CN105129949A - Method for extracting natural flocculation active ingredients from hesperidium peels, method for preparing algaecide and method for removing algae in water through algaecide - Google Patents

Method for extracting natural flocculation active ingredients from hesperidium peels, method for preparing algaecide and method for removing algae in water through algaecide Download PDF

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Publication number
CN105129949A
CN105129949A CN201510558579.8A CN201510558579A CN105129949A CN 105129949 A CN105129949 A CN 105129949A CN 201510558579 A CN201510558579 A CN 201510558579A CN 105129949 A CN105129949 A CN 105129949A
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water
citrus peel
algae
activity composition
hesperidium
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CN201510558579.8A
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CN105129949B (en
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王红强
焦学然
成水平
田长勋
邓启湘
郭一飞
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Henan University of Urban Construction
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Henan University of Urban Construction
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Abstract

The invention relates to a method for extracting natural flocculation active ingredients, in particular to a method for extracting natural flocculation active ingredients from hesperidium peels. According to the method, the pretreated hesperidium peels and ultra-pure water or distilled water or cooled boiling tap water are first mixed according to the mass-volume proportion of 1:2.78-33.33; then leaching liquor is treated, and hesperidium peel residues are removed to obtain water extract of the hesperidium peels. The invention further discloses a method for preparing algaecide through the natural flocculation active ingredients extracted from the hesperidium peels and a method for removing algae in water through the algaecide. 0.5-10 mL of the obtained water extract of the hesperidium peels is diluted to 30 mL through the ultra-pure water or the distilled water or the cooled boiling tap water to prepare a flocculating agent finished product; the flocculating agent is added into the water containing the algae to stand so that the flocculating agent and the algae in the water can react to remove the algae in the water. The algaecide prepared from the natural flocculation active ingredients extracted form the hesperidium peels belongs to a natural ingredient, is used for removing the algae and easy to degrade in the water body and will not cause secondary pollution.

