CN109265631A - A kind of preparation method of silica solution/silicone modified polyacrylamide heavy metal absorbent - Google Patents
A kind of preparation method of silica solution/silicone modified polyacrylamide heavy metal absorbent Download PDFInfo
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- CN109265631A CN109265631A CN201810978327.4A CN201810978327A CN109265631A CN 109265631 A CN109265631 A CN 109265631A CN 201810978327 A CN201810978327 A CN 201810978327A CN 109265631 A CN109265631 A CN 109265631A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/10—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to inorganic materials
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- Inorganic Chemistry (AREA)
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of silica solution/silicone modified polyacrylamide heavy metal absorbent preparation methods, main points using method are by acrylamide pre-polymerization, again with silica solution/organic-silicon-modified, preparation can be used for removing silica solution/silicone modified polyacrylamide heavy metal absorbent of heavy metal in dyeing waste water.The present invention selects the silica solution/organosilicon with large specific surface area and surface-active, the excellent polyacrylamide heavy metal absorbent of modified processability, the heavy metal in dyeing waste water can be effectively removed, especially to lead, arsenic, cadmium sorption significant effect, and then reduce harm of the heavy metal to natural water, there are important environmental and social benefits.
Description
Technical field
The present invention relates to a kind of preparation method of heavy metal absorbent, in particular to a kind of silica solution/organic-silicon-modified poly-
The preparation method of acrylamide heavy metal absorbent, belongs to field of environment engineering technology.
Background technique
Dyeing waste water is the more serious a kind of waste water of the pollution of textile industry generation, is current most important water pollution
One of source.With the fast development of printing technology, effective improvement of dyeing waste water is received significant attention.
Printing and dyeing enterprise in process of production, is added with the heavy metal object of variety classes and dosage in all kinds of dyestuffs and auxiliary agent
Matter.For dyeing and printing sewage, especially in the case where industrial park centralized processing amount is big, although heavy metal concentration is not high, it is total
Amount but can not look down upon.These heavy metals enter sewage disposal system with dyeing waste water, cause sternly to the biological treatment workshop section of system
Ghost image is rung；Heavy metal cannot be degraded by microorganisms, can only Transport And Transformation, generation point between water, substrate and biology with different valence state
Scattered and enrichment.The structure and function that Heavy Metals in Waters accumulation will result in aquatic ecosystem to a certain extent is impaired very
To collapse.In addition, heavy metal mobility also with higher and lower poisoning concentration, make its pollution have certain concealment
With the property delayed.
Polyacrylamide has preferable stabilization, flocculation, at sewage due to containing a large amount of amide groups in structure
The industries such as reason, oil exploitation, paper industry have been widely used, and are known as the title of " all trades auxiliary agent ".Polyacrylamide is easy to carry out
Chemical modification can prepare functionalized polypropylene amide material, make it have and more be widely applied field.
In removal dyeing waste water heavy metal field, " one kind is by bisphenol-A and three for Chinese patent (CN 201810433655.6)
The application of the preparation method and its absorbing heavy metal ions in water of the rich nitride polyporous material of poly cyanamid polycondensation " passes through will be to bisphenol-A
It is copolymerized in alkaline solution with melamine, canescence porous material PBPAM is generated, using in the porous material absorption sewage
Heavy metal ion achievees the purpose that purify sewage；Chinese patent (CN 201810309359.5) is " at a kind of green printing waste water
Manage agent and preparation method thereof " cucurbit urea groups organic silicon resin, aluminic acid natrium doping attapulgite, Na2Fe04 are adulterated into land plaster
It is mixed with green printing waste water treating agent finished product, has suction-operated to heavy metal ions in wastewater, uses safe green environmental protection；
Chinese patent (CN 201810478642.0) " a kind of preparation method of inorganic heavy metal ion adsorbent material " is using flyash
Heavy metal ion adsorbing material made from carrier and nutrient solution and microorganism mixed fermentation 2 times is had and is inhaled well by raw material
Attached effect；Chinese patent (CN201810358215.9) " a kind of micropore carboxylated silica gel, preparation method and applications " uses silicon
The silica gel absorber of Cheap highly effective is made as material in glue, and for handling the heavy metal ion in waste water, not only method is simply easy
Operation, can be with recycling and reusing.So far, it yet there are no using silica solution/organosilicon as modifying agent, to prepare
Except silica solution/silicone modified polyacrylamide heavy metal absorbent related process technologies of heavy metal in dyeing waste water go out
It is existing.
