CN107163964A - A kind of multi-production process of pomelo peel regeneration product, shaddock peel adsorbent, and, shaddock peel essential oil - Google Patents
A kind of multi-production process of pomelo peel regeneration product, shaddock peel adsorbent, and, shaddock peel essential oil Download PDFInfo
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- CN107163964A CN107163964A CN201710483985.1A CN201710483985A CN107163964A CN 107163964 A CN107163964 A CN 107163964A CN 201710483985 A CN201710483985 A CN 201710483985A CN 107163964 A CN107163964 A CN 107163964A
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a kind of multi-production process of pomelo peel regeneration product, shaddock peel adsorbent, and, shaddock peel essential oil, the preparation technology shown in the embodiment of the present application, pomelo peel powder is modified using organic activator, shaddock peel adsorbent prepared by the embodiment of the present application, its even particle size distribution, and pore structure are abundant, big central hole structure accounts for more than 60%, good to the absorption property of dyestuff in sewage and heavy metal.Simultaneously, the embodiment of the present application is modified pomelo peel powder using organic activator, oilpaper peel essential oil in pomelo peel can be dissolved out, realize the extraction to shaddock essential oil, further, the waste liquid produced in preparation process, sequentially passes through distillation and fractionation processing, realizes that shaddock peel essential oil is separated with organic activator;Most organic activator at last, is circulated again into shaddock peel adsorbent preparation process, reaches the recycling purpose of organic activator, reduces environmental pollution.
Description
Technical field
The present invention relates to biomaterial technology field, more particularly to a kind of Poly-generation work of pomelo peel regeneration product
Skill, shaddock peel adsorbent, and, shaddock peel essential oil.
Background technology
Shaddock is a kind of highly important southern fruit, originates in the southern areas such as China Fujian, Jiangxi, Guangdong, Guangxi.Shaddock
Sub- delicate fragrance, sour-sweet, Liang Run, nutritious, medical value is very high, is one of rare fruit of people's eating, is also that medical field is public
The fruit for the most dietotherapy benefit recognized.Pomelo peel is just dropped as a part for shaddock after each edible shaddock, or by
Dry, burn, and easily cause environmental pollution.
The substantial amounts of cellulose of content, the inside of cellulose in loose structure, the white flock layer of pomelo peel is presented in pomelo peel
There is substantial amounts of hole, some hole arrangements are close, in cellular, hole wall has spiral shape section line;The arrangement of some holes is loose, hole wall without
Line is saved, aperture is larger.Due to the characteristic of the loose structure of pomelo peel, pomelo peel is processed into biological adsorption agent, to adsorb dirt
Dyestuff and heavy metal in water, can improve the utilization rate of pomelo peel solid waste, reduce environmental pollution.At present on shaddock
The technique of skin adsorbent is modified method using soda acid, and activator generally uses organic acid or inorganic base.
The technique of prior art pomelo peel regeneration product, generally uses organic acid or inorganic base (sulfuric acid or phosphoric acid, hydroxide
Sodium) produce substantial amounts of soda acid activator solution as activator, in preparation process and be difficult to handle, cause waste and the ring of the energy
The pollution in border.
The content of the invention
The goal of the invention of the present invention is to provide a kind of multi-production process of pomelo peel regeneration product, shaddock peel adsorbent,
And, shaddock peel essential oil.Substantial amounts of acid-base waste fluid is produced in preparation process to solve existing pomelo peel regeneration product technique,
Cause the technical problem of environmental pollution.
The embodiment of the present application first aspect shows a kind of multi-production process of pomelo peel regeneration product, including:By pomelo peel
Dried after cleaning, the pomelo peel after being dried;
Pomelo peel powder after the drying is crushed, pomelo peel powder is obtained;
The pomelo peel powder is immersed in organic activator and is modified, modified mixture is obtained;
The modified mixture is cleaned, is filtered, the pomelo peel powder and waste liquid after cleaning is respectively obtained;
It will be carbonized after pomelo peel powder drying after the cleaning, natural cooling obtains shaddock peel adsorbent;
The waste liquid is distilled, retains organic fraction, the organic fraction includes:Shaddock peel essential oil and organic active
Agent;
The organic fraction is fractionated, shaddock peel essential oil and organic activator is respectively obtained, the organic activator is followed
Ring is used.
