CN104789159B - A kind of pressed active carbon preparation method of shitosan binding agent - Google Patents
A kind of pressed active carbon preparation method of shitosan binding agent Download PDFInfo
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- CN104789159B CN104789159B CN201410022175.2A CN201410022175A CN104789159B CN 104789159 B CN104789159 B CN 104789159B CN 201410022175 A CN201410022175 A CN 201410022175A CN 104789159 B CN104789159 B CN 104789159B
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Abstract
The present invention relates to field of functional materials, more particularly to a kind of pressed active carbon preparation method of shitosan binding agent.The present invention provides a kind of pressed active carbon preparation method of shitosan binding agent, comprises the following steps：Add water configuration aqueous acid, weighs shitosan and is dissolved in aqueous acid, obtains chitosan solution；By in crosslinking agent addition chitosan solution under stirring；To adding appropriate activated carbon in reaction system；20 60 DEG C of temperature of reaction system of control, the mixed liquor 2h of cross-linking reaction 1 under agitation is placed in after standing 2h in air, is defoamed；Gained reaction solution is placed in 15 30min in 100 120 DEG C of baking oven, finally reaction solution is poured into mould, dried.Present invention process is simple, and easy to operate, the binding agent for using is hydrophilic agglomerant, and obtained pressed active carbon remains the water-fast of shitosan binding agent, acid and alkali-resistance, hydrophily advantage performance to a certain extent.
Description
Technical field
The present invention relates to field of functional materials, more particularly to a kind of pressed active carbon preparation side of shitosan binding agent
Method.
Background technology
Activated carbon has flourishing pore structure and huge specific surface area, thus its adsorption capacity to various materials is non-
Chang Qiang.The application of activated carbon widely, at present have been used to environmental protection, Gas Phase Adsorption, liquid phase adsorption, medicine, food, chemical industry,
All many-sides such as agricultural.Present activated carbon product is mainly Powdered Activated Carbon, but Powdered Activated Carbon is difficult storage, easily causes
Dust pollution, and be possible to pile up and cause resistance excessive when material for water treatment is made, treatment effeciency reduction.With Powdered Activated Carbon
Compare, pressed active carbon has larger size and definite shape, bulk density and intensity higher, and no dust pollution.
In storage transportation, the big pressed active carbon of density has more advantage.
Pressed active carbon has been applied to the various aspects in life and industry.In terms of environmental protection of living, pressed active carbon is
Through the main material as filtration core in water purifier, pressed active carbon is also widely used in the purification of air aspect of closing space.
The intensity and machinability of pressed active carbon, are also beneficial to meet some industrial circle applications than general activated carbon.Movable forming
Property charcoal can as needed be prepared into different scale, convenient for assembly in various equipment, device, and long service life.
With binding agent by the method for powder active carbon molding bonded because its simple technique and cheap cost are increasingly received
To concern.In this method, the key factor of pressed active carbon performance quality is turned into using suitable binding agent.The kind of adhesive
Class, addition all have significant effect to the specific surface area of pressed active carbon, intensity and forming ability.Wang Rui etc. is fine by carboxymethyl
Dimension element soaks 24h in quantitative distilled water, and fully dissolving adds certain Powdered Activated Carbon, strong stirring half an hour, to be mixed
It is placed in after uniform in drying box and is concentrated, stirred once with glass bar per half an hour when drying, prevent caking, is taken out after drying,
It is press-formed in cylindrical mold, by 200-300 DEG C of charing, obtains column-shaped active carbon.（Wang Rui, Chen Hua, Liu Shouxin, CMC glue
Connection prepares column pressed active carbon, chemistry of forest product and industry, 2011,31（5）：6-10.）
Suitable binding agent can prepare pressed active carbon for environment water process, and this binding agent is except activated carbon to be kept
Specific surface area high, in addition it is also necessary to strong water-fast acid-fast alkali-proof performance, must also have excellent hydrophilic in addition.Therefore, movable forming
When property charcoal is applied to field of waste water treatment, the organic binder bond for being used also needs to update.
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 pressed active carbon shitosan
The preparation method of binding agent, for solving the problems of the prior art.
The present invention develops shitosan-citric acid-cross linker system as pressed active carbon using various advantages of shitosan
Use binding agent.Shitosan, in 100-120 DEG C of reaction, can occur the condensation reaction generation ester group of hydroxyl and carboxyl with citric acid, real
Now it is crosslinked.Easy and crosslinking agent such as glutaraldehyde crosslinks reaction to shitosan at room temperature.Shitosan-citric acid-the crosslinking of preparation
Agent binding agent composite activated carbon system, using shitosan and crosslinking agent such as glutaraldehyde reaction generation stabilization chemical bond, then carries out heat
Treatment, makes shitosan that heat cross-linking occur with citric acid simultaneously, obtains pressed active carbon, and the system has good water resistance, resistance to
Sour alkali resistance.
