CN101306813B - Method for preparing smooth cord-grass active carbon for treating cadmium-containing waste water - Google Patents
Method for preparing smooth cord-grass active carbon for treating cadmium-containing waste water Download PDFInfo
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- CN101306813B CN101306813B CN2008101242619A CN200810124261A CN101306813B CN 101306813 B CN101306813 B CN 101306813B CN 2008101242619 A CN2008101242619 A CN 2008101242619A CN 200810124261 A CN200810124261 A CN 200810124261A CN 101306813 B CN101306813 B CN 101306813B
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- activated carbon
- spartina alterniflora
- phosphoric acid
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- cadmium
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Abstract
The invention discloses a preparation method of Spartina alterniflora activated carbon, which can be used for treating cadmium wastewater. The method comprises the steps of oven-drying Spartina alterniflora stem and pulverizing; extracting the pulverized Spartina alterniflora powder with 0.1-10% of sulphuric acid solution for 1-10 hours; filtering the extracted solid-liquid mixture, and immersing the filter residue in phosphoric acid solution for 6-30 hours; oven-drying the immersed phosphoric acid-Spartina alterniflora mixture, activating by calcination at 400-700 DEG C under N2 as a protective gas for 0.5-10 hours to obtain activated carbon powder; and washing the obtained activated carbon powder and pulverizing. The inventive preparation method removes the interference of a large quantity of salts, and obtains the surface functional groups-enriched activated carbon product with yield of 42-48%. The obtained activated carbon can be used for treating cadmium wastewater with adsorption capacity in the range of 11-48.25mg/g, which is much higher than that of common commercial activated carbon. The obtained activated carbon takes full use of waste and creates great economic benefit and good social and environmental benefits.
Description
Technical field
The invention belongs to the ecological engineering technology field, be specifically related to a kind of spartina alterniflora loisel of utilization and prepare the process of active carbon that to administer cadmium wastewater.
Background technology
The spartina alterniflora loisel originates in the southeastern US seashore, introduces China in 1979, and purpose is in order to protect the beach shore protection, improve the soil, afforest the seabeach and to improve the seabeach ecotope.Rice grass many mud matter sandy beach that China is coastal becomes the greenery patches, seabeach from barren land over nearly 20 years, and huge productivity is provided, and the aspect such as encloses and cultivates on China's sea wall protection and land and made huge contribution.But its intensive growth, well developed root system, grass-seed can be flown upward with the wind everywhere, spreads rapidly, and resistance and reproductivity are extremely strong, cause the beach disruption of ecological balance, influence beach development aquaculture; Cause the navigation channel to be silted up; Cause deteriorating water quality, marine organisms death by suffocation, and bring out red tide etc.
Current, just belong to the starting stage for the research of spartina alterniflora loisel's utilization, utilize the careless stalk of rice to produce gac and administer the research of cadmium wastewater and rarely have report.Studies show that, contain abundant carboxyl in the gac that utilizes the spartina alterniflora loisel to produce, lactone group, phenolic hydroxyl group, oxygen-containing functional groups such as carbonyl have the good adsorption performance for cadmium ion.
Summary of the invention
The objective of the invention is pollution, thereby a kind of preparation method of active carbon is provided, realized effective utilization of spartina alterniflora loisel and effective removal of cadmium wastewater, have very high economic worth in order effectively to utilize the spartina alterniflora loisel and to administer cadmium wastewater.
Purpose of the present invention can reach by following measure:
A kind of spartina alterniflora loisel's preparation method of active carbon of administering cadmium wastewater, it comprises the steps:
Step 1: with oven dry of spartina alterniflora loisel's stem and pulverizing;
Step 2: with mass content is spartina alterniflora loisel's powder 1～10h after the leaching of 0.1～10% sulphuric acid soln is pulverized;
Step 3: filter the solidliquid mixture after leaching, filter residue is injected phosphoric acid solution flood 6～30h;
Step 4: the phosphoric acid rice grass mixture oven dry after will flooding, at N
2Protection and 400～700 ℃ of following calcining and activating 0.5～10h;
Step 5: the gac that the washing calcining obtains is also pulverized.