Technique shown in the embodiment of the present application, is modified using organic activator to pomelo peel powder, the shaddock prepared
Sub- skin adsorbent, even particle size distribution, and pore structure enrich, and the big central hole structure of shaddock peel adsorbent accounts for more than 60%, right
The absorption property of dyestuff and heavy metal is good in sewage.
Meanwhile, can be molten by the oilpaper peel essential oil in pomelo peel during being modified pomelo peel powder using organic activator
Solution comes out, and realizes the extraction of shaddock essential oil.
Further, the waste liquid produced in preparation process, sequentially pass through distillation with fractionation handle, realize shaddock peel essential oil with
Organic activator is separated;Most organic activator at last, is circulated again into shaddock peel adsorbent preparation process, can reach organic
The recycling purpose of activator, reduces environmental pollution.
Selectable, the control of the particle size range of the pomelo peel powder is in the mesh of 20 mesh~200.
It is selectable, described to be immersed in pomelo peel powder in step modified in organic activator, the shaddock peel powder
The last mass ratio with the organic activator is 1/2~1/5.
Selectable, the temperature of the charing is 500 DEG C~900 DEG C, and the time of the charing is 30min~150min.
Selectable, the organic activator is ethanol, ether, and, any one in ethyl acetate.
Selectable, the organic activator is ethanol, ether mixed solution.
Selectable, the volume ratio of the ethanol and the ether is 2:1.
It is selectable, 25 DEG C~40 DEG C of the modification temperature.
The embodiment of the present application second aspect shows a kind of shaddock peel adsorbent, and the shaddock peel adsorbent is implemented by the application
The technique exemplified is prepared from.
Technique shown in the embodiment of the present application, is modified using organic activator to pomelo peel powder, using organic work
Agent is modified obtained shaddock peel adsorbent to pomelo peel powder, and pore structure enriches, wherein, big central hole structure accounts for 60%
More than, good to the absorption property of dyestuff in sewage and heavy metal, the adsorbance to methylene blue can reach 14.11mgg-1, the absorption to iodine solution can reach 13.46mgg-1。
The specific surface area 1000m of the selectable adsorbent2·g-1~1500m2·g-1。
The embodiment of the present application third aspect shows a kind of shaddock essential oil, and the shaddock essential oil is shown by the embodiment of the present application
Technique be prepared from.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to institute in embodiment
The accompanying drawing needed to use is briefly described, it should be apparent that, drawings in the following description are only some implementations of the present invention
Example, for those of ordinary skill in the art, on the premise of not paying creative work, can also be obtained according to these accompanying drawings
Obtain other accompanying drawings.
Fig. 1 is the flow chart according to a multi-production process for being preferable to carry out a kind of pomelo peel regeneration product exemplified.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Whole description, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
The characterization processes of shaddock peel adsorbent:
The adsorptivity detection of basic-dyeable fibre:Basic-dyeable fibre uses methylene blue and iodine solution, and the measure of adsorptive value selects national standard
Scheme in method is detected, calculated.
The measure of GB/T12496.10-1999 wood activated charcoals test method-methylene blue adsorption value;
The measure of GB/T12496.8-1999 wood activated charcoals test method-iodine sorption value.
The detection of specific surface area, pore structure:The specific surface area and pore structure of activated carbon are carried out with BET analyzers
Analysis.
The yield calculation formula of shaddock peel essential oil:
It is worth noting that the impregnating ratio occurred in the embodiment of the present application is:Quality/organic activator of pomelo peel powder
Volume.
Known macropore is radius>50000nm aperture, mesopore is radius in 22000nm~50000nm aperture, absorption
Agent suction-operated is derived mainly from the pore structure of adsorbent, and macropore and mesopore are the passages of adsorption molecule.Usual adsorbent
Specific surface area is bigger, and absorption property is better.
Referring to Fig. 1, the embodiment of the present application shows a kind of technique of shaddock peel adsorbent, the technique includes:
S101 is dried after pomelo peel is cleaned, the pomelo peel after being dried;
S102 crushes the pomelo peel powder after the drying, obtains pomelo peel powder;
Pomelo peel is cleaned up, drying 2h~5h, the shaddock after being dried in drying box (60 DEG C~120 DEG C)
Skin, the pomelo peel after drying is put into pulverizer, breaks into pomelo peel powder, pomelo peel powder size the mesh of 20 mesh~200 it
Between;
The pomelo peel powder is immersed in organic activator and is modified by S103, obtains modified mixture;
Contain shaddock derived essential oil in known pomelo peel, the embodiment of the present application is modified pomelo peel using organic activator, will
Lipid solubilization in pomelo peel, and then extract separation shaddock essential oil.
