CN105777974B - A kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin - Google Patents
A kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin Download PDFInfo
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- CN105777974B CN105777974B CN201610163954.3A CN201610163954A CN105777974B CN 105777974 B CN105777974 B CN 105777974B CN 201610163954 A CN201610163954 A CN 201610163954A CN 105777974 B CN105777974 B CN 105777974B
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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
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08J2333/00—Characterised 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
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
Abstract
The invention discloses a kind of preparation method for the temperature sensitive magnetic high hydroscopic resin being dehydrated for fine mineral, belong to functional material and solid-liquid separation technique field.The composite is first with raw material FeSO4∙7H2O and Fe (NO3)3∙9H2O formation colloidal solution, adds PAA, acrylic acid, temperature sensitive monomer, crosslinking agent and initiator afterwards.Synthesized temperature sensitive magnetic high hydroscopic resin has lowest critical solution temperature（LCST）, the moisture in the resin after water suction is regenerated after deviating from non-phase transformation mode.This method can quickly prepare the high hydroscopic resin with the composite construction for stablizing temperature sensitive magnetic, can apply to the dehydration of fine mineral raw material.
Description
Technical field
The invention belongs to functional material and solid-liquid separation technique field, it is related to a kind of temperature sensitive magnetic being dehydrated for fine mineral
Property high hydroscopic resin preparation method, this method can quickly prepare with stablize temperature sensitive magnetic composite construction super absorbent resin
Fat.
Background technology
Temperature sensitive magnetic high hydroscopic resin be it is a kind of have high-hydroscopicity concurrently, the function that three kinds of characteristics of Thermo-sensitive and magnetic are integrated
High polymer material.Chinese patent CN103172958A discloses a kind of Thermo-sensitive epoxy resin composite material and preparation method thereof,
It is mainly used in the fields such as smart coatings and functional plastics.Chinese patent CN104072693A discloses a kind of Thermo-sensitive and gathered
Compound is grafted the preparation method of carbon ball compound, and main purpose is the application for expanding carbon material carbon ball.Other Chinese patent
CN103657546A discloses a kind of method for preparing core-shell structure magnetic compound resin microballoon, and the oxidation of magnetic four three is prepared first
Fe nanometer particles, then under the conditions of microwave hydrothermal, using ferriferrous oxide nano-particle as seed, phenol and formaldehyde pass through original position
Polymerization is coated to the surface of ferroso-ferric oxide.Above patent adds solid magnetic material during synthesizing magnetic high polymer material
Particle is difficult to avoid the shortcomings of magnetic homogeneity is poor, magnetic content is low, magnetic is weaker, is provided simultaneously with high-hydroscopicity, Thermo-sensitive and magnetic
The resin of three kinds of good characteristics of property is particularly difficult.
Current fine mineral dehydration is a big technical barrier of mineral processing and utilization industry, using super absorbent resin to thin
It is a kind of brand-new method that moisture in fine mineral is removed by means of absorbent material that grain mineral, which carry out dehydration, but high water absorption
Property resin removing fine mineral in moisture, its dehydration is easily controlled, and the recovery of resin and regenerated highly difficult after absorbing water.
Therefore synthesize temperature sensitive magnetic high hydroscopic resin to be dehydrated applied to fine mineral, by magnetic separation separation resin, afterwards by temperature sensitive
Property recycled with non-phase transformation dehydration regeneration, be also to solve fine mineral dehydration technique problem so as to save big energy
Break through, be theoretical extension and the technology application for realizing fine mineral dehydration.
