CN109647351A - A kind of bagasse load hydrogen iron oxide adsorbent and its preparation method and application - Google Patents
A kind of bagasse load hydrogen iron oxide adsorbent and its preparation method and application Download PDFInfo
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- CN109647351A CN109647351A CN201910013033.2A CN201910013033A CN109647351A CN 109647351 A CN109647351 A CN 109647351A CN 201910013033 A CN201910013033 A CN 201910013033A CN 109647351 A CN109647351 A CN 109647351A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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Abstract
The invention discloses a kind of preparation method of bagasse load hydrogen iron oxide adsorbent and its in the application of processing phosphate in waste water, by the way that the bagasse of crushing is added in iron salt solutions, then lye is added into gained mixed liquor and controls the pH value of gained reaction solution, reaction obtains the sorbent material of bagasse load iron hydroxide.The present invention is using bagasse and iron salt solutions as primary raw material, the building for realizing payload and bagasse porous structure of the iron hydroxide active component on bagasse can be synchronized, gained adsorbent adsorption capacity is big, it is adaptable, the drawbacks such as adsorption capacity is not strong, is not easily recycled can effectively be evaded when bagasse and iron hydroxide is used alone, there is important research and application value；And the preparation method being related to is simple and convenient to operate, it is environmental-friendly, and can realize the resource utilization of bagasse, there is important economic benefit and environmental benefit.
Description
Technical field
The invention belongs to the interdisciplinary fields such as chemistry, biology, material, environmental science, and in particular to a kind of bagasse is negative
It carries the preparation method of iron hydroxide adsorbent and its handles the application of phosphate in waste water.
Background technique
Phosphorus is one of essential nutrient of animal and plant growth, but excessive phosphorus easily causes water eutrophication.
From industry, life phosphate-containing waste water is discharged into rivers,lakes and seas through a variety of ways, and the waters poor in mobility, non-
It often is easy to produce wawter bloom or red tide phenomenon, causes a large amount of aquatic animals and plants dead, causes serious environmental pollution.Place at present
Managing phosphatic method in water body includes the methods of physical method, chemical method, ion-exchange, membrane technology method, biosorption process.Its
Middle biosorption process because it have prepare it is simple, at low cost, be easy promote, adsorption effect it is good, it is nontoxic, not will cause secondary dirt
The research hotspot of dye, easy the advantages that being biodegradable as this field.
Bagasse is the Main By product of sugar manufacturing industry, and only south China produces 7000000 tons of bagasse per year.China sugarcane at present
Slag is mainly used for papermaking, burns even directly discarding, not only causes a large amount of wasting of resources, but also will cause environmental pollution.This
Outside, iron hydroxide is used alone and adsorbs phosphate, reunion is be easy to cause during preparation, and adsorption effect is bad and difficult
With recycling.Therefore, further exploring adsorbent cheap, that absorption phosphate effect is good and preparation method thereof has important research
And application value.
Summary of the invention
The purpose of the present invention is to provide a kind of bagasse load hydrogen iron oxide adsorbent and its processing phosphate in waste water
Application, the present invention is effectively compound by carrying out bagasse and iron hydroxide, and gained adsorbent material can effectively adsorb waste water
The phosphate of middle higher concentration can also solve bagasse bring environmental pollution, realize the resource utilization of bagasse；And it is related to
Preparation method it is simple, raw material is cheap and easy to get, have important economic benefit and environmental benefit, have a extensive future.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of preparation method of bagasse load hydrogen iron oxide adsorbent, it includes the following steps:
1) bagasse pre-processes；The bagasse after squeezing the juice will be collected, washed, boiling filtering repeats boiling filtering step
It is 3-4 times rapid, it to remove soluble saccharide and other impurities, then is washed, further removes the impurity such as carbohydrate, be filtered dry, dry,
It crushes, collects 100-200 mesh bagasse powder, it is spare；
2) bagasse powder is added in iron salt solutions, is uniformly mixed, obtains mixed liquor I；
3) lye is added into mixed liquor I, adjusts the pH value of gained mixed liquor to 4.5-5.0, carries out ultrasonic agitation reaction；
4) reaction solution obtained by step 3) is centrifuged, collects gained sediment, is washed, dried, milled, i.e.,
Obtain bagasse load hydrogen iron oxide adsorbent.
