CN106268678A - A kind of preparation method of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent - Google Patents

A kind of preparation method of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent Download PDF

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Publication number
CN106268678A
CN106268678A CN201610823848.3A CN201610823848A CN106268678A CN 106268678 A CN106268678 A CN 106268678A CN 201610823848 A CN201610823848 A CN 201610823848A CN 106268678 A CN106268678 A CN 106268678A
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CN
China
Prior art keywords
rhizoma dioscoreae
dioscoreae cirrhosae
preparation
heavy metal
tannin
Prior art date
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Pending
Application number
CN201610823848.3A
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Chinese (zh)
Inventor
陈亮
皮振邦
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FOSHAN RESEARCH INSTITUTE CHINA UNIVERSITY OF GEOSCIENCES
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FOSHAN RESEARCH INSTITUTE CHINA UNIVERSITY OF GEOSCIENCES
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Priority to CN201610823848.3A priority Critical patent/CN106268678A/en
Publication of CN106268678A publication Critical patent/CN106268678A/en
Pending legal-status Critical Current

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Classifications

    • 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
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • 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
    • C02F1/286Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/485Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
    • 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
    • C02F2101/20Heavy metals or heavy metal compounds

Abstract

The invention mainly relates to the preparation method of a kind of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent, the preparation method of described novel Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent, including following step: fresh Rhizoma Dioscoreae Cirrhosae is cleaned peeling, pulverize kept dry standby.Microwave extraction 15min after being added extractant by certain solid-to-liquid ratio and added NaOH adjustment pH, after sucking filtration, rotary evaporation is concentrated to give Rhizoma Dioscoreae Cirrhosae extracting solution, is passed through N2Add a certain amount of cross-linking agent, constant temperature stirring reaction 12h, decompression is distilled off solvent, freeze-dried after modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent.Modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent prepared by the present invention, safe and efficient, the heavy metals such as gold, palladium, lead there are preferable selectivity and higher adsorption capacity, have a wide range of applications in processing heavy metal wastewater thereby.

Description

A kind of preparation method of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent
Technical field
The invention belongs to the extraction of natural product and utilize field, particularly relating to modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal adsorption The preparation method of agent.
Background technology
What in water pollution problems, harm was maximum is heavy metal pollution, and plating, intermetallic composite coating, fertilising, house refuse etc. all may be used It can be the source of heavy metal wastewater thereby.Owing to the toxicity of heavy metal is relatively big, easily it is bioaccumulation.The health of people in serious threat Healthy.The method processing at present heavy metal wastewater thereby mainly has: precipitates and flocculates, absorption method, ion exchange and biological method.
Rhizoma Dioscoreae Cirrhosae has another name called Rhizoma Dioscoreae Cirrhosae, abounds with in China Zhejiang, Guangdong, Guangxi, Sichuan and other places.Shunde utilizes Rhizoma Dioscoreae Cirrhosae liquid to dye Preparing watered gauze, Rhizoma Dioscoreae Cirrhosae tannin content about 20%, contained tannin is condensed type tannin.Ortho position due to the B ring of condensed type tannin Phenolic hydroxyl group can form stable five-membered ring structure, in recent years about preparing tannin resin Adsorption of Heavy Metals with heavy metal ion chelating Document report continue to bring out, but also do not have both at home and abroad the document report utilizing Rhizoma Dioscoreae Cirrhosae tannin to prepare metal absorbent.
Summary of the invention
It is an object of the invention to develop a kind of with low cost, heavy metal and have the modified potato that preferable selectivity, adsorbance are big Liang heavy metal absorbent.
In the present invention, the preparation method of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent comprises the following steps:
(1) fresh Rhizoma Dioscoreae Cirrhosae is cleaned peeling, pulverize kept dry standby.Add 50% ethanol by the solid-to-liquid ratio of 1:40 and add NaOH adjusts pH to about 2 ~ 4, microwave extraction 15min, and after sucking filtration, rotary evaporation is concentrated to give Rhizoma Dioscoreae Cirrhosae extracting solution,
(2) it is passed through N2And add formaldehyde as cross-linking agent,
(3) under conditions of stirring, isothermal reaction 12 hours, temperature controls between 90~110 DEG C, and decompression distillation removes solvent, Modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent is obtained after lyophilization.
State modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent belonging to the present invention and the heavy metals such as gold, palladium, lead are had preferable selectivity Higher adsorption capacity.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described
The preparation of embodiment 1 one kinds modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent comprises the following steps:
(1) fresh Rhizoma Dioscoreae Cirrhosae is cleaned peeling, pulverize kept dry standby.Add 50% ethanol by the solid-to-liquid ratio of 1:40 and add NaOH adjusts pH to 2, microwave extraction 15min, is concentrated to give Rhizoma Dioscoreae Cirrhosae extracting solution after sucking filtration,
(2) it is passed through N2And add formaldehyde as cross-linking agent,
(3) under conditions of stirring, constant temperature 90 DEG C reacts 8 hours, and decompression distillation, except solvent, obtains modified Rhizoma Dioscoreae Cirrhosae single after lyophilization Peaceful heavy metal absorbent.
Embodiment 2: the preparation of a kind of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent comprises the following steps:
(1) fresh Rhizoma Dioscoreae Cirrhosae is cleaned peeling, pulverize kept dry standby.Add 50% ethanol by the solid-to-liquid ratio of 1:40 and add NaOH adjusts pH to 3, microwave extraction 15min, is concentrated to give Rhizoma Dioscoreae Cirrhosae extracting solution after sucking filtration,
(2) it is passed through N2And add formaldehyde as crosslinking,
(3) under conditions of stirring, constant temperature 100 DEG C reacts 8 hours, and decompression distillation, except solvent, obtains modified Rhizoma Dioscoreae Cirrhosae after lyophilization Tannin heavy metal absorbent..
Embodiment 3: the preparation of a kind of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent comprises the following steps:
(1) fresh Rhizoma Dioscoreae Cirrhosae is cleaned peeling, pulverize kept dry standby.Add 50% ethanol by the solid-to-liquid ratio of 1:40 and add NaOH adjusts pH to 4, microwave extraction 15min, is concentrated to give Rhizoma Dioscoreae Cirrhosae extracting solution after sucking filtration,
(2) it is passed through N2And add formaldehyde as cross-linking agent,
(3) under conditions of stirring, constant temperature 110 DEG C reacts 8 hours, and decompression distillation, except solvent, obtains modified Rhizoma Dioscoreae Cirrhosae after lyophilization Tannin heavy metal absorbent.