Conventional polypropylene amide is modified using silica solution/organosilicon, silicon dioxide microparticle and silica micelle
Excessive crosslinking, the polymerization that can prevent acrylamide, are formed with conducive to accommodating and combining the hole of heavy metal ion, increase propylene
The specific surface area of amide polymer, and then increase its adsorption area to heavy metal ion.Silica solution/organosilicon enhances multiple
Condensation material is to the heavy metal in dyeing waste water, and adsorption capacity especially to lead, arsenic, cadmium ion reduces heavy metal to nature
The harm of water body has important environmental and social benefits.
Summary of the invention
For the efficient removal for realizing heavy metal in dyeing waste water, especially lead, arsenic, cadmium ion are effectively removed, this hair
Bright purpose is to provide a kind of preparation method of silica solution/silicone modified polyacrylamide heavy metal absorbent.
To achieve the above object, the technical scheme is that using following steps:
1) appropriate silica solution and organosilicon are dissolved in deionized water, adjust pH value of solution to 6.0, at 30-60 DEG C with dilute hydrochloric acid
Lower mixing 12h, obtains modified silicasol；
2) 5g acrylamide is dissolved in deionized water, a small amount of initiator and crosslinking agent is added, be uniformly mixed, 50-100 DEG C pre-
Modified silicasol obtained in step 1) is added thereto and quickly stirs by poly- 10-40min, reacts 30-70min, obtains transparent
Colloidal sol；
3) vitreosol obtained in step 2) is dried, is cut into bulk, be dried in vacuo, be ground into a powder at 40-90 DEG C,
It is rinsed with deionized water, dries, obtain silica solution/silicone modified polyacrylamide heavy metal absorbent.
The mass fraction of the acrylamide solution is 10-40wt%；The mass fraction of silica solution is 2-10wt%, silicon
The mass ratio of colloidal sol and organosilicon is 1:0.05-0.15；The mass ratio of acrylamide and initiator is 1:0.005-0.015；Third
The mass ratio of acrylamide and crosslinking agent is 1:0.05-0.6.
The organosilicon is vinyltrimethoxysilane, (b- methoxy ethoxy) silane of vinyl three and vinyl
One of triethoxysilane；The initiator is potassium peroxydisulfate and ammonium bisulfite mixed initiator；The crosslinking
Agent is one of methylene diacrylamide and hexa.
Compared with the background art, the invention has the advantages that:
The present invention has selected silica solution/organosilicon with large specific surface area and surface-active, and modified processability is excellent
Different polyacrylamide heavy metal absorbent, greatly improves the suction of heavy metal in dyeing waste water, especially lead, arsenic, cadmium ion
Attached efficiency reduces harm of the heavy metal to natural water, has important environmental and social benefits.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1:
1) it is by silica solution and organosilicon mass ratio by the silica solution of mass fraction 2wt% and vinyltrimethoxysilane
1:0.05 is dissolved in deionized water, adjusts pH value of solution to 6.0 with dilute hydrochloric acid, 12h is mixed at 30 DEG C, it is molten to obtain modified silicon
Glue；
2) 5g acrylamide is dissolved in deionized water, being made into mass fraction is 10wt% solution, by acrylamide and is caused
Agent and crosslinking agent quality are than being respectively that potassium peroxydisulfate and ammonium bisulfite mixed initiator and methene is added in 1:0.005 and 1:0.05
Bisacrylamide crosslinker is uniformly mixed, and modified silicasol obtained in step 1) is added thereto simultaneously by 50 DEG C of pre-polymerization 22min
Quickly stirring reacts 30min, obtains vitreosol；
3) vitreosol obtained in step 2) is dried, is cut into bulk, be dried in vacuo, be ground into a powder at 60 DEG C, used
Deionized water is rinsed, and drying obtains silica solution/silicone modified polyacrylamide heavy metal absorbent (a).