In above scheme, dry matter content is 95-99%, each component and its shared quality percentage in the bagasse powder
Than including: cellulose 43-51%, hemicellulose 24-32%, lignin 20-27%, thick protein 1.5-2.3%, crude fat
0.2-0.8%, coarse ash 0.9-1.5%.
In above scheme, the pH value of the iron salt solutions is 1.4-2.2.
In above scheme, the molysite is ferric nitrate or iron chloride etc..
In above scheme, the mass ratio of the source of iron and bagasse powder is (1.5-10): 1.
In above scheme, the lye is the Na that concentration is 3-5wt%2CO3Or NaHCO3Solution.
In above scheme, baking step described in step 1) is the 40-50 DEG C of drying 24-48h in electric drying oven with forced convection.
In above scheme, the partial size of bagasse powder is 100-200 mesh.
In above scheme, the concentration of the iron salt solutions is 7-49.55mmol/L.
In above scheme, the ultrasonic agitation reaction time is 20-30min, ultrasonic power 80-250w.
In above scheme, the addition flow velocity of the lye is 5-8mL/min.
According to bagasse load hydrogen iron oxide adsorbent prepared by above scheme, it is applied to the place of phosphate in waste water
Reason is easily recycled, it can be achieved that phosphatic efficient absorption, is suitble to promote and apply.
Mechanism of the invention are as follows: ferric ion is dispersed in by bagasse surface using carrying method, due to Fe
(NO3)3、FeCl3It is relatively strong (pH value 1.4-2.2) Deng the solution acidic formed in process for preparation, it is unfavorable for loading, the present invention adopts
Dilute Na is slowly added dropwise with constant flow pump2CO3, using ferric nitrate, iron chloride itself acidity in aqueous solution and Na2CO3Reaction produces
Raw carbon dioxide gas, while the pH value of pH meter monitoring mixed solution and combination ultrasonic agitation processing, it is dry by freezing after centrifugation
Dry to obtain bagasse load hydrogen iron oxide adsorbent powder, synchronous realization iron hydroxide active component is effective negative on bagasse
The building of load and bagasse porous structure.
Compared with prior art, the invention has the benefit that
1) present invention is using bagasse and iron salt solutions as primary raw material, by introducing Na thereto2CO3Or NaHCO3Solution
And the pH value of gained reaction solution is controlled, the payload and sugarcane for realizing iron hydroxide active component on bagasse can be synchronized
The building of slag porous structure, gained adsorbent adsorption capacity is big, adaptable, can effectively evade and bagasse and hydrogen is used alone
The drawbacks such as adsorption capacity is not strong when iron oxide, is not easily recycled, have important research and application value.
2) preparation method of the present invention is simple and convenient to operate, environmental-friendly, is suitble to promote and apply.
3) raw material sources of the present invention are extensive, at low cost, it is cheap and easy to get, it can be achieved that bagasse resource utilization,
With important economic benefit and environmental benefit.
Detailed description of the invention
Fig. 1 is that the SEM of 1 gained bagasse load hydrogen iron oxide adsorbent of the embodiment of the present invention schemes.
Fig. 2 is that 1 gained bagasse load hydrogen iron oxide adsorbent of the embodiment of the present invention adsorbs the SEM figure after phosphate.
Fig. 3 is the EDS picture of 1 gained bagasse load hydrogen iron oxide adsorbent of the embodiment of the present invention.
Fig. 4 is that 1 gained bagasse load hydrogen iron oxide adsorbent of the embodiment of the present invention adsorbs the EDS picture after phosphate.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
In following embodiment, the pre-treatment step in the bagasse of use includes the following steps: to collect sweet after squeezing the juice
Bagasse is washed, and boiling filtering repeats boiling filtration step 3-4 times, to remove soluble saccharide and other impurities, then into
Row washing, further removes the impurity such as carbohydrate, is filtered dry, dries, crushes, and collects 100-200 mesh bagasse powder, spare；Gained
The dry matter content of bagasse powder is 98.7wt%, and each component and its shared mass percent include: cellulose 46.1%, half
Cellulose 25.4%, lignin 23.5%, thick protein 1.2%, crude fat 0.7%, coarse ash 1.3%.
