CN102266754B - Method for preparing activated carbon-persimmon tannin compound absorbent - Google Patents

Method for preparing activated carbon-persimmon tannin compound absorbent Download PDF

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CN102266754B
CN102266754B CN2011102157795A CN201110215779A CN102266754B CN 102266754 B CN102266754 B CN 102266754B CN 2011102157795 A CN2011102157795 A CN 2011102157795A CN 201110215779 A CN201110215779 A CN 201110215779A CN 102266754 B CN102266754 B CN 102266754B
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active carbon
persimmon tannin
solution
persimmon
activated carbon
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CN102266754A (en
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王勇
李世安
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HUBEI GUANGFUKANG BIO-TECHNOLOGY Co Ltd
HUBEI SHIWEITIAN PHARMACEUTICAL TECHNOLOGY Co Ltd
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HUBEI GUANGFUKANG BIO-TECHNOLOGY Co Ltd
HUBEI SHIWEITIAN PHARMACEUTICAL TECHNOLOGY Co Ltd
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Abstract

The invention relates to a method for preparing an activated carbon-persimmon tannin compound absorbent. The method comprises the following steps: 1) pre-treating the activated carbon; 2) on the basis that a ratio of the treated activated carbon to a persimmon tannin solution is 0.500g:250ml, preparing the treated activated carbon and the persimmon tannin solution with concentration of 40mg/L; adding the treated activated carbon into the persimmon tannin solution of which the pH value is 3.0; magnetically stirring for 8-24 hours; filtering with oily filter paper; washing with distilled water; and drying in an oven at 85-105 DEG C to finally obtain the activated carbon-persimmon tannin compound absorbent. The method has the advantages that the cost is low, the process is simple and the prepared compound absorbent has better absorbing effect. The compound absorbent can be used for purifying the industrial sewage and domestic water, can be used as a clarifying agent for liquor and an absorbent for cigarette filter tip, and is more beneficial to the health of human.

Description

The preparation method of a kind of active carbon-persimmon tannin compound adsorbent
Technical field
The present invention relates to the preparation method of a kind of active carbon-persimmon tannin compound adsorbent.This compound adsorbent is applicable to purification and the processing of handling the industrial wastewater and the resident living water that contain heavy metal ion.
Background technology
In numerous environmental pollutions, heavy metal is because self can not be by natural degradation, and then is prone to get into human body through food chain, the serious harm human health, and therefore the pollution in water body more and more causes people's attention.Lead, cadmium etc. and compound thereof are because of being widely used in industries such as mining, smelting, electronics, plating, oil, fertilizer manufacturing; Become the important pollution sources in the sewage and enjoyed people's attention, strict its allowance of regulation limitations has all been arranged in department countries in the world such as environmental protection, health, food.
Method plumbous in the present domestic removal water body, cadmium has chemical precipitation method, absorption method, ion-exchange, liquid-film method and electroosmose process etc.; Absorption method is efficient, easy to operate, thereby is widely used in (≤50mg/L) the effective removal of heavy metal ion of low quality concentration in the water body.In recent years, there is report to utilize natural biomass to can be used for pb in the water body for the sorbing material of feedstock production 2+Absorption remove.
Active carbon is as a kind of non-polar adsorbent, and the source is abundant, is to use one of the widest adsorbent in the present wastewater treatment.It has good adsorption performance and stable chemical property, can anti-strong acid, highly basic, can stand water logging, high temperature, high pressure effect, and simultaneously can also activating and regenerating.
Persimmon tannin is a kind of aboundresources natural polymer cheap and easy to get, and soluble in water, ethanol, acetone etc. mainly are present in the fruit of puckery persimmon, are a kind of abundant reproducible natural macromolecular materials.The puckery persimmon resource of China is particularly abundant, the character more complicated of persimmon fruit tannin, and character is very active.It has special uv absorption property, disinfection, deodorizing, effect such as anti-oxidant.A lot of ortho positions, a position phenolic hydroxyl group are arranged in the persimmon tannin molecule, can be used as polyhydroxy part and metal ion and carry out ligand exchange reaction, its structure is as shown in Figure 1.Two adjacent phenolic hydroxyl groups can form stable five-membered ring huge legendary turtle compound with the form and the toxic metals ion of negative oxygen ion; Though the 3rd phenolic hydroxyl group in the pyrogallol structure do not participated in complexing; But can promote the disassociation of two other phenolic hydroxyl group, thereby promote the formation of complex compound to reach stable.Formed netted chelate can have the effect of separating metal ion in different pH value settle.
