CN109603747A - Modified coconut husk charcoal, and preparation method thereof and absorption heavy metal method - Google Patents
Modified coconut husk charcoal, and preparation method thereof and absorption heavy metal method Download PDFInfo
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- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- 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
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- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
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Abstract
The present invention relates to modified coconut husk charcoals and its preparation method and application.Modified coconut husk charcoal is the coconut husk charcoal for being connected with Halogen group elements, and micropore is distributed in coconut husk biology carbon surface, and micro-pore diameter size is 2~3nm；The specific surface area of coconut husk charcoal is 1000~1300m2/g.The step of preparation method of modified coconut husk charcoal is to be placed in coconut husk charcoal in the halide solution that mass concentration is 3~7%, is washed after impregnating and stirring 1~5 hour and dry.The method of modified coconut husk charcoal absorption heavy metal, the modification coconut husk charcoal that granular size is 120~200 purposes is placed in the mixture containing heavy metal, and temperature is 30~100 DEG C.Modified coconut husk charcoal and heavy metal are greater than 20:3 by weight.Modified coconut husk charcoal prepared by the present invention has high-specific surface area and high pore volume, has stronger adsorption capacity.
Description
Technical field
The present invention relates to coconut husk charcoals and preparation method thereof, belong to coconut husk charcoal field.
Background technique
Charcoal, but can be described as biomass carbon (biochar) is got by the abbreviation of English word biocharacoal
, and when 2007 in the charcoal meeting held of Australia by Uniform Name.International bio charcoal action group
Knit (InternationalBiocharInitiative, IBI) define charcoal be it is a kind of by biomass material limit oxygen item
The solid matter being prepared under part through pyrolysis charring.William in 2009 publish an article on " Cell " by " charcoal and its
Using " it is chosen as one of global the Fifteenth National Congress environmental issue in 2010.
Active carbon is a kind of adsorbent most widely used so far, but with natural resources such as coal mine, forests
Scarcity, the cost for preparing active carbon is higher and higher, therefore develops the novel adsorbent of one kind and compel to replace active carbon to seem in eyebrow
Eyelash.Charcoal has the characteristics that raw material sources are extensive, cheap, porosity is big, specific surface area is high, strong adsorption, gradually at
For focus concerned by people.
In the prior art, preparing coconut husk charcoal as raw material using coconut husk has: with CO2For activator, the results showed that in work
Changing temperature is 900 DEG C, and activation time is 240min and CO2The flow velocity of gas is in 800cm3High-ratio surface has been prepared when/min
Long-pending coconut husk charcoal.But required activation time is also long, at high cost, the micropore size of charcoal is distributed more difficult control
System, charcoal specific surface area obtained and Kong Rong be not high, so that the application of charcoal can be limited to a certain extent.
Summary of the invention
(1) technical problems to be solved
In order to solve the above problem of the prior art, the present invention provides a kind of modification coconut husk charcoal of strong adsorption；
Correspondingly, the present invention provides a kind of preparation method of the modification coconut husk charcoal of strong adsorption；
Correspondingly, the present invention provides a kind of strong adsorption and can remove the modification coconut husk charcoal of different pollutants；
Correspondingly, the present invention provides a kind of strong adsorption and the system of the modification coconut husk charcoal that can remove different pollutants
Preparation Method.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include:
A kind of modified coconut husk charcoal is the coconut husk charcoal for including halogen group.The coconut husk biology carbon surface
Micropore is distributed with, the micro-pore diameter size is 2~3nm；The specific surface area of coconut husk charcoal is 1000~1300m2/g。
In the technical program, halogen group is modified on modified coconut husk charcoal first passage coconut husk charcoal, keeps it common
The chemisorption of physisorption and halogen group with coconut husk charcoal makes it show extremely strong absorption and makees
With especially for heavy metal ion or heavy metal simple substance, halogen group is preferably-Cl and-I.The adsorption process of charcoal
Related with the surface nature of charcoal, the micropore specific area of adsorption capacity and charcoal is proportional, high-specific surface area and
The carbonaceous material of pore volume is applied to always in absorption organic pollutant.In the technical program, coconut husk biology carbon surface it is micro-
Pore diameter size is 2~3nm；The specific surface area of coconut husk charcoal is 1000~1300m2/ g, the Kong Rong of coconut husk biology carbon surface
For 0.50~0.7cm3/ g reaches most preferably with the synergistic effect of Halogen group elements, can enhance the chemical adsorption capacity of halogen group.
For the modification coconut husk charcoal for preparing this programme, compared with the existing technology, the cost paid is low, that is, pays lower cost system
The modification coconut husk charcoal of higher specific surface area and Kong Rong in standby this programme, and the ability with stronger absorption pollutant.
