034842 A CN 104034842A CN 201410243599 A CN201410243599 A CN 201410243599A CN 104034842 A CN104034842 A CN 104034842A
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Abstract
The invention relates to a simple and easy method for judging the reaction activity of iron materials. The simple and easy method comprises the specific steps: selecting standard iron materials; preparing a potassium dichromate standard solution; adding 0.1-500g/L of the standard iron materials with the gradient mass into the standard solution under the conditions that the temperature is 15-25 DEG C, the pH (Potential of Hydrogen) value is 3-7, the reaction time is 2-10 hours, and the concentration of hexavalent chromium is 50-1,000mg/L; drawing a standard curve for a reaction of the standard iron materials and potassium dichromate and a standard curvilinear equation; adding 0.1-500g/L of iron materials to be detected with a certain mass into the prepared standards solution and sufficiently reacting under the conditions that the temperature is 15-25 DEG C, the pH value is 3-7, the reaction time is 2-10 hours, and the concentration of hexavalent chromium is 50-1,000mg/L; measuring the chromium removing amount of the iron materials to be detected; and establishing a method for uniformly judging the reaction activity of the iron materials to quantitatively judge the reaction activity of the iron materials to be detected. The simple and easy method is mainly applied to comparison and selection of the iron materials in a wastewater treating process and has the advantages of simple conditions, convenience in operation, reliable results, economical efficiency and safety and the like.
Description
Technical field
The invention provides a kind of simple and easy method of discrimination that is applied to environmental area iron material reactivity, belong to field of waste water treatment.
Background technology
Ferro element is extensively present in occurring in nature, cheap and easy to get, utilizes the different valence state of iron, the strengthening that form is polluted administer and repair significant.Since the eighties in 20th century, Zero-valent Iron (ZVI) is successively applied to the removal of organic pollutants and the original position reparation of Polluted Groundwater, is also a kind of mainstream technology that electroplating wastewater, waste water from dyestuff, heavy metal containing wastewater treatment and soil pollution are administered.Zero-valent Iron technology, as a kind of cheap, simple, nontoxic, efficient environmental pollution improvement and restorative procedure, has become a wide concerned research field.
The iron material that environmental area uses, requires it to have compared with extensive chemical reactivity, and environmental area there is no corresponding sorting technique and operative norm at present.This problem is more outstanding in Administering Practice on Environment.Implement for scale Zero-valent Iron technology, the iron material demand of employing is large, and needs while purchasing clear and definite and understand its reactivity, thereby judges whether selected iron material is the optimization process material of target contaminant.Thereby develop easy, accurate, easy-operating discrimination method, judge that the reactivity of iron material becomes a problem demanding prompt solution.
At present the sign of iron material is adopted to BET-N more
2determination of adsorption method specific surface area.BET-N
2absorption method is also in current environmental area, the most frequently used and only have a measurement measure of standardization iron material.But BET-N
2absorption method is to pass through N for the measurement of iron material surface area
2the mode secondary indication of absorption, is difficult to differentiation and can contacts with pollutant with the surface that can not contact with pollutant and have the surface of reducing power and the surface of non-reduced ability.Iron material also parent pollutant mostly is solid-liquid interface reaction, and this just requires characterizing method should reflect reducing property and the surface adsorption property of iron material simultaneously.The former determines by material surface Zero-valent Iron composition, and the latter is depended on specific surface area size.Correlative study shows, vapour deposition synthesis of nano Zero-valent Iron (nZVI) has higher BET-N than the synthetic nZVI of liquid-phase reduction
2surface area, but its reducing power is inferior to the synthetic nZVI of liquid phase.Visible, BET-N
2absorption method just reflects iron material specific surface area size indirectly, is inaccurate to the sign of its reactivity.
Summary of the invention
The present invention is intended to set up a kind of simple and easy method of judging iron material reactivity.
