CN104437413A - Method of preparing bio-adsorbent - Google Patents
Method of preparing bio-adsorbent Download PDFInfo
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- CN104437413A CN104437413A CN201410827759.7A CN201410827759A CN104437413A CN 104437413 A CN104437413 A CN 104437413A CN 201410827759 A CN201410827759 A CN 201410827759A CN 104437413 A CN104437413 A CN 104437413A
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- adsorption agent
- biological adsorption
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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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- 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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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
-
- 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
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A method of preparing a bio-adsorbent relates to the bio-adsorbent and comprises the steps: cleaning, drying, grinding and filtering raw biomass materials to obtain biomass powder; mixing citric acid and the biomass powder, soaking, heating and stirring to obtain solid-liquid mixture; performing suction filtration to the obtained solid-liquid mixture and collecting filtrate; mixing the filtrate and chitosan, heating, stirring, adjusting the pH value to be 8-10, separating solids, continuously stirring, cooling, performing suction filtration, washing to be neutral and obtaining neutral filter residues; drying and grinding the neutral filter residues to obtain the bio-adsorbent. The bio-adsorbent can be applied to the preparation of the bio-adsorbent for heavy metals and dyeing waste water. The preparation method is simple in operation and wide in applicable range; and the waste acid treatment liquid of various agricultural and forestry residue biomasses can be used for preparing the low-price adsorbent available for heavy metals and dyeing waste water by utilizing the preparation method provided by the invention.
Description
Technical field
The present invention relates to biological adsorption agent, especially relate to the method for the waste liquid of the modified generation of living beings acid for the preparation of biological adsorption agent.
Background technology
Since 20th century, along with the development of modern industry, heavy metal and dyestuff have become great environmental problem urgently to be resolved hurrily to the pollution of water resource.In natural water body, content of beary metal is little, and the heavy metal in polluted water is mainly from industrial departments such as mining, plating, chemical industry.Excessive heavy metal, at human body cylinder accumulation, can cause vomiting, have a headache, dizzy, even life danger of having difficulty in breathing; Excessive heavy metal also can endanger the normal growth of most plants, destroys the osmotic adjustment of aquatic animal.According to estimates, have 4 ~ 80,000 tons of dyestuffs to enter in rivers and lakes, sea and the surface water as waste water in the annual dyestuff process in the whole world, waste water from dyestuff has the features such as COD is high, complicated component, difficult degradation, and carcinogenicity is high.
At present, heavy metal containing wastewater treatment technology mainly contains chemical precipitation method, electrolysis, ion-exchange, membrane separation process etc.; Dye waste water treatment method mainly contains flocculence, oxidizing process, biological treatment, membrane separation process etc.But, the heavy metal of these method process low quality concentration or the efficiency of waste water from dyestuff is lower, processing cost is higher, and easily cause more unmanageable secondary pollution.Based on this, absorption method becomes study hotspot with the advantage of its high efficiency, low cost.
All organism or derivatives thereofs with adsorption capacity are all called biological adsorption agent.Due to living beings there is abundance, enormous amount, the advantage such as renewable and the regeneration period is short, active group is abundant, be widely used in the process of heavy metal and waste water from dyestuff in recent years.In recent years, biological adsorption agent obtains applying more and more widely in wastewater treatment, for making biomass absorbent method more efficient, carries out to biomass material the extensive selection that chemistry or physical modification become researcher.
Citric acid is a kind of tricarboxylic acids compounds, good properties, cheap and easy to get, it is made to have become the conventional chemical modifier of development of new high-efficiency adsorbent, (1. Tang Wen is clear effectively can to improve the adsorption effect of biological adsorption agent heavy metal ion and dye molecule, Zeng Rongying, Feng Yonglan, Wu Wei, Wang Xuexin, Li Xiaoming. citric acid-modified pomelo peel cellulose is to the absorption [J] of Cu in waste water ion. process engineering journal, 2012, 12 (5): 776-780. 2. Lee meet rain, Chen Jinyi, Yu Xunmin, Li Qingxin, Tang Ailin, Wang Yong, Long Hang. a kind of preparation method of citric acid modified rape straw adsorbent and application: China, 102266756A [P] .2011-12-07.).Citric acid generally obtains modification biological adsorbent through process such as solid-liquid contact, filtration, dryings to the chemical modification method of living beings, but modified filtrate is not generally made full use of, there is not yet the pertinent literature report that biomass modified rear filtrate is utilized so far.
