CN104788862A - Preparation method of hydrophilic porous formed activated carbon - Google Patents
Preparation method of hydrophilic porous formed activated carbon Download PDFInfo
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- CN104788862A CN104788862A CN201410023750.0A CN201410023750A CN104788862A CN 104788862 A CN104788862 A CN 104788862A CN 201410023750 A CN201410023750 A CN 201410023750A CN 104788862 A CN104788862 A CN 104788862A
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Abstract
The invention relates to the field of functional materials, and especially relates to a preparation method of hydrophilic porous formed activated carbon. The preparation method of the hydrophilic porous formed activated carbon comprises the following steps: preparing a proper concentration of an aqueous solution of a water-soluble hydroxy polymer; weighing a certain amount of the water-soluble hydroxy polymer, dissolving the certain amount of the water-soluble hydroxy polymer in distilled water, swelling and dissolving, and cooling; adding 2wt% of an aqueous solution of NaOH to alkalize, and adding a proper amount of activated carbon into the above obtained glue system; adding a proper amount of a cross-linking agent chloropropylene oxide, and controlling a mass ratio of the water-soluble hydroxy polymer to chloropropylene oxide; adding a foaming agent ammonium bicarbonate, and uniformly stirring; reacting under stirring in a warm water bath, and neutralizing after the reaction to make the pH be 7; and pouring the above obtained activated carbon mixed solution into a die, and drying in a 110DEG C oven. The preparation method has the advantages of simple process and convenient operation, and the formed activated carbon obtained in the invention has the advantages of water resistance, acid and alkali resistance, and high cost performance.
Description
Technical field
The present invention relates to field of functional materials, particularly relate to a kind of preparation method of hydrophilic porous pressed active carbon.
Background technology
Gac is with raw materials such as coal, timber and shells, obtains, can be divided into powdered carbon, granulated active carbon, fibre active carbon and ball shape active carbon etc. by face shaping through charing, activation and aftertreatment.As a kind of important functional materials, gac not only has unique pore texture, the more important thing is that its surface is containing various active functional group, is generally divided into oxygen-containing functional group and nitrogen-containing functional group.The chemical property of gac is very stable, and water insoluble and organic solvent, used after losing efficacy and can also regenerate, recycling, therefore, gac can be widely used in process waste water, Purge gas, and there is great meaning the aspect such as food-processing, chemical industry, military chemistry protection.
Pressed active carbon has larger size and definite shape, has higher bulk density and intensity, and no dust pollution.Prepare shaping active carbon method and be divided into 3 classes: 1. directly will there is the natural plant carbonated activation such as the timber of setting shape and size.2. with binding agent by carbonaceous precursor material molding bonded, then carbonize, optionally can activate further.3. adopt binding agent by powder active carbon or activated carbon fiber molding bonded, then process caking agent, the overall performance of guarantee type charcoal is stablized.
Gac molding bonded method take activated carbon product as raw material, after interpolation binding agent makes it bonding forming, is suitably processed.The binding agent of pressed active carbon has the mineral binder bond such as the organic binder bonds such as resol, starch, polyvinyl alcohol, methylcellulose gum and derivative thereof and pottery, bentonite, water glass, wax.Zhang Xianglan etc. are prepared into type gac with polyvinyl alcohol glue aqueous systems, take Powdered Activated Carbon as raw material, take polyvinyl alcohol as binding agent, add with the amount of 10%, 15%, 20% respectively, shaping at various pressures after stirring, prepare pressed active carbon, and carry out the test of properties, reach a conclusion: binding agent ratio is 15%, forming pressure is 80MPa, post-processing temperature is 200 DEG C, and the treatment time is 30min is optimum preparating condition.(Zhang Xianglan, Wang Xianglong, Li Ke, appoint Red Star, Li Yuan take polyvinyl alcohol as the research that pressed active carbon prepared by binding agent, clean coal technology, 2008,14(3): 23-25.）
When pressed active carbon commonly uses organic binder bond preparation, due in polyvinyl alcohol, carboxymethyl cellulose molecule containing a large amount of hydroxyl, therefore wetting ability is comparatively strong, water resistance and less stable, thus limits its use properties and range of application.The polymkeric substance such as epoxy chloropropane can be utilized to commonly use linking agent, and the crosslinked organic binder bond of preparation, adds bicarbonate of ammonia whipping agent and prepares for hydrophilic porous pressed active carbon.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide a kind of preparation method of hydrophilic porous pressed active carbon, for solving the problems of the prior art.