A kind of preparation method of modified coconut husk charcoal comprising following steps impregnate coconut husk charcoal through halide
Modification forms.
The improvement of the preparation method of the modified coconut husk charcoal of the present invention comprising following steps: coconut husk charcoal is placed in
It in the halide solution that mass concentration is 3~7%, impregnates and is washed after stirring 1~5 hour, it is raw that modified coconut husk is obtained after dry
Object charcoal.
In the technical program, coconut husk charcoal deionized water constant temperature at 70~90 DEG C stirs 3~5 hours to remove powder
The residual impurity of dirt and coconut husk biology carbon surface uses deionized water filtration washing after stirring.Dry 15 at 100~120 DEG C~
Pretreated coconut husk charcoal is obtained after 30 hours；It is by weight to set at 1: 0.5~1: 3 by pretreated coconut husk charcoal
After being impregnated in the halide solution that mass concentration is 3~7%, after being washed repeatedly with deionized water, modified coconut husk biology
Charcoal is placed in 100~120 DEG C of vacuum oven 15~30 hours dry.Coconut husk charcoal and halide in the technical program
Modified, adsorption capacity is greatly improved.
The improvement of the preparation method of the modified coconut husk charcoal of the present invention, the halide are lodine chloride, potassium iodide or chlorination
One of potassium or two or more combinations.Halide is preferably iodine monochloride.
The improvement of the preparation method of the modified coconut husk charcoal of the present invention, the coconut husk charcoal are mainly living through chemistry by coconut husk
Change is made.
The improvement of the preparation method of the modified coconut husk charcoal of the present invention, the preparation of the coconut husk charcoal: coconut husk is placed in
It is kept for 3~7 hours under 250~310 DEG C of environment, and is soaked in CaCl218~20 hours in solution, addition activator, 30~70
After being stirred 1~3 hour at DEG C, N2Lower sealing is kept for 1~3 hour at 40~70~90 DEG C, and acid solution is cleaned to neutrality
After filter, it is dry at 100~120 DEG C.
In the technical program, selected coconut husk is mechanically pulverized at after powdered after shining in the sun 2~3 days, then is placed in
It is reacted 3~7 hours in 250~310 DEG C of Muffle furnace.Wherein, CaCl2The mass concentration of solution is 20~30%.It will be through superchlorination
Coconut husk after calcium solution immersion, is repeatedly washed with secondary distilled water, and it is small to be placed in baking oven baking 5~7 at 100~120 DEG C
When, the coconut husk after drying mixes in mass ratio for 1:2~1:6 respectively with KOH activator.Wherein, acid solution is 0.1~0.4M
HCl solution, in cleaning, need to be slowly added dropwise, the dry time is 5~10h at 100~120 DEG C, and modified coconut palm is obtained after dry
Shell charcoal, and be sealed, the modification coconut husk charcoal hole prepared by the method for the invention holds and micropore specific area is steady
It is fixed.
A kind of modification coconut husk charcoal of any of the above-described scheme adsorbs the application of following substance as adsorbent: (1) weight
Metal；(2) organic pollutant；(3) zwitterion pollutant；(4) dyestuff contaminant；(5) antibiotic.
A kind of method that modified coconut husk charcoal adsorbs heavy metal as adsorbent comprising following steps are big by particle
Small is that the modification coconut husk charcoal in any of the above-described scheme of 120~200 purposes is placed in the mixture containing heavy metal, keeps temperature
Degree is 30 DEG C~100 DEG C, and time 5min or more is adsorbed.
The improvement of the method for adsorbing metal of the present invention, the modified coconut husk charcoal are greater than by weight with heavy metal
20:3。
A kind of modified coconut husk charcoal is the coconut husk charcoal for including halogen group and amino；The coconut husk biology
Micropore is distributed in carbon surface, and the micro-pore diameter size is 2~3nm；The specific surface area of coconut husk charcoal is 1000~1300m2/
g.Halogen group is preferably-Cl and-I.
It is preferable to the removal effect of cationic pollutant since coconut husk biology carbon surface is negatively charged, but to anion dirt
The removal effect for contaminating object is very poor, changes the charge of coconut husk biology carbon surface institute band by the effect of Halogen group elements and amino,
Make it while there is removal zwitterion pollutant, and the ability with physical absorption and chemisorption pollutant, can be used for
Except pollutant different in environment.Wherein, coconut husk charcoal is environmental waste, realizes turning waste into wealth for coconut husk.
