CN105754048B - A kind of preparation method of the temperature sensitive magnetic water-absorbing resin of high intensity - Google Patents
A kind of preparation method of the temperature sensitive magnetic water-absorbing resin of high intensity Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
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- C—CHEMISTRY; METALLURGY
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- 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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Abstract
The invention discloses a kind of preparation method of the temperature sensitive magnetic high hydroscopic resin of high intensity for fine mineral dehydration, belong to functional material and solid-liquid separation technique field.The composite is first with raw material FeCl2And FeCl3Colloidal solution is formed, sequentially adds citric acid, organic surface modification agent and Coaseries kaolin afterwards, it is standby after stirring.Then acrylic acid, PAA, temperature sensitive monomer, crosslinking agent and initiator for reaction are added in another reaction vessel, foregoing products therefrom is added, stirs, produces the temperature sensitive magnetic water-absorbing resin of high intensity.This method can solve the problems, such as water-absorbing resin dehydration with it is easily rupturable in separation process.
Description
Technical field
The invention belongs to functional material and solid-liquid separation technique field, is related to a kind of temperature sensitive magnetic water-absorbing resin of high intensity
Preparation method, this method can quickly prepare the water-absorbing resin with the high temperature sensitive magnetic of intensity.
Background technology
Super absorbent resin（Super Absorbent Resin abbreviations SAR）It is a kind of very typical feature high score
Sub- material, the moisture of even thousands of times of energy swellable absorbent, be generally otherwise known as " high water absorbency polymer（Super Absorbent
Polymer, abbreviation SAP）”.Compared with water-soluble polymer and adsorbability polymer, not only having for super absorbent resin is super
High water imbibition also has preferable water-retaining property, and is widely used in the fields such as agricultural gardening, health care and industrial building.
The research for the macromolecule hydrogel that can be stimulated and changed by external condition for swelling behavior in recent years is got over
To be more concerned by people, there are Many researchers to report for stimulation energy such as pH, temperature, ionic strength electric field and magnetic fields
The hydrogel material to respond, when by environmental stimuli, its swellbility can change this kind of material, this characteristic
It can be applied in many occasions.Such as the concentration of the sustained release, enzyme of medicine and molecule separation and artificial intelligence etc., thus
Also known as this kind of material is intelligent macromolecule material.
Chinese patent CN103172958A discloses a kind of temperature sensitive epoxy composite material and preparation method thereof, the composite
Can variation with temperature hydrophobicity is changed into from hydrophily, can apply to the fields such as smart coatings, functional plastics.Chinese patent
CN101701051A discloses a kind of pH, temperature sensitive hydrogel and preparation method thereof, and the material has preferably intelligent
And degradability.In the last few years, it is external to there is the scholar of the U.S. and Australia to carry out using super absorbent resin removing particulate
The research of moisture content of coal, and there is not been reported for domestic research in this regard.At present, the external method mainly used is the big grain of synthesis
Footpath resin, then separation resin and Bed for Fine Coal by way of the sieve that shakes.
It is that one kind removes fine mineral by means of absorbent material to carry out dehydration to fine mineral using super absorbent resin
The method of middle moisture, but moisture in super absorbent resin removing fine mineral, its dehydration is easily controlled, and is set after absorbing water
The recovery and regeneration of fat are highly difficult.Therefore when synthesizing temperature sensitive magnetic high hydroscopic resin, it should while improve the intensity of resin
And recycling rate of waterused, so as to save substantial amounts of production cost；And this to be prior art be unable to reach.
The content of the invention
For during water-absorbing resin difference prepared by existing method there is temperature sensitive, magnetic and high-hydroscopicity to be integrated, and
Have that magnetic homogeneity is poor, magnetic content is unstable, magnetic is weaker and the technical problem of low intensity, the present invention is intended to provide a kind of gram
Take the preparation method of the temperature sensitive magnetic water-absorbing resin of high intensity of above mentioned problem.Using temperature sensitive magnetic water-absorbing resin have concurrently water imbibition,
Temperature sensitive and magnetic, use it for removing fine mineral moisture, resin is with after fine mineral mixed dehydration, passing through magnetic separation or the sieve that shakes
Mode temperature sensitive magnetic water-absorbing resin is separated from fine mineral.