In the step 1, the spartina alterniflora loisel of harvesting is dried in the shade, get stem, oven dry, bake out temperature is preferably 100～120 ℃, is crushed to particle diameter less than 150 orders, preferred mistake 100 mesh sieves.The spartina alterniflora loisel is not exclusively dry, just can not effectively pulverize, and can influence the activatory effect.Stalk is only got stem, and the leaf fiber cellulose content is too high, and saltiness is excessive, produces the gac yield and will reduce; Stalk the best is taken from spartina alterniflora loisel's ripening stage, and content of lignin can raise to some extent like this.
In the step 2, the adding of sulphuric acid soln can be removed the inorganic salt in the stalk, reduces the wherein content of ash content, thereby obtains rice grass group; The mass content of sulphuric acid soln is preferably 0.5～2%, and the best is 1%.The mass ratio of the spartina alterniflora loisel's powder after sulphuric acid soln and the pulverizing is 1: 5～15.Leaching time is preferably 4～8h.
In the step 3, the solidliquid mixture that obtains in the step 2 is filtered, filter residue injects phosphoric acid solution, wherein the mass ratio of phosphoric acid in the phosphoric acid solution and former dried rice grass is 0.3: 1～3: 1, the amount of water there is no particular requirement in the phosphoric acid solution, but, generally its mass content is made into 40～80%, as 60% in order to prevent that phosphoric acid solution from crossing rare or moisture very fewly.The reaction times of dipping is preferably 12～24h, obtains phosphoric acid rice grass mixture.
In the step 4, phosphoric acid rice grass mixture is bake drying together without separation, and a phosphoric acid solution and a rice grass mix, and do not remove phosphoric acid solution by filtering; The exsiccant purpose is in order to reduce the corrosion of moisture for activation stage, to make phosphoric acid and rice grass bonding simultaneously, increasing activation effect.Bake out temperature is preferably 100～120 ℃.Carry out in the activation furnace (as tube type resistance furnace) that calcining and activating can generally be used always, the calcining and activating time is preferably 1～4h.Feed N
2Be not reduced yield for the protective reaction material is not subjected to the oxidation of oxygen.
In the step 5, wash with water the gac that obtains of calcining to pH5～7 to remove unnecessary phosphoric acid, preferably be washed till neutrality or near neutral, removing effect under the condition of heating can be better.Be crushed to particle diameter after the washing again less than 150 orders, preferred mistake 100 mesh sieves.
The adsorption effect of the gac that the present invention makes is higher than common gac far away, is higher than existing gac especially far away for the adsorption effect of metal ion.Confirmed that by processing spartina alterniflora loisel's gac of gained of the present invention has good removal effect to cadmium ion among the embodiment to cadmium wastewater.
Invention from spartina alterniflora loisel's stalk, produce the method that gac is administered cadmium wastewater, utilize the invasive species spartina alterniflora loisel of seashore, adopt phosphoric acid activation method to produce the activated carbon treatment cadmium wastewater.Contain a large amount of salinities among the spartina alterniflora loisel, directly utilize it to produce gac as raw material, separating out of inorganic salt will produce bigger influence to follow-up wastewater treatment, so before utilizing phosphoric acid activation, adopt sulphuric acid soln to carry out pre-treatment, dissolve wherein most of salinity, wherein a part of organic composition is removed in hydrolysis simultaneously, for example alcohols, carboxylic-acid etc., these compositions are because oxygen level than higher, easily forms hydrocarbon with charcoal in the pyritous condition, thus the output of reduction gac.Pretreated spartina alterniflora loisel's powder is added phosphate impregnation (utilize the method for phosphoric acid activation method with respect to other, have technology have pollution less, advantage such as carbonization temperature is low, and its yield compares higher), after the compounding substances drying behind the phosphate impregnation, raw material as high-temperature activation, what present method adopted is that charing and activation are carried out simultaneously, can effectively utilize the energy, reduced the step of operation, experimental results show that, the charcoal absorption cadmium ion that adopts this method to produce can reach good removal effect.The gac of producing has obtained activated carbon product through washing, purifying after the drying.Utilize this gac to substitute commercial activated carbon treatment cadmium wastewater, can reach good treatment effect.
