CN105540804A - Method for using camellia oleifera extract product for preparing cationic flocculant - Google Patents

Method for using camellia oleifera extract product for preparing cationic flocculant Download PDF

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Publication number
CN105540804A
CN105540804A CN201510960797.4A CN201510960797A CN105540804A CN 105540804 A CN105540804 A CN 105540804A CN 201510960797 A CN201510960797 A CN 201510960797A CN 105540804 A CN105540804 A CN 105540804A
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add
extract
camellia oleifera
cationic flocculant
oil
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CN105540804B (en
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卢玉栋
周婷
黄雅卿
游瑞云
吴长机
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Fujian Normal University
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Fujian Normal University
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    • 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
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • 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
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5263Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
    • 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
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56Macromolecular compounds

Abstract

The present invention discloses a method for using a camellia oleifera fruit shell extract product for preparing a cationic flocculant, and belongs to the field of fine chemical products. The technical solution is as follows: weighing acrylamide to put into a reaction vessel, adding distilled water, warming to 80-90 DEG C, stirring, adding 2-5% of potassium persulfate, and stirring at 80-90 DEG C for reaction for 1.0-2.5h; adding the camellia oleifera fruit shell extract product to put into the reaction vessel, stirring at 80-90 DEG C for reaction for 1.5-2h; adding dimethyl diallyl ammonium chloride monomers and potassium persulfate into the reaction vessel, stirring at 80 DEG C for reaction for 2-3h, and drying and crushing to obtain the camellia oleifera fruit shell extract product flocculant. The camellia oleifera fruit shell extract product flocculant is prepared from waste camellia oleifera fruit shell as a raw material, the raw material is widely available and inexpensive, and the method is conducive to the comprehensive utilization of the camellia oleifera fruit shell, and reduces waste discharges. The camellia oleifera fruit shell extract product flocculant is used for urban inland river sewage flocculation, sewage turbidity is decreased by 80 to 96%, and the camellia oleifera fruit shell extract product flocculant has good turbidity reducing and decontamination effects.