The simple and easy method of the judgement iron material reactivity that the present invention proposes, concrete steps are as follows:
(1) benchmark iron material is selected: the fresh micron Zero-valent Iron (mFe) that benchmark iron material is selected the fresh nano zero valence iron (nZVI) that laboratory liquid is combined to or purchased, or the clear and definite iron material of reactivity also can be used as benchmark iron material;
(2) adopt and configure sexavalent chrome standard solution; Sexavalent chrome standard solution adopts freshly prepared potassium dichromate (K
2cr
2o
7) standard solution, controlling chromium concn is 50-1000 mg/L;
(3) control reaction conditions, the benchmark iron material that adds into quality gradient reacts with sexavalent chrome standard solution; In batch reaction to the benchmark iron material that adds into step (1) gained of quality gradient in the sexavalent chrome standard solution of step (2) gained; According to the selection of benchmark iron material, select the benchmark iron material of 3-8 different dosages, the concentration of controlling benchmark iron material is 0.1-500 g/L, and controlling sexavalent chrome standard solution initial reaction pH value is 3-7, temperature of reaction is at 15-25 DEG C, and the reaction time is 2-10 hour; Taking benchmark iron material dosage as horizontal ordinate, chromium removal amount is ordinate, draws and is linear response curve;
(4) benchmark iron material typical curve and typical curve equation obtain; React with sexavalent chrome standard solution by benchmark iron material and draw benchmark iron material response curve, by coordinate axis standardization, obtain benchmark iron material typical curve, typical curve equation and typical coefficient K
cr; In coordinate axis standardisation process, constant before and after ordinate, be chromium removal amount (Δ Cr, mg/L); Horizontal ordinate is converted into benchmark active area concentration (m by benchmark iron material dosage (g/L)
2/ L); Its standardized way is: benchmark iron material dosage (g/L) is multiplied by benchmark iron material specific surface area (m
2/ g), obtain benchmark active area concentration (m
2/ L); Plays curvilinear equation of the present invention is as follows:
Δ Cr=K
cr
s
benchmark
Wherein: the removal amount that Δ Cr is chromium;
K
crfor typical coefficient;
S
benchmarkfor benchmark active area concentration;
(5) control reaction conditions, add iron material to be measured and react with sexavalent chrome standard solution; Add iron material to be measured to sexavalent chrome standard solution (chromium concn scope is at 50-1000 mg/L), controlling sexavalent chrome standard solution initial pH value is 3-7, and temperature of reaction is at 15-25 DEG C, and the reaction time is at 2-10 hour; Test can obtain iron material to be measured to chromic removal amount;
(6) set up the unified method of judging iron material reactivity and quantitatively judge iron material reactivity to be measured; By hexavalent chromium removal amount and typical curve equation, obtain corresponding benchmark active area concentration; By the benchmark active area concentration (m of iron material to be measured
2/ L) divided by its dosage (g/L), can calculate the benchmark active area size (m that iron material to be measured has
2/ g), thus can quantize relatively its reactivity.
Beneficial effect of the present invention is: study for a long period of time result and the use experience that the present invention is based on Zero-valent Iron material processed engineering, a kind of simple and easy method of discrimination that is applied to environmental area iron material reactivity is provided, there is the features such as condition is simple, easy to operate, reliable results, economic security.
Brief description of the drawings
Fig. 1 is benchmark iron material of the present invention (fresh nano zero valence iron, nZVI) typical curve and typical curve equation.
Fig. 2 is benchmark iron material of the present invention (fresh micron Zero-valent Iron, mFe) typical curve and typical curve equation.
Embodiment
further illustrate the present invention below by embodiment.