The present invention is achieved through the following technical solutions：A kind of preparation method of the temperature sensitive magnetic high hydroscopic resin of high intensity,
Comprise the following steps：
（1）With raw material FeCl2And FeCl3The solution that concentration is 1.0-2.0mol/L is respectively configured, is 1.0- with concentration
3.0mol/L sodium hydroxide solution is added dropwise in same container simultaneously, and three's mol ratio is 1:1:2-1:3:6, in water-bath plus
Hot 40-90 DEG C, stirred under nitrogen atmosphere 1-2 hours form colloidal solution；Backward colloidal solution in add citric acid, You Jibiao
Face dressing agent and Coaseries kaolin, the citric acid, organic surface modification agent and Coaseries kaolin and raw material FeCl2Mol ratio
For 0.1:1:0.1:1-0.3:2:0.3:1, stir 1-2 hours, it is standby, it is designated as product A；
（2）Under nitrogen protection, by water, acrylic acid, PAA, crosslinking agent using mol ratio as 10:1:0.5:0.01-
10:3:3:0.05 sequentially add after stir half an hour, add initiator afterwards, the mol ratio of the initiator and acrylic acid is
0.03：1 -0.06：1, product A is added afterwards, FeCl in the mixed solution2And FeCl3Total mole number and step（2）Reclaimed water
Mol ratio be 0.01:1-0.03:1, in 10-90 DEG C of reaction 1.0-2.0 hour of heating water bath, it is designated as product B；
（3）Temperature sensitive monomer is soluble in water, and the mol ratio of temperature sensitive monomer and water is 0.1:1-0.3:1, the temperature sensitive monomer
With step（2）The mol ratio ratio of middle acrylic acid is 1:1-3:1, it is then added in product B, adds crosslinking agent, initiator, stir
Mix 10 minutes, and in 10-50 DEG C of reaction 3.0-24.0 hour of heating water bath；Crosslinking agent and acrylic acid described in this step rub
You are than being 0.01:1-0.03:1；The mol ratio of initiator and acrylic acid described in this step is 0.03:1-0.08:1；
（4）Finally step (3) products obtained therefrom is separated under the suction in magnetic field, products therefrom vacuum is done afterwards
It is dry to produce product.
Further, step（1）Middle organic surface modification agent is in oleic acid, tetraethyl orthosilicate, KH-570 silane couplers
Any one.
Further, step（2）Described crosslinking agent is divinylbenzene, diisocyanate, N, N- methylene bisacrylamides
Any one in acid amides；Described initiator is azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN hydrochloric acid potassium, mistake
Any one in ammonium sulfate.
Further, step（3）Described temperature sensitive monomer is NIPA, vinyl acetate, oxirane, ring
Any one in Ethylene Oxide.
Further, step（3）Described crosslinking agent is hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, first
Any one in base hydroxypropyl acrylate, divinylbenzene, DAAM.
Further, step（3）Described in initiator for azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN
Any one in hydrochloric acid potassium, ammonium persulfate.
Beneficial effects of the present invention：The present invention is with FeCl2And FeCl3For raw material, while it is molten to add sodium hydroxide synthesis colloid
Liquid, and then add citric acid, organic surface modification agent and Coaseries kaolin, afterwards using water, acrylic acid, PAA, it is temperature sensitive
The temperature sensitive magnetic water-absorbing resin of monomer, crosslinking agent, initiator synthesizing high-strength, wherein citric acid can make the solid in colloidal solution
Particle stabilized suspension, organic surface modification agent can be such that magnetic-particle uniformly firmly wraps up, and Coaseries kaolin can play enhancing
The effect of mechanical strength of resin.Therefore, the temperature sensitive magnetic water-absorbing resin intensity synthesized by this method is good, improves the repetition of water-absorbing resin
Utilization rate, reduce production cost.
Brief description of the drawings
Fig. 1 is the Magnetic Test result schematic diagram of sample obtained by the specific embodiment of the invention.
SEM photograph before the products obtained therefrom use of Fig. 2 embodiments 1.
SEM photograph after the products obtained therefrom use of Fig. 3 embodiments 1.
SEM photograph before the products obtained therefrom use of Fig. 4 embodiments 2.
SEM photograph after the products obtained therefrom use of Fig. 5 embodiments 2.
SEM photograph before the products obtained therefrom use of Fig. 6 embodiments 3.
SEM photograph after the products obtained therefrom use of Fig. 7 embodiments 3.
Fig. 8 is the Thermo-sensitive measurement result schematic diagram of sample obtained by the specific embodiment of the invention.