The preparation method of above-mentioned modified coconut husk charcoal comprising following steps:
S1: the nitration of coconut husk charcoal:
(1) coconut husk charcoal is placed in the halide solution that mass concentration is 3~7%, impregnates and stirs 1~5 hour
After wash, just coconut husk charcoal is obtained after dry；
(2) preparation of mixed acid solution: in 0 DEG C of ice bath, by concentration be 17~18mol/L sulfuric acid by volume
It is to be uniformly mixed in the nitric acid solution of 15~16mol/L that concentration, which is added, for 1:0.5~2；
S2: first coconut husk charcoal is added in mixed acid solution by mass volume ratio for 10g:100ml, at 0 DEG C
Under the conditions of stir 40~60min, filtrate is obtained by filtration；Be washed with water repeatedly until filtrate be neutrality until, be placed in 80~95
It is dry at DEG C, obtain modified coconut husk charcoal.
(3) beneficial effect
The beneficial effects of the present invention are:
1. the method for the present invention synthesizes coconut husk charcoal, there is high-specific surface area and high pore volume, pollutant is adsorbed
Capacity is big, and adsorption effect is good.
2. the present invention is modified the coconut husk charcoal of the method for the present invention preparation using halide for the first time, improves heavy metal, has
The adsorptivity of the substances such as machine pollutant, zwitterion pollutant, dyestuff, antibiotic.The modified coconut husk charcoal of the present invention can be real
Now continuous absorption.
3. our experiments show that: the removal effect of modified coconut husk charcoal counterweight metal simple-substance and heavy metal ion is obvious
All substantially increased than unmodified.Unmodified coconut husk charcoal counterweight metal simple-substance and the removal rate of heavy metal ion difference
For 12.3% and 57.4%, and the removal effect of modified coconut husk the charcoal counterweight metal simple-substance and heavy metal ion of iodine monochloride
Reach 100%, the coconut husk charcoal effect more modified than potassium iodide and potassium chloride will be good.Counterweight metal simple-substance at high temperature
It still maintains good removal rate and goes removal effect after removing heavy metals simple substance also to have no decline at continuous ten times.Iodine monochloride
Modified coconut husk charcoal, which is significantly larger than common adsorbent to the removal rate of heavy metal ion, may be up to 20 times, and to heavy metal
The adsorption capacity of ion has reached 231.5mg/g.
Detailed description of the invention
Fig. 1 is modified coconut husk charcoal dosage to Hg0Removal effect；
Fig. 2 is modified coconut husk charcoal at different temperatures to Hg0Removal effect；
Fig. 3 is that different coconut husk charcoals continuously remove Hg0Effect；
Fig. 4 is removal effect of the different coconut husk charcoals to mercury ion；
Fig. 5 is removal effect of the CSBC-ICl to different initial concentration mercury ions；
Fig. 6 is removal effect of the CSBC-ICl to mercury ion of different-grain diameter；
Fig. 7 is CSBC-ICl under different temperatures to the removal effect of mercury ion；
Fig. 8 is maximum adsorption capacity of the CSBC-ICl to mercury ion；
Fig. 9 is removal effect comparison diagram of the different adsorbents to mercury ion.
Specific embodiment
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
Embodiment 1: the preparation of modified coconut husk charcoal
The preparation method of the modified coconut husk charcoal of embodiment 1.1 the following steps are included:
Step 1: coconut husk charcoal is prepared；
It is mechanically pulverized after coconut husk being shone in the sun 3 days at after powdered, then is placed in 280 DEG C of Muffle furnace and reacts 3 hours,
And it is soaked in the CaCl that mass concentration is 30%219 hours in solution, is repeatedly washed, be placed in baking oven with secondary distilled water
It is toasted 7 hours at 100 DEG C, the coconut husk after drying mixes in mass ratio for 1:4 respectively with KOH activator, stirs 3 hours at 30 DEG C
Afterwards, N in reaction kettle2Lower sealing keeps 1 hour at 60 DEG C to activate.After activation, it is slowly added dropwise using the HCl solution of 0.4M
Cleaning to neutrality filters, and dry 5h at 110 DEG C, obtains coconut husk charcoal after filtering.
Step 2: coconut husk charcoal is modified；
By the coconut husk charcoal deionized water of step 1 preparation, constant temperature stirs 4 hours to remove dust and coconut palm at 90 DEG C
The residual impurity of shell biology carbon surface uses deionized water filtration washing after stirring, obtain pre- place after 30 hours dry at 100 DEG C
The coconut husk charcoal of reason；By pretreated coconut husk charcoal be by weight 1: 1 be placed in mass concentration be 3% halide solution
In, after soaking and stirring 5 hours, after being washed repeatedly with deionized water, drying 15 hours in 110 DEG C of vacuum oven is placed in, are obtained
To modified coconut husk charcoal.
