CN106423110A - Preparation of magnetic adsorbent efficiently removing polycyclic aromatic hydrocarbon with xanthoceras sorbifolia bunge shell being raw material - Google Patents

Preparation of magnetic adsorbent efficiently removing polycyclic aromatic hydrocarbon with xanthoceras sorbifolia bunge shell being raw material Download PDF

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CN106423110A
CN106423110A CN201610870497.1A CN201610870497A CN106423110A CN 106423110 A CN106423110 A CN 106423110A CN 201610870497 A CN201610870497 A CN 201610870497A CN 106423110 A CN106423110 A CN 106423110A
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aromatic hydrocarbon
polycyclic aromatic
shinyleaf yellowhorn
shell
salt
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CN106423110B (en
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纪俊敏
刘玉兰
汪学德
张振山
王动民
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Henan University of Technology
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    • B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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Abstract

The invention discloses a preparing method of a magnetic adsorbent efficiently removing polycyclic aromatic hydrocarbon with xanthoceras sorbifolia bunge shell being a raw material. The preparing method comprises the steps of conducting pretreatments such as impurity removing, pre-carbonization and alkali dissolution silica removing; matching Fe2+salt and Fe3+salt into a solution and mixing the Fe2+salt and the Fe3+salt in proportion; adding pretreated xanthocaras sorbifolia bunge shell ash alkaline precipitation according to a mass ratio of xanthoceras sorbifolia bunge shell ash to Fe ion, and obtaining xanthoceras sorbifolia bunge shell radical magnetic adsorbent after washing the xanthocaras sorbifolia bunge shell ash alkaline precipitation. According to the preparing method of the magnetic adsorbent efficiently removing the polycyclic aromatic hydrocarbon with the xanthoceras sorbifolia bunge shell being the raw material, preparation of an activated carbon material from the xanthoceras sorbifolia bunge shell is easy, waste utilization of the xanthoceras sorbifolia bunge shell is achieved. Xanthoceras sorbifolia bunge shell activated carbon prepared through modifying of magnetofluid has a large specific surface area and a small aperture and can simultaneously adsorb pigment, benzopyrene, polycyclic aromatic hydrocarbon and the like in fats, and the adsorption rate reaches to 99% or above.

Description

Prepare the magnetic adsorbent of efficient removal polycyclic aromatic hydrocarbon with shinyleaf yellowhorn shell for raw material
Technical field
The present invention relates to a kind of method of the magnetic adsorbent preparing efficient removal polycyclic aromatic hydrocarbon with shinyleaf yellowhorn shell for raw material, Its product has very strong adsorption effect to the pigment in edible oil, polycyclic aromatic hydrocarbon, the invention belongs to technical field of active carbon, specifically It is related to a kind of method that the magnetic adsorbent of polycyclic aromatic hydrocarbon in efficient removal edible oil is prepared for raw material with shinyleaf yellowhorn shell.
Background technology
Shiny-leaved yellowhorn is the distinctive rare woody oleiferous plants crop of China, has a root system of prosperity, strong adaptability, Salt And Alkali Tolerance, anti- Cold, the ground such as meadow, wasteland, mountain area, gully can normal growth, be not only the fine tree species of desertification of checking winds and fixing drifting sand, administer, Also serve as ornamental tree species extensively to plant in gardens, roadside greenbelt.In recent years, because shiny-leaved yellowhorn has higher industrial value And nutritive value, increasingly paid close attention to by people.China now plants shiny-leaved yellowhorn in a large number, and benevolence is used for extracting oil, with shiny-leaved yellowhorn Seed is raw material, can produce substantial amounts of kind of skin discarded object using milling process or solvent extraction when extracting shinyleaf yellowhorn oil.100 kg Shiny-leaved yellowhorn seed can output 40 ~ 50 kg kind skin discarded object, its shell is contained within substantial amounts of cellulose and hemicellulose.Generally literary composition Hat fruit shell is not utilized and be dropped, that is, cause waste and pollute environment.Research to shiny-leaved yellowhorn is main at present for China Around extraction and the preparation biodiesel of shinyleaf yellowhorn oil, and the rarely seen report of research of activated carbon prepared by discarded shinyleaf yellowhorn fruit shell Road.In order to adapt to the needs of shiny-leaved yellowhorn development, adequately and reasonably utilize resource, accessory substance-shiny-leaved yellowhorn that shinyleaf yellowhorn oil is produced Shell develops and utilizes, and may advantageously facilitate shiny-leaved yellowhorn scientific research, the development producing.
