CN106396068B - The preparation method and applications of polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod composite flocculation agent - Google Patents
The preparation method and applications of polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod composite flocculation agent Download PDFInfo
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- CN106396068B CN106396068B CN201610515295.5A CN201610515295A CN106396068B CN 106396068 B CN106396068 B CN 106396068B CN 201610515295 A CN201610515295 A CN 201610515295A CN 106396068 B CN106396068 B CN 106396068B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/11—Turbidity
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Organic Chemistry (AREA)
- Graft Or Block Polymers (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of preparation method and applications of polymer/metallic base vinyl pyrrolidone ionic liquid grafting concave convex rod composite flocculation agent, the preparation method is that: to be grafted on the functional metal base vinylpyrrolidone ionic liquid on concave convex rod surface as monomer, with N, N'- methylene-bisacrylamide is crosslinking agent, and in-situ polymerization is grafted concave convex rod composite flocculation agent at polymer/metallic base vinylpyrrolidone ionic liquid and is used among sewage treatment under the action of initiator.It is an advantage of the invention that, preparation method is simple, raw material is cheap and easily-available, simple production process, and is using covalently key connection between ionic liquid and concave convex rod, in conjunction with than stronger, it not easily runs off, is a kind of compound powerful flocculation material, the processing for sanitary sewage, COD removal rate reaches 85-98%, turbidity removal rate 85%-95%.
Description
Technical field
The invention belongs to water-treatment technology fields, and in particular to a kind of polymer/metallic base vinylpyrrolidone ionic liquid connects
The preparation method and applications of branch concave convex rod composite flocculation agent.
Background technique
Attapulgite also known as palygorskite are a kind of natural non-metallic clay minerals, are mineralogically under the jurisdiction of sepiolite.It is recessed
Convex stick local products have many special excellent performances, with adsorbent, binder, auxiliary agent, add under special geological conditions
The forms such as agent, catalyst carrier are added to be widely used in the industries such as decoloration and water process, building materials, light industry, weaving, geological prospecting.
In recent years, the unique structure of clay mineral and absorption property and be widely used in sewage treatment.Palygorskite is viscous
Soil is due to its hollow structure and bigger serface, so that it has good adsorption capacity and ion-exchange capacity, and its valence
Lattice are cheap, and the storage capacity verified is big, cleanliness without any pollution, are a kind of environmental-friendly adsorbents with fine development prospect.About
There are many report of palygorskite clay adsorption treatment waste water, but palygorskite clay makes it in the later period due to its stable colloid property
Separation process is very troublesome.
Polyvinylpyrrolidone (PVP) is main water soluble polymer fine chemicals, due to it have it is excellent molten
The advantages that Xie Xing, film forming, dispersion stabilization, physiological compatibility, be widely used with medical and health, daily-use chemical industry, do
The key areas such as utility, textile and dyeing industry.Cross-linked pvp has good adsorption capacity for solids, different
In dispersion, the cross-linked pvp of different crosslinking degrees can be used as dispersing agent, thickener and flocculant, in ink, drug, change
There is important purposes in the fields such as cosmetic.
FeCl3It is the inorganic flocculating agent most generallyd use, Fe3+Addition, first is that the zeta potential of suspended solid particles can be made
It reduces, as a result makes to flocculate between coagulated particles；Second is that Fe3+Hydrolysis, increases the quantity of solid particle, to increase sludge granules
Probability is collided, flocculating degree is improved.
Summary of the invention
According to the deficiencies of the prior art described above, It is an object of the present invention to provide a kind of polymer/metallic base vinyl pyrrolidines
Ketone ionic liquid is grafted the preparation method and applications of concave convex rod composite flocculation agent, and the preparation method is to be grafted on concave convex rod surface
Functional metal base vinylpyrrolidone ionic liquid be monomer, in-situ polymerization is at poly- under the action of crosslinking agent and initiator
It closes Metal Substrate vinylpyrrolidone ionic liquid and is grafted concave convex rod composite flocculation agent, and be used for sewage treatment.
