CN107321330A - Purposes of the PAA acrylamide crosslinking copolymer gel in absorption P elements - Google Patents
Purposes of the PAA acrylamide crosslinking copolymer gel in absorption P elements Download PDFInfo
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- CN107321330A CN107321330A CN201710665767.XA CN201710665767A CN107321330A CN 107321330 A CN107321330 A CN 107321330A CN 201710665767 A CN201710665767 A CN 201710665767A CN 107321330 A CN107321330 A CN 107321330A
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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
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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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
- C02F2101/105—Phosphorus compounds
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The embodiments of the invention provide purposes of the PAA acrylamide crosslinking copolymer in absorption P elements, wherein, PAA acrylamide crosslinking copolymer is formed by sodium acrylate monomers and acrylamide monomer copolymerization, and the mass ratio of the sodium acrylate monomers and acrylamide monomer is less than or equal to 2；PAA acrylamide crosslinking copolymer prepared by the present invention, it can effectively adsorb P elements, after cross-linked copolymer formation hydrogel, there is certain mechanical strength, it is non-breakable, so being easy to separation of solid and liquid, therefore, PAA acrylamide crosslinking copolymer prepared by the present invention is expected to be applied in sewage disposal, adsorbs P elements.
Description
Technical field
The present invention relates to technical field of sewage, more particularly to sodium acrylate-acrylamide crosslink copolymer gel
Purposes in absorption P elements.
Background technology
The sewage disposal of current China is owed based on flocculation sediment and bioanalysis to the treatment effect of the pollutants such as phosphorus nitrogen
It is good：The precipitation method are applied to phosphorous higher sewage, and consumption dosage is larger, and operating cost is higher, and the sludge of generation is further being located
Secondary pollution is likely to result in reason；Bioanalysis is unstable in itself, easily occurs telling phosphorus phenomenon.Other processing methods, such as electrolysis,
A large amount of electrode materials can be consumed and precipitation is produced；Membrane processing method treatment effect is more better, but needs other technologies to be combined, running
It is inconvenient.By contrast, absorption method is ideal dephosphorization means.Make phosphorus attached on surface using the bigger serface of adsorbent
, the sludge of generation is few, equipment is simple, and phosphor-removing effect is more stable.Some adsorbents have preferable selectivity to phosphorus, applicable
The Pollution System coexisted in multi-pollutant, while can recycle adsorbent by desorption processing and reclaim phosphor resource.It is conventional
Phosphorus adsorbent mainly have natural material and waste residue, inorganic compound pole and its modifier, synthesis sorbing material.However, preparing
Adsorbent it is often powdered, separation of solid and liquid is difficult in actual applications, and can be partly dissolved and cause secondary pollution.
The content of the invention
Polyacrylic acid (sodium) base co-polymer gel is a kind of known organogel with preferable adsorptivity, be can be used for
Adsorption of Cu2+、pb2+、Zn2+And Cd2+Deng heavy metal cation.But, in the prior art, do not have also using polyacrylic acid (sodium)
Base co-polymer gel adsorption anion, such as the report for adsorbing P elements (in anion being present in phosphate radical).Moreover,
Due to the high water absorbing capacity of polyacrylic acid (sodium) gel so that its swelling ratio is very big, it is unfavorable for liquid in water body in adsorption process
Flowing, while also destroying the intensity of gel, be easily broken gel；This characteristic being easily broken makes it be applied to sewage
During processing, the problem of being difficult to separate is equally existed.
Polyacrylamide gel is conventional to do chromatography media, electrophoretic separation support material etc., and inventor is found through experiments that, gathers
Acrylamide gel does not have the performance of absorption P elements substantially.
It is unexpected, inventor by being extensively studied, be not limited to it is any theoretically find, when by PAA list
Body and acrylamide monomer crosslinking copolymerization are obtained after sodium acrylate-acrylamide cross-linked copolymer, and the copolymer but possesses absorption
The performance of P elements, moreover, the copolymer is when forming hydrogel, compared with polyacrylic acid (sodium) gel, swelling ratio is small, machinery
Intensity is more preferably, non-breakable.Based on this, it is an object of the invention to provide a kind of sodium acrylate-acrylamide cross-linked copolymer
Purposes of the gel in absorption P elements.Concrete technical scheme is as follows：
Present invention firstly provides purposes of the sodium acrylate-acrylamide cross-linked copolymer in absorption P elements, wherein,
Sodium acrylate-acrylamide cross-linked copolymer is formed by sodium acrylate monomers and acrylamide monomer copolymerization, the acrylic acid
The mass ratio of sodium monomer and acrylamide monomer is less than or equal to 2.