Polycyclic aromatic hydrocarbon（Polycyclic aromatic hydrocarbon, abbreviation PAHs）Refer to contain two in molecule Or two or more phenyl ring with wire, horn shape or tufted arrange hydrocarbon, benzo [a] pyrene is a kind of by 5 phenyl ring structures The polycyclic aromatic hydrocarbon becoming.Dong Guangbin, Li Peng etc.（Dong Guangbin, Li Peng. benzo [a] pyrene Analysis of test results, grain in edible vegetable oil Oil processing, 2009,7: 67-68）Determine benzo [a] pyrene in domestic and international edible vegetable oil and fat 262 parts of samples of 19 species Residual content, result shows：The recall rate of benzo [a] pyrene is 98.5%.Wherein, soybean oil recall rate is 96.0%, remaining Species is 100%.According to GB 2716-2005《Edible vegetable oil sanitary standard》Judge, the qualification rate of edible oil is 97.7%.Judge, the qualification rate of edible oil is 60.0% according to No. 208/2005 file regulation of European Union.With China's food row International the integrating with of Ye Yu, the food-safety problem being caused by polycyclic aromatic hydrocarbon, increasingly it is subject to concern and the attention of consumer.State Family has also put into effect relevant legal articles and sanitary index is monitored and constrains.Wang Jianhua（Wang Jianhua. different process peanuts The changes of contents of 16 kinds of polycyclic aromatic hydrocarbon _ PAHs_ in oil, food science and technology, 2013,38 (5): 183）To in different process In peanut oil, the content of 16 kinds of polycyclic aromatic hydrocarbons is studied, and adds all decline of content of polycyclic aromatic hydrocarbon after bleaching earth decolouring, But decline degree inconspicuous it was demonstrated that carclazyte is bad to the removal effect of polycyclic aromatic hydrocarbon.Labyrinth（Labyrinth, Xu Zhong. food hygiene with Security control. Chemical Industry Press, 2007.）Report rapeseed oil is processed with 0.3%～0.5% activated carbon, at 90 DEG C Lower stirring 30 min, then process 4 h through under 140 DEG C and 91.3 kPa vacuum, 89%～95% benzo [a] pyrene can be removed.
The activated carbon producing at present is broadly divided into wooden（Including shell）With ature of coal two class.The World Forests area is being in just to decline Trend, be available for fell utilization industrial woods resource also day by day reduce.Although coal resources in China comparison is enriched, coal production occupies No. 1 in the world, but for producing the low ash content of activated carbon, coal resources of weak type of bond few.In recent ten years, Widen the raw material sources of activated carbon, develop suitable preparation process condition, become the new study hotspot of scholars.Activated carbon Raw materials for production oneself be not limited only to timber and coal, the agricultural such as shell, fruit stone, bamboo, waste paper, tea leaf residual, rice husk, agricultural crop straw Discarded object etc., can be adopted to produce activated carbon.This kind of raw material sources are extensively, with low cost, using suitable process conditions, also can Obtain and there is higher degree and the activated carbon product of micropore structure.
Magnetic adsorptive material a, it has also become study hotspot of various fields.Can be in fast enriching under external magnetic field And directed movement, at present, the main research application of magnetic material has：Heavy metal ion (Hg2+、Pb2+) and organic contamination The sewage treatment area of thing etc., biomedical sector and the hydrogenation catalyst such as protein, DNA separation, target medicine carrier, receives The catalytic fields such as rice precious metal catalyst, photocatalysis, are not yet related to its research to pigment in grease and polycyclic aromatic hydrocarbon removing.
It is an object of the invention to provide a kind of efficient shinyleaf yellowhorn shell acticarbon removing polycyclic aromatic hydrocarbon, gained Activated carbon specific surface area is big, and aperture is little, can the harmful substance such as adsorpting pigment, polycyclic aromatic hydrocarbon and BaP simultaneously, and provide its system Preparation Method, with low cost, preparation technology is easy, good adsorption performance.Grease if aperture is too big, in easy adsorbing edible oil Molecule and nutriment（As sterol, oryzanol etc.）, the nutritive value of impact edible oil.