By pomelo peel powder and finite concentration (concentration:50%~organic activator 95%) (pomelo peel powder with it is organic
The impregnating ratio of activator 1/2~1/5) in (25 DEG C~40 DEG C) progress activation modifications of proper temperature, modification time 1h~12h,
Pomelo peel powder is set to be stirred with organic activator as far as possible in modifying process, it is ensured that pomelo peel powder and organic activator are complete
Portion's immersion contact.
S104 cleans the modified mixture, and filtering respectively obtains the pomelo peel powder and waste liquid after cleaning;
S105 will be carbonized after the pomelo peel powder drying after the cleaning, and natural cooling obtains shaddock peel adsorbent;
Pomelo peel powder after cleaning is placed again into drying 2h~5h in drying box (40 DEG C~80 DEG C), to after cleaning
Pomelo peel powder surface moisture is evaporated, and is fitted into vessel, is put into high temperature furnace and is carbonized, and carbonization temperature is 500 DEG C~900
DEG C, 30min~150min is carbonized, the vessel after charing are taken out, natural cooling obtains shaddock peel adsorbent, and pack is sealed up for safekeeping.
S106 distills the waste liquid, retains organic fraction, and the organic fraction includes:Shaddock peel essential oil and organic work
Agent;
The organic fraction is fractionated by S107, respectively obtains shaddock peel essential oil and organic activator, the organic active
Agent is recycled.
Technique shown in the embodiment of the present application, is modified using organic activator to pomelo peel powder, the shaddock prepared
Sub- skin adsorbent, even particle size distribution, and pore structure enrich, and the big central hole structure of shaddock peel adsorbent accounts for more than 60%, right
The absorption property of dyestuff and heavy metal is good in sewage.
Meanwhile, can be molten by the oilpaper peel essential oil in pomelo peel during being modified pomelo peel powder using organic activator
Solution comes out, and realizes the extraction of shaddock essential oil.
Further, the waste liquid produced in preparation process, sequentially pass through distillation and fractionation processing, realize shaddock peel essential oil with
Organic activator is separated;Most organic activator at last, is circulated again into shaddock peel adsorbent preparation process, can reach organic
The recycling purpose of activator, reduces environmental pollution.
Selectable, the control of the particle size range of the pomelo peel powder is in the mesh of 20 mesh~200.
If the particle diameter of pomelo peel powder is less than 20 mesh, the oxidized possibility of pomelo peel powder is increased.
Consider carbonization efficiency, and, the oxidized possibility of modified pomelo peel powder, the embodiment of the present application will
The particle size range control of pomelo peel powder is in the mesh of 20 mesh~200.
Selectable, the temperature of the charing is 500 DEG C~900 DEG C, and the time of the charing is 30min~150min.
Selectable, the organic activator is ethanol, ether, and, any one in ethyl acetate.
Selectable, the organic activator is ethanol, ether mixed solution.
Selectable, the volume ratio of the ethanol and the ether is 2:1.
It is selectable, 25 DEG C~40 DEG C of the modification temperature.
Modification is carried out at room temperature, and the room temperature in the general north is at 25 DEG C or so, the temperature reachable 40 in southern summer room
DEG C or so.
Embodiment 1:
1. the preparation of shaddock peel adsorbent:
(1) pomelo peel is cleaned up, 4h is dried in 70 DEG C of drying box, after being put into pulverizer after pomelo peel completely drying
In, granularity is broken into the pomelo peel powder more than 100 mesh;
(2) by pomelo peel powder and 90% ethanol solution with 1:5 impregnating ratio, carries out immersion modification at normal temperatures, modified
Pomelo peel powder is set to be stirred with ethanol solution as far as possible in time 2h, modifying process, it is ensured that powder is whole with ethanol solution
Immersion contact.
(3) modified pomelo peel powder is cleaned 3 times with clear water, untill cleaning waste liquid is close to clarification, and collected
Waste liquid after each washing and filtering;Pomelo peel powder after over cleaning is placed again into drying box, 70 DEG C and dries 2h, to shaddock
Sub- skin powder surface water is evaporated, and is fitted into vessel;
(4) vessel that will be equipped with pomelo peel powder are put into high temperature furnace and carbonized, and carbonization temperature is 600 DEG C, charing
90min, takes out the vessel after charing, and natural cooling takes out shaddock peel adsorbent, and pack is sealed up for safekeeping.