Experimental result shows that persimmon tannin has excellent sterilizing and quiet bacterium effect, can be used as the antibacterial green material and uses.Because persimmon tannin is soluble in water, be difficult to directly be used for the removal of water body metal ion.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of active carbon-persimmon tannin compound adsorbent, this method cost is low, technology is simple, and the prepared composite adsorbent has adsorption effect characteristics preferably.
To achieve these goals, the technical scheme that the present invention taked is: the preparation method of a kind of active carbon-persimmon tannin compound adsorbent is characterized in that it comprises the steps:
1) preliminary treatment of activated carbon: 1. press activated carbon: distilled water=100g: 500ml, activated carbon is added distilled water boil (referring to 95~100 ℃) stirring 1h, and then stir 1h; Suction filtration obtains solid; 2. pickling: press activated carbon: hydrochloric acid solution=100g: 250ml chooses the hydrochloric acid solution that concentration is 5~6mg/L, adds hydrochloric acid solution in the resulting solid; Be heated to 90~100 ℃ and stir 1h; Leave standstill 24h subsequently, suction filtration washs with distilled water, until pH=5.0~6.0 of final rinse solution;
3. above step acid cleaning process 2. repeats 3 times at least;
4. resulting solid is dried to constant weight in 85~105 ℃ of baking ovens after the pickling, obtains active carbon after treatment, and is subsequent use;
2) by after treatment active carbon: persimmon tannin solution=0.500g: 250ml; Choose the persimmon tannin solution that after treatment active carbon and concentration are 40mg/L, the active carbon after handling of learning from else's experience adds the persimmon tannin solution of pH=3.0, at magnetic agitation 8~24h; Filter with oiliness filter paper then; Use distilled water flushing, in 85~105 ℃ of baking ovens, dry subsequently, promptly make active carbon-persimmon tannin compound adsorbent.
The active carbon that makes-persimmon tannin compound adsorbent is 17.32mg persimmon tannin/g active carbon, and is higher to the adsorption rate of heavy metal ion through test compound adsorbent at this moment.
Used active carbon is a powdered activated carbon, and the molecular weight of used persimmon tannin is 1~1.5 ten thousand.
The preparation of used persimmon tannin solution: after plucking the fragmentation of blue or green persimmon fruit, by blue or green persimmon: the ratio of the mass ratio of water=1: 0.5~10 was soaked 7 days, squeezed the juice, removed the gred after the filtration, and spontaneous fermentation 1~2 year obtains persimmon tannin solution (red tan solution).
The method of active carbon-persimmon tannin compound adsorbent centering adsorption of metal ions is: the concentration of heavy metal ion is at 10mg/L-50mg/L, and the optimal adsorption condition is PH=5.0, and the compound adsorbent consumption is 2.0g/L, and adsorption time is 1.0h.
The present invention is assembled into the surface of active carbon to natural high molecular substance through composite means, to improve the adsorption efficiency of heavy metal ion.Natural high molecular substance-persimmon tannin is a kind of reproducible living resources, has numerous phenolic hydroxyl groups, can be used as a kind of multidentate ligand and toxic metals ion generation complex reaction, and heavy metal ion is had very strong absorption property.Its antibiotic and sterilizing component of compound adsorbent is a persimmon tannin, and the phenolic hydroxyl group of position has sterilization, deodorization therebetween.
The invention has the beneficial effects as follows:
1, because persimmon tannin has a plurality of ortho positions, a position phenolic hydroxyl group; Can be used as polyhydroxy part and metal ion and carry out ligand exchange reaction; But should not use as adsorbent separately because persimmon tannin is soluble in water, persimmon tannin is fixed on the active carbon so this experiment is probed into.In view of the active site of active carbon also can adsorbing metal ions, fixedly behind the persimmon tannin, too much persimmon tannin can occupy the active site of active carbon to active carbon, and the persimmon tannin molecular weight is bigger, can influence the suction-operated of metal ion.So optimal proportion of both needs reaches optimum absorption property.
