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CN106423110B - The magnetic adsorbent of efficient removal polycyclic aromatic hydrocarbon is prepared using shinyleaf yellowhorn shell as raw material - Google Patents

The magnetic adsorbent of efficient removal polycyclic aromatic hydrocarbon is prepared using shinyleaf yellowhorn shell as raw material Download PDF

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CN106423110B
CN106423110B CN201610870497.1A CN201610870497A CN106423110B CN 106423110 B CN106423110 B CN 106423110B CN 201610870497 A CN201610870497 A CN 201610870497A CN 106423110 B CN106423110 B CN 106423110B
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wenguan
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polycyclic aromatic
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CN106423110A (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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    • B01J20/28078—Pore diameter
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    • B01J20/28078—Pore diameter
    • B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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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

本发明公开了一种以文冠果壳为原料制备高效脱除多环芳烃的磁性吸附剂的方法，文冠果壳先经过除杂、预炭化、碱溶除硅等预处理；然后将Fe2+盐和Fe3+盐配成溶液，按比例混合；按文冠果壳灰质量与Fe离子质量比例，加入预处理后的文冠果壳灰碱沉、水洗后得到文冠果壳基磁性吸附剂。本发明从文冠果壳中制备活性炭原料易得，实现了文冠果壳的废物利用，通过磁流体改性制备得到的文冠果壳活性炭比表面积大、孔径小，可同时吸附油脂中的色素、苯并芘、多环芳烃等物质，吸附率高达99%。The invention discloses a method for preparing a magnetic adsorbent for efficiently removing polycyclic aromatic hydrocarbons by using Wenguan nut shell as a raw material. The salt and Fe3+ salt are made into a solution and mixed according to the proportion; according to the mass ratio of the ash of the nut shell and the mass of Fe ions, the ash of the nut shell after pretreatment is added for alkali precipitation and washed with water to obtain the nut shell-based magnetic adsorbent. The invention prepares activated carbon raw materials from Wenguan fruit shell, which is easy to obtain, realizes the waste utilization of Wenguan fruit shell, and the activated carbon of Wenguan fruit shell prepared by magnetic fluid modification has a large specific surface area and a small pore size, and can simultaneously adsorb the charcoal in the oil. Pigments, benzopyrene, polycyclic aromatic hydrocarbons and other substances, the adsorption rate is as high as 99%.

Description

The magnetic adsorbent of efficient removal polycyclic aromatic hydrocarbon is prepared using shinyleaf yellowhorn shell as raw material
Technical field
The present invention relates to a kind of using shinyleaf yellowhorn shell as the method for the magnetic adsorbent of raw material preparation efficient removal polycyclic aromatic hydrocarbon, Its product has very strong adsorption effect to pigment, the polycyclic aromatic hydrocarbon in edible oil, and 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 as raw material using shinyleaf yellowhorn shell.
Background technique
Shiny-leaved yellowhorn is the distinctive rare woody oleiferous plants crop in China, has flourishing root system, adaptable, and saline-alkali tolerant resists It is cold, the ground such as meadow, wasteland, mountain area, gully can normal growth, the fine tree species for the desertification that is not only to check winds and fix drifting sand, administer, Also it is planted extensively in gardens, roadside greenbelt as ornamental tree species.In recent years, due to shiny-leaved yellowhorn industrial value with higher And nutritive value, it has been to be concerned by more and more people.The existing a large amount of plantation shiny-leaved yellowhorns in China, kernel is chiefly used in extracting oil, with shiny-leaved yellowhorn Seed is raw material, can generate a large amount of kind of skin waste when extracting shinyleaf yellowhorn oil using squeezing method or solvent extraction.100 kg Shiny-leaved yellowhorn seed can 40 ~ 50 kg kind skin waste of output, a large amount of cellulose and hemicellulose are contained in shell.Usually text Hat fruit shell is unutilized and is dropped, that is, causes waste and pollution environment.China is main to the research of shiny-leaved yellowhorn at present Around the extraction and preparation biodiesel of shinyleaf yellowhorn oil, and discarded shinyleaf yellowhorn fruit shell is prepared to the rarely seen report of research of active carbon Road.In order to adapt to the needs of shiny-leaved yellowhorn development, resource is adequately and reasonably utilized, to by-product-shiny-leaved yellowhorn of shinyleaf yellowhorn oil production Shell develops and utilizes, and may advantageously facilitate the development of shiny-leaved yellowhorn scientific research, production.