The object of the invention realization is completed by following technical scheme:
A kind of preparation method of polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod composite flocculation agent, it is special
Sign be the preparation method is that: be single to be grafted on the functional metal base vinylpyrrolidone ionic liquid on concave convex rod surface
Body, with N, N'- methylene-bisacrylamide is crosslinking agent, and in-situ polymerization is at polymer/metallic base ethylene pyrrole under the action of initiator
Pyrrolidone ionic liquid is grafted concave convex rod composite flocculation agent.
The preparation method is that: vinylpyrrolidone (NVP) is mixed instead with 3- chloropropyl triethoxysilane (3-CTS)
Answer systematic function ionic liquid ([NVP-CTS] Cl-)；In functionalized ion liquid ([NVP-CTS] Cl-) in be added tri-chlorination
Iron (FeCl3), prepare Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl4 -)；Using ethyl alcohol as solvent, after acidification
Concave convex rod (ATTP) and Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl4 -) it is added thereto reaction, institute is then added
Initiator and the crosslinking agent are stated, crosslinks polymerization reaction at a certain temperature, preparation generates polymer/metallic base ethylene pyrrole
Pyrrolidone ionic liquid is grafted concave convex rod composite flocculation agent (P [NVP-CTS] FeCl4 -/ ATTP).
The preparation method includes the following steps:
(1) solvent is added in vinylpyrrolidone (NVP) and 3- chloropropyl triethoxysilane (3-CTS), certain
Under reaction temperature and nitrogen protection, react 22-26 hours；Solvent is removed in decompression, and successively carries out ethyl acetate and ethanol washing,
35-45 DEG C of vacuum drying, obtains functionalized ion liquid ([NVP-CTS] Cl-)；
(2) by ferric trichloride (FeCl3) functionalized ion liquid ([NVP-CTS] Cl is added-) in, it is stirring while adding, in nitrogen
Under gas shielded, reacts 22-26 hours, obtain Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl4 -)；
(3) using ethyl alcohol as solvent, the concave convex rod (ATTP) after acidification is added thereto, ultrasonic disperse 8-12 min, then
Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl is added4 -), ultrasonic 25-35 min, heating stirring reflux 22-26h, from
So cooling, ethanol washing washes away unreacted reactant, spare；Using toluene as initiator, N, N'- methylene-bisacrylamide
Be added thereto for crosslinking agent, nitrogen protection and 65-85 DEG C at a temperature of, react 22-26 hour, filtering, alcohol filter wash cake is dry
Dry, grinding obtains polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod composite flocculation agent (P [NVP-CTS]
FeCl4 -/ ATTP).
The molar ratio of vinylpyrrolidone (NVP) and 3- chloropropyl triethoxysilane (3-CTS) is 1:1.
The reaction temperature of vinylpyrrolidone (NVP) and 3- chloropropyl triethoxysilane (3-CTS) is 60-100 DEG C.
Functionalized ion liquid ([NVP-CTS] Cl-) and ferric trichloride (FeCl3) molar ratio be 1:5~1:1.
Concave convex rod (ATTP) and Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl4 -) mass ratio be 1:1~20:
1。
The initiator is any one in azodiisobutyronitrile, ammonium persulfate, potassium peroxydisulfate and benzoyl peroxide
Or it is two or more.
Described Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl4 -) it with the mass ratio of the initiator is 200:1
~100:1, described Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl4 -) it with the mass ratio of the crosslinking agent is 100:1
~10:1
It is a kind of to be related to any above-mentioned polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod composite flocculation agent
Using, it is characterised in that the polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod composite flocculation agent is used for sewage
Processing.
It is an advantage of the invention that preparation method is simple, raw material is cheap and easily-available, simple production process；Polymeric ionic liquid and
It not easily runs off in conjunction with than stronger using covalently key connection between concave convex rod, combines the property of each monomer, but not
Be several substances simple physical it is compound because being in-situ polymerization, by adjust crosslinking agent dosage, it is adjustable solid netted
Structure increases adsorption site, the molecular gap of simple polyvinyl pyrrolidone is also enhanced, pyrrolidones and polyacrylamide
The flocculating property of amine is combined together, characteristic and inorganic FeCl along with the zwitterion of ionic liquid3Flocculability, then
In conjunction with the adsorptivity of concave convex rod, at the same also have it is amphipathic, so material flocculating effect is good, reunion speed is fast, and wadding body is big, sedimentation
Speed is fast, is a compound powerful flocculation material, for the processing of sanitary sewage, COD removal rate reaches 85-98%, turbid
Degree removal rate is 85%-95%.