Embodiment 1
A kind of bagasse load hydrogen iron oxide adsorbent, preparation method include the following steps:
1) 1.0g bagasse powder is added to the Fe (NO that 500ml concentration is 37.1mmol/L3)3(initial pH value is solution
1.51) it in, is put into ultrasonic drilling machine, and is stirred solution 30min with mechanical agitator, obtain mixed liquor I；
2) under pH meter monitoring, the Na that concentration is 5wt% is added in the mixed liquor I obtained by as constant flow pump2CO3Solution, control
Flow velocity processed stops Na when the pH of gained mixed liquor is to 5 in 6.25mL/min2CO3The addition of solution, continuation are in power
Ultrasound and stirring 30min under conditions of 150w；
3) it is centrifuged 20min under the conditions of 4000r/min, collects sediment, and clean sediment for several times with a small amount of distilled water,
Freeze-drying, mills to get bagasse load hydrogen iron oxide adsorbent.
The present embodiment products therefrom is applied to the phosphate in removal waste water, specific steps include: using ammonium molybdate point
Phosphate in light Spectrophotometric Determination solution is the simulated wastewater (sodium radio-phosphate,P-32 solution) of 25mg/L with 50ml concentration, and 0.04g is added
Bagasse load hydrogen iron oxide adsorbent, shaking table 250r/min shake 2h, stand 0.5h, take supernatant detection phosphatic dense
Degree；The result shows that phosphate removal rate is up to 99.1%.
Fig. 1, Fig. 2 are respectively bagasse load hydrogen iron oxide adsorbent obtained by the present embodiment before and after adsorbing phosphate
SEM figure, the results showed that the surface Fig. 1 shows that iron hydroxide is supported on bagasse table well with the presence of a large amount of tiny particles contents
Face, Fig. 2 still remain tiny particles content, though whether cannot intuitively find out has Phosphateadsorption to show that EDS can be passed through at it
Characterize secondary proof.
Fig. 3,4 are respectively EDS of the bagasse load hydrogen iron oxide adsorbent obtained by the present embodiment before and after adsorbing phosphate
Figure, the results showed that phosphorus content is only 0.20wt% before adsorbing, and after absorption, phosphorus content reaches 2.83wt%, illustrates phosphate radical
It can be good at being adsorbed in bagasse load hydrogen iron oxide adsorbent.
Embodiment 2
A kind of bagasse load hydrogen iron oxide adsorbent, preparation method include the following steps:
1) 1.0g bagasse powder is added to the Fe (NO that 500ml concentration is 49.5mmol/L3)3(initial pH value in solution
1.42), to be put into ultrasonic drilling machine, and it is stirred solution 30min with mechanical agitator, obtains mixed liquor I；
2) under pH meter monitoring, the Na that concentration is 4wt% is added in the mixed liquor I obtained by as constant flow pump2CO3Solution, control
Flow velocity processed stops Na when the pH of gained mixed liquor is to 4.5 in 5mL/min2CO3The addition of solution, continuation are in power
Ultrasound and stirring 30min under conditions of 120w；
3) it is centrifuged 20min under the conditions of 4000r/min, collects sediment, and clean sediment for several times with a small amount of distilled water,
Freeze-drying, mills to get bagasse load hydrogen iron oxide adsorbent.
The present embodiment products therefrom is applied to the phosphate in removal waste water, specific steps include: using ammonium molybdate point
Phosphate in light Spectrophotometric Determination solution is the simulated wastewater (sodium radio-phosphate,P-32 solution) of 25mg/L with 50ml concentration, and 0.04g is added
Bagasse load hydrogen iron oxide adsorbent, shaking table 250r/min shake 2h, stand 0.5h, take supernatant detection phosphatic dense
Degree；The result shows that phosphate removal rate is up to 99.8%.
Embodiment 3
A kind of bagasse load hydrogen iron oxide adsorbent, preparation method include the following steps:
1) 1.0g bagasse powder is added to the Fe (NO that 500ml concentration is 49.5mmol/L3)3(initial pH value in solution
1.42), to be put into ultrasonic drilling machine, and it is stirred solution 30min with mechanical agitator, obtains mixed liquor I；
2) under pH meter monitoring, the NaHCO that concentration is 4wt% is added in the mixed liquor I obtained by as constant flow pump3Solution,
Coutroi velocity stops Na when the pH of gained mixed liquor is to 4.5 in 6.25mL/min2CO3The addition of solution continues to continue
Ultrasound and stirring 30min under conditions of power is 150w；
3) it is centrifuged 20min under the conditions of 4000r/min, collects sediment, and clean sediment for several times with a small amount of distilled water,
Freeze-drying, mills to get bagasse load hydrogen iron oxide adsorbent.