The content of the invention
For the water-absorbing resin prepared by existing method it is different when there is temperature sensitive, magnetic and high-hydroscopicity to be integrated, and
There is the technical problem that magnetic homogeneity is poor, magnetic content is unstable, magnetic is weaker, the present invention is intended to provide one kind overcomes above-mentioned ask
The preparation method of the temperature sensitive magnetic high hydroscopic resin of topic.Have water imbibition concurrently using temperature sensitive magnetic water-absorbing resin, temperature sensitive and magnetic, will
It is used to remove fine mineral moisture, and resin is with after fine mineral mixed dehydration, being absorbed water temperature sensitive magnetic by magnetic separation method
Resin is separated from fine mineral, can be recycled after being dehydrated by temperature change with non-phase transformation.The present invention is by following
Technical scheme is realized：A kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, comprises the following steps：
（1）With raw material FeSO4∙7H2O and Fe (NO3)3∙9H2The solution that concentration is 0.5-1.2mol/L is respectively configured in O, and dense
The ammonia spirit for 1.0-2.5mol/L is spent while being added dropwise in same container, and three's molar ratio is 1:1:1.5-1:3:3,
In 40-90 DEG C of heating water bath, stirred under nitrogen atmosphere forms colloidal solution in 1-2 hours；
Under nitrogen protection, by organic media and water with volume ratio 10:1-10:6 mixing, then add above-mentioned colloidal solution
And be uniformly mixed, FeSO in mixed solution4∙7H2O and Fe (NO3)3∙9H2O quality sum and the mass ratio of organic media
For 3:100-7:30, PAA, acrylic acid, crosslinking agent, initiator stirring are added under agitation afterwards, in heating water bath
10-90 DEG C is reacted 0.5-1.0 hours；Described PAA and the mass ratio of organic media are 1:3-1:10；Described propylene
The mass ratio of sour sodium and acrylic acid is 1:0.1-1:0.5；The mass ratio of crosslinking agent and PAA described in this step is
0.01:1-0.03:1；The mass ratio of initiator and PAA described in this step is 0.03:1-0.07:1；
（2）Temperature sensitive monomer solution is formed after the dissolving of temperature sensitive monomer, its dissolving medium used is water, ethanol or water and second
Alcohol mixed solvent, then adds step by temperature sensitive monomer solution（1）Reaction system in；Dissolving medium is mixed using water and ethanol
During solvent, both its reclaimed water and ethanol volume ratio are 1:1-1:4；The temperature sensitive monomer is 0.1 with dissolving medium mass ratio：1-
0.5:1；The mass ratio of the temperature sensitive monomer and PAA is 0.5:1-1.5:1；
Crosslinking agent, initiator are added, is stirred, and in reaction 1-6 hours of 10-50 DEG C of heating water bath；Described in this step
Crosslinking agent and PAA mass ratio be 0.02:1-0.06:1；The matter of initiator and PAA described in this step
Amount is than being 0.06:1-0.15:1；
（3）Finally step (2) products obtained therefrom is separated under the suction of magnet, products therefrom vacuum is done afterwards
It is dry to produce product.
Further, step（1）Described raw material FeSO4∙7H2O and Fe (NO3)3∙9H2The matter of O gross masses and PAA
Amount is than being 0.3:1-0.7:1.
Further, step（1）Described organic media is any one in hexamethylene, normal heptane, ethylbenzene, dimethylbenzene
Or any two kinds of mixture；When using two kinds of organic medias, the volume ratio of the two is 1:1-1:5；The statement refers to, ring
Optional two kinds of independent assortments in hexane, normal heptane, ethylbenzene, dimethylbenzene, and can use the volume ratio.
Further, step（2）Described temperature sensitive monomer is NIPA, methylcellulose, hydroxypropyl
Appointing in cellulose, polyvinyl alcohol, vinyl acetate, N, N- acrylamides, expoxy propane, oxirane, styrene
Anticipate the mixtures of one or any two kinds of monomers, when using two kinds of materials, the two mass ratio is 3:1-5:1；The statement is
Refer to：When choosing is with above-mentioned any two kinds of material independent assortments, the mass ratio can be used.
Further, step（1）Described crosslinking agent is divinylbenzene, diisocyanate, N, N- methylene bisacrylamides
Any one in acid amides.
Further, step（1）Described in initiator be azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN
Any one in hydrochloric acid potassium, ammonium persulfate, benzoyl peroxide.
Further, step（2）Described crosslinking agent is hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, first
In base hydroxy-ethyl acrylate, hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, DAAM
Any one.
Further, step（2）Described in initiator be azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN
Any one in hydrochloric acid potassium, ammonium persulfate.
Step（3）The lowest critical solution temperature that described fine mineral is dehydrated temperature sensitive magnetic high hydroscopic resin is 30-50
℃。
Beneficial effects of the present invention：The present invention is with FeSO4∙7H2O and Fe (NO3)3∙9H2O is Material synthesis colloidal solution,
And then resin monomer, temperature sensitive raw material, crosslinking agent and initiator are added, uniform firm parcel is formed to magnetic ferroferric oxide,
The problem of magnetic homogeneity of existing preparation magnetic water-absorbing resin presence is poor, magnetic content is low, magnetic is weaker can be overcome；Simultaneously
Make resin that there is high-hydroscopicity, Thermo-sensitive and magnetic, using its characteristic, can both complete resin to the efficiently de- of fine mineral
Water, can relatively easily realize the recycling of resin again.
Brief description of the drawings
Fig. 1 is the Magnetic Test result schematic diagram of sample obtained by the specific embodiment of the invention.