The present invention adopts: getting 0.500g active carbon after treatment, to add 250ml concentration be that the persimmon tannin solution of 40mg/L stirs 8~24h at the pH=3.0 lower magnetic force.The prepared composite adsorbent has adsorption effect characteristics preferably, and in content of beary metal 10-50mg/L scope, this compound adsorbent improves about 10% than independent charcoal absorption efficient.
2, this method cost is low, technology is simple.
3, used compound adsorbent has effective sterilization, bacteria removing effect to the epidermidis strain in the water body, coliform, saccharomycete.Made compound adsorbent removes the processing of available sewage, also can be used for the purified treatment of urbanite water consumption.Can also be as the fining agent of drinks, impurity such as the protein substance in the sorbing liquor have improved the pure quality of wine and the class of wine; Can also use adsorbent as cigarette filter, can adsorb the oil smoke in the cigarette, reduce in the cigarette harmful substance (like tar, nicotine etc.), help healthyly more, also can improve grade of cigarette simultaneously the injury of human body.
Description of drawings
Fig. 1 is the molecular structure of persimmon tannin.
The specific embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to following embodiment.
Embodiment 1:
The preparation method of a kind of active carbon-persimmon tannin compound adsorbent, it comprises the steps:
1) preliminary treatment of activated carbon: 1. 100g activated carbon adding 500ml distilled water is stirred 1h for 95~100 ℃, and then (this time stir is to stop to heat continued stirring 1h, to reach the purpose of abundant washing, temperature is not being had strict demand to stir 1h; ); Suction filtration obtains solid; 2. pickling: adding 250ml concentration in the resulting solid is the hydrochloric acid solution of 5~6mg/L, is heated to 90~100 ℃ and stirs 1h, leaves standstill 24h subsequently, and suction filtration is with distilled water washing 3~5 times, until pH=5.0~6.0 of final rinse solution;
3. above step acid cleaning process 2. repeats 3 times;
4. resulting solid is dried to constant weight in 105 ℃ of baking ovens after the pickling, obtains active carbon after treatment, and is subsequent use;
2) getting 0.500g active carbon adding 250ml concentration after treatment is the persimmon tannin solution of 40mg/L, pH=3.0; In temperature is the condition lower magnetic force stirring 8h of 18 ℃ (under room temperatures); Filter (as filtering) with oiliness filter paper then with parchment; Use distilled water flushing, oven dry (being dried to constant weight) in 105 ℃ of baking ovens subsequently promptly makes active carbon-persimmon tannin compound adsorbent.The active carbon that makes-persimmon tannin compound adsorbent is 17.32mg persimmon tannin/g active carbon, and is higher to the adsorption rate of heavy metal ion through test compound adsorbent at this moment.
Used active carbon is a powdered activated carbon, and used persimmon tannin is a condensed tannin, and its molecular weight is 1~1.5 ten thousand (active carbon: Tianjin Kermel Chemical Reagent Co., Ltd., chemical pure);
The preparation of used persimmon tannin solution: after plucking the fragmentation of blue or green persimmon fruit, by blue or green persimmon: the ratio of the mass ratio of water=1: 0.5~10 was soaked 7 days, squeezed the juice, removed the gred after the filtration, and spontaneous fermentation 1~2 year obtains persimmon tannin solution (red tan solution).
Embodiment 2:
The preparation method of a kind of active carbon-persimmon tannin compound adsorbent, it comprises the steps:
1) preliminary treatment of activated carbon: step acid cleaning process 2. repeats 4 times, and remaining is with the step 1) of embodiment 1;
2) magnetic agitation 12h, remaining is with the step 2 of embodiment 1).
Embodiment 3:
The preparation method of a kind of active carbon-persimmon tannin compound adsorbent, it comprises the steps:
1) preliminary treatment of activated carbon: 1. the 100g activated carbon is added 500ml distilled water and boil stirring 1h, and then stir 1h; Suction filtration obtains solid; 2. pickling: adding 250ml concentration in the resulting solid is the hydrochloric acid solution of 5~6mg/L, is heated to 90~100 ℃ and stirs 1h, leaves standstill 24h subsequently, and suction filtration is with distilled water washing 3~5 times, until pH=5.0~6.0 of final rinse solution;
3. above step acid cleaning process 2. repeats 5 times;
4. resulting solid is dried to constant weight in 95 ℃ of baking ovens after the pickling, obtains active carbon after treatment, and is subsequent use;
2) magnetic agitation 24h is dried in 85 ℃ of baking ovens, and remaining is with the step 2 of embodiment 1).