A kind of method that gac is administered cadmium wastewater of from spartina alterniflora loisel's stalk, producing of the present invention, removed the interference of a large amount of salinities, produced the abundant activated carbon product of surface functional group, yield is between 42%～48%, utilize this activated carbon treatment cadmium wastewater, loading capacity is higher than general commercial gac from far away between 11～48.25mg/g, utilize waste fully, created considerable economic, good social benefit and environmental effect.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below by example in detail processing step of the present invention.
Embodiment 1
(1) spartina alterniflora loisel is dried in the shade, get stem, in 120 ℃ of oven dry down of baking oven, pulverizer is pulverized, and crosses 100 mesh sieves.
(2) utilize 1% (mass ratio) sulphuric acid soln leaching spartina alterniflora loisel powder, wherein the mass ratio of sulphuric acid soln and rice grass is 1: 10, and the reaction times is 4h.
(3) solidliquid mixture filters, and filter residue injects phosphoric acid solution, and wherein the mass ratio of phosphoric acid and former dried rice grass is 1: 1, and reaction is to be 12h the time.
(4) phosphoric acid rice grass mixture in the tube type resistance furnace of packing into, is feeding N after oven dry under 120 ℃
2Activate under the condition, wherein calcining temperature is 700 ℃, and intensification is 5 ℃/min, is 2h at 700 ℃ of following calcination times.
(5) gac that utilizes clear water washing calcining to obtain, heated and boiled is washed till near neutral, and drying is pulverized, and crosses 100 mesh sieves, obtains the finished product gac, yield 43%.
The activated carbon product that is obtained by present embodiment is 48.25mgCd for the loading capacity of cadmium
2+/ mg gac, the adsorption efficiency of the cadmium-containing solution of 20mg/L are more than 99%, and it is 0.05mg/L that the cadmium-containing solution of 10mg/L is handled the back strength of solution, has reached national grade one discharge standard.
Embodiment 2:
Other condition is constant, changes the temperature in embodiment 1 (4) into 600 ℃, final yield 45%.
The activated carbon product that is obtained by present embodiment is 41.37mgCd for the loading capacity of cadmium
2+/ mg gac, the adsorption efficiency of the cadmium-containing solution of 20mg/L are more than 98.9%, and it is 0.07mg/L that the cadmium-containing solution of 10mg/L is handled the back strength of solution, has reached national grade one discharge standard.
Embodiment 3:
Other condition is constant, changes the reaction times in embodiment 1 (3) into 20h, changes the temperature in embodiment 1 (4) into 500 ℃, final yield 47%.
The activated carbon product that is obtained by present embodiment is 28.1mgCd for the loading capacity of cadmium
2+/ mg gac, the adsorption efficiency of the cadmium-containing solution of 20mg/L are more than 96.1%, and it is 0.07mg/L that the cadmium-containing solution of 10mg/L is handled the back strength of solution, has reached national grade one discharge standard.
Embodiment 4
Other condition is constant, changes sulphuric acid soln mass content in embodiment 1 (2) into 2%, changes the injection ratio in embodiment 1 (3) into 0.5: 1, and the temperature in embodiment 1 (4) changes 500 ℃ into.
The activated carbon product that is obtained by present embodiment is 21.62mgCd for the loading capacity of cadmium
2+/ mg gac, the adsorption efficiency of the cadmium-containing solution of 12mg/L are more than 86%, and it is 0.132mg/L that the cadmium-containing solution of 6mg/L is handled the back strength of solution.
Embodiment 5:
Other condition is constant, changes the reaction times in embodiment 1 (2) into 7h, and the injection ratio in embodiment 1 (3) changes 2: 1 into, and (4) temperature of embodiment 1 changes 500 ℃ into.
The activated carbon product that is obtained by present embodiment is 22.36mgCd for the loading capacity of cadmium
2+/ mg gac, the adsorption efficiency of the cadmium-containing solution of 13mg/L are more than 87%, and it is 0.176mg/L that the cadmium-containing solution of 6mg/L is handled the back strength of solution.