There are two polycyclic aromatic hydrocarbon (Polycyclic aromatic hydrocarbon, abbreviation PAHs) refers to and contains in molecule Or more than two phenyl ring, with linear, horn shape or the hydrocarbon of tufted arrangement, benzo [a] pyrene is one kind by 5 phenyl ring structures At polycyclic aromatic hydrocarbon.Dong Guangbin, Li Peng equal (Dong Guangbin, benzo [a] pyrene Analysis of test results in Li Peng's edible vegetable oil, grain Oil processing, 2009,7:67-68) determine benzo [a] pyrene in 262 parts of the type sample of domestic and international edible vegetable oil and fat 19 Residual content, the results showed that the recall rate of benzo [a] pyrene be 98.5%.Wherein, soybean oil recall rate is 96.0%, remaining Type is 100%.Determine according to GB 2716-2005 " edible vegetable oil sanitary standard ", the qualification rate of edible oil is 97.7%.Determine that the qualification rate of edible oil is 60.0% according to No. 208/2005 file regulation of European Union.With China's food row Ye Yu is international to integrate with, the food-safety problem as caused by polycyclic aromatic hydrocarbon, increasingly by the concern of consumer and attention.State Family has also put into effect relevant legal articles and sanitary index is monitored and constrains.Wang Jianhua (Wang Jianhua difference process peanut 16 kinds of polycyclic aromatic hydrocarbon _ PAHs_ changes of contents in oil, food science and technology, 2013,38 (5): 183) in different process The content of 16 kinds of polycyclic aromatic hydrocarbons is studied in peanut oil, and all declines of content of polycyclic aromatic hydrocarbon after bleaching earth decoloration are added, But it is unobvious to decline degree, 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 that rapeseed oil is handled with 0.3%~0.5% active carbon, at 90 DEG C 30 min of lower stirring, then 4 h are handled under 140 DEG C and 91.3 kPa vacuum, 89%~95% benzo [a] pyrene can be removed.
The active carbon produced at present is broadly divided into wooden (including shell) and two class of coal quality.The World Forests area is just being in decline Trend, also increasingly reduced for felling the industrial woods resource that utilizes.Although coal resources in China comparison is abundant, coal production is occupied No. 1 in the world, but coal resources of low ash point, weak type of bond for producing active carbon and few.In recent ten years, It widens the raw material sources of active carbon, the preparation process condition that exploitation is suitable for, becomes the new research hotspot of scholars.Active 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 Waste etc. can be adopted to production active carbon.This kind of raw material sources are extensive, low in cost, using process conditions appropriate, also can Obtain the activated carbon product with higher degree and micropore structure.
Magnetic adsorptive material a, it has also become research hotspot of various fields.It can be in fast enriching under external magnetic field And directed movement, currently, the main research application field of magnetic material has: heavy metal ion (Hg2+、Pb2+) and organic contamination The sewage treatment field of object etc., fields of biomedicine and the hydrogenation catalysts such as protein, DNA separation, target medicine carrier are received The catalytic fields such as rice precious metal catalyst, photocatalysis, there has been no about its research to pigment in grease and polycyclic aromatic hydrocarbon removing.
