The method of purification cocoanut active charcoal
Technical field
The present invention relates to gac purification field, more particularly, the present invention relates to a kind of method of cocoanut active charcoal of purifying.
Background technology
Cocoanut active charcoal is Exocarpium cocois (Cocos nucifera L) is raw material, obtain through carbonization and purifying technique, cocoanut active charcoal have hole prosperity, absorption property is good, intensity is high, easy regeneration, the advantage such as economy and durability, product is mainly used in taste removal, Drinking Water Filtrations etc. are a kind of emerging water-purifying materials.
The carbonization of Exocarpium cocois (Cocos nucifera L) comprises chemical carbonization and physics carbonization two kinds of methods, and Exocarpium cocois (Cocos nucifera L) is placed in charring furnace by physics carborization exactly, carries out destructive distillation and anaerobic carbonization under the high temperature conditions.The cocoanut active charcoal obtained by physics carborization contains much impurity, therefore needs the purification processes of carrying out the later stage.
The later purification treatment process of gac also comprises chemical method and Physical two kinds, chemical method is purified the ash and objectionable impurities that can reduce in gac, but also greatly reduce the activity of gac, and introduce new objectionable impurities, cause the Application Areas of gac to be restricted.
Traditional physical purification method directly utilizes water vapour to carry out boiling to gac, the activated carbon capillary obtained is more flourishing, specific surface area is higher, but mesopore is not very flourishing, limit the application of gac, therefore invent a kind of method of purification that can improve the activated coco nut charcoal of mesopore fraction of coverage and be called the problem needing solution badly.
Summary of the invention
An object of the present invention is to solve at least the problems referred to above, and the advantage will illustrated at least is below provided.
The object of the present invention is to provide a kind of method of cocoanut active charcoal of purifying, it uses the treatment process of Chemical bond physics, and the gac obtained is purer, and mesopore fraction of coverage is higher.
A further object of the invention utilizes hydrogen peroxide to Activated Carbon Pretreatment, utilizes alcohol to carry out reprocessing to gac, and recycling high-temperature vapor carries out aftertreatment to gac, improves the purity of gac and the content of mesopore.
A further object of the invention is that hydrogen peroxide is infiltrated gac inside, recycling neutral spirits assimilating activity charcoal internal moisture, improves the concentration of hydrogen peroxide, finally uses high-temperature steam to rinse, make hydrogen peroxide fiercely be decomposed into moisture and oxygen, thus increase the middle hole number of gac.
In order to realize, according to these objects of the present invention and other advantage, providing a kind of method of cocoanut active charcoal of purifying, wherein, comprising:
Step one, rough cocoanut active charcoal is dried to constant weight at 80-85 DEG C, is then soak 2-2.5h in the hydrogen peroxide of 27-35% in the concentration of 1-10 times of volume, filters and obtain product A; Cocoanut active charcoal being dried to constant weight can avoid moisture in coconut husk and other compositions to dioxygen water mitigation, and dried cocoanut active charcoal can absorb and permeate more hydrogen peroxide, after hydrogen peroxide enters gac, rest on the inside of gac, hydrogen peroxide is in the process of infiltrating gac, can carry out slight oxidation to gac, thus the aperture of expansion micropore by a small margin forms mesopore, increases the quantity of mesopore.The micropore size of gac is generally at below 1nm, can filter air molecule, mesopore pore size, generally at more than 1nm, can be used for aspects such as gas adsorption, liquid filtering and Application in Chemical Engineering, and the quantity therefore increasing mesopore can expand or the Application Areas of gac.
Step 2, at 0-3 DEG C, be soak 30-35min in the alcohol of 95-100% by the concentration of products obtained therefrom A and 1-10 times volume, filter obtain product B; After hydrogen peroxide enters gac inside, utilize high density or moisture absorption is fallen by pure alcohol, the hydrogen peroxide of gac inside becomes dense hydrogen peroxide, thus effectively oxidation expansion aperture is carried out to the micropore of gac inside, avoid carrying out over oxidation to the micropore of gac outside.Hydrogen peroxide and alcohol can not react under 0-3 DEG C of state, therefore, it is possible to ensure the security of reaction.
Step 3, at 10-15 DEG C, products obtained therefrom B is left standstill 0.5-3h, ventilation keeps 4-8m
3/ min, obtains products C; After the complete moisture of alcohol absorption, gac is taken out leave standstill rapidly, use large ventilation the alcohol volatilization on gac to be removed rapidly, reduce the content of alcohol as far as possible, avoid the impact on next step, obtain the inner gac containing hydrogen peroxide.