Detailed description of the invention
Fig. 1 is the infrared spectrogram in the present invention before and after concave convex rod graft modification；
Fig. 2 is transmission electron microscope (TEM) figure of concave convex rod before modified in the present invention；
Fig. 3 is the transmission electron microscope that polymer/metallic base vinylpyrrolidone ionic liquid is grafted attapulgite clay in the present invention
(TEM) figure.
Specific embodiment
Feature of the invention and other correlated characteristics are described in further detail by embodiment below in conjunction with attached drawing, with
Convenient for the understanding of technical staff of the same trade:
Embodiment 1:
The present embodiment is grafted concave convex rod composite flocculation more particularly to a kind of polymer/metallic base vinylpyrrolidone ionic liquid
The preparation method and applications of agent, specifically comprise the following steps:
(1) preparation of functionalized ion liquid monomer:
In the three-necked flask of 500 ml, be added 11.1g(0.1mol) vinylpyrrolidone (NVP), 24g(0.1mol)
3- chloropropyl triethoxysilane (3-CTS) and the alcohol solvent of 20ml be stirred, in logical nitrogen protection and 80 DEG C
Under the conditions of temperature, reaction reflux is for 24 hours；Rotary evaporation alcohol solvent later, and ethyl acetate washing and methanol washing are successively carried out,
Vacuum drying, obtains functionalized ion liquid ([NVP-CTS] Cl of 28g yellow transparent-), yield 80%, reaction principle is as follows:
Functionalized ion liquid ([NVP-CTS] Cl of 28g-) be put into the beaker of 250ml, weigh the tri-chlorination of 13g
Iron (FeCl3) be slowly added into the liquid in beaker, it stirs while adding, leads to nitrogen protection, be stirred to react for 24 hours, obtain metal
Base functionalized ion liquid ([NVP-CTS] FeCl4 -), reaction principle is as follows；
(2) concave convex rod original soil is acidified modified
It takes the concave convex rod original soil of 100g to be added in the 100mL hydrochloric acid solution that concentration is 1mol/L, impregnates for 24 hours, clear water washing
To filtrate neutrality, dry, grinding is spare for filtering；
(3) concave convex rod (ATTP) 10g after taking acidification, is put into the three-necked flask of 500mL, and be added into three-necked flask
10g Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl is added in the toluene of 50mL, stirring thereto again later4 -),
The azodiisobutyronitrile of 0.01g and the N of 0.1g, N'- methylene-bisacrylamide, lead to nitrogen protection, 65 DEG C at a temperature of
React 4h, and 85 DEG C at a temperature of react 20h；Ethanol washing, it is dry, 120 mesh are ground into, it is spare, obtain polymer/metallic base
Vinylpyrrolidone ionic liquid is grafted concave convex rod composite flocculation agent (P [NVP-CTS] FeCl4 -/ ATTP), reaction principle is as follows:
(4) sanitary sewage 100mL is taken, the polymer/metallic base vinylpyrrolidone ionic liquid grafting of 0.1g is added into it
Concave convex rod composite flocculation agent (P [NVP-CTS] FeCl4 -/ ATTP), flocculating effect is observed, flocculation time 1 second, wadding body was big at mung bean
Small, wadding body deposition time is 1min；Detecting supernatant C OD removal rate is 88%, turbidity removal rate 85%.
It is the infrared spectrogram before and after concave convex rod graft modification, 3411cm as shown in Figure 1-1、3615cm-1For palygorskite table
The stretching vibration of face hydroxyl, before and after concave convex rod grafting ion liquid, surface hydroxyl vibration peak obviously weakens, this be silicone hydroxyl and from
Sub- liquid is bonded, and occurs C-H stretching vibration absworption peak on butyrolactam ring in attapulgite material after modification
(2896 cm- 1), 1548~1786 cm-1For the strong absorption band of typical amidocarbonylation, in 1388 cm-1Nearby for
The bending vibration characteristic absorption peak of the connected methylene of nitrogen cation, in 1156cm-1There is Si-O-C characteristic absorption peak.