Embodiment
A kind of preparation method of the temperature sensitive magnetic water-absorbing resin of high intensity, comprises the following steps：
（1）With raw material FeCl2And FeCl3It is 1.0-2.0mol/L that concentration, which is respectively configured,（1.0 mol/L, 1.2 can be used
mol/L、1.5 mol/L、1.8 mol/L、2.0 mol/L）Solution, be 1.0-3.0mol/L with concentration（1.0mol/ can be used
L、1.5mol/L、2.0mol/L、2.5mol/L、3.0mol/L）Sodium hydroxide solution simultaneously be added dropwise in same container, three
Person's mol ratio is 1:1:2-1:3:6（It may be selected 1:1:2、1:1:4、1:3:6）, in 40-90 DEG C of heating water bath（Optional 70 DEG C,
40℃、50℃、60℃、80℃、90℃）, stirred under nitrogen atmosphere 1-2 hours form colloidal solution；Backward colloidal solution in
Add citric acid, organic surface modification agent and Coaseries kaolin, the citric acid, organic surface modification agent and Coaseries kaolin with
Raw material FeCl2Mol ratio be 0.1:1:0.1:1-0.3:2:0.3:1（It may be selected 0.1:1:0.1:1、0.2:2:0.2:1、0.3:
2:0.3:1）, stir 1-2 hours, it is standby, it is designated as product A；
（2）Under nitrogen protection, by water, acrylic acid, PAA, crosslinking agent using mol ratio as 10:1:0.5:0.01-
10:3:3:0.05（It may be selected 10:1:0.5:0.01、10:1.5:1.5:0.02、10:2:2.0:0.03、10:3:3:0.05）According to
Stirred half an hour after secondary addition, add initiator afterwards, the mol ratio of the initiator and acrylic acid is 0.03:1 -0.06:1
（It may be selected 0.03:1、0.04:1、0.05:1、0.06:1）, product A is added afterwards, FeCl in the mixed solution2And FeCl3
Total mole number and step（2）The mol ratio of reclaimed water is 0.01:1-0.03:1（It may be selected 0.01:1、0.02:1、0.03:1）, in water
10-90 DEG C of bath heating（It may be selected 70 DEG C, 40 DEG C, 50 DEG C, 10 DEG C, 80 DEG C, 90 DEG C）1.0-2.0 hours are reacted, are designated as product B；
（3）Temperature sensitive monomer is soluble in water, and the mol ratio of temperature sensitive monomer and water is 0.1:1-0.3:1（It may be selected 0.1:1、
0.2:1、0.3:1）, the temperature sensitive monomer and step（2）The mol ratio ratio of middle acrylic acid is 1:1-3:1（It may be selected 1:1、1.5:
1.0、2:1、3:1）, it is then added in product B, adds crosslinking agent, initiator, stirs 10 minutes, and in heating water bath 10-
50℃（It may be selected 30 DEG C, 40 DEG C, 50 DEG C, 10 DEG C, 20 DEG C）React 3.0-24.0 hours（May be selected 9 hours, 6 hours, it is 12 small
When, 15 hours, 24 hours, 18 hours, 21 hours）；The mol ratio of crosslinking agent and acrylic acid described in this step is 0.01:1-
0.03:1（It may be selected 0.01:1、0.02:1、0.03:1）；The mol ratio of initiator and acrylic acid described in this step be for
0.03:1-0.08:1（It may be selected 0.03:1、0.04:1、0.05:1、0.7:1、0.08:1）；
（4）Finally step (3) products obtained therefrom is separated under the suction in magnetic field, products therefrom vacuum is done afterwards
It is dry to produce product.
Step（1）Middle organic surface modification agent is any one in oleic acid, tetraethyl orthosilicate, KH-570 silane couplers
Kind.
Step（2）Described crosslinking agent is appointing in divinylbenzene, diisocyanate, N,N methylene bis acrylamide
Meaning is a kind of；Described initiator is in azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN hydrochloric acid potassium, ammonium persulfate
Any one, step（3）Described temperature sensitive monomer is NIPA, vinyl acetate, oxirane, expoxy propane
In any one.
Step（3）Described crosslinking agent is hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, methacrylic acid
Any one in hydroxypropyl acrylate, divinylbenzene, DAAM.
Step（3）Described in initiator for azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN hydrochloric acid potassium, mistake
Any one in ammonium sulfate.