It is resulting the purpose of the present invention is to provide a kind of shinyleaf yellowhorn shell acticarbon of efficiently removal polycyclic aromatic hydrocarbon Active carbon large specific surface area, aperture is small, can harmful substances such as adsorpting pigment, polycyclic aromatic hydrocarbon and BaP simultaneously, and provide its system Preparation Method, low in cost, preparation process is easy, good adsorption performance.Grease if aperture is too big, in easy adsorbing edible oil Molecule and nutriment (such as sterol, oryzanol), influence the nutritive value of edible oil.
Summary of the invention
It is resulting the purpose of the present invention is to provide a kind of shinyleaf yellowhorn shell acticarbon of efficiently removal polycyclic aromatic hydrocarbon Active carbon large specific surface area, aperture is small, can harmful substances such as adsorpting pigment, polycyclic aromatic hydrocarbon and BaP simultaneously, and provide its system Preparation Method, low in cost, preparation process is easy, good adsorption performance.Grease if aperture is too big, in easy adsorbing edible oil Molecule and nutriment (such as sterol, oryzanol), influence the nutritive value of edible oil.
The technical solution adopted by the invention is as follows:
A method of efficient mycotoxin absorbant being prepared by raw material of shinyleaf yellowhorn shell, it is characterized in that: under successively including Column step:
(1) it cleans: shinyleaf yellowhorn shell being taken to smash it through 100 meshes, washed under stirring with distilled water (20~ 40min), until washing lotion is neutral, the shinyleaf yellowhorn shell after cleaning is placed in baking oven (105 DEG C) and is dried for standby.
(2) pre- charing: the shinyleaf yellowhorn shell dried after cleaning is taken to be put into crucible, (250~350 DEG C) are pre- in Muffle furnace Carbonize 1~2 h；Pre- charing is to allow partial organic substances to be formed in volatilization process microcosmic to crack shinyleaf yellowhorn shell tentatively Pore structure.When pre- carbonization temperature is too high, organic matter is possible to generate complicated thermal decomposition product blocking duct, or causes carbon containing Substance and silica are combined into the compound of indissoluble；Temperature is too low, and organic matter volatilization is not enough, it is difficult to improve the ratio of product The indexs such as surface area and porosity.
(3) alkali soluble removes silicon: taking the shinyleaf yellowhorn shell of pre- charing, 0.5%~5% KOH or NaOH lye is added, and (alkali charcoal ratio is 4:1), it boils, stir 4h, filtered after being neutrality to washing lotion, be dried for standby with 80 DEG C of hot water.Alkali soluble is to remove text except silicon Extra element silicon reduces the adsorption capacity of product because excessive element silicon can be such that the ash content of product increases in hat shell.Separately Outer dipping by lye can significantly improve the specific surface area and total pore volume of product.The concentration and soaking time of lye it is unsuitable excessively high and It is too long, it otherwise will 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: 1~2.5:1 ratio according to molar ratio Then mixing shinyleaf yellowhorn shell ash made from step (3) is added in ferrous solution, 2 h of mechanical stirring, certain mass is then added dropwise 25% glutaraldehyde solution under nitrogen protection after adsorption saturation, heats up by into above-mentioned mixed liquor；PH value 7 is adjusted with aqueous slkali ~9, it is settled out Magnaglo active carbon, ageing is stood.The chemical equation of molysite and ferrous salt under-OH effect is as follows: Fe2++2Fe3++8OH-→ Fe3O4↓ +4H2O。
(5) activation burning: the modified shinyleaf yellowhorn shell ash of magnetic that step (4) obtains is washed with distilled water 3~4 times, until pH =6.8~7.2, it filters again, calcine 4~6 h in 700 DEG C~800 DEG C Muffle furnaces to get magnetic carbon-supported catalyst is arrived.It is high Temperature sintering can make remaining organic matter sufficiently volatilize, and further increase the porosity and total pore volume of product.