Be respectively as shown in Figure 2,3 concave convex rod before modified after transmission electron microscope picture, can be seen from the chart, it is concave-convex before modified
Stick is fine acicular structure, and modified concave convex rod is obviously thicker, has wrapped up one layer of polymeric.
Embodiment 2:
The present embodiment is grafted concave convex rod composite flocculation more particularly to a kind of polymer/metallic base vinylpyrrolidone ionic liquid
The preparation method and applications of agent, specifically comprise the following steps:
(1) preparation of functionalized ion liquid monomer:
In the three-necked flask of 500 ml, be added 11.1g(0.1mol) vinylpyrrolidone (NVP), 24g(0.1mol)
3- chloropropyl triethoxysilane (3-CTS) and the alcohol solvent of 20ml be stirred, in logical nitrogen protection and 80 DEG C
Under the conditions of temperature, reaction reflux is for 24 hours；Rotary evaporation alcohol solvent later, and ethyl acetate washing and methanol washing are successively carried out,
Vacuum drying, obtains functionalized ion liquid ([NVP-CTS] Cl of 28g yellow transparent-), yield 80%:
Functionalized ion liquid ([NVP-CTS] Cl of 28g-) be put into the beaker of 250ml, weigh the tri-chlorination of 13g
Iron (FeCl3) be slowly added into the liquid in beaker, it stirs while adding, leads to nitrogen protection, be stirred to react for 24 hours, obtain metal
Base functionalized ion liquid ([NVP-CTS] FeCl4 -)；
(2) concave convex rod original soil is acidified modified
It takes the concave convex rod original soil of 100g to be added in the 100mL hydrochloric acid solution that concentration is 1mol/L, impregnates for 24 hours, clear water washing
To filtrate neutrality, dry, grinding is spare for filtering；
(3) concave convex rod (ATTP) 20g after taking acidification, is put into the three-necked flask of 500mL, and be added into three-necked flask
10g Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl is added in the toluene of 50mL, stirring thereto again later4 -),
The azodiisobutyronitrile of 0.01g and the N of 0.1g, N'- methylene-bisacrylamide, lead to nitrogen protection, 65 DEG C at a temperature of
React 4h, and 85 DEG C at a temperature of react 20h；Ethanol washing, it is dry, 120 mesh are ground into, it is spare, obtain polymer/metallic base
Vinylpyrrolidone ionic liquid is grafted concave convex rod composite flocculation agent (P [NVP-CTS] FeCl4 -/ ATTP):
(4) sanitary sewage 100mL is taken, the polymer/metallic base vinylpyrrolidone ionic liquid grafting of 0.1g is added into it
Concave convex rod composite flocculation agent (P [NVP-CTS] FeCl4 -/ ATTP), flocculating effect is observed, flocculation time 1 second, wadding body was big at soya bean
Small, wadding body deposition time is 40s；Detecting supernatant C OD removal rate is 95%, turbidity removal rate 90%.
