CN105056894A - Novel adsorbent - Google Patents
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- CN105056894A CN105056894A CN201510490237.7A CN201510490237A CN105056894A CN 105056894 A CN105056894 A CN 105056894A CN 201510490237 A CN201510490237 A CN 201510490237A CN 105056894 A CN105056894 A CN 105056894A
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Abstract
The invention relates to a preparation method of a novel adsorbent. Firstly, rice husks are subjected to pretreatment including impurity removal, pyrolysis and acid pickling, then rice husk charcoal is treated with a Na2CO3 solution with a certain concentration under a certain condition, desiliconized rice husk charcoal is prepared and treated with vapor with a certain temperature, the treated modified desiliconized rice husk charcoal is subjected to esterification modification with succinic anhydride as an esterifying agent, dioxane as a solvent and triethylamine as a catalyst, and the novel adsorbent with a good hydrophobic effect and adsorption performance is prepared.
Description
Technical field
The invention belongs to field of new material preparation, be specifically related to a kind of preparation method of new adsorbent.
Background technology
Rice husk and paddy stalk are the byproduct of eating rice production, are more common agricultural wastes.Rice husk and the common processing method of paddy stalk are for burning, discard or using as low calorie fuels, and this way not only wastes resource, also causes certain pollution to environment and causes soil mineralization simultaneously.Rice husk and paddy stalk are originated as extraordinary charcoal, rice husk after charing and paddy straw-stem active charcoal have higher specific area, adsorbance is large, and the advantages such as advantages of good adsorption effect, the research in recent years for rice husk and paddy stalk comprehensive utilization also more and more comes into one's own.But because they contain abundant hydroxyl, show as stronger hydrophily, make its oil absorbency be difficult to meet the demands, also limit its application in organic matter Special adsorbent field.Common way is for utilizing heat treatment, esterification, hydroxyl wherein removes or by hydrophobic grouping substituting modification by the methods such as etherificate, thus obtain the adsorbent of adsorb organic compound better effects if, it is lower that the material that in conventional method, heat treatment is modified obtains charcoal rate, and hydrophobic effect is not obvious, the present invention take rice husk as raw material, first the silicon in rice husk is separated, again desiliconization rice husk is carried out steam activation and esterification modification, prepare a kind of cheapness and hydrophobic effect and the more superior new adsorbent of absorption property.
Retrieved domestic and foreign databases according to the technology of the present invention feature, find about with rice husk be raw material prepare the report of adsorbent and patent many.Such as, it is raw material with tetrabutyl titanate that Chinese patent CN103949211A proposes a kind of, adopts sol-gel process will to form the preparation method of adsorbent after nano titanium oxide and rice hull ash compound; Chinese patent CN102941066A describes a kind of utilization by certain density H
3pO
4solution-treated, and the rice husk activated at a certain temperature prepares the preparation method of diesel desulfurization sorbents; Chinese patent CN101670278A propose a kind of with rice hull ash or without silicon rice hull ash for raw material, by raw material and inorganic alkali solution mixed processing by a certain percentage, activate at a certain temperature more afterwards, the oily desulfuration adsorbent of obtained light ends.But there is not yet with rice husk is raw material, and it is carried out steam activation and esterification modification again with after desiliconization process, the report of the new adsorbent that preparation hydrophobicity is better, absorption property is more superior.
Summary of the invention
For Problems existing in background technology and deficiency, the object of the invention is to, with the agricultural wastes rice husk of cheapness for raw material, by processing and modification it, prepare a kind of new adsorbent.
Technical scheme of the present invention first rice husk is carried out the pretreatment of removal of impurities pyrolysis and pickling, and then use certain density Na
2cO
3solution processes rice hull carbon under certain condition and obtains desiliconization rice hull carbon, the steam treatment desiliconization rice husk of recycling uniform temperature, and be esterifying agent by the modification desiliconization rice husk after process with succinic anhydride, dioxane is solvent, triethylamine is that catalyst carries out esterification modification, and obtained have good hydrophobic effect and the new adsorbent of absorption property.