In a kind of embodiment of the present invention, the mass ratio of sodium acrylate monomers and acrylamide monomer is
(0.01-1)：1.
In a kind of embodiment of the present invention, the mass ratio of sodium acrylate monomers and acrylamide monomer is
(0.15-0.35)：1.
In a kind of embodiment of the present invention, the polymerization methodses of sodium acrylate monomers and acrylamide monomer are spoke
According to polymerization or thermal polymerization.
In a kind of embodiment of the present invention, the irradiation polymerization includes：Using60Co sources gamma-rays is at room temperature
Irradiation 1-120 minutes, more preferably preferably 10-60 minutes, 30 minutes.
In a kind of embodiment of the present invention, radiation dose rate is 70Gy/ minutes.
In a kind of embodiment of the present invention, the polymerization of sodium acrylate monomers and acrylamide monomer includes：Will
Sodium acrylate monomers, acrylamide monomer and crosslinking agent, which are dissolved in polymer solvent, to be polymerize, and obtains sodium acrylate-acrylamide
Crosslink copolymer gel.
In a kind of embodiment of the present invention, polymer solvent is organic solvent, preferably formamide, obtained production
Thing is sodium acrylate-acrylamide cross-linked copolymer organogel.
In a kind of embodiment of the present invention, the sodium acrylate-acrylamide cross-linked copolymer that polymerization is obtained
Organogel carry out exchange of solvent soluble in water, obtains sodium acrylate-acrylamide cross-linked copolymer hydrogel；By the propylene
Sour sodium-acrylamide crosslinking copolymer hydrogel carries out dewater treatment, obtains sodium acrylate-acrylamide cross-linked copolymer.
In a kind of embodiment of the present invention, sodium acrylate-acrylamide cross-linked copolymer is included with it
Propylene acid group meter, per 0.37-0.42 moles of P elements of mol propylene acid group absorption.
From the foregoing, the sodium acrylate-acrylamide cross-linked copolymer prepared by the present invention, it can effectively be adsorbed
After P elements, cross-linked copolymer formation hydrogel, there is certain mechanical strength, it is non-breakable, so it is easy to separation of solid and liquid, because
This, the sodium acrylate-acrylamide cross-linked copolymer prepared by the present invention is expected to be applied in sewage disposal, adsorbs P elements.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the SEM spectrograms of the organogel prepared by embodiment 1.
Embodiment
Present invention firstly provides purposes of the sodium acrylate-acrylamide cross-linked copolymer in absorption P elements, wherein,
Sodium acrylate-acrylamide cross-linked copolymer is formed by sodium acrylate monomers and acrylamide monomer copolymerization, the acrylic acid
The mass ratio of sodium monomer and acrylamide monomer is less than or equal to 2.Inventor has found, in the course of the polymerization process, in sodium acrylate monomers
It is less than or equal to the mass ratio of acrylamide monomer in the case of 2, resulting sodium acrylate-acrylamide cross-linked copolymer exists
When forming hydrogel, its swelling ratio is proper, and mechanical strength is preferably, non-breakable, is more suitable for application.Described swelling ratio is
Refer to polymer molecule adsorption solvent molecule when reaching swelling equilibrium, the ratio of volume after being swelled and the volume before not being swelled.This
Wen Zhong, term " crosslink copolymer gel " has its common implication, and the class for referring generally to be formed by polymer has three dimensional network
The elastic polymer chain of the material of network structure, wherein polymer is small by method formation basic framework chemically or physically
Molecular fluid calking is wherein；When the small molecule is organic solvent, crosslink copolymer gel is called that " cross-linked copolymer is organic solidifying
Glue "；When described small molecule is water, crosslink copolymer gel is called " cross-linked copolymer hydrogel ".Herein, term is " common
Polymers " has its common implication, generally refers to the polymer formed by two or more polymerized monomer.