Micropore is distributed in its surface of coconut husk charcoal of above method preparation, and the micro-pore diameter size is 2nm；It is described micro-
The Kong Rongwei 0.50cm in hole3/g；The specific surface area of coconut husk charcoal is 1300m2/g。
Embodiment 1.2: the preparation method of modified coconut husk charcoal the following steps are included:
Step 1: coconut husk charcoal is prepared；
It is mechanically pulverized after coconut husk being shone in the sun 2 days at after powdered, then is placed in 310 DEG C of Muffle furnace and reacts 5 hours,
And it is soaked in the CaCl that mass concentration is 20%220 hours in solution, is repeatedly washed, be placed in baking oven with secondary distilled water
It is toasted 5 hours at 110 DEG C, the coconut husk after drying mixes in mass ratio for 1:6 respectively with KOH activator, stirs 1 hour at 50 DEG C
Afterwards, N in reaction kettle2Lower sealing keeps 2 hours at 80 DEG C to activate.After activation, it is slowly added dropwise using the HCl solution of 0.1M
Cleaning to neutrality filters, and dry 8h at 120 DEG C, obtains coconut husk charcoal after filtering.
Step 2: coconut husk charcoal is modified；
By the coconut husk charcoal deionized water of step 1 preparation, constant temperature stirs 5 hours to remove dust and coconut palm at 70 DEG C
The residual impurity of shell biology carbon surface uses deionized water filtration washing after stirring, obtain pre- place after 15 hours dry at 110 DEG C
The coconut husk charcoal of reason；By pretreated coconut husk charcoal be by weight 1: 3 be placed in mass concentration be 5% halide solution
In, after soaking and stirring 1 hour, after being washed repeatedly with deionized water, drying 20 hours in 120 DEG C of vacuum oven is placed in, are obtained
To modified coconut husk charcoal.
Micropore is distributed in its surface of coconut husk charcoal of above method preparation, and the micro-pore diameter size is 2nm；It is described micro-
The Kong Rongwei 0.647cm in hole3/g；The specific surface area of coconut husk charcoal is 1224m2/g。
Embodiment 1.3: the preparation method of modified coconut husk charcoal the following steps are included:
Step 1: coconut husk charcoal is prepared；
It is mechanically pulverized after coconut husk being shone in the sun 2.5 days at after powdered, then to be placed in reaction 7 in 250 DEG C of Muffle furnace small
When, and it is soaked in the CaCl that mass concentration is 25%218 hours in solution, is repeatedly washed with secondary distilled water, be placed in baking oven
In toast 6 hours at 120 DEG C, the coconut husk after drying mix in mass ratio for 1:2 respectively with KOH activator, and stirring 2 is small at 70 DEG C
Shi Hou, N in reaction kettle2Lower sealing keeps 3 hours at 40 DEG C to activate.After activation, slowly dripped using the HCl solution of 0.2M
Cleaning to neutrality is added to filter, dry 5~10h at 100~120 DEG C, obtains coconut husk charcoal after filtering.
Step 2: coconut husk charcoal is modified；
By the coconut husk charcoal deionized water of step 1 preparation, constant temperature stirs 5 hours to remove dust and coconut palm at 70 DEG C
The residual impurity of shell biology carbon surface uses deionized water filtration washing after stirring, obtain pre- place after 15 hours dry at 110 DEG C
The coconut husk charcoal of reason；By pretreated coconut husk charcoal be by weight 1: 3 be placed in mass concentration be 5% halide solution
In, after soaking and stirring 1 hour, after being washed repeatedly with deionized water, drying 20 hours in 120 DEG C of vacuum oven is placed in, are obtained
To modified coconut husk charcoal.
Micropore is distributed in its surface of coconut husk charcoal of above method preparation, and the micro-pore diameter size is 2nm；It is described micro-
The Kong Rongwei 0.7cm in hole3/g；The specific surface area of coconut husk charcoal is 1200m2/g。
Wherein, halide is preferably lodine chloride (ICl), potassium iodide (KI) and potassium chloride (KCl) solution.
The coconut husk charcoal that the present embodiment 1.1-1.3 uses lodine chloride (ICl) modified, is denoted as CSBC-ICl；Potassium iodide
(KI) modified coconut husk charcoal, is denoted as CSBC-KI；Using the modified coconut husk charcoal of KCl, it is denoted as CSBC-KCl；Step 1
The modified coconut husk charcoal of step 2 that do not carry out being prepared is denoted as CSBC.
Embodiment 2:
Modified coconut husk charcoal is to change prepared by the embodiment of the present invention 1.1 as the method for adsorbent absorption heavy metal
Property coconut husk charcoal, which is placed in the mixture containing heavy metal, to be adsorbed.
The CSBC- of the preparation of the embodiment of the present invention 1 of accurate weighing 3.0,5.0,10.0,15.0,20.0,25.0mg respectively
ICl, CSBC-KI, CSBC-KCl, CSBC carry out dress column, measurement different amounts match the ability of lower Adsorption of Mercury simple substance, wherein mercury
Initial mass is 0.5 μ g.The partial size of CSBC-ICl, CSBC-KI, CSBC-KCl, CSBC as adsorbent: 120-200 mesh is inhaled
Enclosure temperature: 30 DEG C.
