CN108503880A - A kind of method of the calcium alginate compounded microballoon of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization- - Google Patents

A kind of method of the calcium alginate compounded microballoon of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization- Download PDF

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CN108503880A
CN108503880A CN201810230011.7A CN201810230011A CN108503880A CN 108503880 A CN108503880 A CN 108503880A CN 201810230011 A CN201810230011 A CN 201810230011A CN 108503880 A CN108503880 A CN 108503880A
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polyacrylamide
synthesis
calcium alginate
microballoon
microemulsion polymerization
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CN108503880B (en
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张鸿
陈涛
曹仕文
王远贞
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Dalian Xi An Technology Co Ltd
Dalian Polytechnic University
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Dalian Xi An Technology Co Ltd
Dalian Polytechnic University
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • 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
    • 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
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/261Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/32Polymerisation in water-in-oil emulsions
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    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52Amides or imides
    • C08F220/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/56Acrylamide; Methacrylamide
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    • C08J2201/00Foams characterised by the foaming process
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    • C08J2333/00Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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    • C08J2405/00Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/04Alginic acid; Derivatives thereof

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Abstract

The present invention relates to a kind of methods of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon.Realize that the polymerization of acrylamide and cross-linking reaction form first network in compound system by conversed phase micro emulsion copolymerization, formation by the ionomer of another component sodium alginate the second network of realization and two kinds of internetwork physical entanglements again, method by being freeze-dried or being spray-dried again is prepared for a kind of micron-size spherical adsorbent with microcellular structure.Complex microsphere is made using sodium alginate and acrylamide in the present invention, adsorption effect of the acrylamide in sewage treatment field to heavy metal ion and the dye of positive ion is not only expanded, and compared with conventional polypropylene amide, there are the outstanding features such as environmental protection and good degradability.

Description

A kind of calcium alginate compounded microballoon of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization- Method
Technical field
The invention belongs to Material Field, it is related to a kind of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded The method of microballoon.
Background technology
With the development of society, people's health requirement is higher and higher, in some industrial wastewaters a large amount of heavy metal from Sub and extra printing and dyeing substance, the harm to human body are huge, and height has gradually been moved towards to the processing of sanitary sewage and industrial wastewater Standard.Needs can no longer meet for the processing of one-component in sewage, novel adsorbent should multiple pollutant have Treatment effect, and also there is certain environment compatibility.
Polyacrylamide amine absorber is a kind of widely used adsorbent, and polyacrylamide itself has certain wadding Solidifying property, after being added to the water, can attract impurity, reach the effect that can be detached to make a variety of small pollutants reunions in water Fruit.Sodium alginate be it is a kind of extracted from seaweed can be with biodegradable macromolecular, containing a large amount of hydroxyl and carboxyl, to more Number cationic substance all has affinity interaction, and the sewage for handling enrichment cation has remarkable result.Virgin pp amide Although having certain flocculability, when being directed to the substances such as the ion in water, removal effect is poor, and conventional method obtains Polyacrylamide in the case of given volume, specific surface area is smaller, and flocculability can not be played effectively.
Invention content
The purpose of the present invention is to provide a kind of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoons Method, this method can improve polyacrylamide substances sewage treatment field deficiency, improve emphatically to heavy metal from The processing of son and the dye of positive ion etc., expands the application field of polyacrylamide, additionally smaller adsorbent secondary pollution The environmental hazard brought has pushed the sustainable development of man and nature.