Shitosan is the living beings that the chitin extensively existed by nature obtains through deacetylation, water insoluble and be soluble in acid, this natural polymer has the features such as good biocompatibility, degradability, and structure is rich in amino and hydroxyl, have certain capturing ability for heavy metal ion and dye molecule, these performances can become the object of falling over each other research at numerous areas such as water treatment, METAL EXTRACTION and recovery, biochemistry and biomedical engineerings.
Summary of the invention
Object of the present invention aims to provide a kind of preparation method of biological adsorption agent.
The present invention includes following steps:
1) living beings raw material are cleaned, dry, pulverized and sieved, obtain powdered biomass;
2) by citric acid solution and powdered biomass hybrid infusion, add thermal agitation and obtain solidliquid mixture;
3) by step 2) gained solidliquid mixture suction filtration, collect filtrate;
4) by step 3) filtrate of gained mixes with shitosan, and add thermal agitation, adjust ph is 8 ~ 10, separates out solids, and continue to stir, then cool, suction filtration, washing, to neutral, obtains neutral filter residue;
5) by step 4) the neutral filter residue of gained dries, pulverizes, and namely obtains described biological adsorption agent.
In step 1) in, the order number of described sieve can be 60 ~ 200 orders, and described living beings can be at least one in tea grounds, bamboo shoot shell, citrus peel residue etc.;
In step 2) in, the molar concentration of described citric acid solution can be 0.1 ~ 1.0mol/L, and the solid-to-liquid ratio of described powdered biomass and citric acid solution can be 1g: (50 ~ 100) mL; The time of described dipping can be 6 ~ 24h; The temperature of described heating can be 80 ~ 120 DEG C, and the time of heating can be 3 ~ 4h.
In step 4) in, the solid-to-liquid ratio of described shitosan and filtrate can be 1g: (50 ~ 100) mL; The temperature of described heating can be 50 ~ 80 DEG C; Described washing can adopt deionized water to wash.
In step 5) in, the temperature of described oven dry can be 50 ~ 80 DEG C.
Described biological adsorption agent can prepare the application in heavy metal and waste water from dyestuff biological adsorption agent.
Compared with the prior art, the present invention has following outstanding advantages:
The present invention utilizes the filtrate that citric acid-modified living beings produce, and for the use of the filtrate of biomass modified generation provides effective method, makes the biomass recycling uses such as agriculture and forestry organic waste material more abundant.Prepared ABSORBENTS ABSORPTION metal ion and dye molecule have good absorption property.The present invention also can be used for the recycling of the filtrate that other sour modified biomass produces.
By sour modified biomass the filtrate of discarding make full use of, and still to can be recycled with the solvent after shitosan compound, decrease the waste of solvent.
Compared to pure chitosan adsorbent after composition compound in shitosan and waste filtrate, it is significantly improved to the treatment effect of waste water, is a kind of cheap, effective new adsorbent preparation method.
The present invention is simple to operate, wide accommodation, and the acid treatment waste liquid of multiple agriculture and forestry organic waste material biolobic material all can adopt this method to prepare the adsorbent of effective cheapness of heavy metal and waste water from dyestuff.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of biological adsorption agent prepared by embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of biological adsorption agent prepared by embodiment 2.
Fig. 3 is the scanning electron microscope (SEM) photograph of the shitosan used with citric acid-modified living beings filtrate composite.
Fig. 4 is the Cu of embodiment 4
2+adsorption curve figure, abscissa is adsorption time (min), and ordinate is adsorption capacity (mg/g).
Fig. 5 is the Cu of embodiment 5
2+adsorption curve figure, abscissa is adsorption time (min), and ordinate is adsorption capacity (mg/g).
Fig. 6 is the acid fuchsin adsorption curve figure of embodiment 6, and abscissa is adsorption time (min), and ordinate is adsorption capacity (mg/g).
Fig. 7 is the equilibrium adsorption capacities comparison diagram of embodiment 7.
Detailed description of the invention
Below by embodiment, the present invention is further illustrated.
