CN104788862B - A kind of preparation method of hydrophilic porous pressed active carbon - Google Patents
A kind of preparation method of hydrophilic porous pressed active carbon Download PDFInfo
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Abstract
The present invention relates to field of functional materials, more particularly to a kind of preparation method of hydrophilic porous pressed active carbon.The present invention provides a kind of preparation method of hydrophilic porous pressed active carbon, comprises the following steps：Prepare the aqueous solution of debita spissitudo water soluble hydroxy polymer：Weigh a certain amount of water-soluble hydroxyl polymer-containing to be dissolved in appropriate distilled water, make swelling dissolving, it is standby after cooling；Add 2wt%NaOH water-soluble basified, appropriate activated carbon is added in glue system；Add the mass ratio of appropriate crosslinking agent epoxychloropropane, control water soluble hydroxy polymer and epoxychloropropane；Foaming agent ammonium hydrogen carbonate is added, is stirred；The stirring reaction under tepidarium, neutralizes pH to neutrality after completion of the reaction；Activated carbon mixed liquor pours into mould, is placed on drying in 110 DEG C of baking oven.Present invention process is simple, easy to operate, can obtain the pressed active carbon binding agent with water-fast, acid-fast alkali-proof, superiority of effectiveness.
Description
Technical field
The present invention relates to field of functional materials, more particularly to a kind of preparation method of hydrophilic porous pressed active carbon.
Background technology
Activated carbon is, with raw materials such as coal, timber and shells, to be obtained through charing, activation and post processing, can be divided by face shaping
It is powdered activated carbon, granular activated carbon, fibre active carbon and spherical activated charcoal etc..It is living as a kind of important functional material
Property charcoal not only there is unique pore structure, it is often more important that various active functional group is contained on its surface, is generally divided into oxygen-containing official
Can group and nitrogen-containing functional group.The chemical property of activated carbon is sufficiently stable, and water insoluble and organic solvent, using may be used also after failure
To regenerate, recycling, therefore, activated carbon can be widely used in treatment waste water, purification gas, and food processing, change
The aspects such as work, military chemistry protection have great meaning.
Pressed active carbon has larger size and definite shape, there is heap density and intensity higher, and no dust pollution.
Prepare shaping active carbon method and be divided into 3 classes：1. will directly there is the natural plant carbonated activation such as the timber of setting shape and size.
2. then carbonaceous precursor material molding bonded is carbonized with binding agent, optionally can further be activated.3. using bonding
Then agent processes bonding agent powder active carbon or activated carbon fiber molding bonded, it is ensured that the overall performance of type charcoal is steady
It is fixed.
, with activated carbon product as raw material, after addition binding agent is allowed to bonding forming, it is appropriate to be subject to for activated carbon molding bonded method
Treatment.The binding agent of pressed active carbon has phenolic resin, starch, polyvinyl alcohol, methylcellulose and its derivative etc. organic viscous
The inorganic binder such as knot agent and ceramics, bentonite, waterglass, wax.Zhang Xianglan etc. is prepared into type activity with polyvinyl alcohol glue aqueous systems
Charcoal, with Powdered Activated Carbon as raw material, with polyvinyl alcohol as binding agent, is added with 10%, 15%, 20% amount respectively, and stirring is equal
It is molded at various pressures after even, prepares pressed active carbon, and carry out the test of properties, it was therefore concluded that：Binding agent ratio
It is 15%, briquetting pressure is 80MPa, post-processing temperature is 200 DEG C, process time is that 30min is optimum preparating condition.（Zhang Xiang
Orchid, Wang Xianglong, Li Ke appoint Red Star, Li Yuan to prepare the research of pressed active carbon as binding agent with polyvinyl alcohol, clean coal technology,
2008,14（3）：23-25.）
When pressed active carbon is often prepared with organic binder bond, due to containing in polyvinyl alcohol, carboxymethylcellulose calcium molecule
Substantial amounts of hydroxyl, therefore hydrophily relatively strong, water resistance and less stable, thus limit its performance and apply model
Enclose.Crosslinking agent is often used using polymer such as epoxychloropropane, crosslinking organic binder bond is prepared, adds ammonium hydrogen carbonate foaming agent to use
Prepared in hydrophilic porous pressed active carbon.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of hydrophilic porous Constitutive active
The preparation method of charcoal, for solving the problems of the prior art.
The present invention is explored with water-soluble hydroxyl polymer-containing and crosslinking agent synthetic binder, and shaping is mixed with activated carbon
Activated carbon, adds foaming agent ammonium hydrogen carbonate to improve perforate effect.Cost of material etc. and reaction complexity are considered, from water solubility
Hydroxy polymer-epoxychloropropane binder system.