2. the recycling of organic activator:
(1) substantial amounts of ethanol waste liquid can be produced during shaddock peel adsorbent is prepared, the ethanol waste liquid is cleaning
During cleaning fluid, containing the shaddock essential oil for leaching out from pomelo peel powder in this ethanol waste liquid, by this waste liquid 60
Under the conditions of DEG C, by air-distillation, organic fraction is collected;
(2) at 55 DEG C by fractionating device after organic fraction is mixed with impregnating agent, liquid fractionation a (ethanol) and fractionation are collected
In liquid b (shaddock peel essential oil), the modified technique that liquid fractionation a is returned to shaddock peel adsorbent production, pomelo peel powder is carried out
It is modified.By liquid fractionation b by anhydrous sodium sulfate drying 24h, that is, shaddock peel essential oil is made, calculates the yield of shaddock peel essential oil.
The adsorptivity experiment and the absorption of iodine solution of methylene blue solution are carried out to shaddock peel adsorbent made from above-mentioned technique
Property experiment and, shaddock peel essential oil carry out yield calculating, the results are shown in Table 1:
Table 1:
Example 2:
1. the preparation of shaddock peel adsorbent:
(1) pomelo peel is cleaned up, 4h is dried in 70 DEG C of drying box, after being put into pulverizer after pomelo peel completely drying
In, powder is broken into, powder size is more than 100 mesh;
(2) by pomelo peel powder and 70% ethanol solution with 1:3 impregnating ratio, carries out immersion modification at normal temperatures, modified
Pomelo peel powder is set to be stirred with ethanol solution as far as possible in time 2h, modifying process, it is ensured that powder is whole with ethanol solution
Immersion contact.
(3) modified pomelo peel powder is cleaned 3 times with clear water, untill cleaning waste liquid is close to clarification, and collected
Waste liquid after each washing and filtering;Pomelo peel powder after over cleaning is placed again into drying box, 70 DEG C and dries 2h, to shaddock
Sub- skin powder surface water is evaporated, and is fitted into vessel;
(4) vessel that will be equipped with pomelo peel powder are put into high temperature furnace and carbonized, and carbonization temperature is 600 DEG C, charing
90min, takes out the vessel after charing, and natural cooling takes out shaddock peel adsorbent, and pack is sealed up for safekeeping.
2. the recycling of organic activator:
(1) prepare shaddock peel adsorbent during can produce substantial amounts of ethanol waste liquid, in this ethanol waste liquid contain from
The shaddock essential oil for leaching out in pomelo peel powder, by this waste liquid under the conditions of 60 DEG C, by air-distillation, collects organic evaporate
Point;
(2) at 55 DEG C by fractionating device after organic fraction is mixed with impregnating agent, liquid fractionation a (ethanol) and fractionation are collected
In liquid b (shaddock peel essential oil), the modified technique that liquid fractionation a is returned to shaddock peel adsorbent production, pomelo peel powder is carried out
It is modified.By liquid fractionation b by anhydrous sodium sulfate drying 24h, that is, shaddock peel essential oil is made, calculates the yield of shaddock peel essential oil.
The adsorptivity experiment and the absorption of iodine solution of methylene blue solution are carried out to shaddock peel adsorbent made from above-mentioned technique
Property experiment and, shaddock peel essential oil carry out yield calculating, the results are shown in Table 2:
Table 2:
Example 3:
1. the preparation of shaddock peel adsorbent:
(1) pomelo peel is cleaned up, 4h is dried in 70 DEG C of drying box, after being put into pulverizer after pomelo peel completely drying
In, powder is broken into, powder size is more than 100 mesh;
(2) by pomelo peel powder and 90% diethyl ether solution with 1:3 impregnating ratio, carries out immersion modification at normal temperatures, modified
Pomelo peel powder is set to be stirred with diethyl ether solution as far as possible in time 2h, modifying process, it is ensured that powder is whole with diethyl ether solution
Immersion contact.
