CN102247809A - Preparation method of bio-adsorbent with using camellia oleifera shell - Google Patents
Preparation method of bio-adsorbent with using camellia oleifera shell Download PDFInfo
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- CN102247809A CN102247809A CN 201010243982 CN201010243982A CN102247809A CN 102247809 A CN102247809 A CN 102247809A CN 201010243982 CN201010243982 CN 201010243982 CN 201010243982 A CN201010243982 A CN 201010243982A CN 102247809 A CN102247809 A CN 102247809A
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Abstract
The invention relates to a preparation method of a water treatment agent, in particular to a preparation method of a bio-adsorbent with using camellia oleifera shells. The preparation method comprises the following steps: mixing the camellia oleifera shells with the particle size of 500-600 mu m with a modifier according to the mass-to-volume ratio of 1 to 0.5-15, putting the mixture in a flask with three mouths, adding a catalyst with stirring, stirring for a modification reaction at the temperature of 30-100 DEG C, filtering and then washing the filter residue with distilled water until the filtrate is neutral, drying the filter residue at the temperature of 40-60 DEG C to constant weight to obtain the bio-adsorbent. The bio-adsorbent is applied for treating heavy metal waste water and dye waste water as the water treatment agent. Compared with the prior art, waste is utilized as raw material, so that the advantages of extensive sources, low cost, benefit for comprehensive utilization, and reduction of waste emissions are achieved; the preparation method has the advantages of simple technology, low cost, large adsorption capacity, and can be widely used for treating pollutant effluents with good water treatment results; and the reaction conditions are mild and easy to control, the steps of modification reaction are simple, and the equipment of the technology is few.
Description
Technical field
The present invention relates to a kind of preparation method of water treatment agent, particularly a kind of preparation method who prepares biological adsorption agent with oil-tea camellia husks.This biological adsorption agent is widely used in the improvement of effluent containing heavy metal ions.
Background technology
Heavy metal is the persistent pollutant that the class in the environment has potential hazard.In recent years, contain heavy metal wastewater thereby the mankind's living environment has been caused huge harm, heavy metal is discharged with waste water, even concentration is very little, also can cause public hazards, serious environment pollution, the heavy metal major part that enters water body changes in the water body bed mud by sedimentation and suction-operated, and the pollution rate that makes China's river,lake and reservior bed mud is up to 80.1%.Simultaneously, heavy metal enters water body, and water ecological setting is destroyed, and can by plants enriched and through food chain amplify step by step or directly by reference water enter human body, be detrimental to health.
The method of removing heavy metal in the waste water mainly contains methods such as redox, chemical precipitation, ion-exchange, absorption, film separation and removes, wherein be adsorbed in ion-exchange and have the treatment effeciency height, easy operating, low power consumption and other advantages are the common methods of heavy metal containing wastewater treatment.
In recent years, the living beings sorbing material causes domestic and international researcher's attention, and bagasse, industrial hemp bar core, corncob, furfural dregs etc. have been carried out a large amount of research.The development and the application of low-cost bio adsorbent obtain remarkable break-throughs, and modification agriculture and forestry organic waste material etc. demonstrates excellent adsorptivity price ratio.
Oil tea and oil palm, olive and coconut also are called the world four big woody edible oil materials plants.Oil tea is the distinctive woody oleiferous plants of China, and according to statistics, more than 347 ten thousand hectares of the existing oil tea areas in the whole nation are produced tea seed 56,600,000,000 kg per year, about 30,000,000,000 kg of oil-tea camellia husks.But a large amount of oil-tea camellia husks is taken as fuel or is used as fertilizer, the great wasting of resources and environmental pollution have been caused, if it is prepared into biological adsorption agent, it will be a kind of important materials of handling heavy metal wastewater thereby, can improve simultaneously the benefit of oil tea plantation, have good economy and Significance for Environment.Oil-tea camellia husks is used to prepare the existing a large amount of research report of active carbon both at home and abroad, but directly prepares biological adsorption agent by modification, yet there are no report in the domestic and foreign literature database at present.
Summary of the invention
Utilize at oil-tea camellia husks that approach is single, added value is low and the high inadequately deficiency of present biological adsorption agent cost performance, a kind of product stability is good, adsorption capacity is big, applied widely oil-tea camellia husks biological adsorption agent and preparation technology thereof are provided.