In order to achieve the above objects and other related objects, the present invention provides a kind of preparation of hydrophilic porous pressed active carbon
Method, comprises the following steps：
Step 1）Prepare the aqueous solution of debita spissitudo water soluble hydroxy polymer：Weigh a certain amount of water-soluble hydroxyl polymerization
Thing, is dissolved in appropriate distilled water, makes swelling dissolving, standby after cooling；
Step 2）2wt%NaOH water-soluble basified half an hour is added, appropriate activated carbon is added in glue system；
Step 3）Add the quality of appropriate crosslinking agent epoxychloropropane, control water soluble hydroxy polymer and epoxychloropropane
Than；
Step 4）Addition accounts for the foaming agent ammonium hydrogen carbonate of system gross weight 0.1%-0.3%, stirs；
Step 5）Under 65 DEG C of water bath with thermostatic control, stirring reaction 1-2 hours；After completion of the reaction with acetic acid and pH is into
Property；
Step 6）Activated carbon mixed liquor pours into mould, is placed on drying in 110 DEG C of baking oven.
Preferably, the water-soluble hydroxyl polymer-containing is mainly polyvinyl alcohol（1788）, carboxymethylcellulose calcium（Molecular weight
It is 5400-7400）, water soluble starch（Molecular weight is 342.3）.
It is furthermore preferred that the concentration of the aqueous solution of the water-soluble hydroxyl polymer-containing is 8wt%.
Those skilled in the art can empirically determined appropriate swelling solution temperature.
Preferably, the step 2）In, the ratio between addition of carboxymethylcellulose calcium and the 2wt%NaOH aqueous solution is g：ml=2：
5。
Preferably, the step 2）In, the mass ratio of glue system and activated carbon（Glue/charcoal ratio）It is 1-2：1.
Preferably, the step 3）In, the mass ratio of water soluble hydroxy polymer and epoxychloropropane is 3-5：1.
The beneficial effects of the invention are as follows：Present invention process is simple, easy to operate, can obtain with water-fast, acid-fast alkali-proof,
The pressed active carbon binding agent of superiority of effectiveness.The binding agent for using is can not in hydrophilic polymer, and manufacturing process
Later stage high temperature carbonization is carried out, obtained porous activated carbon is remained the hydrophilicity of binding agent to a certain extent.The present invention
Economic worth is higher, efficient, the cheap pressed active carbon of exploitation, can be used for the place of sewage disposal particularly heavy metal wastewater thereby
Reason.
Specific embodiment
Embodiments of the present invention are illustrated below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages of the invention and effect easily.The present invention can also be by specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
It should be clear that process equipment not specific dated in the following example or device using conventional equipment in the art or
Device；All pressure values and scope are all referring to absolute pressure.
In addition, it is to be understood that one or more method and steps mentioned in the present invention do not repel before and after the combination step
Can also there is other method step or other method step can also be inserted between the step of these are specifically mentioned, unless separately
It is described；It should also be understood that the combination annexation between one or more the equipment/devices mentioned in the present invention is not repelled
Can also exist before and after the unit equipment/device other equipment/device or two equipment/devices specifically mentioning at these it
Between can also insert other equipment/device, unless otherwise indicated.And, unless otherwise indicated, the numbering of various method steps is only
Differentiate the convenient tool of various method steps, rather than to limit the ordering of various method steps or limiting enforceable model of the invention
Enclose, being altered or modified for its relativeness is of the invention enforceable when being also considered as in the case of without essence change technology contents
Category.
A kind of preparation method of hydrophilic porous pressed active carbon, comprises the following steps：
Step 1）According to the difference of water soluble hydroxy polymer, the aqueous solution of debita spissitudo is prepared：Weigh a certain amount of water-soluble
Property hydroxyl polymer-containing, is dissolved in appropriate distilled water, makes swelling dissolving, standby after cooling.
Step 2）2wt%NaOH water-soluble basified half an hour is added, appropriate activated carbon is added in glue system, controlled
Glue/charcoal ratio.
Step 3）Add the mass ratio of appropriate crosslinking agent epoxychloropropane, control polymer and epoxychloropropane.
Step 4）Addition accounts for the foaming agent ammonium hydrogen carbonate of system gross weight 0.1%-0.3%, stirs.
Step 5）Under 65 DEG C of water bath with thermostatic control, stirring reaction 1-2 hours.After completion of the reaction with acetic acid and pH is into
Property.