Embodiment 1: the step of the present embodiment is as follows:
(1) choose fresh nano zero valence iron (nZVI) that laboratory liquid is combined to as benchmark iron material, reaction equation is:
(2) preparation potassium dichromate (K
2cr
2o
7) standard solution, chromium concn is 100 mg/L;
(3) in 6 reaction bulbs, inject 50 mL potassium dichromate standard solution, initial pH is 4.6, adds respectively 0,0.1,0.2,0.5,0.8,1 g/L nZVI.Sealing, puts into 25 DEG C of constant-temperature tables, reacts 10 hours;
(4) take out sample, water sample is through 0.22 μ m membrane filtration, and filtrate, through clearing up constant volume, is utilized chromium content in inductive coupling plasma emission spectrograph working sample;
(5) taking benchmark iron material dosage (g/L) as horizontal ordinate, chromium removal amount (mg/L) is ordinate, draws response curve;
(6) coordinate axis standardization: benchmark iron material dosage (g/L) in horizontal ordinate is multiplied by nZVI specific surface area 20(m
2/ g), obtain benchmark active area concentration (m
2/ L); Ordinate is constant, is chromium removal amount (mg/L).Typical curve as shown in Figure 1.Typical curve equation is as follows:
Δ Cr=K
cr
s
benchmark
Wherein: the removal amount that Δ Cr is chromium;
K
crfor typical coefficient, K in this mode
cr=4.2;
S
benchmarkfor benchmark active area concentration;
(7) in 11 reaction bulbs, inject 50 mL potassium dichromate standard solution, wherein 1 does not add iron material, and other 10 add respectively 5 kinds of different iron materials (2 every kind), and initial pH is 4.6, and throwing amount is unfixing.Sealing, puts into 25 DEG C of constant-temperature tables, reacts 10 hours;
(8) take out sample, water sample is through 0.22 μ m membrane filtration, and filtrate, through clearing up constant volume, is utilized chromium content in inductive coupling plasma emission spectrograph working sample;
(9) bring chromium removal amount into typical curve equation, can obtain the benchmark active area concentration that iron material to be measured is corresponding;
(10), by the benchmark active area concentration of the iron material to be measured obtaining, divided by its dosage, can calculate the benchmark active area size that iron material to be measured has, thereby can quantize to judge to its reactivity.
Experimental result is as shown in the table:
Experimental result is as shown in the table:
table 1iron material analysis result to be measured
Benchmark active area size by iron material more to be measured can quantitatively judge its reactivity.In this embodiment: the benchmark active area maximum of No. 5 iron materials, its reactivity is the strongest; The benchmark active area minimum of No. 1 iron material, its reactivity is the most weak; All the other iron material reactivity sequences are 1 < 4 < 3 < 2 < 5.
embodiment 2
Present embodiment step is as follows:
(1) choose the fresh micron Zero-valent Iron (mFe) of purchasing as benchmark iron material;
(2) preparation potassium dichromate (K
2cr
2o
7) standard solution, chromium concn is 100 mg/L;
(3) in 6 reaction bulbs, inject 50 mL potassium dichromate standard solution, initial pH is 4.6, adds respectively 0,10,20,50,100,200g/LmFe.Sealing, puts into 25 DEG C of constant-temperature tables, reacts 10 hours;
(4) take out sample, water sample is through 0.22 μ m membrane filtration, and filtrate, through clearing up constant volume, is utilized chromium content in inductive coupling plasma emission spectrograph working sample;
(5) taking benchmark iron material dosage (g/L) as horizontal ordinate, chromium removal amount (mg/L) is ordinate, draws response curve;
(6) coordinate axis standardization: benchmark iron material dosage (g/L) in horizontal ordinate is multiplied by mFe specific surface area 3(m
2/ g), obtain benchmark active area concentration (m
2/ L); Ordinate is constant, is chromium removal amount (mg/L).Typical curve as shown in Figure 2.Typical curve equation is as follows:
Δ Cr=K
cr
s
benchmark
Wherein: the removal amount that Δ Cr is chromium;
K
crfor typical coefficient, K in this mode
cr=0.13;
S
benchmarkfor benchmark active area concentration.
(7) in 11 reaction bulbs, inject 50 mL potassium dichromate standard solution, wherein 1 does not add iron material, and other 10 add respectively 5 kinds of different iron materials (2 every kind), and initial pH is 4.6, and throwing amount is unfixing.Sealing, puts into 25 DEG C of constant-temperature tables, reacts 10 hours;
(8) take out sample, water sample is through 0.22 μ m membrane filtration, and filtrate, through clearing up constant volume, is utilized chromium content in inductive coupling plasma emission spectrograph working sample;
(9) bring chromium removal amount into typical curve equation, can obtain the benchmark active area concentration that iron material to be measured is corresponding;
(10), by the benchmark active area concentration of the iron material to be measured obtaining, divided by its dosage, can calculate the benchmark active area size that iron material to be measured has, thereby can quantize to judge to its reactivity.