The technical solution used in the present invention specifically comprises the steps:
1. rice husk pretreatment: rice husk distilled water is cleaned the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, then the HCl solution being 1mol/L by dried rice husk and appropriate concentration mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
2. the preparation of desiliconization rice hull carbon: rice hull carbon pretreated in step 1 is put into flask and adds a certain amount of certain density Na
2cO
3solution, wherein, rice hull carbon and Na
2cO
3the mass ratio of solution is 0.3:1, Na
2cO
3the concentration of solution is 15%, flask is placed in constant temperature oil bath and boils 5h, and afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
3. the steam activation of desiliconization rice hull carbon: the desiliconization rice hull carbon in step 2 is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
4. the esterification modification of the rear desiliconization rice hull carbon of activation: the desiliconization rice hull carbon of getting in a certain amount of step 3 after steam activation is placed in and magnetic stirring apparatus is housed, in the there-necked flask of reflux condensing tube and thermometer, then succinic anhydride (esterifying agent) is added, dioxane (solvent) and certain density triethylamine (catalyst), back flow reaction certain hour under magnetic agitation and uniform temperature, wherein the concentration of catalyst is 0.65% ~ 0.95%, reaction temperature is 25 ~ 55 DEG C, reaction time is 7 ~ 10h, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, the i.e. obtained new adsorbent with good hydrophobic effect and larger adsorbance.
The invention has the advantages that:
(1) the present invention utilizes agricultural wastes Adsorbent Manufactured from Rice Husk, has higher economic worth, and solves an environmental issue serious greatly.
(2) the present invention utilizes salt Na
2cO
3solution extracts the silicon in rice hull carbon, compares other and utilizes highly basic NaOH solution to extract the method for silicon, reduce waste water handling problem, and more economy, safety, environmental protection;
(3) the present invention is directed to concrete purposes and simple esterification modification is carried out to adsorbent, effectively can improve the ability of its hydrophobicity and adsorb organic compound.
Specific embodiment
Illustrate this patent below by some embodiments, but the present invention does not limit by embodiment:
Embodiment 1:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h, obtained adsorbent 1.
Embodiment 2:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
(4) above-mentioned desiliconization rice hull carbon after steam activation is placed in the there-necked flask that magnetic stirring apparatus, reflux condensing tube and thermometer are housed, then the triethylamine that succinic anhydride, dioxane and concentration are 0.85% is added, back flow reaction 9h at magnetic agitation and 45 DEG C, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, obtained adsorbent 2.
Embodiment 3:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
(4) above-mentioned desiliconization rice hull carbon after steam activation is placed in the there-necked flask that magnetic stirring apparatus, reflux condensing tube and thermometer are housed, then the triethylamine that succinic anhydride, dioxane and concentration are 0.65% is added, back flow reaction 9h at magnetic agitation and 45 DEG C, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, obtained adsorbent 3.
Embodiment 4:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
(4) above-mentioned desiliconization rice hull carbon after steam activation is placed in the there-necked flask that magnetic stirring apparatus, reflux condensing tube and thermometer are housed, then the triethylamine that succinic anhydride, dioxane and concentration are 0.75% is added, back flow reaction 9h at magnetic agitation and 45 DEG C, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, obtained adsorbent 4.
Embodiment 5:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
(4) above-mentioned desiliconization rice hull carbon after steam activation is placed in the there-necked flask that magnetic stirring apparatus, reflux condensing tube and thermometer are housed, then the triethylamine that succinic anhydride, dioxane and concentration are 0.95% is added, back flow reaction 9h at magnetic agitation and 45 DEG C, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, obtained adsorbent 5.
Embodiment 6:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
(4) above-mentioned desiliconization rice hull carbon after steam activation is placed in the there-necked flask that magnetic stirring apparatus, reflux condensing tube and thermometer are housed, then the triethylamine that succinic anhydride, dioxane and concentration are 0.85% is added, back flow reaction 9h at magnetic agitation and 25 DEG C, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, obtained adsorbent 6.