(3) modified pomelo peel powder is cleaned 3 times with clear water, untill cleaning waste liquid is close to clarification, and collected
Waste liquid after each washing and filtering;Pomelo peel powder after over cleaning is placed again into drying box, 70 DEG C and dries 2h, to shaddock
Sub- skin powder surface water is evaporated, and is fitted into vessel;
(4) vessel that will be equipped with pomelo peel powder are put into high temperature furnace and carbonized, and carbonization temperature is 600 DEG C, charing
90min, takes out the vessel after charing, and natural cooling takes out shaddock peel adsorbent, and pack is sealed up for safekeeping.
2. the recycling of organic activator:
(1) prepare shaddock peel adsorbent during can produce substantial amounts of ether waste liquid, in this ether waste liquid contain from
The shaddock essential oil for leaching out in pomelo peel powder, by this waste liquid under the conditions of 60 DEG C, by air-distillation, collects organic evaporate
Point;
(2) at 55 DEG C by fractionating device after organic fraction is mixed with impregnating agent, liquid fractionation a (ether) and fractionation are collected
In liquid b (shaddock peel essential oil), the modified technique that liquid fractionation a is returned to shaddock peel adsorbent production, pomelo peel powder is carried out
It is modified.By liquid fractionation b by anhydrous sodium sulfate drying 24h, that is, shaddock peel essential oil is made, calculates the yield of shaddock peel essential oil.
The adsorptivity experiment and the absorption of iodine solution of methylene blue solution are carried out to shaddock peel adsorbent made from above-mentioned technique
Property experiment and, shaddock peel essential oil carry out yield calculating, the results are shown in Table 3:
Table 3:
Example 4:
1. the preparation of shaddock peel adsorbent
(1) pomelo peel is cleaned up, 4h is dried in 70 DEG C of drying box, after being put into pulverizer after pomelo peel completely drying
In, powder is broken into, powder size is more than 100 mesh;
(2) by pomelo peel powder and 80% ethyl acetate solution with 1:3 impregnating ratio, carries out immersion modification at normal temperatures,
Pomelo peel powder is set to be stirred with ethyl acetate solution as far as possible in modification time 2h, modifying process, it is ensured that powder and acetic acid
The all immersion contacts of ethyl ester solution.
(3) modified pomelo peel powder is cleaned 3 times with clear water, untill cleaning waste liquid is close to clarification, and collected
Waste liquid after each washing and filtering;Pomelo peel powder after over cleaning is placed again into drying box, 70 DEG C and dries 2h, to shaddock
Sub- skin powder surface water is evaporated, and is fitted into vessel;
(4) vessel that will be equipped with pomelo peel powder are put into high temperature furnace and carbonized, and carbonization temperature is 600 DEG C, charing
90min, takes out the vessel after charing, and natural cooling takes out shaddock peel adsorbent, and pack is sealed up for safekeeping.
2. the recycling of organic activator:
(1) substantial amounts of ethyl acetate waste liquid can be produced during shaddock peel adsorbent is prepared, this ethyl acetate waste liquid
In containing the shaddock essential oil that leaches out from pomelo peel powder, by this waste liquid under the conditions of 60 DEG C, pass through air-distillation, collect
Organic fraction;
(2) at 55 DEG C by fractionating device after organic fraction is mixed with impregnating agent, collect liquid fractionation a (ethyl acetate) and
In liquid fractionation b (shaddock peel essential oil), the modified technique that liquid fractionation a is returned to shaddock peel adsorbent production, to pomelo peel powder
It is modified.By liquid fractionation b by anhydrous sodium sulfate drying 24h, that is, shaddock peel essential oil is made, calculates the receipts of shaddock peel essential oil
Rate.
The adsorptivity experiment and the absorption of iodine solution of methylene blue solution are carried out to shaddock peel adsorbent made from above-mentioned technique
Property experiment and, shaddock peel essential oil carry out yield calculating, the results are shown in Table 4:
Table 4:
Example 5:
1. the preparation of shaddock peel adsorbent:
(1) pomelo peel is cleaned up, 4h is dried in 70 DEG C of drying box, after being put into pulverizer after pomelo peel completely drying
In, powder is broken into, powder size is more than 100 mesh;
(2) it is activator, two kinds of solution by the mixed liquor of pomelo peel powder and 90% ethanol solution and 80% diethyl ether solution
The ratio between be 2:1, with 1:5 impregnating ratio, carries out making shaddock as far as possible in immersion modification, modification time 2h, modifying process at normal temperatures
Sub- skin powder is stirred with mixed solution, it is ensured that all immersion is contacted powder with mixed solution.