The present embodiment products therefrom is applied to the phosphate in removal waste water, specific steps include: using ammonium molybdate point
Phosphate in light Spectrophotometric Determination solution is with the 50ml concentration that pH is respectively 2,3,4,5,6,7,8,9,10,11,12
0.04g bagasse load hydrogen iron oxide adsorbent, shaking table 250r/min vibration is added in the simulated wastewater (sodium radio-phosphate,P-32 solution) of 25mg/L
2h is shaken, 0.5h is stood, supernatant is taken to detect phosphatic concentration；The result shows that phosphate removal rate be respectively 99.7%,
99.8%, 99.6%, 99.3%, 99.6%, 99.6%, 99.3%, 98.7%, 93.4%, 50.2%, 33.4%.
The above results show that the adsorption capacity of gained bagasse load hydrogen iron oxide adsorbent of the invention is big, and to waste water
The wide adaptability of pH value of solution condition.
Comparative example 1
A kind of bagasse load hydrogen iron oxide adsorbent, preparation method include the following steps:
1) 1.0g bagasse powder is added to the Fe (NO that 500ml concentration is 37.1mmol/L3)3(initial pH value in solution
1.51), to be put into ultrasonic drilling machine, and it is stirred solution 30min with mechanical agitator, obtains mixed liquor I；
2) under pH meter monitoring, the NaHCO that concentration is 6.25wt% is added in the mixed liquor I obtained by as constant flow pump3It is molten
Liquid, coutroi velocity stop Na when the pH of gained mixed liquor is to 2 in 5mL/min2CO3The addition of solution, continuation are in power
Ultrasound and stirring 30min under conditions of 180w；
3) it is centrifuged 20min under the conditions of 4000r/min, collects sediment, and clean sediment for several times with a small amount of distilled water,
Freeze-drying, mills to get bagasse load hydrogen iron oxide adsorbent.
The present embodiment products therefrom is applied to the phosphate in removal waste water, specific steps include: using ammonium molybdate point
Phosphate in light Spectrophotometric Determination solution is the simulated wastewater (sodium radio-phosphate,P-32 solution) of 25mg/L with 50ml concentration, and 0.04g is added
Bagasse load hydrogen iron oxide adsorbent, shaking table 250r/min shake 2h, stand 0.5h, take supernatant detection phosphatic dense
Degree；The result shows that the adsorbent is to phosphate almost without adsorption effect.
Comparative example 2
A kind of bagasse load hydrogen iron oxide adsorbent, preparation method include the following steps:
1) 1.0g bagasse powder is added to the Fe (NO that 500ml concentration is 49.5mmol/L3)3(initial pH value in solution
1.42), to be put into ultrasonic drilling machine, and it is stirred solution 30min with mechanical agitator, obtains mixed liquor I；
2) under pH meter monitoring, the Na that concentration is 4wt% is added in the mixed liquor I obtained by as constant flow pump2CO3Solution, control
Flow velocity processed stops Na when the pH of gained mixed liquor is to 7 in 5mL/min2CO3The addition of solution continues in power to be 200w
Under conditions of ultrasound and stirring 30min；
3) it is centrifuged 20min under the conditions of 4000r/min, collects sediment, and clean sediment for several times with a small amount of distilled water,
Freeze-drying, mills to get bagasse load hydrogen iron oxide adsorbent.
The present embodiment products therefrom is applied to the phosphate in removal waste water, specific steps include: using ammonium molybdate point
Phosphate in light Spectrophotometric Determination solution is the simulated wastewater (sodium radio-phosphate,P-32 solution) of 25mg/L with 50ml concentration, and 0.04g is added
Bagasse load hydrogen iron oxide adsorbent, shaking table 250r/min shake 2h, stand 0.5h, take supernatant detection phosphatic dense
Degree；The result shows that phosphate removal rate is up to 9.6%.