In order to achieve the above objects and other related objects, the present invention is achieved through the following technical solutions：
The present invention provides a kind of pressed active carbon preparation method of shitosan binding agent, comprises the following steps：
Step 1）：Add water the certain density aqueous acid of configuration, weighs appropriate shitosan and is dissolved in aqueous acid, obtains
Obtain chitosan solution；The acid is mainly citric acid；
Step 2）：By in crosslinking agent addition chitosan solution under stirring, the mass ratio of shitosan and crosslinking agent is controlled；
Step 3）：To the charge ratio that appropriate activated carbon, control system and activated carbon are added in reaction system；
Step 4）：20-60 DEG C of temperature of reaction system of control, mixed liquor cross-linking reaction 1-2h under agitation is placed in air
After standing 2h, defoam；
Step 5）：By step 4）Gained reaction solution is placed in 15-30min in 100-120 DEG C of baking oven, finally falls reaction solution
Enter in mould, dry.
Preferably, the concentration of the lemon aqueous acid is 5-15wt%.
Preferably, the chitosan dosage accounts for the 1-2wt% of aqueous acid weight.
Preferably, the crosslinking agent mainly has glutaraldehyde, epoxychloropropane, polysuccinimide, ethylene glycol two to shrink sweet
Oily ether, sodium polyphosphate.
Preferably, shitosan and the mass ratio of crosslinking agent are 15-25：1, more preferably 15-20：1.
Preferably, the step 3）In, when adding activated carbon, the mass ratio of control system and activated carbon（Glue/charcoal ratio）For
1-2：1.
The beneficial effects of the invention are as follows：Present invention process is simple, and easy to operate, the binding agent for using is hydrophilic binder
Agent, obtained pressed active carbon remains the water-fast of shitosan binding agent, acid and alkali-resistance, hydrophily dominance to a certain extent
Energy.
Brief description of the drawings
Fig. 1 is the infrared spectrum of shitosan of the present invention and 7wt% citric acid heat cross-linking product；
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 pressed active carbon preparation method of shitosan binding agent, comprises the following steps：
Step 1）Add water the certain density acid solution of configuration, weighs appropriate shitosan and is dissolved in acid solution；
Step 2）By in crosslinking agent addition chitosan solution under stirring, the mass ratio of shitosan and crosslinking agent is controlled；
Step 3）To the charge ratio that appropriate activated carbon, control binding agent and activated carbon are added in reaction system；
Step 4）20-60 DEG C of temperature of reaction system of control, mixed liquor cross-linking reaction 1-2h under agitation is placed in quiet in air
After putting 2h, defoam；
Step 5）Reaction solution is placed in 15-30min in 100-120 DEG C of baking oven, finally reaction solution is poured into mould,
Dry.
Further, the acid is mainly citric acid.
Further, the crosslinking agent mainly has glutaraldehyde, epoxychloropropane, polysuccinimide, the shrink of ethylene glycol two
Glycerin ether, sodium polyphosphate.
Further, it is described can be used as use in waste water treatment pressed active carbon.
Embodiment 1：
The preparation of shitosan-citric acid heat cross-linking binding agent：
Shitosan-lemon acid binder composite activated carbon sample is prepared in a heated state.1g shitosans are taken, is added into
During 50ml percentage by weights are 7% aqueous citric acid solution, stirring is to dissolving.A certain amount of activated carbon of stirring addition, control glue/
Charcoal ratio is 1:1、2:1, solution is put into 120 DEG C of drying box, taken out after half an hour.During product moved into mould, sky is placed in
Drying at room temperature in gas.Shitosan and citric acid reacts half an hour at 100-120 DEG C in activated carbon mixed liquor can realize crosslinking, make
Composite activated carbon samples with water, the 3wt%HCl aqueous solution, the 10wt%NaOH aqueous solution carry out long-acting immersion test.Research hair
Existing, shitosan-citric acid binder system, without swelling, can keep original grain shape, and energy in water, acid, aqueous slkali
Place more than 15 days, do not come unglued, without breakage, good water-fast, resistance to acids and bases, hydrophilicity is presented.
1g shitosans are taken, is added into the aqueous citric acid solution that 50ml percentage by weights are 7%, stirring to dissolving.Will be molten
Liquid is put into 120 DEG C of drying box, and the cross-linking products of shitosan and citric acid are taken out after half an hour.With absolute ethyl alcohol by unreacted
Citric acid and after other small molecules wash away, examination of infrared spectrum is carried out, shown in result figure 1.With reference to shitosan and citric acid
Knowable to design feature and characteristic absorption peak, 3250cm-1O-H characteristic absorption bands in the citric acid carboxyl at place disappear,
1700cm-1And 1750cm-1Two C ﹦ O characteristic absorption bands of diverse location disappear in neighbouring citric acid, but in 1735cm-1Nearby there are C ﹦ O characteristic absorption bands.Result shows that shitosan is crosslinked in a heated state with citric acid, generates ester
Base.