Embodiment 2:
1) by mass fraction be 4wt% silica solution and (b- methoxy ethoxy) silane of vinyl three by silica solution with have
Machine silicon mass ratio is that 1:0.08 is dissolved in deionized water, adjusts pH value of solution to 6.0 with dilute hydrochloric acid, 12h is mixed at 40 DEG C, obtains
To modified silicasol；
2) 5g acrylamide is dissolved in deionized water, being made into mass fraction is 25wt% solution, by acrylamide and is caused
Agent and crosslinking agent quality are than being respectively that potassium peroxydisulfate and ammonium bisulfite mixed initiator and methene is added in 1:0.008 and 1:0.25
Bisacrylamide crosslinker is uniformly mixed, and modified silicasol obtained in step 1) is added thereto simultaneously by 70 DEG C of pre-polymerization 40min
Quickly stirring reacts 60min, obtains vitreosol；
3) vitreosol obtained in step 2) is dried, is cut into bulk, be dried in vacuo, be ground into a powder at 80 DEG C, used
Deionized water is rinsed, and drying obtains silica solution/silicone modified polyacrylamide heavy metal absorbent (b).
Embodiment 3:
1) silica solution and vinyltriethoxysilane that mass fraction is 6wt% are pressed into silica solution and organosilicon mass ratio
It is dissolved in deionized water for 1:0.12, pH value of solution is adjusted to 6.0 with dilute hydrochloric acid, 12h is mixed at 60 DEG C, it is molten to obtain modified silicon
Glue；
2) 5g acrylamide is dissolved in deionized water, being made into mass fraction is 35wt% solution, by acrylamide and is caused
Agent and crosslinking agent quality are than being respectively that potassium peroxydisulfate and ammonium bisulfite mixed initiator and six Asias is added in 1:0.012 and 1:0.45
Tetramine crosslinking agent is uniformly mixed, 90 DEG C of pre-polymerization 10min, modified silicasol obtained in step 1) is added thereto simultaneously fast
Speed stirring, reacts 70min, obtains vitreosol；
3) vitreosol obtained in step 2) is dried, is cut into bulk, be dried in vacuo, be ground into a powder at 40 DEG C, used
Deionized water is rinsed, and drying obtains silica solution/silicone modified polyacrylamide heavy metal absorbent (c).
Embodiment 4:
1) silica solution and vinyltriethoxysilane that mass fraction is 10wt% are pressed into silica solution and organosilicon quality
Than being dissolved in deionized water for 1:0.15, pH value of solution is adjusted to 6.0 with dilute hydrochloric acid, 12h is mixed at 50 DEG C, obtains modified silicon
Colloidal sol；
2) 5g acrylamide is dissolved in deionized water, being made into mass fraction is 40wt% solution, by acrylamide and is caused
Agent and crosslinking agent quality are than being respectively that potassium peroxydisulfate and ammonium bisulfite mixed initiator and six Asias is added in 1:0.015 and 1:0.6
Tetramine crosslinking agent is uniformly mixed, 100 DEG C of pre-polymerization 30min, modified silicasol obtained in step 1) is added thereto simultaneously fast
Speed stirring, reacts 50min, obtains vitreosol；
3) vitreosol obtained in step 2) is dried, is cut into bulk, be dried in vacuo, be ground into a powder at 90 DEG C, used
Deionized water is rinsed, and drying obtains silica solution/silicone modified polyacrylamide heavy metal absorbent (d).
Silica solution/silicone modified polyacrylamide heavy metal absorbent prepared by embodiment 1,2,3,4 applies Mr. Yu
The treatment process of printing and dyeing enterprise waste water, to lead, arsenic, cadmium ion removal rate data, table 1 is to be prepared by embodiment 1,2,3,4 for measurement
Silica solution/silicone modified polyacrylamide heavy metal absorbent handle certain enterprise's dyeing waste water lead, arsenic, cadmium ion removal
Rate measurement result.As seen from Table 1, the silica solution of preparation/silicone modified polyacrylamide heavy metal absorbent is useless to printing and dyeing
Lead ion removal rate is in 93.9-95.7% in water, and arsenic ion removal rate is in 83.8-85.1%, and cadmium ion removal rate is in 90.6-
94.5%, lead, arsenic, cadmium ion removal effect are significant, show the silica solution/silicone modified polyacrylamide heavy metal absorbent
There is preferable treatment effect to the Heavy Metals in removal dyeing waste water, be expected to substitution conventional metals ion adsorbent application
In the wastewater treatment process of printing and dyeing enterprise.