Embodiment 7:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
(4) above-mentioned desiliconization rice hull carbon after steam activation is placed in the there-necked flask that magnetic stirring apparatus, reflux condensing tube and thermometer are housed, then the triethylamine that succinic anhydride, dioxane and concentration are 0.85% is added, back flow reaction 9h at magnetic agitation and 75 DEG C, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, obtained adsorbent 7.
Embodiment 8:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
(4) above-mentioned desiliconization rice hull carbon after steam activation is placed in the there-necked flask that magnetic stirring apparatus, reflux condensing tube and thermometer are housed, then the triethylamine that succinic anhydride, dioxane and concentration are 0.85% is added, back flow reaction 9h at magnetic agitation and 55 DEG C, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, obtained adsorbent 8.
Embodiment 9:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
(4) above-mentioned desiliconization rice hull carbon after steam activation is placed in the there-necked flask that magnetic stirring apparatus, reflux condensing tube and thermometer are housed, then the triethylamine that succinic anhydride, dioxane and concentration are 0.85% is added, back flow reaction 7h at magnetic agitation and 45 DEG C, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, obtained adsorbent 9.
Embodiment 10:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
(4) above-mentioned desiliconization rice hull carbon after steam activation is placed in the there-necked flask that magnetic stirring apparatus, reflux condensing tube and thermometer are housed, then the triethylamine that succinic anhydride, dioxane and concentration are 0.85% is added, back flow reaction 8h at magnetic agitation and 45 DEG C, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, obtained adsorbent 10.
Embodiment 11:
(1) get appropriate rice husk distilled water and clean the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
(2) be the Na of 15% by above-mentioned pretreated rice hull carbon 30g and mass concentration
2cO
3flask is put in the ratio mixing of solution 0.3:1 in mass ratio, and flask is placed in constant temperature oil bath and boils 5h, afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
(3) above-mentioned obtained desiliconization rice hull carbon is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
(4) above-mentioned desiliconization rice hull carbon after steam activation is placed in the there-necked flask that magnetic stirring apparatus, reflux condensing tube and thermometer are housed, then the triethylamine that succinic anhydride, dioxane and concentration are 0.85% is added, back flow reaction 10h at magnetic agitation and 45 DEG C, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, obtained adsorbent 11.
In above-described embodiment, in embodiment 1, adsorbent 1 is the desiliconization rice hull active carbon not carrying out esterification modification, and embodiment 2 ~ embodiment 11 changes catalyst concn, reaction temperature, reaction time in desiliconization rice hull active carbon esterification modification respectively and prepares different adsorbent.
The performance evaluation of new adsorbent
The performance of new adsorbent is evaluated by the test result of its oil absorbency and water absorption rate under similarity condition.Oil absorbency and wash water rate calculate by formula (1):
In formula: X---oil suction (water) rate of adsorbent, %;
M
1---the quality of adsorbed oil (water) front adsorbent, g;
M
2---the quality of adsorbed oil (water) adsorbent afterwards, g.
The experimental result of embodiment is as shown in table 1 below.
The performance test tables of data of table 1 new adsorbent
Can find out according to the oil suction of new adsorbent of display in table 1 and water absorption rate: catalyst concn, reaction temperature, the absorption property of reaction time on adsorbent all have impact; The oil absorbency of the adsorbent 2 that embodiment 2 is obtained is the highest, and reach 9.76g/g, corresponding hydrophobicity is best, water absorption rate drops to 0.11g/g, thus the optimum preparation condition of known new adsorbent is catalyst of triethylamine concentration is 0.85%, reaction temperature 45 DEG C, reaction time 9h.
Claims (5)
1. a new adsorbent, is characterized in that: the pretreatment first rice husk being carried out removal of impurities pyrolysis and pickling, and then uses certain density Na
2cO
3solution processes rice hull carbon under certain condition and obtains desiliconization rice hull carbon, the steam treatment desiliconization rice husk of recycling uniform temperature, and be esterifying agent by the modification desiliconization rice husk after process with succinic anhydride, dioxane is solvent, triethylamine is that catalyst carries out esterification modification, and obtained have good hydrophobic effect and the new adsorbent of absorption property.