(3) the pomelo peel powder for separating modified pomelo peel powder with impregnating agent is cleaned 3 times with clear water, until cleaning
Untill the close clarification of waste liquid, and collect the waste liquid after each washing and filtering;Pomelo peel powder after over cleaning is placed again into
Drying box, dries 2h in 70 DEG C, is evaporated, is fitted into vessel to pomelo peel powder surface water;
(4) vessel that will be equipped with pomelo peel powder are put into high temperature furnace and carbonized, and carbonization temperature is 600 DEG C, charing
90min, takes out the vessel after charing, and natural cooling takes out shaddock peel adsorbent, and pack is sealed up for safekeeping.
2. the recycling of organic activator:
(1) prepare shaddock peel adsorbent during can produce substantial amounts of mixed waste liquor, in this mixed waste liquor contain from
The shaddock essential oil for leaching out in pomelo peel powder, by this waste liquid under the conditions of 60 DEG C, by air-distillation, collects organic evaporate
Point;
(2) at 55 DEG C by fractionating device after organic fraction is mixed with impregnating agent, liquid fractionation a (ether) and fractionation are collected
Liquid b (shaddock peel essential oil) and liquid fractionation c (ethanol), 1 is pressed by liquid fractionation a and liquid fractionation c:After 2 is well mixed, pomelo peel is returned to
In the modified technique of adsorbent production, pomelo peel powder is modified.By liquid fractionation b by anhydrous sodium sulfate drying 24h, i.e.,
Shaddock peel essential oil is made, the yield of shaddock peel essential oil is calculated.
The adsorptivity experiment and the absorption of iodine solution of methylene blue solution are carried out to shaddock peel adsorbent made from above-mentioned technique
Property experiment and, shaddock peel essential oil carry out yield calculating, the results are shown in Table 5:
Table 5:
It is selectable, described to be immersed in pomelo peel powder in step modified in organic activator, the shaddock peel powder
The last mass ratio with the organic activator is 1/2~1/5.
Embodiment 6:
The preparation of shaddock peel adsorbent:
(1) pomelo peel is cleaned up, 4h is dried in 70 DEG C of drying box, after being put into pulverizer after pomelo peel completely drying
In, granularity is broken into the pomelo peel powder more than 100 mesh;
(2) by pomelo peel powder and 90% ethanol solution with 1:7 impregnating ratio, carries out immersion modification at normal temperatures, modified
Pomelo peel powder is set to be stirred with ethanol solution as far as possible in time 2h, modifying process, it is ensured that powder is whole with ethanol solution
Immersion contact.
(3) modified pomelo peel powder is cleaned 3 times with clear water, untill cleaning waste liquid is close to clarification, and collected
Waste liquid after each washing and filtering;Pomelo peel powder after over cleaning is placed again into drying box, 70 DEG C and dries 2h, to shaddock
Sub- skin powder surface water is evaporated, and is fitted into vessel;
(4) vessel that will be equipped with pomelo peel powder are put into high temperature furnace and carbonized, and carbonization temperature is 600 DEG C, charing
90min, takes out the vessel after charing, and natural cooling takes out shaddock peel adsorbent, and pack is sealed up for safekeeping.
The adsorbance 13.71mgg of shaddock peel adsorbent prepared by embodiment 6 to methylene blue-1, to the adsorbance of iodine solution
For 11.65mgg-1
Embodiment 7:
The preparation of shaddock peel adsorbent:
(1) pomelo peel is cleaned up, 4h is dried in 70 DEG C of drying box, after being put into pulverizer after pomelo peel completely drying
In, granularity is broken into the pomelo peel powder more than 100 mesh;
(2) by pomelo peel powder and 90% ethanol solution with 1:5 impregnating ratio, carries out immersion modification at normal temperatures, modified
Pomelo peel powder is set to be stirred with ethanol solution as far as possible in time 2h, modifying process, it is ensured that powder is whole with ethanol solution
Immersion contact.
(3) modified pomelo peel powder is cleaned 3 times with clear water, untill cleaning waste liquid is close to clarification, and collected
Waste liquid after each washing and filtering;Pomelo peel powder after over cleaning is placed again into drying box, 70 DEG C and dries 2h, to shaddock
Sub- skin powder surface water is evaporated, and is fitted into vessel;
(4) vessel that will be equipped with pomelo peel powder are put into high temperature furnace and carbonized, and carbonization temperature is 600 DEG C, charing
90min, takes out the vessel after charing, and natural cooling takes out shaddock peel adsorbent, and pack is sealed up for safekeeping.