The present invention compared with the existing technology, has the advantage that
The present invention meets the sustainable of China's formulation using abundance, cheap, reproducible shinyleaf yellowhorn shell as raw material Development and the strategic requirement for extending agricultural industry chain.Shinyleaf yellowhorn shell activated carbon pore size produced by the present invention small (1.5~50 nm), Large specific surface area (650~1000m2/ g), methylene blue value > 12mL/g can effectively remove polycyclic aromatic hydrocarbon in grease, to grease The removal efficiency of middle polycyclic aromatic hydrocarbon is up to 85%~95%.It can be achieved with solid-liquid point after absorbing multiring aromatic hydrocarbon under the action of externally-applied magnetic field From being handled after separation by desorption, adsorbent can reuse, save the cost again.
Detailed description of the invention
[Fig. 1] is process flow chart schematic diagram of the invention.
Specific embodiment
Embodiment 1:
(1) it weighs 800 g of shinyleaf yellowhorn shell and smashes it through 100 meshes, washed under stirring with distilled water Shinyleaf yellowhorn shell after cleaning is dried for standby by 40min until washing lotion is neutral in 105 DEG C of baking ovens.
(2) shinyleaf yellowhorn shell dried after cleaning is taken to be put into crucible, (250 DEG C) carbonize 1 h in advance in Muffle furnace；
(3) shinyleaf yellowhorn shell of pre- charing is taken, 0.5% NaOH(alkali charcoal ratio of addition is 4:1), it boils, stir 4 h, with 80 DEG C Hot water is filtered be neutral to washing lotion after, it is spare after drying in an oven；
(4) 4.05gFeCl is added into flask3·6H2O and 2.78gFeSO4·7H2O adds 100mL distilled water to dissolve, adds Enter shinyleaf yellowhorn shell ash 6.83g made from step (3), 2mol/LNaOH lye is then added dropwise and makes system pH=7, is heated to 80 DEG C, reaction 4 h；After reaction, precipitating is separated by filtration, and for several times, precipitating is after drying, charing in 750 DEG C of horses for distillation water washing 6 h are not calcined in furnace, product is shinyleaf yellowhorn shell base magnetic active carbon adsorbent.Through detecting, the specific surface area of adsorbent is 746.5 m2/g。
Weigh 50 g peanut oil (763.94 μ g/kg of polycyclic aromatic hydrocarbon total content, wherein 24.01 μ g/ of benzo [a] pyrene content Kg it) is placed in three-necked flask, the above-mentioned shinyleaf yellowhorn shell base magnetic active carbon adsorbent prepared of 0.075 g is added, in absorption temperature Heating stirring is carried out at 100 DEG C of degree, and maximum (top) speed must not cause grease to splash when stirring, after adsorbing 25 min, filter to isolate Adsorbent to get to absorption absolute oil.Benzo [a] pyrene content in gained absolute oil is measured, and calculates removal efficiency.It spends after measured Polycyclic aromatic hydrocarbon residual quantity is 245.35 μ g/kg in oil generation, 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 additive amount is small, the influence to grease fragrance is unobvious.
Embodiment 2:
(1) it weighs 600 g of shinyleaf yellowhorn shell and smashes it through 100 meshes, washed under stirring with distilled water Shinyleaf yellowhorn shell after cleaning is placed in baking oven (105 DEG C) and is dried for standby by 30min until washing lotion is neutral.
(2) shinyleaf yellowhorn shell dried after cleaning is taken to be put into crucible, (250 DEG C) carbonize 1h in advance in Muffle furnace；
(3) shinyleaf yellowhorn shell of pre- charing is taken, 0.5% KOH(alkali charcoal ratio of addition is 4:1), it boils, stir 4 h, with 80 DEG C of heat Water is filtered be neutral to washing lotion after, it is spare after drying in an oven
(4) 8.08g Fe (NO is added into flask3)3 ·9H2O and 1.98gFeCl2·4H2O adds 100mL distillation water-soluble Shinyleaf yellowhorn shell ash 10.06g made from step (3) is added in solution, and 2mol/LKOH lye is then added dropwise and makes system pH=7, heats To 80 DEG C, 4 h of reaction；After reaction, precipitating is separated by filtration, and for several times, precipitating is after drying, charing in 800 for distillation water washing 4h is calcined in DEG C Muffle furnace, product is shinyleaf yellowhorn shell base magnetic active carbon adsorbent.