The present invention explores with water-soluble hydroxyl polymer-containing and linking agent synthetic adhesive, is mixed with pressed active carbon, adds whipping agent bicarbonate of ammonia and improve perforate effect with gac.Consideration raw materials cost etc. and reaction complexity, select water soluble hydroxy polymkeric substance-epoxy chloropropane binder system.
For achieving the above object and other relevant objects, the invention provides a kind of preparation method of hydrophilic porous pressed active carbon, comprise the steps:
The aqueous solution of step 1) preparation proper concn water soluble hydroxy polymkeric substance: take a certain amount of water-soluble hydroxyl polymer-containing, be dissolved in appropriate distilled water, make swelling dissolving, for subsequent use after cooling;
Step 2) add the 2wt%NaOH aqueous solution alkalization half an hour, in glue system, add appropriate gac;
Step 3) adds appropriate linking agent epoxy chloropropane, controls the mass ratio of water soluble hydroxy polymkeric substance and epoxy chloropropane;
Step 4) adds the whipping agent bicarbonate of ammonia accounting for system gross weight 0.1%-0.3%, stirs;
Step 5) under the water bath with thermostatic control of 65 DEG C, stirring reaction 1-2 hour; Use in acetic acid after completion of the reaction and pH extremely neutrality;
Mould poured into by step 6) gac mixed solution, is placed in the baking oven of 110 DEG C and dries.
Preferably, described water-soluble hydroxyl polymer-containing is mainly polyvinyl alcohol (1788), carboxymethyl cellulose (molecular weight is 5400-7400), water soluble starch (molecular weight is 342.3).
Preferred, the concentration of the aqueous solution of described water-soluble hydroxyl polymer-containing is 8wt%.
Those skilled in the art rule of thumb can determine suitable swelling solvent temperature.
Preferably, described step 2) in, carboxymethyl cellulose is g:ml=2:5 with the ratio of the add-on of the 2wt%NaOH aqueous solution.
Preferably, described step 2) in, the mass ratio (glue/charcoal ratio) of glue system and gac is 1-2:1.
Preferably, in described step 3), the mass ratio of water soluble hydroxy polymkeric substance and epoxy chloropropane is 3-5:1.
The invention has the beneficial effects as follows: present invention process is simple, easy to operate, can obtain and have water-fast, acid-fast alkali-proof, superiority of effectiveness pressed active carbon binding agent.The binding agent adopted is hydrophilic polymer, and can not carry out later stage high temperature carbonization in making processes, makes the porous activated carbon obtained remain the hydrophilicity of binding agent to a certain extent.Economic worth of the present invention is higher, efficient, the cheap pressed active carbon of exploitation, can be used for the process of sewage disposal particularly heavy metal wastewater thereby.
Embodiment
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Notice, in the following example, the concrete processing unit that indicates or device all adopt conventional equipment in this area or device; All force value and scope all refer to absolute pressure.
In addition should be understood that the one or more method stepss mentioned in the present invention do not repel and can also to there is additive method step or can also insert additive method step before and after described combination step between these steps clearly mentioned, except as otherwise noted; Will also be understood that, the relation that is connected between the one or more equipment/devices mentioned in the present invention is not repelled and can also to be there are other equipment/devices or can also insert other equipment/devices before and after described clustered aggregates/device between these two equipment/devices clearly mentioned, except as otherwise noted.And, except as otherwise noted, the numbering of various method steps is only the convenient tool differentiating various method steps, but not be ordering or the enforceable scope of restriction the present invention of restriction various method steps, the change of its relativeness or adjustment, when changing technology contents without essence, when being also considered as the enforceable category of the present invention.