Description

A kind of method utilizing oil tea extract to prepare cationic flocculant
Technical field
The present invention discloses a kind of method utilizing oil-tea camellia husks extract to prepare cationic flocculant, belongs to Field of Fine Chemicals.
Background technology
Flocculence applies one of the most general method in wastewater treatment, has the feature of the simple and low cost of technique.In current industry, widely used flocculation agent mainly contains inorganic flocculating agent and organic synthesis polymeric flocculant.Inorganic flocculating agent dosage is large, and sludge quantity is large; Organic synthesis polymeric flocculant price is high, is difficult to biological degradation, and the monomer that part remains is poisonous, is restricted in the waste water treatment applications of reality.
Oil tea is the distinctive woody oleiferous plants of China, and according to statistics, national existing oil tea area more than 347 ten thousand hectares, produces tea seed 56,600,000,000 kg per year, about 30,000,000,000 kg of oil-tea camellia husks.But a large amount of oil-tea camellia husks is taken as fuel or is used as fertilizer, causing the great wasting of resources and environmental pollution, if be prepared into flocculation agent, will be a kind of important material, the benefit of oil tea plantation can be improved simultaneously, there is good ecnomics and enviroment meaning.
Summary of the invention
The invention provides a kind of method utilizing oil tea extract to prepare cationic flocculant, have nontoxic, environmental friendliness, without potential safety hazard, and with low cost, the feature such as in water residual rate is low.
To achieve these goals, present invention employs following technical scheme:
Take acrylamide in reactor, add the distilled water that consumption is acrylamide 5 ~ 6 times, be warming up to 80 ~ 90 DEG C, stir 2 ~ 5% Potassium Persulphates that add-on accounts for acrylamide weight, stirring reaction 1.0 ~ 2.5h at 80 ~ 90 DEG C; Add-on accounts for the oil-tea camellia husks extract (content of polyphenol is 50-85%) of 2 ~ 3 times of acrylamide weight in reactor, stirring reaction 1.5 ~ 2h at 80 ~ 90 DEG C; Add-on accounts for the Potassium Persulphate that the dimethyldiallylammonchloride chloride monomer of 50 ~ 100% of acrylamide weight and consumption are 0.5 ~ 0.75% of acrylamide weight in a kettle., stirring reaction 2 ~ 3h at 80 DEG C, namely drying and crushing obtains oil-tea camellia husks extract flocculation agent.
Oil-tea camellia husks extract of the present invention utilizes the ethanol of 30% mass concentration for Extraction solvent, to extract obtain according to solid-liquid ratio 5:1 at the temperature of 60 degree.
Dimethyldiallylammonchloride chloride monomer of the present invention, purchased from Shandong Lu Yue Chemical Co., Ltd..
Oil-tea camellia husks extract flocculation agent the present invention prepared, for the flocculation of city inland river sewage, the turbidity of sewage declines 80 ~ 96%, has the good effect of falling turbid decontamination.Concrete correlation data is as follows:
Sample 1 Sample 2 Sample 3 Sample 4
Before process (NTU) 28 28 28 28
After process (NTU) 1.5 1.7 1.4 1.3
Sorbent material of the present invention compared with prior art, has following advantage:
(1) the present invention utilizes waste oil-tea camellia husks for raw materials, and wide material sources are cheap; Be conducive to the comprehensive utilization of oil-tea camellia husks, reduce the discharge of refuse.
(2) preparation technology of the present invention is simple, mild condition, cost are lower, the advantages such as easy degraded, use safety.
(3) to have flocculating effect good for flocculation agent of the present invention, and wadding aggressiveness consolidation, in water, residual rate is low, nontoxic, environmental friendliness, without features such as potential safety hazards.
Embodiment
Below by embodiment, technical scheme of the present invention is done more specifically bright.
Embodiment 1
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 50 kilograms, is warming up to 80 DEG C, stirs the Potassium Persulphate adding 0.3 kilogram, stirring reaction 2h at 85 DEG C; Add the oil-tea camellia husks extract of 28 kilograms, stirring reaction 1h at 80 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 6 kilograms and the Potassium Persulphate of 0.05 kilogram, stirring reaction 2.5h at 80 DEG C, namely drying and crushing obtains cationic flocculant.
Get the inland river sewage 1000ml that turbidity is the prompt river, Taijiang District, Fuzhou City at ebb tide three of 35NUT, add biomass flocculation agent 50 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Be separated and adopt turbidometer to measure upper strata water body afterwards, its turbidity is 1.8NUT, compared with the turbidity of former state basis, have dropped 95%.