The 860-870 DEG C of high-temperature steam that step 4, use pressure are 3-4mpa rinses 30-40min to the products C of gained, obtains product D; Utilize high-temperature steam to carry out activation treatment to gac, high-temperature steam drives gac constantly to roll in reaction tank, and is cemented out by the impurity in gac; Meanwhile, the hydrogen peroxide of gac inside is at high temperature decomposed into rapidly oxygen G&W, and oxygen can make gac form more hole, and the filter pore quantity of the gac increased, improves the strainability of gac.
Step 5, continuation use the 760-770 DEG C of high-temperature steam that pressure is 4-5mpa to rinse 70-90min to the product D of gained, obtain product E; Continue to use high-temperature vapor to activate gac, substitutional impurity, residue such as cleaning hydrogen peroxide or alcohol etc., make the brighter of gac, purity is higher, and because hydrogen peroxide is at high temperature decomposed into oxygen G&W completely, alcohol is also rinsed totally, therefore the gac obtained does not have other impurity or objectionable impurities, and the field of application is more wide.
Above step does not arrange stirring rod and stirs gac as traditional method, avoids the collision of gac and hard object, reduces charcoal loss rate.
Step 6, products obtained therefrom E to be shifted out, use atmospheric steam to rinse, until temperature drops to 110-115 DEG C, obtain product F; Continue to use water vapour to rinse, make gac slow cooling, avoid huge temperature variation to impact Properties of Activated Carbon.
Step 7, namely products obtained therefrom F dry 13-15h at 110-115 DEG C is obtained cocoanut active charcoal of the present invention.Seal up for safekeeping packing after gac drying.
Preferably, in the method for described purification cocoanut active charcoal, the preparation method of rough coconut husk described in step one is: after Exocarpium cocois (Cocos nucifera L) carbonization, grinds to form the particle that particle diameter is 0.6-4mm, obtains described rough cocoanut active charcoal.In order to improve active efficiency and effect, cocoanut active charcoal is ground to form certain size, then carry out activation treatment.
Preferably, in the method for described purification cocoanut active charcoal, carbonization machine is utilized to carry out physics carbonization to described Exocarpium cocois (Cocos nucifera L).The carbonization of Exocarpium cocois (Cocos nucifera L) comprises Physical carbonization and chemical method carbonization, and candidate logos uses carbonization machine to carry out mechanical carbonization to Exocarpium cocois (Cocos nucifera L) here, avoids introducing impurity atom.
Preferably, in the method for described purification cocoanut active charcoal, utilize waterproof ventilated membrane to filter the water vapour after being utilized by step 5, collect the hot water leached and carry out recycle.A kind of existing macromolecular material of waterproof ventilated membrane, with here can by the moisture filter in water vapour and the current that congeal into, gas then can be drained by air film.
Preferably, in the method for described purification cocoanut active charcoal, in step 4, washing condition is time 35min, temperature 865 DEG C, and pressure is 3.5mpa.Temperature is 865 degrees Celsius time, and the activation rate of carbon is the highest, and the time, 35min was best again, and long meeting makes the loss on ignition of gac increase, and yield rate reduces.
Preferably, in the method for described purification cocoanut active charcoal, in step 5, washing condition is time 80min, temperature 765 DEG C, and pressure is 4.5mpa.Temperature is 765 degrees Celsius time, and the activation rate of carbon is higher, and the time, 80min was best again, and this process mainly carries out displacement and the cleaning of impurity to gac, therefore temperature needs lower, and the time is longer.
Preferably, in the method for described purification cocoanut active charcoal, in described step one, the concentration of hydrogen peroxide is 30%.The concentration of hydrogen peroxide is best with 30%, and the external oxidation of gac was destroyed by too high words before hydrogen peroxide does not infiltrate gac inside, the too low micropore being not enough to again magnesium oxide/absorbent charcoal.
The present invention at least comprises following beneficial effect: first, the chemical process that abandoning tradition gac of the present invention is purified and pure physical method, chemical process and physical method are combined, both the impurity in scavenging capacity charcoal and objectionable impurities, the content of gac mesopore can be improved again, can not introduce new objectionable impurities and impurity, therefore than traditional physico-chemical process, environmental protection is effective more simultaneously.
Secondly, method of the present invention does not need stirring rod to stir gac, decreases the collision of gac, reduces charcoal loss rate, and method of the present invention does not reduce the mechanical abrasive wear resistance of gac, and the surface of gac is brighter.
Again, first method of the present invention uses hydrogen peroxide to soak gac, hydrogen peroxide is made to enter gac inside, expand the aperture of gac, and then utilize moisture in alcohol in high concentration assimilating activity charcoal, make hydrogen peroxide persist gac inside, finally utilize high-temperature vapor to rinse gac, make fast decoupled under hydrogen peroxide high temperature form water and oxygen, these oxygen can increase the aperture of gac and increase the quantity in charcoal absorption hole.Whole process does not introduce new impurity, and hydrogen peroxide used and alcohol are all decomposed or evaporate, therefore very clean and effective.