Embodiment 3:
The present embodiment is grafted concave convex rod composite flocculation more particularly to a kind of polymer/metallic base vinylpyrrolidone ionic liquid
The preparation method and applications of agent, specifically comprise the following steps:
(1) preparation of functionalized ion liquid monomer:
In the three-necked flask of 500 ml, be added 11.1g(0.1mol) vinylpyrrolidone (NVP), 24g(0.1mol)
3- chloropropyl triethoxysilane (3-CTS) and the alcohol solvent of 20ml be stirred, in logical nitrogen protection and 80 DEG C
Under the conditions of temperature, reaction reflux is for 24 hours；Rotary evaporation alcohol solvent later, and ethyl acetate washing and methanol washing are successively carried out,
Vacuum drying, obtains functionalized ion liquid ([NVP-CTS] Cl of 28g yellow transparent-), yield 80%:
Functionalized ion liquid ([NVP-CTS] Cl of 28g-) be put into the beaker of 250ml, weigh the tri-chlorination of 13g
Iron (FeCl3) be slowly added into the liquid in beaker, it stirs while adding, leads to nitrogen protection, be stirred to react for 24 hours, obtain metal
Base functionalized ion liquid ([NVP-CTS] FeCl4 -)；
(2) concave convex rod original soil is acidified modified
It takes the concave convex rod original soil of 100g to be added in the 100mL hydrochloric acid solution that concentration is 1mol/L, impregnates for 24 hours, clear water washing
To filtrate neutrality, dry, grinding is spare for filtering；
(3) concave convex rod (ATTP) 30g after taking acidification, is put into the three-necked flask of 500mL, and be added into three-necked flask
10g Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl is added in the toluene of 50mL, stirring thereto again later4 -),
The azodiisobutyronitrile of 0.01g and the N of 0.1g, N'- methylene-bisacrylamide, lead to nitrogen protection, 65 DEG C at a temperature of
React 4h, and 85 DEG C at a temperature of react 20h；Ethanol washing, it is dry, 120 mesh are ground into, it is spare, obtain polymer/metallic base
Vinylpyrrolidone ionic liquid is grafted concave convex rod composite flocculation agent (P [NVP-CTS] FeCl4 -/ ATTP):
(4) sanitary sewage 100mL is taken, the polymer/metallic base vinylpyrrolidone ionic liquid grafting of 0.1g is added into it
Concave convex rod composite flocculation agent (P [NVP-CTS] FeCl4 -/ ATTP), flocculating effect is observed, flocculation time 0.5 second, wadding body was in blocks,
Wadding body deposition time is 20s；Detecting supernatant C OD removal rate is 98%, turbidity removal rate 95%.
Embodiment 4:
The present embodiment is grafted concave convex rod composite flocculation more particularly to a kind of polymer/metallic base vinylpyrrolidone ionic liquid
The preparation method and applications of agent, specifically comprise the following steps:
(1) preparation of functionalized ion liquid monomer:
In the three-necked flask of 500 ml, be added 11.1g(0.1mol) vinylpyrrolidone (NVP), 24g(0.1mol)
3- chloropropyl triethoxysilane (3-CTS) and the alcohol solvent of 20ml be stirred, in logical nitrogen protection and 80 DEG C
Under the conditions of temperature, reaction reflux is for 24 hours；Rotary evaporation alcohol solvent later, and ethyl acetate washing and methanol washing are successively carried out,
Vacuum drying, obtains functionalized ion liquid ([NVP-CTS] Cl of 28g yellow transparent-), yield 80%:
Functionalized ion liquid ([NVP-CTS] Cl of 28g-) be put into the beaker of 250ml, weigh the tri-chlorination of 13g
Iron (FeCl3) be slowly added into the liquid in beaker, it stirs while adding, leads to nitrogen protection, be stirred to react for 24 hours, obtain metal
Base functionalized ion liquid ([NVP-CTS] FeCl4 -)；
(2) concave convex rod original soil is acidified modified
It takes the concave convex rod original soil of 100g to be added in the 100mL hydrochloric acid solution that concentration is 1mol/L, impregnates for 24 hours, clear water washing
To filtrate neutrality, dry, grinding is spare for filtering；
(3) concave convex rod (ATTP) 20g after taking acidification, is put into the three-necked flask of 500mL, and be added into three-necked flask
10g Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl is added in the toluene of 50mL, stirring thereto again later4 -),
The azodiisobutyronitrile of 0.01g and the N of 0.1g, N'- methylene-bisacrylamide, lead to nitrogen protection, 65 DEG C at a temperature of
React 4h, and 85 DEG C at a temperature of react 20h；Ethanol washing, it is dry, 120 mesh are ground into, it is spare, obtain polymer/metallic base
Vinylpyrrolidone ionic liquid is grafted concave convex rod composite flocculation agent (P [NVP-CTS] FeCl4 -/ ATTP):
(4) sanitary sewage 100mL is taken, the polymer/metallic base vinylpyrrolidone ionic liquid grafting of 0.2g is added into it
Concave convex rod composite flocculation agent (P [NVP-CTS] FeCl4 -/ ATTP), flocculating effect is observed, flocculation time 1 second, wadding body was big at soya bean
Small, wadding body deposition time is 40s；Detecting supernatant C OD removal rate is 97%, turbidity removal rate 93%.
