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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
peel
shaddock
pomelo peel
powder
adsorbent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710483985.1A
Other languages
Chinese (zh)
Inventor
崔帅
吕武华
赵静
喻娜
向丹
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangan Vocational and Technical College
Original Assignee
Guangan Vocational and Technical College
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangan Vocational and Technical College filed Critical Guangan Vocational and Technical College
Priority to CN201710483985.1A priority Critical patent/CN107163964A/en
Publication of CN107163964A publication Critical patent/CN107163964A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10BDESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/02Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid 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
    • B01J20/28057Surface area, e.g. B.E.T specific surface area
    • B01J20/28066Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/12Halogens or halogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/10Biofuels, e.g. bio-diesel
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00Technologies for the production of fuel of non-fossil origin
    • Y02E50/30Fuel from waste, e.g. synthetic alcohol or diesel

Landscapes

  • 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

A kind of multi-production process of pomelo peel regeneration product, shaddock peel adsorbent, and, shaddock Sub- peel essential oil
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.
CN201710483985.1A 2017-06-23 2017-06-23 A kind of multi-production process of pomelo peel regeneration product, shaddock peel adsorbent, and, shaddock peel essential oil Pending CN107163964A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710483985.1A CN107163964A (en) 2017-06-23 2017-06-23 A kind of multi-production process of pomelo peel regeneration product, shaddock peel adsorbent, and, shaddock peel essential oil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710483985.1A CN107163964A (en) 2017-06-23 2017-06-23 A kind of multi-production process of pomelo peel regeneration product, shaddock peel adsorbent, and, shaddock peel essential oil

Publications (1)

Publication Number Publication Date
CN107163964A true CN107163964A (en) 2017-09-15

Family

ID=59820509

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710483985.1A Pending CN107163964A (en) 2017-06-23 2017-06-23 A kind of multi-production process of pomelo peel regeneration product, shaddock peel adsorbent, and, shaddock peel essential oil

Country Status (1)

Country Link
CN (1) CN107163964A (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109735426A (en) * 2019-03-25 2019-05-10 内蒙古农业大学 A kind of brewing method retaining anthocyanidin blueberry fruit vinegar
CN111154554A (en) * 2020-01-03 2020-05-15 长沙凯泽工程设计有限公司 Safe and residue-free skin-care detergent and preparation method thereof
CN111616209A (en) * 2020-05-09 2020-09-04 广东省农业科学院蚕业与农产品加工研究所 Bacteriostatic agent prepared from pomelo peel and seed and preparation method thereof
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

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103484257A (en) * 2013-10-14 2014-01-01 厦门大学 Comprehensive utilization method for pomelo peels
CN104206436A (en) * 2014-09-04 2014-12-17 淮阴师范学院 Method for preparing series products by using pummelo fruit full skin without residue
CN106065332A (en) * 2016-06-03 2016-11-02 浙江科技学院 A kind of method and the application that utilize pomelo peel hydro-thermal carbonization to prepare charcoal
CN106345428A (en) * 2016-11-02 2017-01-25 梁玉峰 Efficient formaldehyde adsorbent with fruit fragrance

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103484257A (en) * 2013-10-14 2014-01-01 厦门大学 Comprehensive utilization method for pomelo peels
CN104206436A (en) * 2014-09-04 2014-12-17 淮阴师范学院 Method for preparing series products by using pummelo fruit full skin without residue
CN106065332A (en) * 2016-06-03 2016-11-02 浙江科技学院 A kind of method and the application that utilize pomelo peel hydro-thermal carbonization to prepare charcoal
CN106345428A (en) * 2016-11-02 2017-01-25 梁玉峰 Efficient formaldehyde adsorbent with fruit fragrance

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘新社,杜保伟主编: "《果蔬贮藏与加工技术》", 30 April 2014, 北京:中国轻工业出版社 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109735426A (en) * 2019-03-25 2019-05-10 内蒙古农业大学 A kind of brewing method retaining anthocyanidin blueberry fruit vinegar
CN111154554A (en) * 2020-01-03 2020-05-15 长沙凯泽工程设计有限公司 Safe and residue-free skin-care detergent and preparation method thereof
CN111154554B (en) * 2020-01-03 2021-03-23 广州市家真惠实业有限公司 Safe and residue-free skin-care detergent and preparation method thereof
CN111616209A (en) * 2020-05-09 2020-09-04 广东省农业科学院蚕业与农产品加工研究所 Bacteriostatic agent prepared from pomelo peel and seed and preparation method thereof
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
CN112979219B (en) * 2021-03-16 2022-08-23 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

Similar Documents

Publication Publication Date Title
CN107163964A (en) A kind of multi-production process of pomelo peel regeneration product, shaddock peel adsorbent, and, shaddock peel essential oil
CN106861622B (en) A kind of water treatment agent handling eutrophication water
CN105217629B (en) The preparation method of coffee grounds activated carbon
CN106995224A (en) A kind of method for going to remove water moderate resistance life element
CN108439402B (en) A kind of supercapacitor ginger stalk matrix activated carbon and preparation method thereof
CN104891491A (en) Method for preparing bamboo shoot shell-based activated carbon for super capacitor
CN105344322A (en) Method for preparing biological activated carbon from waste maidenhair tree leaves and folium ginkgo herb residue
CN106966390B (en) A kind of preparation method and products therefrom of alkali lignin matrix activated carbon
CN104326471A (en) Method for preparing active carbon from licorice waste residue
CN103464111B (en) Softex kw modification walnut shell adsorbent and its preparation method and application
CN106044744B (en) A kind of preparation method and its usage of graphene/lignin-base combined multi-stage hole carbon plate material
CN103539119A (en) Preparation method of activated carbon for electrochemical energy storage device
CN107445163A (en) A kind of preparation method of bacteriostatic activated carbon
CN108862274A (en) A kind of preparation method and applications of cellulose base level porous carbon materials
CN107555430A (en) A kind of ultracapacitor pine needle matrix activated carbon and one step charing preparation method
CN107583609A (en) A kind of modified mangosteen shell charcoal and the method using vanadium in its reduction water body
CN110449122A (en) Load the sludge-based activated carbon and its preparation method and application of national standard method
CN106824083A (en) A kind of preparation method and applications of attapulgite/biomass carbon compound adsorbent
CN107445160A (en) A kind of insolubility alginic acid alkali super capacitor active carbon and one step charing preparation method of adjustable aperture
CN108046254A (en) A kind of corncob derives active carbon electrode material and preparation method thereof
CN103877934A (en) Method for preparing porous carbon material from bean dregs and application of porous carbon material serving as adsorbent in wastewater treatment
CN107913677A (en) A kind of nanometer heavy metal wastewater thereby ionic adsorption microballoon and preparation method thereof
CN102424383B (en) Method for preparing mesoporous carbon material for electrochemical capacitor
CN109650388A (en) A kind of method and its application preparing biomass-based functional activity Carbon Materials using concentrated seawater auxiliary
CN106423062A (en) Preparation method of orange-peel-based adsorbent for removing hexavalent chromium ions in water

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20170915