The adsorbance 9.42mgg of shaddock peel adsorbent prepared by embodiment 7 to methylene blue-1, to the adsorbance of iodine solution
For 7.78mgg-1
Integrated embodiment 1, embodiment 6 and embodiment 7 are visible, with the impregnating ratio of pomelo peel powder and organic activator
Reduction, the shaddock peel adsorbent prepared gradually increases the adsorbance of methylene blue and iodine solution, but works as pomelo peel
The impregnating ratio of powder and organic activator reaches 1:Continue the pomelo peel absorption for increasing the consumption of organic activator, preparing when 5
Agent is not further added by the adsorbance of methylene blue and iodine solution, and that now continues increase organic activator can only cause organic active
The waste of agent.
The scope that the mass ratio of pomelo peel powder and the organic activator is 1/2~1/5 is interior by the embodiment of the present application.
Those skilled in the art will readily occur to its of the present invention after considering specification and putting into practice invention disclosed herein
Its embodiment.The application be intended to the present invention any modification, purposes or adaptations, these modifications, purposes or
Person's adaptations follow the general principle of the present invention and including undocumented common knowledge in the art of the invention
Or conventional techniques.Description and embodiments are considered only as exemplary, and true scope and spirit of the invention are by following
Claim is pointed out.
It should be appreciated that the invention is not limited in the precision architecture for being described above and being shown in the drawings, and
And various modifications and changes can be being carried out without departing from the scope.The scope of the present invention is only limited by appended claim.
Claims (10)
1. a kind of multi-production process of pomelo peel regeneration product, it is characterised in that including:
Dried after pomelo peel is cleaned, the pomelo peel after being dried;
Pomelo peel powder after the drying is crushed, pomelo peel powder is obtained;
The pomelo peel powder is immersed in organic activator and is modified, modified mixture is obtained;
The modified mixture is cleaned, is filtered, the pomelo peel powder and waste liquid after cleaning is respectively obtained;
It will be carbonized after pomelo peel powder drying after the cleaning, natural cooling obtains shaddock peel adsorbent;
The waste liquid is distilled, retains organic fraction, the organic fraction includes:Shaddock peel essential oil and organic activator;
The organic fraction is fractionated, shaddock peel essential oil and organic activator is respectively obtained, the organic activator circulation makes
With.
2. technique according to claim 1, it is characterised in that the particle size range control of the pomelo peel powder 20 mesh~
200 mesh.
3. technique according to claim 2, it is characterised in that described pomelo peel powder is immersed in organic activator changes
Property the step of in, the mass ratio of the pomelo peel powder and the organic activator is 1/2~1/5.
4. technique according to claim 3, it is characterised in that the temperature of the charing is 500 DEG C~900 DEG C, the charcoal
The time of change is 30min~150min.
5. the technique according to any one of Claims 1 to 4, it is characterised in that the organic activator is ethanol, ether,
And, any one in ethyl acetate.
6. the technique according to any one of Claims 1 to 4, it is characterised in that the organic activator is ethanol and ether
Mixed solution.
7. technique according to claim 6, it is characterised in that the volume ratio of the ethanol and the ether is 2:1.
8. a kind of shaddock peel adsorbent, the shaddock peel adsorbent is as the technique preparation described in claim 1~7 any one
Into.
9. adsorbent according to claim 8, it is characterised in that the specific surface area 1000m of the adsorbent2·g-1~
1500m2·g-1。
10. a kind of shaddock peel essential oil, the shaddock peel essential oil is prepared from by the technique described in claim 1~7 any one.
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CN109168895A (en) * | 2018-09-29 | 2019-01-11 | 广西百乐德农业投资有限公司 | A kind of implantation methods of citrus |
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CN112409990A (en) * | 2020-11-20 | 2021-02-26 | 上海智勇教育培训有限公司 | Oil absorption material and preparation method thereof |
CN112979219A (en) * | 2021-03-16 | 2021-06-18 | 浙江理工大学 | Porous carbon fiber material with photo-thermal and joule-thermal essential oil controlled release functions and preparation method thereof |
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