Fig. 2 is the SEM photograph of sample obtained by the specific embodiment of the invention.
Fig. 3 is the Thermo-sensitive measurement result schematic diagram of sample obtained by the specific embodiment of the invention.
Embodiment
A kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, comprises the following steps：
（1）With raw material FeSO4∙7H2O and Fe (NO3)3∙9H2Concentration is respectively configured for 0.5-1.2mol/L in O（0.5 can be used
mol/L、0.7 mol/L、1.2 mol/L、1.0 mol/L）Solution, with concentration be 1.0-2.5mol/L（1.0 can be used
mol/L、1.5 mol/L、2.0 mol/L、2.5mol/L）Ammonia spirit simultaneously be added dropwise in same container, three mole
Ratio is 1:1:1.5-1:3:3（It may be selected 1:1:1.5、1:1.5:2.5、1:3:3）, in 40-90 DEG C of heating water bath（It may be selected 70
℃、40℃、50℃、60℃、80℃、90℃）, 1-2 hours formation colloidal solution of stirred under nitrogen atmosphere；
Under nitrogen protection, by organic media and water with volume ratio 10:1-10:6（It may be selected 10:2、10:1、10:3、10:
6、10:5、10:4）Mixing, then adds above-mentioned colloidal solution and is uniformly mixed, FeSO in mixed solution4∙7H2O and Fe
(NO3)3∙9H2O quality sum and the mass ratio of organic media are 3:100-7:30（It may be selected 3:100、5:50、7:30）, it
PAA, acrylic acid, crosslinking agent, initiator stirring are added under agitation afterwards, in 10-90 DEG C of heating water bath（It may be selected
30℃、50℃、90℃、70℃、10℃）Reaction 0.5-1.0 hours；Described PAA and the mass ratio of organic media are 1:
3-1:10（It may be selected 1:9、1:10、1:3、1:5、1:7）；Described PAA and the mass ratio of acrylic acid are 1:0.1-1:
0.5（It may be selected 1:0.3、1:0.1、1:0.5）；The mass ratio of crosslinking agent and PAA 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 mass ratio of initiator and PAA described in this step is
0.03:1-0.07:1（It may be selected 0.03:1、0.05:1、0.07:1）；
（2）Temperature sensitive monomer solution is formed after the dissolving of temperature sensitive monomer, its dissolving medium used is water, ethanol or water and second
Alcohol mixed solvent, then adds step by temperature sensitive monomer solution（1）Reaction system in；Dissolving medium is mixed using water and ethanol
During solvent, both its reclaimed water and ethanol volume ratio are 1:1-1:4（It may be selected 1:1、1: 3、1: 2、1: 4）；The temperature sensitive monomer
It is 0.1 with dissolving medium mass ratio：1-0.5:1（0.1：1、0.5:1、0.4:1、0.3:1、0.2:1）；The temperature sensitive monomer and third
The mass ratio of olefin(e) acid sodium is 0.5:1-1.5:1（It may be selected 1.5:1、0.5:1、0.7:1、0.9:1、1.1:1、1.3:1）；
Crosslinking agent, initiator are added, is stirred, and in 10-50 DEG C of heating water bath（May be selected 30 DEG C, 20 DEG C, 40 DEG C, 50
℃、10℃）Reaction 1-6 hours（May be selected 2,3,5,4,6 hours）；The quality of crosslinking agent and PAA described in this step
Than for 0.02:1-0.06:1（It may be selected 0.03:1、0.06:1、0.04:1、0.05:1、0.02:1）；Drawing described in this step
The mass ratio for sending out agent and PAA is 0.06:1-0.15:1（It may be selected 0.09:1、0.06:1、0.12:1、0.15:1）；
（3）Finally step (2) products obtained therefrom is separated under the suction of magnet, products therefrom vacuum is done afterwards
It is dry to produce product.
Step（1）Described raw material FeSO4∙7H2O and Fe (NO3)3∙9H2The mass ratio of O gross masses and PAA is
0.3:1-0.7:1（It may be selected 0.3:1、0.5:1、0.7:1）.
Step（1）Described organic media is any one in hexamethylene, normal heptane, ethylbenzene, dimethylbenzene or any
Two kinds of mixture；When using two kinds of organic medias, the volume ratio of the two is 1:1-1:5（It may be selected 1:1、1:1.2、1:
1.5、1：1.3、1:1.4）.