Weigh 50 g peanut oil (763.94 μ g/kg of polycyclic aromatic hydrocarbon total content, wherein 24.01 μ g/ of benzo [a] pyrene content Kg it) is placed in three-necked flask, the above-mentioned shinyleaf yellowhorn shell base magnetic active carbon adsorbent prepared of 0.1 g is added, in adsorption temp Carry out heating stirring at 100 DEG C, maximum (top) speed must not cause grease to splash when stirring, after adsorbing 25 min, filter to isolate suction Attached dose to get to absorption absolute oil.Polycyclic aromatic hydrocarbon content in gained absolute oil is measured, and calculates removal efficiency.Peanut after measured Polycyclic aromatic hydrocarbon residual quantity is 131.21 μ g/kg in oil, and wherein benzo [a] pyrene residual quantity is 0.23 μ g/kg.Polycyclic virtue in grease The removal efficiency of hydrocarbon is 83%, and benzo [a] pyrene removal efficiency is up to 99%.And because its additive amount is small, the influence to grease fragrance is unknown It is aobvious.

Claims (2)

1.一种高效去除花生油中多环芳烃的方法，其特征在于：称取50g花生油置于三口烧瓶中，加入0.1g文冠果壳基磁性活性炭吸附剂，在吸附温度100℃下进行加热搅拌，搅拌时最大转速不得引起油脂飞溅，吸附25min后，过滤分离出吸附剂，即得到吸附净油；所述文冠果壳基磁性活性炭吸附剂的制备方法如下：1. a method for efficiently removing polycyclic aromatic hydrocarbons in peanut oil, is characterized in that: take by weighing 50g peanut oil and place in there-necked flask, add 0.1g Wenguan nutshell-based magnetic activated carbon adsorbent, carry out heating and stirring at 100 ℃ of adsorption temperature , the maximum rotational speed during stirring shall not cause the splash of grease, after 25min of adsorption, the adsorbent is filtered and separated to obtain the adsorbed net oil; the preparation method of the described Wenguan nut shell-based magnetic activated carbon adsorbent is as follows: （1）称取文冠果壳600g粉碎后过100目筛，在搅拌作用下用蒸馏水进行水洗30min，至洗液为中性为止，将洗净后的文冠果壳置于烘箱中，105℃烘干备用；(1) Weigh 600g of Wenguan nut shells and crush them and pass through a 100-mesh sieve, wash with distilled water for 30 minutes under stirring, until the washing liquid is neutral, place the washed Wenguan nut shells in an oven for 105 ℃ drying for use; （2）取洗净后烘干的文冠果壳放入坩埚中，在马弗炉中250℃预炭化1h；(2) Put the washed and dried Wenguan nut shell into a crucible, and pre-carbonize it in a muffle furnace at 250°C for 1 hour; （3）取预炭化的文冠果壳，加入0.5% 的KOH，碱炭质量比为4:1，煮沸、搅拌4h，用80℃热水抽滤至洗液为中性后，在烘箱中烘干后备用；(3) Take the pre-carbonized Wenguan nut shell, add 0.5% KOH, the mass ratio of alkali to carbon is 4:1, boil, stir for 4 hours, filter with 80 ℃ hot water until the washing liquid is neutral, put it in an oven Reserve after drying; （4）向烧瓶中加入8.08g Fe(NO3)3·9H2O和1.98g FeCl2·4H2O，加100mL蒸馏水溶解，加入步骤（3）制得的文冠果壳灰10.06g，然后滴加2mol/L KOH碱液使得体系pH=7，加热至80℃、反应4 h；反应结束后，沉淀过滤分离，蒸馏水洗涤数次，沉淀经干燥、炭化后于800℃马弗炉中煅烧4h，产品即为文冠果壳基磁性活性炭吸附剂。