Part is embodied by explanation below by other advantage of the present invention, target and feature, part also will by research and practice of the present invention by those skilled in the art is understood.
Embodiment
Below in conjunction with example, the present invention is described in further detail, can implement according to this with reference to specification sheets word to make those skilled in the art.
Example 1
One, the preparation of gac
After Exocarpium cocois (Cocos nucifera L) being used carbonization machine carbonization, grind to form the particle that particle diameter is 0.85mm, obtain rough cocoanut active charcoal; Rough cocoanut active charcoal is dried to constant weight at 80 DEG C, is then soak 2h in the hydrogen peroxide of 27% in the concentration of 2 times of volumes, filters and obtains product A; At 0 DEG C, be soak 35min in the alcohol of 95% by the concentration of products obtained therefrom A and 2 times volume, filter and obtain product B; At 10 DEG C, products obtained therefrom B is left standstill 0.5h, ventilation keeps 8m
3/ min, obtains products C; Use 860 DEG C of high-temperature steams that pressure is 3mpa to rinse 40min to the products C of gained, obtain product D; Continue to use 760 DEG C of high-temperature steams that pressure is 4mpa to rinse 90min to the product D of gained, obtain product E; Products obtained therefrom E is shifted out, uses atmospheric steam to rinse, until temperature drops to 110 DEG C, obtain product F; Namely products obtained therefrom F dry 15h at 110 DEG C is obtained cocoanut active charcoal of the present invention.
Two, performance test
Measure the yield (i.e. the weight ratio of gained gac and crude active charcoal) of cocoanut active charcoal of the present invention, the method specified according to GB GB/T12496.10-1999 carries out the mensuration of methylene blue adsorption value to cocoanut active charcoal of the present invention, the method specified according to GB/T12496.5-1999 measures tetracol phenixin adsorption rate (activity), and result is as following table 1:
From upper table 1, the yield of gac of the present invention is all up to state standards up to the yield of 72% ultra-traditional method far away, methylene blue adsorption value and tetracol phenixin adsorption rate.
Example 2
One, the preparation of gac
After Exocarpium cocois (Cocos nucifera L) being used carbonization machine carbonization, grind to form the particle that particle diameter is 1.4mm, obtain rough cocoanut active charcoal; Rough cocoanut active charcoal is dried to constant weight at 82 DEG C, is then soak 2h in the hydrogen peroxide of 30% in the concentration of 5 times of volumes, filters and obtains product A; At 3 DEG C, be soak 31min in the alcohol of 99.9% by the concentration of products obtained therefrom A and 5 times volume, filter and obtain product B; At 15 DEG C, products obtained therefrom B is left standstill 3h, ventilation keeps 4m
3/ min, obtains products C; Use 870 DEG C of high-temperature steams that pressure is 4mpa to rinse 30min to the products C of gained, obtain product D; Continue to use 760 DEG C of high-temperature steams that pressure is 5mpa to rinse 90min to the product D of gained, obtain product E; Products obtained therefrom E is shifted out, uses atmospheric steam to rinse, until temperature drops to 115 DEG C, obtain product F; Namely products obtained therefrom F dry 13h at 115 DEG C is obtained cocoanut active charcoal of the present invention.
Two, performance test
Measure the yield (i.e. the weight ratio of gained gac and crude active charcoal) of cocoanut active charcoal of the present invention, the method specified according to GB GB/T12496.10-1999 carries out the mensuration of methylene blue adsorption value to cocoanut active charcoal of the present invention, the method specified according to GB/T12496.5-1999 measures tetracol phenixin adsorption rate (activity), and result is as following table 2:
From upper table 2, the yield of gac of the present invention is all up to state standards up to the yield of 75% ultra-traditional method far away, methylene blue adsorption value and tetracol phenixin adsorption rate.
Example 3
One, the preparation of gac
After Exocarpium cocois (Cocos nucifera L) being used carbonization machine carbonization, grind to form the particle that particle diameter is 2mm, obtain rough cocoanut active charcoal; Rough cocoanut active charcoal is dried to constant weight at 83 DEG C, is then soak 2h in the hydrogen peroxide of 30% in the concentration of 7 times of volumes, filters and obtains product A; At 0 DEG C, be soak 33min in the alcohol of 97% by the concentration of products obtained therefrom A and 7 times volume, filter and obtain product B; At 10 DEG C, products obtained therefrom B is left standstill 2.5h, ventilation keeps 6m
3/ min, obtains products C; Use 865 DEG C of high-temperature steams that pressure is 3.5mpa to rinse 35min to the products C of gained, obtain product D; Continue to use 765 DEG C of high-temperature steams that pressure is 3.5mpa to rinse 80min to the product D of gained, obtain product E; Products obtained therefrom E is shifted out, uses atmospheric steam to rinse, until temperature drops to 110 DEG C, obtain product F; Namely products obtained therefrom F dry 14h at 110 DEG C is obtained cocoanut active charcoal of the present invention.