The present invention is further illustrated below by embodiment, but is not limited to following examples.
Molar concentration 1.0mol/L and 1.0mol/L FeCl is respectively configured in embodiment 12And FeCl3Solution 10ml, with
1.0mol/L sodium hydroxide solutions 20ml is added dropwise simultaneously, and in 40 DEG C of heating water bath, it is molten that stirred under nitrogen atmosphere forms colloid in 1 hour
Liquid.0.192g citric acids, 2.82g oleic acid and 0.258g Coaseries kaolins are added afterwards, are stirred 1 hour, it is standby, it is designated as product A；
Under nitrogen protection, by 36g water, 14.4g acrylic acid, 9.4g PAAs, 0.308g N, N- methylene bisacrylamides
Acid amides, stirred half an hour after sequentially adding, add 1.369g ammonium persulfates afterwards, then product A is added, added in 90 DEG C of water-baths
Heat, react 1.0 hours, be designated as product B；
22.72g NIPAs are dissolved in 36g water, is then added in product B, adds 0.232g
Hydroxy-ethyl acrylate, 1.382g azo-bis-iso-dimethyls, stir 10 minutes, and in 50 DEG C of heating in water bath for reaction 3.0 hours,
Products therefrom is dried in vacuo, and ferroso-ferric oxide content is 22% after measured, its saturation magnetization 61emu/g（Such as Fig. 1 curves
a）, water absorption rate (SR) is up to 585g/g, lowest critical solution temperature at room temperature（LCST）For 31 DEG C（Such as Fig. 8 curves a）.
Molar concentration 1.5mol/L and 1.5mol/L FeCl is respectively configured in embodiment 22And FeCl3Solution 10ml, with
2.0mol/L sodium hydroxide solutions 30ml is added dropwise simultaneously, and in 60 DEG C of heating water bath, stirred under nitrogen atmosphere forms colloid in 1.5 hours
Solution.0.576g citric acids, 7.45g KH-570 silane couplers and 0.776g Coaseries kaolins are added afterwards, and stirring 1.5 is small
When, it is standby, it is designated as product A；
Under nitrogen protection, by 54g water, 32.4g acrylic acid, 42.3g PAAs, 0.925g N, N- di-2-ethylhexylphosphine oxide third
Acrylamide, stirred half an hour after sequentially adding, add 4.107g ammonium persulfates afterwards, then product A added, in 50 DEG C of water-baths
Heating, react 1.5 hours, be designated as product B；
77.48g vinyl acetates are dissolved in 81g water, are then added in product B, add 0.775g metering systems
Acid, 4.145g azo-bis-iso-dimethyls, stir 10 minutes, and in 30 DEG C of heating in water bath for reaction 12.0 hours, products therefrom
Vacuum drying, ferroso-ferric oxide content is 26% after measured, its saturation magnetization 63.7emu/g（Such as Fig. 1 curves b）, at room temperature
Water absorption rate (SR) is up to 668g/g, lowest critical solution temperature（LCST）For 32 DEG C（Such as Fig. 8 curves b）.
Molar concentration 2.0mol/L and 2.0mol/L FeCl is respectively configured in embodiment 32And FeCl3Solution 10ml, with
3.0mol/L sodium hydroxide solutions 40ml is added dropwise simultaneously, and in 90 DEG C of heating water bath, it is molten that stirred under nitrogen atmosphere forms colloid in 2 hours
Liquid.1.153g citric acids, 11.29g oleic acid and 1.549g Coaseries kaolins are added afterwards, are stirred 2 hours, it is standby, it is designated as product
A；
Under nitrogen protection, by 48g water, 57.6g acrylic acid, 75.2g PAAs, 1.736g divinylbenzenes, successively
Stirred after addition half an hour, add 10.95g ammonium persulfates afterwards, then product A is added, in 40 DEG C of heating water baths, reaction
2.0 hours, it is designated as product B；
271.58g NIPAs are dissolved in 144g water, is then added in product B, adds
2.787g hydroxy-ethyl acrylates, 14.73g azo-bis-iso-dimethyls, stir 10 minutes, and in 50 DEG C of heating in water bath for reaction
24.0 hours, products therefrom vacuum drying, ferroso-ferric oxide content was 20% after measured, its saturation magnetization 69.6emu/g
（Such as Fig. 1 curves c）, water absorption rate (SR) is up to 717g/g, lowest critical solution temperature at room temperature（LCST）For 34 DEG C（Such as Fig. 8
Curve c）.