Each raw material cited by the present invention can realize that the bound value of the present invention and each raw material, interval value can
Realize the present invention；Embodiment numerous to list herein.The bound value of technological parameter of the invention, interval value can realize this
Invention, embodiment numerous to list herein.
Claims (10)
1. a kind of preparation method of bagasse load hydrogen iron oxide adsorbent, which is characterized in that it includes the following steps:
1) bagasse pre-processes；The bagasse after squeezing the juice will be collected, is washed, boiling filtering, then washed, dried, powder
It is broken, obtain bagasse powder；
2) bagasse powder is added in iron salt solutions, is uniformly mixed, obtains mixed liquor I；
3) lye is added into mixed liquor I, adjusts the pH value of gained mixed liquor to 4.5-5.0, carries out ultrasonic agitation reaction；
4) reaction solution obtained by step 3) is centrifuged, collects gained sediment, is washed, dried to get bagasse
Load hydrogen iron oxide adsorbent.
2. preparation method according to claim 1, which is characterized in that dry matter content is 95- in the bagasse powder
99%, each component and its shared mass percent include: cellulose 43-51%, hemicellulose 24-32%, lignin 20-
27%, thick protein 1.5-2.3%, crude fat 0.2-0.8%, coarse ash 0.9-1.5%.
3. preparation method according to claim 1, which is characterized in that the pH value of the iron salt solutions is 1.4-2.2.
4. preparation method according to claim 1, which is characterized in that the mass ratio of the molysite and bagasse powder is
(1.5-10):1。
5. preparation method according to claim 1, which is characterized in that the lye is the Na that concentration is 3-5wt%2CO3Or
NaHCO3Solution.
6. preparation method according to claim 1, which is characterized in that the concentration of the iron salt solutions is 7-49.55mmol/
L。
7. preparation method according to claim 1, which is characterized in that the ultrasonic agitation reaction time is 20-30min.
8. preparation method according to claim 1, which is characterized in that the addition flow velocity of the lye is 5-8mL/min.
9. bagasse load hydrogen iron oxide adsorbent made from any one of the claim 1-8 preparation method.
10. the application of the processing phosphate in waste water of bagasse load hydrogen iron oxide adsorbent described in claim 9.
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| CN110314655A (en) * | 2019-06-03 | 2019-10-11 | 武汉工程大学 | A kind of bagasse load zeroth order iron adsorbent and its preparation method and application |
| CN111229171A (en) * | 2020-01-19 | 2020-06-05 | 武汉工程大学 | Straw-loaded MOF material adsorbent and preparation method and application thereof |
| CN113648976A (en) * | 2021-09-08 | 2021-11-16 | 赣州晶鑫新材料有限公司 | Preparation method of biochar for efficiently adsorbing carbon dioxide |
| CN113926422A (en) * | 2020-07-13 | 2022-01-14 | 广西大学 | Preparation and application of magnetic bagasse carbon-loaded ferrihydrite composite adsorbent |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110314655A (en) * | 2019-06-03 | 2019-10-11 | 武汉工程大学 | A kind of bagasse load zeroth order iron adsorbent and its preparation method and application |
| CN110314655B (en) * | 2019-06-03 | 2022-05-10 | 武汉工程大学 | Bagasse-loaded zero-valent iron adsorbent and preparation method and application thereof |
| CN111229171A (en) * | 2020-01-19 | 2020-06-05 | 武汉工程大学 | Straw-loaded MOF material adsorbent and preparation method and application thereof |
| CN111229171B (en) * | 2020-01-19 | 2022-05-10 | 武汉工程大学 | Straw-loaded MOF material adsorbent and preparation method and application thereof |
| CN113926422A (en) * | 2020-07-13 | 2022-01-14 | 广西大学 | Preparation and application of magnetic bagasse carbon-loaded ferrihydrite composite adsorbent |
| CN113648976A (en) * | 2021-09-08 | 2021-11-16 | 赣州晶鑫新材料有限公司 | Preparation method of biochar for efficiently adsorbing carbon dioxide |
| CN113648976B (en) * | 2021-09-08 | 2023-11-28 | 云南铂鑫环保技术有限公司 | Preparation method of biochar capable of efficiently adsorbing carbon dioxide |
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| CN109647351B (en) | 2022-10-21 |
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