Step 6）Activated carbon mixed liquor pours into mould, is placed on drying in 110 DEG C of baking oven.
Further, the water-soluble hydroxyl polymer-containing is mainly polyvinyl alcohol, carboxymethylcellulose calcium, water-soluble shallow lake
Powder.
Embodiment 1：
Polyvinyl alcohol-epoxychloropropane bonds the implementation of activated carbon
The accurate polyvinyl alcohol for weighing 2g, is dissolved in the distilled water of 23g, the swelling dissolving in 93 DEG C of baking oven.Add 5ml
2wt%NaOH water-soluble basified half an hour.Appropriate Powdered Activated Carbon is added in glue system, makes glue/charcoal ratio be 1:1.Point
0.133g, 0.2g, 0.25g, 0.4g, 0.67g epoxychloropropane are not added, make the mass ratio of polyvinyl alcohol and epoxychloropropane
It is 15:1、10:1、8:1、5:1、3:1, numbering is respectively I -1, I -2, I -3, I -4, I -5.It is put into 65 DEG C of water bath with thermostatic control and stirs
After mixing heating 1 hour, stop stirring, under the water bath with thermostatic control of this temperature, place 45 minutes.It is neutralized to acetic acid after completion of the reaction
It is neutral.Mixed liquor is poured into mould, drying in 110 DEG C of baking oven is placed on.After it is completely dried solidification, with water, 3wt%
HCl, 10wt%NaOH soak, and carry out water-fast, acidproof, alkaline resistance properties test.
The water-acid resistance test result of 1 polyvinyl alcohol of table-epoxychloropropane adhesive composite activated carbon system
Polyethylene glycol binding agent is water-fast, acid-fast alkali-proof experimental result is as shown in table 1.As it can be seen from table 1 polyethylene glycol
Different with epoxychloropropane mass ratio, the water-fast, acidproof of sample, alkali resistance are presented difference, and water-fast, resistance to acids and bases is with poly- second two
The reduction of alcohol and epoxychloropropane mass ratio, i.e. dosage of crosslinking agent increase and improve.When polyvinyl alcohol and the matter of epoxychloropropane
Amount proportioning is 5：1、3:When 1, the composite activated carbon system being made is matched with this has optimal water-fast, acid-fast alkali-proof.
The etherification modified principle of polyvinyl alcohol is, using the chemical activity of polyvinyl alcohol hydroxyl, to introduce corresponding monomer pair
Hydroxyl is etherified, so as to obtain etherification modified polyvinyl alcohol.It is real using the 2wt%NaOH aqueous solution as catalyst in experiment
The etherification reaction of the hydroxyl on existing epoxychloropropane and polyvinyl alcohol, and then realize crosslinking.
It is 1 with the quality proportioning of activated carbon to control polyvinyl alcohol glue aqueous systems：1, the pressed active carbon being made has preferable
Water wettability.The methylene blue adsorption value and raw material activated carbon of each group pressed active carbon sample than have it is different degrees of under
Drop.Analyze its reason, it may be possible to because have a certain amount of Binder Composition in the grain active carbon for preparing, and not by charcoal
Change.In the sample of one side phase homogenous quantities, the amount of activated carbon has declined；Another aspect binding agent has to the pore structure of activated carbon
Certain inhibition.
Embodiment 2：
Carboxymethylcellulose calcium-epoxychloropropane bonds the implementation of activated carbon
The accurate carboxymethylcellulose calcium for weighing 2g, is dissolved in the distilled water of 23g, swelling dissolving under stirring.Add 5ml's
2wt%NaOH basified half an hour.Appropriate Powdered Activated Carbon is added in glue system, makes glue/charcoal ratio be 2:1、1:1, compile
Number represent II -1, II -2.0.4g, 0.67g epoxychloropropane are separately added into, have made the matter of carboxymethylcellulose calcium and epoxychloropropane
Amount is than being 5:1、3:1, numbering is respectively II -1-1, II -1-2, II -2-1, II -2-2.It is put into stirring in 65 DEG C of water bath with thermostatic control
After heating 1 hour, stop stirring, under the water bath with thermostatic control of this temperature, place 45 minutes.After completion of the reaction with acetic acid and pH extremely
It is neutral.Mixed liquor is poured into mould, drying in 110 DEG C of baking oven is placed on.After it is completely dried solidification, with water, 3wt%
HCl, 10wt%NaOH soak, and carry out water-fast, acidproof, alkaline resistance properties test.