Comparing embodiment 1:
1) preliminary treatment of activated carbon: with the step 1) of embodiment 1;
2) getting 8 groups of 0.500g active carbon after treatment corresponding respectively is that 40mg/L persimmon tannin solution carries out compound (concentration of every group of persimmon tannin solution is identical) with 8 groups of 250ml concentration; The pH value 3.0-10.0 that regulates persimmon tannin solution (divides 8 groups; The pH value is 3.0,4.0,5.0,6.0,7.0,8.0,9.0,10.0); Magnetic agitation 60min; With remaining persimmon tannin content in the UV spectrophotometer measuring solution, find that the optimal pH that persimmon tannin is fixed on the active carbon is 3.0, the persimmon tannin fixed rate is the fastest with this understanding.
Comparing embodiment 2:
1) preliminary treatment of activated carbon: with embodiment 1;
2) get 13 groups of 0.500g active carbon after treatment corresponding respectively with 13 groups of 250ml concentration be that 40mg/L persimmon tannin solution carries out compound; The pH value of regulating persimmon tannin solution is 3.0; Temperature is magnetic agitation (absorption) 0.5,1,2,3,4,5,6,8,10,12,15,20 and 24h (dividing 13 groups) respectively under 18 ℃ the condition; With remaining persimmon tannin content in the UV spectrophotometer measuring solution; Find that the amount that persimmon tannin is fixed on the active carbon after stirring 8h is tending towards constant, promptly charcoal absorption 8h can reach adsorption equilibrium basically.
One, compound adsorbent is to pb 2+Suction-operated,
Application example 1:
50ml is contained pb 2+Concentration is that the solution of 10mg/L is packed in the boiling flask, and the pH value of solution is adjusted to 5.0.The compound adsorbent that adds 0.1g embodiment 1 then will act on liquid as for stir effect 60min on the magnetic stirring apparatus at 20 ℃ of lower magnetic forces.The centrifugal 10min of 3500rpm utilizes atomic absorption method to record pb in the supernatant then 2+Concentration, according to n=(C 0-C e)/C 0* 100% and q=(C 0-C e) V/M calculating adsorption rate and adsorbance q.C 0Initial concentration (mg/L) for metal ion in the aqueous solution; C eEquilibrium concentration (mg/L) for metal ion in the aqueous solution; V is liquor capacity (L); M is compound adsorbent weight (g).Calculate acquisition adsorbent this moment to pb 2+Adsorption rate reach 96.5%, adsorbance is 4.83mg/g.
Application example 2:
50ml is contained pb 2+Concentration is that the solution of 20mg/L is packed in the boiling flask, and the pH value of solution is adjusted to 5.0.The compound adsorbent that adds 0.1g embodiment 2 then will act on liquid as for stir effect 60min on the magnetic stirring apparatus at 20 ℃ of lower magnetic forces.The centrifugal 10min of 3500rpm utilizes atomic absorption method to record pb in the supernatant then 2+Concentration, calculate to obtain this adsorbent to pb 2+Adsorption rate reach 87.1%, adsorbance is 9.30mg/g.
Application example 3:
50ml is contained pb 2+Concentration is that the solution of 50mg/L is packed in the boiling flask, and the pH value of solution is adjusted to 5.0.The compound adsorbent that adds 0.1g embodiment 3 then will act on liquid as for stir effect 60min on the magnetic stirring apparatus at 20 ℃ of lower magnetic forces.The centrifugal 10min of 3500rpm utilizes atomic absorption method to record pb in the supernatant then 2+Concentration, calculate to obtain this adsorbent to pb 2+Adsorption rate reach 73.7%, adsorbance is 14.92mg/g.
Two, compound adsorbent is to Cd 2+Suction-operated,
Application example 4:
50ml is contained Cd 2+Concentration is that the solution of 5mg/L is packed in the boiling flask, and the pH value of solution is adjusted to 5.0.The compound adsorbent that adds 0.1g embodiment 1 then will act on liquid as for stir effect 60min on the magnetic stirring apparatus at 20 ℃ of lower magnetic forces.The centrifugal 10min of 3500rpm utilizes atomic absorption method to record Cd in the supernatant then 2+Concentration, calculate this compound adsorbent to Cd in this experimental solutions 2+Average adsorption rate be 80.0%, adsorbance is 2.0mg/g.Explain that the compound adsorbent that synthesized also has significantly suction-operated to the cadmium ion of low concentration.