Content of the invention
It is an object of the invention to provide a kind of efficient shinyleaf yellowhorn shell acticarbon removing polycyclic aromatic hydrocarbon, gained Activated carbon specific surface area is big, and aperture is little, can the harmful substance such as adsorpting pigment, polycyclic aromatic hydrocarbon and BaP simultaneously, and provide its system Preparation Method, with low cost, preparation technology is easy, good adsorption performance.Grease if aperture is too big, in easy adsorbing edible oil Molecule and nutriment（As sterol, oryzanol etc.）, the nutritive value of impact edible oil.
The technical solution used in the present invention is as follows：
A kind of method preparing efficient mycotoxin absorbant for raw material with shinyleaf yellowhorn shell, is characterized in that：Include following step successively Suddenly：
（1）Removal of impurities：Take shinyleaf yellowhorn shell to cross 100 mesh sieves after pulverizing, washed with distilled water under stirring（20～ 40min）, being neutrality to washing lotion, the shinyleaf yellowhorn shell after cleaning is placed in baking oven（105 ℃）Dry for standby.
（2）Pre- charing：The shinyleaf yellowhorn shell taking clean post-drying is put in crucible, in Muffle furnace（250～350 DEG C）In advance Charing 1～2 h；Pre- charing is in order that shinyleaf yellowhorn shell tentatively cracks, and allows partial organic substances form microcosmic in volatilization process Pore structure.When pre- carbonization temperature is too high, organic matter is possible to generate complicated thermal decomposition product blocking duct, or leads to carbon containing Material and silica are combined into the compound of indissoluble；Temperature is too low, and organic matter volatilization is not fully it is difficult to improve the ratio of product The index such as surface area and porosity.
（3）Alkali soluble removes silicon：Take the shinyleaf yellowhorn shell of pre- charing, add 0.5%～5% KOH or NaOH alkali lye（Alkali charcoal ratio is 4：1）, boil, stir 4h, after being neutrality with 80 DEG C of hot water suction filtration to washing lotion, dry for standby.Alkali soluble is to remove literary composition except silicon In hat shell, unnecessary element silicon, because excessive element silicon can make the ash content of product increase, reduces the adsorption capacity of product.Separately Outer dipping by lye can significantly improve specific surface area and the total pore volume of product.The concentration of alkali lye and soak time unsuitable too high and Long, otherwise can lead to the corrosion of equipment and the increase of cost.
（4）Magnetic is modified：By Fe3+And Fe2+Soluble-salt wiring solution-forming, is 1.5 according to mol ratio:1～2.5:1 ratio Mixing, then by step（3）Prepared shinyleaf yellowhorn shell ash adds in ferrous solution, and mechanical agitation 2 h then drips certain mass 25% glutaraldehyde solution, by above-mentioned mixed liquor, under nitrogen protection after adsorption saturation, heats up；Adjust pH value 7 with aqueous slkali ～9, it is settled out Magnaglo activated carbon, ageing, standing.The molysite and ferrous salt chemical equation under-OH effect is as follows： Fe2++2Fe3++8OH-→ Fe3O4↓ +4H2O.
（5）Activation burning：By step（4）The magnetic modification shinyleaf yellowhorn shell ash distillation water washing obtaining 3～4 times, until pH =6.8～7.2, again suction filtration, in 700 DEG C～800 DEG C Muffle furnaces calcine 4～6 h, that is, obtain magnetic carbon-supported catalyst.High Temperature sintering can make the organic matter of residual fully volatilize, and improves porosity and the total pore volume of product further.
The present invention, with respect to prior art, has the advantage that：
The present invention, with abundance, cheap, reproducible shinyleaf yellowhorn shell as raw material, meets the sustainable development of China's formulation With the strategic requirement extending agricultural industry chain.The shinyleaf yellowhorn shell activated carbon pore size that the present invention is obtained is little（1.5～50 nm）, compare table Area is big（650～1000m2/g）, methylene blue value ＞ 12mL/g, can effectively remove polycyclic aromatic hydrocarbon in grease, to many in grease The removal efficiency of PAH reaches 85%～95%.Separation of solid and liquid is can be achieved with the presence of externally-applied magnetic field after absorbing multiring aromatic hydrocarbon, Process through desorption after separating, adsorbent can reuse again, cost-effective.
Brief description
【Fig. 1】Process chart schematic diagram for the present invention.
Specific embodiment
Embodiment 1：
（1）Weigh after shinyleaf yellowhorn shell 800 g pulverizes and cross 100 mesh sieves, carried out with distilled water under stirring washing 40min, To washing lotion be neutrality, will clean after shinyleaf yellowhorn shell in 105 DEG C of baking ovens dry for standby.