Embodiment 6:
Other condition is constant, changes the injection ratio in embodiment 1 (3) into 3: 1, and (4) temperature of embodiment 1 changes 500 ℃ into.
The activated carbon product that is obtained by present embodiment is 11.7mgCd for the loading capacity of cadmium
2+/ mg gac, the adsorption efficiency of the cadmium-containing solution of 12mg/L are more than 50%.
Embodiment 7:
Other condition is constant, changes the injection ratio in embodiment 1 (3) into 1: 1, and (4) temperature of embodiment 1 changes 400 ℃ into, and calcination time changes 3h into, final yield 48%.
The activated carbon product that is obtained by present embodiment is 11mgCd for the loading capacity of cadmium
2+/ mg gac, the adsorption efficiency of the cadmium-containing solution of 6mg/L are more than 66%.
Claims (5)
1. the spartina alterniflora loisel's preparation method of active carbon that can administer cadmium wastewater, it comprises the steps:
Step 1: with oven dry of spartina alterniflora loisel's stem and pulverizing;
Step 2: with mass content is spartina alterniflora loisel's powder 1～10h after the leaching of 0.1～10% sulphuric acid soln is pulverized; Wherein the mass ratio of the spartina alterniflora loisel's powder after sulphuric acid soln and the pulverizing is 1: 5～15;
Step 3: filter the solidliquid mixture after leaching, filter residue is injected phosphoric acid solution flood 6～30h;
Step 4: the phosphoric acid rice grass mixture oven dry after will flooding, at N2 protection and 400～700 ℃ of following calcining and activating 0.5～10h;
Step 5: the gac that the washing calcining obtains is also pulverized.
2. preparation method according to claim 1 is characterized in that the bake out temperature in the step 1 is 100～120 ℃, is crushed to particle diameter less than 150 orders.
3. preparation method according to claim 1, the mass ratio of the spartina alterniflora loisel's powder after it is characterized in that phosphoric acid in the step 3 and pulverizing is 0.3: 1～3: 1, dipping time is 12～24h.
4. preparation method according to claim 1 is characterized in that bake out temperature is 100～120 ℃ in the step 4, and the calcining and activating time is 1～4h.
5. preparation method according to claim 1 is characterized in that in the step 5 that gac that the washing calcining obtains to pH5～7, is crushed to particle diameter less than 150 orders.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008101242619A CN101306813B (en) | 2008-07-04 | 2008-07-04 | Method for preparing smooth cord-grass active carbon for treating cadmium-containing waste water |
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| CN2008101242619A CN101306813B (en) | 2008-07-04 | 2008-07-04 | Method for preparing smooth cord-grass active carbon for treating cadmium-containing waste water |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101857225A (en) * | 2010-06-30 | 2010-10-13 | 福建师范大学 | Method for preparing activated carbon with waste canna slag |
| CN102872800B (en) * | 2011-07-11 | 2015-05-20 | 北京联合大学生物化学工程学院 | Preparation method of heavy metal mercury-enriched material |
| CN102602913A (en) * | 2012-03-23 | 2012-07-25 | 上海大学 | Preparation method of biochar |
| CN102600799A (en) * | 2012-03-23 | 2012-07-25 | 上海大学 | Method for treating wasterwater containing copper by utilizing Spartina alterniflora Loisel-based biochar |
| CN102698724B (en) * | 2012-04-06 | 2014-11-05 | 淮北市大华活性炭有限公司 | Method for producing active carbon for gasoline vapor adsorption |
| CN104016512B (en) * | 2014-06-10 | 2016-01-13 | 上海大学 | A kind of method utilizing spartina alterniflora loisel's base charcoal Treatment of Copper waste water |
| CN104030286A (en) * | 2014-06-25 | 2014-09-10 | 无锡市崇安区科技创业服务中心 | Spartina alterniflora straw active carbon and preparation method thereof |
| CN104549154B (en) * | 2015-01-23 | 2017-07-07 | 浙江大学 | The preparation method of the charcoal of cadmium in the safe adsorbed water body of energy |
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