(4) Add 8.08g Fe(NO 3 ) 3 ·9H 2 O and 1.98g FeCl 2 ·4H 2 O to the flask, add 100mL of distilled water to dissolve, add 10.06g of Wenguan fruit shell ash obtained in step (3), Then, 2mol/L KOH alkali solution was added dropwise to make the pH of the system=7, heated to 80°C, and reacted for 4 h; after the reaction, the precipitate was separated by filtration, washed with distilled water for several times, and the precipitate was dried and carbonized in a muffle furnace at 800°C. After calcination for 4h, the product is Wenguan nut shell-based magnetic activated carbon adsorbent. 2.一种高效去除花生油中多环芳烃的方法，其特征在于：称取50g花生油置于三口烧瓶中，加入0.075g文冠果壳基磁性活性炭吸附剂，在吸附温度100℃下进行加热搅拌，搅拌时最大转速不得引起油脂飞溅，吸附25min后，过滤分离出吸附剂，即得到吸附净油；所述文冠果壳基磁性活性炭吸附剂的制备方法如下：2. a method for efficiently removing polycyclic aromatic hydrocarbons in peanut oil, it is characterized in that: take 50g peanut oil and place in three-necked flask, add 0.075g Wenguan nutshell-based magnetic activated carbon adsorbent, and carry out heating and stirring at 100 ℃ of adsorption temperature , the maximum rotational speed during stirring shall not cause the splash of grease, after 25min of adsorption, the adsorbent is filtered and separated to obtain the adsorbed net oil; the preparation method of the described Wenguan nut shell-based magnetic activated carbon adsorbent is as follows: （1）称取文冠果壳800g粉碎后过100目筛，在搅拌作用下用蒸馏水进行水洗40min，至洗液为中性为止，将洗净后的文冠果壳于105℃烘箱中烘干备用；(1) Weigh 800 g of Wenguan nut shells and crush them and pass through a 100-mesh sieve. Wash with distilled water for 40 minutes under stirring until the washing liquid is neutral. Dry the washed Wenguan nut shells in an oven at 105 °C. dry spare; （2）取洗净后烘干的文冠果壳放入坩埚中，在马弗炉中250℃预炭化1 h；(2) Put the washed and dried Wenguan nut shell into a crucible, and pre-carbonize it in a muffle furnace at 250 °C for 1 h; （3）取预炭化的文冠果壳，加入0.5% 的NaOH，碱炭质量比为4:1，煮沸、搅拌4h，用80℃热水抽滤至洗液为中性后，在烘箱中烘干后备用；(3) Take the pre-carbonized Wenguan nut shell, add 0.5% NaOH, the mass ratio of alkali to carbon is 4:1, boil, stir for 4 hours, filter with 80 ℃ hot water until the washing liquid is neutral, put it in an oven Reserve after drying; （4）向烧瓶中加入4.05gFeCl3·6H2O和2.78g FeSO4·7H2O，加100mL蒸馏水溶解，加入步骤（3）制得的文冠果壳灰6.83g，然后滴加2mol/L NaOH碱液使得体系pH=7，加热至80 ℃、反应4 h；反应结束后，沉淀过滤分离，蒸馏水洗涤数次，沉淀经干燥、炭化后于750℃马弗炉中煅烧6h，产品即为文冠果壳基磁性活性炭吸附剂。(4) Add 4.05g FeCl 3 ·6H 2 O and 2.78g FeSO 4 ·7H 2 O to the flask, add 100mL of distilled water to dissolve, add 6.83g of Wenguan fruit shell ash obtained in step (3), and then dropwise add 2mol/ L NaOH alkali solution to make the pH of the system = 7, heated to 80 °C, and reacted for 4 h; after the reaction, the precipitate was filtered and separated, washed with distilled water for several times, the precipitate was dried and carbonized, and then calcined in a 750 °C muffle furnace for 6 h, the product was It is a magnetic activated carbon adsorbent based on Wenguan nut shell.
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