To achieve the above object, the present invention adopts the following technical scheme that realize:
A kind of method of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon, includes the following steps: Following raw material in parts by mass,
(1) continuous phase is prepared:7.5 parts of emulsifier I and 2.5 parts of emulsifier II are dissolved in 100 parts of solvents at 50 DEG C In oil, it is uniformly mixed, is cooled to room temperature;
(2) dispersed phase is prepared:By 5 parts of acrylamide monomer, 0.5~2 part of crosslinking agent, 0.2~1 part of sodium alginate It is dissolved at 60 DEG C in 30 parts of deionized waters, is configured to dispersed phase, is cooled to room temperature;
(3) initiator solution is prepared:0.1~0.7 part of initiator is dissolved at room temperature in remaining deionized water, is matched Solution is made;
(4) calcium chloride solution is prepared:1.5 parts of anhydrous calcium chlorides are dissolved at room temperature in 50 parts of deionized water and prepare chlorine Change calcium solution;
(5) it is mixed in 30 DEG C, mixing speed for dispersion is added in continuous phase under conditions of 3000~5000r/min Emulsification 20~40 minutes is closed, then initiator solution is added in mixed liquor, continues emulsification 5-15 minutes;
(6) mixing speed is reduced to 800~1200r/min, and polymerisation is carried out at 50~70 DEG C, is reacted to 1 hour Later, calcium chloride solution is added in reaction system, the reaction was continued 0.5 hour;
(7) reaction terminates, and mixed solution absolute ethyl alcohol is demulsified, washing, obtained precipitation is freezed or sprayed dry It is dry, obtain the polyacrylamide with microcellular structure/calcium alginate compounded microballoon;
Wherein, acrylamide monomer, crosslinking agent, initiator, sodium alginate, deionization in the step (2) and step (3) The gross mass of water is 50 parts.
According to technical solution above, in the case of preferred, the emulsifier in the step (1) is non-ionic surfactant Agent, emulsifier I are selected from at least one of Span 20, Span 60, Span 80, and emulsifier II is selected from Tween 20, Tween 60 Or at least one of Tween 80.
According to technical solution above, in the case of preferred, the solvent naphtha in the step (1) include aliphatic compound, Aromatic compound, naphthene-based compounds etc., selected from kerosene, white oil, atoleine, benzene,toluene,xylene, hexamethylene, just The one or more of hexane, normal octane.
According to technical solution above, in the case of preferred, the crosslinking agent in the step (2) is selected from N, N- di-2-ethylhexylphosphine oxide first Base acrylamide, N, penylene bismaleimide, ethylene glycol dimethacrylate, polyethyleneglycol diacrylate, season between N- At least one of penta tetrol triacrylate.
According to technical solution above, in the case of preferred, the initiator in the step (3) is peroxide initiator, Selected from least one of ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate, hydrogen peroxide, benzoyl peroxide.
According to technical solution above, in the case of preferred, the freeze-drying condition in the step (7) is:Time is 12 ~for 24 hours, temperature is 50 DEG C of 100 DEG C~﹣ of ﹣.
According to technical solution above, in the case of preferred, the spray drying condition in the step (7) is:Inlet air temperature It it is 150~190 DEG C, pan feeding flow is 500~1000ml/h, and charge flow rate is 500~900L/h.
According to technical solution above, in the case of preferred, the crosslinking agent is 0.75 part, and the initiator is 0.25 part, The polymeric reaction temperature is 60 DEG C.
According to technical solution above, in the case of preferred, mixing speed is 4000r/min, the step in the step (5) Suddenly mixing speed is 1000r/min in (6).
Moreover, it relates to polyacrylamide/calcium alginate compounded microballoon prepared by the Sustainable use above method.
Advantageous effect of the present invention:
The present invention provides a kind of methods of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon. The sodium alginate of addition can crosslink reaction under the action of bivalent cation, form a kind of network structure, in conjunction with poly- third The cross-linking reaction of acrylamide forms dual network structure, can effectively expand adsorption area, promotes effect.And sodium alginate is from plant A kind of substance extracted in object, it is pollution-free, it is biodegradable, it can greatly alleviate the problem of secondary pollution.
Complex microsphere is made using sodium alginate and acrylamide in the present invention, has not only expanded acrylamide in sewage disposal Field is to the adsorption effect of heavy metal ion and the dye of positive ion, and compared with conventional polypropylene amide, have environmental protection and The outstanding features such as good degradability.