Description

From Citrus peel, extracting natural flocculation activity composition, preparing algicide and the method for removing algae in water thereof
Technical field
The present invention relates to a kind of for except the natural flocculation activity component extracting method of algae, especially relate to and a kind ofly from Citrus peel, extract natural flocculation activity composition, prepare flocculation agent and for the method except middle algae of anhydrating.
Background technology
Body eutrophication is one of topmost water pollution problems of facing of the world today.Along with modern cityization and industrial development, body eutrophication is on the rise, and has become the principal element of restriction Chinese national economy and social development.Body eutrophication causes wawter bloom again and again to be broken out, and function of water body is subject to expensive damage.
In breakout of water bloom emergency processing, at substantial manpower salvaged by machinery, the biological treatment startup optimization time is longer again, so people develop and variously kill removing algae agent, process for algae achieves certain effect, but algicide has certain residual toxicity, and along with going deep into of studying Algae toxins, traditional algicide adds the drawback that rear Algae toxins is discharged into water body and also displays.In plant materials, extract natural flocculation activity composition for except algae, have safe and harmless, can not frustule be destroyed in flocculation is except algae process, can not the plurality of advantages such as secondary pollution be caused, and abundant raw material, cheap.Therefore, to utilizing natural flocculating agent to algae-containing water body except the research of algae obtains the attention of people.
Chinese invention patent " being prepared method and the application of environment-friendly type flocculation agent by discarded pericarp " (application number: 201310568550.9) disclose and a kind ofly utilize the peel of Citrus reticulata Blanco of natural air drying to roll to be crushed to particle, particle is added ethanol in a kettle., soak, filtration under diminished pressure is to flowing out without solution, be dried to constant weight, cationic polymers is mixed with the pericarp being dried to constant weight, stir, pulverize, sieve, powder and calcium oxide or clay are mixed to get the method for flocculation agent, the handling object of this patent gained flocculation agent to use it for process field produces sewage or waste water-base drilling liquid process.Described flocculation agent making processes is loaded down with trivial details, also needs to use reactor equal pressure container.
Summary of the invention
The present invention is directed to prior art deficiency, propose and a kind ofly from Citrus peel, extract natural flocculation activity composition, prepare algicide and for the method except algae in water, for being that the Small-scale Landscape Water Bodies of sociales is except algae with blue-green algae, except algae is thorough, speed fast, algal bloom can be controlled safely and effectively.
The technical solution adopted in the present invention:
From Citrus peel, extract a method for natural flocculation activity composition, comprise step as follows:
(1) by pretreated Citrus peel and ultrapure water, distilled water or boil cooling tap water according to quality: volume ratio is the ratio mixing of 1:2.78 ~ 33.33;
(2) vat liquor is processed, remove Citrus peel slag and obtain Citrus peel aqueous extract.
The described method extracting natural flocculation activity composition from Citrus peel, pretreated step comprises Citrus peel cleaning, the process of drying or drying, pulverizing: Citrus peel is clean with the tap water or ultrapure water boiling cooling, naturally dry or drying and processing 2 ~ 4 days under 40 ~ 60 DEG C of conditions, obtain dry Citrus peel material, being then crushed to granular size is 20 ~ 80 orders.
The described method extracting natural flocculation activity composition from Citrus peel, in step (1), places 0.5 ~ 48 hour after Citrus peel and ultrapure water, distilled water or the tap water boiling cooling mix, with the abundant stripping of activeconstituents contained by promoting in Citrus peel.
The described method extracting natural flocculation activity composition from Citrus peel, in step (2), uses whizzer to process vat liquor, removes Citrus peel slag and obtains after Citrus peel aqueous extract again through 0.45 μm or 0.22 μm of membrane filtration.
The described method extracting natural flocculation activity composition from Citrus peel, is characterized in that: centrifuge speed controls at 1000 ~ 9000r/min.
Utilizing the aforementioned natural flocculation activity composition extracted from Citrus peel to prepare a method for algicide, is that gained Citrus peel aqueous extract 0.5 ~ 10mL ultrapure water, distilled water or the tap water that boils cooling are diluted to 30mL.
Utilizing the aforementioned natural flocculation activity composition extracted from Citrus peel to prepare algicide and a method for removing algae in water, the steps include:
1) gained Citrus peel aqueous extract 0.5 ~ 10mL ultrapure water, distilled water or the tap water that boils cooling are diluted to 30mL, obtained flocculation agent finished product;
2) add in algae-containing water by described flocculation agent, leave standstill 3 ~ 4 hours, to make the algae in flocculation agent and water react, the flco of generation fully precipitates, thus removes algae from water.
The described natural flocculation activity composition extracted from Citrus peel prepares algicide and method for removing algae in water, during use, is determined by experiment flocculant usage according to frustule quantity in water body.
Beneficial effect of the present invention:
1, the present invention extracts natural flocculation activity composition and prepares algicide and for except the method for algae, obtain the algicide that the natural flocculation activity composition of Citrus peel is obtained, belong to natural component, easily degrade in water body, can not cause secondary pollution from Citrus peel.Except algae is thorough, speed fast, easy to operate.