Table 1
The above enumerated are only specific embodiments of the present invention.Present invention is not limited to the above embodiments, can also there are many
Deformation.All deformations that those skilled in the art directly can export or associate from present disclosure, should all
It is considered protection scope of the present invention.
Claims (3)
1. a kind of silica solution/silicone modified polyacrylamide heavy metal absorbent preparation method, which is characterized in that including with
Lower step:
1) appropriate silica solution and organosilicon are dissolved in deionized water, adjust pH value of solution to 6.0 with dilute hydrochloric acid, is mixed at 30-60 DEG C
Stirring 12h is closed, modified silicasol is obtained；
2) 5g acrylamide is dissolved in deionized water, a small amount of initiator and crosslinking agent is added, be uniformly mixed, 50-100 DEG C of pre-polymerization
Modified silicasol obtained in step 1) is added thereto and quickly stirs by 10-40min, reacts 30-70min, obtains transparent molten
Glue；
3) vitreosol obtained in step 2) is dried, is cut into bulk, be dried in vacuo, be ground into a powder at 40-90 DEG C, spend
Ionized water rinses, and drying obtains silica solution/silicone modified polyacrylamide heavy metal absorbent.
2. a kind of preparation of silica solution/silicone modified polyacrylamide heavy metal absorbent according to claim 1
Method, it is characterised in that: the mass fraction of the acrylamide solution is 10-40wt%；The mass fraction of silica solution is 2-
The mass ratio of 10wt%, silica solution and organosilicon is 1:0.05-0.15；The mass ratio of acrylamide and initiator is 1:0.005-
0.015；The mass ratio of acrylamide and crosslinking agent is 1:0.05-0.6.
3. a kind of preparation of silica solution/silicone modified polyacrylamide heavy metal absorbent according to claim 1
Method, it is characterised in that: the organosilicon is vinyltrimethoxysilane, vinyl three (b- methoxy ethoxy) silane
One of with vinyltriethoxysilane；The initiator is potassium peroxydisulfate and ammonium bisulfite mixed initiator；Institute
The crosslinking agent stated is one of methylene diacrylamide and hexa.
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| CN201810978327.4A CN109265631A (en) | 2018-08-26 | 2018-08-26 | A kind of preparation method of silica solution/silicone modified polyacrylamide heavy metal absorbent |
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| CN201810978327.4A CN109265631A (en) | 2018-08-26 | 2018-08-26 | A kind of preparation method of silica solution/silicone modified polyacrylamide heavy metal absorbent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112774642A (en) * | 2020-12-18 | 2021-05-11 | 西南民族大学 | Preparation method of nano magnetic adsorbent with selective adsorption function on Pb (II) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111088A (en) * | 2016-07-11 | 2016-11-16 | 常州大学 | A kind of preparation method of silicon dioxide/cationic-type polyacrylamide hybrid sorbents |
| CN108409901A (en) * | 2018-03-08 | 2018-08-17 | 东南大学 | A kind of Nanometer composite hydrogel and preparation method thereof |
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2018
- 2018-08-26 CN CN201810978327.4A patent/CN109265631A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111088A (en) * | 2016-07-11 | 2016-11-16 | 常州大学 | A kind of preparation method of silicon dioxide/cationic-type polyacrylamide hybrid sorbents |
| CN108409901A (en) * | 2018-03-08 | 2018-08-17 | 东南大学 | A kind of Nanometer composite hydrogel and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| FUQIANG AN等: "Adsorption of aniline from aqueous solution using novel adsorbent PAM/SiO2", 《CHEMICAL ENGINEERING JOURNAL》 * |
| WANG HONGJIE等: "Preparation of organically functionalized silica gel as adsorbent for copper ion adsorption", 《JOURNAL OF ENVIRONMENTAL SCIENCES》 * |
| 李云龙等: "PAM/SiO2磺甲基化改性及吸附重金属离子研究", 《化工新型材料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112774642A (en) * | 2020-12-18 | 2021-05-11 | 西南民族大学 | Preparation method of nano magnetic adsorbent with selective adsorption function on Pb (II) |
| CN112774642B (en) * | 2020-12-18 | 2022-09-16 | 西南民族大学 | Preparation method of nano magnetic adsorbent with selective adsorption function on Pb (II) |
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