（2）The shinyleaf yellowhorn shell taking clean post-drying is put in crucible, in Muffle furnace（250 ℃）Pre- charing 1 h；
（3）Take the shinyleaf yellowhorn shell of pre- charing, add 0.5% NaOH（Alkali charcoal is than for 4:1）, boil, stir 4 h, with 80 DEG C of hot water After suction filtration is neutrality to washing lotion, standby after drying in an oven；
（4）4.05gFeCl is added in flask3·6H2O and 2.78gFeSO4·7H2O, plus 100mL distillation water dissolves, add step Suddenly（3）Prepared shinyleaf yellowhorn shell ash 6.83g, then dropping 2mol/LNaOH alkali lye make system pH=7, be heated to 80 DEG C, anti- Answer 4 h；After reaction terminates, precipitate filtration separation, for several times, precipitation drying, charing are after 750 DEG C of Muffle furnaces for distillation water washing Middle calcining 6 h, product is shinyleaf yellowhorn shell base magnetic active carbon adsorbent.After testing, the specific surface area of adsorbent is 746.5 m2/g.
Weigh 50 g peanut oil（Polycyclic aromatic hydrocarbon total content 763.94 μ g/kg, wherein benzo [a] pyrene content 24.01 μ g/ kg）It is placed in there-necked flask, adds the above-mentioned shinyleaf yellowhorn shell base magnetic active carbon adsorbent preparing of 0.075 g, in absorption temperature Carry out heating stirring at 100 DEG C of degree, during stirring, maximum (top) speed must not cause grease to splash, after absorption 25 min, filter to isolate Adsorbent, that is, obtain adsorbing absolute oil.Benzo [a] pyrene content in gained absolute oil is measured, and calculates removal efficiency.Spend after measured In oil generation, polycyclic aromatic hydrocarbon residual quantity is 245.35 μ g/kg, and wherein benzo [a] pyrene residual quantity is 2.40 μ g/kg, benzo in grease The removal efficiency of [a] pyrene is up to 93%.And because its addition is little, the impact to grease fragrance is inconspicuous.
Embodiment 2：
（1）Weigh after shinyleaf yellowhorn shell 600 g pulverizes and cross 100 mesh sieves, carried out with distilled water under stirring washing 30min, Being neutrality to washing lotion, the shinyleaf yellowhorn shell after cleaning is placed in baking oven（105 ℃）Dry for standby.
（2）The shinyleaf yellowhorn shell taking clean post-drying is put in crucible, in Muffle furnace（250 ℃）Pre- charing 1h；
（3）Take the shinyleaf yellowhorn shell of pre- charing, add 0.5% KOH（Alkali charcoal is than for 4:1）, boil, stir 4 h, taken out with 80 DEG C of hot water Filter after being neutrality to washing lotion, standby after drying in an oven
（4）8.08g Fe (NO is added in flask3)3·9H2O and 1.98gFeCl2·4H2O, plus 100mL distillation water dissolves, Add step（3）Prepared shinyleaf yellowhorn shell ash 10.06g, then drips 2mol/LKOH alkali lye and makes system pH=7, be heated to 80 DEG C, reaction 4 h；After reaction terminates, precipitate filtration separation, for several times, precipitation drying, charing are after 800 DEG C of horses for distillation water washing Not calcine 4h in stove, product is shinyleaf yellowhorn shell base magnetic active carbon adsorbent.
Weigh 50 g peanut oil（Polycyclic aromatic hydrocarbon total content 763.94 μ g/kg, wherein benzo [a] pyrene content 24.01 μ g/ kg）It is placed in there-necked flask, add the above-mentioned shinyleaf yellowhorn shell base magnetic active carbon adsorbent preparing of 0.1 g, in adsorption temp Carry out heating stirring at 100 DEG C, during stirring, maximum (top) speed must not cause grease to splash, after absorption 25 min, filter to isolate suction Attached dose, that is, obtain adsorbing absolute oil.Polycyclic aromatic hydrocarbon content in gained absolute oil is measured, and calculates removal efficiency.Peanut after measured In oil, polycyclic aromatic hydrocarbon residual quantity is 131.21 μ g/kg, and wherein benzo [a] pyrene residual quantity is 0.23 μ g/kg.Many cyclophanes in grease The removal efficiency of hydrocarbon is 83%, and benzo [a] pyrene removal efficiency is up to 99%.And because its addition is little, the impact to grease fragrance is failed to understand Aobvious.