Embodiment 1
Tea grounds discarded for beverage production plant is reclaimed, dries to constant weight in 80 DEG C of baking ovens after washing in hot boiling water, pulverize subsequently, sieve.Get 60 ~ 200 order tea grounds powder, join in 0.1mol/L citric acid solution, solid-to-liquid ratio is 1:50 (g:mL), under Keep agitation condition, 120 DEG C are warming up to after dipping 24h, and continue 90min, naturally cool to room temperature, suction filtration gained filtrate is the filtrate that citric acid-modified tea grounds produces.
Get above-mentioned filtrate 300mL, add 3.0g shitosan, Keep agitation 4h at 50 DEG C, after in stirring by the NaOH solution adjust ph to 8 of 1mol/L, rear continuations stirring 1h; Nature cooled and filtered, washing, gained solid particle, in 50 DEG C of oven for drying, pulverizing, namely makes described biological adsorption agent.
Fig. 1 is the scanning electron microscope (SEM) photograph of biological adsorption agent prepared by the present embodiment 1, and Fig. 3 is the scanning electron microscope (SEM) photograph of the shitosan used with citric acid-modified living beings filtrate composite.Contrast can find out with Fig. 3, shitosan and filtrate active ingredient compound rear surface more coarse, having more the more gap structure, is the good adsorbent of structural behaviour.
Embodiment 2
Reclaimed by bamboo shoot shell discarded for bamboo shoot processing factory, washing is dried to constant weight after removing its surface dust in 80 DEG C of baking ovens, pulverizes subsequently, sieves.Get 40 ~ 200 order bamboo shoot shell powder, join in 0.5mol/L citric acid solution, solid-to-liquid ratio is 1:100, under Keep agitation condition, 80 DEG C are warming up to after dipping 6h, and continue 90min, naturally cool to room temperature, suction filtration gained filtrate is the filtrate that citric acid-modified bamboo shoot shell produces.
Get above-mentioned filtrate 300mL, add 6.0g shitosan, Keep agitation 4h at 80 DEG C, after in stirring by the NaOH solution adjust ph to 8 of 1mol/L, and continue to stir 1h; Naturally suction filtration after cooling, spend deionized water constant to pH, natural cooled and filtered, washing, gained solid particle, in 50 DEG C of oven for drying, pulverizing, namely makes described biological adsorption agent.
Fig. 2 is the scanning electron microscope (SEM) photograph of biological adsorption agent prepared by the present embodiment 2, and Fig. 3 is the scanning electron microscope (SEM) photograph of the shitosan used with citric acid-modified living beings filtrate composite.Contrast known with Fig. 3, shitosan, through having abundanter pleated structure with filtrate active ingredient compound rear surface, is the good adsorbent of structural behaviour equally.
Embodiment 3
Citrus peel slag discarded after pectin factory being extracted pectin reclaims, and dries to constant weight, pulverize subsequently, sieve after cleaning in 80 DEG C of baking ovens.Get 40 ~ 200 order citrus peel residue powder, join in 1.0mol/L citric acid solution, solid-to-liquid ratio is 1:80, under Keep agitation condition, 100 DEG C are warming up to after dipping 15h, and continue 90min, naturally cool to room temperature, suction filtration gained filtrate is the filtrate that citric acid-modified citrus peel residue produces.
Get above-mentioned filtrate 300mL, add 4.5g shitosan, Keep agitation 4h at 60 DEG C, after in stirring by the NaOH solution adjust ph to 9 of 1mol/L, rear continuations stirring 1h; Nature cooled and filtered, washing, gained solid particle, in 50 DEG C of oven for drying, pulverizing, namely makes described biological adsorption agent.
Embodiment 4
In 250mL conical flask, respectively put into 40 ~ 80 order biological adsorption agent 0.1g prepared by embodiment 1, add the Cu of 50.0mL190.65mg/L
2+solution, in 25 DEG C, constant temperature oscillation 1 under 150r/min condition, 3,5,10,20,30,45,60,90,120,240min, take out and filter, after filtrate dilution, utilize atomic absorption spectrophotometer to measure Cu in solution
2+concentration, thus draw its adsorption capacity curve (see Fig. 4).