Claims (9)
1. a kind of preparation method of polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod composite flocculation agent, feature
Be the preparation method is that: be single to be grafted on the functional metal base vinylpyrrolidone ionic liquid on concave convex rod surface
Body, with N, N'- methylene-bisacrylamide is crosslinking agent, and in-situ polymerization is at polymer/metallic base ethylene pyrrole under the action of initiator
Pyrrolidone ionic liquid is grafted concave convex rod composite flocculation agent；The preparation method is that: by vinylpyrrolidone (NVP) with 3- chlorine third
Ethyl triethoxy silicane alkane (3-CTS) hybrid reaction systematic function ionic liquid ([NVP-CTS] Cl-)；In functionalization ionic liquid
Body ([NVP-CTS] Cl-) in be added ferric trichloride (FeCl3), prepare Metal Substrate functionalized ion liquid ([NVP-CTS]
FeCl4 -)；Using ethyl alcohol as solvent, by the concave convex rod (ATTP) and Metal Substrate functionalized ion liquid ([NVP-CTS] after acidification
FeCl4 -) it is added thereto reaction, the initiator and the crosslinking agent is then added, crosslinks polymerization at a certain temperature
Reaction, preparation generate polymer/metallic base vinylpyrrolidone ionic liquid and are grafted concave convex rod composite flocculation agent (P [NVP-CTS]
FeCl4 -/ ATTP).
2. a kind of polymer/metallic base vinylpyrrolidone ionic liquid according to claim 1 is grafted concave convex rod composite flocculation
The preparation method of agent, it is characterised in that the preparation method includes the following steps:
(1) solvent is added in vinylpyrrolidone (NVP) and 3- chloropropyl triethoxysilane (3-CTS), in certain reaction
At temperature and nitrogen protection, react 22-26 hours；Solvent is removed in decompression, and successively carries out ethyl acetate and ethanol washing, 35-45
DEG C vacuum drying, obtain functionalized ion liquid ([NVP-CTS] Cl-)；
(2) by ferric trichloride (FeCl3) functionalized ion liquid ([NVP-CTS] Cl is added-) in, it is stirring while adding, it is protected in nitrogen
Under shield, reacts 22-26 hours, obtain Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl4 -)；
(3) using ethyl alcohol as solvent, the concave convex rod (ATTP) after acidification is added thereto, ultrasonic disperse 8-12 min, is then added
Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl4 -), ultrasonic 25-35 min, heating stirring flow back 22-26h, it is naturally cold
But, ethanol washing washes away unreacted reactant, spare；Using toluene as initiator, N, N'- methylene-bisacrylamide is to hand over
Connection agent is added thereto, nitrogen protection and 65-85 DEG C at a temperature of, react 22-26 hour, filtering, alcohol filter wash cake is dried,
Grinding obtains polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod composite flocculation agent (P [NVP-CTS] FeCl4 -/
ATTP).
3. a kind of polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod according to claim 1 or 2 is compound
The preparation method of flocculant, it is characterised in that vinylpyrrolidone (NVP) and 3- chloropropyl triethoxysilane (3-CTS's) rubs
You are than being 1:1.
4. a kind of polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod according to claim 1 or 2 is compound
The preparation method of flocculant, it is characterised in that vinylpyrrolidone (NVP) and 3- chloropropyl triethoxysilane (3-CTS) it is anti-
Answering temperature is 60-100 DEG C.
5. a kind of polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod according to claim 1 or 2 is compound
The preparation method of flocculant, it is characterised in that functionalized ion liquid ([NVP-CTS] Cl-) and ferric trichloride (FeCl3) mole
Than for 1:5~1:1.
6. a kind of polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod according to claim 1 or 2 is compound
The preparation method of flocculant, it is characterised in that concave convex rod (ATTP) and Metal Substrate functionalized ion liquid ([NVP-CTS]
FeCl4 -) mass ratio be 1:1~20:1.
7. a kind of polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod according to claim 1 or 2 is compound
The preparation method of flocculant, it is characterised in that the initiator is azodiisobutyronitrile, ammonium persulfate, potassium peroxydisulfate and peroxidating
In benzoyl any one or it is two or more.