2, the Citrus peel natural flocculating agent prepared of the present invention, effectively can remove algae, and frustule flocculation is agglomerating to sink under water, little on the impact of environment, non-secondary pollution, and water body is limpid, does not affect water body attractive in appearance, is applicable to be that the Small-scale Landscape Water Bodies of sociales is except algae with blue-green algae.
3, Citrus peel natural flocculating agent of the present invention and algae-removing method thereof, without the need to stirring after adding, having the advantages such as efficient, energy-saving and environmental protection, and frond can be made to be settled down to the bottom, is a kind of comparatively ideal algicide making algae sedimentation.The present invention is practical, except algae cost is low, is easy to apply.
4. the present invention is raw materials used is Citrus peel, thus proposes new approach for its recycling; It is simple that the present invention simultaneously has flocculation agent extraction process, and easy and simple to handle, without the need to plurality of advantages such as large-scale instrument and equipments, the flocculation agent of extraction has good flocculating effect, can effectively remove algae in water, for algae removal provides new method.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1
The present invention extracts natural flocculation activity composition and prepares algicide and for the method except algae, comprise the following steps from Citrus peel:
(1) being cleaned, naturally dry or dry, be crushed to granular size by fresh Citrus peel is 20 ~ 80 orders;
(2) by Citrus peel and ultrapure water or the distilled water after pulverizing, boil the tap water of cooling according to quality: the ratio mixing of volume=1:2.78 ~ 1:33.33, preferred 1:11.11, and place 0.5 ~ 48 hour after stirring, preferably 24 hours, to promote the abundant stripping of activeconstituents contained in Citrus peel;
(3) use whizzer to carry out centrifugal treating to vat liquor, remove Citrus peel slag and obtain Citrus peel aqueous extract;
(4) get extracting solution 0.5 ~ 10mL ultrapure water or distilled water, boil the tap water of cooling and be diluted to 30mL, this is final flocculation agent;
(5) get the flocculation agent described in step (4), add in pending algae-containing water, algae in water can be removed, be determined by experiment the optimum amount of flocculation agent according to frustule quantity in water body.
Embodiment 2
The present embodiment extracts the method for natural flocculation activity composition from Citrus peel, comprises step as follows:
(1) by pretreated Citrus peel and ultrapure water, distilled water or boil cooling tap water according to quality: volume ratio is the ratio mixing of 1:2.78 ~ 33.33.
(2) vat liquor is processed, remove Citrus peel slag and obtain Citrus peel aqueous extract.
The quality that foregoing embodiments is mentioned: volume ratio, mass unit with gram or kilogram metering, volume unit is corresponding with milliliter or rise metering, lower with.
Embodiment 3
The present embodiment extracts the method for natural flocculation activity composition from Citrus peel, be with the difference of embodiment 2, the pretreated step of Citrus peel comprises: Citrus peel cleaning, the process of naturally drying or drying, pulverizing: Citrus peel is clean with the tap water or ultrapure water boiling cooling, naturally dry or drying and processing 2 ~ 4 days under 40 ~ 60 DEG C of conditions, obtain dry Citrus peel material, being then crushed to granular size is 20 ~ 80 orders.
Embodiment 4
The present embodiment extracts the method for natural flocculation activity composition from Citrus peel, be with the difference of embodiment 2 or embodiment 3: in step (1), places 0.5 ~ 48 hour after Citrus peel and ultrapure water, distilled water or the tap water boiling cooling mix, with the abundant stripping of activeconstituents contained by promoting in Citrus peel.
Embodiment 5
The present embodiment extracts the method for natural flocculation activity composition from Citrus peel, be with the difference of foregoing embodiments: in step (2), whizzer is used to process vat liquor, centrifuge speed controls at 1000 ~ 9000r/min, removes Citrus peel slag and obtains after Citrus peel aqueous extract again through 0.45 μm or 0.22 μm of membrane filtration.
Embodiment 6
The present embodiment is utilize the aforementioned natural flocculation activity composition extracted from Citrus peel to prepare the method for algicide, that is: gained Citrus peel aqueous extract 0.5 ~ 10mL ultrapure water, distilled water or the tap water that boils cooling are diluted to 30mL, obtained final flocculation agent (algicide).
Embodiment 7
The present embodiment is utilize the aforementioned natural flocculation activity composition extracted from Citrus peel to prepare algicide and method for removing algae in water, 1) gained Citrus peel aqueous extract 0.5 ~ 10mL ultrapure water, distilled water or the tap water that boils cooling are diluted to 30mL, this is final flocculation agent;
2) add in algae-containing water by described flocculation agent, leave standstill 3 ~ 4 hours, to make the algae in flocculation agent and water react, the flco of generation fully precipitates, thus removes algae from water.
The described natural flocculation activity composition extracted from Citrus peel, for removing the method for algae in water, is determined by experiment the optimum amount of flocculation agent according to frustule quantity in water body.
Embodiment 8
The present embodiment extracts the method for natural flocculation activity composition from Citrus peel, is with the difference of foregoing embodiments: by pretreated Citrus peel and ultrapure water, distilled water or boil cooling tap water according to quality: volume ratio is that the ratio of 1:2.78 mixes.
Embodiment 9
