CN103755005B - Ferric ion reduction method - Google Patents
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Abstract
The invention discloses a kind of Ferric ion reduction method, first the carbon containing biomass collected are carried out, air-dry, dry, pulverize, sieve, obtain the particle diameter carbon containing biomass dry powder less than 100 mesh；Then carbon containing biomass dry powder and water are mixed in proportion and be placed in autoclave, answering the hydrothermal temperature in still is 100 ~ 300 DEG C, after reactant heating 1 ~ 24h, cooling, rinse constant to cleaning mixture pH, refilter drying, then with 100 ~ 300 DEG C of activation 1 ~ 30min, then obtain hydro-thermal biology powdered carbon after grinding and sieving；Finally hydro-thermal biology powdered carbon is added Fe according to the dosage that adds of 0.1 ~ 10g/L3+In solution, reduction reaction 0 ~ 120h, after reduction reaction, obtain Fe2+Solution.The present invention develops a kind of Fe simple, cheap, efficient3+Reducing/regenerating Fe2+Method, realizes the recycling to abandoned biomass simultaneously, has a extensive future.
Description
Technical field
The present invention relates to a kind of reducing agent preparation method and oxide-reduction method, especially relate to a kind of high valent metal
Ion reduction is the method for low valent metal ion, is applied to biomass recycling use, metal ion regeneration and organic waste
The oxidation technology field of water.
Background technology
Fenton reaction has that speed is fast, mild condition, simple to operation, reaction efficiently, flocculation, Yi Jishi can be produced
By advantages such as scope are wide, be suitable to difficult for biological degradation or the oxidation processes of organic wastewater that general chemical oxidation difficulty is proved effective.In acidity
Under the conditions of, H2O2Pass through Fe2+Catalytic action can generate the hydroxyl radical free radical OH with very Strong oxdiative ability, then cause
A series of radical reactions, make Organic substance and some reducing substanceses comparatively fast aoxidize.Its main course of reaction is as follows:
Fe2++H2O2→Fe3++OH-+·OH (1)
Fe3++H2O2→Fe2++H++HO2· (2)
Fe2++·OH→Fe3++OH- (3)
H2O2+·OH→H2O+ HO2· (4)
Fe2++HO2·→Fe3++HO2 - (5)
Fe3++HO2·→Fe2++H++O2 (6)
The reaction of whole Fenton system is more complicated, it is critical only that H2O2At Fe2+Catalytic action and transmittance process in send out
Raw chain reaction is until exhausting.Owing to the reaction rate of formula (2) formula (6) is relatively slow, cause Fe in course of reaction2+A large amount of streams
Lose, have influence on mineralization degree and the H treating degradation of organic substances2O2Utilization rate.
For ensureing Fe2+Concentration, is allowed to the most persistently be catalyzed H2O2, basis that relevant scholar reacts in traditional F enton
On carried out two aspects improve.A kind of light-Fenton method being introduced into ultraviolet irradiation, Fe3+Can with the OH compound ion in water
Directly produce hydroxyl radical free radical OH and Fe2+, the latter continues and H2O2Reaction generates OH, ultraviolet and Fe2+For catalysis H2O2
Create cooperative effect；Another kind is to increase the electricity-Fenton method of electrochemical appliance, by the effect of impressed current by Fe3+Also
Originally it was Fe2+.Although the two is overcoming traditional F enton reaction Fe3+To Fe2+Conversion ratio is too low, improves H2O2Utilization rate and entirety
The aspects such as reaction rate have positive role, but the high cost of auxiliary device, higher energy consumption and relatively low solar photovoltaic utilization rate are systems
The about limiting factor of its scale application.Therefore, the Fe of a kind of high efficiency low cost is found3+Method of reducing has important reality meaning
Justice.
In recent years, the approach that biological carbon materials comprehensively utilizes as biomass resource, due to its significant environment and
Social benefit, causes worldwide broad interest and concern.The pore structure of its prosperity, preferable environmental stability exist
Keeping soil moisture, nutrient, the absorption pollutant aspect effect such as Organic substance, heavy metal is notable.Existing scientific experiments research is main
Concentrate on and charcoal is solved respective environment problem as a kind of adsorbing material, and its reduction characteristic rarely has report.
Summary of the invention
In order to solve traditional F enton reaction Fe3+To Fe2+The technical problem that conversion ratio is too low, it is an object of the invention to
Overcome the deficiency that prior art exists, it is provided that a kind of Ferric ion reduction method, a kind of Fe simple, cheap, efficient of exploitation3+
Reducing/regenerating Fe2+Method, realizes the recycling to abandoned biomass simultaneously, it is achieved environmental pollution decrement, has the widest
Wealthy scale and industrialization space, have a extensive future.