Embodiment 2
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 60 kilograms, is warming up to 90 DEG C, stirs the Potassium Persulphate adding 0.35 kilogram, stirring reaction 2h at 80 DEG C; Add the oil-tea camellia husks extract of 25 kilograms, stirring reaction 1.5h at 85 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 6.5 kilograms and the Potassium Persulphate of 0.05 kilogram, stirring reaction 2.5h at 80 DEG C, namely drying and crushing obtains cationic flocculant.
Get the inland river sewage 1000ml that turbidity is the prompt river, Taijiang District, Fuzhou City at ebb tide three of 35NUT, add biomass flocculation agent 50 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Be separated and adopt turbidometer to measure upper strata water body afterwards, its turbidity is 2.7NUT, compared with the turbidity of former state basis, have dropped 92%.
Embodiment 3
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 50 kilograms, is warming up to 85 DEG C, stirs the Potassium Persulphate adding 0.4 kilogram, stirring reaction 2h at 80 DEG C; Add the oil-tea camellia husks extract of 28 kilograms, stirring reaction 2h at 90 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 7.5 kilograms and the Potassium Persulphate of 0.05 kilogram, stirring reaction 3h at 80 DEG C, namely drying and crushing obtains cationic flocculant.
Get the inland river sewage 1000ml that turbidity is the prompt river, Taijiang District, Fuzhou City at ebb tide three of 35NUT, add biomass flocculation agent 50 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Be separated and adopt turbidometer to measure upper strata water body afterwards, its turbidity is 1.3NUT, compared with the turbidity of former state basis, have dropped 96%.
Embodiment 4
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 50 kilograms, is warming up to 90 DEG C, stirs the Potassium Persulphate adding 0.4 kilogram, stirring reaction 2h at 90 DEG C; Add the oil-tea camellia husks extract of 27.5 kilograms, stirring reaction 1h at 90 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 5.5 kilograms and the Potassium Persulphate of 0.05 kilogram, stirring reaction 2h at 90 DEG C, namely drying and crushing obtains cationic flocculant.
Get turbidity be 415NUT Jinan District, Fuzhou City south waterways, east gate, building materials market in sewage 1000ml, add biomass flocculation agent 60 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Adopt turbidometer to measure upper strata water body after being separated levels, its turbidity is 17NUT, compared with the turbidity of former state basis, have dropped 96%.
Embodiment 5
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 55 kilograms, is warming up to 80 DEG C, stirs the Potassium Persulphate adding 0.45 kilogram, stirring reaction 2h at 80 DEG C; Add the oil-tea camellia husks extract of 27.5 kilograms, stirring reaction 1h at 80 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 5.5 kilograms and the Potassium Persulphate of 0.05 kilogram, at 80 DEG C, stirring reaction 2h, obtains cationic flocculant.
Get turbidity be 415NUT Jinan District, Fuzhou City south waterways, east gate, building materials market in sewage 1000ml, add biomass flocculation agent 60 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Adopt turbidometer to measure upper strata water body after being separated levels, its turbidity is 15NUT, compared with the turbidity of former state basis, have dropped 96%.
Embodiment 6
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 55 kilograms, is warming up to 90 DEG C, stirs the Potassium Persulphate adding 0.45 kilogram, stirring reaction 2h at 90 DEG C; Add the oil-tea camellia husks extract of 28.5 kilograms, stirring reaction 1h at 80 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 6.5 kilograms and the Potassium Persulphate of 0.05 kilogram, at 80 DEG C, stirring reaction 2.5h, obtains cationic flocculant.
Get turbidity be 415NUT Jinan District, Fuzhou City south waterways, east gate, building materials market in sewage 1000ml, add biomass flocculation agent 60 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Adopt turbidometer to measure upper strata water body after being separated levels, its turbidity is 15NUT, compared with the turbidity of former state basis, have dropped 96%.
Embodiment 7
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 55 kilograms, is warming up to 90 DEG C, stirs the Potassium Persulphate adding 0.25 kilogram, stirring reaction 2h at 90 DEG C; Add the oil-tea camellia husks extract of 28.5 kilograms, stirring reaction 1h at 80 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 6.5 kilograms and the Potassium Persulphate of 0.05 kilogram, at 80 DEG C, stirring reaction 2.5h, obtains cationic flocculant.