In a kind of embodiment of the present invention, the mass ratio of sodium acrylate monomers and acrylamide monomer is
(0.15-1)：1.
In another embodiment of the present invention, the mass ratio of sodium acrylate monomers and acrylamide monomer is
(0.15-0.35)：1.
For sodium acrylate monomers and acrylamide monomer Mechanism of Copolymerization, radical polymerization can be used, can specifically be adopted
With irradiation polymerization or thermal polymerization.It is preferred to use irradiation polymerization.
In the embodiment of sodium acrylate-acrylamide cross-linked copolymer is prepared using irradiation polymerization, it can use60Co sources gamma-rays is irradiated 1-120 minutes at room temperature, preferably 10-60 minutes, more preferably 30 minutes.In a kind of specific reality
Apply in mode, radiation dose rate is 70Gy/ minutes.
Described thermal polymerization, refers to the polymerization methodses by adding thermal-initiated polymerization, mechanism or radical polymerization in the present invention
Close, by opening the double bond in monomer molecule, in the addition reaction of intermolecular progress repeatedly, many monomers are connected
Come, form macromolecular.The method of the most frequently used generation free radical is being thermally decomposed for initiator, can also use heating, ultraviolet
The methods such as irradiation, high-energy irradiation, electrolysis and plasma initiation produce free radical.
In a kind of embodiment of the present invention, the polymerization of sodium acrylate monomers and acrylamide monomer includes：Will
Sodium acrylate monomers, acrylamide monomer and crosslinking agent, which are dissolved in polymer solvent, to be polymerize, and obtains sodium acrylate-acrylamide
Crosslink copolymer gel.The polymer solvent used can use organic solvent, such as formamide, it would however also be possible to employ water is made molten
Agent.When being polymerize using organic solvent, sodium acrylate-acrylamide cross-linked copolymer organogel is obtained；Make molten using water
When agent is polymerize, sodium acrylate-acrylamide cross-linked copolymer hydrogel is obtained.
When being polymerize using organic solvent, the sodium acrylate-acrylamide cross-linked copolymer obtained by it is organic solidifying
Glue needs to be further processed to be used to adsorb P elements.Specifically, in a kind of embodiment of the present invention
In, the sodium acrylate-acrylamide cross-linked copolymer organogel that polymerization is obtained is placed in water carry out exchange of solvent, obtains third
Olefin(e) acid sodium-acrylamide crosslinking copolymer hydrogel；The sodium acrylate-acrylamide cross-linked copolymer hydrogel is taken off
Water process, dries, obtains sodium acrylate-acrylamide cross-linked copolymer, is referred to as sodium acrylate-acrylamide crosslinking altogether
Polymers xerogel.Certainly, it is necessary to which explanation, during using water as solvent polymeric, obtained by it is PAA-acryloyl
Amine cross-linked copolymer hydrogel, need not now carry out exchange of solvent processing, but before application, it is desired nonetheless to carry out at dehydration
Reason.
Crosslinking agent employed in polymerization process can use crosslinking agent commonly used in the art, and the present invention is herein without limit
It is fixed.In a kind of embodiment of the present invention, using N, N- methylene-bisacrylamides (BIS) are used as crosslinking agent.For
The consumption of crosslinking agent, on the basis of acrylamide, the mass ratio of crosslinking agent and acrylamide can be 0.01-0.08, be preferably
0.02-0.06。
In the present invention, the amount of polymer solvent is not required particularly, as long as it can guarantee that being smoothed out for polymerisation
.In a kind of embodiment, on the basis of acrylamide, the volume of polymer solvent and the quality of acrylamide monomer
Ratio can be (5-20) mL/1g, be preferably (7-12) mL/1g.