Step（2）Described temperature sensitive monomer is NIPA, methylcellulose, hydroxy propyl cellulose, poly-
In vinyl alcohol, vinyl acetate, N, N- acrylamides, expoxy propane, oxirane, styrene any one or
The mixture of any two kinds of monomers of person, when using two kinds of materials, the two mass ratio is 3:1-5:1（It may be selected 3:1、4:1、5:
1）.
Step（1）Described crosslinking agent is times in divinylbenzene, diisocyanate, N,N methylene bis acrylamide
Meaning is a kind of.
Step（1）Described in initiator be azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN hydrochloric acid potassium, mistake
Any one in ammonium sulfate, benzoyl peroxide.
Step（2）Described crosslinking agent is hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, methacrylic acid
It is any one in hydroxyl ethyl ester, hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, DAAM
Kind.
Step（2）Described in initiator be 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 0.5mol/L and 1.0mol/L FeSO is respectively configured in embodiment 14∙7H2O and Fe (NO3)3∙9H2O
Solution 10ml, is added dropwise simultaneously with 2.0mol/L ammonia spirits 15ml, in 60 DEG C of heating water bath, 1 hour shape of stirred under nitrogen atmosphere
Into colloidal solution.
Under nitrogen protection, 50ml hexamethylenes, 25ml ethylbenzene and 20ml water are added into above-mentioned sol solution simultaneously and stirred
It is well mixed, once add 8g PAAs, 2g acrylic acid, 0.08g crosslinking agents N, N- di-2-ethylhexylphosphine oxide under agitation afterwards
Acrylamide, 0.24g initiator ammonium persulfates, in heating water bath, 50 DEG C are reacted 0.5 hour.
4g NIPAs are dissolved in 20ml water, above-mentioned reaction system is subsequently added into, is eventually adding 0.2g
Crosslinking agent hydroxy-ethyl acrylate and 0.5g initiator azo-bis-iso-dimethyls, stirring, then in 40 DEG C of reactions 2 of heating water bath
Hour.Products therefrom is dried in vacuo, and ferroso-ferric oxide content is 33%, its saturation magnetization 123emu/g after measured（As schemed
1a）, water absorption rate at room temperature（SR）Up to 972g/g, lowest critical solution temperature（LCST）For 32 DEG C（Such as Fig. 3 a）.
Molar concentration 1.0mol/L and 1.0mol/L FeSO is respectively configured in embodiment 24∙7H2O and Fe (NO3)3∙9H2O
Solution 10ml, is added dropwise simultaneously with 2.5mol/L ammonia spirits 20ml, in 80 DEG C of heating water bath, 2 hours shapes of stirred under nitrogen atmosphere
Into colloidal solution.
Under nitrogen protection, 100ml hexamethylenes and 10ml water are added into above-mentioned sol solution simultaneously and are uniformly mixed,
Once add 20g PAAs, 8g acrylic acid, 0.4g crosslinking agents diisocyanate, 0.8g initiators under agitation afterwards
Azo dicyclohexyl formonitrile HCN hydrochloric acid potassium, in heating water bath, 30 DEG C are reacted 1.0 hours.
14g NIPAs and 6g oxirane are dissolved in 180ml water, above-mentioned reaction system is subsequently added into,
1.0g crosslinking agents methacrylic acid and 1.5g initiator ammonium persulfates are eventually adding, is stirred, then in 50 DEG C of reactions 4 of heating water bath
Hour.Products therefrom is dried in vacuo, and ferroso-ferric oxide content is 27%, its saturation magnetization 75emu/g after measured（As schemed
1b）, water absorption rate (SR) is up to 650g/g, lowest critical solution temperature at room temperature（LCST）For 42 DEG C（Such as Fig. 3 b）.
Water absorption rate can be in 500-972 g/g, and magnetic can show that synthesizing temperature sensitive magnetic inhales in 70-123 emu/g. SEM photographs
The magnetic-particle of water-resin is evenly distributed.Fig. 2 a are the SEM photograph of the products obtained therefrom of embodiment 1, and Fig. 2 b are the products obtained therefrom of embodiment 2
SEM photograph.