Measurement result is as shown in Figure 1.
The removal effect of CSBC-ICl is best as can be known from Fig. 1, and the removal effect for reaching 100%, CSBC-KI is taken second place,
When the content of CSBC-KI is 15mg, removal rate has also reached 100%.With the increase of adsorbent amount, coconut husk charcoal
Removal rate also slowly rise, but KCl modified coconut husk charcoal CSBC-KCl and unmodified coconut husk charcoal CSBC
Overall removal effect slightly poor do not surpass 50%.
As shown in Figure 1, the removal effect of unmodified coconut husk charcoal is worst, may be unmodified coconut husk charcoal
Active site on surface is few, the suction-operated to mercury simple substance be only rely on physical absorption, and it is halogen modified after increase coconut palm
The active site of shell biology carbon surface.
Hg0Active site by catalysis oxidation be Hg2+, halogen meeting and Hg2+In conjunction with enhancing adsorption capacity, to improve de-
Mercury ability.Wherein iodine is easier to react the high-valence state mercury compound for generating and easily removing with Elemental Mercury, and adsorption process therein is main
Based on chemisorption, supplemented by physical absorption, thus the adsorption capacity of mercury simple substance is increased substantially, oxidation of the iodine to mercury simple substance
Performance is more superior than other halogens, due between the london dispersion force transition state formed and gas molecule between mercury simple substance and iodine
Stable HgI can be formed after collision2, there is stronger Adsorption effect.Therefore CSBC-KI ratio CSBC-KCl is to mercury simple substance
Removal effect is more preferable, while finding the polymer modified CSBC-ICl of chlorosulfonylation to the adsorption effect of mercury simple substance than two kinds of modifications of appeal
Coconut husk charcoal effect is all good, illustrates that combining two kinds (iodine, chlorine) has the substance preparation compared with strong affinity effect to mercury simple substance
Adsorbent is more preferable to the removal effect of mercury simple substance.
Embodiment 3:
Modified coconut husk charcoal is to change prepared by the embodiment of the present invention 1.2 as the method for adsorbent absorption heavy metal
Property coconut husk charcoal, which is placed in the mixture containing heavy metal, to be adsorbed.
CSBC-ICl, CSBC-KI, CSBC-KCl, CSBC prepared by the embodiment of the present invention 1 of accurate weighing 5.0mg respectively
Dress column is carried out, measures the ability of Adsorption of Mercury simple substance under different temperatures, wherein the initial mass of mercury is 0.5 μ g.CSBC-ICl,
The partial size of CSBC-KI, CSBC-KCl, CSBC as adsorbent: 120-200 mesh, dosage: 5mg, Elemental Mercury quality: 0.5 μ g.
As shown in Fig. 2, coconut husk charcoal is modified at a temperature of differential responses to the removal rate of mercury simple substance, as a result, it has been found that with
The removal rate of the raising of temperature, four kinds of coconut husk charcoals is declined, this may be since coconut husk charcoal removes removal of mercury simple substance
During existing physical absorption have chemisorption again, and chemisorption is exothermic reaction, therefore as the rising of temperature is adsorbed
Product can decompose to be begun to decline so as to cause mercury simple substance removal rate.
The removal rate of CSBC-ICl has reached 100% between 30 DEG C to 100 DEG C, this may be due to coconut husk biology
The adsorption capacity of charcoal itself is strong, under the influence of increasing the decline of temperature adsorption ability, is still able to maintain very high removal rate.And from
Removal rate is begun to decline after 100 DEG C, this may be because the temperature of reaction has reached the boiling point of iodine monochloride, so that being supported
ICl is detached from coconut husk charcoal and enters directly into gas on coconut husk charcoal, so that suction of the CSBC-ICl to mercury simple substance
Attached removal effect is declined.It can be found that the lasting raising with temperature, the decline degree ratio CSBC- of CSBC-ICl simultaneously
The small and whole removal rate that KI, CSBC-KCl and CSBC come is more much higher than them.Therefore, CSBC-ICl can remove height
Mercury simple substance in warm coal-fired flue-gas.
Embodiment 4:
Modified coconut husk charcoal is to change prepared by the embodiment of the present invention 1.3 as the method for adsorbent absorption heavy metal
Property coconut husk charcoal, which is placed in the mixture containing heavy metal, to be adsorbed.