Get the stream 1000ml in Minhou, Fuzhou City Xi Yuanjiang that turbidity is 28NUT, add biomass flocculation agent 50 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Adopt turbidometer to measure upper strata water body after being separated levels, its turbidity is 2.5NUT, compared with the turbidity of former state basis, have dropped 91%.
Embodiment 8
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 57.5 kilograms, is warming up to 90 DEG C, stirs the Potassium Persulphate adding 0.25 kilogram, stirring reaction 2h at 90 DEG C; Add the oil-tea camellia husks extract of 28 kilograms, stirring reaction 1h at 80 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 6.5 kilograms and the Potassium Persulphate of 0.05 kilogram, at 80 DEG C, stirring reaction 2.5h, obtains cationic flocculant.
Get the stream 1000ml in Minhou, Fuzhou City Xi Yuanjiang that turbidity is 28NUT, add biomass flocculation agent 50 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Adopt turbidometer to measure upper strata water body after being separated levels, its turbidity is 2.8NUT, compared with the turbidity of former state basis, have dropped 90%.
Embodiment 9
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 55 kilograms, is warming up to 90 DEG C, stirs the Potassium Persulphate adding 0.4 kilogram, stirring reaction 2h at 90 DEG C; Add the oil-tea camellia husks extract of 28 kilograms, stirring reaction 1h at 80 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 8.5 kilograms and the Potassium Persulphate of 0.05 kilogram, at 80 DEG C, stirring reaction 3h, obtains cationic flocculant.
Get the stream 1000ml in Minhou, Fuzhou City Xi Yuanjiang that turbidity is 28NUT, add biomass flocculation agent 50 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Adopt turbidometer to measure upper strata water body after being separated levels, its turbidity is 1.7NUT, compared with the turbidity of former state basis, have dropped 94%.
Embodiment 10
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 58 kilograms, is warming up to 90 DEG C, stirs the Potassium Persulphate adding 0.375 kilogram, stirring reaction 2h at 90 DEG C; Add the oil-tea camellia husks extract of 29 kilograms, stirring reaction 1h at 80 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 9 kilograms and the Potassium Persulphate of 0.05 kilogram, at 80 DEG C, stirring reaction 3h, obtains cationic flocculant.
Get the river 1000ml that turbidity is the river, Jin An, Jinan District, Fuzhou City of 31NUT, add biomass flocculation agent 60 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Adopt turbidometer to measure upper strata water body after being separated levels, its turbidity is 2.1NUT, compared with the turbidity of former state basis, have dropped 93%.
Embodiment 11
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 55 kilograms, is warming up to 90 DEG C, stirs the Potassium Persulphate adding 0.375 kilogram, stirring reaction 2h at 90 DEG C; Add the oil-tea camellia husks extract of 29 kilograms, stirring reaction 1h at 80 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 8.5 kilograms and the Potassium Persulphate of 0.05 kilogram, at 80 DEG C, stirring reaction 3h, obtains cationic flocculant.
Get the river 1000ml that turbidity is the river, Jin An, Jinan District, Fuzhou City of 31NUT, add biomass flocculation agent 60 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Adopt turbidometer to measure upper strata water body after being separated levels, its turbidity is 2.4NUT, compared with the turbidity of former state basis, have dropped 92%.
Embodiment 12
The acrylamide taking 10 kilograms, in reactor, adds the distilled water of 50 kilograms, is warming up to 90 DEG C, stirs the Potassium Persulphate adding 0.35 kilogram, stirring reaction 2h at 90 DEG C; Add the oil-tea camellia husks extract of 28 kilograms, stirring reaction 1h at 80 DEG C; Add the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 8 kilograms and the Potassium Persulphate of 0.05 kilogram, at 80 DEG C, stirring reaction 2.5h, obtains cationic flocculant.
Get the river 1000ml that turbidity is the river, Jin An, Jinan District, Fuzhou City of 31NUT, add biomass flocculation agent 60 milligrams prepared by the present embodiment, leave standstill 10 minutes after stirring, the obvious layering of water body, upper strata water body is obviously clarified, the visible flocculating settling thing of lower floor.Adopt turbidometer to measure upper strata water body after being separated levels, its turbidity is 2.8NUT, compared with the turbidity of former state basis, have dropped 91%.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection model of application claims.