A preparation method for hydrophilic porous pressed active carbon, comprises the following steps:
Step 1), according to the difference of water soluble hydroxy polymkeric substance, prepares the aqueous solution of proper concn: take a certain amount of water-soluble hydroxyl polymer-containing, be dissolved in appropriate distilled water, make swelling dissolving, for subsequent use after cooling.
Step 2) add the 2wt%NaOH aqueous solution alkalization half an hour, in glue system, add appropriate gac, control glue/charcoal ratio.
Step 3) adds appropriate linking agent epoxy chloropropane, controls the mass ratio of polymkeric substance and epoxy chloropropane.
Step 4) adds the whipping agent bicarbonate of ammonia accounting for system gross weight 0.1%-0.3%, stirs.
Step 5) under the water bath with thermostatic control of 65 DEG C, stirring reaction 1-2 hour.Use in acetic acid after completion of the reaction and pH extremely neutrality.
Mould poured into by step 6) gac mixed solution, is placed in the baking oven of 110 DEG C and dries.
Further, described water-soluble hydroxyl polymer-containing is mainly polyvinyl alcohol, carboxymethyl cellulose, water soluble starch.
Embodiment 1:
The enforcement of polyvinyl alcohol-epoxy chloropropane bonding gac
Accurately take the polyvinyl alcohol of 2g, be dissolved in the distilled water of 23g, swelling dissolving in the baking oven of 93 DEG C.Add the 2wt%NaOH aqueous solution alkalization half an hour of 5ml.In glue system, adding appropriate Powdered Activated Carbon, making glue/charcoal than being 1:1.Add 0.133g, 0.2g, 0.25g, 0.4g, 0.67g epoxy chloropropane respectively, make the mass ratio of polyvinyl alcohol and epoxy chloropropane be 15:1,10:1,8:1,5:1,3:1, numbering is respectively I-1, I-2, I-3, I-4, I-5.Put into the water bath with thermostatic control stirring heating of 65 DEG C after 1 hour, stop stirring, under the water bath with thermostatic control of this temperature, place 45 minutes.Neutrality is neutralized to after completion of the reaction with acetic acid.Mixed solution is poured in mould, be placed in the baking oven of 110 DEG C and dry.After the solidification of its complete drying, soak with water, 3wt%HCl, 10wt%NaOH, carry out water-fast, acidproof, alkaline resistance properties test.
The water-acid resistance test result of table 1 polyvinyl alcohol-epoxy chloropropane sizing agent composite activated carbon system
Polyoxyethylene glycol binding agent is water-fast, acid-fast alkali-proof experimental result is as shown in table 1.As can be seen from Table 1, polyoxyethylene glycol is different with epoxy chloropropane mass ratio, and water-fast, acidproof, the alkali resistance of sample present difference, and water-fast, resistance to acids and bases is along with the reduction of polyoxyethylene glycol and epoxy chloropropane mass ratio, and namely dosage of crosslinking agent increases and improves.When the quality proportioning of polyvinyl alcohol and epoxy chloropropane is 5:1,3:1, the composite activated carbon system made with this proportioning has best water-fast, acid-fast alkali-proof.
The etherification modified principle of polyvinyl alcohol is the chemical activity utilizing polyvinyl alcohol hydroxyl, introduces corresponding monomer and carries out etherificate to hydroxyl, thus obtain etherification modified polyvinyl alcohol.In experiment, using the 2wt%NaOH aqueous solution as catalyzer, realize the etherification reaction of the hydroxyl on epoxy chloropropane and polyvinyl alcohol, and then realize crosslinked.
The quality proportioning controlling polyvinyl alcohol glue aqueous systems and gac is 1:1, and the pressed active carbon made has good water wettability.The methylene blue adsorption value of each constitutive activity charcoal sample with raw material gac than the decline had in various degree.Analyzing its reason, may be because have a certain amount of Binder Composition in the grain active carbon prepared, and not through charing.In the sample of one side equal in quality, the amount of gac declines to some extent; The pore structure of binding agent to gac has certain inhibition on the other hand.