CSBC-ICl, CSBC-KI, CSBC-KCl, CSBC prepared by the embodiment of the present invention 1 of accurate weighing 5.0mg respectively
Carry out dress column, measure the ability of Adsorption of Mercury simple substance under different read-around ratios, wherein CSBC-ICl, CSBC-KI, CSBC-KCl,
Partial size of the CSBC as adsorbent: 120-200 mesh, dosage: 5mg, Elemental Mercury quality: 0.5 μ g, adsorption temp: 30 DEG C
As shown in figure 3, the removal rate of CSBC-ICl is stable 100% with the increase of read-around ratio, illustrate the biology
The mercury simple substance content adsorbed on charcoal is much also not up to saturated.And the removal effect of other three kinds of coconut husk charcoals under
Drop.Illustrating as the mercury simple substance content of absorption is more and more on these three charcoals, the active site on surface is opposite to be also reduced,
Adsorption effect is also just gradually reduced.Mercury simple substance is constantly adsorbed to surface by coconut husk charcoal, and the mercury simple substance adsorbed is with non-
Often fast speed is aoxidized by ICl, i.e. ICl can promptly be reacted with the mercury simple substance for being attracted to coconut husk biology carbon surface, by it
It is oxidized to mercury ion.Therefore coconut husk charcoal ICl modified in the adsorption process of continuous several times is able to maintain 100% removal of mercury
Efficiency.
Therefore, CSBC-ICl, CSBC-KI prepared by the present invention have good removal effect to mercury simple substance, and removal rate reaches
100% can be reached.Wherein the effect of CSBC-ICl is best, is much higher than unmodified coconut husk charcoal, and at high temperature to mercury list
Matter also has very high removal rate.Removal rate also has no decline after continuous absorption ten times, experiments have shown that CSBC-ICl is a kind of
Effective mercury simple substance adsorbent.
Embodiment 5:
Modified coconut husk charcoal is to change prepared by the embodiment of the present invention 1.1 as the method for adsorbent absorption heavy metal
Property coconut husk charcoal, which is placed in the mixture containing heavy metal, to be adsorbed.
The 120-200 mesh for adding 20mg embodiment 1 to prepare respectively in the centrifuge tube containing 10mL 100ppm mercury ion solution
After CSBC-ICl, CSBC-KI, CSBC-KCl, CSBC vibrate 10min at room temperature, supernatant is detected, calculates removal rate.Wherein,
Ion concentration of mercury: 100ppm, adsorption temp: 25 DEG C, adsorption time: 10min.
As shown in figure 4, CSBC-ICl has reached 100% to the removal rate of mercury ion, and CSBC-KI, CSBC-KCl and
The removal rate of CSBC is only between 60%-70%.Therefore through halogen modified coconut husk charcoal than unmodified coconut husk charcoal
Effect will be got well.CSBC is more to rely on physical action to the removal effect of mercury ion, and be modified coconut husk charcoal to mercury from
There are also chemical actions other than having physical action for son, and overall effect is greater than the chemisorption of simple halogen.
Embodiment 6:
Modified coconut husk charcoal is to change prepared by the embodiment of the present invention 1.2 as the method for adsorbent absorption heavy metal
Property coconut husk charcoal, which is placed in the mixture containing heavy metal, to be adsorbed.
It is separately added into the centrifuge tube of the 120-200 mesh CSBC-ICl prepared containing 1 method of 20mg embodiment different dense
The mercury ion solution 10mL of degree after vibrating 10min at room temperature, detects supernatant, calculates removal rate, it is initial to compare different mercury ions
To the adsorption effect of mercury ion under concentration.
As shown in figure 5, the removal rate of CSBC-ICl has reached 100%, explanation when ion concentration of mercury is less than 300ppm
Mercury ion in solution is all chlorinated the active site of the modified coconut husk biology carbon surface of iodine and intrapore adsorption potential is adsorbed,
It is a chemisorption and the process that physical absorption coexists.And when mercury ion initial concentration is greater than 300ppm, with dense
The increase removal rate of degree gradually decreases, and illustrates that coconut husk charcoal absorption mercury ion tends to be saturated, and excessive concentration is unfavorable for adsorbing.
Embodiment 7:
Modified coconut husk charcoal is to change prepared by the embodiment of the present invention 1.3 as the method for adsorbent absorption heavy metal
Property coconut husk charcoal, which is placed in the mixture containing heavy metal, to be adsorbed.
The CSBC-ICl charcoal that the present embodiment takes 1 method of embodiment of three kinds of different-grain diameters to prepare respectively, comparison biology
Influence of the charcoal partial size to mercury ion adsorption effect.It is separately added into the centrifuge tube containing 10mL 300ppm mercury ion solution
The CSBC-ICl of 20mg 50-80 mesh, 80-120 mesh and 120-200 mesh after vibrating 10min at 25 DEG C, detects supernatant, meter
Calculate removal rate.