Creating purpose for reaching foregoing invention, the present invention uses following technical proposals:
A kind of Ferric ion reduction method, comprises the following steps:
A. raw material prepares: is carried out the carbon containing biomass collected, air-dries, then carries out 100 ~ 120 DEG C of drying, powder
Broken, sieve, obtain particle diameter less than the carbon containing biomass dry powder of 100 mesh；
B. prepared by hydro-thermal charcoal: the carbon containing biomass dry powder after sieving in above-mentioned steps a and water are according to weighing body
Long-pending than being 1:(2 ~ 10) gram weight mix homogeneously with the ratio of milliliter volume and be placed in autoclave, then to autoclave
Sealing after interior logical nitrogen deoxygenation, the hydrothermal temperature controlled in autoclave is 100 ~ 300 DEG C, to the reaction in autoclave
After thing heating 1 ~ 24h, in autoclave, take out hydrothermal carbonization product, and make its room temperature cool down, then hydrothermal carbonization is produced
Thing dehydrated alcohol and distilled water rinse to cleaning mixture pH constant repeatedly, refilter drying, then with 100 ~ 300 DEG C activation 1 ~
30min, then obtain hydro-thermal biology powdered carbon after grinding and sieving, store for future use；Preferably control the hydro-thermal temperature in autoclave
Degree is hydrothermal temperature 160-240 DEG C, and preferably the reactant in autoclave is heated 2-6h；The most further preferably activation temperature
For 200-240 DEG C, and preferably soak time is 5-10min；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 0.1
The dosage that adds of ~ 10g/L adds the Fe that concentration is 10 ~ 1000ppm, pH=0 ~ 33+In solution, reduction reaction 0 ~ 120h, through also
Fe is obtained after former reaction2+Solution；Preferably hydro-thermal biology powdered carbon is added the Fe that concentration is 100 ~ 900ppm, pH=1 ~ 33+Solution
In, and preferably reduction reaction 70 ~ 120h；Preferably hydro-thermal biology powdered carbon is joined Fe according to the dosage that adds of 1 ~ 4g/L3+Solution
In.
The present invention uses the Fe that chemical analysis method measures after reduction reaction in solution3+And Fe2+Concentration, carries out Fe3+Reduction
Regeneration Fe2+Effect detection analysis.
The present invention compared with prior art, has and the most obviously highlights substantive distinguishing features and remarkable advantage:
1. the present invention prepares the raw material sources of reproducibility hydro-thermal biological carbon materials and extensively and is conveniently easy to get, garden garbage, green
Change rubbish, crop material, instruction plant etc., it is achieved that the recycling of abandoned biomass；
2. the preparation process of the reproducibility hydro-thermal charcoal of the present invention is simple, can scale application；
3. the biological carbon materials pore structure that the present invention is utilized is extensively and reducing property is good, is not required to add any chemistry
Medicine, non-secondary pollution；
Reduction process the most of the present invention is very simple, and operating condition requires relatively low；
5. the present invention utilizes the reduction characteristic of hydro-thermal biological carbon materials, by disposal and the Fe of abandoned biomass3+Reduction process
Combine, use simple processing method to achieve the recycling of refuse, and have the most wide scale,
Industrialization space, meets ecological, environmental protective and the theory of sustainable development and requirement.
Accompanying drawing explanation
Fig. 1 is the Technology Roadmap of the embodiment of the present invention one Ferric ion reduction method.
Fig. 2 is the Fe of inventive embodiments one2+The kinetics trendgram of concentration and time relationship.
Fig. 3 is different initial Fe in the embodiment of the present invention one～embodiment nine3+Concentration is to Fe3+The impact of reduction effect becomes
Gesture figure.
Detailed description of the invention
Details are as follows for the preferred embodiments of the present invention:
Embodiment one:
In the present embodiment, see Fig. 1 and Fig. 2, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: the original biomass distilled water collected is cleaned, is air-dried, is placed on blowing-type drying baker
In in 105 DEG C of drying, then with pulverizer pulverize, sieve, obtain the carbon containing biomass dry powder that particle diameter is 100 mesh；
B. prepared by hydro-thermal charcoal: the carbon containing biomass dry powder after sieving in above-mentioned steps a weighs 10g and 50ml
Distilled water mix homogeneously is placed in autoclave, seals, control height after leading to nitrogen deoxygenation in 10 minutes with the speed of 100ml/min
Hydrothermal temperature in pressure reactor is 240 DEG C, after the reactant in autoclave is heated 4h, takes out in autoclave
Hydrothermal carbonization product, and make its room temperature cool down, then hydrothermal carbonization product dehydrated alcohol and distilled water are rinsed repeatedly to washing
Wash liquid pH constant, refilter drying, then with 240 DEG C of activation 10min, then obtain hydro-thermal biology powdered carbon after grinding and sieving,
Gained hydro-thermal charcoal productivity is 13%, is stored for future use by this hydro-thermal biology powdered carbon；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 1g/
The dosage that adds of L adds the Fe that concentration is 200 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution.