Embodiment 2:
The enforcement of carboxymethyl cellulose-epoxy chloropropane bonding gac
Accurately take the carboxymethyl cellulose of 2g, be dissolved in the distilled water of 23g, stir lower swelling dissolving.Add the 2wt%NaOH basified half an hour of 5ml.In glue system, adding appropriate Powdered Activated Carbon, making glue/charcoal than being 2:1,1:1, numbering expression II-1, II-2.Add 0.4g, 0.67g epoxy chloropropane respectively, make the mass ratio of carboxymethyl cellulose and epoxy chloropropane be 5:1,3:1, numbering is respectively II-1-1, II-1-2, II-2-1, II-2-2.Put into the water bath with thermostatic control stirring heating of 65 DEG C after 1 hour, stop stirring, under the water bath with thermostatic control of this temperature, place 45 minutes.Use in acetic acid after completion of the reaction and pH extremely neutrality.Mixed solution is poured in mould, be placed in the baking oven of 110 DEG C and dry.After the solidification of its complete drying, soak with water, 3wt%HCl, 10wt%NaOH, carry out water-fast, acidproof, alkaline resistance properties test.
The water-acid resistance test result of table 2 carboxymethyl cellulose-epoxy chloropropane sizing agent composite activated carbon system
When the quality proportioning controlling carboxymethyl cellulose-epoxy chloropropane and gac is 2:1,1:1, the pressed active carbon made with this proportioning all has good water wettability.On the whole, glue/charcoal is than during for 2:1,1:1, and both glue charcoals can soak preferably, and glue consumption is too much unsuitable.As can be seen from Table 2, the better performances of water-fast, acidproof, the alkali resistance of the carboxymethyl cellulose gum-charcoal series of samples of preparation.
Carboxymethyl cellulose is a kind of water white transparency, nontoxic odorless organic adhesion agent, is widely used in food-processing and field of medicaments, is also well suited for the bonding of pressed active carbon in field of Environment Protection application.In experiment, utilize carboxymethyl cellulose-epoxy chloropropane binding agent obtain activated carbon sample water-fast, acid-fast alkali-proof is all fine.
Due to adding of binding agent, and binding agent is undeveloped compared with gac hole, must produce larger negative impact to the specific surface area of unit weight granulated active carbon, also may to block the hole of a part of gac without the binding agent of charing simultaneously.Therefore, the specific surface area of the grain active carbon that this experiment is obtained, absorption property smaller compared with raw material powder gac comparatively raw material gac decline to some extent.If sample specific surface area will be improved further, can by active carbon powder and carboxymethyl cellulose-epoxy chloropropane binding agent mixing, compound stalk forming, follow-up 200 DEG C of solidification heat process.
Embodiment 3:
The enforcement of polyvinyl alcohol-epoxy chloropropane-bicarbonate of ammonia binding agent
Accurately take the polyvinyl alcohol of 5 parts of 2g, be dissolved in the distilled water of 23g respectively, be placed in Erlenmeyer flask, in the baking oven of 93 DEG C, swelling dissolving, for subsequent use after cooling.Add the 2wt%NaOH aqueous solution alkalization half an hour of 5ml respectively.Add 0.4g epoxy chloropropane, make the mass ratio of polyvinyl alcohol and epoxy chloropropane be 5:1.Gac is added than for 1:1 by glue/charcoal.Then, add 0.1% of system gross weight respectively, 0.15%, 0.2%, 0.25%, the bicarbonate of ammonia of 0.3%, stirs, and numbering is respectively III-1, III-2, III-3, III-4, III-5.Put into the water bath with thermostatic control stirring heating of 65 DEG C after 1 hour, stop stirring, under the water bath with thermostatic control of this temperature, place 45 minutes.Use in acetic acid after completion of the reaction and pH extremely neutrality.Mixed solution is poured in mould, be placed in the baking oven of 110 DEG C and dry, solidification.After the solidification of its complete drying, soak with water, 3wt%HCl, 10wt%NaOH, carry out water-fast, acidproof, alkaline resistance properties test.As can be seen from table 3 result, though sample adds a small amount of bicarbonate of ammonia, produce gas, form pore, water-acid resistance is consistent with the effect not adding bicarbonate of ammonia.