As shown in fig. 6, the particle size of coconut husk charcoal is different, also different to the removal effect of mercury ion, particle is smaller,
Removal effect is better.It is reachable to the removal rate of 300ppm mercury ion solution when the partial size of CSBC-ICl is 120-200 mesh
100%.The partial size of coconut husk charcoal is smaller, can accelerate the mass transport process between adsorbent and adsorbate in oscillatory process, from
And coconut husk charcoal is increased to the Adsorption efficiency of mercury ion.
Embodiment 8
Modified coconut husk charcoal is to change prepared by the embodiment of the present invention 1.1 as the method for adsorbent absorption heavy metal
Property coconut husk charcoal, which is placed in the mixture containing heavy metal, to be adsorbed.
The CSBC-ICl and 10mL of the 120-200 mesh of 1 method of 20mg embodiment preparation is added in the present embodiment in centrifuge tube
The mercury ion solution of 300ppm after vibrating 10min at different temperatures respectively, detects supernatant, calculates removal rate.
In Fig. 7 as can be seen that in the range of 25 DEG C to 45 DEG C, as the temperature rises, removal effect does not change
Reach 100%, it may be possible to the reason is that the raising of reaction temperature can accelerate in solution mercury ion to modified coconut palm to a certain extent
The movement of shell charcoal adsorption site, therefore removal rate remains to be maintained at 100% without declining.And the suction from 45 DEG C to 65 DEG C
Removal rate has decreased to 91.20~30% from 100% during attached, it may be possible to although can accelerate between substance because temperature is excessively high
Mass transport process, but can also accelerate the desorption behavior of mercury ion, so that removal effect be caused to decline.In view of actual application
It will be using 25 DEG C of room temperature as adsorption temp.
Embodiment 9
Modified coconut husk charcoal is to change prepared by the embodiment of the present invention 1.2 as the method for adsorbent absorption heavy metal
Property coconut husk charcoal, which is placed in the mixture containing heavy metal, to be adsorbed.
The present embodiment is separately added into 10mL various concentration in the centrifuge tube containing 20mg 120-200 mesh CSBC-ICl
Mercury ion solution.After vibrating 12h at 25 DEG C, supernatant is detected, calculates adsorption capacity.
As can be seen that in the case where fixed absorbent dosage in Fig. 8, when ion concentration of mercury 50ppm-600ppm, absorption
Capacity enhances with the increase of ion concentration of mercury.When concentration is greater than 600ppm, adsorption capacity reaches saturation and levels off to
231.5mg/g.The furol biological charcoal specific surface area that Yardim et al. is prepared using dense sulfuric acid treatment reaches 1100m2/ g, to mercury from
The saturated adsorption capacity of son is 174mg/g, and CSBC-ICl prepared by the present invention to the removal effect of mercury ion more preferably.
Embodiment 10
Modified coconut husk charcoal is to change prepared by the embodiment of the present invention 1.3 as the method for adsorbent absorption heavy metal
Property coconut husk charcoal, which is placed in the mixture containing heavy metal, to be adsorbed.
Adsorbent CSBC-ICl, CSBC and adsorbent aluminium oxide that the present embodiment prepares 1 method of embodiment, graphene,
Silica gel does absorption comparative test.Weigh respectively above-mentioned adsorbent 20mg different adsorbents be added to it is molten containing 10mL mercury ion
In the centrifuge tube of liquid, after vibrating 10min, supernatant is detected, calculates removal rate.
It can be seen that modified coconut husk charcoal CSBC-ICl is best to the removal effect of mercury ion in Fig. 9, active carbon AC
Take second place, but removal rate is about only 35% or so.In addition the removal effect of several adsorbents is undesirable is no more than 25%.Thus
It can be seen that good relative to other adsorbents using the adsorption effect that ICl is modified coconut husk charcoal.
A kind of modified coconut husk charcoal of embodiment 11, is the coconut husk charcoal for including halogen group and amino；It is described
Micropore is distributed in coconut husk biology carbon surface, and the micro-pore diameter size is 2~3nm；The specific surface area of coconut husk charcoal is 1000
~1300m2/g.Wherein, micropore size 2nm, 2.5nm or 3nm, the specific surface area of coconut husk charcoal are 1038m2/g、
1224m2/ g or 1185m2/g；The Kong Rongwei 0.532cm of coconut husk biology carbon surface3/g、0.647cm3/ g or 0.689cm3/g.Its
In, halogen group includes chloro-Cl and iodo-I, and the amino is-NH2。
Adsorptivity test:
Chloro-Cl, iodo-I and amino-NH are modified into the present embodiment coconut husk charcoal upper surface2, preparation method is will
The first coconut husk charcoal nitration being prepared by the method for embodiment 1.2: being 18mol/L by 50mL concentration in 0 DEG C of ice bath
Sulfuric acid be added slowly to 50mL concentration be 15.7mol/L nitric acid solution in obtain mixed acid solution.By coconut husk at the beginning of 10g
Charcoal is slowly added into mixed acid solution, stirs 50min under conditions of 0 DEG C, filtrate is obtained by filtration；Use deionized water
Washing repeatedly until filtrate is neutral, in 90 DEG C of dryings in vacuum oven, obtains modified coconut husk charcoal.