Using three carboxyls are contained in citric acid, can be reacted with hydroxyl or amino.Conventional second is substituted with citric acid
Acid, shitosan can be dissolved in citric acid solution.Due to containing great amount of hydroxy group in shitosan, in experiment, shitosan and polynary sour lime
Acid is heated to more than 100 DEG C, the condensation reaction generation ester group that hydroxyl and carboxyl can occur, and realizes heat cross-linking.
Embodiment 2：
The implementation of shitosan-citric acid-glutaraldehyde binding agent：
Prepare shitosan-citric acid-glutaraldehyde binding agent composite activated carbon.1g shitosans are dissolved in the lemon of 50ml7wt%
After lemon aqueous acid, stirring is lower to add glutaraldehyde（The 25wt% aqueous solution）, shitosan and the mass ratio of glutaraldehyde is respectively 15:
1、20:1, numbering is I, II, and agitating solution makes cross-linking reaction 1h, is placed in after standing 2h in air, is defoamed.Then to reaction
Activated carbon is added in system, it is 1 to control glue/charcoal ratio:1、2:1, sample number into spectrum is I -1, I -2, II -1, II -2, is reacted 2 hours
Afterwards, reaction solution is placed in 15min in 100 DEG C of baking oven, finally pours into mould reaction solution, dried.Then used water,
The 3wt%HCl aqueous solution, 10wt%NaOH aqueous solution soakings, carry out water-fast, acidproof, alkaline resistance properties test.
Shitosan can be crosslinked by the aldehyde of difunctional or acid anhydrides etc., form the insoluble product of network structure.First
Aldehyde, dialdehyde and glutaraldehyde can crosslink reaction with shitosan, and reaction can be carried out at room temperature, by aldehyde radical and shitosan
Amino form schiff base structure, reaction rate is very fast, can both carry out in aqueous, can also be reacted in heterogeneous medium
PH scopes it is also very wide.Reaction is mainly carried out, but be also not excluded for the cross-linking reaction of intramolecular intermolecular.
Easy and glutaraldehyde crosslinks reaction to shitosan at room temperature, and chitosan gel rubber has good water resistance, choosing
Adhesive is prepared with shitosan and glutaraldehyde reaction, then is heat-treated, while realizing the heat cross-linking with citric acid.Work as adhesive
1 is reached with active carbon powder mass ratio:When more than 1, both bonding agent and Powdered Activated Carbon can be soaked preferably.Adhesive it is resistance to
Water resistance to acids and bases represents that experimental result is as shown in table 1 using the time that water, acid, aqueous slkali soaking are come unglued to it.Can by table 1
Know that composite activated carbon sample does not rupture in each solution, avalanche can keep original grain shape, and can place more than 15
My god, show good patience.Result shows that the alternative acetic acid of citric acid realizes the dissolving of shitosan, while being handed over as heat
Connection agent, network cross-linked structure is constituted together with crosslinking agent glutaraldehyde with chitosan reaction, glues shitosan-citric acid-glutaraldehyde
Knot agent composite activated carbon has preferable water-fast and acid-proof alkaline.
Shitosan-citric acid-glutaraldehyde the binding agent for observing solidification finds that the binder system is tougher, and to commonly use second
Acid is more crisp for the shitosan binding agent of solvent.After dissolving shitosan with citric acid, then with glutaraldehyde carry out chemical crosslinking prepare it is viscous
Tie the water resistance of agent composite activated carbon more preferably, hardening time is also relatively short.Comprehensive shitosan-citric acid-glutaraldehyde binding agent
Solidification phenomenon and patience experiment, it is known that because citric acid take part in reaction, the adhesive structure after crosslinking is there occurs change, lead
Caused its structure and performance has notable difference with the binding agent prepared as solvent with acetic acid.
1 shitosan of table-citric acid-glutaraldehyde binding agent composite activated carbon water-acid resistance the performance test results
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 (2)
1. a kind of pressed active carbon preparation method of shitosan binding agent, comprises the following steps：
Step 1)：Add water configuration aqueous acid, and the acid is citric acid, and the concentration of the lemon aqueous acid is 5-
15wt%, weighs shitosan and is dissolved in aqueous acid, obtains chitosan solution, and the chitosan dosage accounts for aqueous acid weight
The 1-2wt% of amount；
Step 2)：Will be during crosslinking agent adds chitosan solution under stirring, the mass ratio of control shitosan and crosslinking agent, shitosan with
The mass ratio of crosslinking agent is 15-25：1；
Step 3)：To activated carbon is added in reaction system, the mass ratio of control system and activated carbon is 1-2：1；
Step 4)：20-60 DEG C of temperature of reaction system of control, mixed liquor cross-linking reaction 1-2h under agitation is placed in air and stands
After 2h, defoam；
Step 5)：By step 4) gained reaction solution be placed in 15-30min in 100-120 DEG C of baking oven, reaction solution is finally poured into mould
In tool, dry.
2. a kind of pressed active carbon as claimed in claim 1 preparation method of shitosan binding agent, it is characterised in that described
Crosslinking agent is selected from glutaraldehyde, epoxychloropropane, polysuccinimide, ethylene glycol diglycidylether, sodium polyphosphate.
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