The present embodiment extracts the method for natural flocculation activity composition from Citrus peel, is with the difference of foregoing embodiments: by pretreated Citrus peel and ultrapure water, distilled water or boil cooling tap water according to quality: volume ratio is that the ratio of 1:33.33 mixes.
Embodiment 10
The present embodiment extracts the method for natural flocculation activity composition from Citrus peel, is with the difference of foregoing embodiments: by pretreated Citrus peel and ultrapure water, distilled water or boil cooling tap water according to quality: volume ratio is that the ratio of 1:6 mixes.
Embodiment 11
The present embodiment extracts the method for natural flocculation activity composition from Citrus peel, is with the difference of foregoing embodiments: by pretreated Citrus peel and ultrapure water, distilled water or boil cooling tap water according to quality: volume ratio is that the ratio of 1:20 mixes.
Embodiment 12
The present embodiment extracts the method for natural flocculation activity composition from Citrus peel, is with the difference of foregoing embodiments: by pretreated Citrus peel and ultrapure water, distilled water or boil cooling tap water according to quality: volume ratio is that the ratio of 1:26 mixes.
Below in conjunction with laboratory result of study to the extracting method of the present invention's natural flocculation activity composition, the preparation of algicide (flocculation agent) and in water except dry method and process further illustrate.
Experiment 1
Get fresh Citrus peel ultrapure water clean, naturally dry, being crushed to granular size is 80 orders.Take ultrapure water as water source, 5.625g Citrus peel powder is immersed in the water of 125mL, place 24 hours, whizzer is used to carry out centrifugal treating to vat liquor, rotating speed is 5000r/min, removes Citrus peel slag and obtains Citrus peel aqueous extract, with ultrapure water, the volume of extracting solution is adjusted to 125mL; Get extracting solution 1mL ultrapure water or distilled water, boil the tap water of cooling and be diluted to 30mL, this is final flocculation agent; Getting flocculation agent 5mL, to be added to 45 milliliters of concentration of algae be 7.6 × 10 6in the water body of individual/mL, leave standstill 3h, part algae is deposited to the bottom, and detecting its alga-killing rate is 71.73%; When extracting solution becomes 3mL from 1mL, its alga-killing rate can reach 93.46%.
Experiment 2
Get fresh Citrus peel clean with the tap water boiling cooling, naturally dry, being crushed to granular size is 20 orders.Take ultrapure water as water source, 5.625g Citrus peel powder is immersed in the water of 125mL, place 24 hours, whizzer is used to carry out centrifugal treating to vat liquor, rotating speed is 5000r/min, removes Citrus peel slag and obtains Citrus peel aqueous extract, with ultrapure water, the volume of extracting solution is adjusted to 125mL; Get extracting solution 3mL ultrapure water or distilled water, boil the tap water of cooling and be diluted to 30mL, this is final flocculation agent; Getting flocculation agent 5mL, to be added to 45 milliliters of concentration of algae be 4.3 × 10 6in the water body of individual/mL, leave standstill 3h, algae is deposited to the bottom, and detecting its alga-killing rate is 82.53%.
Experiment 3
Get fresh Citrus peel clean with the tap water boiling cooling, naturally dry, being crushed to granular size is 80 orders.Take ultrapure water as water source, 11.25g Citrus peel powder is immersed in the water of 62.5mL, place 24 hours, whizzer is used to carry out centrifugal treating to vat liquor, rotating speed is 5000r/min, removes Citrus peel slag and obtains Citrus peel aqueous extract, with ultrapure water, the volume of extracting solution is adjusted to 62.5mL; Get extracting solution 3mL ultrapure water or distilled water, boil the tap water of cooling and be diluted to 30mL, this is final flocculation agent; Getting flocculation agent 5mL, to be added to 45 milliliters of concentration of algae be 5.0 × 10 6in the water body of individual/mL, leave standstill 3h, part algae is deposited to the bottom, and detecting its alga-killing rate is 23.87%; When the volume of vat liquor is increased to 125 milliliters, its alga-killing rate is 94.52%.
Experiment 4
Get fresh Citrus peel clean with the tap water boiling cooling, naturally dry, being crushed to granular size is 80 orders.Take ultrapure water as water source, 5.625g Citrus peel powder is immersed in the water of 125mL, place 24 hours, whizzer is used to carry out centrifugal treating to vat liquor, rotating speed is 1000r/min, removes Citrus peel slag and obtains Citrus peel aqueous extract, with ultrapure water, the volume of extracting solution is adjusted to 125mL; Get extracting solution 3mL ultrapure water or distilled water, boil the tap water of cooling and be diluted to 30mL, this is final flocculation agent; Getting flocculation agent 5mL, to be added to 45 milliliters of concentration of algae be 5.9 × 10 6in the water body of individual/mL, leave standstill 3h, algae is deposited to the bottom, and detecting its alga-killing rate is 85.08%.
Experiment 5
Get fresh Citrus peel clean with the tap water boiling cooling, naturally dry, being crushed to granular size is 80 orders.Take ultrapure water as water source, 5.625g Citrus peel powder is immersed in the water of 125mL, place 24 hours, whizzer is used to carry out centrifugal treating to vat liquor, rotating speed is 3000r/min, removes Citrus peel slag and obtains Citrus peel aqueous extract, with ultrapure water, the volume of extracting solution is adjusted to 125mL; Get extracting solution 3mL ultrapure water or distilled water, boil the tap water of cooling and be diluted to 30mL, this is final flocculation agent; Getting flocculation agent 5mL, to be added to 45 milliliters of concentration of algae be 6.1 × 10 6in the water body of individual/mL, leave standstill 3h, algae is deposited to the bottom, and detecting its alga-killing rate is 97.42%; When by flocculation agent with 0.22 μm of membrane filtration after carry out floc test again, its alga-killing rate reduces to 75.17%.