To achieve these goals, the present invention has adopted following technical scheme:
The oil-tea camellia husks that with particle diameter is 500～600um mixes by mass volume ratio 1: 0.5～15 with modifier, places there-necked flask, stirs to add catalyst, at 30～100 ℃ of following stirring reaction 0.5～3h; Filter, wash filter residue with distilled water, be neutral to filtrate, filter residue is dried to constant weight under 40～60 ℃, promptly get the oil-tea camellia husks biological adsorption agent.
Described modifier is a kind of in formaldehyde, glyoxal or the glutaraldehyde, or two kinds of composite modifiers that arbitrary proportion is formed wherein.
Described catalyst is that concentration is 5～15% hydrochloric acid, 1～10% sulfuric acid or 1～8% nitric acid, and catalyst amount is 0.5～2 times of oil-tea camellia husks quality.
Adsorbent of the present invention compared with prior art has following advantage:
(1) the present invention utilizes the discarded object oil-tea camellia husks to be the preparation raw material, and wide material sources are cheap; Help the comprehensive utilization of oil-tea camellia husks, reduce the discharging of refuse.
(2) preparation technology of the present invention is simple, and cost is lower, and adsorption capacity is big, can be widely used in the improvement of pollutant effluents, and has water treatment effect preferably.
(3) reaction condition gentleness of the present invention is easy to control, and modification procedure is simple, and process equipment is few, easy operating.
The specific embodiment
Below by embodiment, technical scheme of the present invention is done further specific description.
The present invention is as follows to the measuring method of dyestuff adsorption capacity: the 0.1g adsorbent is joined 50ml contain in the solution of methylene blue, behind the 24h (adsorption equilibrium) that vibrates under 25 ℃ of conditions, measure the concentration of methylene blue in the solution, calculate adsorption capacity according to following formula.
Q
e＝(C
0-C
e)V/W(mg/g)
Wherein: Q
eBe adsorption capacity; C
0Be methylene blue concentration (mg/L) before adsorbing; C
eConcentration (mg/L) for methylene blue after the adsorption equilibrium; W is adsorbent dry weight (g); V is the volume (L) of methylene blue solution.
The present invention is as follows to the measuring method of adsorption of metal ions capacity: the 0.1g adsorbent is joined in the solution of 50ml metal ion, behind the 24h (adsorption equilibrium) that vibrates under 25 ℃ of conditions, measure GOLD FROM PLATING SOLUTION and belong to ion concentration, calculate adsorption capacity according to following formula.
Q
e＝(C
0-C
e)V/W(mg/g)
Wherein: Q
eBe adsorption capacity; C
0For adsorbing preceding concentration of metal ions (mg/L); C
eConcentration (mg/L) for metal ion after the adsorption equilibrium; W is adsorbent dry weight (g); V is the volume (L) of metal ion solution.Embodiment 1
The oil-tea camellia husks that takes by weighing the 200g particle diameter and be 500～600um adds 200ml concentration and is 20% formaldehyde in there-necked flask, after stirring, adding 120ml concentration and be 10% hydrochloric acid is catalyst, at 70 ℃ of following stirring reaction 2h; Filter, wash filter residue with distilled water, be neutral to filtrate, filter residue is dried to constant weight under 50 ℃, promptly get the oil-tea camellia husks biological adsorption agent.This adsorbent is 196.5mg/g to the adsorbance of methylene blue, is 178mg/g to the adsorbance of hexavalent chromium, is 56mg/g to the adsorbance of copper ion, is 135mg/g to the adsorbance of lead ion.
Embodiment 2
The oil-tea camellia husks that takes by weighing the 200g particle diameter and be 500～600um adds 500ml concentration and is 5% glutaraldehyde in there-necked flask, after stirring, adding 150ml concentration and be 10% hydrochloric acid is catalyst, at 70 ℃ of following stirring reaction 2h; Filter, wash filter residue with distilled water, be neutral to filtrate, filter residue is dried to constant weight under 50 ℃, promptly get the oil-tea camellia husks biological adsorption agent.This adsorbent is 183.7mg/g to the adsorbance of methylene blue, is 152mg/g to the adsorbance of hexavalent chromium, is 51mg/g to the adsorbance of copper ion, is 115mg/g to the adsorbance of lead ion.