Polyacrylamide and sodium alginate is compound, acrylamide in compound system is realized by conversed phase micro emulsion copolymerization Polymerization and cross-linking reaction form first network, then the shape of the second network is realized by the ionomer of another component sodium alginate At and two kinds of internetwork physical entanglements, then the method by being freeze-dried or being spray-dried, be prepared for a kind of there is micropore knot The micron-size spherical adsorbent of structure.Gathered polyacrylamide flocculability and sodium alginate to the compatibility of cationic substance, The adsorption range for expanding adsorbent keeps it all effective for multiple pollutant.In addition, using the method for emulsion polymerization, reduce The size of adsorbent, increasing specific surface area increase contact area when absorption, further increase effect.Sodium alginate is one Kind Nantural non-toxic, degradable substance, can reduce the secondary pollution of adsorbent energetically.By the way that sodium alginate is added, expand poly- Acrylamide promotes the R and D to marine resources and other biological metallic substances in the application of sewage treatment field, The contradiction for alleviating resource growing tension, can also realize the sustainable development of environment, push the process of world's environmental protection cause.
Description of the drawings
Fig. 1 is the nitrogen adsorption and desorption curve figure of polyacrylamide of the present invention/calcium alginate compounded microballoon;
Fig. 2 is Dye Adsorption of the polyacrylamide of the present invention/calcium alginate compounded microballoon under different sodium alginate contents It can try hard to;
Fig. 3 is the scanning electron microscope (SEM) photograph of polyacrylamide of the present invention/calcium alginate compounded microballoon.
Specific implementation mode
In order to keep the purpose of the present invention, scheme, flow and advantage more clear apparent, in conjunction with the embodiments to the present invention do into The detailed description of one step, it is notable that specific embodiment is not used to limit this only as the present invention is illustrated herein Invention.In following embodiments, unless otherwise specified, used experimental method is conventional method, and material therefor, reagent etc. are equal It can be bought from biological or chemical company.
Embodiment 1
Present embodiment discloses a kind of sides of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon Method is prepared by following methods:
7.5g Span 60 and 2.5g Tween 60 and 100g hexamethylenes are mixed, is dissolved at 50 DEG C, is cooled to room Temperature.It weighs 5g acrylamides, 0.5g N, N- methylene-bisacrylamide, 0.2g sodium alginates and 30ml water to mix, at 60 DEG C Dissolving, postcooling to room temperature.0.25g ammonium persulfates are taken, are dissolved in 14.05ml water, wiring solution-forming.1.5g calcium chloride is dissolved in In 50ml water, it is configured to the calcium chloride solution that mass concentration is 3%.
So that cyclohexane solution is placed under 30 DEG C of water bath conditions, then by the solution containing acrylamide and sodium alginate with The speed of 1.33ml/min is added in cyclohexane solution, and in adding procedure, it is 4000r/min to maintain churned mechanically rate. After addition, persistently stir 30 minutes, then ammonium persulfate solution is added to same adding speed in mixed liquor, followed by Continuous stirring 10 minutes.Mechanical agitation speed is reduced to 1000r/min, bath temperature is increased to 60 DEG C, and maintains 1 hour.Again Calcium chloride solution is added to same adding speed in mixed solution, rear the reaction was continued 30 minutes.
The ethyl alcohol of mixed solution two volumes is taken to be demulsified, the sediment after centrifugation continues to be washed 2-3 times with ethyl alcohol, then uses water Washing one time.It is put into water removal in freeze drier later, 100 DEG C of water removals of freeze drier ﹣ maintain 12 hours to obtain polyacrylamide Amine/calcium alginate compounded microballoon.
It is tested according to GB/T 21851-2008, the methylene blue adsorption number ability of complex microsphere prepared by the present embodiment method For 49.76mg/g.
The nitrogen adsorption and desorption of the present embodiment Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon Curve judges as shown in Figure 1, apparent adsorption hysteresis ring as we can see from the figure according to the shape of hysteresis loop, polyacrylamide/ Pore structure in calcium alginate compounded microballoon is meso-hole structure.
The scanning electron microscope (SEM) photograph of the present embodiment Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon is as schemed Shown in 3, complex microsphere shape is regular, is in complete spherical.
Embodiment 2
Present embodiment discloses a kind of sides of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon Method is prepared by following methods:
7.5g Span 60 and 2.5g Tween 60 and 100g hexamethylenes are mixed, is dissolved at 50 DEG C, is cooled to room Temperature.It weighs 5g acrylamides, 0.5g N, N- methylene-bisacrylamide, 0.4g sodium alginates and 30ml water to mix, at 60 DEG C Dissolving, postcooling to room temperature.0.25g ammonium persulfates are taken, are dissolved in 13.25ml water, wiring solution-forming.1.5g calcium chloride is dissolved in In 50ml water, it is configured to 3% calcium chloride solution.