In the present embodiment, the Fe in solution after employing chemical analysis method measures reduction reaction3+And Fe2+Concentration, is carried out
Fe3+Reducing/regenerating Fe2+Effect detection analysis.After taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, adopts
With its Fe of spectrophotometric determination o-phenanthroline3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Also
Former rate is 60%, sees Fig. 3.
The present embodiment Fe solion fixed time interval is sampled, measures Fe in solution3+And Fe2+Concentration, result such as Fig. 2, from
Fe2+The kinetics trend of concentration and time relationship is visible, and when reduction reaction proceeds to 70h, reduction reaction is flat close to chemistry
Weighing apparatus, when reduction reaction proceeds to 120h, reduction reaction basically reaches chemical equilibrium.
Original biomass is first prepared as biological carbon materials by water-heat process and activation process by the present embodiment, is subsequently adding
Fe3+Solution carries out reduction reaction, have compared with tradition method of reducing simple the most efficiently, the most easy advantage, and have relatively
For wide scale, industrialization space, meet ecological, environmental protective and the theory of sustainable development and requirement.
Embodiment two:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: identical with embodiment one；
B. prepared by hydro-thermal charcoal: identical with embodiment one；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 1g/
The dosage that adds of L adds the Fe that concentration is 100 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution, after taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, uses Phen to divide
Its Fe of light spectrphotometric method for measuring3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Percent reduction is 100%, sees
Fig. 3.
Embodiment three:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: identical with embodiment one；
B. prepared by hydro-thermal charcoal: identical with embodiment one；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 1g/
The dosage that adds of L adds the Fe that concentration is 300 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution, after taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, uses Phen to divide
Its Fe of light spectrphotometric method for measuring3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Percent reduction is 50%, sees
Fig. 3.
Embodiment four:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: identical with embodiment one；
B. prepared by hydro-thermal charcoal: identical with embodiment one；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 1g/
The dosage that adds of L adds the Fe that concentration is 400 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution, after taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, uses Phen to divide
Its Fe of light spectrphotometric method for measuring3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Percent reduction is 40%, sees
Fig. 3.
Embodiment five:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: identical with embodiment one；
B. prepared by hydro-thermal charcoal: identical with embodiment one；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 1g/
The dosage that adds of L adds the Fe that concentration is 500 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution, after taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, uses Phen to divide
Its Fe of light spectrphotometric method for measuring3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Percent reduction is 34%, sees
Fig. 3.
Embodiment six:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: identical with embodiment one；
B. prepared by hydro-thermal charcoal: identical with embodiment one；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 1g/
The dosage that adds of L adds the Fe that concentration is 600 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution, after taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, uses Phen to divide
Its Fe of light spectrphotometric method for measuring3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Percent reduction is 29%, sees
Fig. 3.
Embodiment seven:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: identical with embodiment one；
B. prepared by hydro-thermal charcoal: identical with embodiment one；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 1g/
The dosage that adds of L adds the Fe that concentration is 700 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution, after taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, uses Phen to divide
Its Fe of light spectrphotometric method for measuring3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Percent reduction is 25%, sees
Fig. 3.
Embodiment eight:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: identical with embodiment one；
B. prepared by hydro-thermal charcoal: identical with embodiment one；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 1g/
The dosage that adds of L adds the Fe that concentration is 800 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution, after taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, uses Phen to divide
Its Fe of light spectrphotometric method for measuring3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Percent reduction is 22%, sees
Fig. 3.
Embodiment nine:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: identical with embodiment one；
B. prepared by hydro-thermal charcoal: identical with embodiment one；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 1g/
The dosage that adds of L adds the Fe that concentration is 900 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution, after taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, uses Phen to divide
Its Fe of light spectrphotometric method for measuring3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Percent reduction is 20%, sees
Fig. 3.
In figure 3, from embodiment one～embodiment nine, along with Fe in solution3+Concentration from 100 mg/L to 900 mg/L,
Fe3+Percent reduction drops to 20% from 100%, it is seen that relatively low Fe3+Concentration be conducive to Fe3+Concentration is to Fe3+Reduction effect.
Embodiment ten:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: identical with embodiment one；
B. prepared by hydro-thermal charcoal: identical with embodiment one；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 2g/
The dosage that adds of L adds the Fe that concentration is 200 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution, after taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, uses Phen to divide
Its Fe of light spectrphotometric method for measuring3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Percent reduction is 80%.