The water-acid resistance test result of 2 carboxymethylcellulose calciums of table-epoxychloropropane adhesive composite activated carbon system
It is 2 with the quality proportioning of activated carbon when carboxymethylcellulose calcium-epoxychloropropane is controlled：1、1：1, matched with this and be made
Pressed active carbon be respectively provided with preferable water wettability.On the whole, glue/charcoal ratio is 2：1、1：When 1, both glue charcoals can be preferably
Wetting, glue consumption should not be excessive.From table 2 it can be seen that prepare carboxymethyl cellulose gum-charcoal series of samples it is water-fast, acidproof,
The better performances of alkali resistance.
Carboxymethylcellulose calcium is a kind of water white transparency, nontoxic odorless organic adhesion agent, is widely used in food processing
And field of medicaments, it is well suited for the bonding of pressed active carbon in field of Environment Protection application.In experiment, using carboxymethylcellulose calcium-ring
It is fine that oxygen chloropropane binding agent is obtained the water-fast of activated carbon sample, acid-fast alkali-proof.
Due to the addition of binding agent, and binding agent is compared with hole for activated carbon and undeveloped, necessarily to Unit Weight particle
The specific surface area of activated carbon produces larger negative effect, while the binding agent without charing is also possible to block a part of activated carbon
Hole.Therefore, the specific surface area of grain active carbon obtained in this experiment is smaller compared with material powder activated carbon, absorption property is more former
Material activated carbon has declined.If further to improve sample specific surface area, can be by active carbon powder and carboxymethylcellulose calcium-ring
The mixing of oxygen chloropropane binding agent, compound stalk forming, follow-up 200 DEG C of solidifications heat treatment.
Embodiment 3：
The implementation of polyvinyl alcohol-epoxychloropropane-ammonium hydrogen carbonate binding agent
5 parts of polyvinyl alcohol of 2g accurately are weighed, the distilled water of 23g is dissolved in respectively, be placed in conical flask, in 93 DEG C of baking oven
In swelling dissolving, it is standby after cooling.It is separately added into the 2wt%NaOH water-soluble basified half an hour of 5ml.Add 0.4g epoxy chlorine
Propane, the mass ratio for making polyvinyl alcohol and epoxychloropropane is 5:1.It is 1 by glue/charcoal ratio:1 adds activated carbon.Then, add respectively
Enter the 0.1% of system gross weight, 0.15%, 0.2%, 0.25%, 0.3% ammonium hydrogen carbonate stirs, numbering respectively III -1,
Ⅲ-2、Ⅲ-3、Ⅲ-4、Ⅲ-5.Agitating heating stops stirring, in the perseverance of this temperature after 1 hour in being put into 65 DEG C of water bath with thermostatic control
Under tepidarium, place 45 minutes.After completion of the reaction with acetic acid and pH is to neutrality.Mixed liquor is poured into mould, 110 DEG C are placed on
Baking oven in dry, solidification.After it is completely dried solidification, soaked with water, 3wt%HCl, 10wt%NaOH, carried out water-fast, resistance to
Acid, alkaline resistance properties test.Though can be seen that sample by the result of table 3 adds a small amount of ammonium hydrogen carbonate, gas is produced, forms stomata,
But water-acid resistance is consistent with the effect for being not added with ammonium hydrogen carbonate.
The water-acid resistance test result of the type charcoal of the different ammonium bicarbonate contents of table 3
Foaming agent ammonium hydrogen carbonate is added during pressed active carbon is prepared, the amount containing ammonium hydrogen carbonate is 0.15% sample
Specific surface area than content 0.1%, 0.2%, 0.3% sample will be big.In experiment, glue body is made up containing 0.15% ammonium hydrogen carbonate
It is the best results to the blocking of pressed active carbon hole, its specific surface area is maximum, preliminary survey result is 414.2m2/g.Add hair
Infusion ammonium hydrogen carbonate has considerable influence to activated carbon structure, can produce more bigger holes.In experiment, the Constitutive active of preparation
If charcoal is thicker, in preparation process, Powdered Activated Carbon because Action of Gravity Field can sink under, and binding agent can be in activated carbon
Above.The pressed active carbon thinner thickness for preparing is controlled, effect is more preferable.