Claims (10)
1. a kind of fine mineral is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is characterised in that comprise the following steps：
（1）With raw material FeSO4∙7H2O and Fe (NO3)3∙9H2The solution that concentration is 0.5-1.2mol/L is respectively configured in O, is with concentration
1.0-2.5mol/L ammonia spirit is added dropwise in same container simultaneously, and three's molar ratio is 1:1:1.5-1:3:3, in water
40-90 DEG C of bath heating, stirred under nitrogen atmosphere forms colloidal solution in 1-2 hours；
Under nitrogen protection, by organic media and water with volume ratio 10:1-10:6 mixing, then add above-mentioned colloidal solution and stir
Mix well mixed, FeSO in mixed solution4∙7H2O and Fe (NO3)3∙9H2O quality sum and the mass ratio of organic media are 3:
100-7:30, PAA, acrylic acid, crosslinking agent, initiator stirring are added under agitation afterwards, in heating water bath 10-
90 DEG C are reacted 0.5-1.0 hours；Described PAA and the mass ratio of organic media are 1:3-1:10；Described PAA
Mass ratio with acrylic acid is 1:0.1-1:0.5；The mass ratio of crosslinking agent and PAA described in this step is 0.01:1-
0.03:1；The mass ratio of initiator and PAA described in this step is 0.03:1-0.07:1；
（2）Temperature sensitive monomer solution is formed after the dissolving of temperature sensitive monomer, its dissolving medium used is that water, ethanol or water and ethanol are mixed
Bonding solvent, then adds step by temperature sensitive monomer solution（1）Reaction system in；Dissolving medium uses water and alcohol mixed solvent
When, both its reclaimed water and ethanol volume ratio are 1:1-1:4；The temperature sensitive monomer is 0.1 with dissolving medium mass ratio：1-0.5:1；
The mass ratio of the temperature sensitive monomer and PAA is 0.5:1-1.5:1；
Crosslinking agent, initiator are added, is stirred, and in reaction 1-6 hours of 10-50 DEG C of heating water bath；Friendship described in this step
The mass ratio for joining agent and PAA is 0.02:1-0.06:1；The mass ratio of initiator and PAA described in this step
For 0.06:1-0.15:1；
（3）Finally step (2) products obtained therefrom is separated under the suction of magnet, products therefrom vacuum drying afterwards is
Obtain product.
2. a kind of fine mineral according to claim 1 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, its feature
It is：Step（1）Described raw material FeSO4∙7H2O and Fe (NO3)3∙9H2The mass ratio of O gross masses and PAA is 0.3:1-
0.7:1。
3. a kind of fine mineral according to claim 1 or 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is special
Levy and be：Step（1）Described organic media is any one in hexamethylene, normal heptane, ethylbenzene, dimethylbenzene or any two
The mixture planted；When using two kinds of organic medias, the volume ratio of the two is 1:1-1:5.
4. a kind of fine mineral according to claim 1 or 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is special
Levy and be：Step（2）Described temperature sensitive monomer is NIPA, vinyl acetate, N, N- diethyl acryloyls
The mixture of any one or any two kinds in amine, expoxy propane, oxirane；When using two kinds of materials, the two matter
Amount is than being 3:1-5:1.
5. a kind of fine mineral according to claim 1 or 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is special
Levy and be：Step（1）Described crosslinking agent is times in divinylbenzene, diisocyanate, N,N methylene bis acrylamide
Meaning is a kind of.
6. a kind of fine mineral according to claim 1 or 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is special
Levy and be：Step（1）Described in initiator be azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN hydrochloric acid potassium, mistake
Any one in ammonium sulfate, benzoyl peroxide.
7. a kind of fine mineral according to claim 1 or 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is special
Levy and be：Step（2）Described crosslinking agent is hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, hydroxyethyl methacrylate
Any one in ethyl ester, hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, DAAM.
8. a kind of fine mineral according to claim 3 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, its feature
It is：Step（2）Described crosslinking agent is hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid, hydroxyethyl methacrylate second
Any one in ester, hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, DAAM.
9. a kind of fine mineral according to claim 1 or 2 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, it is special
Levy and be：Step（2）Described in initiator be azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN hydrochloric acid potassium, mistake
Any one in ammonium sulfate.
10. a kind of fine mineral according to claim 3 is dehydrated the preparation method of temperature sensitive magnetic high hydroscopic resin, its feature
It is：Step（2）Described in initiator be azo-bis-iso-dimethyl, azo dicyclohexyl formonitrile HCN hydrochloric acid potassium, over cure
Any one in sour ammonium.
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| US4707523A (en) * | 1985-10-11 | 1987-11-17 | California Institute Of Technology | Magnetic particles |
| CN103242494A (en) * | 2013-05-27 | 2013-08-14 | 上海交通大学 | Preparation method of composite microgel with temperature, pH and magnetic field sensitivities |
-
2016
- 2016-03-22 CN CN201610163954.3A patent/CN105777974B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4707523A (en) * | 1985-10-11 | 1987-11-17 | California Institute Of Technology | Magnetic particles |
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