Experimental result is as shown in the table:
table 2iron material analysis result to be measured
Benchmark active area size by iron material more to be measured can quantitatively judge its reactivity.In this embodiment: the benchmark active area maximum of No. 5 iron materials, its reactivity is the strongest; The benchmark active area minimum of No. 1 iron material, its reactivity is the most weak; The sequence of all the other iron material reactivities is 1 < 4 < 3 < 2 < 5, and comes to the same thing in embodiment 1.
Claims (1)
1. judge a simple and easy method for iron material reactivity, it is characterized in that concrete steps are as follows:
(1) benchmark iron material is selected: the fresh micron Zero-valent Iron (mFe) that benchmark iron material is selected the fresh nano zero valence iron (nZVI) that laboratory liquid is combined to or purchased, or the clear and definite iron material of reactivity also can be used as benchmark iron material;
(2) adopt and configure sexavalent chrome standard solution; Sexavalent chrome standard solution adopts freshly prepared potassium dichromate (K
2cr
2o
7) standard solution, controlling chromium concn is 50-1000 mg/L;
(3) control reaction conditions, the benchmark iron material that adds into quality gradient reacts with sexavalent chrome standard solution; In batch reaction to the benchmark iron material that adds into step (1) gained of quality gradient in the sexavalent chrome standard solution of step (2) gained; According to the selection of benchmark iron material, select the benchmark iron material of 3-8 different dosages, the concentration of controlling benchmark iron material is 0.1--500 g/L, and controlling sexavalent chrome standard solution initial reaction pH value is 3-7, temperature of reaction is at 15-25 DEG C, and the reaction time is 2-10 hour; Taking benchmark iron material dosage as horizontal ordinate, chromium removal amount is ordinate, draws and is linear response curve;
(4) benchmark iron material typical curve and typical curve equation obtain; React with sexavalent chrome standard solution by benchmark iron material and draw benchmark iron material response curve, by coordinate axis standardization, obtain benchmark iron material typical curve, typical curve equation and typical coefficient K
cr; In coordinate axis standardisation process, constant before and after ordinate, be chromium removal amount (Δ Cr, mg/L); Horizontal ordinate is converted into benchmark active area concentration (m by benchmark iron material dosage (g/L)
2/ L); Its standardized way is: benchmark iron material dosage (g/L) is multiplied by benchmark iron material specific surface area (m
2/ g), obtain benchmark active area concentration (m
2/ L); Plays curvilinear equation of the present invention is as follows:
Δ Cr=K
cr
s
benchmark
Wherein: the removal amount that Δ Cr is chromium;
K
crfor typical coefficient;
S
benchmarkfor benchmark active area concentration;
(5) control reaction conditions, add iron material to be measured and react with sexavalent chrome standard solution; In sexavalent chrome standard solution, add iron material to be measured, controlling sexavalent chrome standard solution initial pH value is 3-7, controls chromium concn scope at 50-1000 mg/L, and temperature of reaction is at 15-25 DEG C, and the reaction time is at 2-10 hour; Test can obtain iron material to be measured to chromic removal amount;
(6) set up the unified method of judging iron material reactivity and quantitatively judge iron material reactivity to be measured; By hexavalent chromium removal amount and typical curve equation, obtain corresponding benchmark active area concentration; By the benchmark active area concentration (m of iron material to be measured
2/ L) divided by its dosage (g/L), can calculate the benchmark active area size (m that iron material to be measured has
2/ g), thus can quantize relatively its reactivity.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104807762A (en) * | 2015-04-15 | 2015-07-29 | 刘骁勇 | Method for detecting content of zero-valent iron in NZVI (nanoscale zero valent iron) particles |
-
2014
- 2014-06-04 CN CN201410243599.1A patent/CN104034842B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 谢丽萍: "基于零价铁的技术去除含铬废水的基础研究", 《中国优秀硕士论文全文数据库工程科技Ⅰ辑B027-244页》, no. 10, 15 October 2013 (2013-10-15) * |
| 陈芳艳 等: "纳米零价铁对水中Cr(Ⅵ)的还原动力学研究", 《化学世界》, no. 3, 31 December 2007 (2007-12-31) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104807762A (en) * | 2015-04-15 | 2015-07-29 | 刘骁勇 | Method for detecting content of zero-valent iron in NZVI (nanoscale zero valent iron) particles |
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