So that cyclohexane solution is placed under 30 DEG C of water bath conditions, then by the solution containing acrylamide and sodium alginate with 1.33ml/min speed is added in cyclohexane solution, and in adding procedure, it is 4000r/min to maintain churned mechanically rate.Add After adding, persistently stirs 30 minutes, then ammonium persulfate solution is added to same adding speed in mixed liquor, be further continued for Stirring 10 minutes.Mechanical agitation speed is reduced to 1000r/min, bath temperature is increased to 60 DEG C, and maintains 1 hour.Again will Calcium chloride solution is added to same adding speed in mixed solution, and rear the reaction was continued 30 minutes.
The ethyl alcohol of mixed solution two volumes is taken to be demulsified, the sediment after centrifugation continues to be washed 2-3 times with ethyl alcohol, then uses water Washing one time.It is put into water removal in freeze drier later, 90 DEG C of water removals of freeze drier ﹣ maintain 12 hours to obtain polyacrylamide Amine/calcium alginate compounded microballoon.
It is tested according to GB/T 21851-2008, the methylene blue adsorption number ability of complex microsphere prepared by the present embodiment method For 36.2661mg/g.
Embodiment 3
Present embodiment discloses a kind of sides of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon Method is prepared by following methods:
7.5g Span 60 and 2.5g Tween 60 and 100g hexamethylenes are mixed, is dissolved at 50 DEG C, is cooled to room Temperature.It weighs 5g acrylamides, 0.5g N, N- methylene-bisacrylamide, 0.6g sodium alginates and 30ml water to mix, at 60 DEG C Dissolving, postcooling to room temperature.0.25g ammonium persulfates are taken, are dissolved in 13.65ml water, wiring solution-forming.1.5g calcium chloride is dissolved in In 50ml water, it is configured to 3% calcium chloride solution.
So that cyclohexane solution is placed under 30 DEG C of water bath conditions, then by the solution containing acrylamide and sodium alginate with 1.33ml/min speed is added in cyclohexane solution, and in adding procedure, it is 4000r/min to maintain churned mechanically rate.Add After adding, persistently stirs 30 minutes, then ammonium persulfate solution is added to same adding speed in mixed liquor, be further continued for Stirring 10 minutes.Mechanical agitation speed is reduced to 1000r/min, bath temperature is increased to 60 DEG C, and maintains 1 hour.Again will Calcium chloride solution is added to same adding speed in mixed solution, and rear the reaction was continued 30 minutes.
The ethyl alcohol of mixed solution two volumes is taken to be demulsified, the sediment after centrifugation continues to be washed 2-3 times with ethyl alcohol, then uses water Washing one time.It is put into water removal in freeze drier later, 50 DEG C of water removals of freeze drier ﹣ maintain 12 hours to obtain polyacrylamide Amine/calcium alginate compounded microballoon.
It is tested according to GB/T 21851-2008, the methylene blue adsorption number ability of complex microsphere prepared by the present embodiment method For 33.879mg/g.
Embodiment 4
Present embodiment discloses a kind of sides of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon Method is prepared by following methods:
7.5g Span 60 and 2.5g Tween 60 and 100g hexamethylenes are mixed, is dissolved at 50 DEG C, is cooled to room Temperature.It weighs 5g acrylamides, 0.5g N, N- methylene-bisacrylamide, 0.8g sodium alginates and 30ml water to mix, at 60 DEG C Dissolving, postcooling to room temperature.0.25g ammonium persulfates are taken, are dissolved in 13.45ml water, wiring solution-forming.1.5g calcium chloride is dissolved in In 50ml water, it is configured to 3% calcium chloride solution.