8. a kind of polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod according to claim 1 or 2 is compound
The preparation method of flocculant, it is characterised in that described Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl4 -) draw with described
The mass ratio for sending out agent is 200:1~100:1, described Metal Substrate functionalized ion liquid ([NVP-CTS] FeCl4 -) and the friendship
The mass ratio for joining agent is 100:1~10:1.
9. it is multiple that one kind is related to any polymer/metallic base vinylpyrrolidone ionic liquid grafting concave convex rod in claim 1-8
Close the application of flocculant, it is characterised in that the polymer/metallic base vinylpyrrolidone ionic liquid is grafted concave convex rod composite flocculation
Agent is used for sewage treatment.
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| CN113244954B (en) * | 2021-05-20 | 2023-03-21 | 贵州大学 | Preparation method and application of olefin oxidation carboxylation heterogeneous catalyst |
| CN114159575B (en) * | 2022-01-10 | 2024-02-02 | 西北师范大学 | Domperidone sustained release preparation and sustained release carrier |
| CN115193418B (en) * | 2022-07-26 | 2023-09-26 | 西北师范大学 | Preparation method of polyion liquid/attapulgite hybrid material and application of polyion liquid/attapulgite hybrid material in adsorption of p-nitrophenol |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000073596A1 (en) * | 1999-05-26 | 2000-12-07 | Alberta Research Council Inc. | Reinforced networked polymer/clay alloy composite |
| CN102847533A (en) * | 2012-10-12 | 2013-01-02 | 南京师范大学 | Microwave method for synthesizing attapulgite and palladium nanocomposite catalyst |
| CN102897879A (en) * | 2012-09-26 | 2013-01-30 | 暨南大学 | Inorganic-organic composite flocculant, preparation method and application thereof |
| CN103623787A (en) * | 2013-11-15 | 2014-03-12 | 西北师范大学 | Preparation method of acrylic acid/polyvinylpyrrolidone/palygorskite composite adsorbing material |
| CN104190353A (en) * | 2014-08-06 | 2014-12-10 | 明光市国星凹土有限公司 | Modified attapulgite adsorbent for defluorination and preparation method of modified attapulgite adsorbent |
| CN104275161A (en) * | 2014-11-07 | 2015-01-14 | 中国科学院兰州化学物理研究所 | Granular cationic dye adsorbent and preparation method thereof |
| CN104399527A (en) * | 2014-11-12 | 2015-03-11 | 淮阴师范学院 | Preparation method of attapulgite/polymerized ionic liquid composite catalyst |
| CN104828918A (en) * | 2015-05-06 | 2015-08-12 | 海南大学 | Inorganic-organic covalent hybrid flocculant and preparation method thereof |
-
2016
- 2016-07-04 CN CN201610515295.5A patent/CN106396068B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000073596A1 (en) * | 1999-05-26 | 2000-12-07 | Alberta Research Council Inc. | Reinforced networked polymer/clay alloy composite |
| CN102897879A (en) * | 2012-09-26 | 2013-01-30 | 暨南大学 | Inorganic-organic composite flocculant, preparation method and application thereof |
| CN102847533A (en) * | 2012-10-12 | 2013-01-02 | 南京师范大学 | Microwave method for synthesizing attapulgite and palladium nanocomposite catalyst |
| CN103623787A (en) * | 2013-11-15 | 2014-03-12 | 西北师范大学 | Preparation method of acrylic acid/polyvinylpyrrolidone/palygorskite composite adsorbing material |
| CN104190353A (en) * | 2014-08-06 | 2014-12-10 | 明光市国星凹土有限公司 | Modified attapulgite adsorbent for defluorination and preparation method of modified attapulgite adsorbent |
| CN104275161A (en) * | 2014-11-07 | 2015-01-14 | 中国科学院兰州化学物理研究所 | Granular cationic dye adsorbent and preparation method thereof |
| CN104399527A (en) * | 2014-11-12 | 2015-03-11 | 淮阴师范学院 | Preparation method of attapulgite/polymerized ionic liquid composite catalyst |
| CN104828918A (en) * | 2015-05-06 | 2015-08-12 | 海南大学 | Inorganic-organic covalent hybrid flocculant and preparation method thereof |
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