Claims (8)

1. from Citrus peel, extract a method for natural flocculation activity composition, comprise step as follows:
(1) by pretreated Citrus peel and ultrapure water, distilled water or boil cooling tap water according to quality: volume ratio is the ratio mixing of 1:2.78 ~ 33.33;
(2) vat liquor is processed, remove Citrus peel slag and obtain Citrus peel aqueous extract.
2. the method extracting natural flocculation activity composition from Citrus peel according to claim 1, it is characterized in that: described pretreated step comprises Citrus peel cleaning, the process of drying or drying, pulverizing: Citrus peel is clean with the tap water or ultrapure water boiling cooling, naturally dry or drying and processing 2 ~ 4 days under 40 ~ 60 DEG C of conditions, obtain dry Citrus peel material, being then crushed to granular size is 20 ~ 80 orders.
3. the method extracting natural flocculation activity composition from Citrus peel according to claim 1 and 2, it is characterized in that: in step (1), places 0.5 ~ 48 hour after Citrus peel and ultrapure water, distilled water or the tap water boiling cooling mix, with the abundant stripping of activeconstituents contained by promoting in Citrus peel.
4. the method extracting natural flocculation activity composition from Citrus peel according to claim 3, it is characterized in that: in step (2), use whizzer to process vat liquor, remove Citrus peel slag and obtain after Citrus peel aqueous extract again through 0.45 μm or 0.22 μm of membrane filtration.
5. the method extracting natural flocculation activity composition from Citrus peel according to claim 4, is characterized in that: centrifuge speed controls at 1000 ~ 9000r/min.
6. utilize the natural flocculation activity composition extracted from Citrus peel described in claim 1 to prepare a method for algicide, it is characterized in that: gained Citrus peel aqueous extract 0.5 ~ 10mL ultrapure water, distilled water or the tap water that boils cooling are diluted to 30mL.
7. utilizing the natural flocculation activity composition extracted from Citrus peel described in claim 1 to prepare algicide and a method for removing algae in water, it is characterized in that:
1) gained Citrus peel aqueous extract 0.5 ~ 10mL ultrapure water, distilled water or the tap water that boils cooling are diluted to 30mL, obtained flocculation agent finished product;
2) add in algae-containing water by described flocculation agent, leave standstill 3 ~ 4 hours, to make the algae in flocculation agent and water react, the flco of generation fully precipitates, thus removes algae from water.
8. the natural flocculation activity composition extracted from Citrus peel according to claim 7 prepares algicide and method for removing algae in water, it is characterized in that: be determined by experiment flocculant usage according to frustule quantity in water body.
CN201510558579.8A 2015-09-06 2015-09-06 Natural flocculation activity composition is extracted from Citrus peel, algicide is prepared and its method for going algae in water removal Expired - Fee Related CN105129949B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106614768A (en) * 2016-12-26 2017-05-10 河南城建学院 Method for extracting algal-inhibition active component from herba portulacae seeds and using same for preparing algistat

Citations (3)

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Publication number Priority date Publication date Assignee Title
US4455245A (en) * 1982-02-19 1984-06-19 Klein Pearl M Flocculating reagent
CN103539248A (en) * 2013-11-15 2014-01-29 陕西延长石油油田化学科技有限责任公司 Method for preparing environment-friendly flocculating agent from waste fruit peels and application of environment-friendly flocculating agent
CN103588890A (en) * 2013-11-15 2014-02-19 西安石油大学 Modification method of citrus peel and application of citrus peel in drilling fluid treatment

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4455245A (en) * 1982-02-19 1984-06-19 Klein Pearl M Flocculating reagent
CN103539248A (en) * 2013-11-15 2014-01-29 陕西延长石油油田化学科技有限责任公司 Method for preparing environment-friendly flocculating agent from waste fruit peels and application of environment-friendly flocculating agent
CN103588890A (en) * 2013-11-15 2014-02-19 西安石油大学 Modification method of citrus peel and application of citrus peel in drilling fluid treatment

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106614768A (en) * 2016-12-26 2017-05-10 河南城建学院 Method for extracting algal-inhibition active component from herba portulacae seeds and using same for preparing algistat
CN106614768B (en) * 2016-12-26 2019-03-15 河南城建学院 The method extracted algistatic activity ingredient from purslane seed and be used to prepare algae-inhibiting agent

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