The water-acid resistance test result of the type charcoal of the different ammonium bicarbonate content of table 3
Add whipping agent bicarbonate of ammonia preparing in pressed active carbon process, the amount containing bicarbonate of ammonia be the specific surface area of the sample of 0.15% than content 0.1%, the sample of 0.2%, 0.3% all wants large.In experiment, the bicarbonate of ammonia containing 0.15% makes up the best results of glue system to the blocking of pressed active carbon hole, and its specific surface area is maximum, and preliminary survey result is 414.2m
2/ g.Add whipping agent bicarbonate of ammonia and have considerable influence to activated carbon structure, more larger holes can be produced.In experiment, if the pressed active carbon of preparation is thicker, in preparation process, under Powdered Activated Carbon can sink to because of action of gravity, and binding agent can on gac.Control the pressed active carbon thinner thickness of preparation, better effects if.
Application Example:
Polyvinyl alcohol-epoxy chloropropane-bicarbonate of ammonia binding agent composite activated carbon process is containing the enforcement of cadmium simulated wastewater
In the volumetric flask of 1L, use CdCl
2the Cd of configuration containing 50mg
2+solution.Use Atomic Absorption Spectroscopy AAS test different concns containing Cd
2+the atom absorbancy of solution.Experimentally Plotting data typical curve.Composite activated carbon sample is: with mass percent 8% polyvinyl alcohol water solution, binding agent is prepared into the quality proportioning of 5:1 with epoxy chloropropane, glue/charcoal than being 1:1, add 0.1% of system gross weight respectively, 0.15%, 0.2%, 0.3% bicarbonate of ammonia obtains type charcoal, carries out Cd
2+adsorption effect is tested.Take 1g series composite activated carbon sample and be placed in the 50mg/L of 100ml containing Cd
2+in solution, standing adsorption, different time sections is got supernatant liquor and is measured on Atomic Absorption Spectroscopy AAS, obtains mean value.The Cd of different adsorption time is obtained by typical curve
2+concentration, then the specific absorption obtaining final each activated carbon sample.
The speed of type charcoal sample adsorption cadmium ion is very fast, and after absorption 1h, the speed of type charcoal Adsorption of Cadmium slows down, and becomes steady, and through the absorption of 12 hours, in solution, the concentration of cadmium ion was basicly stable, finally reaches absorption saturated.Relatively obtain, the binding agent prepared with the quality proportioning of 5:1 with mass percent 8% polyvinyl alcohol water solution and epoxy chloropropane, adding pressed active carbon prepared by 0.1% bicarbonate of ammonia is 78.8% to the adsorption rate of cadmium ion; Adding type charcoal prepared by 0.15% bicarbonate of ammonia is 89.5% to the adsorption rate of cadmium ion; Adding type charcoal prepared by 0.2% bicarbonate of ammonia is 93.4% to the adsorption rate of cadmium ion; The type charcoal adding 0.3% bicarbonate of ammonia is 98.9% to the adsorption rate of cadmium ion.Polyvinyl alcohol-epoxy chloropropane-bicarbonate of ammonia binding agent composite activated carbon is in the application of 50mg/L cadmium ion process, and the treatment effect of the pressed active carbon of the bicarbonate of ammonia containing 0.3% is best.