Embodiment 3
The oil-tea camellia husks that takes by weighing the 200g particle diameter and be 500～600um adds 500ml concentration and is 10% glyoxal in there-necked flask, after stirring, adding 200ml concentration and be 10% hydrochloric acid is catalyst, at 70 ℃ of following stirring reaction 2h; Filter, wash filter residue with distilled water, be neutral to filtrate, filter residue is dried to constant weight under 50 ℃, promptly get the oil-tea camellia husks biological adsorption agent.This adsorbent is 137.6mg/g to the adsorbance of methylene blue, is 165mg/g to the adsorbance of hexavalent chromium, is 49mg/g to the adsorbance of copper ion, is 105mg/g to the adsorbance of lead ion.
Embodiment 4
The oil-tea camellia husks that takes by weighing the 200g particle diameter and be 500～600um adds 1000ml concentration and is 5% formaldehyde in there-necked flask, after stirring, adding 250ml concentration and be 3% hydrochloric acid is catalyst, at 50 ℃ of following stirring reaction 2.5h; Filter, wash filter residue with distilled water, be neutral to filtrate, filter residue is dried to constant weight under 50 ℃, promptly get the oil-tea camellia husks biological adsorption agent.This adsorbent is 227.8mg/g to the adsorbance of methylene blue, is 189mg/g to the adsorbance of hexavalent chromium, is 62mg/g to the adsorbance of copper ion, is 123mg/g to the adsorbance of lead ion.
Embodiment 5
The oil-tea camellia husks that takes by weighing the 100g particle diameter and be 500～600um adds 1000ml concentration and is 8% glutaraldehyde in there-necked flask, after stirring, adding 150ml concentration and be 5% sulfuric acid is catalyst, at 60 ℃ of following stirring reaction 1.5h; Filter, wash filter residue with distilled water, be neutral to filtrate, filter residue is dried to constant weight under 50 ℃, promptly get the oil-tea camellia husks biological adsorption agent.This adsorbent is 179.5mg/g to the adsorbance of methylene blue, is 108mg/g to the adsorbance of hexavalent chromium, is 46mg/g to the adsorbance of copper ion, is 97mg/g to the adsorbance of lead ion.
Embodiment 6
The oil-tea camellia husks that takes by weighing the 100g particle diameter and be 500～600um is in there-necked flask, add 1000ml concentration and be 5% formaldehyde and 500ml concentration and be 8% glutaraldehyde, after stirring, adding 80ml concentration and be 12% hydrochloric acid is catalyst, at 50 ℃ of following stirring reaction 1.5h; Filter, wash filter residue with distilled water, be neutral to filtrate, filter residue is dried to constant weight under 50 ℃, promptly get the oil-tea camellia husks biological adsorption agent.This adsorbent is 185.7mg/g to the adsorbance of methylene blue, is 123mg/g to the adsorbance of hexavalent chromium, is 49mg/g to the adsorbance of copper ion, is 107mg/g to the adsorbance of lead ion.
Embodiment 7
The oil-tea camellia husks that takes by weighing the 200g particle diameter and be 500～600um adds 500ml concentration and is 10% glyoxal in there-necked flask, after stirring, adding 150ml concentration and be 3% nitric acid is catalyst, at 70 ℃ of following stirring reaction 1h; Filter, wash filter residue with distilled water, be neutral to filtrate, filter residue is dried to constant weight under 50 ℃, promptly get the oil-tea camellia husks biological adsorption agent.This adsorbent is 176.6mg/g to the adsorbance of methylene blue, is 162mg/g to the adsorbance of hexavalent chromium, is 52mg/g to the adsorbance of copper ion, is 127mg/g to the adsorbance of lead ion.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (6)
1. the preparation method of an oil-tea camellia husks biological adsorption agent, it is characterized in that with particle diameter being that the oil-tea camellia husks of 500～600um mixes by mass volume ratio 1: 0.5～15 with modifier, place there-necked flask, stir and add catalyst, under 30～100 ℃, stir and carry out modified-reaction, filter the back and be neutral with distilled water washing filter residue to filtrate, filter residue is dried to constant weight under 40～60 ℃, get the oil-tea camellia husks biological adsorption agent.