So that cyclohexane solution is placed under 30 DEG C of water bath conditions, then by the solution containing acrylamide and sodium alginate with 1.33ml/min speed is added in cyclohexane solution, and in adding procedure, it is 4000r/min to maintain churned mechanically rate.Add After adding, persistently stirs 30 minutes, then ammonium persulfate solution is added to same adding speed in mixed liquor, be further continued for Stirring 10 minutes.Mechanical agitation speed is reduced to 1000r/min, bath temperature is increased to 60 DEG C, and maintains 1 hour.Again will Calcium chloride solution is added to same adding speed in mixed solution, and rear the reaction was continued 30 minutes.
The ethyl alcohol of mixed solution two volumes is taken to be demulsified, the sediment after centrifugation continues to be washed 2-3 times with ethyl alcohol, then uses water Washing one time.It is put into water removal in freeze drier later, 50 DEG C of water removals of freeze drier ﹣ maintain 12 hours to obtain polyacrylamide Amine/calcium alginate compounded microballoon.
It is tested according to GB/T 21851-2008, the methylene blue adsorption number ability of complex microsphere prepared by the present embodiment method For 35.1555mg/g.
Embodiment 5
Present embodiment discloses a kind of sides of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon Method is prepared by following methods:
7.5g Span 60 and 2.5g Tween 60 and 100g hexamethylenes are mixed, is dissolved at 50 DEG C, is cooled to room Temperature.5g acrylamides, 0.5g N, N- methylene-bisacrylamide, 1g sodium alginates and 30ml water is weighed to mix, it is molten at 60 DEG C Solution, postcooling to room temperature.0.25g ammonium persulfates are taken, are dissolved in 13.25ml water, wiring solution-forming.1.5g calcium chloride is dissolved in In 50ml water, it is configured to 3% calcium chloride solution.
So that cyclohexane solution is placed under 30 DEG C of water bath conditions, then by the solution containing acrylamide and sodium alginate with 1.33ml/min speed is added in cyclohexane solution, and in adding procedure, it is 4000r/min to maintain churned mechanically rate.Add After adding, persistently stirs 30 minutes, then ammonium persulfate solution is added to same adding speed in mixed liquor, be further continued for Stirring 10 minutes.Mechanical agitation speed is reduced to 1000r/min, bath temperature is increased to 60 DEG C, and maintains 1 hour.Again will Calcium chloride solution is added to same adding speed in mixed solution, and rear the reaction was continued 30 minutes.
The ethyl alcohol of mixed solution two volumes is taken to be demulsified, the sediment after centrifugation continues to be washed 2-3 times with ethyl alcohol, then uses water Washing one time.It is put into water removal in freeze drier later, 50 DEG C of water removals of freeze drier ﹣ maintain 12 hours to obtain polyacrylamide Amine/calcium alginate compounded microballoon.
It is tested according to GB/T 21851-2008, the methylene blue adsorption number ability of complex microsphere prepared by the present embodiment method For 53.94mg/g.
Embodiment 6 (blank control group)
Method in accordance with the above-mentioned embodiment 1 prepares microballoon, and difference is not add sodium alginate and calcium chloride.
It is tested according to GB/T 21851-2008, the methylene blue adsorption number ability of microballoon prepared by the present embodiment method is 50mg/g。
Microballoon methylene blue adsorption number capability analysis prepared by embodiment 1-6 methods is as shown in Fig. 2, as seen from the figure with seaweed The increase of sour sodium content, complex microsphere is to the adsorption capacity of methylene blue totally in the trend risen, it can be seen that addition seaweed Sour sodium significantly improves the adsorption capacity of polyacrylamide.
It is above to be told, only it is the preferable embodiment of the present invention, the above various embodiments is only to illustrate the technology of the present invention Scheme, rather than its limitations;Although present invention has been described in detail with reference to the aforementioned embodiments, the common skill of this field Art personnel should understand that:Its still can with technical scheme described in the above embodiments is modified, or to its middle part Divide or all technical features carries out equivalent replacement;And these modifications or replacements, do not make the essence of corresponding technical solution de- Range from various embodiments of the present invention technical solution.