Application example 5:
50ml is contained Cd 2+Concentration is that the solution of 20mg/L is packed in the boiling flask, and the pH value of solution is adjusted to 5.0.The compound adsorbent that adds 0.1g embodiment 2 then will act on liquid as for stir effect 60min on the magnetic stirring apparatus at 20 ℃ of lower magnetic forces.The centrifugal 10min of 3500rpm utilizes atomic absorption method to record Cd in the supernatant then 2+Concentration, calculate this compound adsorbent to Cd in this experimental solutions 2+Average adsorption rate be 65.1%, adsorbance is 6.51mg/g.
Application example 6:
50ml is contained Cd 2+Concentration is that the solution of 50mg/L is packed in the boiling flask, and the pH value of solution is adjusted to 5.0.The compound adsorbent that adds 0.1g embodiment 3 then will act on liquid as for stir effect 60min on the magnetic stirring apparatus at 20 ℃ of lower magnetic forces.The centrifugal 10min of 3500rpm utilizes atomic absorption method to record Cd in the supernatant then 2+Concentration, calculate this compound adsorbent to Cd in this experimental solutions 2+Average adsorption rate be 33.0%, adsorbance is 8.25mg/g.
Three, bactericidal properties experimental study:
Get a certain amount of epidermidis strain, coliform, saccharomycete thalline and join in the conical flask that fills 50ml distilled water, add the 0.1g compound adsorbent, measure aerobic plate count behind the magnetic agitation 24h, its result sees table 1.Possessing in the active carbon compound adsorbent sample of persimmon tannin, epidermidis strain, coliform, saccharomycete reduce in a large number, show that this compound adsorbent has stronger bactericidal effect, have to suppress the effect that bacterial classification increases.
The bactericidal properties of table 1 compound adsorbent
Annotate: control group is fixing persimmon tannin not.Find that through antibacterial tests this compound adsorbent has kept the sterilization and the quiet bacterium characteristic (seeing table 1) of persimmon tannin, can be used for Industrial Wastewater Treatment better and the resident drinks water purification.
The compound adsorbent of embodiment 2-3 has stronger bactericidal effect (identical with embodiment 1) equally.

Claims (3)

1. the preparation method of active carbon-persimmon tannin compound adsorbent is characterized in that it comprises the steps:
1) preliminary treatment of active carbon: 1. press active carbon: distilled water=100g: 500ml, active carbon is added distilled water boil stirring 1h, and then stir 1h; Suction filtration obtains solid;
2. pickling: press active carbon: hydrochloric acid solution=100g: 250ml chooses the hydrochloric acid solution that concentration is 5~6mg/L, adds hydrochloric acid solution in the resulting solid; Be heated to 90~100 ℃ and stir 1h; Leave standstill 24h subsequently, suction filtration washs with distilled water, until pH=5.0~6.0 of final rinse solution;
3. above step acid cleaning process 2. repeats 3 times at least;
4. resulting solid is dried to constant weight in 85~105 ℃ of baking ovens after the pickling, obtains active carbon after treatment, and is subsequent use;
2) by after treatment active carbon: persimmon tannin solution=0.500g: 250ml; Choose the persimmon tannin solution that after treatment active carbon and concentration are 40mg/L, the active carbon after handling of learning from else's experience adds the persimmon tannin solution of pH=3.0, at magnetic agitation 8~24h; Filter with oiliness filter paper then; Use distilled water flushing, in 85~105 ℃ of baking ovens, dry subsequently, promptly make active carbon-persimmon tannin compound adsorbent.
2. the preparation method of a kind of active carbon according to claim 1-persimmon tannin compound adsorbent is characterized in that: used active carbon is a powdered activated carbon.
3. the preparation method of a kind of active carbon according to claim 1-persimmon tannin compound adsorbent; It is characterized in that: the preparation of used persimmon tannin solution: after plucking the fragmentation of blue or green persimmon fruit; Ratio in mass ratio=1 ﹕ 0.5~10 of Qing Shi ﹕ water was soaked 7 days; Squeeze the juice, remove the gred after the filtration, spontaneous fermentation 1~2 year obtains persimmon tannin solution.
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