Embodiment 5
In 250mL conical flask, respectively put into 40 ~ 80 order adsorbent 0.1g prepared by embodiment 2, add the Cu of 50.0mL 190.65mg/L
2+solution, in 25 DEG C, constant temperature oscillation 1 under 150r/min condition, 3,5,10,20,30,45,60,90,120,240min, take out and filter, after filtrate dilution, utilize atomic absorption spectrophotometer to measure Cu in solution
2+concentration, thus draw its adsorption capacity curve (see Fig. 5).
Embodiment 6
40 ~ 80 order adsorbent 0.1g prepared by embodiment 2 are respectively put in 250mL conical flask, add the acid fuchsine solution of 50.0mL 250mg/L, in 25 DEG C, constant temperature oscillation 5 under 150r/min condition, 10,15,20,30,45,60min, take out and filter, use the acid fuchsin concentration in ultraviolet specrophotometer mensuration solution after filtrate dilution, thus draw its adsorption capacity curve (see Fig. 6).
Embodiment 7
Biological adsorption agent prepared by biological adsorption agent prepared by embodiment 1, embodiment 2 and pure chitosan (deacetylation is 70%) each 0.1g is put into respectively in 3 250mL conical flasks, in 25 DEG C, constant temperature oscillation 4h under 150r/min condition, after filtration, filtrate is diluted, measure Cu in solution with atomic spectrophotometer
2+concentration.Result display shitosan through with the composition composite in living beings filtrate after gained adsorbent there is adsorption effect (see Fig. 7) more better than shitosan itself.
Claims (10)
1. a preparation method for biological adsorption agent, is characterized in that comprising the following steps:
1) living beings raw material are cleaned, dry, pulverized and sieved, obtain powdered biomass;
2) by citric acid solution and powdered biomass hybrid infusion, add thermal agitation and obtain solidliquid mixture;
3) by step 2) gained solidliquid mixture suction filtration, collect filtrate;
4) by step 3) filtrate of gained mixes with shitosan, and add thermal agitation, adjust ph is 8 ~ 10, separates out solids, and continue to stir, then cool, suction filtration, washing, to neutral, obtains neutral filter residue;
5) by step 4) the neutral filter residue of gained dries, pulverizes, and namely obtains described biological adsorption agent.
2. the preparation method of a kind of biological adsorption agent as claimed in claim 1, is characterized in that in step 1) in, the order number of described sieve is 60 ~ 200 orders.
3. the preparation method of a kind of biological adsorption agent as claimed in claim 1, is characterized in that in step 1) in, described living beings are at least one in tea grounds, bamboo shoot shell, citrus peel residue.
4. the preparation method of a kind of biological adsorption agent as claimed in claim 1, is characterized in that in step 2) in, the molar concentration of described citric acid solution is 0.1 ~ 1.0mol/L.
5. the preparation method of a kind of biological adsorption agent as claimed in claim 1, is characterized in that in step 2) in, the solid-to-liquid ratio of described powdered biomass and citric acid solution is 1g: (50 ~ 100) mL.
6. the preparation method of a kind of biological adsorption agent as claimed in claim 1, is characterized in that in step 2) in, the time of described dipping is 6 ~ 24h.
7. the preparation method of a kind of biological adsorption agent as claimed in claim 1, is characterized in that in step 2) in, the temperature of described heating is 80 ~ 120 DEG C, and the time of heating is 3 ~ 4h.
8. the preparation method of a kind of biological adsorption agent as claimed in claim 1, is characterized in that in step 4) in, the solid-to-liquid ratio of described shitosan and filtrate is 1g: (50 ~ 100) mL.
9. the preparation method of a kind of biological adsorption agent as claimed in claim 1, is characterized in that in step 4) in, the temperature of described heating is 50 ~ 80 DEG C; Described washing can adopt deionized water to wash.