Claims (9)

1. a kind of method of Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization/calcium alginate compounded microballoon, which is characterized in that including Following steps:Following raw material in parts by mass,
(1) continuous phase is prepared:7.5 parts of emulsifier I and 2.5 parts of emulsifier II are dissolved at 50 DEG C in 100 parts of solvent naphthas, It is uniformly mixed, is cooled to room temperature;
(2) dispersed phase is prepared:By 5 parts of acrylamide monomer, 0.5~2 part of crosslinking agent, 0.2~1 part of sodium alginate 60 It is dissolved at DEG C in 30 parts of deionized waters, is configured to dispersed phase, is cooled to room temperature;
(3) initiator solution is prepared:0.1~0.7 part of initiator is dissolved at room temperature in remaining deionized water, is configured to Solution;
(4) calcium chloride solution is prepared:1.5 parts of anhydrous calcium chlorides are dissolved at room temperature in 50 parts of deionized water and prepare calcium chloride Solution;
(5) in 30 DEG C, mixing speed for dispersion is added in continuous phase under conditions of 3000~5000r/min, mixing breast Change 20~40 minutes, then initiator solution is added in mixed liquor, continues emulsification 5-15 minutes;
(6) mixing speed is reduced to 800~1200r/min, and polymerisation is carried out at 50~70 DEG C, is reacted to after 1 hour, Calcium chloride solution is added in reaction system, the reaction was continued 0.5 hour;
(7) reaction terminates, and mixed solution absolute ethyl alcohol is demulsified, washing, and obtained precipitation is freezed or is spray-dried, obtained To the polyacrylamide with microcellular structure/calcium alginate compounded microballoon;
Wherein, acrylamide monomer in the step (2) and step (3), crosslinking agent, initiator, sodium alginate, deionized water Gross mass is 50 parts.
2. the method for Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization according to claim 1/calcium alginate compounded microballoon, It is characterized in that, emulsifier I is selected from at least one of Span 20, Span 60, Span 80, emulsifier II in the step (1) At least one selected from Tween 20, Tween 60 or Tween 80.
3. the method for Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization according to claim 1/calcium alginate compounded microballoon, It is characterized in that, solvent naphtha in the step (1) be selected from kerosene, white oil, atoleine, benzene,toluene,xylene, hexamethylene, The one or more of n-hexane, normal octane.
4. the method for Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization according to claim 1/calcium alginate compounded microballoon, It is characterized in that, the crosslinking agent in the step (2) is selected from N, N- methylenebismethacrylamides, N, penylene span comes between N- At least one in acid imide, ethylene glycol dimethacrylate, polyethyleneglycol diacrylate, pentaerythritol triacrylate Kind.
5. the method for Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization according to claim 1/calcium alginate compounded microballoon, It is characterized in that, the initiator in the step (3) is selected from ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate, hydrogen peroxide, peroxide Change at least one of benzoyl.
6. the method for Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization according to claim 1/calcium alginate compounded microballoon, It is characterized in that, the freeze-drying condition in the step (7) is:Time be 12~for 24 hours, temperature be 50 DEG C of 100 DEG C~﹣ of ﹣.
7. the method for Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization according to claim 1/calcium alginate compounded microballoon, It is characterized in that, the spray drying condition in the step (7) is:150~190 DEG C of inlet air temperature, pan feeding flow 500~ 1000ml/h, 500~900L/h of charge flow rate.
8. the method for Synthesis of Polyacrylamide Using Anti-phase Microemulsion Polymerization according to claim 1/calcium alginate compounded microballoon, It is characterized in that, the crosslinking agent is 0.75 part, the initiator is 0.25 part, and the polymeric reaction temperature is 60 DEG C.
9. polyacrylamide/calcium alginate compounded the microballoon prepared such as claim 1-8 any one the methods.
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CN109174047A (en) * 2018-09-30 2019-01-11 天津市金鳞水处理科技有限公司 One kind having both detection of heavy metal ion and absorbent-type polyacrylamide microgel
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CN116747844A (en) * 2023-08-09 2023-09-15 常熟华虞环境科技有限公司 Preparation method of calcium chloride crosslinked sodium alginate material for water treatment
CN116747844B (en) * 2023-08-09 2023-11-10 常熟华虞环境科技有限公司 Preparation method of calcium chloride crosslinked sodium alginate material for water treatment

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