Modification coconut husk charcoal prepared by the modification coconut husk charcoal and embodiment 1.2 that the present embodiment is prepared,
The Congo red CR and Crystal Violet CV of dyestuff is adsorbed respectively, for the modification coconut husk charcoal of embodiment 1.2, to dye
Have in terms of the removal effect for expecting crystal violet CV and greatly improves.The modified coconut husk charcoal of the present embodiment is to Congo red and crystallization
Purple maximum adsorption capacity is up to 228.1mg/g and 215.8mg/g, and the maximum of the modification coconut husk charcoal of embodiment 1.2 is inhaled
Attached capacity is 136.3mg/g and 234.2mg/g.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (10)
1. a kind of modified coconut husk charcoal, which is characterized in that it is the coconut husk charcoal for including halogen group；The coconut husk is raw
Micropore is distributed in object carbon surface, and the micro-pore diameter size is 2~3nm；The specific surface area of coconut husk charcoal be 1000~
1300m2/g。
2. the preparation method of modification coconut husk charcoal as described in claim 1, which is characterized in that it includes the following steps, incites somebody to action
Coconut husk charcoal is formed through halide dipping modification.
3. the preparation method of modified coconut husk charcoal as described in claim 1, which is characterized in that it will be the following steps are included: will
Coconut husk charcoal is placed in the halide solution that mass concentration is 3~7%, is impregnated and is washed after stirring 1~5 hour, after dry
Obtain modified coconut husk charcoal.
4. the preparation method of modified coconut husk charcoal as described in claim 1, it is characterised in that: the halide is chlorination
One of iodine, potassium iodide or potassium chloride or two or more combinations.
5. the preparation method of modified coconut husk charcoal as described in claim 1, it is characterised in that: the coconut husk charcoal is main
It is made of coconut husk through chemical activation.
6. the preparation method of modified coconut husk charcoal as described in claim 1, which is characterized in that the system of the coconut husk charcoal
Preparation Method are as follows: coconut husk is placed under 250~310 DEG C of environment and is kept for 3~7 hours, and is soaked in CaCl218~20 is small in solution
When, activator is added, after being stirred 1~3 hour at 30~70 DEG C, N2Lower sealing is kept for 1~3 hour at 40~80 DEG C, and acid
Property solution clean to neutrality after filter, it is dry at 100~120 DEG C.
7. a kind of method of modified coconut husk charcoal as adsorbent absorption heavy metal, which is characterized in that include the following steps, it will
Granular size is that modification coconut husk charcoal described in the claim 1-7 any one of 120~200 mesh is placed in containing heavy metal
With absorption in mixture, keeping temperature is 30~100 DEG C.
8. method of the modified coconut husk charcoal as adsorbent absorption heavy metal as claimed in claim 7, is characterized in that: described
Modified coconut husk charcoal and heavy metal are greater than 20:3 by weight.
9. a kind of modified coconut husk charcoal, which is characterized in that it is the coconut husk charcoal for including halogen group and amino；It is described
Micropore is distributed in coconut husk biology carbon surface, and the micro-pore diameter size is 2~3nm；The specific surface area of coconut husk charcoal is 1000
~1300m2/g。
10. the preparation method of modified coconut husk charcoal as claimed in claim 9, which is characterized in that itself the following steps are included:
S1: the nitration of coconut husk charcoal:
(1) coconut husk charcoal is placed in the halide solution that mass concentration is 3~7%, impregnates and is washed after stirring 1~5 hour
It washs, just coconut husk charcoal is obtained after dry；
(2) preparation of mixed acid solution: being 1 by the sulfuric acid that concentration is 17~18mol/L in 0 DEG C of ice bath by volume:
0.5~2 is added in the nitric acid solution that concentration is 15~16mol/L, is uniformly mixed；
S2: first coconut husk charcoal is slowly added into mixed acid solution, and 40~60min, filtering are stirred under conditions of 0 DEG C
Obtain filtrate；It is washed with water repeatedly until until filtrate is neutral, is placed at 80~95 DEG C dry, it is biological to obtain modified coconut husk
Charcoal.
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| CN110433768A (en) * | 2019-04-26 | 2019-11-12 | 福建工程学院 | A kind of preparation method of high-specific surface area cocoanut active charcoal |
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| CN113086981A (en) * | 2021-04-29 | 2021-07-09 | 石嘴山市鹏盛化工有限公司 | Modified coconut shell activated carbon and application thereof in preparation of pharmaceutical-grade guanidine hydrochloride |
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