Claims (8)

1. utilize oil tea extract to prepare a method for cationic flocculant, it is characterized in that:
Take acrylamide in reactor, add distilled water, be warming up to 80 ~ 90 DEG C, stir again add-on 2 ~ 5% Potassium Persulphate, stirring reaction 1.0 ~ 2.5h at 80 ~ 90 DEG C;
Add oil-tea camellia husks extract in reactor, stirring reaction 1.5 ~ 2h at 80 ~ 90 DEG C; Add dimethyldiallylammonchloride chloride monomer and Potassium Persulphate in a kettle., stirring reaction 2 ~ 3h at 80 DEG C, namely drying and crushing obtains oil-tea camellia husks extract flocculation agent.
2. a kind of method utilizing oil tea extract to prepare cationic flocculant according to claim 1, it is characterized in that described adding distilled water, add-on is acrylamide 5 ~ 6 times.
3. a kind of method utilizing oil tea extract to prepare cationic flocculant according to claim 1, it is characterized in that adding Potassium Persulphate described in step 1), add-on is 2 ~ 5% of acrylamide weight.
4. a kind of method utilizing oil tea extract to prepare cationic flocculant according to claim 1, it is characterized in that described adding oil-tea camellia husks extract, add-on is 2 ~ 3 times of acrylamide weight.
5. a kind of method utilizing oil tea extract to prepare cationic flocculant according to claim 1, it is characterized in that described oil-tea camellia husks extract, its polyphenol content is 50-85%.
6. a kind of method utilizing oil tea extract to prepare cationic flocculant according to claim 1, it is characterized in that described oil-tea camellia husks extract, be utilize the ethanol of mass concentration 30% for Extraction solvent, extract at the temperature of 60 degree according to solid-liquid ratio 5:1 and obtain.
7. a kind of method utilizing oil tea extract to prepare cationic flocculant according to claim 1, is characterized in that step 2) described in add dimethyldiallylammonchloride chloride monomer, add-on is 50 ~ 100% of acrylamide weight.
8. a kind of method utilizing oil tea extract to prepare cationic flocculant according to claim 1, is characterized in that step 2) described in add Potassium Persulphate, its add-on is 0.5 ~ 0.75% of acrylamide weight.
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Publication number Priority date Publication date Assignee Title
CN107474936A (en) * 2017-09-30 2017-12-15 福建师范大学 A kind of pregnant woman's later stage of pregnancy edible oil and its processing technology
CN107494770A (en) * 2017-09-30 2017-12-22 福建师范大学 A kind of pregnant woman oil and its processing technology
CN107502442A (en) * 2017-09-30 2017-12-22 福建师范大学 A kind of pregnant woman's nursing period edible oil and its processing technology
CN107586596A (en) * 2017-09-30 2018-01-16 福建胜华农业科技发展有限公司 A kind of pregnant woman's pregnancy edible oil early stage and its processing technology
CN107670647A (en) * 2017-09-30 2018-02-09 福建省林业科学研究院 A kind of method that adsorbent for heavy metal is prepared using oil-tea camellia husks
CN107694526A (en) * 2017-09-30 2018-02-16 福建省林业科学研究院 Adsorbent prepared by a kind of oil-tea camellia husks extract and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107474936A (en) * 2017-09-30 2017-12-15 福建师范大学 A kind of pregnant woman's later stage of pregnancy edible oil and its processing technology
CN107494770A (en) * 2017-09-30 2017-12-22 福建师范大学 A kind of pregnant woman oil and its processing technology
CN107502442A (en) * 2017-09-30 2017-12-22 福建师范大学 A kind of pregnant woman's nursing period edible oil and its processing technology
CN107586596A (en) * 2017-09-30 2018-01-16 福建胜华农业科技发展有限公司 A kind of pregnant woman's pregnancy edible oil early stage and its processing technology
CN107670647A (en) * 2017-09-30 2018-02-09 福建省林业科学研究院 A kind of method that adsorbent for heavy metal is prepared using oil-tea camellia husks
CN107694526A (en) * 2017-09-30 2018-02-16 福建省林业科学研究院 Adsorbent prepared by a kind of oil-tea camellia husks extract and preparation method thereof
CN107670647B (en) * 2017-09-30 2020-05-22 福建省林业科学研究院 Method for preparing heavy metal ion adsorbent by using camellia oleifera shells

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