Claims (7)

1. the preparation method of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent, comprises the following steps:
Fresh Rhizoma Dioscoreae Cirrhosae is cleaned peeling, pulverizes kept dry standby,
Microwave extraction 15min after being added extractant by certain solid-to-liquid ratio and added NaOH adjustment pH, after sucking filtration, rotary evaporation is dense Contract to obtain Rhizoma Dioscoreae Cirrhosae extracting solution, adds a certain amount of cross-linking agent, N2Protection constant temperature stirring reaction 12h, decompression is distilled off solvent, chilled Dried modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent.
2. according to the preparation method described in claim 1, it is characterised in that Rhizoma Dioscoreae Cirrhosae powder and extractant solid-to-liquid ratio are 1:30.
3. according to the preparation method described in claim 1, it is characterised in that the extractant used is ethanol (50:50).
4. according to the preparation method described in claim 1, it is characterised in that cross-linking agent is 37% formaldehyde.
5. according to the preparation method described in claim 1, it is characterised in that before extracting, pH value should be adjusted to about 2 ~ 4.
6. according to the preparation method described in claim 1, it is characterised in that the power of microwave extraction is 150W.
7. according to the preparation method described in claim 1, it is characterised in that reaction temperature control 90~110 DEG C it Between.
CN201610823848.3A 2016-09-16 2016-09-16 A kind of preparation method of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent Pending CN106268678A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610823848.3A CN106268678A (en) 2016-09-16 2016-09-16 A kind of preparation method of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610823848.3A CN106268678A (en) 2016-09-16 2016-09-16 A kind of preparation method of modified Rhizoma Dioscoreae Cirrhosae tannin heavy metal absorbent

Publications (1)

Publication Number Publication Date
CN106268678A true CN106268678A (en) 2017-01-04

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112108124A (en) * 2020-09-26 2020-12-22 江西师范大学 Water body iron and manganese efficient adsorbent and optimization method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5330986A (en) * 1976-09-03 1978-03-23 Nippon Steel Chem Co Ltd Removing method for heavy metals contained in exhaust water
CN102614834A (en) * 2011-01-28 2012-08-01 华中农业大学 Method for adsorbing and recovering heavy metals of lead and copper by persimmon tannin-containing metal adsorbent
CN103736463A (en) * 2014-01-07 2014-04-23 华中农业大学 Modification method and application of metal adsorbent containing persimmon tannin

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5330986A (en) * 1976-09-03 1978-03-23 Nippon Steel Chem Co Ltd Removing method for heavy metals contained in exhaust water
CN102614834A (en) * 2011-01-28 2012-08-01 华中农业大学 Method for adsorbing and recovering heavy metals of lead and copper by persimmon tannin-containing metal adsorbent
CN103736463A (en) * 2014-01-07 2014-04-23 华中农业大学 Modification method and application of metal adsorbent containing persimmon tannin

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112108124A (en) * 2020-09-26 2020-12-22 江西师范大学 Water body iron and manganese efficient adsorbent and optimization method thereof
CN112108124B (en) * 2020-09-26 2023-03-31 江西师范大学 Water body iron and manganese efficient adsorbent and optimization method thereof

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