Two, performance test
Measure the yield (i.e. the weight ratio of gained gac and crude active charcoal) of cocoanut active charcoal of the present invention, the method specified according to GB GB/T12496.10-1999 carries out the mensuration of methylene blue adsorption value to cocoanut active charcoal of the present invention, the method specified according to GB/T12496.5-1999 measures tetracol phenixin adsorption rate (activity), and result is as following table 3:
From upper table 3, the yield of gac of the present invention is all up to state standards up to the yield of 73% ultra-traditional method far away, methylene blue adsorption value and tetracol phenixin adsorption rate.
Example 4
One, the preparation of gac
After Exocarpium cocois (Cocos nucifera L) being used carbonization machine carbonization, grind to form the particle that particle diameter is 2.8mm, obtain rough cocoanut active charcoal; Rough cocoanut active charcoal is dried to constant weight at 85 DEG C, is then soak 2.2h in the hydrogen peroxide of 31% in the concentration of 8 times of volumes, filters and obtains product A; At 1 DEG C, be soak 33min in the alcohol of 99% by the concentration of products obtained therefrom A and 8 times volume, filter and obtain product B; At 13 DEG C, products obtained therefrom B is left standstill 2h, ventilation keeps 5m
3/ min, obtains products C; Use 868 DEG C of high-temperature steams that pressure is 3mpa to rinse 38min to the products C of gained, obtain product D; Continue to use 766 DEG C of high-temperature steams that pressure is 4.5mpa to rinse 85min to the product D of gained, obtain product E; Products obtained therefrom E is shifted out, uses atmospheric steam to rinse, until temperature drops to 115 DEG C, obtain product F; Namely products obtained therefrom F dry 13h at 115 DEG C is obtained cocoanut active charcoal of the present invention.
Two, performance test
Measure the yield (i.e. the weight ratio of gained gac and crude active charcoal) of cocoanut active charcoal of the present invention, the method specified according to GB GB/T12496.10-1999 carries out the mensuration of methylene blue adsorption value to cocoanut active charcoal of the present invention, the method specified according to GB/T12496.5-1999 measures tetracol phenixin adsorption rate (activity), and result is as following table 4:
From upper table 4, the yield of gac of the present invention is all up to state standards up to the yield of 78% ultra-traditional method far away, methylene blue adsorption value and tetracol phenixin adsorption rate.
Example 5
One, the preparation of gac
After Exocarpium cocois (Cocos nucifera L) being used carbonization machine carbonization, grind to form the particle that particle diameter is 4mm, obtain rough cocoanut active charcoal; Rough cocoanut active charcoal is dried to constant weight at 82 DEG C, is then soak 2h in the hydrogen peroxide of 33% in the concentration of 8 times of volumes, filters and obtains product A; At 0 DEG C, be soak 30min in the alcohol of 99% by the concentration of products obtained therefrom A and 10 times volume, filter and obtain product B; At 13 DEG C, products obtained therefrom B is left standstill 2h, ventilation keeps 5m
3/ min, obtains products C; Use 870 DEG C of high-temperature steams that pressure is 3mpa to rinse 38min to the products C of gained, obtain product D; Continue to use 760 DEG C of high-temperature steams that pressure is 4.5mpa to rinse 85min to the product D of gained, obtain product E; Products obtained therefrom E is shifted out, uses atmospheric steam to rinse, until temperature drops to 115 DEG C, obtain product F; Namely products obtained therefrom F dry 13h at 115 DEG C is obtained cocoanut active charcoal of the present invention.
Two, performance test
Measure the yield (i.e. the weight ratio of gained gac and crude active charcoal) of cocoanut active charcoal of the present invention, the method specified according to GB GB/T12496.10-1999 carries out the mensuration of methylene blue adsorption value to cocoanut active charcoal of the present invention, the method specified according to GB/T12496.5-1999 measures tetracol phenixin adsorption rate (activity), and result is as following table 5:
From upper table 5, the yield of gac of the present invention is all up to state standards up to 69% yield exceeding traditional method, methylene blue adsorption value and tetracol phenixin adsorption rate.
Although embodiment of the present invention are open as above, it is not restricted to listed in specification sheets and embodiment utilization.It can be applied to various applicable the field of the invention completely.For those skilled in the art, can easily realize other amendment.Therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the example described.