2. a kind of new adsorbent as claimed in claim 1, it is characterized in that: the pretreated step of described rice husk is: rice husk distilled water is cleaned the impurity such as mud, to be placed in vacuum atmosphere sintering furnace dry 12h at 120 DEG C, the HCl solution being 1mol/L by dried rice husk and appropriate concentration afterwards mixes puts into flask, reflux condensation mode in constant temperature oil bath and boil 3h under constantly stirring, filter after removing most of impurity, filter residue distilled water be washed till neutrality and at 120 DEG C dry 12h, then dried rice husk is placed in pyrolysis 5h at vacuum atmosphere sintering furnace 500 DEG C, obtained rice hull carbon.
3. a kind of new adsorbent as claimed in claim 1, is characterized in that: the preparation process of described desiliconization rice hull carbon is: rice hull carbon pretreated in step 1 is put into flask and adds a certain amount of certain density Na
2cO
3solution, wherein, rice hull carbon and Na
2cO
3the mass ratio of solution is 0.3:1, Na
2cO
3the concentration of solution is 15%, flask is placed in constant temperature oil bath and boils 5h, and afterwards by suspension filtered, filter residue distilled water is washed till neutrality, and at 120 DEG C dry 12h, obtained desiliconization rice hull carbon.
4. a kind of new adsorbent as claimed in claim 1, is characterized in that: the steam activation step of described desiliconization rice hull carbon is: the desiliconization rice hull carbon in step 2 is placed in vacuum atmosphere sintering furnace, at steam flow 450cm
3under/min, be warming up to 500 DEG C, activation 0.5h.
5. a kind of new adsorbent as claimed in claim 1, it is characterized in that: after described activation, the esterification modification step of desiliconization rice hull carbon is: the desiliconization rice hull carbon of getting in a certain amount of step 3 after steam activation is placed in and magnetic stirring apparatus is housed, in the there-necked flask of reflux condensing tube and thermometer, then succinic anhydride (esterifying agent) is added, dioxane (solvent) and certain density triethylamine (catalyst), back flow reaction certain hour under magnetic agitation and uniform temperature, wherein the concentration of catalyst is 0.65% ~ 0.95%, reaction temperature is 25 ~ 55 DEG C, reaction time is 7 ~ 10h, suction filtration after the cooling of question response thing, wash for several times respectively with ethanol and distilled water again, and at 120 DEG C dry 12h, namely obtained have good hydrophobic effect and the new adsorbent of absorption property.
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| CN109081341A (en) * | 2018-09-30 | 2018-12-25 | 江苏斯沃得环保科技有限公司 | A kind of preparation method of mesoporous activated carbon |
| CN110042016A (en) * | 2019-05-08 | 2019-07-23 | 北京市新美达工贸有限公司 | A kind of use in dishwasher solid cleaning agent and preparation method thereof |
| CN110639479A (en) * | 2019-11-07 | 2020-01-03 | 江西省科学院能源研究所 | Rice husk ash/aluminum oxide decolorizing agent for treating printing and dyeing wastewater |
| CN111905696A (en) * | 2020-07-20 | 2020-11-10 | 长江大学 | Isatis root hydrothermal carbon oil absorbent and preparation method thereof |
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| CN110042016A (en) * | 2019-05-08 | 2019-07-23 | 北京市新美达工贸有限公司 | A kind of use in dishwasher solid cleaning agent and preparation method thereof |
| CN110639479A (en) * | 2019-11-07 | 2020-01-03 | 江西省科学院能源研究所 | Rice husk ash/aluminum oxide decolorizing agent for treating printing and dyeing wastewater |
| CN111905696A (en) * | 2020-07-20 | 2020-11-10 | 长江大学 | Isatis root hydrothermal carbon oil absorbent and preparation method thereof |
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