In a kind of embodiment of the present invention, dehydrating agent progress dewater treatment can be used as using ethanol；Work as handle
Hydrogel is put into ethanol, and the hydrone in gel is replaced by ethanol molecule, afterwards ethanol molecule and the macromolecular chain in gel
It is mutually exclusive to reduce solvent in gel.After after ethanol volatilization, xerogel is obtained.Specifically, can be by PAA-acryloyl
Amine cross-linked copolymer hydrogel is placed in ethanol, is dehydrated it, after drying, and forms sodium acrylate-acrylamide cross-linked copolymer
Xerogel.
, can will be above prepared organic in solvent exchange procedure in a kind of embodiment of the present invention
Gel is mixed in the ratio of 1g organogels and 10-30mL water, carries out exchange of solvent, exchange process is about at 0.5-2 hours.
It is determined by experiment, the sodium acrylate-acrylamide cross-linked copolymer prepared by the present invention, third included with it
Olefin(e) acid root meter, 0.37-0.42 moles of P elements can be adsorbed per mol propylene acid group.It should be noted that in practical application
In, entered because sodium acrylate monomers are substantially all in polymerization process in cross-linked copolymer, therefore, PAA-acryloyl
The amount of propylene acid group included in amine cross-linked copolymer substantially corresponds to the amount of sodium acrylate monomers.
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Prepare embodiment
Embodiment 1 prepares sodium acrylate-acrylamide cross-linked copolymer
(1) cross-linked copolymer organogel is prepared：By polymerized monomer PAA, acrylamide and crosslinking agent N, N- methylene
Base bisacrylamide (BIS) is dissolved in formamide solvent, and the amount for adding each reactant is shown in Table 1.The mixing obtained after being completely dissolved
Solution lead to nitrogen protection 10min after be injected into the glass plate reaction vessel of subsidiary silicone gasket (packing ring specification be long 10cm, it is wide
8cm, thick 2mm), 30min is irradiated using 60Co sources gamma-rays at room temperature, radiation dose rate is 70Gy/min, obtain organic solidifying
Glue；
(2) exchange of solvent：The organogel obtained in (1) is placed in water progress exchange of solvent 1 hour, water-setting is obtained
Glue；The ratio of the quality of organogel and the volume of water is 1g:20mL；
(3) dewater treatment：The hydrogel obtained in (2) is placed in ethanol, dewater treatment 1 hour；The quality of hydrogel
Ratio with the volume of ethanol is 1g:After 20mL, dewater treatment, in being dried at 40 DEG C to constant weight, PAA-acryloyl is obtained
Amine cross-linked copolymer, also referred to as sodium acrylate-acrylamide cross-linked copolymer xerogel.
Embodiment 2-3
According to the method described in embodiment 1, using the addition of each reactant described in table 1, reality is prepared respectively
Apply the sodium acrylate-acrylamide cross-linked copolymer in a 2-3.
Comparative example 1
According to the method described in embodiment 1, using the addition of each reactant described in table 1, comparative example 1 is prepared
In acrylamide crosspolymer cross-linked copolymer.
The amount of each reactant in the embodiment 1-3 of table 1 and comparative example 1
Testing example
After hydrogel freeze-drying (be put into after liquid nitrogen frozen and vacuumize drying again) prepared in embodiment 1-3, then
Electron microscope (SEM) sign is scanned to it, is entered below by taking the SEM spectrograms of the organogel prepared by embodiment 1 as an example
Row explanation.Fig. 1 be embodiment 1 prepared by organogel SEM spectrograms, from figure this it appears that gel network it is microcosmic
Cavernous structure.
On in addition, synthesized organogel color is transparent, it is stretched and and compression, have certain machinery strong
Degree, it is non-breakable, advantageous as Applied Materials.
Phosphorus absorption property is tested
The Example 1-3 and organogel 1g prepared by comparative example 1, after being changed into xerogel through processing, is added to phosphorus and contains
Measure the NaH for 400mg/L2PO4In solution, vibration absorption 2 days at 22 DEG C.Solution centrifugal is filtered after absorption, uses inductive
Plasma spectrometry (ICP), which determines phosphorus concentration in filtrate, to be changed, and phosphorus absorption result is as shown in table 2.
The embodiment 1-3 of table 2 and comparative example 1 phosphorus absorption result
Note：In table 2, mg-P/g represents the P (phosphorus) of every gram of organogel absorption milligram number；AA-Represent propylene acid group；
mol-P/mol-AA-Represent every mole of propylene acid group absorption P (phosphorus) molal quantity；mg-P/g-AA-The acrylic acid of every gram of expression
Root absorption P (phosphorus) milligram number.