Embodiment 11:
The present embodiment is essentially identical with embodiment one, is particular in that:
In the present embodiment, Ferric ion reduction method, comprise the following steps:
A. raw material prepares: identical with embodiment one；
B. prepared by hydro-thermal charcoal: identical with embodiment one；
C. reduction process: weigh the hydro-thermal biology powdered carbon of preparation in above-mentioned steps b, by hydro-thermal biology powdered carbon according to 4g/
The dosage that adds of L adds the Fe that concentration is 200 mg/L, pH=2 ± 0.13+In solution, carry out reduction reaction 120h, through reduction
Fe is obtained after reaction2+Solution, after taking detection the desired amount of the present embodiment reaction, solution carries out fast filtering, uses Phen to divide
Its Fe of light spectrphotometric method for measuring3+And Fe2+Concentration, by testing result comparing calculation, the Fe of the present embodiment3+Percent reduction is 97%.
In embodiment one, embodiment ten and embodiment 11, hydro-thermal biology powdered carbon add dosage when increasing to 4g/L,
Fe3+Percent reduction is substantially close to 100%.Hydro-thermal biology powdered carbon is joined Fe according to the dosage that adds of 1 ~ 4g/L3+In solution, Fe3+
Percent reduction is 60～97%, reaches the requirement of industrial high-efficiency application.
Above in conjunction with accompanying drawing, the embodiment of the present invention is illustrated, but the invention is not restricted to above-described embodiment, it is also possible to
The purpose of the innovation and creation according to the present invention makes multiple change, under all spirit according to technical solution of the present invention and principle
The change made, modifying, substitute, combine, simplify, all should be the substitute mode of equivalence, as long as meeting the goal of the invention of the present invention, only
Protection scope of the present invention is broadly fallen into without departing substantially from the know-why of Ferric ion reduction method of the present invention and inventive concept.
Claims (3)
1. a Ferric ion reduction method, it is characterised in that comprise the following steps:
A. raw material prepare: to collect carbon containing biomass be carried out, air-dry, then carry out 100 ~ 120 DEG C of drying, pulverizing,
Sieve, obtain the particle diameter carbon containing biomass dry powder less than 100 mesh；
B. prepared by hydro-thermal charcoal: the carbon containing biomass dry powder after sieving in above-mentioned steps a and water are according to w/v
For 1:(2 ~ 10) gram weight mix homogeneously with the ratio of milliliter volume and be placed in autoclave, more logical in autoclave
Sealing after nitrogen deoxygenation, the hydrothermal temperature controlled in autoclave is 100 ~ 300 DEG C, adds the reactant in autoclave
After heat 1 ~ 24h, in autoclave, take out hydrothermal carbonization product, and make its room temperature cool down, then hydrothermal carbonization product is used
Dehydrated alcohol and distilled water rinse to cleaning mixture pH constant repeatedly, refilter drying, then with 100 ~ 300 DEG C of activation 1 ~ 30min,
After grinding and sieving, obtain hydro-thermal biology powdered carbon again, store for future use；
C. reduction process: weigh in above-mentioned steps b the hydro-thermal biology powdered carbon of preparation, by hydro-thermal biology powdered carbon according to 0.1 ~
The dosage that adds of 10g/L adds the Fe that concentration is 100 ~ 900ppm, pH=1 ~ 33+In solution, reduction reaction 70 ~ 120h, through also
Fe is obtained after former reaction2+Solution.
Ferric ion reduction method the most according to claim 1, it is characterised in that: in above-mentioned steps b, control high pressure
Hydrothermal temperature in reactor is hydrothermal temperature 160-240 DEG C, and the reactant in autoclave is heated 2-6h；Activation temperature
For 200-240 DEG C, soak time is 5-10min.
Ferric ion reduction method the most according to claim 1, it is characterised in that: in above-mentioned steps c, hydro-thermal is raw
Thing powdered carbon joins Fe according to the dosage that adds of 1 ~ 4g/L3+In solution.
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| CN105084512A (en) * | 2015-08-12 | 2015-11-25 | 华中师范大学 | Method for promoting Fe(III)/H2O2 system to repair organic polluted water through biochar synthesized by composting products |
| CN109013693A (en) * | 2018-08-28 | 2018-12-18 | 上海大学 | The green restorative procedure of organic polluted soil |
| CN111333117A (en) * | 2020-01-22 | 2020-06-26 | 青岛农业大学 | Preparation of cupronickel type structure CuFeO2Method for preparing biochar composite material |
| CN114057279B (en) * | 2021-11-09 | 2023-12-26 | 广东石油化工学院 | Method for accelerating iron circulation by utilizing hydrothermal carbon to promote catalytic degradation of organic pollutants |
| CN116440859A (en) * | 2023-04-25 | 2023-07-18 | 上海大学 | Method for promoting biochar loaded zero-valent iron to efficiently degrade perfluorooctanoic acid by using hydrothermal alkali |
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