In sum, the present invention effectively overcomes various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (6)
1. a preparation method for hydrophilic porous pressed active carbon, comprises the steps:
The aqueous solution of step 1) preparation proper concn water soluble hydroxy polymkeric substance: take a certain amount of water-soluble hydroxyl polymer-containing, be dissolved in appropriate distilled water, make swelling dissolving, for subsequent use after cooling;
Step 2) add the 2wt%NaOH aqueous solution alkalization half an hour, in glue system, add appropriate gac;
Step 3) adds appropriate linking agent epoxy chloropropane, controls the mass ratio of water soluble hydroxy polymkeric substance and epoxy chloropropane;
Step 4) adds the whipping agent bicarbonate of ammonia accounting for system gross weight 0.1%-0.3%, stirs;
Step 5) is under the water bath with thermostatic control of 65 DEG C, and stirring reaction 1-2 hour, uses in acetic acid and pH extremely neutrality after completion of the reaction;
Mould poured into by step 6) gac mixed solution, is placed in the baking oven of 110 DEG C and dries.
2. the preparation method of a kind of hydrophilic porous pressed active carbon as claimed in claim 1, is characterized in that, described water-soluble hydroxyl polymer-containing is selected from the one in polyvinyl alcohol, carboxymethyl cellulose, water soluble starch.
3. the preparation method of a kind of hydrophilic porous pressed active carbon as claimed in claim 2, is characterized in that, the concentration of the aqueous solution of described water-soluble hydroxyl polymer-containing is 8wt%.
4. the preparation method of a kind of hydrophilic porous pressed active carbon as claimed in claim 1, is characterized in that, described step 2) in, carboxymethyl cellulose is g:ml=2:5 with the ratio of the add-on of the 2wt%NaOH aqueous solution.
5. the preparation method of a kind of hydrophilic porous pressed active carbon as claimed in claim 1, is characterized in that, described step 2) in, the mass ratio of glue system and gac is 1-2:1.
6. the preparation method of a kind of hydrophilic porous pressed active carbon as claimed in claim 1, is characterized in that, in described step 3), the mass ratio of water soluble hydroxy polymkeric substance and epoxy chloropropane is 3-5:1.
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| CN105131661A (en) * | 2015-09-30 | 2015-12-09 | 江苏通瑞环保科技发展有限公司 | Preparation method for paint with activated carbon as base material |
| CN106188925A (en) * | 2016-08-09 | 2016-12-07 | 叶剑 | A kind of polyphenylacetylene combination for clad plate and manufacture method thereof |
| CN106824074A (en) * | 2017-02-17 | 2017-06-13 | 南平元力活性炭有限公司 | A kind of liquid phase preparation technology of rapid dispersion granular activated carbon |
| CN110128202A (en) * | 2019-05-31 | 2019-08-16 | 襄阳农博源农业有限公司 | A kind of biological organic fertilizer and preparation method thereof |
| 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 |
| CN114314582A (en) * | 2022-01-03 | 2022-04-12 | 安徽大学 | Preparation method of cross-linked porous activated carbon based on PVA gel |
| CN114381028A (en) * | 2020-10-16 | 2022-04-22 | 自然资源部天津海水淡化与综合利用研究所 | Photothermal conversion material, preparation method and application thereof, and method for seawater desalination, sewage treatment, water purification or solution purification |
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| CN105131661A (en) * | 2015-09-30 | 2015-12-09 | 江苏通瑞环保科技发展有限公司 | Preparation method for paint with activated carbon as base material |
| CN106188925A (en) * | 2016-08-09 | 2016-12-07 | 叶剑 | A kind of polyphenylacetylene combination for clad plate and manufacture method thereof |
| CN106824074A (en) * | 2017-02-17 | 2017-06-13 | 南平元力活性炭有限公司 | A kind of liquid phase preparation technology of rapid dispersion granular activated carbon |
| CN110128202A (en) * | 2019-05-31 | 2019-08-16 | 襄阳农博源农业有限公司 | A kind of biological organic fertilizer and preparation method thereof |
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| CN114381028A (en) * | 2020-10-16 | 2022-04-22 | 自然资源部天津海水淡化与综合利用研究所 | Photothermal conversion material, preparation method and application thereof, and method for seawater desalination, sewage treatment, water purification or solution purification |
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| CN114314582A (en) * | 2022-01-03 | 2022-04-12 | 安徽大学 | Preparation method of cross-linked porous activated carbon based on PVA gel |
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