From Table 2, it can be seen that acrylamide crosslinking copolymer does not have suction-operated substantially to phosphorus.But PAA-
Acrylamide crosslinking copolymer but has obvious phosphorus absorption property, and average adsorption amount is 0.406mol-P/mol-AA-, i.e.,
177.3mg-P/g-AA-。
Above to sodium acrylate-acrylamide crosslink copolymer gel provided by the present invention absorption P elements in use
Way is described in detail.Specific embodiment used herein is set forth to the principle and embodiment of the present invention, with
The explanation of upper embodiment is only intended to the method and its central idea for helping to understand the present invention.It should be pointed out that for this area
For those of ordinary skill, under the premise without departing from the principles of the invention, some improvement and modification can also be carried out to the present invention,
These are improved and modification also falls into the protection of the claims in the present invention.
Claims (10)
1. purposes of the sodium acrylate-acrylamide cross-linked copolymer in absorption P elements, wherein, sodium acrylate-acrylamide
Cross-linked copolymer is formed by sodium acrylate monomers and acrylamide monomer copolymerization, the sodium acrylate monomers and acrylamide list
The mass ratio of body is less than or equal to 2.
2. purposes as claimed in claim 1, wherein, the mass ratio of sodium acrylate monomers and acrylamide monomer is (0.01-
1)：1.
3. purposes as claimed in claim 1, wherein, the mass ratio of sodium acrylate monomers and acrylamide monomer is (0.15-
0.35)：1.
4. purposes as claimed in claim 1, wherein, the polymerization methodses of sodium acrylate monomers and acrylamide monomer are poly- for irradiation
Close or thermal polymerization.
5. purposes as claimed in claim 4, wherein, the irradiation polymerization includes：Using60Co sources gamma-rays is irradiated at room temperature
1-120 minutes, more preferably preferably 10-60 minutes, 30 minutes.
6. purposes as claimed in claim 5, wherein, radiation dose rate is 70Gy/ minutes.
7. purposes as claimed in claim 4, wherein, the polymerization of sodium acrylate monomers and acrylamide monomer includes：By propylene
Sour sodium monomer, acrylamide monomer and crosslinking agent are dissolved in polymer solvent and polymerize, and obtain sodium acrylate-acrylamide crosslinking
Copolymer gel.
8. purposes as claimed in claim 7, wherein, polymer solvent is organic solvent, preferably formamide, and obtained product is
Sodium acrylate-acrylamide cross-linked copolymer organogel.
9. purposes as claimed in claim 8, wherein, the sodium acrylate-acrylamide cross-linked copolymer that polymerization is obtained is organic
Gel carry out exchange of solvent soluble in water, obtains sodium acrylate-acrylamide cross-linked copolymer hydrogel；By the acrylic acid
Sodium-acrylamide crosslinking copolymer hydrogel carries out dewater treatment, obtains sodium acrylate-acrylamide cross-linked copolymer.
10. purposes as claimed in any one of claims 1-9 wherein, wherein, sodium acrylate-acrylamide cross-linked copolymer is with its institute
Comprising propylene acid group meter, 0.37-0.42 moles of P elements are adsorbed per mol propylene acid group.
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Cited By (2)
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| CN110592702A (en) * | 2019-09-26 | 2019-12-20 | 东华大学 | Photoresponse and anti-freezing elastic gel fiber and preparation method thereof |
| CN114558556A (en) * | 2022-01-11 | 2022-05-31 | 河南工程学院 | Method for jointly preparing gel filler for purifying nitrogen and phosphorus in sewage by using solid wastes |
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| CN110592702B (en) * | 2019-09-26 | 2021-11-09 | 东华大学 | Photoresponse and anti-freezing elastic gel fiber and preparation method thereof |
| CN114558556A (en) * | 2022-01-11 | 2022-05-31 | 河南工程学院 | Method for jointly preparing gel filler for purifying nitrogen and phosphorus in sewage by using solid wastes |
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