10. the preparation method of a kind of biological adsorption agent as claimed in claim 1, is characterized in that in step 5) in, the temperature of described oven dry is 50 ~ 80 DEG C.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111178A (en) * | 2015-10-10 | 2015-12-02 | 哈尔滨商业大学 | Method for purifying anthocyanin by adopting bio-adsorbent |
| CN105413648A (en) * | 2015-12-20 | 2016-03-23 | 吴涛 | Folium ginkgo adsorbing material and preparation method thereof |
| CN106000348A (en) * | 2016-08-01 | 2016-10-12 | 广西南宁桂尔创环保科技有限公司 | Preparation method of adsorbent for treating zinc-containing wastewater |
| CN106040207A (en) * | 2016-08-01 | 2016-10-26 | 广西南宁桂尔创环保科技有限公司 | Adsorbent for treating cadmium-containing wastewater |
| CN106186156A (en) * | 2016-08-01 | 2016-12-07 | 广西南宁桂尔创环保科技有限公司 | A kind of method preparing arsenic-removing adsorption agent |
| CN106186157A (en) * | 2016-08-01 | 2016-12-07 | 广西南宁桂尔创环保科技有限公司 | A kind of method preparing adsorbents for lead ion pyrolytic |
| CN106623379A (en) * | 2016-11-04 | 2017-05-10 | 上海立昌环境工程股份有限公司 | Resource recycling method of construction waste and repairing agent for heavy-metal-polluted soil |
| CN106984282A (en) * | 2017-05-04 | 2017-07-28 | 凤台县双利生物科技有限公司 | A kind of preparation method of the magnetic green substance adsorber of sulfydryl lignocellulosic montmorillonite Composite |
| CN107751712A (en) * | 2017-11-01 | 2018-03-06 | 广西吉朋投资有限公司 | A kind of feed takes off mould dose and preparation method thereof |
| CN110292914A (en) * | 2019-07-10 | 2019-10-01 | 广州美颂化妆品有限公司 | Natural biological charcoal-chitosan-based tea oil composite material and preparation method |
| CN110422904A (en) * | 2019-09-05 | 2019-11-08 | 昆明理工大学 | A method of effluent containing heavy metal ions are handled using modified biomass |
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| CN101239305A (en) * | 2008-03-06 | 2008-08-13 | 上海交通大学 | Method for preparing modified plant fibrous sale price biological adsorption agent |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111178A (en) * | 2015-10-10 | 2015-12-02 | 哈尔滨商业大学 | Method for purifying anthocyanin by adopting bio-adsorbent |
| CN105413648A (en) * | 2015-12-20 | 2016-03-23 | 吴涛 | Folium ginkgo adsorbing material and preparation method thereof |
| CN106000348A (en) * | 2016-08-01 | 2016-10-12 | 广西南宁桂尔创环保科技有限公司 | Preparation method of adsorbent for treating zinc-containing wastewater |
| CN106040207A (en) * | 2016-08-01 | 2016-10-26 | 广西南宁桂尔创环保科技有限公司 | Adsorbent for treating cadmium-containing wastewater |
| CN106186156A (en) * | 2016-08-01 | 2016-12-07 | 广西南宁桂尔创环保科技有限公司 | A kind of method preparing arsenic-removing adsorption agent |
| CN106186157A (en) * | 2016-08-01 | 2016-12-07 | 广西南宁桂尔创环保科技有限公司 | A kind of method preparing adsorbents for lead ion pyrolytic |
| CN106623379A (en) * | 2016-11-04 | 2017-05-10 | 上海立昌环境工程股份有限公司 | Resource recycling method of construction waste and repairing agent for heavy-metal-polluted soil |
| CN106984282A (en) * | 2017-05-04 | 2017-07-28 | 凤台县双利生物科技有限公司 | A kind of preparation method of the magnetic green substance adsorber of sulfydryl lignocellulosic montmorillonite Composite |
| CN107751712A (en) * | 2017-11-01 | 2018-03-06 | 广西吉朋投资有限公司 | A kind of feed takes off mould dose and preparation method thereof |
| CN110292914A (en) * | 2019-07-10 | 2019-10-01 | 广州美颂化妆品有限公司 | Natural biological charcoal-chitosan-based tea oil composite material and preparation method |
| CN110292914B (en) * | 2019-07-10 | 2022-04-29 | 广州美颂化妆品有限公司 | Natural biochar-chitosan-based tea oil composite material and preparation method thereof |
| CN110422904A (en) * | 2019-09-05 | 2019-11-08 | 昆明理工大学 | A method of effluent containing heavy metal ions are handled using modified biomass |
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