Claims (7)

1. a kind of method of the magnetic adsorbent being prepared efficient removal polycyclic aromatic hydrocarbon with shinyleaf yellowhorn shell for raw material, be is characterized in that：According to Secondary comprise the following steps：
（1）Removal of impurities：Shinyleaf yellowhorn shell is taken to cross 100 mesh sieves after pulverizing, it is neutral for being carried out with distilled water being washed to washing lotion, then will wash Shinyleaf yellowhorn shell after net is placed in baking oven（105 ℃）Dry for standby；
（2）Pre- charing：The shinyleaf yellowhorn shell taking clean post-drying is put in crucible, carbonizes in advance in Muffle furnace；
（3）Alkali soluble removes silicon：Take the shinyleaf yellowhorn shell of pre- charing, add the alkali lye of 0.5 %～5 %, boil, stir 4h, with 80 DEG C After hot water suction filtration is neutrality to washing lotion, dry for standby；
（4）Magnetic is modified：By Fe3+And Fe2+Soluble-salt wiring solution-forming, is 1.5 according to mol ratio:1～2.5:1 ratio is mixed Close, then by step（3）Prepared shinyleaf yellowhorn shell ash adds in ferrous solution, and mechanical agitation 2h then drips the 25% of certain mass Glutaraldehyde solution, by above-mentioned mixed liquor, under nitrogen protection after adsorption saturation, heats up；Adjust pH=7～9 with aqueous slkali, sink Form sediment Magnaglo activated carbon, ageing, standing；
（5）Activation burning：By step（4）The magnetic modification shinyleaf yellowhorn shell ash distillation water washing obtaining 3～4 times, until pH=6.8 ～7.2, again suction filtration, calcine 6 h in 700 DEG C～800 DEG C Muffle furnaces, that is, obtain magnetic carbon-supported catalyst.
2. the side of the magnetic adsorbent preparing efficient removal polycyclic aromatic hydrocarbon with shinyleaf yellowhorn shell for raw material according to claim 1 Method, is characterized in that：Step（2）In the carbonization temperature of pre- charing be 250～350 DEG C, carbonization time 1～2 h.
3. the side of the magnetic adsorbent preparing efficient removal polycyclic aromatic hydrocarbon with shinyleaf yellowhorn shell for raw material according to claim 1 Method, is characterized in that：Step（3）It is 0.5%～5% KOH or 0.5%～5% NaOH that alkali soluble removes the alkali lye adding in silicon, alkali carbonaceous Amount ratio is 4: 1.
4. the magnetic adsorbent preparing efficient removal polycyclic aromatic hydrocarbon with shinyleaf yellowhorn shell for raw material according to claim 1 Method, is characterized in that：Step（4）Fe used by magnetic modification3+Soluble-salt be FeCl3·6H2O、Fe2(SO4)3·9H2O or Fe(NO3)3·9H2One kind of O；Fe2+Soluble-salt be FeCl2·4H2O、FeSO4·7H2O or Fe (NO3)2·9H2In O One kind.
5. the magnetic adsorbent preparing efficient removal polycyclic aromatic hydrocarbon with shinyleaf yellowhorn shell for raw material according to claim 1 Method, is characterized in that：Step（4）The modified described Fe of magnetic3+Salt and Fe2+Reactant salt generates Fe3O4During, described mixing The temperature of thing solution is 40～60 DEG C, Fe3+Salt and Fe2+The mol ratio of salt is 1.5:1～2.5:1.
6. the magnetic adsorbent preparing efficient removal polycyclic aromatic hydrocarbon with shinyleaf yellowhorn shell for raw material according to claim 1 Method, is characterized in that：Step（4）Described shinyleaf yellowhorn shell ash and Fe3+Salt and Fe2+The gross weight of salt is than for 0.6:1～3.8:1.
7. the magnetic adsorbent preparing efficient removal polycyclic aromatic hydrocarbon with shinyleaf yellowhorn shell for raw material according to claim 1 Method, is characterized in that：Step（4）Described adsorption time under nitrogen protection is 3～5 h；It is warming up to 60～80 DEG C；Control System and the pH aqueous slkali adjusting mixed solution are ammoniacal liquor, one of NaOH or KOH solution；Adjust pH to 7～9； The concentration of aqueous slkali is 2～4 mol/L；Digestion time is 2～4 h, and time of repose is 12～16 h.
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