The water absorption rate of products therefrom of the present invention can be in 60-70 emu/g in 500-715 g/g, magnetic.SEM photograph table
The magnetic-particle of the bright temperature sensitive magnetic water-absorbing resin of synthesizing high-strength is evenly distributed.Fig. 2,3 are respectively that the products obtained therefrom of embodiment 1 uses
Front and rear SEM photograph, the SEM photograph before and after the respectively products obtained therefrom use of embodiment 2 of Fig. 4,5, Fig. 6,7 are respectively embodiment 3
SEM photograph before and after products obtained therefrom use.It can be seen that resin is strong using the contrast of the temperature sensitive magnetic water-absorbing resin of front and rear high intensity
Degree is preferable.
Claims (6)
1. a kind of preparation method of the temperature sensitive magnetic water-absorbing resin of high intensity, it is characterised in that comprise the following steps：
（1）With raw material FeCl2And FeCl3The solution that concentration is 1.0-2.0mol/L is respectively configured, is 1.0-3.0mol/L with concentration
Sodium hydroxide solution simultaneously be added dropwise in same container, three's mol ratio be 1:1:2-1:3:6, in heating water bath 40-90
DEG C, stirred under nitrogen atmosphere 1-2 hours form colloidal solution；Backward colloidal solution in add citric acid, organic surface modification
Agent and Coaseries kaolin, the citric acid, organic surface modification agent and Coaseries kaolin and raw material FeCl2Mol ratio be 0.1:
1:0.1:1-0.3:2:0.3:1, stir 1-2 hours, it is standby, it is designated as product A；
（2）Under nitrogen protection, by water, acrylic acid, PAA, crosslinking agent using mol ratio as 10:1:0.5:0.01-10:3:
3:0.05 sequentially add after stir half an hour, add initiator afterwards, the mol ratio of the initiator and acrylic acid is 0.03：1
-0.06：1, product A is added afterwards, FeCl in the mixed solution2And FeCl3Total mole number and step（2）Mole of reclaimed water
Than for 0.01:1-0.03:1, in 10-90 DEG C of reaction 1.0-2.0 hour of heating water bath, it is designated as product B；
（3）Temperature sensitive monomer is soluble in water, and the mol ratio of temperature sensitive monomer and water is 0.1:1-0.3:1, the temperature sensitive monomer is with walking
Suddenly（2）The mol ratio of middle acrylic acid is 1:1-3:1, it is then added in product B, adds crosslinking agent, initiator, stirs 10 points
Clock, and in 10-50 DEG C of reaction 3.0-24.0 hour of heating water bath；The mol ratio of crosslinking agent and acrylic acid described in this step is
0.01:1-0.03:1；The mol ratio of initiator and acrylic acid described in this step is 0.03:1-0.08:1；
（4）Finally step (3) products obtained therefrom is separated under the suction in magnetic field, products therefrom vacuum drying afterwards is
Obtain product.
A kind of 2. preparation method of the temperature sensitive magnetic water-absorbing resin of high intensity according to claim 1, it is characterised in that：It is organic
Coating material is any one in oleic acid, tetraethyl orthosilicate, KH-570 silane couplers.
A kind of 3. preparation method of the temperature sensitive magnetic water-absorbing resin of high intensity according to claim 1 or 2, it is characterised in that：
Step（2）Described in crosslinking agent be divinylbenzene, it is diisocyanate, any one in N,N methylene bis acrylamide
Kind；Described initiator is any in azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN hydrochloric acid potassium, ammonium persulfate
It is a kind of.
A kind of 4. preparation method of the temperature sensitive magnetic water-absorbing resin of high intensity according to claim 1 or 2, it is characterised in that：
Step（3）Described temperature sensitive monomer is any in NIPA, vinyl acetate, oxirane, expoxy propane
It is a kind of.
A kind of 5. preparation method of the temperature sensitive magnetic water-absorbing resin of high intensity according to claim 1 or 2, it is characterised in that：
Step（3）Described crosslinking agent is hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, hydroxy propyl methacrylate, two
Any one in vinyl benzene, DAAM.
A kind of 6. preparation method of the temperature sensitive magnetic water-absorbing resin of high intensity according to claim 1 or 2, it is characterised in that：
Step（3）Described in initiator be azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN hydrochloric acid potassium, in ammonium persulfate
Any one.
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