2. the preparation method of oil-tea camellia husks biological adsorption agent according to claim 1 is characterized in that described modifier is a kind of in formaldehyde, glyoxal or the glutaraldehyde, or two kinds of composite modifiers that arbitrary proportion is formed wherein.
3. the preparation method of oil-tea camellia husks biological adsorption agent according to claim 1, it is characterized in that described catalyst is that concentration is 5～15% hydrochloric acid, 1～10% sulfuric acid or 1～8% nitric acid, catalyst amount is 0.5～2 times of oil-tea camellia husks quality.
4. the preparation method of oil-tea camellia husks biological adsorption agent according to claim 1 is characterized in that the described modified-reaction time is 0.5～3h.
5. the preparation method of oil-tea camellia husks biological adsorption agent according to claim 1 is characterized in that described modified-reaction temperature is 50～100 ℃.
6. the preparation method of oil-tea camellia husks biological adsorption agent according to claim 1 is characterized in that described oil-tea camellia husks biological adsorption agent uses in heavy metal wastewater thereby, dye wastewater treatment as water treatment agent.
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Cited By (16)
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|---|---|---|---|---|
| CN102784621A (en) * | 2012-08-29 | 2012-11-21 | 西南科技大学 | Method for preparing biomass adsorption material based on modified rice husks |
| CN103203218A (en) * | 2012-05-30 | 2013-07-17 | 湖南大三湘油茶科技有限公司 | Oil processing adsorbent and preparation method thereof |
| CN103272568A (en) * | 2013-05-29 | 2013-09-04 | 浙江大学宁波理工学院 | Method for preparing bifunctional modified cellulose adsorbing agent from peanut shells and application of method |
| CN103357381A (en) * | 2013-07-18 | 2013-10-23 | 华南理工大学 | Method for preparation of bio-adsorbent by modifying tea residue and application of bio-adsorbent |
| CN104525115A (en) * | 2014-12-25 | 2015-04-22 | 东华大学 | Preparation method for environment-friendly advanced water treatment agent by combining carbon nano tube and WO3 |
| CN104645941A (en) * | 2013-11-15 | 2015-05-27 | 北京林业大学 | Preparation method and use of white-rot fungus mycelium biological adsorbent |
| CN105289522A (en) * | 2015-11-04 | 2016-02-03 | 梅庆波 | Preparation method for denitriding and dephosphorizing adsorbing agent for chimney waste gas of factory |
| CN105440225A (en) * | 2015-12-21 | 2016-03-30 | 福建师范大学 | Preparation method of polyphenol biomass flocculating agent |
| CN105883956A (en) * | 2014-09-29 | 2016-08-24 | 广西科学院 | Method for removing heavy metal in water by using dried sargasso |
| CN107159141A (en) * | 2017-06-05 | 2017-09-15 | 福建师范大学 | A kind of method that utilization oil-tea camellia husks grafting TGA prepares metal ion adsorbent |
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| CN107670647A (en) * | 2017-09-30 | 2018-02-09 | 福建省林业科学研究院 | A kind of method that adsorbent for heavy metal is prepared using oil-tea camellia husks |
| CN107694526A (en) * | 2017-09-30 | 2018-02-16 | 福建省林业科学研究院 | Adsorbent prepared by a kind of oil-tea camellia husks extract and preparation method thereof |
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| CN103203218A (en) * | 2012-05-30 | 2013-07-17 | 湖南大三湘油茶科技有限公司 | Oil processing adsorbent and preparation method thereof |
| CN103203218B (en) * | 2012-05-30 | 2015-07-22 | 湖南大三湘油茶科技有限公司 | Oil processing adsorbent and preparation method thereof |
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| CN103272568A (en) * | 2013-05-29 | 2013-09-04 | 浙江大学宁波理工学院 | Method for preparing bifunctional modified cellulose adsorbing agent from peanut shells and application of method |
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| CN107670647B (en) * | 2017-09-30 | 2020-05-22 | 福建省林业科学研究院 | Method for preparing heavy metal ion adsorbent by using camellia oleifera shells |
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Application publication date: 20111123 |