Application Example：
Polyvinyl alcohol-epoxychloropropane-ammonium hydrogen carbonate binding agent composite activated carbon implementation of the treatment containing cadmium simulated wastewater
In the volumetric flask of 1L, CdCl is used2Cd of the configuration containing 50mg2+Solution.Tested not using Atomic Absorption Spectrometer
Contain Cd with concentration2+The atom absorbance of solution.Standard curve is drawn according to experimental data.Composite activated carbon sample is：With quality
The polyvinyl alcohol water solution of percentage 8%, with epoxychloropropane with 5：1 quality proportioning is prepared into binding agent, and glue/charcoal ratio is 1:1,
0.1%, 0.15%, 0.2%, 0.3% ammonium hydrogen carbonate for being separately added into system gross weight is obtained type charcoal, carries out Cd2+Adsorption effect is tested.
Weigh 1g series composite activated carbon samples and be placed in the 50mg/L of 100ml containing Cd2+In solution, standing adsorption, different time sections take
Clear liquid is determined on Atomic Absorption Spectrometer, obtains average value.The Cd of different adsorption times is obtained by standard curve2+Concentration, then
Obtain the absorptivity of final each activated carbon sample.
Quickly, after absorption 1h, the speed of type charcoal Adsorption of Cadmium slows down the speed of type charcoal sample adsorption cadmium ion, becomes
Steadily, by the absorption of 12 hours, the concentration of cadmium ion is basicly stable in solution, is finally reached adsorption saturation.Compare and obtain, with
The polyvinyl alcohol water solution of mass percent 8% is with epoxychloropropane with 5：Binding agent prepared by 1 quality proportioning, adds 0.1% carbon
Pressed active carbon prepared by sour hydrogen ammonium is 78.8% to the adsorption rate of cadmium ion；Type charcoal prepared by 0.15% ammonium hydrogen carbonate is added to cadmium
The adsorption rate of ion is 89.5%；It is 93.4% to the adsorption rate of cadmium ion to add type charcoal prepared by 0.2% ammonium hydrogen carbonate；Add
The type charcoal of 0.3% ammonium hydrogen carbonate is 98.9% to the adsorption rate of cadmium ion.Polyvinyl alcohol-epoxychloropropane-ammonium hydrogen carbonate binding agent
In the application that 50mg/L cadmium ions are processed, the treatment effect of the pressed active carbon containing 0.3% ammonium hydrogen carbonate is most for composite activated carbon
It is good.
In sum, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
The personage for knowing this technology all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should be covered by claim of the invention.
Claims (3)
1. a kind of preparation method of hydrophilic porous pressed active carbon, comprises the following steps：
Step 1) prepare debita spissitudo water soluble hydroxy polymer the aqueous solution：A certain amount of water-soluble hydroxyl polymer-containing is weighed,
It is dissolved in appropriate distilled water, makes swelling dissolving, it is standby after cooling；
Step 2) 2wt%NaOH water-soluble basified half an hour is added, appropriate activated carbon is added in glue system；
Step 3) appropriate crosslinking agent epoxychloropropane is added, control the mass ratio of water soluble hydroxy polymer and epoxychloropropane；
Step 4) the foaming agent ammonium hydrogen carbonate for accounting for system gross weight 0.1%-0.3% is added, stir；
Step 5) under 65 DEG C of water bath with thermostatic control, stirring reaction 1-2 hours, after completion of the reaction with acetic acid and pH is to neutrality；
Step 6) activated carbon mixed liquor pours into mould, and it is placed in 110 DEG C of baking oven and dries；
The water-soluble hydroxyl polymer-containing is selected from the one kind in polyvinyl alcohol, carboxymethylcellulose calcium；
The step 2) in, the ratio between addition of water-soluble hydroxyl polymer-containing and the 2wt%NaOH aqueous solution is g：Ml=2：5；
The step 3) in, the mass ratio of water soluble hydroxy polymer and epoxychloropropane is 3-5：1.
2. a kind of preparation method of hydrophilic porous pressed active carbon as claimed in claim 1, it is characterised in that described water-soluble
Property hydroxyl polymer-containing the aqueous solution concentration be 8wt%.
3. a kind of preparation method of hydrophilic porous pressed active carbon as claimed in claim 1, it is characterised in that the step
2) in, glue system is 1-2 with the mass ratio of activated carbon：1.
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| CN111849100A (en) * | 2020-05-14 | 2020-10-30 | 内蒙古浦瑞芬环保科技有限公司 | Activated carbon binder and preparation method thereof |
| CN114381028B (en) * | 2020-10-16 | 2024-04-12 | 自然资源部天津海水淡化与综合利用研究所 | Photo-thermal conversion material, preparation method and application thereof, and method for sea water desalination, sewage treatment, water purification or solution purification |
| CN114314582B (en) * | 2022-01-03 | 2023-07-25 | 安徽大学 | Preparation method of PVA gel-based crosslinked porous activated carbon |
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